15032_800 Chatham Rd QAPP Appendix 1_2011

APPENDIX 1
OF ADDENDUM 1.A
Site-Specific QAPP Addendum
Grant Number BF-96413504

Remedial Design and Confirmatory Sampling/Testing
CHATHAM MILL PROPERTY
800 CHATHAM ROAD
WINSTON-SALEM, NORTH CAROLINA

Laboratory Standard Operating Procedures

PROVIDED ON A SEPARATE CD
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CERTIFICATIONS 1-1
1.0 INTRODUCTION 1-2
1.1 QUALITY OBJECTIVE ...............................................................................................1-3
1.2 QUALITY MANAGEMENT SYSTEM...........................................................................1-3
1.3 INFORMATION MANAGEMENT SYSTEM ..................................................................1-7

2.0 ORGANIZATION 2-1
2.1 STAFF QUALIFICATIONS AND RESPONSIBILITIES ....................................................2-1
2.2 FACILITIES ...............................................................................................................2-5
2.3 EQUIPMENT AND INSTRUMENTATION .....................................................................2-5

3.0 QUALITY PROGRAM PLAN 3-1
3.1 DOCUMENTING ........................................................................................................ 3-1
3.1.1 The Quality Assurance Manual ................................................................. 3-1
3.1.2 Standard Operating Procedures/Methods Manual ..................................... 3-1
3.1.3 Revisions to SOPs...................................................................................... 3-3
3.1.4 Documenting Method Specific Deviations ................................................ 3-3
3.1.5 Documenting Project Specific Deviations ................................................. 3-7
3.2 TRAINING ................................................................................................................ 3-8
3.2.1 Team Training ...........................................................................................3-8
3.2.2 External Training .......................................................................................3-9 3.2.3 Quality Training ........................................................................................3-9 3.2.4 Health and Safety Training ........................................................................3-10 3.3 ASSESSING ADHERENCE AND COMMUNICATING FINDINGS....................................3-10
3.3.1 Data Review ...............................................................................................3-11
3.3.2 Corrective Action Program ........................................................................3-12
3.3.3 QA Management Meetings ........................................................................3-15
3.3.4 Conducting Internal Assessments ..............................................................3-15
3.4 COMMUNICATING WITH MANAGEMENT .................................................................3-15

4.0 QUALITY OBJECTIVES 4-1
4.1 PRECISION, ACCURACY, REPRESENTATIVENESS, COMPLETENESS, AND COMPARABILITY
................................................................................................................................ 4-1
4.1.1 Precision .................................................................................................... 4-1
4.1.2 Accuracy .................................................................................................... 4-1
4.1.3 Representativeness ..................................................................................... 4-1
4.1.4 Completeness ............................................................................................. 4-1
4.1.5 Comparability ............................................................................................ 4-2
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4.2 LIMIT OF DETECTION, LIMIT OF QUANTITATION, AND
INSTRUMENT CALIBRATION REQUIREMENTS.......................................................... 4-2
4.2.1 Limit of Detection ..................................................................................... 4-2
4.2.2 Limit of Quantitation ................................................................................. 4-2
4.2.3 Instrument Calibration ............................................................................... 4-2
4.2.4 Retention Time Windows .......................................................................... 4-3
4.3 ELEMENTS OF QUALITY CONTROL .......................................................................... 4-3
4.3.1 Analytical Batch Definition ....................................................................... 4-3
4.3.2 Continuing Calibration Verification (CCV) .............................................. 4-4
4.3.3 Laboratory Control Spike (LCS) ............................................................... 4-4
4.3.4 Internal Standard (IS) ................................................................................ 4-4
4.3.5 Surrogates .................................................................................................. 4-4
4.3.6 Laboratory Blank ....................................................................................... 4-5
4.3.7 Laboratory Duplicate ................................................................................. 4-5
4.3.8 Matrix Spike .............................................................................................. 4-5
4.3.9 Field QC Samples ...................................................................................... 4-6
4.4 QUALITY CONTROL PROCEDURES .......................................................................... 4-6
4.4.1 Holding Times ........................................................................................... 4-6
4.4.2 Confirmation .............................................................................................. 4-6
4.4.3 Standard Materials ..................................................................................... 4-6 4.4.3.1 Liquid Standards ....................................................................... 4-7 4.4.3.2 Gas Standards ............................................................................ 4-7 4.4.3.3 Reagent Water ........................................................................... 4-7 4.4.4 Expiration Dates of Standards ................................................................... 4-8
4.4.4.1 Primary Standards ..................................................................... 4-8
4.4.4.2 Secondary Standards ................................................................. 4-8

5.0 SAMPLE HANDLING 5-1 5.1 SAMPLING MEDIA AND PRESERVATION REQUIREMENTS ....................................... 5-1
5.1.1 Sample Containers ..................................................................................... 5-1
5.1.1.1 SummaTM Canisters ................................................................... 5-1
5.1.1.2 Sorbent Tubes ............................................................................ 5-2
5.1.1.3 Polyurethane Foam (PUF/XAD) Cartridges ............................. 5-2
5.1.1.4 DNPH Impinger Solution and Cartridges .................................. 5-2
5.2 SAMPLE COLLECTION PROCEDURES - FIELD GUIDELINES ...................................... 5-3
5.2.1 Information for Canister Sampling ............................................................ 5-3
5.2.2 Information for Sorbent Tube Sampling .................................................... 5-4
5.3 SAMPLE RECEIVING PROCEDURES .......................................................................... 5-4
5.3.1 Sample Acceptance Policy ........................................................................ 5-4
5.3.2 The Sample Receipt Confirmation ............................................................ 5-6
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5.3.3 The Work Order Folder ............................................................................. 5-7
5.4 SAMPLE TRACKING PROCEDURES .......................................................................... 5-8
5.5 INTERNAL SAMPLE CUSTODY AND STORAGE PROCEDURES ................................... 5-10
5.6 SAMPLE DISPOSAL .................................................................................................. 5-10
5.7 SUBCONTRACTING .................................................................................................. 5-11

6.0 ANALYTICAL METHODS AND PROCEDURES 6-1
6.1 ASTM D-1945 – FIXED GASES ...............................................................................6-1
6.2 ASTM D-1946 – ATMOSPHERIC GASES .................................................................6-4
6.3 ASTM D-5504 – SULFUR COMPOUNDS ..................................................................6-7
6.4 PASSIVE SAMPLING – VOLATILE ORGANIC COMPOUNDS.......................................6-9
6.5 PM10/TSP ..............................................................................................................6-18
6.6 TO-3 – BTEX AND TPH .........................................................................................6-19
6.7 TO-4A/TO-10A – PESTICIDES AND PCBS ..............................................................6-22
6.8 TO-5, TO-11A, METHOD 0011, CARB 430 – ALDEHYDES AND KETONES ……..6-26
6.9 TO-12 – NMOC ......................................................................................................6-29
6.10 TO-13A AND 8270C – SEMIVOLATILE COMPOUNDS .............................................6-31
6.11 TO-14A/TO-15 – VOLATILE ORGANIC COMPOUNDS .............................................6-44
6.12 TO-14A/TO-15 – VOLATILE ORGANIC COMPOUNDS BY SIM ...............................6-50
6.13 TO-15 – ALIPHATIC AND AROMATIC VOLATILE PETROLEUM HYDROCARBON (VPH) FRACTIONS BY GC/MS ...........................................................................................6-53 6.14 AIR PHASE PETROLEUM HYDROCARBONS (MA APH) ...........................................6-57 6.15 TO-17 – VOLATILE ORGANIC COMPOUNDS ............................................................6-60
6.16 TO-17 – ‘VAPOR INTRUSION’ VOLATILE AND SEMIVOLATILE ORGANIC
COMPOUNDS……………………... ........................................................................6-70
6.17 PASSIVE SAMPLING ANALYZED BY THERMAL DESORPTION – VOLATILE ORGANIC
COMPOUNDS …………...........................................................................................6-75
6.18 VOST – SW-846 5041A .........................................................................................6-82

7.0 DATA COLLECTION, REVIEW, REPORTING, AND
RECORDS 7-1
7.1 DATA COLLECTION ................................................................................................. 7-1
7.2 DATA REVIEW ......................................................................................................... 7-2
7.3 FINAL REPORT PRODUCTION .................................................................................. 7-2
7.3.1 Automatic Data Transfer System............................................................... 7-2
7.3.2 Manual Data Entry System ........................................................................ 7-3
7.3.3 Report Compilation ................................................................................... 7-3
7.4 ELECTRONIC REPORTING AND REVIEW .................................................................. 7-4
7.5 eCVP/EDD AND REPORTING IN ADOBE FORMAT OR DISKETTE…………….. ........ 7-4
7.6 RECORDS OF METHOD CAPABILITY ........................................................................ 7-7
7.7 RECORD STORAGE................................................................................................... 7-7
7.8 CONFIDENTIALITY OF DATA ................................................................................... 7-9

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8.0 ESTABLISHING ACCEPTANCE CRITERIA 8-1 8.1 CONTROL CHART PROGRAM ...................................................................................8-1
8.2 ESTABLISHING CONTROL LIMITS ............................................................................8-1
8.3 INTERPRETING CONTROL LIMITS ............................................................................8-1
8.4 MEASUREMENT UNCERTAINTY……………………………………………. .........8-1

9.0 PREVENTATIVE MAINTENANCE 9-1
9.1 ROUTINE MAINTENANCE ........................................................................................ 9-1
9.2 SERVICE CONTRACTS ............................................................................................. 9-1
9.3 SPARE PARTS INVENTORY……………………………………………………….. 9-1
9.4 CONTROL OF MISCELLANEOUS MONITORING, MEASURING, TESTING, AND
DATA COLLECTION EQUIPMENT ............................................................................. 9-2
9.4.1 Analytical Balances and Weight Sets ........................................................ 9-2
9.4.2 Pressure Gauges ......................................................................................... 9-2
9.4.3 Fume Hood Testing Device………………………………………. ........... 9-3
9.4.4 Thermometers ............................................................................................ 9-3
9.4.4.1 Reference Thermometers .......................................................... 9-3
9.4.4.2 Working Liquid-Filled Thermometers ...................................... 9-3
9.4.4.3 Oven and IS Station Thermometers…………………… .......... 9-4
9.4.4.4 Non-Contact Thermometers…………………………….. ........ 9-4 9.4.5 Temperature/Humidity Recorders ............................................................. 9-4 9.4.6 Flow Meters ............................................................................................... 9-5 9.4.7 Mass Flow Controllers............................................................................... 9-5 9.4.8 Mechanical Volumetric Devices ............................................................... 9-5
9.4.9 Oven Vacuum Gauges………………………………………………… ... 9-6

10.0 PROFICIENCY TESTING PROGRAM 10-1 10.1 NELAP PT TESTING PROGRAM ..............................................................................10-1
10.2 EXTERNAL (NON-NELAP) PT SAMPLES .................................................................10-2

11.0 MANAGEMENT OF COMPUTER AND SOFTWARE SYSTEMS 11-1
11.1 SECURITY ................................................................................................................11-1
11.2 BACK UP AND STORAGE OF DATA ..........................................................................11-1
11.3 SOFTWARE AND ELECTRONIC DATA VALIDATION .................................................11-1
11.3.1 Developer Testing ......................................................................................11-2
11.3.2 Non-Production Testing.............................................................................11-2
11.3.3 Validation ..................................................................................................11-2
11.3.4 User Acceptance Verification ....................................................................11-2
11.4 IMPLEMENTATION ...................................................................................................11-2
11.5 COMMERCIAL SOFTWARE DATA VALIDATION .......................................................11-3

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12.0 CONTROL OF PURCHASED ITEMS AND EXTERNAL SERVICES 12-1
13.0 THE PROJECT MANAGEMENT SYSTEM 13-1
13.1 REVIEW OF PROJECT SPECIFIC DOCUMENTS ..........................................................13-1
13.2 NEGOTIATIONS AND VARIANCE REQUESTS ............................................................13-6
13.3 DOCUMENTATION OF PROJECT REQUIREMENTS .....................................................13-6
13.4 DOCUMENTING CLIENT DISCUSSIONS ....................................................................13-7
13.5 DOCUMENTING CLIENT CONCERNS ........................................................................13-7
13.6 SCHEDULING SAMPLING MEDIA .............................................................................13-7
13.7 TRACKING SAMPLE ANALYSIS AND REPORTING ....................................................13-7
13.8 PROJECT FOLLOW -UP ............................................................................................13-7

14.0 DATA INTEGRITY PROCEDURES 14-1

14.1 TRAINING.. ...............................................................................................................14-1
14.2 PERIODIC MONITORING ...........................................................................................14-2
14.3 MECHANISMS FOR REPORTING INFRACTIONS .........................................................14-2

APPENDICES

A. DEFINITIONS & TERMS .......................................................................................................A-1
B. LIST OF STANDARD OPERATING PROCEDURES (SOPS) ...................................................... B-1

REFERENCES .......................................................................................................................... R-1

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This Quality Manual was designed to meet the NELAC (National Environmental Laboratory
Accreditation Conference) standard as well as the current version of the Department of Defense Quality Systems Manual and supports assessment programs and/or certifications with the following
agencies:
Certifying Agency ATL Certificate # Basis of Certification/Approval Location of Certificate and Parameter List
Arizona DHS AZ0719 Onsite assessment (annual), LQAP and SOP Laboratory internal network: O:\QA\Certifications
California DPH
(Primary NELAP) 02110CA Onsite assessment (biennial) LQAP, SOP
and WP PTs
Laboratory internal network:
O:\QA\Certifications
Florida DOH (Primary NELAP) E87680 Onsite assessment (biennial) LQAP and SOP Review Laboratory internal network: O:\QA\Certifications
Louisiana DEQ 02089 LQAP, SOP Review, WP PTs, Secondary
NELAP
Laboratory internal network:
O:\QA\Certifications
New York State DOH 11291 LQAP, Secondary NELAP Laboratory internal network: O:\QA\Certifications
Oregon DHS CA200012-001 Secondary NELAP Laboratory internal network:
O:\QA\Certifications
Texas CEQ T104704434-08-TX LQAP, Secondary NELAP Laboratory internal network: O:\QA\Certifications
State of Utah DOH AIR LQAP, WP PT, Secondary NELAP Laboratory internal network:
O:\QA\Certifications
Washington DOE C2067 PT, Secondary NELAP Laboratory internal network: O:\QA\Certifications
DoD-ELAP ADE-1451 DOD QSM for Environmental
Laboratories v.4.1
Laboratory internal network:
O:\QA\Certifications
Pennsylvania State Dept. Health 68-690 Laboratory internal network: O:\QA\Certifications

MANAGEMENT QUALITY POLICY STATEMENT
At ATL, we strive to be the BEST in everything that we do. Our very existence is based on our continued ability to provide innovative, dependable, and cost effective environmental services to our
clients. We CARE about our clients as well as our co-workers and manage our daily activities to build relationships based on mutual TRUST, HONESTY, and RESPECT. We are LEADERS in
our field and accept the risks associated with building new frontiers in our professional lives. Our
strength comes from our TEAMS for through them we can achieve our goals. Our business is guided by four key principles: 1) Providing unmatched data integrity; 2) Establishing long term relationships;
3) Delivering quality client service; and 4) Exceeding client expectations. This Quality Assurance
Manual defines and documents the core systems surrounding good professional as well as laboratory best practices for all staff in accordance to the NELAC standard and the current version of the
Department of Defense Quality Systems Manual. As such, all laboratory staff are required to familiarize themselves with the quality documentation and implement these policies and procedures in their work. The management signatures on the cover page represent our commitment to the
NELAC standard and the Department of Defense Quality Systems Manual as well as our commitment to continually define, assess, and improve the quality systems, which provide the basic infrastructure in support of these goals.

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1.0 INTRODUCTION
The Air Toxics Limited (ATL) Quality Manual describes the Quality Assurance (QA) program and
Quality Control (QC) procedures used to ensure that data of known and documented quality are produced. It is designed to be used as a manual that outlines the process by which we ensure that the customer expectations are met, and hence, the quality goal is met. ISO/IEC Guide 17025-General
Requirements for Competence of Calibration and Testing Laboratories are incorporated wherever possible; however the primary guidance document is Volume 1: Management and Technical
Requirements for Laboratories Performing Environmental Analysis as published in the 2009 TNI
Standard (EL-V1-2009) and the Department of Defense (DoD) Quality Systems Manual for Environmental Laboratories Version 4.2 dated 10/25/2010.

The Quality Manual contains a discussion of the following topics:
Introduction: The quality objective is discussed along with management and information systems in support of the objective.
Organization: Staff qualifications and responsibilities, management organization, laboratory facilities, and
equipment are detailed in this section. Quality Assurance Program:
This section deals with project management, standard operating procedures, staff members’ training, evaluation and documentation of adherence to quality assurance and quality control requirements,
corrective action system, and health and safety.
Quality Objectives:
This section explains the quality control parameters and procedures, procedures to establish limits of
detection and quantitation and perform calibrations, traceability, and preparation of standards.
Sample Handling: Sampling containers, preservation and Chain-of-Custody requirements, sample receiving and tracking procedures, internal custody, storage and disposal are discussed.
Analytical Methods and Procedures: In this section, a brief method description is given for all analytical procedures carried out at ATL.
The limit of quantitation concentrations, quality control acceptance criteria and method modifications are provided as well.
Data Review and Reporting: This section explains the procedures involved in data collection/reduction, data review, and final
report production. Electronic data production, data flagging, and data storage are also discussed in
this section.
Establishing Acceptance Criteria:
The control chart program is outlined in this section along with generating and evaluating in-house statistical limits.

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Preventative Maintenance:
Routine maintenance, service contracts, and control of miscellaneous monitoring equipment are explained briefly.
Assessments and PT Samples: A brief explanation of internal and external assessments programs and NELAP/DoD PT samples
program is provided.
Computer and Software Systems:
This section of the quality manual deals with the management of computer and software systems.
Data storage, back-up routines, and internal software validation efforts are included.
Control of Purchased Items:
Control of purchased items and external services as well as the purchase requisition system are outlined in this section.
Project Management System: This part of the quality manual gives a brief description of steps to ensure that the customer
expectations are met once the project is undertaken. 1.1 QUALITY OBJECTIVE
Air Toxics Limited is committed to producing data that meet or exceed the client’s measurement
needs. Customer satisfaction is the motivating force behind most of the ATL processes. An
underlying network of systems designed to define, document, and process each individual customer’s need supports this primary objective. This systems network includes Sales, Project Management, IT,
Laboratory Production, Support Services, Technical Services, Quality Assurance, and Finance. Each
of these operational areas is organized around an empowered work team accountable for delivering an automated, on time and defensible result.

We believe the ultimate responsibility for quality resides at the team level. Every team member has the responsibility and authority to suspend a process if it appears that the quality objectives are not
being met. Analytical team members are informed of the quality objectives via documented Standard
Operation Procedures (SOPs) and project related information systems (ATL’s Project Profiles and Project Requirement tables). Team members work closely with the Project Management and QA
Departments to ensure that the quality objectives are met. 1.2 QUALITY MANAGEMENT SYSTEM
The role of the ATL management team is to design, implement, maintain and audit the quality systems. Quality systems are designed and documented on each functional team through Standard
Operating Procedures. Once designed, the management team ensures through ongoing daily activity that adequate funding, equipment, staffing and training exist to support the success and effectiveness
of the quality systems. Management helps ensure that the quality objective is met by establishing a
continuous and reiterative program of audit review and process improvement. Establishing goals at the team and individual levels that support the objectives of the quality systems is an essential
management activity as well providing adequate individual accountability measures and feedback.
The primary role of the management team is to establish strategic performance goals at the corporate and team levels and to produce quantifiable measures of performance against these goals (e.g.,
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customer satisfaction index, sales quotas, report turn around time, net profit, days to complete
corrective actions, etc.). The success or failure of every relevant quality system is the ultimate responsibility of management. The management team consists of Business Directors, Managers and Team/Task Leaders.
Quality Assurance Management:
The role of the ATL Quality Assurance team is to help ensure that the systems described above are
designed, documented, and operating in accordance with the quality objectives. This is accomplished via coordination and dissemination of internal and external assessment information, review of SOPs
to document variances taken to published methods, monitoring of the Quality Manual to assure
consistency with actual practices, maintenance of an ongoing Corrective Action Program with quarterly reports to the senior management team, and a leadership role in employee training
programs. A secondary function of the QA team deals with data review and other quality control
related programs.
The QA team is free from any commercial, financial, or production pressures when making assessments or decisions regarding the quality of work produced or effectiveness of the quality systems. The Quality Assurance Manager reports directly to the Vice President/Technical Director II
in order to maintain independence from business operating units and facilitate communications regarding quality related issues.
Communication between the QA team and other management teams occurs on a regular basis via bi-weekly status meetings. Information regarding outstanding corrective action items, upcoming
assessments, assessment results or general observations are brought up and documented via a
database of agenda notes. The quality assurance database along with the ATLAS database are used to compile a ‘Quarterly Quality Assurance Status Report’, which is distributed to the senior
management team for review.
Sales and Project Management:
The role of the ATL Sales and Project Management teams is to effectively document and
communicate the needs of the customer. These teams represent the customer in all matters and serve as a liaison between the customer and the Technical Services, Laboratory, Support Services, Finance,
and Quality Assurance areas. The ATL Sales and Project Management teams work with laboratory management to ensure that client needs are matched by laboratory resources. Strong communication linkages exist between the Laboratory Director, Laboratory Manager, and the ATL Sales and Project
Management teams. Information regarding customer needs flows into all ATL systems via these two teams. Interactions may be as complex as Quality Assurance Project Plan (QAPP), contract or Scope of Work (SOW) review or as simple as processing shipments of canisters and other sampling media.
Project specifics are documented and stored via an interactive database that assigns a unique identifier for every reference. Every contact with the customer is documented in the database by the Project
Management team so that management and laboratory technical staff can make decisions based on
electronic sorted one touch information.
Sample Receiving:
The goal of the department is to enable every sample to be received and processed into a unique laboratory Work Order within 24 hours of sample receipt. Sample non-conformities are
communicated to the clients in the same time frame. Custody information relating to sample receipt, a copy of the sample receipt summary, and the compound list and reporting limits for the requested analysis is e-mailed or faxed to the client for review and comments.
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Laboratory Management:
The Laboratory management work teams are equipped with necessary resources to complete the sample analysis, review, data reporting and creation of all electronic data packages, which include e-mail, EDD and eCVP. The laboratory work team is responsible for verifying the quality of the
standard reports by reviewing each final product. In this way, team members are easily able to accept the control and accountability for quality. The Support Services team is responsible for cleaning,
assembling, coordinating media certification and shipping all sampling media. The primary
responsibility of the Team/Task Leaders and/or Laboratory Manager is to monitor customer needs versus resource availability. Staff and equipment management are carefully balanced with customer
needs. The goal for the laboratory team is to deliver defensible data within the time frame promised
to the client. The Laboratory Manager or Team/Task Leaders review daily sample receipt work lists to determine that the laboratory has adequate resources to perform the work. In those cases where
either the technical or sample capacity demands cannot be met, the Laboratory Manager works with
the Project Manager and the client to provide a solution via inside resource re-allocation or outside subcontracting. The ATLAS laboratory automation system creates and tracks special analytical lists,
deliverables, or Turn Around Time (TAT) requests which are automated via customized linkages (work tools) into the centralized Structured Query Language (SQL) database. Performance measurements against the goal are routinely monitored using the same SQL database. Performance
and quality related information is shared with team members during team meetings. Project or client related information resides both in the project management module and in sample tracking modules, reducing the need for relying on verbal communication of project specifics to the team. Laboratory
management and personnel are free from any commercial, financial, or production pressures when making technical judgments or decisions regarding the quality of work produced. The Team/Task
Leaders report to the Laboratory Manager who reports to the Laboratory Director.
The remaining team positions are divided into four levels:

1) Senior Scientist (Lab Personnel) or Senior Associate (non-Lab Personnel): This is the highest level professional position reporting to a Director or Manager. The Senior Scientist
or Senior Associate works independently at a company wide level. In addition to all of the
responsibilities of the Scientist described below, the Senior Scientist or Senior Associate is recognized within the company as an expert in his/her field. He or she is often asked to work outside
of the team whenever the need arises, and is able to demonstrate above average leadership skills. Senior Scientists or Senior Associates are responsible for method development activities and take a lead role in proprietary software and hardware design and testing. High profile projects or client
relations, including more intricate analyses and data interpretations, are assigned to a Senior Scientist to oversee. The Senior Scientist or Senior Associate maintains knowledge at the level of Masters Degree or equivalent with a minimum of 5 years of analytical environmental experience.
Scientist (Lab Personnel) or
Associate (Non-Lab Personnel):
The Scientist or Associate works independently at the team level. A Scientist or Associate
demonstrates a high level of skill, judgment, problem solving ability, and is able to independently
perform troubleshooting. The responsibilities of a Scientist/Associate include: scheduling of work, providing routine as well as non-routine bench level activities in a highly efficient manner, writing
SOPs, reviewing data, performing non-routine instrument maintenance and troubleshooting, and representing the team during internal/external assessments. Individuals in this position play a lead role in monitoring health and safety on the team, and acting as a resource or trainer. A Scientist or
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Associate must have a Bachelor’s Degree and a minimum of three years of analytical environmental
experience. Analyst (Lab Personnel
and Non-Lab Personnel):
The Analyst works under the direct supervision of a Scientist, Senior Scientist, Team/Task Leader,
and/or Manager at all times. He/she follows a specific formal training program to learn the necessary skills required of the position and demonstrates the ability to recognize problems and to seek
assistance. The primary responsibility of an Analyst is to follow written laboratory SOPs in an
efficient and well-informed manner. The Analyst performs routine maintenance on the equipment, prepares standards, and performs all relevant bench level activities. The minimum qualification for a
laboratory analyst is a Bachelor’s Degree.
The laboratory team has a mix of Scientists and Analysts. The Team/Task Leader and/or Laboratory
Manager coordinates the activities of the team, serves as a resource to the Analysts and Scientists, communicates the corporate objectives to the team, and monitors team progress against the quality objective, which is customer satisfaction. A Scientist may be assigned as ‘team lead’ in a subset of
team activities. As ‘team lead’ the Scientist is responsible for all the technical activities of the assigned area, oversees both the quality and quantity of work produced, and serves as resource for the Analysts. The Analyst performs all of the routine activities and quality checks (i.e., makes sure the
customer expectations are met).
Every team member is empowered to make sure that the customer expectations are met, is trained in
the elements of the quality process, and has the responsibility and authority to stop or suspend a process when the quality objective is in jeopardy.

Technician (Lab Personnel
and Non-Lab Personnel):
The Technician works directly under the supervision of a more experienced team member,
Team/Task Leader and/or Manager at all times. He/she is responsible for meeting the team’s production and quality goals. The Technician performs a variety of tasks in whatever area of the
laboratory they are assigned. For example, the Technician’s responsibilities may include washing and
solvent rinsing glassware, cleaning and preparing media to ship to clients, pressurizing and screening samples, logging samples, assist in preparing standards and other duties as assigned. He/she is also
expected to communicate issues to a team Scientist and/or Team/Task Leader. The minimum
qualification for a Technician is a High School Diploma.
Information Technology:
The Information Technology (IT) team is responsible for the design and maintenance of the SQL server based data system. Its primary goal is to ensure that customer satisfaction is achieved by the
way information is transferred, processed, or queried. This includes systems relating to telephone service, e-mail service, Internet access, project management, data acquisition, assessment trails, data
security, and automated data reporting linkages. The group consists of the IT Manager, and one full
time programmer. Around-the-clock, system support is achieved via a combination of in-house and contract support. Additional programmers are hired on a project specific basis. All of the ATL
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information systems are designed, coded, and tested in house and as such, are proprietary in nature.
The IT Manager reports to the President. Financial Management:
The quality systems rely on bottom line profitability to provide strength to the framework that produces quality results. The ATL Finance team is responsible for monitoring the profitability of all
operations. Customer satisfaction goals are built into budgeting, purchasing, invoicing, employee
compensation and benefits programs, collections, contracts, insurance, and banking. The primary goal of the team is help ensure bottom line profitability while achieving the quality objective, which is
customer satisfaction. The group consists of a Controller (Finance Manager), an Accounts
Receivable Associate and an Accounts Payable Associate. The Finance Manager reports to the President.

Data Integrity Procedures: Since a commitment to data integrity is a vital component for credibility of our core product, Air
Toxics Limited cannot function as a business entity without a clear definition of ethical expectations for all employees. Integrity is defined as the ability to discern right from wrong, and the commitment to do what is right, good and proper. Data integrity procedures relating to generation of analytical
reports are built into the systems via the operational SOPs, which describe appropriate practices. Additional systems and training programs that safeguard strict adherence to the SOPs ultimately ensure that data integrity procedures are employed. Intentional fraud will be grounds for severe
reprimand and/or termination of complicit employees. In addition, employees who witness or are otherwise aware of data integrity violations, even if they are not a party to such acts, are expected to
immediately report these lapses to their Team/Task Leader, their Manager or to a member of the
Board of Directors.
Data integrity training is conducted within a variety of frameworks and is mandatory for all Air Toxics
Limited employees. New employees read both the LQAP and the Employee Handbook to properly orient ethical expectations. In addition, within one month of date of hire there is basic training
provided by the Quality Assurance Department to familiarize new employees with principles of
documentation to pre-empt practices that would call into question the data integrity procedures of the laboratory. The Chief Executive Officer (CEO) of Air Toxics conducts a Standards of Conduct
presentation that defines data integrity expectations, potential penalties and consequences for lapses of integrity for new employees as they join the company. In addition, the CEO conducts a yearly ongoing Ethics and Integrity Training II for the remainder of the employees. The Inappropriate Lab
Practices Class (also done on a yearly basis) defines allowable parameters for the lab to assure defensibility and to define illegal practices. The purpose of all training is to provide specific examples of data integrity expectations that are relevant to actual job functions. Employees document the
training in their training records (see Section 3.2.1).

1.3 INFORMATION MANAGEMENT SYSTEM
Information is stored in the Air Toxics Laboratory Automation System (ATLAS) databases using ATL designed hardware and proprietary software. This in-house Laboratory Information
Management System (LIMS) is an evolving development project designed to find more efficient means to meet the customer needs. Each client contact (telephone call, quote, shipping request, or
inquiry) is stored in a database, which can be queried for sample log-in, project backlogs, project
TAT or revenue statistics.
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Some modules are designed to track non-traditional information such as the sample history of
individual canisters, number of reports completed per analyst per shift, and overdue work by reason code. These types of information directly affect the ability of the management team to provide quality process improvements. Some non-traditional calculations such as the boiling point distribution
of a hydrocarbon background, EPA rounding, and percent difference calculations have been made available at the bench. This type of information directly affects the ability of the individual employee
to meet the quality objectives.

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2.0 ORGANIZATION
2.1 STAFF QUALIFICATIONS AND RESPONSIBILITIES
ATL’s management organization includes the Board of Directors comprising five core areas: Laboratory, Operations, Finance, IT, and Sales. In addition there are Managers and Team/Task Leaders. Each operating area is lead by a Manager and/or a Team/Task Leader. In the absence of a
member of the management team responsibilities are fulfilled as follows: If the President is absent, the Vice President/Technical Director II may fulfill the responsibilities as President. In addition, if the
primary Technical Director is absent the second Technical Director will fulfill the responsibilities. If
the QA Manager is absent, the Technical Directors may fulfill QA responsibilities. In the absence of a Manager or Team/Task Leader, one of the Directors will name an interim successor.

LINDA L. FREEMAN CHIEF EXECUTIVE OFFICER, PRESIDENT AND LABORATORY TECHNICAL DIRECTOR (I)
Ms. Linda L. Freeman is the President and the Chief Executive Officer of Air Toxics Ltd. providing leadership that ensures the founding mission and core values of the company are put into practice.
Ms. Freeman leads programs relating to the development of long range strategy, quality systems, and financial infrastructure. Ms. Freeman provides day-to-day leadership and management of programs for overseeing the processes and resources necessary for establishing long-range service objectives,
plans and policies, in cooperation with the Board of Directors. She is responsible for the measurement and effectiveness of both internal and external processes by providing accurate and timely feedback on the operating condition of the company. In addition, Ms. Freeman also directs
the definition and operation of the laboratory production by fostering a success-oriented and accountable environment within the company. She holds a Master of Science Degree in Chemistry from the University of Wisconsin-Madison. Ms. Freeman has 24 years of combined environmental
experience and 20 years of laboratory business management experience.
ROBERT MITZEL
VICE PRESIDENT OF BUSINESS DEVELOPMENT
Mr. Mitzel is the Vice President of Business Development at Air Toxics Ltd and is responsible for
establishing strategic direction for the sales team to ensure day-to-day sales support and communication with the project management team. He plays a lead role in establishing and
negotiating terms for all strategic new accounts. In addition, Mr. Mitzel provides sales support to AirLab, a subsidiary of Air Toxics Ltd. Mr. Mitzel plays an integral role in the development of new methods and processes in the laboratory. He is responsible for bringing new business opportunities
for the company to the Board of Directors. Mr. Mitzel has over 30 years of combined environmental
laboratory experience. He holds a Bachelor of Science Degree from California State University, Chico in Chemistry and Biology.
HEIDI C. HAYES VICE PRESIDENT, LABORATORY DIRECTOR AND TECHNICAL DIRECTOR (II)
Ms. Heidi C. Hayes is the Vice President of Research & Development and Laboratory Director of Air
Toxics Ltd. Ms. Hayes is responsible for developing products and solutions to meet client and
industry needs. Ms. Hayes oversees the validation process to insure quality objectives are met as defined. Her focus is on the testing of new media, protocols, and technology related to air phase
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Revision 22.1, 09/2011 Page 2-2 analysis. She serves as a resource for the regulatory community in evaluating soil gas and indoor air
sampling and analytical protocols. As Laboratory Director, Ms. Hayes provides additional oversight over the quality systems and technical performance of the laboratory. She is responsible for the
overall management and direction of laboratory operations and is responsible for implementing structures and measurement matrices to facilitate management communication, prioritization and feedback as needed to achieve corporate goals. Ms. Hayes has over 17 years of environmental
laboratory experience. She holds a Master of Science Degree in Chemistry from the Colorado School
of Mines.

MELANIE LEVESQUE
QUALITY ASSURANCE MANAGER
Ms. Levesque develops and supervises programs intended to ensure that the laboratory is producing data of known and acceptable quality. Ms. Levesque oversees QC activities including various independent checks of laboratory systems, SOP generation, and corrective action procedures, as well
as monitoring laboratory certification programs. Ms. Levesque has documented training in the approved methods and can verify that the laboratory is following SOPs. Ms. Levesque maintains
independence from the operations by not engaging in production activities and reports directly to the
Technical Director. The QA Department conducts a yearly independent audit of the quality systems and methods criteria, and notifies executive management and laboratory managers of deficiencies via
a written quarterly status report. Ms. Levesque holds a Master of Science degree in Analytical
Chemistry from Rochester Institute of Technology, followed by 12 years of environmental laboratory experience. Ms. Levesque has worked in a variety of positions that include analytical and
supervisory experience. SEPIDEH SAEED LABORATORY MANAGER
Ms. Sepideh Saeed is the Laboratory Manager. She is responsible for managing and overseeing all
processes resources involved in the daily operations of the SVOC, VOC, Sample Receiving, and Support Services departments. As the SVOC and VOC Laboratory Manager she is responsible for overseeing the GC, HPLC and GC/MS analysis, which includes EPA Method TO-3/TO-12, ASTM
D-1945/1946, TO-14A/TO-15, TO-17, SW8260B, Extractions, ASTM D-5504, TO-13A, TO-5/CARB 430, TO-11, Method 0011, PM10, TSP, NIOSH 5515, Siloxanes, Pesticide, and PCB
Analytical Group. She provides technical support to client services, sales, and is also responsible for
supporting the Team/Task Leaders in managing staff and production. Ms. Saeed has 17 years of laboratory experience as a GC, HPLC, GC/MS and extraction chemist and 11 years of supervisory
experience and has been employed at Air Toxics since 1998. Ms. Saeed has a Bachelor of Science
Degree in Biochemistry from the University of California, Davis.
BING WANG
INFORMATION TECHNOLOGY MANAGER
Mr. Bing Wang joined Air Toxics in 2009 as Information Technology Manager. Mr. Wang oversees
all aspects of software engineering and development, database administration, and network administration. He brings more than 12 years information technology experience to our organization, including 10 years of commercial software development experience. His expertise spans all aspects of
direction, design, development, and implementation of customized Laboratory Information Management Systems in an FDA Good Laboratory Practices regulated environment. Mr. Wang has
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Revision 22.1, 09/2011 Page 2-3 been instrumental in designing and implementing model work flow processes, defining user
requirements, and proposing software design and implementation to satisfy long-term company business goals. He has established policies and procedures to ensure continuous database and server
environment integrity and reliability. Mr. Wang holds a Master of Science Degree in Civil Engineering from the University of California at Berkeley; and, Master of Science Degree in Engineering from Central South University of Technology, China.
CHRIS LA BELLA SUPPORT SERVICES TEAM LEADER
Mr. Chris S. La Bella is the Team Leader for the Support Services Team. This team is responsible for
cleaning and certification of Canisters. Other responsibilities include preparation of flow controllers,
TO-17 tubes, VOST tubes for Method 0031. As the Support Services Team Leader, Mr. La Bella works under the guidance of the Laboratory Manager and is expected to communicate production and
technical issues to the manager. Mr. La Bella has about 1 year experience in doing bench work for
Support Services; currently Mr. La Bella is spending 50% of his time on the bench.
CATHLEEN ROUSH
LABORATORY TASK LEADER
Ms. Cathleen Roush is the Task Leader for the VOC department. She is responsible for overseeing
the daily production of the GC/MS volatiles analysis using EPA TO-15 methodology. The team is sufficiently staffed so that Ms. Roush spends no more than 20% of her time at the bench to ensure
adequate time for training, data review, and scheduling. As a Task Leader, Ms. Roush works under
the guidance of the Laboratory Manager and is expected to communicate production and technical issues to the manager. Ms. Roush has 2 years of laboratory experience and has been employed at Air
Toxics Ltd. for 2 years. Ms. Roush has a Master of Science Degree in Chemistry from Sacramento
State University.
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The ATL laboratory occupies 35,000 square feet of space in Folsom, California with approximately
7,000 square feet of office space. The single story building is custom designed to suit the specifications of an air laboratory. Design criteria included floor plans to accommodate segregation of conflicting tests and provide an environment that is conducive for cross-functional work teams.
The main instrumentation laboratory is based on an “open” concept in which walls are removed to promote a sense of community and teamwork. Wide hallways with alcoves are designed to encourage
congregation and discussion. The number of private offices is minimized so that barriers between
management and staff are removed. Elements of the quality system are evident throughout the facility design.

Sample receiving occupies approximately 950 square feet. There is sufficient floor space to receive, unpack, and tag up to 150 SummaTM canisters per day. The main laboratory is centrally located and
houses twenty four GC/MS systems, eight GCs, and a network of computers.
A caged canister storage area was constructed on one side of the laboratory to securely hold all
canister and Tedlar bag samples. An isolated negative pressure room was designed for solvent handling and extraction activities. Approximately 500 square feet of air-conditioned space is designated for research and development activities, and a work shop/tooling area. Sorbent tube
preparation and canister cleaning operations are located in segregated areas. Long-term file storage occurs off site. A local document storage and retrieval service picks up files for storage. Files are kept in bar coded boxes making retrieval easier. Typically a file can be retrieved within one
working day from the original request. Security is maintained through a controlled access system. Representatives of State, Federal or
private entities have access to the laboratory facility and records during laboratory normal business hours. Guests must enter/exit through a central reception area. The receptionist keeps a date/time
log. After work hours, the building is secured and linked to a commercial security agency. The
security system is equipped with perimeter alarms, motion sensors, and speakers that monitor background sounds. Heat activated fire alarms are monitored by an outside agency. A fire alarm also
activates the security system. ATL SOP #30 describes the security and controlled access protocols.
2.3 EQUIPMENT AND INSTRUMENTATION
The laboratory is equipped with over $2,000,000 of instrumentation, dedicated exclusively to the analysis of air samples. Much of the commercially available equipment is modified in-house in order
to enhance performance in the areas of:

• Overcoming challenging sampling problems;
• Analyzing difficult matrices;
• Achieving greater sensitivity. A staff of design engineers and 500 square feet fabrication shop is maintained by ATL in order to
build, test, and service the custom equipment. A facilities map and equipment list can be found in Exhibit 2.2 and Tables 2.1 and 2.2.

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Revision 22.1, 09/2011 Page 2-7 Table 2.1. Laboratory Instrumentation and Equipment

# Description
1 Agilent 6890 GC/MSD
5 Agilent 5973 GC/MSD
18 Agilent 5975 GC/MSD
8 Markes Autosampler
1 Hewlett-Packard 5973 GC/ECD/ECD
2 Hewlett-Packard 5973 GC/SCD
1 Hewlett-Packard 6890 GC/FID
1 Hewlett-Packard 6890 GC/TCD/FID
2 Hewlett-Packard 6890 GC/PID/FID
1 Hewlett-Packard 5890 GC/TCD/ECD
1 Hewlett-Packard 1200 Gradient HPLC
4 Air Toxics Canister Autosampler
2 Air Toxics Custom Sorbent Tube Desorption Unit
8 Canister pressurization stations
15 Soxhlets Extractors
2 Accelerated Solvent Extraction (ASE) System
4 Custom Pressure/Vacuum Canister Cleaning Manifold
10 Custom Convectron Vacuum Canister Cleaning Manifold

Table 2.2. Sampling Media
Description Quantity
Air sampling canisters
6-Liter Summa canister 2380
1-Liter Summa canister 1700
PAC250 Summa Canister 300
High Pressure Sample Cylinder 31
Flow Controllers for air sampling canisters 800
24-hour flow controllers for canisters 750
Vacuum gauges 200
Tedlar bags: 1, 3, 10 liter In inventory
MM5 air sampling traps 10
Midget impingers 30
VOST tubes kept in inventory 50 pair
TO-13 PUF/XAD and TO-4/TO-10 air sampling cartridges 200
TO-17 air sampling tubes various sorbents 450

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Air Toxics Limited maintains comprehensive Quality Assurance programs to ensure that analyses are
being conducted according to prescribed analytical methodology, and are within project specific QAPP requirements. The program is an integrated system of activities involving planning, quality assessment, quality control, reporting, and quality improvement. The basic elements of this program
include:
• DOCUMENTING procedures, method requirements, and project requirements
• Organizing, monitoring, and leading TRAINING programs on quality related issues

• ASSESSING adherence to requirements, including maintenance of a system which documents, tracks, and provides closure when corrective actions are necessary
• Formally COMMUNICATING results of those assessments to laboratory management
These critical elements of the Quality Plan are described in detail in the following sections.
3.1 DOCUMENTING
3.1.1 The Quality Assurance Manual
The Quality Assurance Manual describes the major programs or systems by which the laboratory
provides data of known and predictable quality. The QA Manager and the Technical Director are responsible for the content, accuracy and completeness of the Manual. The Manual must comply
with all State and Federal requirements for those programs in which the laboratory maintains accreditation. The Quality Assurance Manual is a required reading for all laboratory staff and everyone must comply with the procedures documented as a condition of continued employment.
The QA personnel inform the Managers and the Team/Task Leaders of the availability of the revised Quality Assurance Manual. The Managers or the Team/Task Leaders inform team members who then access the Manual from the network in order to read it. All personnel are required to document in
his/her training record that the latest revision of the Quality Manual has been read and understood. The Manager and/or the Team/Task Leaders assess the accuracy and completeness of the documentation annually at the time of the employee’s performance review. Missing or incomplete
documentation is noted in the performance review.
The Quality Assurance Manual is reviewed and updated annually. The Manual is signed and dated by
the Technical Directors, the Laboratory Manager and the Quality Assurance Manager as acknowledgment of review and approval prior to use.

3.1.2 Standard Operating Procedures/Methods Manual
The laboratory procedures used at ATL are documented in method-specific standard operating procedures (SOPs). These procedures are based on standard EPA or ASTM methodology whenever possible. The SOPs contain all necessary QC parameters, acceptance criteria, and directions for
corrective action measures. The SOPs govern the laboratory response to results that are outside acceptance limits and address anticipated problems with associated recommended corrective action to eliminate the problem or further occurrences of the problem. SOPs also specify the type of written
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anticipated as well as unanticipated problems. The SOPs are maintained in numerical order in binders, which also serve as the laboratories Methods Manual. The SOPs address the following
(where applicable):
• Identification of the test method
• Applicable matrix or matrices
• Detection Limit (MDL)
• Method reporting limits
• Scope and application (includes target analytes)
• Summary of the method
• Table of significant variances from the method
• Definitions and interferences
• Safety
• Equipment and supplies
• Reagents and calibration standards
• Sample preservation and storage requirements
• Quality control
• Calibration, validation, and standardization
• Procedures
• Data analysis and calculations
• Method performance objectives
• Pollution prevention (if applicable)
• Data review and acceptance QC criteria
• Corrective Action for out of control data
• Waste management (if applicable)
• Method identifier and references
• Any relevant tables, flow charts or diagrams

The SOPs are written by the Manager, the Team/Task Leader or an experienced Scientist/Analyst and are reviewed annually for technical accuracy and adherence to general QA/QC protocols. The SOP is signed and dated by the author, then is submitted for technical review, QA review, and final review
by the Laboratory Director. Each method SOP contains a detailed table of all modifications taken against the actual reference method if applicable. Modifications and/or additions to the SOP are
similarly reviewed and signed. Each hard copy SOP carries a unique revision number, control copy
number, and date of generation. The SOPs are treated as confidential and proprietary and are maintained under the authority of the QA Department. The original is kept in the QA Department
and extra copies in various laboratory sections as needed. Electronic versions of the SOPs are stored
on a secured network drive, which only the QA Department can access. SOP summaries that include analyte lists, reporting limits, QC criteria and current variances to published methods are available to
clients in .pdf form as the ATL Methods Manual Summary. Copies of SOPs are made available to State and Federal accreditation and regulatory entities.
Current SOPs are stored electronically in a secured read-only database to allow review online by laboratory personnel. Whenever an SOP is updated and implemented, it appears in the electronic
database. The QA personnel inform the Laboratory Manager and the Team/Task Leaders of the
availability of the revised SOP. The Laboratory Manager or the Team/Task Leaders inform team members who then access the SOP from the laboratory network in order to read the SOP. Once the
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Revision 22.1, 09/2011 Page 3-3 Scientist/Analyst reads the SOP, he/she logs the date in the SOP tracking software. This
documentation is then filed in his/her training record. The Laboratory Manager and/or the Team/Task Leaders assess the accuracy and completeness of the documentation annually at the time of the
employee’s performance review. Missing or incomplete documentation is noted in the employee’s performance review.
A comprehensive list of ATL’s SOPs can be found in Appendix B.
3.1.3 Revisions to SOPs
The revision number of the referenced method is noted in the method-specific SOPs. The protocols
and deviations are specific to that revision number. Air Toxics does not operate under more than one
version of a referenced method at any time. The specific protocol used for analysis can be tracked using the effective date noted on the front page of the SOP.

Each SOP update is identified by a unique revision number. As with referenced method revisions, only one revision of an SOP is used in the laboratory at any one time. A complete description of
ATL’s system for writing and updating SOPs can be found in ATL’s SOP #46. 3.1.4 Documenting Method Specific Deviations
Most air methods were not written as definitive and all have a strong performance based component to them. It is not unusual for the lab to have to design and create sampling interfaces or moisture
control devices or to add additional quality assurance requirements to the methods in order to meet more stringent project or program requirements. Any variances to referenced methods are
summarized in tabular form in the laboratory SOP. Signatures of the Laboratory Director and QA
Manager on the front page of each SOP indicate review and approval of these variances. A copy of the method modifications table from the SOP appears in the Laboratory Narrative section of the
Comprehensive Validation Package or standard final report (Table 3.1). The QA team maintains and
updates the templates used to create the Laboratory Narrative section of each work order. Each template has a revision date to ensure that only the most recent SOP table appears in the Laboratory
Narrative.
On occasion, the need arises to change some aspect of an established SOP to accommodate
enhancements to either the equipment or the method. The bench chemist documents the request for the change and the reasons behind it in the ‘Request for Technical Change’ form (Exhibit 3.1). The form is routed through the Laboratory Manager and Team/Task Leaders with approval for the change
noted by signature of the QA Manager, Laboratory Director and Technical Director(s). The form also identifies any established SOPs which should be revised/amended to incorporate the changes made. The forms are serialized in order to track progress and implementation. SOP Amendment forms are
also used to reflect changes that are made to SOPs prior to a new revision.

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Revision 22.1, 09/2011 Page 3-4 Table 3.1. Example Method Modification Table
Requirement EPA Method TO-4A/TO-10A ATL Modifications
Extraction Solvent 10 % (5 % TO-10A) Diethyl
Ether in Hexane
DCM, exchanging to Hexane during the
concentration step
Reagent Blank Set up extraction system without filter/PUF; reflux with solvent No Reagent Blank is extracted. Reagent lots are certified as acceptable prior to
use
Media certification (TO-10A
only)
< 0.01 ug for single peak analytes,
< 0.1 ug for PCBs
< Reporting Limit for all analytes
Frequency of Continuing Calibration Verification Every 10 samples Every 20 samples with internal standard
PCB Quantitation Requires a minimum of 5 peaks Use 4 peaks for quantitation

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Exhibit 3.1. Example Technical Change Request Form

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Exhibit 3.1. Example Technical Change Request Form (Continued)

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3.1.5 Documenting Project Specific Deviations
Project specific QAPPs are reviewed by the Project Management Department (or a qualified
designee). The laboratory may also take variances against method criteria established in project specific SOWs or QAPPs. The Project Management personnel (or qualified designee) reviews the project specific criteria during project proposal and notes any variances from standard laboratory SOP
in a table. A variance table (Table 3.2) is then incorporated into the bid proposal for review and acceptance by the prospective client. The client notes acceptance by signature or initial and date in the
designated field of the table. The project specific variance table is stored on a secured network drive
following approval. A Project Profile (Exhibit 3.2) is initiated at the same time. A summary of the analytical requirements which differ from ATL’s relevant SOP is documented in a Project
Requirement Table and included in each Work Order folder. The Project Profile may also be accessed
through the ATLAS database. The Project Manager is responsible for noting the location of the Project Requirement Table in the Project Profile. Finally, the variance table is included in the
Comprehensive Validation Package (CVP). The project specific QAPPs are maintained in electronic form on a network drive.
Table 3.2. Example Project Specific Variance Table
SOW ATL SOP VARIANCE APPROVAL*
Method 2720C Fixed Gases ASTM D-1945 Fixed Gases
RDLs determined upon receipt
of lab MDLs
Standard lab RDLs of 10 ppmv
Field blank can one per batch Not provided
Canister released 90 days past
reporting
Canisters released 30 days past
day of sampling

72 hour retention time study ±0.06 minutes standard SW-
846

Calibration verification daily
with all analytes ±25%
expected value
All compounds within 15%;
Spike concentration is 25 ppbv

Accuracy/precision study per
analyst with project limits
Per analyst once every 12
months using ATL standard limits only

LCS once per 5 point, ±25%
difference for all compounds
All compounds within ±15%;
Spike concentration is 25 ppbv

*NOTE: Each variance must be approved by the client’s initial and date. An initialed copy of this
variance table will appear in the Comprehensive Validation Package.
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3.2 TRAINING
3.2.1 Team Training
ATL laboratory staff members have sufficient education, training, and technical knowledge to perform their assigned duties. The laboratory team has both experienced and in-training staff
members. Those in training work under the supervision of a more experienced peer who is typically the lead Scientist assigned to that area.

Training of laboratory staff in analysis consists of three developmental stages:
• Initial instruction by the Laboratory Manager or a designated peer concerning basic elements of the method and brief overview of instrumentation. Applicable SOPs and methods are read. During this
time, the trainee is an observer.
STAGE I. Introduction
• Periods of close contact and direct supervision by the Laboratory Manager or a designated peer. During this time, which may last for several weeks, the Analyst/Scientist performs tasks
independently as assigned. All aspects of his/her work are reviewed by the Laboratory Manager or a designated peer.

STAGE II. Training
•
Independent work with data review by the analytical Laboratory Manager or a designated peer.
The final step in the training process allows the Analyst/Scientist to document competency by analyzing four consecutive Laboratory Control Samples which is documented by a Demonstration of
Capability Form for Initial Method Proficiency (see Exhibit 3.5). A Continuing Demonstration of Capability must occur on an annual basis and documented by a Continued Method Proficiency Form
(see Exhibit 3.6). ATL’s system for performing an Initial and Continuing Demonstration of
Capability can be found in ATL’s SOP #87.
The QA team ensures that training of each member of the technical staff is complete, documented,
and up to date. Exhibit 3.4 is an example of a Training Record form. It is the responsibility of the employee to keep his/her record current. An Analyst’s/Scientist’s training is considered current if the
training record contains evidence that the employee has:

STAGE III. Advanced Operation
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The Laboratory Manager and/or Team/Task Leader review the training record on a yearly basis during an employee’s annual performance review. Deficiencies in the training record are documented
and returned for correction (see Exhibit 3.7). Consistent failure to maintain updated training records
is noted in the performance review and effects the employees overall job rating.
A series of classes taught by members of the management team are typically offered on a yearly
basis. Exhibit 3.8 contains a sample of internal courses that are offered. The list of courses is subject to change on a yearly basis depending on requests and topics. Course attendance is mandatory for
topics specifically related to an employee’s job function. The QA Department and management teams determine which courses are mandatory. Course attendees may be tested to ensure that they have achieved an acceptable understanding of the material presented. Completion of courses is
documented in the employee’s training record.
Training Record Checklist

• QA Orientation documentation
• Safety Orientation documentation
• Read the current version of the LQAP (QA Manual)
• Completed the training class on ethical responsibilities
• Read and understood the current version of relevant SOPs
• Completed necessary internal or external training classes
• Demonstrated initial proficiency in the methods by acceptable performance on four Laboratory
Control Samples; proficiency is measured by accuracy and precision
• Demonstrated continued proficiency in the methods by acceptable performance on four
Laboratory Control Samples or duplicate analysis with RPD ≤ 25% between two analysts; proficiency is measured by accuracy and precision

3.2.2 External Training
External training courses offered by software experts, instrument manufacturers, or other recognized experts in analytical instrumentation and/or analysis are attended by ATL employees. The course
description, dates offered and record of attendance are kept in the employee’s training records. The company maintains a budget for external training classes and higher education.

3.2.3 Quality Training
All new Air Toxics Limited employees are required to attend the Quality Assurance Orientation
course. Completion of the course is documented in the employee’s training record. The course outline includes:

• Introduction to QA and Laboratory Nomenclature
• Definitions of SOPs and LQAP
• How to use CARs
• Logbook protocol
• Chain of Custody procedures
• Training documentation
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• ATL classes
• Ethics and Integrity I (Overview)
• Ethics and Integrity II (Annual )
• Overall Training Record organization and upkeep
3.2.4 Health and Safety Training Laboratory staff may, on occasion, be exposed to the handling of flammable solvents, compressed gases or toxic calibration standards. There are four to six staff members comprising the Safety
Committee. Some members are 40 hour OSHA trained and respirator fitted. Education in the safe
handling and disposal of these materials is accomplished as follows:
• Each new employee is given a safety tour of the facility within the first two weeks of employment. Documentation of this orientation appears in the employee’s training record.

• The Safety Committee meets quarterly (or more frequently if needed) to discuss safety concerns
and ways of improving safety in the work place.

• The Safety Committee schedules on going safety training throughout the year.

• If special precautions must be taken to perform a method, a safety section is included in the
method SOP which discusses protocols and other measures for risk reduction through exposure prevention.
• ATL maintains Material Safety Data Sheets (MSDS) for each chemical used on-site. The MSDS are accessible to all personnel in the library area immediately outside the standards room and/or
electronically through the chemical inventory database (CISpro).
• ATL has access to MSDSs on the Internet through its vendors.
The Safety Committee staff members are assigned to duties including hazardous waste disposal,
incident or spill management, scheduling staff training, safety site assessments, Chemical Hygiene Plan review, and the overall leadership of the safety program.
3.3 ASSESSING ADHERENCE AND COMMUNICATING FINDINGS
The QA team plays a key role in establishing quality policy and protocols. The QA Department ensures that the established guidelines are followed through various quality control programs, which
are designed to detect non-compliance or departure from protocol. Each quality control program
includes documentation of the assessment process and timely feedback to the management and staff involved.

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3.3.1 Data Review
The QA team reviews Work Orders which the client has requested 100% QA review. For work that
falls under the scope of the DoD, the QA team reviews 10% of the Work Orders. Deficiencies noted during review are documented and communicated to the staff involved.
QA REVIEW CHECKLIST  Assessing Analysis/Reporting vs. Project Profile/SOP requirements  Verification of reporting list, units and report header information  Assessing accuracy and completeness of the laboratory narrative  Documentation of any corrective actions  Documentation of unusual circumstances  Verification of the QC meeting criteria  Verification of sample holding time  Verification of appropriate data flags  Appropriate peak integration and documentation for manual integration  Verification of adherence to analytical sequence clock times  Verification of the appropriate Initial Calibration  Manual verification of one sample result from raw area counts  Verification of sample dilution factors  Checked samples for trends  Verification of sample id’s vs. COC  Assessing accuracy and completeness of the Client Lumen report (if applicable)

The QA reviewer will look both for appropriate as well as inappropriate laboratory practices. Inappropriate practices are those which fall outside established laboratory SOPs. If inappropriate practices are suspected, the QA reviewer will verify the result with the QA Manager and the
Laboratory Manager, initiate a Corrective Action Request, and if necessary, form a committee consisting of but not limited to the Laboratory Manager, Technical Director, and Laboratory Director. Most Corrective Action Requests may be traced to human error. Oversights of this nature are simply
documented and feedback is given to the Analyst or Scientist involved. On occasion, the committee may determine that the Corrective Action Request was not attributable to
simple human error. The reasons for the non-conformance and appropriate action to be taken are discussed and implemented by this committee. Typical actions include retraining of the individual
involved along with a remedial period of close monitoring by the Laboratory Manager. The QA team
or an approved peer reviews all data reported by the Analyst during the remedial period. The laboratory uses a three-strike rule with respect to non-compliance issues. New Analysts are
rigorously trained to follow SOPs. This training lasts several months. Re-training is done if there is
cause to suspect non-compliance. Secondary training typically lasts 30 days. Any further evidence of non-compliance may result in termination.
Project Managers document in the Project Profiles projects that specify 100% QA review. When samples are received the Sample Receiving Team will automatically add a QA review to a Work
Order if 100% frequency has been requested as per the profile. After QA review is complete the reviewer enters the review date in the sample tracking database. If a
QA reviewer discovers an error, necessary corrections are made and the work order is reissued.
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Another tool used for data review involves the use of proprietary in-house data validation software to
review every data point generated and to alert the reviewer when manual integrations occur. The software is also programmed to report each analyte that does not meet acceptance criteria in the QC
and/or sample(s). (Validation software currently reviews all method TO-14A/TO-15, TO-17, ASTM D-5504, TO-3, TO-12 and SW8260B results. Further software development is ongoing to bring more methods on line).
3.3.2 Corrective Action Program
The QA Department manages the Corrective Action Program and maintains the Corrective Action tracking database using the c.Support software program. A Corrective Action Request (CAR) is
initiated any time sample results are adversely affected by system non-conformance with established
SOPs or program requirements, any time an internal or external assessment results in a finding, any time there is a failed proficiency evaluation sample, any time there is a failure quality system such
that data quality is (or could be) affected, and lastly, any time there is a client inquiry into the
laboratory’s data quality and laboratory error is found (see Exhibit 3.2). Requests are documented in the CAR database using the c.Support software (see Exhibit 3.9). The database is also used to track
corrective action and preventive action taken, the date of resolution, the necessity for a follow-up, and the date the follow-up action is completed.
Corrective Action Requests which require immediate resolution must be completed and finalized within 2 business days. All other CARs must be resolved within 30 business days. The status of unresolved corrective actions, including follow-up actions, is discussed during the bi-weekly QA
meetings.
Whenever a client raises an issue relating to data quality, the inquiry is documented in the Client
Contacts database. A representative of the Laboratory management or QA personnel reviews the data in question and investigates any systematic problem that may be evident. If results of the review and
investigation merit corrective action a CAR will be initiated along with any necessary follow-up
action. Examples of when the client inquiry CAR may be initiated include:

• Blind field duplicates that do not agree
• Field blanks that had contamination present.
• Blind proficiency sample that did not meet accuracy objectives
• Sample splits that do not meet precision objectives
• Outlet sample results that were higher than inlet sample results
• Sample results that cannot be manually verified
• Sample results that do not meet program requirements
A portion of the CAR database is associated with sample receiving and analysis and the identification of a short-term resolution directly related to the handling of client sample results affected by the
specific non-conformance. Should a malfunction occur with a pending sample, the client is contacted prior to analysis to confirm if the analysis should continue. The CAR documents the contact and
resolution of the issue. Should the decision be made to proceed with analysis then any malfunction
affecting data quality is detailed in the laboratory narrative. Instructions to proceed with analysis and narration of the affected results are documented in the CAR. A record of the CAR is included in the
relevant client workorder for documentation.

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In addition to the short-term resolution, the Manager and/or Team/Task Leader must review the CAR
and perform a root cause analysis and determine whether a long-term corrective action and preventative action are warranted. If the CAR casts doubts on the laboratory’s compliance with its
quality assurance program or the NELAP and DoD QSM standards, the QA Manager or QA Scientist will audit the lab team’s practices as soon as possible. After the corrective and preventative actions have been outlined and implemented, the QA Department follows up approximately 30 days
following the closure of the CAR to evaluate effectiveness of the resolution. A complete description of ATL’s Corrective Action Request system can be found in ATL’s SOP #61.

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Exhibit 3.2. Types of Corrective Action Requests

Sample Related
Corrective Action Request (CAR)
Client Inquiry Assessment
Finding
Lab
Receiving
Reporting
IT
General
PM
Support Services
External Assessment
Internal Assessment
Proficiency Testing
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3.3.3 QA Management Meetings
Approximately every two weeks the QA Manager leads a meeting with the Laboratory Director, the
Laboratory Manager, the IT Manager, the Team/Task Leaders and the QA staff. All other Managers and Directors are invited as optional attendees. These meetings are called to discuss the effectiveness of the quality systems, specific quality issues that may have surfaced from the time of the last
meeting, and to monitor progress with respect to open Corrective Action items. Agenda items are added and removed at the discretion of the QA Manager or QA staff.

The meeting is used as an interactive forum in which non-compliance issues are discussed with respect to the overall suitability of the quality system involved. Non-compliances are screened to see
if the quality system itself is in need of a review or modification. If it is determined that a particular
quality system needs to be designed or revised then the committee takes responsibility for restructuring that system. The issue cannot be removed from the agenda until the new system is in
place. Minutes of each meeting are kept in a QA electronic form on the QA network drive.
3.3.4 Conducting Internal Assessments The QA Department and qualified personnel conduct internal assessments of all major areas of the company on a yearly basis. Each area is separated into assessment modules by referenced
methodology and/or procedures. Whenever possible audits are scheduled to occur after the yearly update and revision of the relevant SOP. Audits are composed of three events:
• Laboratory or department assessment based on the current SOP or procedures by the QA Department and qualified personnel.

• Circulation of the assessment report and issuing of any necessary corrective action forms.

• Satisfactory response to audit findings and verification of the implementation and effectiveness of the corrective action taken.
An assessment checklist is developed for each area by the QA Manager or designated staff. The
checklist contains general, procedural, method specific, and SOP specific practices (Exhibit 3.10).
The assessment process addresses whether or not quality systems (e.g., adherence to the current revision of the SOP, proper and complete documentation practices, compliance with current
procedures etc.) are in place and understood. Health and safety issues are also covered.
Results of the assessment are summarized in the checklist which also serves as the report. Findings
that are determined to be in need of corrective action are processed through the standard CAR
program. If findings imply that there has been a significant impact on the data, the client will be contacted within 2 business days and the report will be corrected and reissued. Copies of the internal
assessment report are circulated to the Managers and Team/Task Leaders and other members of ATL management team as needed.
3.4 COMMUNICATING WITH MANAGEMENT
A review of the laboratory’s systems is performed by Senior Management on a quarterly basis to
evaluate effectiveness and to identify areas requiring improvement. This review includes internal assessment of the quality program and lab operations and external assessment through client feedback
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and audits. Reports from QA, Production, Project Management/Sales, and Safety are submitted for
review to the senior management team for discussion of key issues, identification of action items, establishment of timelines for resolution, and assignment of accountability.
To support the Management Review, the following reports are submitted to the senior management team: The QA Status Report summarizes the results of internal and external assessments, the
numbers and types of CARs generated, the status of any outstanding CARs, a summary of customer inquiries received, PT results, and the number and types of reissued sample reports.
The Production Status Report summarizes performance against key metrics such as TAT, details
changes in sample mix and sample numbers, and outlines resource needs. The Client Assessment Report summarizes feedback from our clients based on daily communication with our project
management and sales team as well as feedback collected by a third party as part of our Client
Satisfaction Index (CSI) determination. The Safety Assessment Report outlines the safety incidents and near-misses for the quarter and lists site assessment deficiencies. Details of the Management
Review system are provided in SOP#106.

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Exhibit 3.3. Example ATL Project Profile

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Exhibit 3.4. Example Laboratory Training Record

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Exhibit 3.5. Demonstration of Capability Form

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Exhibit 3.6. Continued Method Proficiency Form

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Exhibit 3.7. Example Training Record Review Check Sheet

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Exhibit 3.7. Example Training Record Review Check Sheet (Continued)

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Exhibit 3.8. Examples of Internal Training Courses
(Subject to Change)

Quality Assurance
Quality Assurance Orientation
Quality Assurance Protocols
Ethics and Integrity Training (I & II)
Inappropriate Laboratory Practices
Manual Integration Protocol

Safety
Health & Safety Training

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Exhibit 3.9. Example CAR

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Exhibit 3.10. Example Internal Audit Checklist

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Exhibit 3.10. Example Internal Audit Checklist (Continued)

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Exhibit 3.10. Example Internal Audit Checklist (Continued)

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The primary objective of the QA Program is to ensure that the laboratory is producing data that meet
the laboratory’s standard acceptance criteria for each method. Acceptance criteria from project-
specific QAPPs are also used when required.
The laboratory’s standard acceptance criteria and the sources of those criteria are specified throughout
Section 6.0 of this Quality Manual. Definitions of parameters used to assess the quality of the data are defined below.

4.1 PRECISION, ACCURACY, REPRESENTATIVENESS, COMPLETENESS, AND COMPARABILITY
4.1.1 Precision Precision measures the reproducibility of measurements. Analytical precision is the agreement among duplicate (two) or replicate (more than two) analyses of the same sample. The acceptance for
precision is determined using the relative percent difference (RPD) between the duplicate sample results. The %RSD (relative standard deviation) is used to document precision of linearity for the
initial calibrations. The formula for the RPD and RSD calculations are provided in Exhibit 4.1.
Field duplicate samples represent total precision, the reproducibility associated with the entire
sampling, and analysis process. However, the identification of field duplicate samples are typically
not known to the laboratory, and therefore not specifically evaluated by the laboratory’s QA department.

4.1.2 Accuracy
Accuracy measures correctness and includes components of random error (variability due to
imprecision) and systemic error. Analytical accuracy is measured by comparing the percent recovery of analytes spiked (as compared to the expected value) to pre-established accuracy limits (i.e., acceptance criteria). Any type of spiked sample measures accuracy. The formula for calculation of
accuracy is included in Exhibit 4.1 as percent recovery (%R) from pure and sample matrices. 4.1.3 Representativeness

Representativeness is achieved through use of the standard analytical procedures described in this Quality Manual.

4.1.4 Completeness
Completeness is the percentage of data, which meets the established acceptance criteria referenced in
Section 6.0. ATL’s goal is to achieve at least 95% completeness for both normal turn-around-time (TAT) and rush TAT data. Meeting the method specification outlined in each SOP prior to analyzing
project samples is our means of achieving this goal.

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4.1.5 Comparability
Comparability is the confidence with which one data set may be compared to another. The objective
for this QA/QC program is to produce data with the greatest possible degree of comparability.
Comparability is achieved by using standard analytical methods, reporting data in standard units, and using standard and comprehensive reporting formats.

4.2 DETECTION LIMIT, LIMIT OF QUANTITATION, AND INSTRUMENT CALIBRATION REQUIREMENTS
4.2.1 Detection Limit
The Detection Limit - DL (or Method Detection Limit) is a statistically determined value (by Method Detection Limit per 40CFR Part 136 Appendix B). The DL must be less than the Limit of Quantitation (LOQ). If the true concentration is below this value, the analyte may not be detected.
Each DL study is repeated at least once per twelve-month period, when a new instrument is installed, when there is a major change in the analytical configuration such as column, detector, sample
concentrator, sample loop size, etc. or when there is a major change in the extraction method such as
solvent, extraction apparatus, clean-up procedure, etc.
All analytical constituents noted by methods in Section 6.0 are to be reported with a valid and current
DL, but in the case of special request compounds DLs are performed only when a client specifies it to be a project requirement. Special request compounds are reviewed by the Laboratory Manager to
determine the cost to the laboratory for additional DL analyses. The additional value added is then factored into the bid that is submitted to the prospective client.
4.2.2 Limit of Quantitation
ATL reports to the Limit of Quantitation - LOQ (or Reporting Limit) which is the lowest
concentration contained in a linear calibration.
The LOQ represents a uniform value that can be accurately detected for any particular analyte on
each instrument thereby providing consistency for samples analyzed on different instruments. The LOQ is verified by the statistical and analytical DL studies.
The acceptance criterion for the DL study is a value of less than the LOQ. Corrective action including raising the LOQ may be performed if the statistically and analytically determined DL does not meet the stated criterion.

4.2.3 Instrument Calibration
Analytical instruments are calibrated in accordance with the referenced analytical methods and
internal SOPs. The acceptance criteria are summarized in Section 6.0. All specific target analytes are included in the initial and continuing calibrations.

If multi-point calibrations do not meet acceptance criteria stated in the relevant SOPs, an option to narrow the range of the curve either by eliminating the low point or the high point of the curve may
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be considered providing all project criteria are still met. Otherwise, the entire calibration curve is
repeated. Reanalysis of any level of the multi-point calibration in order to meet QC acceptance criteria is not allowed unless there is evidence of an anomaly such as instrument malfunction or an
improper load volume. Documentation of the anomaly must accompany the raw data for the Initial Calibration. Elimination of any of the inner levels of the multi-point calibration in order to meet QC acceptance criteria is not allowed.
Records of instrument calibration and records that unambiguously trace the preparation of standards
and their use in instrument calibration are maintained for 5 years. Calibration standards are traceable
to standard materials.
An Initial Calibration Verification (ICV) standard that contains all target compounds, as noted in the
Section 6.0 tables, is analyzed after each initial calibration curve to verify that the standards are correct and the calibration is accurate. The ICV is derived from a second source (or different lot)
standard. The acceptance criteria for the ICV recoveries are presented in Section 6.0. For work that
falls under the scope of the DoD, the ICV recoveries must match the CCV criteria.
In the case of special request compounds, an ICV (second source) analysis is performed only when a client specifies it as a project requirement. Special request compounds are reviewed by the Laboratory Manager to determine the cost to the laboratory for additional second source analyses. The additional
value added is then factored into the bid that is submitted to the prospective client. Analyte concentrations are determined primarily using the average RF from the initial multi-point
calibration. 4.2.4 Retention Time Windows
The techniques used to establish retention time windows for GC and HPLC analyses vary by method, based on the class of compounds targeted, as well as the instrument specifications (e.g., column type,
etc.). Protocol for establishing retention time windows can be found in the method-specific SOPs.
4.3 ELEMENTS OF QUALITY CONTROL
The various types of QC samples are described below. The method specific laboratory QC sample frequency and acceptance criteria may be found in Section 6.0.

4.3.1 Analytical Batch Definition
For non-extractable methods, samples analyzed during a single 24-hour period along with associated
matrix specific laboratory QC samples make up an analytical batch. At a minimum, any analytical batch will include a Laboratory Blank, CCV, LCS, LCSD and an end check for non-GC/MS methods.
Reporting of the batch QC samples varies according to project requirements. The number of field
samples included in any one analytical batch is limited to 20.
In the case of samples that require extraction prior to analysis, the sample preparation process defines the batch. At a minimum, the sample preparation batch will include a Laboratory Blank and a Laboratory Control Sample (LCS). The maximum number of samples included within one
preparation batch may not exceed 20 in one given day.
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4.3.2 Continuing Calibration Verification (CCV)
A Continuing Calibration Verification (CCV) containing all analytes of concern is performed at the
start of each day and, if required, at the start of every 12 or 24 hour clock for GC/MS analyses. GC
and HPLC sample analyses are generally bracketed by opening and end check CCVs (TO-4A and TO-10A methods excluded). Mid-batch CCVs are also analyzed as per individual SOP.

The concentration of the CCV is usually near the mid-level of the calibration. The CCV is analyzed at other concentrations within the working range at least once a quarter, or more frequently if specified
in an SOP. If the CCV fails to meet the performance criteria then the test is repeated with the same standard (or optionally with a different preparation of the same calibration mix). If the second analysis fails criteria, maintenance should be performed and the test repeated a third time. If the
system still fails the calibration verification, a new multi-point calibration curve is performed.
4.3.3 Laboratory Control Spike (LCS)
Each analytical or extraction batch contains at least one mid-level spike using a second source (or different lot) standard containing all the target analytes or the target analytes required by the method.
In the case of non-extracted batches, the LCS is generally analyzed daily prior to sample analysis, but
may also serve as an End Check standard. If the stated criteria are not met, the system is checked and the standard reanalyzed. In the event that the criteria cannot be met, the instrument is recalibrated. In
the case of extracted LCS, out-of-control recoveries result in data flags since samples cannot be re-
extracted.
For work that falls under the scope of the DoD QSM the LCS control limits must be derived from historically generated limits. Marginal Exceedances are also evaluated for the LCS and must be within criteria for the analysis to continue.

4.3.4 Internal Standard (IS)
For all GC/MS methods an IS blend is introduced into each standard and blank to monitor the
stability of the analytical system. The internal standard acceptance criteria vary by method, but for all applicable analyses at ATL, if the internal standards for the blank do not pass the acceptance criteria,
the system is inspected and the blank reanalyzed. Analyses are discontinued until the blank meets the
internal standard criteria.
4.3.5 Surrogates

For GC/MS methods and some GC methods, the recovery of the surrogate standard is used to monitor for unusual matrix effects, gross sample processing errors, and to provide a measure of recovery for
every sample matrix. The surrogate recovery acceptance criteria vary by method, but for all applicable analyses at ATL, if the surrogate recoveries for the Laboratory Blank do not pass the acceptance criteria, the system is inspected and the blank is reanalyzed. Analyses are discontinued
until the blank meets the surrogate recovery criteria. In some extractable methods, surrogates are added prior to extraction to monitor the efficiency of the
extraction process. If the surrogate recoveries are outside acceptance limits, reanalysis occurs. Re-extraction of samples is not possible.
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If the surrogate recoveries for a sample are outside the limits, the sample is reanalyzed unless obvious matrix interference is documented. If the surrogate recoveries are within limits in the reanalysis, the
second analysis will be reported. If the surrogate recoveries are out of limits a second time, the initial analysis is reported with a narrative indicating that the acceptance criteria for surrogate recoveries are exceeded. Upon request, the data from the matrix effect confirmation analysis is provided to the
client.
For work that falls under the scope of the DoD QSM the Surrogate control limits must be derived
from historically generated limits 4.3.6 Laboratory Blank A Laboratory Blank is analyzed after any applicable standards and prior to the analysis of project samples. A blank is also analyzed in the event saturation-level concentrations are incurred to
demonstrate that contamination does not exist. For methods that involve an extraction, a Laboratory Blank is prepared with each set of no more than 20 samples per method per matrix.

The acceptance criterion for the Laboratory Blank is a result less than the Limit of Quantitation (Reporting Limit). The Laboratory Blank is analyzed immediately after the LCS (non-extractable
analysis) or the CCV (extractable analysis) to ensure that both the instrument and extraction process
are free from contamination. When samples that are extracted together are analyzed on different analytical clocks, a solvent (instrument) blank is analyzed to demonstrate that the instrument is free
from contamination. For work that falls under the scope of the DoD, the acceptance criterion for the Method Blank is as
follows:
No analytes detected at ≥ ½ the RL. For common laboratory contaminants, no analytes detected ≥ the RL. If an analyte in the laboratory blank fails these criteria the associated samples must be
reprocessed in another analytical batch unless the analyte resulted in a non-detect. If no sample volume remains for re-analysis, the results will be reported with the appropriate data qualifying code (B flag).

4.3.7 Laboratory Control Spike Duplicate (LCSD)
To provide a measure of instrument precision, the LCS is analyzed twice to provide an LCSD
per analytical batch. The LCSD is analyzed once per analytical batch. The RPD between
duplicates must be ≤ 25% for detections greater than 5 times the reporting limit. If this limit
is exceeded, the sample is re-analyzed for a third time. If the limit is exceeded again, the
cause is investigated. If no problem is found on the system, the last two results are reported,
and the data is narrated to note the non-conforming event.
4.3.8 Matrix Spike
Matrix spiking permanently alters the native concentrations of whole air samples. Therefore, matrix spiking is performed only on samples, such as condensates, submitted as part of a sampling train or on extractable samples provided they are submitted in duplicate for matrix spike and in triplicate for
the matrix spike duplicate. When applicable, matrix and matrix duplicate spiking is performed using a
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subset of target analytes. Recoveries and demonstrated reproducibility values, which do not meet the
acceptance criteria, are flagged and explained in the laboratory narrative.
4.3.9 Field QC Samples
Field blanks, field spikes, and field duplicates are generally treated as normal project samples by the
laboratory. The exceptions include methods in which the laboratory at the direction of the client specifically prepares the sample media. To assure consistency it is recommended that certified
Summa canisters connected to a sampling tee be used for the collection of field duplicate samples.

4.4 QUALITY CONTROL PROCEDURES
4.4.1 Holding Times All sample preparation and analysis are to be completed within the method-required holding times. The analytical holding time for a non-extractable method begins the day of sample collection. For
extractable methods, the holding time is calculated from the day of sample collection for the extraction process and from the day the extraction process begins for the analytical process.

If holding times are exceeded, a CAR form (Section 3.3.2) is generated, the client is notified, and situation is narrated on the final report.

4.4.2 Confirmation
GC and HPLC methods do generally not perform quantitative confirmation for air sample analysis.
The exception is for analysis of pesticides by SW-846 methodology, in which case, second column confirmation is completed within the method-required holding times.
4.4.3 Standard Materials
All purchased supplies, reagents, solvents and standards are verified as acceptable and meeting
criteria for analysis prior to use. All neat and liquid standards used are traceable to the National
Institute of Standards and Technology (NIST) and NIST traceable weights are used to verify balance calibration. Documentation from the manufacturers is maintained to verify each standard. Gaseous
standards (which are by nature unable to be quantified on a balance) are verified by accuracy
documentation supplied by the manufacturer.
A second source (or different lot) standard is used to confirm the accuracy of primary source
calibration standards. Ideally the second source is obtained from a vendor other than that of the primary standard. In the case of TO-14A/TO-15 a reliable second source vendor may be difficult to
find and therefore a different lot standard may be used for this purpose. These standards are used for the laboratory control spikes as well. Non-standard and polar TO-14A/TO-15 compounds may be prepared from neat standards. Second source standards for these compounds are either derived from a
different vendor or from a different lot if only one vendor exists.

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4.4.3.1 Liquid Standards
Liquid Standards are prepared by dilution from commercial sources. Stock solutions are purchased
and stored in a designated refrigerator/freezer separate from samples. Dilutions to working ranges are
prepared using high purity solvents. Solvents are logged into the receiving logbook and the date of arrival is documented. Open solvent containers are stored in a vented, flammables cabinet.

4.4.3.2 Gas Standards Gas standards are purchased from a commercial supplier and stored in vendor recommended
cylinders using high purity regulators. Standards that are not available in certified blends from commercial suppliers are purchased in neat form. Neat materials are purchased with a purity of at
least 96% whenever possible.
Certified gas blends are purchased at parts per million volume (ppmv) levels and diluted into the working range by transfer into 1.0 L or 6.0 L certified evacuated SummaTM canister. The canister is
then pressurized to 5.0 psi or 15.0 psi depending on the volume. Alternatively, a high purity flow controller is used to fill a conditioned Tedlar bag with a controlled volume of N2 or zero air. Neat
liquid standards are transferred into the Tedlar bag by injection to achieve the desired concentration.
The standard is given sufficient time for equilibration and then is transferred into a conditioned SummaTM canister and pressurized appropriately to achieve the desired final concentration.

Concentration of the blend is determined using density based calculation:
ppbv =
∗ 24.45 is the molar volume of any gas at normalized pressure (1 atmosphere) and temperature
(25°C), derived form the ideal gas law (PV = nRT), where R = the universal gas constant.
ng/MW
vol(L)/24.45*

Once blended, the standard is transferred into a SummaTM canister for long-term storage and stability.

The preparation of working standards, in gaseous or liquid states, is documented in bound standard preparation logbooks. Each standard is given a unique identification number. Additional information
including the solvent or standard lot number and stock standard concentration is noted. Each page is signed and dated by the analyst.
4.4.3.3 Reagent Water
The laboratory uses water to prepare moist Laboratory Blank canister samples, VOST condensate
water blanks and water impinger blanks. The volume of water required for these purposes is insignificant. As such, the laboratory relies on high purity HPLC grade bottle reagent water, which is
subjected to a constant purge flow of Ultra High Purity Nitrogen. The water is purchase certified and
then supported by certifying Laboratory Blank analyses.

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4.4.4 Expiration Dates of Standards
4.4.4.1 Primary Standards
Primary standards expire according to the manufacturer’s expiration date. If the manufacturer does not assign an expiration date, a period of one year from the date of opening is applied. Expiration
dates are noted on standard labels. Expired standard materials are either revalidated by comparison
with unexpired independently prepared standards, or are discarded. The acceptance criterion for standards revalidation is documented in ATL SOP #33. The newer of the two standards is always
used as the primary source. Expiration dates for laboratory-prepared stock and diluted standards are no later than the expiration
date of the stock solution or material. All efforts are made to obtain the highest purity possible when purchasing neat chemical standards.
The vast majority of neat standards are ≥ 96% pure. The concentration of material purchased at less
than 96% purity is corrected mathematically to assure that dilutions for working standards are accurate.
Neat liquid standards are used until analysis by GC/FID indicates a purity of less than 96% (or less than the stated purity for the exceptions). The date of the purity check is noted on the neat standard
vial. Purity analysis is performed once per year or as needed.

4.4.4.2 Secondary Standards
Secondary Standards are assigned based on the expiration date of the primary source standard (i.e., no
later than), the compounds present, and container type. Typical expiration dates are presented in Exhibit 4.2.

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Exhibit 4.1. Statistical Calculations

Statistic Symbol Formula Definition Uses
Mean 
n
Σ Xii=1n
Measure of central tendency
Used to determine average value of measurements
Standard
Deviation S Σ(Xi-X)2
(n-1)
½

Measure of relative
scatter of the data
Used in calculating
variation of measurements
Relative Standard Deviation RSD ()S /X x 100
Relative standard deviation, adjusts for magnitude of observations
Used to assess precision for replicate results
Percent Difference %D
1
21
X
XX− x 100 Measure of the difference of 2 observations
Used to assess accuracy
Relative
Percent
Difference
RPD

Measure of
variability that adjusts for the
magnitude of observations
Used to assess total
and analytical precision of
duplicate measurements
Percent
Recovery %R XmeasXtrue x 100

Recovery of spiked
compound in pure
matrix
Used to assess
accuracy
Percent Recovery %R 
value of value of
spiked - unspiked
sample sample
Value of added spike
Recovery of spiked
compound in sample matrix x 100
Used to assess matrix effects and total precision
Correlation Coefficient r see SW8000B section 7.5.3 Evaluation of “goodness of fit” of
a regression line

X = Observation (concentration) n = Number of observations
X
(X1 - X2)
(X1 + X2)/2 x 100
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Exhibit 4.2. Expiration Dates

Gas Standards Prepared from Certified Cylinders

TO-14A/15 List 3 days 3 months Compounds Tedlar Bag Standard Summa Canister
BTEX/TPH 3 days 3 months
Sulfur Compounds > 3000 ppbv 7 days NA
Sulfur Compounds < 3000 ppbv* 1 day NA
Gas Standards Prepared from Neat Materials
TO-14A/15 Extra Compounds 3 days 6 months Compounds Tedlar Bag Standard Summa Canister
Other Compounds 3 days 6 months

Liquid Manufacturer’s Certified Mix and Single Component Standards The manufacturer’s expiration date is used when indicated. If none is supplied, the following expiration dates are applied:

Liquid Stock Standards Prepared from Neat Materials
Compound Expiration
Gases in Liquid 1 month after opening ampule
Other Volatile compounds 6 months after opening ampule Semivolatile/Pesticides/PCBs 1 year after opening ampule

Semivolatile/Pesticides/PCBs 1 year
Compound Expiration Gases in Liquid 1 month
Other Volatile Compounds 6 months

* Used for Initial Calibration only.
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5.0 SAMPLE HANDLING
5.1 SAMPLING MEDIA AND PRESERVATION REQUIREMENTS
General guidelines regarding sampling media, preservation, and holding time requirements are summarized in Exhibit 5.1. The laboratory first refers to project specific requirements. These
requirements can be found in the individual Statement of Work (SOW) or Quality Assurance Program Plan (QAPP). If there are no project specific guidelines, the lab uses the criteria presented in Exhibit
5.1.
Disclaimer: ATL assumes no real or implied responsibility or liability for client-related field
sampling and shipping activities. It is the responsibility of the individual client to ensure that referenced methodologies are followed with respect to sample collection and shipment to the laboratory. Air sampling media and equipment should only be used by experienced field engineers. It
is the ultimate responsibility of the client to be knowledgeable both in sample preservation requirements as well as relevant State, Federal, and International shipping requirements. Any time a chemical substance is collected using ATL media, the client bears sole responsibility to understand
and abide by the laws involving shipment of potentially hazardous substances by common carrier. 5.1.1 Sample Containers Items provided by the laboratory include:
• Sampling media such as Tenax®, Anasorb®-747, charcoal traps, TO-17 tubes, TO-11A cartridges, SummaTM polished canisters, PAC 250s, Tedlar bags, PUF/XAD, Passive samplers,
Methanol impingers, QMA filters, XAD-2 Traps, and DNPH impinger solution
• Chain-of-custody forms
• Sampling labels
• Chemical ice packs
• Shipping containers
• Custody Seals (per client request)
• Sample Acceptance Policy
Air sampling media prepared by the laboratory for field use must be certified for cleanliness. Tenax®, Anasorb®-747, charcoal traps, TO-17 tubes, PUF/XAD, TO-11A, XAD-2 Traps, and DNPH impinger solutions are certified for each preparation batch. The canister cleaning process is batch
certified. Individually certified canisters are also available per specific client request. 5.1.1.1 SummaTM Canisters
The Support Services Department has dedicated approximately 2600 ft2 for canister cleaning and
certification functions. Approximately 150 canisters can be cleaned daily and up to 100 canisters
individually certified daily. This area is also sufficient for storage of approximately 600 canisters and the entire in-house inventory of flow controllers (see Table 2.2).

When canisters are first purchased they are all cleaned, certified and verified as meeting acceptance criteria prior to use. After that, canisters that are cleaned per ATL SOP #7 are batch certified by
GC/MS analysis for TO-14A/TO-15 target compounds. 6.0 L and 1.0 L canisters are certified to be
clean to 0.2/0.5/0.8 ppbv for the standard product TO-14A/TO-15 target compound list.
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If a canister fails certification, the cleaning process is repeated. The canister is not returned to the
inventory until it has passed certification. More information on the preparation and certification of SummaTM canisters can be found in ATL SOP #7.
ATL recommends use of 100% certified canisters for projects that require Low Level and SIM TO-14A/TO-15 analysis. Project Managers document requests of this nature in the Project Profile to
assure that all shipped media meet this requirement. Canisters and associated sampling train equipment intended for projects that are defined as Low Level or SIM are certified at or below the
Limit of Quantitation. An increase in the percent of canisters certified is also recommended for
projects of a very sensitive nature.
Each ATL canister is barcoded, allowing the history of the canister to be maintained through a
canister tracking system. The database keeps information, such as, date shipped, client name, date received, and the analytical work order number.

5.1.1.2 Sorbent Tubes
Each batch of sorbent tubes is certified using the prescribed analytical methodology which most commonly is either SW-846 5041A/8260B or Modified EPA TO-17. One set of tubes from each
preparation batch are stored at 4°C ± 2°C and then certified by GC/MS analysis. Certification is
performed before the media is shipped or used to collect samples. The background level of each target VOC must be less than the project reporting limits. The client may allow an exception to this
criterion for common laboratory contaminents such as Methylene Chloride but must provide written documention to verify acceptance. The client will be notified in advance of sampling if the batch fails and a replacement shipment provided if necessary. Tube certification results are reported with
the associated Work Order Comprehensive Validation Package. More information of the preparation
and certification of sorbent tube media can be found in ATL SOP #4.
5.1.1.3 Polyurethane Foam (PUF/XAD) Cartridges PUF and PUF/XAD cartridges are batch cleaned using a large soxhlet extraction apparatus per SOP
#14. The weekly cleaning capacity is 200 PUF/XAD cartdriges and approximately 50 media are available for shipping at any point in time (see Table 2.2). For Method TO-13A, two PUFs from each
batch are cleaned and extracted and analyzed by GC/MS. For Methods TO-4A and TO-10A, one PUF
from each batch is extracted and analyzed by GC/ECD. For Method TO-13A XAD media, 20 mLs of the media is extracted and analyzed by GC/MS. For XAD-2 trap (mm5 sampling train),
approximately 30 grams of media is extracted and analyzed by GC/MS.
The background level of each target analyte must be less than the project reporting limits. Analysis
of the extract is performed typically prior to shipping or at very least within 24 hours of shipping. The client is notified in advance of sampling if the batch fails and a replacement shipment is provided if necessary.

5.1.1.4 2,4-Dinitrophenylhydrazine (DNPH) Impinger Solution and Cartridges
The DNPH solution is prepared in bulk solution. An aliquot is removed, extracted and analyzed according to the particular method (CARB 430, Method 0011, Compendium Methods TO-5 and TO-
11A). The DNPH reagent and the TO-11A media are certified as acceptable when the concentration
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of each analyte in the certification is below the reporting limit. In the case that contamination is
present above the reporting limit; the source must be identified and eliminated prior to shipping of the reagent and the TO-11A media. If the contamination can not be eliminated, the presence of any
aldehyde necessitates a call to the client. The data user, particularly in the case of source testing, may tolerate concentrations of target aldehydes near the reporting limit. Certification is completed before solution is shipped to the field. Per client request, results are shipped with the media or faxed to the
site and are also kept on file in the laboratory. More information of the preparation and certification of DNPH media can be found in ATL SOP #62.

5.2 SAMPLE COLLECTION PROCEDURES
– FIELD GUIDELINES
5.2.1 Information for Canister Sampling Air Toxics Ltd. provides a technical “how to” guide on canister sampling. The guide includes the
following information:
AIR TOXICS’
GUIDE TO AIR SAMPLING AND ANALYSIS
Canisters and Tedlar Bags
Sixth Edition
1.0 Introduction 1.1 Whole Air Sampling of VOCs 1.2 Choosing Between Canisters and Tedlar Bags
2.0 Canisters and Associated Media 2.1 Introduction to Canisters 2.2 Associated Canister Hardware
3.0 Sampling with Cansiters 3.1 Grab Samples 3.2 Integrated Samples
4.0 Sampling with Tedlar Bags 4.1 Introduction to Tedlar Bags 4.2 Tedlar Bag Sampling
5.0 Special Consideration Sampling 5.1 Special Sampling Configurations 5.2 Considerations for Sampling at Altitude
5.3 Considerations for Soil Gas/Landfill Gas Sampling
Tables
1.2 Comparison of Canisters to Tedlar Bags 2.2.3 Fill Times for Canisters
3.2.3 Flow rates For Selected Sampling Intervals 3.2.4 Relationship Between Final Canister Vacuum, Volume Sampled and Dilution Factor

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5.2.2 Information for Sorbent Tube Sampling
Contents of the guide include:

AIR TOXICS’
GUIDE TO AIR SAMPLING AND ANALYSIS
Sorbents and Solutions
Second Edition 1.0 Introduction
2.0 Sorbent Sampling 2.1 Considerations for Sorbent Sampling 2.2 Method Specific Sampling Instructions
EPA Method TO-4A EPA Method TO-10A EPA Method TO-13A High Volume EPA Method TO-13A Low Volume EPA Method 0010/8270C by MM5 Train EPA Method TO-17
EPA Method VOST 0030/5041A NIOSH 5515 3.0 Solution Sampling 3.1 Method Specific Sampling Instructions EPA Method TO-5 EPA Method TO-11A
CARB 430 Method EPA Methods 0011 Air Toxics Ltd. Method - Siloxanes
4.0 Filter Sampling 4.1 Method Specific Sampling Instructions EPA Method PM10 & TSP

The information provided in ATL’s Sampling Guide is meant to serve only as general guidelines. In all cases, field sampling personnel are ultimately responsible for having expertise and knowledge in
air sampling methodology sufficient to ensure that the defensibility of the data will not be
compromised due to deficiencies in field sampling, handling or transportation. 5.3 SAMPLE RECEIVING PROCEDURES
Upon arrival at the laboratory, samples are received and inspected following Air Toxics’ sample acceptance criteria as outlined in SOP #50. The SOP establishes specific guidelines for sample
acceptance, which are generally accepted practices under EPA, DoD, and NELAP protocols. When
samples do not meet the established guidelines, discrepancies are documented and the client is notified. Samples are noted in the individual Work Order and discrepancies noted in the Laboratory
Narrative portion of the sample report. 5.3.1 Sample Acceptance Policy
Samples received by Air Toxics Ltd. must be relinquished following standard EPA approved
guidelines. These include full and complete Chain of Custody (COC) documentation indicating:

• Unique sample name
• Location, date, and time of collection
• Canister Number
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• Collector’s name
• Preservation type (if applicable)
• Matrix
• Any special remarks
The COC form (Exhibits 5.2 to 5.2d) must be filled out in ink and indicate proper preservation and
use of sample container specified by the method. Each sample should be labeled with unique, durable, and indelible identification and must be of adequate volume for the tests requested. Never affix a label directly on a SummaTM canister. A tag is attached to each canister for this purpose.

Proper, full, and complete inspection and documentation will be performed upon laboratory receipt in the following areas:

• Evidence of container’s physical damage
• Status of the container’s custody seal
• Presence or absence of a COC form
• Incomplete or incorrect COC form
• Number of samples
• Name of each sample
• Sample collection date/time
• Name of the Project Manager
• Canister ID (if applicable)
• Preservation type (if applicable)
• Sample type (canister, XAD, DNPH etc.)
• Sample tag information complete
• Temperature (if applicable)
• Pressure (canisters)
• Presence of unlabeled samples
• Presence of mis-labeled samples
• Presence of unused media
• Method required trip blanks, field blanks, equipment blanks, field duplicates, or field spikes
Any sample discrepancies against the above criteria are documented on the Sample Discrepancy
Form (Exhibit 5.3), and communicated to the client via Electronic Sample Receipt Confirmation within 1 day of sample receipt. The client is contacted by the Project Manager for discrepancies of a more serious nature, e.g.,

• Chain of Custody Record was not received with sample(s).
• Analysis method(s) is(are) not specified.
• Sample(s) received out of holding time.
• Sample container (Tube/VOA vial) was received broken.
• Canister sample received at >15”Hg (not identified as a Trip/Field Blank).
• Tedlar Bag received leaking.
• Tedlar Bag received flat.
• Tedlar bag / canister received emitting a strong odor (sample cannot be analyzed).

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Documentation of client notification is included on the form along with any instructions from the
client on how to proceed. Project Managers complete this section and return the form to the Receiving group to complete the login process. The form is archived in the Work Order folder.
Whenever there is any uncertainty of how the laboratory is to proceed or when the desired method is unclear, the Receiving staff places the Login process ON HOLD and delivers the Work Order file to a Project Manager for follow-up. The Project Manager contacts the client to clarify the situation.
Phone calls between the Project Manager and the client are documented in the Project Management Software. The phone contact and client instructions to resolve the issue are logged into the database
and a hardcopy report is placed in the Work Order folder. The folder is then returned to the
Receiving team to complete the Login process. Air bills, packing lists, Chain of Custody records, and any other documentation that may accompany the samples are placed in the Work Order folder.

Laboratory malfunctions occurring during/after sample receipt are documented via the laboratory Corrective Action system. Examples of receiving problems, which would necessitate a Corrective
Action Request, include:

• Hold time expired due to laboratory error.
• Canister sample pressurized with wrong type of gas.
• Sample placed On Hold was released in error.
• Sample logged in for incorrect analysis method.
• DANGER tag was not affixed to an odiferous canister sample before sending to the lab.
• Canister was released and cleaned before second analysis method was run.
• Canister valve was left open following pressurization. Sample vented to ambient. 5.3.2 The Sample Receipt Confirmation When a Work Order is completed, Sample Receipt Confirmation (SRC) is sent to the client to
confirm receipt of samples. A fax is sent if no email address is available. The Sample Receipt
Confirmation has six sections:
Section 1 Introduction Page (not available if faxed) Section 2 Cover page with discrepancies noted Section 3 Sample Receipt Summary (sample names, etc.)
Section 4 Copy of Chain of Custody Section 5 Reporting template showing referenced method, target compound list, and reporting limits Section 6 Media outstanding (if relevant)

Discrepancies are noted on the cover page using a template of pre-approved statements. The QA Department is responsible for maintaining the approved template. Receiving staff electronically copy
relevant statements from the template and onto the SRC cover page. Typical statements include:
• Volume I 2009 TNI Standard (EL-V1-2009) specifies that a legal Chain of Custody must
accompany samples when they arrive at the laboratory. In this case a chain of custody was not received with the samples. The discrepancy was noted in the Login email.

• The Chain of Custody (COC) form was not relinquished properly. A <signature OR date> was
not provided.

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• Samples were received past the recommended hold time of _____ days. Analysis proceeded.
• The sample collection date was incomplete on the Chain of Custody (COC) for samples(s) <insert
names>. The client was contacted and a date of <enter date> was provided.
• The Tedlar bag for sample _____ was received flat. The client was notified that analysis was not possible.
• A Temperature Blank was included with the shipment. Temperature was measured and was not within 4±2 °C. Coolant in the form of ice/blue ice was present. Analysis proceeded.

5.3.3 The Work Order Folder
A folder is created during the Login process to hold all relevant documents. The folder is labeled with the unique Work Order number, client name and analysis. One folder for each desired analysis is created so that laboratory analyses can be efficiently handled as separate processes. The folder
contains the following receiving/login documents:
• Original COC record, airbill, and any other packing documents
• Sample Receipt Summary with individual field sample names, dates of collection and project
reference
• Specific method cited, and a copy of the reporting target compound template for review
• Login Review Checklist
• The Sample Discrepancy Report (attached electronically)
• Copy of the Project Management Project Profile with associated special analysis and reporting
requirements
• The Receiving Report (for ATL media only)
• ATL Shipment Report (attached electronically if shipping charges apply)
• Copy of any approved Project Requirement Tables generated after the bid has been won
The folder is passed to the analytical teams after Login, and follows the same process stream as the samples. All original documents generated during the processing of the samples are filed in this folder. The unique Work Order file makes archival and retrieval of evidentiary and custodial
documents easier. The majority of analytical documentation is archived electronically. Documentation that remains in hard copy form includes:
• COC
• Data Review Checklist
•
• Scan Packets (run logs, spectral defenses, manual integrations etc.)
• Phone contacts and e-mails
• Fed-Ex/UPS air bill/freight bill

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Alternatively, the Work Order folder is placed in a bar coded storage box for long-term storage. The
storage boxes are either stored on-site or Work Order inventory of each box is taken prior to offsite storage and maintained along with the bar code address. A private storage company archives the
boxes by barcode and provides one-day retrieval service upon request. 5.4 SAMPLE TRACKING PROCEDURES
After samples have been inspected, they are given a unique tracking number and logged into an
electronic sample receiving database. The tracking number consists of the year and month plus a
sequential Work Order number. As an example, the first set of samples received in July, 2004 would have the format:

0407001
If this set of samples consisted of eight individual samples, then each sample is identified by a consecutive postscript such as:
0407001-01A through 08A
If more than one analysis is requested for the samples, an alphabetic designation is given to each analysis sample set:
0407001A-01A TO-15 0407001B-01A TO-3
Laboratory assigned duplicates are designated using a double postscript such as:
0407001-01AA
A more detailed discussion of the sample receiving function is given in ATL SOP #50. The
laboratory processes thousands of samples each month divided into hundreds of individual Work
Orders. An efficient user-friendly database is critical in keeping track of each individual sample, monitoring hold times, monitoring due dates, and scheduling analyses. In addition, most air projects
have specific target compound lists, reporting limit requirements, quality assurance requirements, analysis requirements, and data submission requirements. Relevant project information is immediately available as each processing step occurs. The ultimate goal of the ATL sample-
processing system is to deliver what the customer wants the first time. Report re-issues and sample re-analyses are monitored and kept to a minimum. In order to meet the quality objective (customer satisfaction), every team member has access to information describing what the customer has
requested.
The sample tracking database consists of a variable number of data fields sufficient to store project
and sample batch information. The users can then query any field in the database. Each department creates work lists from the database and inputs relevant information (e.g., completion dates, etc.)
throughout the day.
The database resides on a secured network server equipped with a daily-automated back up system.
Multiple PCs are available to each team in their respective work areas. Access privileges are defined
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and maintained by the IT team. The database is designed such that Work Order status can be
determined at any point in time. The ‘status’ field is updated each time the work progresses to a new stage in its processing. Status data include:

• Client Services
• Extractions
• Log-in
• Lab Bins
• Individual Instrument Assignment
• Data Review
• QA
• FAX
• EDD Generation
• Final Report
• Financial Hold
• Filed
Complete documentation of sample processing is maintained in the database. Each team completes
relevant portions of the database as work is finished. Selected information includes:
SAMPLE TRACKING FIELDS

Work Order number Client Services contact
Date received Client name Project name
Project ID number #Samples Date sampled
#Lab dups #Sample holds Container type
Expiration date Method specific analysis code Date promised Rush turn 24 hour clock
Screen done Date receiving done Receiving analyst initials
Log-in date Log-in analyst initials Date analysis done
Date reported Bench analyst initials Date of final report
CVP due date
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Date CVP completed Date CVP shipped
CVP analyst initials EDD due date EDD completed date
Date EDD shipped EDD analyst initials Reissue due date
Reissue reason Time Due

The electronic database is used to document and ensure that analytical hold times, reporting requirements, and project specific QC requirements are met. The database is used by the user to
provide project specific activity reports and status of incomplete work. Users may query the database
and easily produce a printed report. The sample database is the key to efficient information transfer and, as such, is a critical tool to meet the quality objective.
5.5 INTERNAL SAMPLE CUSTODY AND STORAGE PROCEDURES
The chain-of-custody for samples is documented from time of receipt until time of disposal. Internal sample chain-of-custody documentation consists of:
• Storage area logbooks
• Instrument run logs
• Raw analytical data for samples, calibrations and QC checks
The samples are stored in the custody cage, in a secure refrigerator, or in the event of late delivery in the receiving section until the next morning. The Receiving staff or pressurization personnel log the samples into the Internal Sample or Extractable Sample Tracking Logbook in the storage area.
Samples are tracked in/out of the limited access area by initials, date, and time. All staff members have access to the storage areas and all members are trained on proper custody documentation in the
logs. Logbook protocol training is mandatory for all staff. The training and documentation of
training is handled by the QA team. The QA team checks the Logbook Review Checksheet monthly to ensure that the analysts have reviewed their logbooks on a timely basis.

5.6 SAMPLE DISPOSAL
Samples are released for disposal upon satisfactory completion of analysis unless prior contractual arrangements have been made. The release of samples is documented in the Internal Sample Tracking Log via a “Released” stamp that includes the date and initials of the person who releases the
sample for disposal. Samples are released following the procedures outlined in ATL’s SOP #63.
Sample disposal varies based on the sampling media. Whole air samples are vented through a
charcoal scrubber, while liquid (i.e., solvent and water) samples are disposed of according to the procedures noted in ATL’s Chemical Hygiene Plan.

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5.7 SUBCONTRACTING
Air Toxics Limited subcontracts samples on an infrequent basis. Subcontracting is generally
performed for contractual reasons in fields of testing which the laboratory does not perform. In the event that subcontracting is necessary, the client, working with the Sales or Project Manager, selects a suitable subcontract laboratory that meets the project specified certification criteria. Work that falls
under the scope of NELAC accreditation shall be placed with a laboratory accredited under NELAP for the tests to be performed or with a laboratory that meets applicable statutory and regulatory
requirements for performing the tests and submitting the results of tests performed. The laboratory
performing the subcontracted work shall be indicated in the final report and non-NELAP accredited work shall be clearly identified. If the project has no criteria, then the client may choose to select a
subcontract laboratory based on state certification in the desired field of testing. If subcontracting
samples is necessary for an analysis that we normally perform, the Project Manager shall advise the client of the arrangement in writing and, when possible, gain the approval of the client, preferably in
writing. Work that falls under the scope of the DoD shall be placed with a laboratory that is DoD accredited
and meets the DoD QSM requirements for the tests to be performed. In addition, the subcontracted laboratory must receive project-specific approval from the DoD client before any samples are analyzed. More information for subcontracting samples can be found in ATL SOP #90.

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Exhibit 5.1. Requirements for Containers, Preservation Techniques, and Holding Times
Method Parameter Type Container Preservation Extraction Analytical
Holding Time Holding Time
VOST VOCs GC/MS Sorbent Tube 4°C NA 14 days
5041A/8260B
TO-14A, BTEX/TPH GC/FID/PID Summa Canister NA NA 30 days
TO-3 & CARB 410A Tedlar Bag NA NA 3 days
TO-4A & Pesticides GC/ECD PUF 4°C 7 days 40 days TO-10A PCBs
TO-5 & Aldehydes HPLC/UV DNPH Impinger 4°C 7 days 30 days CARB 430 & Ketones
TO-11A Aldehydes HPLC/UV Sep-PAK 4°C 14 days 30 days
& Ketones
TO-12 NMOC GC/FID Summa Canister NA NA 30 days
Tedlar Bag NA NA 3 days
TO-13A/ PAHs/ GC/MS XAD/PUF 4°C 7 days 40 days 8270 Semivolatiles
TO-14A/15 VOCs GC/MS Summa Canister NA NA 30 days Tedlar Bag NA NA 3 days
TO-17 VOCs GC/MS Sorbent Tube 4°C NA 30 days

ASTM Fixed GC/TCD/FID Summa Canister NA NA 30 days
D1946 Gases Tedlar Bag NA NA 3 days CH4, C2+
ASTM Fixed & GC/TCD/FID Summa Canister NA NA 30 days
D1945 Natural Gases Tedlar Bag NA NA 3 days
ASTM Sulfur Gases GC/SCD Tedlar Bag NA NA 24 hours
D5504
Method 0011 Aldehydes HPLC/UV DNPH Impinger 4°C 7 days 30 days
& Ketones
PM10/TSP Particulate Analytical Quartz Filter 59°F – 86°F NA 14 days
Matter Balance RH< 45%

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Exhibit 5.2. General Chain-of-Custody
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Exhibit 5.2b. Chain-of-Custody for Sorbent Media

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Exhibit 5.2c. Chain-of-Custody for Passive Media

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Exhibit 5.2d. Chain-of-Custody for TO-17 Media

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Exhibit 5.3. Sample Discrepancy Form

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Exhibit 5.3. Sample Discrepancy Form (Continued)

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6.0 ANALYTICAL METHODS AND PROCEDURES
This section contains subsections for each analytical procedure. Each subsection contains the following information:
• A brief method description
• Laboratory variances to Compendium and SW-846 methodologies
• A table of LOQs and QC acceptance criteria
• A table of calibration procedures and QC procedures
This Quality Manual references methods in a general manner. The specific revisions used by the
laboratory can be found in the method-specific SOPs.
6.1 ASTM D- 1945 – FIXED GASES
This method involves GC analysis of landfill gas, ambient air, or stack gas collected in SummaTM
canisters, Tedlar bags, or any vessel that has been demonstrated to be clean and leak free. Samples are
analyzed for Methane and fixed gases and can be used to speciate individual light hydrocarbons up to C6. This method is also used to determine caloric content of the gas. Because the sample is withdrawn from
the vessel by positive pressure, rigid containers are first filled to positive pressure using UHP Helium or
Nitrogen. Samples are then analyzed using a GC equipped with a FID and a Thermal Conductivity Detector (TCD).
Certain compounds are not included in ATL’s standard target analyte list. These compounds are communicated at the time of client proposal request. Unless otherwise directed, ATL reports these non-standard compounds with partial validation. Validation includes a 3-point calibration with the lowest
concentration defining the reporting limit, no second source verification is analyzed, and no method detection limit study is performed unless previous arrangements have been made. In addition, stability of the non-standard compound during sample storage is not validated. Full validation may be available upon
request.
Air Toxics Ltd. performs a modified version of this method. The method modifications, standard target analyte list, Limit of Quantitation, QC criteria, and QC summary can be found in the following tables.
Table 6.1.1 Summary of Method Modifications
Requirement ASTM D-1945 Air Toxics Ltd. Modifications
Sample Injection Volume 0.50 mL to achieve Methane
linearity.
1.0 mL.
Reference Standard Concentration should not be < half of nor differ by more than 2X the
concentration of the sample. Run 2 consecutive checks; must agree
within 1%.
A minimum 3-point linear calibration. The
acceptance criterion is RSD ≤15%. All
target analytes must be within the linear range of calibration (with the exception of
O2, N2, and C6+ Hydrocarbons).
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Requirement ASTM D-1945 Air Toxics Ltd. Modifications
Sample Analysis Equilibrate samples to 20-50° F. above source temperature at field sampling.
Heating of samples is not performed.
Sample Calculation Response factor is calculated using peak height for C5 and lighter
compounds.
Peak areas are used for all target analytes to quantitate concentrations.
Normalization Sum of original values should not differ from 100.0% by more than
1.0%.
Sum of original values may range between 85-115%; normalization of data not
performed, unless requested by client.
Table 6.1.2 ASTM Modified Method D-1945 Standard Analyte List
Analyte RL (%)
Acceptance Criteria
Initial
Calibration (%RSD) CCV/LCS (%R) Precision (%RPD)
Carbon Dioxide 0.01 ≤ 15% 85 – 115 < 25%
Carbon Monoxide 0.01 ≤ 15% 85 – 115 < 25%
Ethene 0.001 ≤ 15% 85 – 115 < 25%
Ethane 0.001 ≤ 15% 85 – 115 < 25%
Acetylene 0.001 ≤ 15% 85 – 115 < 25%
Isobutane 0.001 ≤ 15% 85 – 115 < 25%
Methane 0.0001 ≤ 15% 85 – 115 < 25%
n-Butane 0.001 ≤ 15% 85 – 115 < 25%
Neopentane 0.001 ≤ 15% 85 – 115 < 25%
Isopentane 0.001 ≤ 15% 85 – 115 < 25%
n-Pentane 0.001 ≤ 15% 85 – 115 < 25%
Nitrogen* 0.10 ≤ 15% 85 – 115 < 25%
NMOC (C6+) 0.01 ≤ 15% 85 – 115 < 25%
Oxygen 0.10 ≤ 15% 85 – 115 < 25%
Propane 0.001 ≤ 15% 85 – 115 < 25%
Hydrogen 0.01*** ≤ 15% 85 – 115 < 25%
Helium 0.05** ≤ 15% 85 – 115 < 25%
* For samples that have been pressurized with N2, the amount of N2 in the sample is determined by subtraction.
** Included by special request only. *** RL is 1.0% when sample is pressurized with Helium.
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-3 Table 6.1.3 Summary of Calibration and QC Procedures ASTM Modified Method D-1945
QC Check
Minimum
Frequency
Acceptance
Criteria
Corrective
Action
Initial Calibration
Curve (ICAL)
Prior to Sample Analysis. ICAL criteria in Table 6.1.2. Correct problem, then repeat Initial Calibration.
Independent Source Check
Verification (LCS)
Once per Initial Calibration and with each
analytical batch.
LCS criteria in Table 6.1.2. Check the system and re-analyze the standard. Re-calibrate the instrument if
the criteria cannot be met.
Continuing
Calibration Verification
(CCV)

Daily prior to sample
analysis and after every 20 samples or at the end
of the analytical batch.
CCV criteria in Table
6.1.2.
Check the system and re-analyze the
standard. Re-calibrate the instrument if the criteria cannot be met. If the closing
CCV fails, the system is checked and the standard is re-analyzed. If the
second analysis fails, identify and correct the problem, then re-analyze all
samples since the last acceptable CCV.
Laboratory Blank Daily. Results less than the laboratory RL. Inspect the system and troubleshoot until the system is free of
contamination.
Laboratory Control Spike
(LCSD)
1 dup/analytical batch. RPD ≤25%. Inspect the system and re-analyze; if out again, narrate.

Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-4 6.2 ASTM D-1946 - ATMOSPHERIC GASES
This method involves GC analysis of landfill gas, ambient air, or stack gas collected in SummaTM canisters, Tedlar bags, or any vessel that has been demonstrated to be clean and leak free. Samples are
analyzed for Methane, fixed gases, and Non-Methane Organic Carbon (NMOC) using ASTM D-1946 protocols. Because the sample is withdrawn from the vessel by positive pressure, rigid containers are first
filled to positive pressure using UHP Helium or Nitrogen. Samples are then analyzed using a GC
equipped with a FID and a TCD.
Certain compounds are not included in ATL’s standard target analyte list. These compounds are
communicated at the time of client proposal request. Unless otherwise directed, ATL reports these non-
standard compounds with partial validation. Validation includes a 3-point calibration with the lowest concentration defining the reporting limit, no second source verification is analyzed, and no method
detection limit study is performed unless previous arrangements have been made. In addition, stability of
the non-standard compound during sample storage is not validated. Full validation may be available upon request.
Air Toxics Ltd. performs a modified version of this method. The method modifications, standard target
analyte list, Limit of Quantitation, QC criteria, and QC summary can be found in the following tables.
Table 6.2.1 Summary of Method Modifications
Requirement ASTM D-1946 Air Toxics Ltd. Modifications
Calibration A single point calibration is performed using a reference standard closely
matching the composition of the unknown.
A minimum 3-point calibration curve is performed. Quantitation is based on a daily
calibration standard, which may or may not resemble the composition of the associated
samples.
Reference Standard The composition of any reference standard must be known to within 0.01
mol % for any component.
The standards used by Air Toxics Ltd. are
blended to a ≥ 95% accuracy.
Sample Injection
Volume
Components whose concentrations are
in excess of 5 % should not be
analyzed by using sample volumes greater than 0.5 mL.
The sample container is connected directly to
a fixed volume sample loop of 1.0 mL.
Linear range is defined by the calibration curve. Bags may be loaded by vacuum or by positive pressure.
Normalization Normalize the mole percent values by multiplying each value by 100 and
dividing by the sum of the original values. The sum of the original values
should not differ from 100% by more than 1.0%.
Results are not normalized (unless requested by client). The sum of the reported values
can differ from 100% by as much as 15%, either due to analytical variability or an
unusual sample matrix.
Precision Precision requirements established at each concentration level. Duplicates should agree within 25 % RPD for detections >5 X’s the RL.
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Revision 22.1, 09/2011 Page 6-5 Table 6.2.2 ASTM Modified Method D-1946 Standard Analyte List
Compound RL (%)
ICAL
Criteria (%RSD)
LCS
Criteria (%R)
CCV
Criteria (%D)
Precision
Limits (RPD)
Carbon Dioxide*** 0.010 ≤ 15% 85 – 115 ±15 < 25%
Carbon Monoxide*** 0.010 ≤ 15% 85 – 115 ±15 < 25%
Methane 0.00010 ≤ 15% 85 – 115 ±15 < 25%
Ethene* 0.0010 ≤ 15% 85 – 115 ±15 < 25%
Ethane* 0.0010 ≤ 15% 85 – 115 ±15 < 25%
Nitrogen 0.10 ≤ 15% 85 – 115 ±15 < 25%
NMOC (C2+) 0.010 ≤ 15% 85 – 115 ±15 < 25%
Oxygen 0.10 ≤ 15% 85 – 115 ±15 < 25%
Hydrogen* 0.010** ≤ 15% 85 – 115 ±15 < 25%
Helium 0.050 ≤ 15% 85 – 115 ±15 < 25%
* Ethene, Ethane and Hydrogen are included by special request only.
** RL is 1.0 % when sample is pressurized with He. *** RL can be lowered to 0.001% using a Nickel catalyst and reporting from the FID by special request.
Table 6.2.3 Summary of Calibration and QC Procedures ASTM Modified Method D-1946
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Initial Calibration Curve
(ICAL)
Prior to Sample analysis. RSD ≤ 15 %. Correct problem then repeat
Initial Calibration.
Second Source Verification (LCS) All analytes - once per Initial Calibration, and with each analytical batch.
%R 85 – 115%. Check the system and re-analyze the standard. Re-calibrate the instrument if the criteria cannot
be met.
Continuing Calibration Verification (CCV) Daily prior to sample analysis and after every 20 samples. %R 85 – 115 %. Check the system and re-analyze the standard. Re-calibrate the
instrument if the criteria cannot be met.
Laboratory Blank (He)
(N2 for He and H2 analysis)
Immediately after each daily
check standard and prior to sample analysis, or when contamination is present.
Results < RL. Inspect the system and re-analyze
the Blank.
End Check At the end of analytical
sequence. It can be primary (CCV) or second source (LCS).
%R 85 – 115 %. Check system and re-analyze the
standard. If the 2nd analysis fails, correct the problem. Re-analyze
all samples since the last acceptable CCV.
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Revision 22.1, 09/2011 Page 6-6
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Laboratory Control
Spike (LCSD)
1 dup/analytical batch. RPD ≤ 25 %. Inspect the system and re-
analyze; if out again, narrate.
Chromatographic
Resolution of CH4 from CO (FID)
As needed. < 50 % valley. Re-condition the molecular sieve
column at similar levels.
Response of CO and
CO2 (FID)
As needed. < 30 %. Re-pack the tube with fresh
catalyst and allow to stabilize.

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Revision 22.1, 09/2011 Page 6-7 6.3 ASTM D-5504 - SULFUR COMPOUNDS
This method involves GC analysis of whole air samples collected in Tedlar bags. Samples are analyzed for reduced sulfur compounds using ASTM D-5504 protocols using a Sulfur Chemiluminescence
Detector (SCD).
Certain compounds are not included in ATL’s standard target analyte list. These compounds are communicated at the time of client proposal request. Unless otherwise directed, ATL reports these non-
standard compounds with partial validation. Validation includes a 3-point calibration with the lowest concentration defining the reporting limit, no second source verification is analyzed, and no method
detection limit study is performed unless previous arrangements have been made. In addition, stability of
the non-standard compound during sample storage is not validated. Full validation may be available upon request.
ASTM D-5504 is not a prescriptive method therefore modification documentation is not necessary.
Table 6.3.1 ASTM Modified Method D-5504 (Sulfur Compounds) Standard Analyte List
Analyte
RL
(ppbv)
Acceptance Criteria
ICAL
(% RSD)
LCS/ CCV
(% R)
Precision
(% RPD)
2,5-Dimethylthiophene 4.0 ≤ 30 70 -130 ≤ 25
2-Ethylthiophene 4.0 ≤ 30 70 -130 ≤ 25
3-Methylthiophene** 4.0 ≤ 30 70 -130 ≤ 25
Carbon Disulfide 5.0 ≤ 30 70 -130 ≤ 25
Carbonyl Sulfide 4.0 ≤ 30 70 -130 ≤ 25
Diethyl Disulfide 4.0 ≤ 30 70 -130 ≤ 25
Diethyl Sulfide 4.0 ≤ 30 70 -130 ≤ 25
Dimethyl Disulfide 4.0 ≤ 30 70 -130 ≤ 25
Dimethyl Sulfide 4.0 ≤ 30 70 -130 ≤ 25
Ethyl Mercaptan 4.0 ≤ 30 70 -130 ≤ 25
Ethyl Methyl Sulfide** 4.0 ≤ 30 70 -130 ≤ 25
Hydrogen Sulfide 4.0 ≤ 30 70 -130 ≤ 25
Isobutyl Mercaptan 4.0 ≤ 30 70 -130 ≤ 25
Isopropyl Mercaptan 4.0 ≤ 30 70 -130 ≤ 25
Methyl Mercaptan 4.0 ≤ 30 70 -130 ≤ 25
n-Butyl Mercaptan** 4.0 ≤ 30 70 -130 ≤ 25
n-Propyl Mercaptan 4.0 ≤ 30 70 -130 ≤ 25
tert-Butyl Mercaptan 4.0 ≤ 30 70 -130 ≤ 25
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Revision 22.1, 09/2011 Page 6-8
Analyte RL (ppbv)
Acceptance Criteria
ICAL (% RSD) LCS/ CCV (% R) Precision (% RPD)
Tetrahydrothiophene 4.0 ≤ 30 70 -130 ≤ 25
Thiophene 4.0 ≤ 30 70 -130 ≤ 25
 Average %RSD ≤ 30%, not to exceed 40% for any individual compounds. H2S %RSD must be ≤ 30%.
 Up to 10% allowed to exceed %R criterion (not to exceed ±50%); end check may have 20% exceed criterion. All compounds must be within %R limit for short list (five compounds or less)
** Compounds co-elute
Table 6.3.2 Summary of Calibration and QC Procedures for Modified ASTM Method D 5504
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Min of 3 or more points Calibration
(ICAL)
Prior to sample analysis. RSD ≤ 30% (average).
H2S must be ≤ 30%. All
others must be ≤ 40%.
Repeat calibration.
Second Source
Verification (LCS)
With each Initial
Calibration; with each analytical batch.
70 - 130 % of the
expected values for all compounds.

Check the system, re-prepare and/or re-
analyze standard. Re-calibrate instrument if criteria cannot be met.
Continuing Calibration Verification (CCV)
Daily prior to sample analysis. % R for all compounds within 70 – 130 %.

Check the system and re-analyze the standard. If the 2nd analysis fails,
identify and correct the problem.
Corrective action may include re-analysis of affected samples out of Hold Time per client request.
Laboratory Blank In between analysis of standards and project
samples.
Results less than the laboratory Limit of
Quantitation.
Inspect the system and re-analyze the blank. If the third blank still has
contamination, consult a Scientist or Laboratory Manager.
End Check At the end of the
analytical sequence.
Recoveries within 70 -
130% with 20% (4 target analytes) allowed out.
Check system and re-analyze the
standard. If the 2nd analysis fails, identify and correct the problem.
Corrective action may include re-analysis of affected samples out of Hold
Time per client request.
Laboratory Control
Spike Duplicate (LCSD)
1 dup/analytical batch. RPD ≤ 25 %. Inspect the system and re-analyze; if
out again, narrate.

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Revision 22.1, 09/2011 Page 6-9
6.4 PASSIVE SAMPLING - VOLATILE ORGANIC COMPOUNDS
This method involves GC/MS analysis of VOCs collected using charcoal-based passive samplers. These samplers are used to measure vapor-phase VOCs in a variety of gaseous matrices including indoor air,
outdoor air, extracted soil gas, and emissions from materials. VOCs in the sampling environment pass through the diffusive barrier or permeable membrane of the sampler at a known, controlled rate (defined
as the sampling rate) and adsorb to the charcoal-based sorbent pad of the sampler. The sorbent is
extracted using a volume of carbon disulfide, and the extract is directly injected into a gas chromatograph equipped with a mass spectrometer. The retention time and spectral pattern of a compound are compared with that of known standard. Concentrations of the analytes are calculated from the average relative
response factors of calibration curves obtained from analysis of standard solutions. The results are
reported in units of µg/sample or µg/m3 if the sampling rate and duration is known.
There are no regulatory methods for the preparation and analysis of the Radiello and WMS samplers, and OSHA methods are available for workplace exposure measurements for several of the VOCs using 3M OVM 3500 and SKC 575 series samplers. The OSHA methods and the recommended procedures
published by Radiello (FSM) and 3M serve as the basis for this standard operating procedure for the analysis of environmental samples. Additionally, QC elements outlined in EPA SW-846 8260 and 8270
are incorporated as applicable. One variance of note that ATL has taken to the OSHA, Radiello, and the
OVM 3500 methods is the use of GC/MS instead of GC/FID.
Table 6.4.1 Target Analytes * Acceptance limits based on Desorption efficiency studies. ** 60 – 130% for WMS
Analytes
Reporting Limit
(µg/mL )
Acceptance Criteria
ICAL
(%RSD)
ICV
(% R)
LCS
(% R) CCV
Chloromethane 0.2 30 70 – 130 50 – 140 %D ≤40%
Vinyl Chloride 0.2 30 50 – 140 50 – 140 %D ≤40%
Ethanol 0.5 30 70 – 130 50 – 130* %D ≤30%
1,1-Dichloroethene 0.2 30 70 – 130 70 – 130 %D ≤30%
Acetone 0.1 30 70 – 130 70 – 130 %D ≤30%
2-Propanol 0.1 30 50 – 130 50 – 130 %D ≤30%
MTBE 0.05 30 70 – 130 70 – 130 %D ≤30%
trans-1,2-Dichloroethene 0.1 20 80 – 120 70 – 130 %D ≤20%
Hexane 0.05 30 70 – 130 70 – 130 %D ≤30%
1,1-Dichloroethane 0.05 20 80 – 120 70 – 130 %D ≤20%
Ethyl Acetate 0.2 30 70 – 130 70 – 130 %D ≤30%
2-Butanone 0.05 30 70 – 130 70 – 130 %D ≤30%
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Revision 22.1, 09/2011 Page 6-10
Analytes
Reporting Limit
(µg/mL )
Acceptance Criteria
ICAL
(%RSD)
ICV
(% R)
LCS
(% R) CCV
cis-1,2-Dichloroethene 0.1 20 80 – 120 70 – 130 %D ≤20%
Chloroform 0.05 20 80 – 120 70 – 130 %D ≤20%
Cyclohexane 0.05 20 80 – 120 70 – 130 %D ≤20%
1,1,1-trichloroethane 0.05 20 80 – 120 70 – 130 %D ≤20%
Carbon Tetrachloride 0.05 20 80 – 120 70 – 130 %D ≤20%
Benzene 0.1 30 70 – 130 70 – 130 %D ≤30%
1,2-Dichloroethane 0.05 20 80 – 120 70 – 130 %D ≤20%
Heptane 0.05 20 80 – 120 70 – 130 %D ≤20%
Trichloroethene 0.05 20 80 – 120 70 – 130 %D ≤20%
4-Methyl-2-pentanone 0.1 30 70 – 130 70 – 130 %D ≤30%
Toluene 0.05 20 80 – 120 70 – 130 %D ≤20%
1,1,2-Trichloroethane 0.05 20 80 – 120 70 – 130 %D ≤20%
Tetrachloroethene 0.05 20 80 – 120 70 – 130 %D ≤20%
Chlorobenzene 0.05 20 80 – 120 70 – 130 %D ≤20%
Ethylbenzene 0.05 20 80 – 120 70 – 130 %D ≤20%
m,p-Xylene 0.05 20 80 – 120 70 – 130 %D ≤20%
o-Xylene 0.05 20 80 – 120 70 – 130 %D ≤20%
Styrene 0.05 30 70 – 130 20-100* %D ≤30%
1,1,2,2-Tetrachloroethane 0.05 30 70 – 130 60 – 130 %D ≤30%
Propylbenzene 0.05 20 80 – 120 70 – 130 %D ≤20%
1,3,5-Trimethylbenzene 0.05 20 80 – 120 70 – 130 %D ≤20%
1,2,4-Trimethylbenzene 0.05 20 80 – 120 70 – 130 %D ≤20%
1,3-Dichlorobenzene 0.05 30 70 – 130 50 – 110** %D ≤30%
1,4-Dichlorobenzene 0.05 30 70 – 130 50 – 110** %D ≤30%
1,2-Dichlorobenzene 0.05 30 70 – 130 50 – 110** %D ≤30%
Naphthalene 0.05 30 70 – 130 5-80* %D ≤30%

Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-11 Table 6.4.2 Internal Standard
Analyte CCV IS (%R) Sample IS (%)R
2-Fluorotoluene 50 – 200 50 – 200
Table 6.4.3 Surrogate
Analyte %R
Toluene-d8 70-130
Table 6.4.4 Sampling Rates for “Standard” target compounds (RAD 130)
Analytes
Reporting Limit
(µg/mL )
Reporting Limit
(µg/sampler)
Sampling Rates for
Radiello 130 Sampler
Chloromethane 0.2 0.4 Estimated
Vinyl Chloride 0.2 0.4 Estimated
Ethanol 0.5 1.0 102
1,1-Dichloroethene 0.2 0.4 Estimated
Acetone 0.1 0.2 77
2-Propanol 0.1 0.2 52
MTBE 0.05 0.1 65
trans-1,2-Dichloroethene 0.1 0.2 Estimated
Hexane 0.05 0.1 66
1,1-Dichloroethane 0.05 0.1 Estimated
Ethyl Acetate 0.2 0.4 78
2-Butanone 0.05 0.1 79
cis-1,2-Dichloroethene 0.1 0.2 Estimated
Chloroform 0.05 0.1 75
Cyclohexane 0.05 0.1 54
1,1,1-trichloroethane 0.05 0.1 62
Carbon Tetrachloride 0.05 0.1 67
Benzene 0.1 0.2 80
1,2-Dichloroethane 0.05 0.1 77
Heptane 0.05 0.1 58
Trichloroethene 0.05 0.1 69
4-Methyl-2-pentanone 0.1 0.2 67
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Revision 22.1, 09/2011 Page 6-12
Analytes
Reporting Limit (µg/mL )
Reporting Limit (µg/sampler) Sampling Rates for Radiello 130 Sampler
Toluene 0.05 0.1 74
1,1,2-Trichloroethane 0.05 0.1 Estimated
Tetrachloroethene 0.05 0.1 59
Chlorobenzene 0.05 0.1 68
Ethylbenzene 0.05 0.1 68
m,p-Xylene 0.05 0.1 70
o-Xylene 0.05 0.1 65
Styrene 0.05 0.1 61
1,1,2,2-Tetrachloroethane 0.05 0.1 Estimated
Propylbenzene 0.05 0.1 57
1,3,5-Trimethylbenzene 0.05 0.1 Estimated
1,2,4-Trimethylbenzene 0.05 0.1 50
1,3-Dichlorobenzene 0.05 0.1 Estimated
1,4-Dichlorobenzene 0.05 0.1 51
1,2-Dichlorobenzene 0.05 0.1 Estimated
Naphthalene 0.05 0.1 25
Table 6.4.5 Sampling Rates for “Standard” target compounds (OVM) Varied sampling rates for each compound (1 to 8hr) see the OVM Technical bulletin
Analytes
Reporting Limit
(µg/mL )
Reporting Limit
(µg/sampler)
Sampling Rates for
OVM Sampler
Chloromethane 0.2 0.30 Estimated
Vinyl Chloride 0.2 0.30 41
Ethanol 0.5 0.75 44
1,1-Dichloroethene 0.2 0.30 Estimated
Acetone 0.1 0.15 40
2-Propanol 0.1 0.15 39
MTBE 0.05 0.075 38
trans-1,2-Dichloroethene 0.1 0.15 Estimated
Hexane 0.05 0.075 32
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Revision 22.1, 09/2011 Page 6-13
Analytes
Reporting Limit (µg/mL )
Reporting Limit (µg/sampler) Sampling Rates for OVM Sampler
1,1-Dichloroethane 0.05 0.075 33
Ethyl Acetate 0.2 0.3 34
2-Butanone 0.05 0.075 36
cis-1,2-Dichloroethene 0.1 0.15 Estimated
Chloroform 0.05 0.075 34
Cyclohexane 0.05 0.075 32
1,1,1-trichloroethane 0.05 0.075 31
Carbon Tetrachloride 0.05 0.075 30
Benzene 0.1 0.15 80
1,2-Dichloroethane 0.05 0.075 33
Heptane 0.05 0.075 29
Trichloroethene 0.05 0.075 31
4-Methyl-2-pentanone 0.1 0.15 30
Toluene 0.05 0.075 31
1,1,2-Trichloroethane 0.05 0.075 30
Tetrachloroethene 0.05 0.075 28
Chlorobenzene 0.05 0.075 29
Ethylbenzene 0.05 0.075 27
m,p-Xylene 0.05 0.075 27
o-Xylene 0.05 0.075 27
Styrene 0.05 0.075 29
1,1,2,2-Tetrachloroethane 0.05 0.075 28
Propylbenzene 0.05 0.075 Estimated
1,3,5-Trimethylbenzene 0.05 0.075 Estimated
1,2,4-Trimethylbenzene 0.05 0.075 Estimated
1,3-Dichlorobenzene 0.05 0.075 Estimated
1,4-Dichlorobenzene 0.05 0.075 27.8
1,2-Dichlorobenzene 0.05 0.075 27.8
Naphthalene 0.05 0.075 25
Chloromethane 0.2 0.30 Estimated
Vinyl Chloride 0.2 0.30 41
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Revision 22.1, 09/2011 Page 6-14
Analytes
Reporting Limit (µg/mL )
Reporting Limit (µg/sampler) Sampling Rates for OVM Sampler
Ethanol 0.5 0.75 44
1,1-Dichloroethene 0.2 0.30 Estimated
Acetone 0.1 0.15 40
2-Propanol 0.1 0.15 39
MTBE 0.05 0.075 38
trans-1,2-Dichloroethene 0.1 0.15 Estimated
Hexane 0.05 0.075 32
1,1-Dichloroethane 0.05 0.075 33
Ethyl Acetate 0.2 0.3 34
2-Butanone 0.05 0.075 36
cis-1,2-Dichloroethene 0.1 0.15 Estimated
Chloroform 0.05 0.075 34
Cyclohexane 0.05 0.075 32
1,1,1-trichloroethane 0.05 0.075 31
Carbon Tetrachloride 0.05 0.075 30
Benzene 0.1 0.15 80
1,2-Dichloroethane 0.05 0.075 33
Heptane 0.05 0.075 29
Trichloroethene 0.05 0.075 31
4-Methyl-2-pentanone 0.1 0.15 30
Toluene 0.05 0.075 31
1,1,2-Trichloroethane 0.05 0.075 30
Tetrachloroethene 0.05 0.075 28
Chlorobenzene 0.05 0.075 29
Ethylbenzene 0.05 0.075 27
m,p-Xylene 0.05 0.075 27
o-Xylene 0.05 0.075 27
Styrene 0.05 0.075 29
1,1,2,2-Tetrachloroethane 0.05 0.075 28
Propylbenzene 0.05 0.075 Estimated
1,3,5-Trimethylbenzene 0.05 0.075 Estimated
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Revision 22.1, 09/2011 Page 6-15
Analytes
Reporting Limit (µg/mL )
Reporting Limit (µg/sampler) Sampling Rates for OVM Sampler
1,2,4-Trimethylbenzene 0.05 0.075 Estimated
1,3-Dichlorobenzene 0.05 0.075 Estimated
1,4-Dichlorobenzene 0.05 0.075 27.8
1,2-Dichlorobenzene 0.05 0.075 27.8
Naphthalene 0.05 0.075 25
Table 6.4.6 Sampling Rates for “Standard” target compounds (SKC Badge)
Analytes
Reporting Limit
(µg/mL )
Reporting Limit
(µg/sampler)
Sampling Rates for Indoor Air Applications ‘Zero
Face velocity’
Sampling Rates for Outdoor/worker
exposure (ml/min)
Chloromethane 0.2 0.4 Estimated Estimated
Vinyl Chloride 0.2 0.4 17.4 Estimated
Ethanol 0.5 1.0 Estimated 20.9*
1,1-Dichloroethene 0.2 0.4 9.74 12.3
Acetone 0.1 0.2 12.6 15.2
2-Propanol 0.1 0.2 Estimated 17.8*
MTBE 0.05 0.1 9.84 13.6
trans-1,2-Dichloroethene 0.1 0.2 10.2 14.8
Hexane 0.05 0.1 9.59 14.3
1,1-Dichloroethane 0.05 0.1 13.14 Estimated
Ethyl Acetate 0.2 0.4 9.26 13.1
2-Butanone 0.05 0.1 6.27 16.88
cis-1,2-Dichloroethene 0.1 0.2 11.10 14.8
Chloroform 0.05 0.1 Estimated 13
Cyclohexane 0.05 0.1 7.76 15.6
1,1,1-trichloroethane 0.05 0.1 9.40 14.1
Carbon Tetrachloride 0.05 0.1 10.41 14.1
Benzene 0.1 0.2 10.69 16
1,2-Dichloroethane 0.05 0.1 11.79 14.2
Heptane 0.05 0.1 9.38 13.9
Trichloroethene 0.05 0.1 11.47 14.9
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Revision 22.1, 09/2011 Page 6-16
Analytes
Reporting
Limit (µg/mL )
Reporting
Limit (µg/sampler)
Sampling Rates for Indoor Air
Applications ‘Zero Face velocity’
Sampling Rates for
Outdoor/worker exposure (ml/min)
4-Methyl-2-pentanone 0.1 0.2 Estimated 13.62
Toluene 0.05 0.1 8.90 14.5
1,1,2-Trichloroethane 0.05 0.1 Estimated 12.5
Tetrachloroethene 0.05 0.1 10.02 13.1
Chlorobenzene 0.05 0.1 Estimated 14.2*
Ethylbenzene 0.05 0.1 9.02 12.9
m,p-Xylene 0.05 0.1 8.1 12.65
o-Xylene 0.05 0.1 8.11 11.9
Styrene 0.05 0.1 9.04 13.7
1,1,2,2-Tetrachloroethane 0.05 0.1 Estimated 11.8
Propylbenzene 0.05 0.1 Estimated 11.69*
1,3,5-Trimethylbenzene 0.05 0.1 Estimated 12.1*
1,2,4-Trimethylbenzene 0.05 0.1 9.92 12.1*
1,3-Dichlorobenzene 0.05 0.1 Estimated 12.7*
1,4-Dichlorobenzene 0.05 0.1 10.74 12.7*
1,2-Dichlorobenzene 0.05 0.1 Estimated 12.6*
Naphthalene 0.05 0.1 Estimated 12.2*
Table 6.4.7 Summary of Calibration and QC Procedure Note: These criteria are used specifically for the standard list of analytes listed in Table 6.4.1.
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Tuning Criteria Prior to calibration and
at the start of every 12-hour clock.
Method 8260B tuning
criteria.

Correct problem then repeat
tune.
Initial 5-Point Calibration Prior to sample analysis. Compound criteria in
Table 6.4.1
Correct problem then repeat
initial calibration. Analysis may proceed if no more than 2
VOCs exceed criteria or 5% of VOCs if short list is used.
Narrate exceedences.
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-17
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Initial Calibration
Verification (ICV)
Once per initial
calibration.
See Table 6.4.1 Verify concentrations and
standard preparation. Analysis may proceed if no more than 2
VOCs exceed criteria or 5% of VOCs if short list is used.
Narrate exceedences.
Continuing Calibration Verification (CCV) At the start of every shift immediately after the
BFB tune check.
See "CCV criteria" column in Table 6.4.1

Investigate and correct the problem, up to and including
recalibration if necessary. Analysis may proceed if no
more than 2 VOCs exceed criteria or 5% of VOCs if
short list is used. Associated results are flagged.
Internal Standards (IS) IS is added at the time of
extraction to all samples and QC samples.
For CCVs: area counts
50% - 200%, RT w/in 30 sec of mid-point in
ICAL.
For blanks, samples and
non-CCV QC Checks: area counts 50 – 200%,
RT w/in 20 sec. of RT in CCV.
CCV: inspect and correct
system prior to sample analysis.
For blanks: inspect the system and re-analyze the
blank.
For samples: re-analyze; if
out again, flag data.
Surrogate Surrogate is added at the time of extraction to all
samples and QC samples.
See Table 6.4.3. Same as for Internal Standards.
Solvent Blanks Immediately after the
calibration standard or after samples with high
concentrations
Results less than
laboratory reporting limit (see Table 6.4.1).
Re-aliquot and re-analyze
solvent blank. If detections remain, flag concentrations in
associated samples.
Extracted Laboratory Blank Each set of up to 20 samples Results less than the reporting limit. Flag sample concentrations in associated extraction batch.
Extracted LCS Each set of up to 20
samples.
See Table 6.4.1 Re-aliquot and re-analyze the
extract. If within limits, report the re-analysis.
Otherwise, narrate.
Extracted LCSD Each set of up to 20 samples. %RPD < 25% Analysis may proceed if no more than 2 VOCs exceed
criteria (or 5% for short list exceed criteria). Run a 3rd
time, perform corrective action or narrate as
appropriate.

Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-18 6.5 PM10/TSP
This method involves equilibrating quartz filters in a conditioning environment of a specified temperature and humidity range and weighing the filters before and after field sampling. Samples are analyzed for
PM10 using 40 CFR Part 50 Appendix J or for Total Suspended Particulate (TSP) using 40 CFR Part 50 Appendix B. An analytical balance with 0.1 mg resolution is used to measure the filter weights. The
corresponding change in mass represents the TSP or PM10 result, expressed in µg or µg/m3. The reporting
limit is typically 1000 µg. Sampling volumes are required to calculate in units of µg/m3.
Table 6.5.1 Conditioning Environment Criteria
Method
Conditioning Environment Temperature
(˚F)
Conditioning Environment Relative Humidity
(%)
PM10 59°F – 86°F ± 5°F 20% – 45% ± 5%
TSP 59°F – 86°F ± 5°F ≤ 50% ± 5%
Table 6.5.2 Summary of Calibration and QC Procedures for Methods PM10 and TSP
QC Check
Minimum
Frequency
Acceptance
Criteria
Corrective
Action
Calibration Calibration checks of 3.00
g and 5.00 g are weighed to bracket the expected
filter weight of ~4.5 g prior to sample analysis
and at the end of the analytical batch.
Accuracy limits of 3.00 g weight:
2.997 g – 3.003 g
Accuracy limits of 5.00 g weight:
4.995 g - 5.005 g
Correct problem then
repeat calibration.
Laboratory
Duplicates
Unexposed Filters: one per
analytical batch.
Exposed Filters: one
duplicate per workorder.
Unexposed Filters: Weights of the
clean filters should be within ±0.0028 g of the original value.
Exposed Filters: ≤ 25% RPD and weights must be within ±0.005 g.
Re-condition the filter and
re-weigh.

Laboratory
Blanks
Immediately after the
calibration checks.
Post weight of Lab Blank is less
than pre weight and the difference is < 0.0028 g.
Confirm the weight
difference and narrate.

Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-19 6.6 TO-14A AND TO-3 - BTEX AND TPH
This method involves GC analysis of whole air samples collected in Summa canisters or Tedlar bags.
Samples are analyzed for Benzene, Toluene, Ethylbenzene, Xylenes, and Total Petroleum Hydrocarbons
(TPH) using EPA Method TO-14A or EPA Method TO-3 protocols. Samples are analyzed using a Photo Ionization Detector (PID) and a Flame Ionization Detector (FID). Depending on the client’s request, TPH
is analyzed and referenced to either gasoline or jet fuel.
Certain compounds are not included in ATL’s standard target analyte list. These compounds are communicated at the time of client proposal request. Unless otherwise directed, ATL reports these non-
standard compounds with partial validation. Validation includes a 3-point calibration with the lowest concentration defining the reporting limit, no second source verification is analyzed, and no method detection limit study is performed unless previous arrangements have been made. In addition, stability of
the non-standard compound during sample storage is not validated. Full validation may be available upon request.
Air Toxics Ltd. performs a modified version for each of these methods. The method modifications,
standard target analyte list, RL, QC criteria, and QC summary can be found in the following tables.
Table 6.6.1 Summary of Method Modifications
Requirement EPA Method TO-14A Air Toxics Ltd. Modifications
Sample Drying System* Nafion Dryer Multi-bed sorbent
Sample collection containers Specially treated stainless steel
canisters.
Method TO-14A is validated for samples
collected in specially treated canisters. As such, the use of Tedlar bags for sample
collection is outside the scope of the method and not recommended for ambient
or indoor air samples. Associated results are considered qualified.
Table 6.6.2 Summary of Method Modifications
Requirement EPA Method TO-3 Air Toxics Ltd. Modifications
Sample Collection In-line field method Collection of sample in specially treated canisters or alternative containers for
transport to and analysis by an off-site laboratory
Preparation of Standards Levels achieved through dilution of gas mixture. Levels achieved through loading various volumes of the gas mixture.
Initial Calibration
Calculation
4-point calibration using a
linear regression model.
5-point calibration using average Response
Factor.
Initial Calibration Frequency Weekly. When daily calibration standard recovery is
outside 75-125%, or upon significant changes to the procedure or
instrumentation.
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-20
Requirement EPA Method TO-3 Air Toxics Ltd. Modifications
Daily Calibration Standard Frequency Prior to sample analysis and every 4-6 hrs. Prior to sample analysis and after the
analytical batch ≤ 20 samples.
Minimum Detection Limit
(MDL)
Calculated using the equation
DL = A+3.3S, where A is intercept of calibration line and
S is the standard deviation of at least 3 reps of low level
standard.
40 CFR Pt. 136 App. B.
Sample preconcentration and
moisture management
Cyrogenic preconcentrator with
a Nafion dryer
Multi-bed Sorbent system
Table 6.6.3 Method TO-14A/TO-3 Standard Analyte List
Analyte
RL
(ppmv)
Acceptance Criteria
ICAL
(%RSD)
LCS & CCV
(%R)
Precision
(%RPD)
Benzene 0.001 ≤ 30 ± 25 ≤ 25
Toluene 0.001 ≤ 30 ± 25 ≤ 25
Ethyl Benzene 0.001 ≤ 30 ± 25 ≤ 25
Total Xylenes 0.001 ≤ 30 ± 25 ≤ 25
TPH* (Gasoline Range) 0.025 ≤ 30 ± 25 ≤ 25
TPH** (JP 4 Range) 0.025 ≤ 30 ± 25 ≤ 25
* TPH referenced to Gasoline (MW = 100) ** TPH referenced to JP 4 (MW = 156)
Table 6.6.4 Surrogate
Surrogate PID Accuracy (%R) FID Accuracy (%R)
Fluorobenzene 75-125% 75-150%
Table 6.6.5. Summary of Calibration and QC Procedures for Method TO-14A/TO-3
(BTEX & TPH)
QC Checks
Minimum
Frequency
Acceptance
Criteria Corrective Action
Five Point
Calibration (ICAL)
Prior to sample
Analysis
%RSD < 3.0 Repeat the calibration
Laboratory
Control Sample (LCS)
With each initial
calibration, and with each analytical batch.
±25% of the
expected value.
Check the system and re-analyze the standard.
Re-prepare the standard or re-calibrate the instrument if the criteria cannot be met.
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-21
QC Checks Minimum Frequency Acceptance Criteria Corrective Action
Continuing Calibration Verification
(CCV)
Daily prior to sample analysis. ±25% of the expected value. For initial CCV: Check the system and re-analyze the standard. Re-calibrate the instrument if the criteria cannot be met.
Mid/End Check At the end of the analytical batch, not to exceed 20
samples.
±25% of the expected value. Check system and re-analyze the standard. If the 2nd analysis fails, identify and correct the problem, then re-analyze all samples since the
last acceptable CCV.
Laboratory Blank In between analysis of standards and
project samples.
Results less than the laboratory Reporting Limit.
Repeat the Laboratory Blank. If the re-analysis of the Lab Blank contains compounds above but at less than 5 X the reporting limit, sample
analysis may proceed and the associated sample results will be reported with a B flag.
Surrogate Spikes As each standard, blank,
and sample is being loaded.
75-125% recovery on the PID, 75-
150% on the FID.
Low surrogate recovery results in re-analysis (at a higher dilution if high levels of moisture
are present). If recovery is out and still low, report the analysis with the better recovery and flag. Because of TPH interference, high surrogate recoveries do not result in re-
analysis. Data is flagged to note high recovery.
Laboratory Control Spike
(LCSD)
1 dup/analytical batch. RPD ≤ 25%. Inspect the system and re-analyze; if out again, narrate.

Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-22 6.7 TO-4A/TO-10A – PESTICIDES AND PCBS
This method involves GC analysis of Pesticides and Aroclor Polychlorinated Biphenyls (PCBs) in ambient air samples collected on polyurethane foam (PUF) cartridges.
Adsorbent PUF cartridges are cleaned using solvents and vacuum dried. Cartridges are sent to the field wrapped tightly in aluminum foil to prevent degradation by ultraviolet (UV) light. The PUF cartridges are batch certified for cleanliness prior to shipping. In addition, the laboratory analyzes one clean PUF
cartridge for each extraction set to serve as a Laboratory Blank.
A high volume sampler is used for TO-4A and a low volume sampler is used for method TO-10A.
The filters and cartridges are prepared for analysis by either Soxhlet or Pressurized Fluid Extraction
(PFE) by EPA Method 3545A. The extract is concentrated, exchanged into Hexane and concentrated again to final volume. Analysis is performed using a GC/ECD (Electron Capture Detector).
Certain compounds are not included in ATL’s standard target analyte list. These compounds are
communicated at the time of client proposal request. Unless otherwise directed, ATL reports these non-standard compounds with partial validation. Validation includes a 3-point calibration with the lowest
concentration defining the reporting limit, no second source verification is analyzed, and no method
detection limit study is performed unless previous arrangements have been made. For the extraction process, the non-standard compound recovery is evaluated in the extracted laboratory control spike. In
addition, stability of the non-standard compound during sample storage is not validated. Full validation
may be available upon request.
Air Toxics Ltd. performs a modified version of this method. The method modifications, standard target
analyte list, Limit of Quantitation, QC criteria, and QC summary can be found in the following tables.
Table 6.7.1 Summary of Method Modifications for TO-4A/TO-10A
Requirement EPA Method TO-4A/TO-10A Air Toxics Ltd. Modifications
Extraction Solvent 10 % (5 % TO-10A) Diethyl Ether in Hexane. DCM, exchanging to Hexane during the concentration step.
Reagent Blank Set up extraction system without filter/PUF; reflux with solvent. No Reagent Blank is extracted. Reagent lots are certified as
acceptable prior to use.
Media certification (TO-10A only) < 0.01 µg for single peak analytes, <
0.1 µg for PCBs.
< Reporting Limit for all analytes.
Frequency of Continuing
Calibration Verification
Every 10 samples. Every 20 samples with internal
standard.
PCB Quantitation Requires a minimum of 5 peaks. Use 4 peaks for quantitation.
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-23 Table 6.7.2 Methods TO-4A/TO-10A Pesticides and PCBs Reporting and QC Limits
Analyte RL (µg)
Acceptance Criteria
ICAL (%RSD) ICV (%R) CCV (%D) LCS (%R)
Precision (%RPD)
4,4’-DDD 0.10 < 20 ± 15 ± 15 ≤ 25%
4,4’-DDE 0.10 < 20 ± 15 ± 15 ≤ 25%
4,4’-DDT 0.10 < 20 ± 15 ± 15 65-125 ≤ 25%
4,4’-Methoxychlor 1.0 < 20 ± 15 ± 15 ≤ 25%
Aldrin 0.10 < 20 ± 15 ± 15 65-125 ≤ 25%
alpha-BHC 0.10 < 20 ± 15 ± 15 ≤ 25%
alpha-Chlordane 0.10 < 20 ± 15 ± 15 ≤ 25%
Aroclor 1016/1242 1.0 < 20 ± 15 ± 15 65-125 ≤ 25%
Aroclor 1221 1.0 < 20 ± 15 ± 15 ≤ 25%
Aroclor 1232 1.0 < 20 ± 15 ± 15 ≤ 25%
Aroclor 1248 1.0 < 20 ± 15 ± 15 ≤ 25%
Aroclor 1254 1.0 < 20 ± 15 ± 15 ≤ 25%
Aroclor 1260 1.0 < 20 ± 15 ± 15 65-125 ≤ 25%
beta-BHC 0.10 < 20 ± 15 ± 15 ≤ 25%
delta-BHC 0.10 < 20 ± 15 ± 15 ≤ 25%
Dieldrin 0.10 < 20 ± 15 ± 15 65-125 ≤ 25%
Endosulfan I 0.10 < 20 ± 15 ± 15 ≤ 25%
Endosulfan II 0.10 < 20 ± 15 ± 15 ≤ 25%
Endosulfan Sulfate 0.10 < 20 ± 15 ± 15 ≤ 25%
Endrin 0.10 < 20 ± 15 ± 15 65-125 ≤ 25%
Endrin Aldehyde 0.10 < 20 ± 15 ± 15 ≤ 25%
Endrin Ketone 0.10 < 20 ± 15 ± 15 ≤ 25%
gamma-BHC (Lindane) 0.10 < 20 ± 15 ± 15 65-125 ≤ 25%
gamma-Chlordane 0.10 < 20 ± 15 ± 15 ≤ 25%
Heptachlor 0.10 < 20 ± 15 ± 15 65-125 ≤ 25%
Heptachlor Epoxide 0.10 < 20 ± 15 ± 15 ≤ 25%
Technical Chlordane 1.0 < 20 ± 15 ± 15 ≤ 25%
Toxaphene 1.0 < 20 ± 15 ± 15 ≤ 25%
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-24
 The noted multi-component compounds use a one-point calibration.
 Recovery limits are derived from Compendium Method TO-10A January, 1999.
 Recovery limits are for extracted samples only. Non-extracted samples use limits of 85 – 115 %R.
 Not routinely reported, available at client request
Table 6.7.3 Surrogates
Surrogate %R
TCMX 60 – 120
DCB 60 – 120
Table 6.7.4 Summary of Calibration and QC Procedures for Methods TO-4A/TO-10A
QC Check
Minimum
Frequency
Acceptance
Criteria
Corrective
Action
Five Point
ICAL*
Prior to sample
analysis. %RSD ≤ 20 for each
compound or average %RSD ≤
20.
Use linear regression per SW-846 or re-
calibrate.
Independent
Calibration Verification
(ICV)
After each Initial
Calibration.
Recovery of an individual
component or the average of all the target components for a list
of 5 or more target components within 85 to 115 % recovery.
Not to exceed 75-125% for any individual compounds.
Investigate the source of discrepancy,
including re-preparation and re-analysis of standard. Re-calibrate if needed.
Breakdown
Check
Daily, CCV
Pesticides only. Degradation ≤ 15%. Perform maintenance. Repeat breakdown
check.
Continuing
Calibration Verification
(CCV)
Daily prior to
sample analysis, every 20 samples,
and at the end of the analysis
sequence.
Recovery of an individual
component or the average of all the Pesticide target components
for a list of 5 or more target components, within 15% of the
expected values. Not to exceed 75-125% for any individual
compounds.
Analyze new ICAL and/or prepare fresh
standards. If the standard analyzed is high and associated samples are ND, "Q"
flag the high recoveries. If the standard analyzed is low, re-analyze all samples.
Laboratory
Control Spike (LCS)
Extracted with
each set of up to 20 samples.
As mentioned in Table 6.7.2. Analyze another aliquot. If it still fails,
"Q" flag the compounds outside the control limits.
Surrogates All samples, QC, and blanks prior to
extraction.
As mentioned in Table 6.7.3 Analyze another aliquot, if it still fails, "Q" flag the compounds outside the
control limits.
Internal Standard With all analyses. CCV 50-200% compared to midpoint of ICAL; Samples
50-200% compared to first CCV of the daily analytical
batch.
Analyze another aliquot. If a CCV fails, correct problem before proceeding. If a
sample fails, analyze a second time. If it still fails, dilute the sample until IS meet
the criteria. Narrate the matrix
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-25
QC Check Minimum Frequency Acceptance Criteria Corrective Action
interference.
Laboratory Blanks With each set of up to 20 samples
extracted.
Results less than the Laboratory reporting limit. Analyze another aliquot. If it still fails, "B" flag the compounds that do not meet
the acceptance criteria.
Laboratory Control Spike (LCSD)
1 dup/analytical batch. RPD ≤ 25%. Inspect the system and re-analyze as appropriate; if out again, narrate.
Second-
Column Confirmation
100% for all
positive results, for both Pesticide
/PCB analyses.
Same as for initial or primary
column analysis.
Same as for initial or primary column
analysis.
* A single point calibration is performed for Technical Chlordane, Toxaphene, and certain Aroclors

Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-26 6.8 TO-5, TO-11A, METHOD 0011, CARB 430 – ALDEHYDES, AND KETONES
These methods involve High-Pressure Liquid Chromatography (HPLC) analysis of Aldehydes and Ketones in stationary and ambient air samples. The sampling media consist either of various-sized
impingers containing 2,4-Dinitrophenylhydrazine (DNPH) reagent, or a Sep-PAK (silica) cartridge coated in-situ with a solution of DNPH. Aldehydes and Ketones are readily converted to a stable Hydrazone
derivative. The impinger contents are extracted with a 70:30 Methylene Chloride/Hexane solution or
Methylene Chloride only, concentrated, solvent exchanged and analyzed on the HPLC. The Sep-PAK cartridges are eluted with Acetonitrile using gravity feed technique. Analysis is performed by reverse phase HPLC with UV detection at 360 nm.
Certain compounds are not included in ATL’s standard target analyte list. These compounds are communicated at the time of client proposal request. Unless otherwise directed, ATL reports these non-
standard compounds with partial validation. Validation includes a 3-point calibration with the lowest
concentration defining the reporting limit, no second source verification is analyzed, and no method detection limit study is performed unless previous arrangements have been made. For the extraction
process, the non-standard compound recovery is evaluated in the extracted laboratory control spike. In
addition, stability of the non-standard compound during sample storage is not validated. Full validation may be available upon request.
Air Toxics Ltd. performs a modified version of this method. The method modifications, standard target analyte list, Limit of Quantitation, QC criteria, and QC summary can be found in the following tables.
Table 6.8.1 Summary of TO-5/CARB 430 Method Modifications
Requirement TO-5/CARB 430 Air Toxics Ltd. Modifications
Initial Calibration (ICAL) TO-5: Linear regression, R ≥ 0.999. Average Response Factor (RF), composite % RSD ≤ 10. Linear
regression is performed when requested.
Sample Quantitation Use daily RF. Use ICAL RF.
Calibration Standard Precision % RSD ±10%. Recovery of all Continuing Cal.
standards must be 90% - 110%.
Retention Time (RT) Precision %RPD < 2% for daily
calibration standards.
RT windows determined by bracketing
standards.
Limit of Detection CARB 430: The “limit of detection” is defined as the
upper bound of the 95% confidence interval for the
analysis of at least 4 reagent blanks.
Detection Limit is based on the current MDL study which is calculated from a
minimum of 7 extracted spikes following 40 CFR Part 136 Appendix B.
Field Blank Subtraction CARB 430: Subtract the average of the field blanks
from the samples.
The samples and Field Blanks are not blank subtracted.
Laboratory Control Spike (LCS) CARB 430: If the LCS is out it must be re-extracted
until it is in or recalibrate.
The LCS is only extracted once with out of control recoveries flagged.
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-27
Requirement TO-5/CARB 430 Air Toxics Ltd. Modifications
UV Absorption Detector TO-5: Operate at 370 nm. Operate at 360 nm.
Mobile Phase TO-5: Methanol/Water. Acetonitrile/Water.
Table 6.8.2 Summary of Method TO-11A Modifications
Requirement TO-11A Air Toxics Ltd. Modifications
Initial Calibration Curve (ICAL) Multi-point using linear regression performed every 6
months.
Multi-point using average Response Factor; re-calibration if daily cal. fails,
major maintenance or column change. Linear regression is performed when
requested.
ICAL Criteria R2 for curve > 0.999 %RSD ≤ 10% unless Linear regression is requested.
Blank Subtraction Average blank
concentrations calculated. Blank value subtracted from
sample result.
One Lab Blank is analyzed per batch; no
blank subtraction performed on samples.
Table 6.8.3 Methods TO-5/CARB 430, TO-11A, and Method 0011 Standard Analyte List
Analyte
TO-5/
Method 0011/ CARB430 RL (µg)
TO-11A RL (µg)
Acceptance Criteria
ICAL (%RSD) ICV (%R) CCV (%R)
Formaldehyde 0.5 0.05 < 10 ± 15 ± 10
Acetaldehyde 0.5 0.10 < 10 ± 15 ± 10
Acrolein a 0.5 N/A < 10 ± 15 ± 10
Acetone* NA 0.25 < 10 ± 15 ± 10
Propanal 0.5 0.25 < 10 ± 15 ± 10
Crotonaldehyde* 0.5 0.25 < 10 ± 15 ± 10
n- Butyraldehydeb 0.5 0.25 < 10 ± 15 ± 10
Isopentanal* 0.5 0.25 < 10 ± 15 ± 10
Pentanal 0.5 0.25 < 10 ± 15 ± 10
m,p-Tolualdehyde* 0.5 0.25 < 10 ± 15 ± 10
o-Tolualdehyde* 0.5 0.25 < 10 ± 15 ± 10
Hexanal 0.5 0.25 < 10 ± 15 ± 10
Dimethylbenzaldehye** 0.5 0.25 < 10 ± 15 ± 10
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-28 a Because its derivative is not stable, when the target analyte list includes Acrolein, the sample will need to be extracted in field. A special order should be placed with the laboratory during the project set up stage.
b Methyl Ethyl Ketone, Iso-Butyraldehyde and the n-Butyraldehydes co-elute(report as n-Butyraldehyde) * Not included in the extracted LCS compound list for methods CARB 430/TO-5 and method 0011.
** Special request compound
Table 6.8.4 Summary of Calibration and QC Procedures for Methods TO-5/CARB 430, TO-11A, and Method 0011
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Five Point Initial
Calibration Curve (ICAL)
Analyzed in triplicate
prior to sample analysis %RSD ≤ 10. Repeat calibration.
Instrument LCS With each ICAL %R = 85-115%. Check the system and re-analyze the
standard. Re-calibrate the instrument if the criteria cannot be met.
Continuing Calibration Verification (CCV) Daily prior to sample analysis, after a
maximum of every 10 injections, and at the
end of the analytical batch.
Within ± 10% of the expected value. Check the system and re-analyze the standard. If the criteria cannot be met,
re-calibrate the instrument. If the standard is biased low, re-analyze all
samples since last acceptable CCV. If biased high and samples are “ND”, re-
analysis is not required. Q-flag high recoveries.
Instrument (Solvent)
Blank Analysis
Following analysis of
Standards.
Results less than the
laboratory RL.
Inspect the system and re-analyze the
blank.
Laboratory Control
Spike (LCSD)
1 dup/analytical batch. RPD ≤ 25%. Inspect the system and re-
analyze; if out again, narrate.

Inspect the system and re-analyze; if
out again, narrate.

Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-29 6.9 TO-12-NMOC
This method involves GC analysis of whole air samples collected in SummaTM canisters or Tedlar bags. Samples are analyzed for Non-Methane Organic Compounds (NMOC) using EPA Method TO-12
protocols. After concentration on a sorbent bed, samples are analyzed using a Flame Ionization Detector (FID). This method is used when speciation is not required.
Certain compounds are not included in ATL’s standard target analyte list. These compounds are
communicated at the time of client proposal request. Unless otherwise directed, ATL reports these non-standard compounds with partial validation. Validation includes a 3-point calibration with the lowest
concentration defining the reporting limit, no second source verification is analyzed, and no method
detection limit study is performed unless previous arrangements have been made. In addition, stability of the non-standard compound during sample storage is not validated. Full validation may be available upon
request.
Air Toxics Ltd. performs a modified version of this method. The method modifications, standard target analyte list, Reporting Limits, QC criteria, and QC summary can be found in the following tables:
Table 6.9.1 Summary of Method Modifications
Requirement EPA Method TO-12 Air Toxics Ltd. Modifications
Reporting Limit 0.02 ppmc. 0.010 ppmv.
Reported Units Ppmc. Ppmv, or if ref to CH4, multiply by 7. Units in ppmvc.
Initial Calibration Five levels – each level three runs with %RSD < 3%;
Linearity criterion not specified.
Minimum of three single levels;
%RSD ≤ 30%.
Sample Analysis Frequency Duplicate analysis with RPD
<5%, report average result.
Single analysis. Duplicate 10% of samples
with RPD ≤ 25% for detections > 5 X’s the RL.
Sample Hold Time None specified. Canister 30 days, Tedlar bags 3 days.
Column GC column not used. GC column used for analysis.
Table 6.9.2 Method TO – 12 Standard Analyte List
Analyte RL (ppmv) ICAL (%RSD) CCV %D LCS %R Duplicates %RPD
TNMOC ref. to Heptane 0.010 ≤ 30 ± 25 75-125 ≤ 25
Heptane MW = 100
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-30 Table 6.9.3 Summary of Calibration and QC Procedures for Method TO-12
QC Check
Minimum
Frequency
Acceptance
Criteria
Corrective
Action
Initial
Calibration Curve (ICAL)
Prior to sample analysis. % RSD ≤ 30. Repeat the calibration.
Laboratory
Control Sample (LCS)
With each initial
calibration and analytical batch.
75-125% of the
expected value.
Check the system and re-analyze the Standard.
Re-calibrate the instrument if the criteria cannot be met.
Continuing Calibration
Verification (CCV)
Daily prior to sample analysis and after every
20 samples or at the end of the analytical
sequence.
% Difference ± 25. Check the system and re-analyze the standard. Re-calibrate the instrument if the criteria cannot
be met. Re-analyze all samples since the last acceptable CCV.
Laboratory Blank In between analysis of standards and project
samples.
Results less than laboratory
reporting limit.
Repeat the Laboratory Blank. If the re-analysis of the Lab Blank contains compounds above but
at less than 5 X the reporting limit, sample analysis may proceed and the associated sample
results will be reported with a B flag.
Laboratory
Control Spike (LCSD)
1 dup/analytical batch.. ≤ 25%RPD. Inspect the system and re-analyze; if out again,
narrate.
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-31
6.10 TO-13A AND 8270C –SEMIVOLATILE COMPOUNDS
This method involves GC/MS full scan or SIM mode analysis of semi-volatile organic compounds in ambient air samples collected on PUF/XAD2 cartridges. In relation to the prescribed media, sampling and
collection efficiency for compounds not listed in TO-13A has not been evaluated. Samples are analyzed for Polynuclear Aromatic Hydrocarbons (PAHs) using a quadrupole GC/MS in full scan or SIM mode by
TO-13A protocol. In addition, the target compound list is often extended to include analysis of Method
8270 semi-volatile compounds. Air Toxics Ltd. performs a modified version of this method. The method modifications, standard target analyte list, Limit of Quantitation, QC criteria, and QC summary can be found in the following tables.
Certain compounds are not included in ATL’s standard target analyte list. These compounds are communicated at the time of client proposal request. Unless otherwise directed, ATL reports these non-
standard compounds with partial validation. Validation includes a 3-point calibration with the lowest
concentration defining the reporting limit, no second source verification is analyzed, and no method detection limit study is performed unless previous arrangements have been made. In addition, stability of
the non-standard compound during sample storage is not validated. Full validation may be available upon
request.
Air Toxics Ltd. also performs semi-volatile analysis by SW-846 Method 8270C. The extraction process
of MM5 trains follows SW846 Method 3542, and the QC criteria differ from Method TO-13A analysis. The QC criteria and QC summary tables for Method 8270C analysis are in the section following the TO-13A tables.
Table 6.10.1 Summary of Method Modifications for TO-13A
Requirements EPA Method TO-13A Air Toxics Ltd. Modifications
Extraction Solvent 10% ether in hexane for PUF; DCM for XAD sorbent. Final
extract in hexane.
DCM for PUF/XAD cartridge and XAD sorbent. Final extract in DCM.
Glassware Cleaning Muffle furnace is utilized. Solvent cleaning procedure is used.
Extraction Technique Soxhlet extraction. Soxhlet extraction or pressurized fluid extraction (PFE).
Reporting List 19 PAHs. See Tables 6.10.2 & 6.10.3.
Calibration range: 0.1-2.5 µg/mL in Hexane 1.0-160 µg/mL in Methylene chloride for quad or 0.1-40 µg/mL for SIM.
Surrogate Field surrogates: Fluoranthene-
d10 and Benzo(a)pyrene-d12.
Field surrogates: provided upon request.

Solvent Process Blank One each analytical batch. Not performed: each solvent lot is certified.
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-32
Requirements EPA Method TO-13A Air Toxics Ltd. Modifications
Method Blank < MDL. <Reporting Limit.
Table 6.10.2 Modified Method TO-13A
Analyte
SIM RL (µg) RL (µg)
Minimum ICAL RRF ICAL (%RSD) ICV (%R) CCV (%R) Precision (%RPD)
2-Chloronaphthalene* 0.1 1.0 NA < 30 ± 30 ± 30 < 25%
2-Methylnaphthalene* 0.1 1.0 NA < 30 ± 30 ± 30 < 25%
Acenaphthylene 0.1 1.0 1.3 < 30 ± 30 ± 30 < 25%
Acenaphthene 0.1 1.0 0.8 < 30 ± 30 ± 30 < 25%
Anthracene 0.1 1.0 0.7 < 30 ± 30 ± 30 < 25%
Benzo(a)anthracene 0.1 1.0 0.8 < 30 ± 30 ± 30 < 25%
Benzo(e)pyrene* 0.1 1.0 NA < 30 ± 30 ± 30 < 25%
Benzo(a)pyrene 0.1 1.0 0.7 < 30 ± 30 ± 30 < 25%
Benzo(b)fluoranthene 0.1 1.0 0.7 < 30 ± 30 ± 30 < 25%
Benzo(g,h,i)perylene 0.1 1.0 0.5 < 30 ± 30 ± 30 < 25%
Benzo(k)fluoranthene 0.1 1.0 0.7 < 30 ± 30 ± 30 < 25%
Chrysene 0.1 1.0 0.7 < 30 ± 30 ± 30 < 25%
Dibenz(a,h)anthracene 0.1 1.0 0.4 < 30 ± 30 ± 30 < 25%
Fluoranthene 0.1 1.0 0.6 < 30 ± 30 ± 30 < 25%
Fluorene 0.1 1.0 0.9 < 30 ± 30 ± 30 < 25%
Indeno(1,2,3-c,d)pyrene 0.1 1.0 0.5 < 30 ± 30 ± 30 < 25%
Naphthalene 0.1 1.0 0.7 < 30 ± 30 ± 30 < 25%
Phenanthrene 0.1 1.0 0.7 < 30 ± 30 ± 30 < 25%
Pyrene 0.1 1.0 0.6 < 30 ± 30 ± 30 < 25%
* Not included in the TO-13A method.
The following two compounds can be analyzed upon client’s request.
Analyte
SIM RL (µg) RL (µg)
Minimum ICAL RRF ICAL (%RSD) ICV (%R) CCV (%R) Precision (%RPD)
Perylene NA 1.0 0.5 < 30 ± 30 ± 30 < 25%
Coronene NA 1.0 0.7 < 30 ± 30 ± 30 < 25%
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-33 Table 6.10.3 Modified Method TO-13A-Extended
Analyte
Minimum
ICAL RRF RL (µg) ICAL (1) (%RSD) ICV (%R) Precision %RPD
1,2,4-Trichlorobenzene NA 1.0 < 30 ± 30 < 25%
1,2-Dichlorobenzene NA 1.0 < 30 ± 30 < 25%
1,3-Dichlorobenzene NA 1.0 < 30 ± 30 < 25%
1,4-Dichlorobenzene - CCC NA 1.0 < 30 ± 30 < 25%
2,4,5-Trichlorophenol NA 5.0 < 30 ± 30 < 25%
2,4,6-Trichlorophenol - CCC NA 5.0 < 30 ± 30 < 25%
2,4-Dichlorophenol - CCC NA 5.0 < 30 ± 30 < 25%
2,4-Dimethylphenol NA 5.0 < 30 ± 30 < 25%
2,4-Dinitrophenol - SPCC 0.05 20 < 30 ± 30 < 25%
2,4-Dinitrotoluene NA 5.0 < 30 ± 30 < 25%
2,6-Dinitrotoluene NA 5.0 < 30 ± 30 < 25%
2-Chloronapthalene NA 1.0 < 30 ± 30 < 25%
2-Chlorophenol NA 5.0 < 30 ± 30 < 25%
2-Methylnapthalene NA 1.0 < 30 ± 30 < 25%
2-Methylphenol NA 5.0 < 30 ± 30 < 25%
2-Nitroaniline NA 10 < 30 ± 30 < 25%
2-Nitrophenol – CCC NA 5.0 < 30 ± 30 < 25%
3,3-Dichlorobenzidine NA 20 < 30 ± 30 < 25%
3-Nitroaniline NA 10 < 30 ± 30 < 25%
4,6-Dinitro-2-methylphenol NA 10 < 30 ± 30 < 25%
4-Bromophenyl-phenyl ether NA 1.0 < 30 ± 30 < 25%
4-Chloro-3-methylphenol - CCC NA 5.0 < 30 ± 30 < 25%
4-Chloroaniline NA 10 < 30 ± 30 < 25%
4-Chlorophenyl-phenyl ether NA 1.0 < 30 ± 30 < 25%
4-Methylphenol NA 5.0 < 30 ± 30 < 25%
4-Nitroaniline NA 10 < 30 ± 30 < 25%
4-Nitrophenol – SPCC 0.05 20 < 30 ± 30 < 25%
Acenaphthylene 1.3 1.0 < 30 ± 30 < 25%
Acenaphthene – CCC 0.8 1.0 < 30 ± 30 < 25%
Anthracene 0.7 1.0 < 30 ± 30 < 25%
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Revision 22.1, 09/2011 Page 6-34
Analyte
Minimum ICAL
RRF
RL
(µg)
ICAL (1)
(%RSD)
ICV
(%R)
Precision
%RPD
Benzo(a)anthracene NA 1.0 < 30 ± 30 < 25%
Benzo(a)pyrene - CCC 0.7 1.0 < 30 ± 30 < 25%
Benzo(e)pyrene 0.5 1.0 < 30 ± 30 < 25%
Benzo(b)fluoranthene 0.7 1.0 < 30 ± 30 < 25%
Benzo(g,h,i)perylene NA 1.0 < 30 ± 30 < 25%
Benzo(k)fluoranthene NA 1.0 < 30 ± 30 < 25%
Benzoic Acid NA 30 < 30 ± 30 < 25%
Bis(2-Chloroethoxy) Methane NA 1.0 < 30 ± 30 < 25%
Bis(2-Chloroispropyl) Ether NA 1.0 < 30 ± 30 < 25%
Bis(2-Chlroethyl) Ether NA 1.0 < 30 ± 30 < 25%
Bis(2-Ethylhexyl)phthalate NA 5.0 < 30 ± 30 < 25%
Butylbenzylphthalate NA 5.0 < 30 ± 30 < 25%
Chrysene 0.7 1.0 < 30 ± 30 < 25%
di-n-Butylphthalate NA 5.0 < 30 ± 30 < 25%
di-n-Octylphthalate - CCC NA 5.0 < 30 ± 30 < 25%
Dibenz(a,h)anthracene 0.4 1.0 < 30 ± 30 < 25%
Dibenzofuran NA 1.0 < 30 ± 30 < 25%
Diethylphthalate NA 5.0 < 30 ± 30 < 25%
Dimethylphthalate NA 5.0 < 30 ± 30 < 25%
Fluoranthene – CCC 0.6 1.0 < 30 ± 30 < 25%
Fluorene 0.9 1.0 < 30 ± 30 < 25%
Hexachlorobenzene NA 1.0 < 30 ± 30 < 25%
Hexachlorobutadiene - CCC NA 1.0 < 30 ± 30 < 25%
Hexachlorocylcopentadiene- SPCC 0.05 20 < 30 ± 30 < 25%
Hexachloroethane NA 1.0 < 30 ± 30 < 25%
Indeno(1,2,3-c,d)pyrene 0.5 1.0 < 30 ± 30 < 25%
Isophorone NA 1.0 < 30 ± 30 < 25%
n-Nitroso-di-n-propylamine– SPCC 0.05 1.0 < 30 ± 30 < 25%
n-Nitrosodiphenylamine – CCC NA 10 < 30 ± 30 < 25%
Naphthalene 0.7 1.0 < 30 ± 30 < 25%
Nitrobenzene NA 1.0 < 30 ± 30 < 25%
Pentachlorophenol – CCC NA 20 < 30 ± 30 < 25%
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Revision 22.1, 09/2011 Page 6-35
Analyte
Minimum ICAL
RRF
RL
(µg)
ICAL (1)
(%RSD)
ICV
(%R)
Precision
%RPD
Phenanthrene 0.7 1.0 < 30 ± 30 < 25%
Phenol – CCC NA 5.0 < 30 ± 30 < 25%
Pyrene 0.6 1.0 < 30 ± 30 < 25%
(1) With 10% exception not to exceed 40%
Table 6.10.4 Surrogates (Full Scan) Table 6.10.5 Internal Standards Analyte (%R) Analyte (%)
2,4,6-Tribromophenol 50 – 150 Acenaphthene-d10 50 – 200
2-Fluorophenol 50 – 150 Chrysene-d12 50 – 200
Nitrobenzene-d5 50 – 150 1,4-Dichlorobenzene-d4 50 – 200
Phenol-d5 50 – 150 Naphthalene-d8 50 – 200
Fluorene-d10 60 – 120 Perylene-d12 50 – 200
Pyrene-d10 60 – 120 Phenanthrene-d10 50 – 200
Table 6.10.6. TO-13A-Surrogates (Standard and SIM)
Analyte Accuracy (% R)*
Fluorene-d10 60 - 120
Pyrene-d10 60 - 120
Table 6.10.7 Extracted Laboratory Control Spikes for Modified TO-13A-Extended
Analyte (%R)
1,2,4-Trichlorobenzene*** 50 – 150
1,4-Dichlorobenzene*** 50 – 150
2,4-Dinitrotoluene*** 50 – 150
2-Chlorophenol*** 50 – 150
4-Chloro-3-methylphenol*** 50 – 150
4-Nitrophenol*** 38 – 96
Acenaphthene* 60 – 120
N-Nitroso-di-n-propylamine*** 50 – 150
Pentachlorophenol** 39 – 106
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Revision 22.1, 09/2011 Page 6-36
Analyte (%R)
Phenol*** 50 – 150
Pyrene* 60 – 120
* The LCS and Surrogate limits are derived from Compendium Method TO-13A Sections 13.3.7.4 and 13.4.6.3 January, 1999. These limits only apply to samples that are extracted by Air Toxics Ltd.
When sample extracts are sent to Air Toxics Ltd., limits of 50 – 150 % are applied. ** Pentachlorophenol is not included in Compendium Method TO-13A and has been shown to be erratically recovered from XAD media therefore historical Control Limits are used. Limits are
updated periodically as needed. *** Compounds outside of the TO-13A method
Table 6.10.8 Extracted Laboratory Control Samples for TO-13A (PAHs) in Full Scan and SIM
Analyte (%R)
Napthalene 60 – 120
Acenapthylene 60 – 120
Acenaphtene 60 – 120
Flourene 60 – 120
Phenanthrene 60 – 120
Anthracene 60 – 120
Fluoranthene 60 – 120
Pyrene 60 – 120
Benzo (a) anthracene 60 – 120
Chrysene 60 – 120
Benzo (b) flouranthene 60 – 120
Benzo (k) flouranthene 60 – 120
Benzo (a) pyrene 60 – 120
Indeno (1,2,3-cd) pyrene 60 – 120
Dibenzo (a,h) anthracene 60 – 120
Benoz (g,,h,i) perylene 60 – 120
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-37 Table 6.10.9 Summary of Calibration and QC Procedures for EPA Method TO-13A
QC Check
Minimum
Frequency
Acceptance
Criteria
Corrective
Action
Tuning Criteria Prior to calibration and at start of every 12 hrs. SW-846 tuning criteria for semivolatiles
analysis. DDT% Breakdown< 20%.
Correct problem then repeat tune.
Initial 5-Point Calibration Prior to sample analysis. ICAL criteria in tables 6.10.2 and 6.10.3. Correct problem then repeat initial calibration.
ICAL LCS All analytes – Once per
initial calibration.
All target compound
recoveries must be between 70 – 130%.
Determine the source of discrepancy
between standards. Re-calibrate if needed.
Continuing Calibration
Verification (CCV)
At the start of every clock immediately after the
DFTPP tune check.
PAHs list: meet min. RRF requirement PAHs
list/ short list %D ≤ 30%
Semivol full list: SPCCs:
RF ≥ 0.050, %D ≤ 30%
with 10% exception not to exceed 40%. Flag all
results outside of compliance with the
exception of high bias associated with non-
detects.
Investigate and correct the problem, up to and including re-calibration if
necessary. High bias associated with non-detects in samples will not result
in re-analysis.
Internal Standards (IS) As each standard, blank, and sample is being
aliquoted.
For CCV: Area count within 50 to 200% of the
mid point of ICAL.
For blanks, samples and
non-CCV QC Checks: retention times within ±
0.33 minutes (20 seconds) and area counts
within 50 to 200% of the CCV.
For CCVs: Investigate and correct the problem before proceeding with
sample analysis. If interferences are present, a secondary ion may be
selected.
For blanks: inspect the system and re-
analyze the blank.
For samples and non-CCV QC: unless
there is obvious matrix effect, re-analyze the samples and dilute the
sample until the IS meet the criteria, narrate the data to indicate
interference.
Surrogates With all samples and
blanks prior to extraction.
See Table 6.10.4. A new aliquot of the extract is
analyzed. If Surrogate recoveries are out-of-control a second time, data is
flagged and narrated. Re-analysis is not necessary for obvious matrix
effects (data is flagged for out-of-control surrogate recoveries). Air
samples cannot be re-extracted.
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Revision 22.1, 09/2011 Page 6-38
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Extracted LCS With each set of up to 20
extracted samples.
See LCS Criteria in
tables 6.10.7 and 6.10.8.
Re-aliquot and re-analyze the extract.
If within limits, report the re-analysis. Otherwise, narrate.
Laboratory Blank With each set of up to 20 extracted samples. Results less than laboratory reporting limit.
Flag the data.
Solvent Blanks When samples that are extracted together are
analyzed on different analytical shifts.
All target compounds below the reporting limit. Flag the data.
Laboratory Control Spike
Duplicate (LCSD)
1 dup/analytical batch. RPD ≤ 25%. Inspect the system and re-analyze; if out again, narrate.

Table 6.10.10 Summary of Method Modifications for EPA Methods 3510/3542 and 8270C
Requirements EPA Method 8270C Air Toxics Ltd. Modifications
Linearity of ICAL Use mean RF for non-CCC
compounds if %RSD≤ 15%. If
%RSD>15%, use a) linear regression equation that does not
pass through the origin. R >/= 0.99, or b) non-linear (i.e., 6
points for a quadratic model).
Use mean RF for non-CCC compounds when
%RSD≤ 15%, RF for CCC≤30%.
RT for CCV Within +/- 30 seconds of the mid-point standard from the initial
curve.
Frequent column maintenance results in RT shift; therefore this requirement is not
practical.
Table 6.10.11 SW-846 Modified Method 8270C Standard Analyte List
Analyte RL (µg)
Acceptance Criteria
ICAL (%RSD) ICV (%R) CCV Precision\%RPF
1,2,4-Trichlorobenzene 1.0 < 15 + 30 %D < 20% < 25%
1,2-Dichlorobenzene 1.0 < 15 + 30 %D < 20% < 25%
1,3-Dichlorobenzene 1.0 < 15 + 30 %D < 20% < 25%
1,4-Dichlorobenzene - CCC 1.0 < 30 + 30 %D < 20% < 25%
2,4,5-Trichlorophenol 5.0 < 15 + 30 %D < 20% < 25%
2,4,6-Trichlorophenol - CCC 5.0 < 30 + 30 %D < 20% < 25%
2,4-Dichlorophenol - CCC 5.0 < 30 + 30 %D < 20% < 25%
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Revision 22.1, 09/2011 Page 6-39
Analyte
RL
(µg)
Acceptance Criteria
ICAL
(%RSD)
ICV
(%R) CCV
Precision\%RP
F
2,4-Dimethylphenol 5.0 < 15 + 30 %D < 20% < 25%
2,4-Dinitrophenol - SPCC 20 < 30 + 30 RF > 0.050 < 25%
2,4-Dinitrotoluene 5.0 < 15 + 30 %D < 20% < 25%
2,6-Dinitrotoluene 5.0 < 15 + 30 %D < 20% < 25%
2-Chloronaphthalene 1.0 < 15 + 30 %D < 20% < 25%
2-Chlorophenol 5.0 < 15 + 30 %D < 20% < 25%
2-Methylnaphthalene 1.0 < 15 + 30 %D < 20% < 25%
2-Methylphenol 5.0 < 15 + 30 %D < 20% < 25%
2-Nitroaniline 10 < 15 + 30 %D < 20% < 25%
2-Nitrophenol – CCC 5.0 < 30 + 30 %D < 20% < 25%
3,3-Dichlorobenzidine 20 < 15 + 30 %D < 20% < 25%
3-Nitroaniline 10 < 15 + 30 %D < 20% < 25%
4,6-Dinitro-2-methylphenol 10 < 15 + 30 %D < 20% < 25%
4-Bromophenyl-phenyl ether 1.0 < 15 + 30 %D < 20% < 25%
4-Chloro-3-methylphenol - CCC 5.0 < 30 + 30 %D < 20% < 25%
4-Chloroaniline 10 < 15 + 30 %D < 20% < 25%
4-Chlorophenyl-phenyl ether 1.0 < 15 + 30 %D < 20% < 25%
4-Methylphenol 5.0 < 15 + 30 %D < 20% < 25%
4-Nitroaniline 10 < 15 + 30 %D < 20% < 25%
4-Nitrophenol – SPCC 20 < 30 + 30 RF > 0.050 < 25%
Acenaphthylene 1.0 < 15 + 30 %D < 20% < 25%
Acenaphthene – CCC 1.0 < 30 + 30 %D < 20% < 25%
Anthracene 1.0 < 15 + 30 %D < 20% < 25%
Benzo(a)anthracene 1.0 < 15 + 30 %D < 20% < 25%
Benzo(a)pyrene - CCC 1.0 < 30 + 30 %D < 20% < 25%
Benzo(b)fluoranthene 1.0 < 15 + 30 %D < 20% < 25%
Benzo(g,h,i)perylene 1.0 < 15 + 30 %D < 20% < 25%
Benzo(k)fluoranthene 1.0 < 15 + 30 %D < 20% < 25%
Benzoic Acid 30 < 15 + 30 %D < 20% < 25%
Bis(2-Chloroethoxy) Methane 1.0 < 15 + 30 %D < 20% < 25%
Bis(2-Chloroispropyl) Ether 1.0 < 15 + 30 %D < 20% < 25%
Bis(2-Chlroethyl) Ether 1.0 < 15 + 30 %D < 20% < 25%
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Revision 22.1, 09/2011 Page 6-40
Analyte
RL
(µg)
Acceptance Criteria
ICAL
(%RSD)
ICV
(%R) CCV
Precision\%RP
F
Bis(2-Ethylhexyl)phthalate 5.0 < 15 + 30 %D < 20% < 25%
Butylbenzylphthalate 5.0 < 15 + 30 %D < 20% < 25%
Chrysene 1.0 < 15 + 30 %D < 20% < 25%
di-n-Butylphthalate 20 < 15 + 30 %D < 20% < 25%
di-n-Octylphthalate - CCC 5.0 < 30 + 30 %D < 20% < 25%
Dibenz(a,h)anthracene 1.0 < 15 + 30 %D < 20% < 25%
Dibenzofuran 1.0 < 15 + 30 %D < 20% < 25%
Diethylphthalate 5.0 < 15 + 30 %D < 20% < 25%
Dimethylphthalate 5.0 < 15 + 30 %D < 20% < 25%
Fluoranthene – CCC 1.0 < 30 + 30 %D < 20% < 25%
Fluorene 1.0 < 15 + 30 %D < 20% < 25%
Hexachlorobenzene 1.0 < 15 + 30 %D < 20% < 25%
Hexachlorobutadiene – CCC 1.0 < 30 + 30 %D < 20% < 25%
Hexachlorocylcopentadiene – SPCC 20 < 30 + 30 RF > 0.050 < 25%
Hexachloroethane 1.0 < 15 + 30 %D < 20% < 25%
Indeno(1,2,3-c,d)pyrene 1.0 < 15 + 30 %D < 20% < 25%
Isophorone 1.0 < 15 + 30 %D < 20% < 25%
n-Nitroso-di-n-propylamine – SPCC 1.0 < 30 + 30 RF > 0.050 < 25%
n-Nitrosodiphenylamine – CCC 10 < 30 + 30 %D < 20% < 25%
Naphthalene 1.0 < 15 + 30 %D < 20% < 25%
Nitrobenzene 1.0 < 15 + 30 %D < 20% < 25%
Pentachlorophenol – CCC 20 < 30 + 30 %D < 20% < 25%
Phenanthrene 1.0 < 15 + 30 %D < 20% < 25%
Phenol – CCC 5.0 < 30 + 30 %D < 20% < 25%
Pyrene 1.0 < 15 + 30 %D < 20% < 25%
 Can use the mean RSD criterion of < 15% as noted in par. 7.5.1.2.1 of SW-846, 8000B.
 No more than 10% of the target compounds are allowed to exceed the limit.
 If %D for all CCC is less than or equal to 20%, then the CCV is assumed to be valid. If the CCCs are
not included in the list of analytes for a project, then all analytes must meet the 20% D.
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Revision 22.1, 09/2011 Page 6-41
Table 6.10.12 Surrogates Table 6.10.13 Internal Standards
Analyte
Accuracy
(% R) Analyte
Accuracy
(% R)
2,4,6-Tribromophenol 10 – 123 Acenaphthene-d10 -50 to +100
2-Fluorobiphenyl 43 – 116 Chrysene-d12 -50 to +100
2-Fluorophenol 21 – 110 1,4-Dichlorobenzene-d4 -50 to +100
Nitrobenzene-d5 35 – 114 Naphthalene-d8 -50 to +100
Phenol-d5 10 – 110 Perylene-d12 -50 to +100
p-Terphenyl-d14 33 – 141 Phenanthrene-d10 -50 to +100
 The Surrogate limits are derived from USEPA CLP OLM 03.0 and OLM04.2. Air Toxics Ltd. receives a numerically insufficient number of liquid samples for SW 8270C analysis to allow semi-annual updating of in-house Control Limits.
Table 6.10.14 Extracted Laboratory Control Spikes Table 6.10.15 Pre-Spike Surrogates
Analyte
Accuracy
(% R)

Analyte
Accuracy
(%R)
1,2,4-Trichlorobenzene 39 – 98 Benzo(a)Pyrene-d12 50 – 150
1,4-Dichlorobenzene 36 – 97 Fluoranthene- d10 50 – 150
2,4-Dinitrotoluene 24 – 96
2-Chlorophenol 27 – 123
4-Chloro-3-methylphenol 23 – 97
4-Nitrophenol 10 – 80
Acenaphthene 46 – 118
N-Nitroso-di-n-propylamine 41 – 116
Pentachlorophenol 9 – 103
Phenol 12 – 110
Pyrene 26 – 127
 The LCS limits are derived from USEPA CLP OLM03.0 and OLM04.2. Air Toxics Ltd. receives a
numerically insufficient number of samples for SW 8270C analysis to allow semi-annual updating of in-house Control Limits. These limits only apply to samples that are extracted by Air Toxics Ltd. When sample extracts are sent to Air Toxics Ltd., limits of 50 - 150% are applied.
 The pre-spike Surrogates limits are arbitrary. Air Toxics Ltd. received a numerically insufficient number of samples for SW 8270C analysis to allow semi-annual updating of in-house control limits.
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-42 Table 6.10.16 Summary of Calibration and QC Procedures SW-846 Modified Method 8270C
QC Check
Minimum
Frequency
Acceptance
Criteria
Corrective
Action
Tuning Criteria Prior to calibration and at start of
every 12 hrs.
SW-846 tuning criteria for Semi-
volatiles analysis.
Correct problem then repeat tune.
Initial 5-Point
Calibration
Prior to sample
analysis.
ICAL criteria in Table
6.10.11.
Correct problem then repeat Initial
Calibration.
Independent Calibration
Verification (ICV)
All analytes – once per Initial
Calibration.
At least 90% of the target compounds
recoveries must be between 70 – 130%.
Determine the source of discrepancy between standards. Re-calibrate if needed.
Continuing Calibration
Verification (CCV)
At the start of every clock,
immediately after the DFTPP tune
check.
SPCCs: RF>0.050
CCCs: %D <20%;
Non-CCC’s when CCC compounds are
not requested %D <20%.
Investigate and correct the problem, up to and including re-calibration if necessary. High
bias for one or more compounds associated with non-detects in the samples will not result
in re-analysis.

Internal Standards
(IS)
As each standard,
blank, and sample is being aliquoted.

For CCVs: area
counts within -50% to +100% from the most
recent ICAL.
For blanks, samples and non-CCV QC Checks: Retention
Times within ± 0.33 minutes (20 seconds)
and area counts within -50% to +100% of the
CCV.
For CCVs: Investigate and correct the
problem before proceeding with sample analysis.
For blanks: Inspect the system and re-analyze the blank.
For samples and non-CCV QC: Re-analyze the samples. If the criteria are not met a
second time, dilute sample until IS meet criteria.
Surrogates

With all samples
and blanks prior to extraction.
See Table 6.10.12. Re-aliquot and re-analyze the extract. If
within limits, report the re-analysis. Otherwise narrate.
Extracted LCS With each set of up to 20 extracted
samples.
See LCS Criteria in Table 6.10.14. Re-aliquot and re-analyze the extract. If within limits, report the re-analysis.
Otherwise narrate.
Laboratory Blank With each set of up
to 20 extracted samples.
Results less than
laboratory RL.
Re-aliquot and re-analyze the extract to
confirm the presence of the target compound. If it doesn’t confirm, investigate and correct
the problem before re-analyzing all the affected samples.
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Revision 22.1, 09/2011 Page 6-43
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Solvent Blanks When samples that
are extracted together are
analyzed on different analytical
shifts.
All target compounds
below the RL.
Investigate and correct the problem before re-
analyzing all the affected samples.
Laboratory Control
Spike Duplicate (LCSD)
1 dup/analytical
batch. RPD ≤ 25%. Inspect the system and re-analyze; if out
again, narrate.

Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-44 6.11 TO-14A/TO-15 – VOLATILE ORGANIC COMPOUNDS
This method involves full scan GC/MS analysis of whole air samples collected in evacuated stainless steel canisters. Samples are analyzed for volatile organic compounds using EPA Method TO-14A/TO-15
protocols. An aliquot of the sample is withdrawn from the canister through a mass flow controller and concentrated using a hydrophobic multisorbent bed. The hydrophobic multisorbent bed functions as a
drying system which removes water from the sample stream prior to analysis by full scan GC/MS. During
analysis, the sample may be focused onto a cryogenic cooled column and/or a cryogenic cooled sleeve for analysis by full scan GC/MS.
Air Toxics maintains three TO-14A/TO-15 full scan configurations and one SIM configuration. (See
section 6.12 for the TO-14A/TO-15 SIM configuration). The ‘5&20’ configuration is designed for high moisture soil gas and ppmv range vapor matrices. The ‘5&20’ refers to the base reporting limits
achievable via this method (5 ppbv and 20 ppbv). Samples can be efficiently analyzed without dilution at
concentrations up to 5 ppmv. The second configuration is referred to as TO-15 (or Quad) and is set up to meet the reporting limits described in EPA Method TO-15 ( 0.5 ppbv to 2 ppbv). This application is used
primarily for ppbv-level soil gas and ambient air. The third configuration is referred to as ‘Low-level’
and is optimized reporting limits below those listed in Method TO-15 with reporting limits in the 0.1 ppbv to 0.5 ppbv range. This ‘Low-level’ application is often used for indoor air applications. The ‘Low-
level’ application is not designed for soil gas applications due to high levels of moisture and potentially high VOC concentrations.
Certain compounds are not included in ATL’s standard target analyte list. These compounds are
communicated at the time of client proposal request. Unless otherwise directed, ATL reports these non-standard compounds with partial validation. Validation includes a 3-point calibration with the lowest concentration defining the reporting limit, no second source verification is analyzed, and no method
detection limit study is performed unless previous arrangements have been made. In addition, stability of the non-standard compound during sample storage is not validated. Full validation may be available upon
request.
Air Toxics Ltd. takes no modifications of technical significance to Method TO-15 for the ‘Quad’ and 5&20 configurations. The modifications for TO-15 Low-level are listed in Table 6.11.1.A. Since Air
Toxics applies TO-15 methodology to all Summa canisters regardless of whether TO-14A or TO-15 is
specified by the project, Air Toxics performs a modified version of method TO-14A as detailed in Table
6.11.1.B. Please note that Methods TO-14A and TO-15 were validated for specially treated canisters.
As such, the use of Tedlar bags for sample collection is outside the scope of the method and not
recommended for ambient or indoor air samples. It is the responsibility of the data user to
determine the usability of TO-14A (and TO-15) results generated from Tedlar bags.
Table 6.11.1.A Summary of TO-15 ‘Low Level’ Method Modifications
Requirement TO-15 ‘ Low Level’ ATL Modifications
Initial Calibration ≤ 30% RSD with 2 compounds
allowed out to ≤ 40% RSD.
≤ 30% RSD with 4 compounds allowed out to
≤ 40%.
Blanks and standards Zero Air Nitrogen

Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-45 Table 6.11.1.B Summary of TO-14A Method Modifications
Requirement TO-14A ATL Modifications
Sample Drying System Nafion Drier Multibed hydrophobic sorbent
Blank acceptance criteria < 0.2 ppbv < RL
BFB absolute abundance criteria Within 10% of that from the previous day. CCV internal standard area counts are compared to ICAL, corrective action for > 40% D.
Daily CCV 70-130% for listed 39 VOCs. 70-130%. ATL’s 62 standard compound list exceeding this criterion and associated data will be flagged and narrated.
If more than two compounds from the standard list recover outside of 70-130%, corrective action will be taken. Unless
prior client approval; under no circumstances will samples be analyzed if any compound exceeds 60-140%.
Initial Calibration ≤ 30% RSD for listed 39
VOCs
≤ 30% RSD with 2 of ATL’s 62 standard compounds
allowed out to ≤ 40%..
The standard target analyte list, Limit of Quantitation, QC criteria, and QC summary can be found in
Tables 6.11.2 – 6.11.6.
Table 6.11.2 Method TO-14A/TO-15 Analyte List
Analyte
RL (ppbv) LL/TO-
15/5&20
%RSD

Acceptance Criteria
LCS
(%R)
Precision Limits
(Max. RPD)
1,1,2,2-Tetrachloroethane 0.1/0.5/5.0 30% 70 - 130 ≤ 25
1,1,2-Trichloroethane 0.1/0.5/5.0 30% 70 - 130 ≤ 25
1,1-Dichloroethane 0.1/0.5/5.0 30% 70 - 130 ≤ 25
1,1-Dichloroethene 0.1/0.5/5.0 30% 70 - 130 ≤ 25
1,2,4-Trichlorobenzene 0.5/2.0/20 30% 70 - 130 ≤ 25
1,2,4-Trimethylbenzene 0.1/0.5/5.0 30% 70 - 130 ≤ 25
1,2-Dibromoethane (EDB) 0.1/0.5/5.0 30% 70 - 130 ≤ 25
1,2-Dichlorobenzene 0.1/0.5/5.0 30% 70 - 130 ≤ 25
1,2-Dichloroethane 0.1/0.5/5.0 30% 70 - 130 ≤ 25
1,2-Dichloropropane 0.1/0.5/5.0 30% 70 - 130 ≤ 25
1,3,5-Trimethylbenzene 0.1/0.5/5.0 30% 70 - 130 ≤ 25
1,3-Dichlorobenzene 0.1/0.5/5.0 30% 70 - 130 ≤ 25
1,4-Dichlorobenzene 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Benzene 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Bromomethane 0.1/0.5/5.0 30% 70 - 130 ≤ 25
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Revision 22.1, 09/2011 Page 6-46
Analyte
RL
(ppbv) LL/TO-
15/5&20
%RSD

Acceptance Criteria
LCS
(%R)
Precision Limits
(Max. RPD)
Carbon Tetrachloride 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Chlorobenzene 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Chloroethane 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Chloroform 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Chloromethane 0.1/2.0/20 30% 70 - 130 ≤ 25
α-Chlorotoluene (Benzyl Chloride) 0.1/0.5/5.0 30% 70 - 130 ≤ 25
cis-1,2-Dichloroethene 0.1/0.5/5.0 30% 70 - 130 ≤ 25
cis-1,3-Dichloropropene 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Dichloromethane 0.2/0.5/5.0 30% 70 - 130 ≤ 25
Ethylbenzene 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Freon 11 (Trichlorofluoromethane) 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Freon 113 (Trichlorotrifluoroethane) 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Freon 114 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Freon 12 (Dichlorodifluoromethane) 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Hexachlorobutadiene 0.5/2.0/20 30% 70 - 130 ≤ 25
m,p-Xylene 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Methyl Chloroform (1,1,1-
Trichloroethane) 0.1/0.5/5.0 30% 70 - 130 ≤ 25
o-Xylene 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Styrene 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Tetrachloroethene 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Toluene 0.1/0.5/5.0 30% 70 - 130 ≤ 25
trans-1,3-Dichloropropene 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Trichloroethene 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Vinyl Chloride 0.1/0.5/5.0 30% 70 - 130 ≤ 25
Table 6.11.3 Method TO-14A/TO-15 Analyte List
Analyte
RL (ppbv)
LL/TO-15/ 5&20

%RSD
Acceptance Criteria
LCS (%R) Precision Limits
1,3-Butadiene 0.1/0.5/5.0 30% 60 – 140 ≤ 25
1,4-Dioxane 0.1/2.0/20 30% 60 – 140 ≤ 25
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Revision 22.1, 09/2011 Page 6-47
Analyte
RL (ppbv)
LL/TO-15/ 5&20

%RSD
Acceptance Criteria
LCS (%R) Precision Limits
2-Butanone (Methyl Ethyl Ketone) 0.1/0.5/5.0 30% 60 – 140 ≤ 25
2-Hexanone 0.5/2.0/20 30% 60 – 140 ≤ 25
4-Ethyltoluene 0.1/0.5/5.0 30% 60 – 140 ≤ 25
4-Methyl-2-Pentanone (MIBK) 0.1/0.5/5.0 30% 60 – 140 ≤ 25
Acetone 0.5/2.0/20 30% 60 – 140 ≤ 25
Bromodichloromethane 0.1/0.5/5.0 30% 60 – 140 ≤ 25
Bromoform 0.1/0.5/5.0 30% 60 – 140 ≤ 25
Carbon Disulfide 0.5/0.5/5.0 30% 60 – 140 ≤ 25
Cyclohexane 0.1/0.5/5.0 30% 60 – 140 ≤ 25
Dibromochloromethane 0.1/0.5/5.0 30% 60 – 140 ≤ 25
Ethanol 0.5/2.0/20 30% 60 – 140 ≤ 25
Heptane 0.1/0.5/5.0 30% 60 – 140 ≤ 25
Hexane 0.1/0.5/5.0 30% 60 – 140 ≤ 25
Isopropanol (2-Propanol) 0.5/2.0/20 30% 60 – 140 ≤ 25
Methyl t-Butyl Ether (MTBE) 0.1/0.5/5.0 30% 60 – 140 ≤ 25
Propylene 0.5/2.0/20 30% 60 – 140 ≤ 25
Tetrahydrofuran 0.5/0.5/5.0 30% 60 – 140 ≤ 25
trans-1,2-Dichloroethene 0.1/0.5/5.0 30% 60 – 140 ≤ 25
2,2,4-Trimethylpentane 0.5/0.5/5.0 30% 60 – 140 ≤ 25
Cumene 0.1/0.5/5.0 30% 60 – 140 ≤ 25
Propylbenzene 0.1/0.5/5.0 30% 60 – 140 ≤ 25
3-Chloroprene 0.5/2.0/20 30% 60 – 140 ≤ 25
Naphthalene 0.5/2.0/20 30% 60 – 140 ≤ 25
TPH (Gasoline) or NMOC
(Hexane/Heptane) 10/25/100 One Point
Calibration NA ≤ 25
Table 6.11.4 Internal Standards Table 6.11.5 Surrogates
Analyte Accuracy (% R) Analyte Accuracy (% R)
Bromochloromethane 60 - 140 1,2-Dichloroethane-d4 70 – 130
1,4-Difluorobenzene 60 - 140 Toluene-d8 70 – 130
Chlorobenzene-d5 60 - 140 4-Bromofluorobenzene 70 – 130

Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-48 Table 6.11.6 Summary of Calibration and QC Procedures for Methods TO-14A/TO-15
QC Check
Minimum
Frequency
Acceptance
Criteria
Corrective
Action
Tuning Criteria Every 24 hours, or every 12
hours if project requires.
SW – 846 tune criteria. Correct problem then repeat tune.
5-Point Calibration Prior to sample analysis. % RSD ≤ 30 with two
compounds allowed out to ≤ 40% RSD for QUAD and
5&20 (4 allowed out for LL).
Correct problem then repeat Initial Calibration Curve.
LCS After each initial calibration
curve, and daily, prior to sample
analysis.
Recoveries for 90% of "Standard" compounds must be
70-130%; for 80% of "Non-standard" compounds,
recoveries must be 60-140%. No recovery may be <50%.
* If specified by the client in-house generated control limits
may be used.
Check the system and reanalyze the standard. Re-prepare the standard if
necessary. Re-calibrate the instrument if the criteria cannot be met.
Continuing
Calibration Verification
(CCV)
At the start of
each day and, if required by a
specific project, every 12 hours.
For QUAD and 5&20: 70-
130%. Compounds exceeding this criterion and associated
data will be flagged and narrated with the exception of
high bias associated with non-detects.
If more than two compounds from the standard list recover
outside of 70-130%, corrective action will be taken. Unless
prior client approval; under no circumstances will samples be
analyzed if any compound exceeds 60-140%.
For Low Level analysis the above applies except corrective
action will be taken if more than four compounds from the
standard list recover outside of 70-130%.
Perform maintenance and repeat test. If
the system still fails the CCV, perform a new 5 point calibration curve.
Laboratory Blank After the
CCV/LCS.
Results less than the laboratory
reporting limit.
Inspect the system and re-analyze the
blank.
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Revision 22.1, 09/2011 Page 6-49
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Internal Standard
(IS)
As each
standard, blank, and sample is
being loaded.
Retention time (RT) for blanks
and samples must be within ±0.33 min of the RT in the
CCV and within ±40% of the area counts of the daily CCV
internal standards.

For blanks: inspect the system and
reanalyze the blank. Analysis is discontinued until the blank meets the IS
criteria.
For samples: re-analyze the sample. If
the ISs are within limits in the re-analysis, report the second analysis. If
ISs are out-of-limits a second time, dilute the sample until ISs are within
acceptance limits and narrate.
Surrogates As each
standard, blank, and sample is
being loaded.
70 - 130%.
* If specified by the client in-house generated control limits may be used.
For blanks: inspect the system and
reanalyze the blank. Analysis is discontinued until the blank meets the
surrogate recovery criteria
For samples: re-analyze the sample
unless obvious matrix interference is documented. If the %R is within limits
in the re-analysis, report the second analysis. If %R is out-of-limits a second time, then narrate results.
Laboratory Control Spike Duplicate
(LCSD)
1 dup/analytical batch. RPD ≤25%. Inspect the system and re-analyze; if out again, narrate.

Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-50 6.12 TO-14A/TO-15 VOLATILE ORGANIC COMPOUNDS BY SIM
This method involves Selective Ion Monitoring (SIM) GC/MS analysis of whole air samples collected in evacuated stainless steel canisters. Samples are analyzed for volatile organic compounds using EPA
Method TO-14A/TO-15 protocols. An aliquot of the sample is withdrawn from the canister through a mass flow controller and concentrated onto a hydrophobic drying system that removes water from the
sample stream. The sample is then focused onto a cryogenic cooled column prior to analysis by GC/MS
in the (SIM) mode.
Some MSD’s can be set to acquire both SIM and full scan data simultaneously. This generates two
separate data files in the analytical software. One file contains full scan data and the other contains SIM
data for selected compounds. The results for each sample in a report will be from two separate data files originating from the same analytical run. The two data files have the same base file name and are
differentiated with a "sim" extension on the SIM data file.
Certain compounds are not included in ATL’s standard target analyte list. These compounds are communicated at the time of client proposal request. Unless otherwise directed, ATL reports these non-
standard compounds with partial validation. Validation includes a 3-point calibration with the lowest
concentration defining the reporting limit, no second source verification is analyzed, and no method detection limit study is performed unless previous arrangements have been made. In addition, stability of
the non-standard compound during sample storage is not validated. Full validation may be available upon request.
Air Toxics Ltd. performs a modified version of this method. The target analyte list and Limit of
Quantitation reflect relevant risk driving compounds and are available upon request. The method modifications, QC criteria, and QC summary may be found in the following tables.
Table 6.12.1.A Summary of TO-15 SIM Method Modifications
Requirement TO-15 ATL Modifications
Initial Calibration ≤ 30% RSD with 2 compounds allowed out to ≤ 40% RSD. ≤ 30% RSD with 10% of compounds allowed out to ≤ 40%.
Blanks and standards Zero Air Nitrogen
Table 6.12.1.B Summary of TO-14A Method Modifications
Requirement TO-14A ATL Modifications
Sample Drying System Nafion Drier Multibed hydrophobic sorbent
Blank acceptance criteria < 0.2 ppbv < RL
BFB absolute abundance criteria Within 10% of that from the previous day. CCV internal standard area counts are compared to ICAL, corrective action for > 40% D.
Daily CCV 70-130% for listed 39
VOCs.
70-130%. ATL’s 62 standard compound list
exceeding this criterion and associated data will be flagged and narrated.
If more than two compounds from the standard list
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Revision 22.1, 09/2011 Page 6-51
Requirement TO-14A ATL Modifications
recover outside of 70-130%, corrective action will be taken. Unless prior client approval; under no
circumstances will samples be analyzed if any compound exceeds 60-140%.
Initial Calibration ≤ 30% RSD for listed 39
VOCs
≤ 30% RSD with 2 of ATL’s 62 standard
compounds allowed out to ≤ 40%..
Table 6.12.2 Internal Standards Table 6.12.3 Surrogates
Analyte Accuracy
(% R)
Analyte Accuracy
(% R)
Bromochloromethane 60 - 140 1,2-Dichloroethane-d4 70 – 130
1,4-Difluorobenzene 60 - 140 Toluene-d8 70 – 130
Chlorobenzene-d5 60 - 140 4-Bromofluorobenzene 70 – 130
Table 6.12.4 Summary of Calibration and QC Procedures for Methods TO-14A/TO-15 by SIM
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Tuning
Criteria
Every 24 hours, or
every 12 hours if
project requires.
SW – 846 tune criteria. Correct problem then repeat tune.
Minimum 5-Point
Calibration
Prior to sample analysis ≤ 30% for standard compounds with 10% of the compound list
allowed out to ≤ 40% RSD.
Correct problem then repeat Initial Calibration Curve.
Laboratory Control
Standard (LCS)
After each initial calibration curve,
and daily prior to sample analysis.
Recoveries for 90% of "Standard" compounds must be ±30%; for
80% of "Non-standard" compounds, recoveries must be
±40%. No recovery may be <50%.
* If specified by the client in-
house generated control limits may be used.
Check the system and re-analyze the standard. Re-prepare the standard if
necessary. Re-calibrate the instrument if the criteria cannot be met.
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Revision 22.1, 09/2011 Page 6-52
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Continuing
Calibration Verification
(CCV)
At the start of each
day and, if required by a specific
project, every 12 hours.
70-130%. Compounds exceeding
this criterion and associated data will be flagged and narrated with
the exception of high bias associated with non-detects.
If more than 10% of compounds from the standard list recover
outside of 70-130%, corrective action will be taken. Unless prior
client approval; under no circumstances will samples be
analyzed if any compound exceeds 60-140%.
Perform maintenance and repeat test.
If the system still fails the CCV, perform a new calibration curve.
Laboratory Blank After the LCS. Results less than the laboratory reporting limit. Inspect the system and re-analyze the blank.
Internal
Standard (IS)
As each standard,
blank, and sample is being loaded.
Retention time (RT) for blanks
and samples must be within ±0.33 min of the RT in the CCV and
within ±40% of the area counts of the daily CCV internal standards.

For blanks: inspect the system and re-
analyze the blank.
For samples: re-analyze the sample. If
the ISs are within limits in the re-analysis, report the second analysis. If
ISs are out-of-limits a second time, dilute the sample until ISs are within
acceptance limits and narrate.
Surrogates As each standard, blank, and sample is being loaded.
70 - 130%.
* If specified by the client in-house generated control limits may be used.
For blanks: inspect the system and re-analyze the blank.
For samples: re-analyze the sample unless obvious matrix interference is
documented. If the %R is within limits in the re-analysis, report the second analysis. If %R is out-of-limits a
second time, report data from first analysis and narrate.
Laboratory
Control Spike
Duplicate (LCSD)
1 dup/analytical batch. RPD ≤ 25% .

Inspect the system and re-analyze; if
out again, narrate.

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Revision 22.1, 09/2011 Page 6-53 6.13 TO-15 ALIPHATIC AND AROMATIC VOLATILE PETROLEUM HYDROCARBONS
(VPH) FRACTIONS BY GC/MS
The TO-15 VPH outlines procedures to estimate the concentrations of gaseous phase Aliphatic and
Aromatic ranges in ambient air and soil gas collected in stainless steel Summa canisters. The volatile Aliphatic hydrocarbons are collectively quantified within the C5 to C6 range, C6 to C8 range, C8 to C10
range and the C10 to C12 range. Additionally, the volatile Aromatic hydrocarbons are collectively
quantified within the C8 to C10 range and the C10 to C12 range. The Aromatic ranges refer to the equivalent carbon (EC) ranges.
Data is acquired using standard TO-15 GC/MS instrumentation. Procedures are largely based on the hydrocarbon ranges and calibration reference compounds defined by the Washington State Department of Ecology (WSDE) Method for the Determination of Volatile Petroleum Hydrocarbons (VPH) fractions
dated June 1997. Additionally, the WSDE VPH calibration and quantitation procedures for the Aromatic fraction have been enhanced to more effectively isolate the compounds of interest. The Aromatic fraction measurement is based on a modification of the Massachusetts Department of Environmental Protection
(MADEP) Air Phase Hydrocarbon Method (2008).
Air Toxics Ltd. performs a modified version of this method. The method modifications, standard target
analyte list, Limit of Quantitation, QC criteria, and QC summary can be found in the following tables.
Table 6.13.1. Summary of Method Modifications
Requirement VPH ATL Modifications
Detector Tandem GC/FID/PID GC/MS
Matrix Soil, Water and Sediments Whole Air Samples

C6-C8 Reference Compound Octane Heptane
Surrogate 2,5-Dibromotoluene Bromochloromethane, 1,2-Dichloroethane-d4, Toluene-d8,
Chlorobenzene-d5 and 4-Bromofluorobenzene
%RSD for Reference
Compounds
<20% RSD <30% RSD with the exception of
Decane, Dodecane, 1,2,4,5-Tetramethylbenzene and
Naphthalene at ≤ 40% RSD
%D for the CCV +20% D +30% D with the exception of
Decane, Dodecane, 1,2,4,5-Tetramethylbenzene- and
Naphthalene at +40% D
Laboratory Control Spike Matrix Spiking Solution Independently Prepared Source: performed after initial calibration,
70-130% recovery with the exception of Decane,
Dodecane,1,2,4,5-
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-54
Requirement VPH ATL Modifications
Tetramethylbenzene- and Naphthalene at 60-140%
CCV Frequency Before and After Every 10 Samples Daily, Before Sample Analysis

IDOC
4 Replicates of a CCV, with
recovery of +20% and a %RSD <20%
Not performed for this method as
the requirement is met by TO-15 IDOC performed on the same
instrument
Table 6.13.2 VPH Standard Analyte List (Note: TO-15 analytes can also be included).
Analyte
Reporting Limit
(ppbv)
Acceptance Criteria
ICAL (%RSD
)
ICV
(%R)
CCV
(% D)
Pentane NA ≤ 30% 70-130 ≤ 30%
Hexane NA ≤ 30% 70-130 ≤ 30%
C5-C6 Aliphatics Pentane + Hexane 10 ≤ 30% 70-130 ≤ 30%
C6-C8 Aliphatics ref. to Heptane 10 ≤ 30% 70-130 ≤ 30%
C8-C10 Aliphatics ref. to Decane 10 ≤ 30% 70-130 ≤ 30%
C10-C12 Aliphatics ref. to Dodecane 10 ≤ 30% 70-130 ≤ 30%
Ethylbenzene 2 ≤ 30% 70-130 ≤ 30%
m/p-Xylene 2 ≤ 30% 70-130 ≤ 30%
o-Xylene 2 ≤ 30% 70-130 ≤ 30%
C8-C10 Aromatics ref. to 1,2,3-Trimethylbenzene 10 ≤ 30% 70-130 ≤ 30%
C10-C12 Aromatics ref. to 1,2,4,5-Tetramethylbenzene 10 ≤ 40% 60-140 ≤ 40%
Naphthalene 2 ≤ 40% 60-140 ≤ 40%
Table 6.13.3 Internal Standards (evaluated in associated TO-15 analysis)
Analyte Accuracy Limits (%)
Bromochloromethane 50 to 200
1,4-Difluorobenzene 50 to 200
Chlorobenzene-d5 50 to 200
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-55 Table 6.13.4 Summary of Calibration and QC Procedures
QC Check
Minimum
Frequency
Acceptance
Criteria
Corrective
Action
Tuning Criteria Every 24 hours. Compendium of Methods for Toxic Organic Air Pollutants, Method TO-14A, January 1999.
Correct problem then repeat tune.
6 Point Calibration Prior to sample Analysis. %RSD ≤30% for VPH Target Analyte with the exceptions for1,2,4,5-
Tetramethylbenzene and Naphthalene which are <40%.
Correct problem then repeat initial calibration curve.
ICV

After each initial
calibration curve
Recoveries for the VPH target
compounds 70-130% or 60-140% for 1,2,4,5-Tetramethylbenzene and
Naphthalene. If recovery of any compound is above 130%. Analyze
samples as long as compound is not detected.
Check the system and re-
analyze the standard. Re-prepare the standard if
necessary. Re-calibrate the instrument if the
criteria cannot be met.
Continuing
Calibration Verification (CCV)
At the beginning of each
day. %D ≤ 30% for VPH target compounds with the exceptions for 1,2,4,5-
Tetramethylbenzene and Naphthalene which are <40%. One compound is
allowed to be out as long as it is < 50%D. If recovery of any compound
is above 150% the instrument must be re-calibrated.
Perform maintenance and
repeat test. If the CCV still fails, perform
maintenance and a new 6 point calibration curve.
Laboratory Blank After the CCV. Results less than the laboratory RL
(Table B-1).
Inspect the system and
re-analyze the blank.
Internal Standard (IS) As each standard, Blank, and sample is being
loaded.
Retention time (RT) for the blanks and samples must be within ±0.33 min of
the RT in the CCV.
The IS area must be within -50 to
200% of the CCV’s IS area for the blanks and samples. This evaluation
occurs during the associated TO-15 analysis.
For blanks: inspect the system and re-analyze the
blank;
For samples: If there is
not obvious interference with the internal
standard, re-analyze the sample. If the ISs are
within limits in the re-analysis, report the
second analysis. Dilution of the sample to get IS
areas within limits may be used if the RL is being
obtained.
Laboratory Control Spike
Duplicate (LSCD)
One per analytical batch; since VPH
analysis occurs with TO-15 analysis, the
RPD ≤ 25% for detections >5 X's the RL.
Inspect the system and re-analyze; if out again,
narrate.
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Revision 22.1, 09/2011 Page 6-56
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Duplicate is reported
from the daily TO-15 LCS/LCSD pair. The
result is not reported with the VPH fraction

Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-57 6.14 AIR PHASE PETROLEUM HYDROCARBONS (MA APH)
The MADEP APH method describes techniques for the analysis of air-phase petroleum hydrocarbons (APH) collected as whole air samples in stainless steel canisters. Up to 0.5 Liters of air is withdrawn
from the canister through a mass flow controller and is concentrated using a multisorbent trap which also serves as a hydrophobic dryer for moisture removal. The focused air sample is then flash heated through
the hydrophobic drying system which removes the water from the sample stream prior to analysis by full
scan GC/MS. Air Toxics Ltd. performs this analysis without taking modifications to the MADEP APH method. The standard target analyte list, Limit of Quantitation, QC criteria, and QC summary can be found in the following tables.
Table 6.14.1 APH Target Compound List
Analyte
Reporting
Limit (ug/m3)
Acceptance Criteria
Accuracy
Limits (%R)
Precision
Limits (RPD)
1,3-Butadiene* 2.0 70 - 130 ± 25
Methyl-tert-butyl ether (MTBE)* 2.0 70 - 130 ± 25
Benzene* 2.0 70 - 130 ± 25
Toluene* 2.0 70 - 130 ± 25
Ethyl benzene* 2.0 70 - 130 ± 25
m/p-Xylene* 2.0 70 - 130 ± 25
o-Xylene* 2.0 70 - 130 ± 25
Naphthalene 2.0 60 - 140 ± 25
*Compounds comprise the LCS/2nd Source Standard.
Table 6.14.2 Aliphatics & Aromatics Hydrocarbon Ranges
Analyte Reporting Limit
(µg/m3)
Acceptance Criteria
Accuracy Limits
(%R)
Precision Limits
(RPD)
C5-C8 Aliphatics 12 70 - 130 ± 25
C9-C12 Aliphatics 12 70 - 130 ± 25
C9-C10 Aromatics 10 70 - 130 ± 25
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-58 Table 6.14.3 Internal Standards
Analyte Accuracy Limits (%)
Bromochloromethane 50 to 200
1,4-Difluorobenzene 50 to 200
Chlorobenzene-d5 50 to 200
Table 6.14.4 Surrogates
Analyte Accuracy Limits (%R)
1,2-Dichloroethane-d4 70 – 130
Toluene-d8 70 – 130
4-Bromofluorobenzene 70 – 130
Table 6.14.5 Summary of Calibration and QC Procedures
QC Check
Minimum
Frequency
Acceptance
Criteria
Corrective
Action
Tuning
Criteria
Every 24 hours. Compendium of Methods for Toxic
Organic Air Pollutants, Method TO-14A, January 1999.
Correct problem then
repeat tune.
5 Point
Calibration
Prior to sample
Analysis. %RSD ≤30% for APH Target Analyte or hydrocarbon range. Naphthalene is
<40%.
Correct problem then
repeat initial calibration curve.
LCS (Subset of Target
Compounds)
After each initial calibration curve, daily
prior to sample analysis.
Recoveries for the APH target compounds and hydrocarbon ranges
must be ±30%. If recovery of any compound is above 130%. Analyze
samples as long as compound is not detected.
Check the system and re-analyze the standard. Re-
prepare the standard if necessary. Re-calibrate
the instrument if the criteria cannot be met.
Continuing
Calibration Verification
(CCV)
At the beginning of
each day. %D ≤ 30% for APH target compounds
and hydrocarbon ranges. One compound is allowed to be out as long as it is < 50%D. Target compound
Naphthalene allowed %D ≤ 40%. If recovery of any compound is above
150%. Instrument must be re-calibrated.
Perform maintenance and
repeat test. If the CCV still fails, perform
maintenance and a new 5-7 point calibration curve.
Laboratory
Blank
After the CCV/LCS. Results less than the laboratory RL
(Tables 6.14.1 and 6.14.2). Naphthalene and C12 are allowed to
be 2X the RL.
Inspect the system and re-
analyze the blank.
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Revision 22.1, 09/2011 Page 6-59
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Internal
Standard (IS)
As each standard,
Blank, and sample is being loaded.
Retention time (RT) for the blanks and
samples must be within ±0.33 min of the RT in the CCV.
The IS area must be within -50 to 200% of the CCV’s IS area for the
blanks and samples.
For blanks: inspect the
system and re-analyze the blank;
For samples: If there is not obvious interference
with the internal standard, re-analyze the sample. If
the ISs are within limits in the re-analysis, report the
second analysis. Dilution of the sample to get IS
areas within limits may be used if the RL is being
obtained.
Surrogates As each standard, blank, and sample is
being loaded.
70 – 130% R. For blanks: inspect the system and re-analyze the
blank;
For samples: re-analyze
sample unless obvious matrix interference is
documented. If the %R is within limits in the re-
analysis, report the 2nd analysis. If %R is out-of-
limits a 2nd time, report data from 1st analysis and
narrate.
Laboratory Control
Spike Duplicate
(LCSD)
1 dup/analytical batch. RPD ≤ 30%. Inspect the system and re-analyze; if out again,
narrate.

Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-60 6.15 TO-17 VOLATILE ORGANIC COMPOUNDS
This method is an alternative to the canister based sampling and analysis methods that are presented in EPA Compendium Methods TO-14 and TO-15. Sorbent sampling is also amenable to efficient collection
and measurement of semi-volatile compounds which are prone to condensing on the surface of the canister. Thermal desorption GC/MS can be applied to matrices beyond ambient air such as soil gas and
materials emissions by carefully selecting the appropriate sorbent and sampling parameters.
Samples are collected by drawing a volume of air through a sorbent packed tube. Samples can also be collected using passive sampling techniques relying on principles of diffusion to collect VOCs onto the
exposed sorbent. The sample cartridges are thermally desorbed by heating and purging with UHP
Helium. The resulting gaseous effluent is transferred to secondary trap for re-concentration and desorption onto the GC/MS.
Occasionally, samples may be analyzed by thermal desorption followed by introduction of the effluent
into a purge and trap system containing 5.0mL of boiled and purged reagent grade VOA free water. The compounds are then purged onto a GC/MS for analysis. This is a modification to Method TO-17.
Certain compounds are not included in ATL’s standard target analyte list. These compounds are
communicated at the time of client proposal request. Unless otherwise directed, ATL reports these non-standard compounds with partial validation. Validation includes a 3-point calibration with the lowest
concentration defining the reporting limit, no second source verification is analyzed, and no method detection limit study is performed unless previous arrangements have been made. In addition, stability of the non-standard compound during sample storage is not validated. Full validation may be available upon
request.
Air Toxics Ltd. performs a modified version of this method. The method modifications, standard target analyte list, Limit of Quantitation, QC criteria, and QC summary can be found in the following tables.
Table 6.15.1 Summary of Method Modifications
Requirements EPA Method TO-17 Air Toxics Ltd. Modifications
Lab Blank At least 2 tubes from the same cleaning batch as the samples are
analyzed at the beginning and end of the analytical sequence.
Do not dry purge Lab Blanks.
Tubes used for daily lab blank may or may not be from the same batch or sampling media. Only 1 lab blank is
analyzed prior to sample analysis. Lab blanks are dry purged to eliminate the possibility of sample anomaly
attributed to Dry purge process.
*Sample desorption Method involves primary and secondary desorption. Modification applies only when using a Tekmar P&T system. After primary desorption, the stream of effluent
gas is passed through 5ml of clean purged D.I. water before the secondary desorption. D.I. water acts as a
filter for excessive acidic moisture in the samples.

*Modifications are dependent on application.
Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-61 Table 6.15.2 Summary of Sorbent Applications
Sorbent Typical Analyte Range Water management Primary Applications
Carbotrap 300 C3 – C12 High levels of moisture
may interfere with
analysis.
Indoor air and outdoor air.
Tenax TA C7 – C26 Hydrophobic. All vapors including soil gas.
Tenax GR C7 – C30 Hydrophobic. All vapors including soil gas.
Tenax TA/
Carbograph 1/Carbograph 5
C4-C26 Hydrophobic. All vapors including soil gas.
Table 6.15.3 TO-17 Carbotrap 300 Analyte List
Analytes RL (ng)
Acceptance Criteria
ICAL (%RSD) LCS (% R) CCV (%D)
1,1,1-Trichloroethane 10 30 70 – 130 30
1,1,1,2-Tetrachloroethane 10 30 70 – 130 30
1,1,2,2-Tetrachloroethane 10 30 70 – 130 30
1,1,2-Trichloroethane 10 30 70 – 130 30
1,1-Dichloroethane 10 30 70 – 130 30
1,1-Dichloroethene 10 30 70 – 130 30
1,1-Dichloropropene 10 30 70 – 130 30
1,2,3-Trichlorobenzene 50 30 70 – 130 30
1,2,3-Trichloropropane 10 30 70 – 130 30
1,2,4-Trichlorobenzene 50 30 70 – 130 30
1,2,4-Trimethylbenzene 10 30 70 – 130 30
1,2-Dibromo-3-chloropropane 50 30 70 – 130 30
1,2-Dichlorobenzene 10 30 70 – 130 30
1,2-Dichloroethane 10 30 70 – 130 30
1,2-Dichloropropane 10 30 70 – 130 30
1,3,5-Trimethylbenzene 10 30 70 – 130 30
1,3-Butadiene 50 30 50 – 150 30
1,3-Dichlorobenzene 10 30 70 – 130 30
1,3-Dichloropropane 10 30 70 – 130 30
1,4-Dichlorobenzene 10 30 70 – 130 30
2,2-Dichloropropane 50 30 70 – 130 30
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Revision 22.1, 09/2011 Page 6-62
Analytes RL (ng)
Acceptance Criteria
ICAL (%RSD) LCS (% R) CCV (%D)
2-Chloropropane 50 30 70 – 130 30
2-Chlorotoluene 10 30 70 – 130 30
Allyl chloride 50 30 70 – 130 30
4-Chlorotoluene 10 30 70 – 130 30
Acrylonitrile 50 30 70 – 130 30
Benzene 10 30 70 – 130 30
Bromobenzene 10 30 70 – 130 30
Bromochloromethane 10 30 70 – 130 30
Bromodichloromethane 10 30 70 – 130 30
Bromoform 10 30 70 – 130 30
Bromomethane 10 30 50 – 150 30
Butylbenzene 10 30 70 – 130 30
Carbon Disulfide 10 30 70 – 130 30
Carbon Tetrachloride 10 30 70 – 130 30
Chlorobenzene 10 30 70 – 130 30
Chloroethane 10 30 50 – 150 30
Chloroform 10 30 70 – 130 30
Chloromethane 10 30 50 – 150 30
cis-1,2-Dichloroethene 10 30 70 – 130 30
cis-1,3-Dichloropropene 10 30 70 – 130 30
cis-1,4-Dichloro-2-butene 50 30 70 – 130 30
Cumene 10 30 70 – 130 30
Dibromochloromethane 10 30 70 – 130 30
Dibromomethane 10 30 70 – 130 30
Dichlorodifluoromethane 10 30 50 – 150 30
Ethylbenzene 10 30 70 – 130 30
Ethylene Dibromide 10 30 70 – 130 30
Freon 11 10 30 70 – 130 30
Freon 113 10 30 70 – 130 30
Hexachlorobutadiene 50 30 70 – 130 30
Hexane 10 30 70 – 130 30
Iodomethane 50 30 70 – 130 30
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Revision 22.1, 09/2011 Page 6-63
Analytes RL (ng)
Acceptance Criteria
ICAL (%RSD) LCS (% R) CCV (%D)
Methylene Chloride 10 30 70 – 130 30
Methyl t-butyl ether (MTBE) 10 30 70 – 130 30
Naphthalene 50 30 70 – 130 30
m,p-Xylene 10 30 70 – 130 30
o-Xylene 10 30 70 – 130 30
p-Cymene 10 30 70 – 130 30
Propylbenzene 10 30 70 – 130 30
sec-Butylbenzene 10 30 70 – 130 30
Styrene 10 30 70 – 130 30
tert-Butylbenzene 10 30 70 – 130 30
Tetrachloroethene 10 30 70 – 130 30
Toluene 10 30 70 – 130 30
trans-1,2-Dichloroethene 10 30 70 – 130 30
trans-1,3-Dichloropropene 10 30 70 – 130 30
trans-1,4-Dichloro-2-butene 50 30 70 – 130 30
Trichloroethene 10 30 70 – 130 30
Vinyl Bromide * 50 30 50 – 150 30
Vinyl Chloride 10 30 50 – 150 30
* Independent Source Verification Check not available for this compound.
Table 6.15.4 Internal Standard Recovery Limits (Carbotrap 300) Table 6.15.5 Field Surrogate Recovery Limits (Carbotrap 300)
Analyte
CCV IS
(%R)
Sample IS
(%R)

Analyte
Accuracy
(%R)
1,4-Dichlorobenzene-d4 50 – 200 60 – 140 Benzene-d6 50 – 150
Chlorobenzene-d5 50 – 200 60 – 140 4-Bromofluorobenzene 70 – 130
Fluorobenzene 50 – 200 60 – 140 Naphthalene-d8 70 – 130
Toluene-d8 70 – 130
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Revision 22.1, 09/2011 Page 6-64 Table 6.15.6 TO-17 (Tenax GR/TA)
Analytes
Reporting Limit (ng)
Acceptance Criteria
ICAL (%RSD) LCS (% R) CCV
1,1,1-Trichloroethane 5.0 30 70 – 130 30
1,1,1,2-Tetrachloroethane 5.0 30 70 – 130 30
1,1,2,2-Tetrachloroethane 5.0 30 70 – 130 30
1,1,2-Trichloroethane 5.0 30 70 – 130 30
1,1-Dichloropropene 5.0 30 70 – 130 30
1,2,3-Trichlorobenzene 5.0 30 70 – 130 30
1,2,3-Trichloropropane 5.0 30 70 – 130 30
1,2,4-Trichlorobenzene 5.0 30 70 – 130 30
1,2,4-Trimethylbenzene 5.0 30 70 – 130 30
1,2-Dibromo-3-chloropropane 5.0 30 70 – 130 30
1,2-Dichlorobenzene 5.0 30 70 – 130 30
1,2-Dichloroethane 5.0 30 70 – 130 30
1,2-Dichloropropane 5.0 30 70 – 130 30
1,3,5-Trimethylbenzene 5.0 30 70 – 130 30
1,3-Dichlorobenzene 5.0 30 70 – 130 30
1,3-Dichloropropane 5.0 30 70 – 130 30
1,4-Dichlorobenzene 5.0 30 70 – 130 30
2-Chlorotoluene 5.0 30 70 – 130 30
4-Chlorotoluene 5.0 30 70 – 130 30
Benzene 5.0 30 70 – 130 30
Bromobenzene 5.0 30 70 – 130 30
Bromodichloromethane 5.0 30 70 – 130 30
Bromoform 5.0 30 70 – 130 30
Butylbenzene 5.0 30 70 – 130 30
Carbon Tetrachloride 5.0 30 70 – 130 30
Chlorobenzene 5.0 30 70 – 130 30
Styrene 5.0 30 70 – 130 30
tert-Butylbenzene 5.0 30 70 – 130 30
Tetrachloroethene 5.0 30 70 – 130 30
Toluene 5.0 30 70 – 130 30
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Revision 22.1, 09/2011 Page 6-65
Analytes
Reporting
Limit (ng)
Acceptance Criteria
ICAL (%RSD) LCS (% R) CCV
trans-1,3-Dichloropropene 5.0 30 70 – 130 30
trans-1,4-Dichloro-2-butene 5.0 30 70 – 130 30
Trichloroethene 5.0 30 70 – 130 30
Chloroform 5.0 30 70 – 130 30
cis-1,3-Dichloropropene 5.0 30 70 – 130 30
cis-1,4-Dichloro-2-butene 5.0 30 70 – 130 30
Cumene 5.0 30 70 – 130 30
Dibromochloromethane 5.0 30 70 – 130 30
Dibromomethane 5.0 30 70 – 130 30
Ethylbenzene 5.0 30 70 – 130 30
Ethylene Dibromide 5.0 30 70 – 130 30
Hexachlorobutadiene 5.0 30 70 – 130 30
Naphthalene 5.0 30 70 – 130 30
m,p-Xylene 10 30 70 – 130 30
o-Xylene 5.0 30 70 – 130 30
p-Cymene 5.0 30 70 – 130 30
Propylbenzene 5.0 30 70 – 130 30
sec-Butylbenzene 5.0 30 70 – 130 30
Table 6.15.7 Internal Standard Recovery Limits (Tenax GR/TA) Table 6.15.8 Field Surrogate Recovery Limits (Tenax GR/TA)
Analyte CCV IS (%R) Sample IS (%R)

Analyte Accuracy (%R)
1,4-Dichlorobenzene-d4 50 – 200 60 – 140 Benzene-d6 50 – 150
Chlorobenzene-d5 50 – 200 60 – 140 4-Bromofluorobenzene 70 – 130
Fluorobenzene 50 – 200 60 – 140 Toluene-d8 70 – 130
Naphthalene-d8 (optional) 70 – 130

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Revision 22.1, 09/2011 Page 6-66 Table 6.15.9 TO-17 TPH External Calibration (Tenax GR/TA)
Analytes Reporting Limit (ng)
Acceptance Criteria
ICAL
(%RSD)
LCS
(% R) CCV
Mineral Spirits (C9 – C12 range) 500 30 70 – 130 30
Surrogates (optional) % Recovery
Chlorobenzene-d5 70 – 140
Naphthalene – d8 70 - 140
Analytes Reporting Limit
(ng)
Acceptance Criteria
ICAL (%RSD) LCS (% R) CCV
Diesel 1000 30 70 – 130 30
Gasoline 1000 30 70 – 130 30
Kerosene 1000 30 70 – 130 30
Surrogates (optional) % Recovery
Toluene-d8
4-Bromofluorobenzene
70 – 140
70 - 140
Naphthalene – d8 70 - 140
Table 6.15.10 TO-17 (Tenax TA - Passive)
Analytes
Reporting Limit
(ng)
Acceptance Criteria
ICAL
(%RSD)
LCS
(% R) CCV
Benzene 5.0 30 70 – 130 30
Toluene 5.0 30 70 – 130 30
Ethyl benzene 1.0 30 70 – 130 30
m,p-xylene 2.0 30 70 – 130 30
o-Xylene 1.0 30 70 – 130 30
Trichloroethene 1.0 30 70 – 130 30
Tetrachloroethene 1.0 30 70 – 130 30
Cis-1,2-Dichloroethene 1.0 30 70 – 130 30
Trans-1,2-Dichloroethene 1.0 30 70 – 130 30
1,1-Dichloroethene 1.0 30 70 – 130 30
Internal Standards
Analyte CCV IS % Recovery Sample IS % Recovery
1,4-Dichlorobenzene-d4 50 – 200 60 – 140
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Chlorobenzene-d5 50 – 200 60 – 140
Fluorobenzene 50 – 200 60 – 140
Surrogates
Analyte % Recovery
1,2-Dichloroethane-d4 70 – 130
4-Bromofluorobenzene 70 – 130
Dibromofluoromethane 70 – 130
Table 6.15.11 TO-17 (Tenax GR-SVOC)
Analytes
Reporting
Limit (ng)
Acceptance Criteria
ICAL (%RSD) LCS (% R) CCV
Naphthalene 5.0 30 70 – 130 30
2-Methylnaphthalene 5.0 30 70 – 130 30
Acenaphthylene 5.0 30 70 – 130 30
Acenaphthene 5.0 30 70 – 130 30
Fluorene 5.0 30 70 – 130 30
Phenanthrene 5.0 30 70 – 130 30
Anthracene 5.0 30 70 – 130 30
Fluoranthene 5.0 30 70 – 130 30
Pyrene 10 30 70 – 130 30
Internal Standards
Analyte CCV IS % Recovery Sample IS % Recovery
Naphthalene-d8 50 – 200 60 – 140
Acenaphthene-d10 50 – 200 60 – 140
Phenanthrene-d10 50 – 200 60 – 140
Surrogates
Analyte % Recovery
Fluorene-d10 70 – 130
Pyrene-d10 70 – 130

Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-68 Table 6.15.12 Summary of Calibration and QC Procedures for Method TO-17 (Volatile Organic
Compounds)
QC Check
Minimum
Frequency
Acceptance
Criteria
Corrective
Action
Tuning Criteria Every 24 hours, or
every 12 hours if project requires.
SW - 846 tune criteria. Correct problem then repeat tune.
5-Point Calibration Prior to sample Analysis. %RSD < 30%, 2 allowed out up to 40%. Correct problem then repeat Initial Calibration Curve.
LCS After each initial
Calibration Curve and daily prior to analysis.
Recovery 70- 130% or
50- 150% as noted in Table 6.15.3.
Check the system and reanalyze the
standard. Re-prepare the standard if necessary. Re-calibrate the instrument
if the criteria cannot be met.
Continuing Calibration
Verification (CCV)
At the start of each day and, if required by
a specific project, every 12 hours.
70 - 130 %. If project specified risk drivers exceed this criteria, more than 5% of the
compounds exceed this criteria, or any VOC exceeds 50-150% recovery, maintenance is performed and the CCV test repeated. If the system still fails
the CCV, perform a new 5-point Calibration Curve.
Laboratory Blank After the CCV. Results less than the RL. Inspect the system and re-analyze the
Blank.
Internal Standard
(IS)
As each standard,
Blank, and sample is being loaded.
CCVs: area counts 50%
- 200%, RT w/in 30 sec of mid-point in ICAL.
Blanks and samples: Retention time (RT) must
be within ±0.33 minutes of the RT in the CCV.
The IS area must be within ±40% of the
CCV's IS area for the Blanks and samples.
CCV: inspect and correct system prior
to sample analysis.
Blanks: inspect the system and re-
analyze the Blank.
Samples: samples cannot be re-analyzed due to the nature of the sorbent
cartridges. However investigate the
problem by reviewing the data. If necessary, run a Lab Blank to check the
instrument performance. Report the data and narrate.
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Revision 22.1, 09/2011 Page 6-69
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Surrogates As each standard, Blank, and sample is
being loaded.
70 – 130%. For blanks: inspect the system and re-analyze the Blank.
For samples: samples cannot be re-analyzed due to the nature of sorbent
cartridges. However investigate the problem by reviewing the data. If
necessary, run a Lab Blank to check the instrument performance. Report the
data and narrate the problem.
Laboratory Control Spike (LCSD) One/analytical batch. RPD ≤25% Inspect the system and re-analyze; if out again, narrate.

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Revision 22.1, 09/2011 Page 6-70 6.16 TO-17 ‘VAPOR INTRUSION’ VOLATILE AND SEMIVOLATILE ORGANIC
COMPOUNDS
The TO-17 ‘Vapor Intrusion’ (VI) method is an alternative to the canister-based sampling and analysis
methods that are presented in EPA Compendium Methods TO-14A and TO-15 as well as an alternative to PUF/XAD sampling for semivolatile compounds as described by EPA Compendium TO-13A. The VI
tube provides sufficient retention of light VOCs such as 1,3-Butadiene while providing an efficient
desorption of semi-volatile compounds such as Pyrene.
Samples are collected by drawing a volume of air through a sorbent packed tube. The sample cartridges
are thermally desorbed by heating and purging with UHP Helium onto a secondary trap. Analysis is
accomplished by heating the sorbent tube and sweeping the desorbed compounds onto a secondary ‘cold’ trap for water management and analyte refocusing. The secondary trap is heated for efficient transfer of
compounds onto the gas chromatograph (GC) for separation followed by detection using mass
spectrometry (MS). The MS can be run in either full scan mode or SIM mode.
The procedures in this method outline the use of EPA Method TO-17 protocols to determine the
concentrations of volatile organic compounds in air samples collected on sorbent tubes.
Certain compounds are not included in ATL’s standard target analyte list. These compounds are communicated at the time of client proposal request. Unless otherwise directed, ATL reports these non-
standard compounds with partial validation. Validation includes a 3-point calibration with the lowest concentration defining the reporting limit, no second source verification is analyzed, and no method detection limit study is performed unless previous arrangements have been made. In addition, stability of
the non-standard compound during sample storage is not validated. Full validation may be available upon request.
The protocols followed for the method contain no modifications to EPA Method TO-17 of material
significance. The standard target analyte list, Limit of Quantitation, QC criteria, and QC summary can be found in the following tables.
Table 6.16.1 VI Target Analyte List
Volatile Organic Compounds
Reporting
Limit (ng)
Acceptance Criteria
ICAL (%RSD) ICV (% R) CCV (%D) LCS (%R)
Freon 114 7.0 30 70 – 130 30 60 – 140
Vinyl Chloride 2.6 30 70 – 130 30 60 – 140
1,3-Butadiene 2.2 30 70 – 130 30 60 – 140
Isopentane 3.0 30 70 – 130 30 60 – 140
Freon 11 5.6 30 70 – 130 30 60 – 140
1,1-Dichloroethene 4.0 30 70 – 130 30 60 – 140
Methylene Chloride 21 30 70 – 130 30 60 – 140
Freon 113 7.7 30 70 – 130 30 60 – 140
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Volatile Organic Compounds
Reporting
Limit (ng)
Acceptance Criteria
ICAL (%RSD) ICV (% R) CCV (%D) LCS (%R)
Trans-1,2-Dichloroethene 4.0 30 70 – 130 30 60 – 140
1,1-Dichloroethane 4.0 30 70 – 130 30 60 – 140
Cis-1,2-Dichloroethene 4.0 30 70 – 130 30 60 – 140
1,3-Dichloropropane 5.0 30 70 – 130 30 60 – 140
Hexane 3.5 30 70 – 130 30 60 – 140
Chloroform 4.9 30 70 – 130 30 60 – 140
1,2-Dichloroethane 4.0 30 70 – 130 30 60 – 140
1,1,1-Trichloroethane 5.4 30 70 – 130 30 60 – 140
Benzene 3.2 30 70 – 130 30 60 – 140
Carbon Tetrachloride 6.3 30 70 – 130 30 60 – 140
Cyclohexane 3.4 30 70 – 130 30 60 – 140
3-Chloropropene 19 30 70 – 130 30 60 – 140
1,2-Dichloropropane 4.6 30 70 – 130 30 60 – 140
Trichloroethene 5.4 30 70 – 130 30 60 – 140
1,4-Dioxane 3.6 30 70 – 130 30 60 – 140
2,2,4-Trimethylpentane 4.7 30 70 – 130 30 60 – 140
Heptane 4.1 30 70 – 130 30 60 – 140
Methylcyclohexane 4.0 30 70 – 130 30 60 – 140
1,1,2-Trichloroethane 5.4 30 70 – 130 30 60 – 140
Methyl isobutyl ketone 4.1 30 70 – 130 30 60 – 140
Toluene 3.8 30 70 – 130 30 60 – 140
Methylbutylketone 4.1 30 70 – 130 30 60 – 140
Tetrachloroethene 6.8 30 70 – 130 30 60 – 140
Chlorobenzene 4.6 30 70 – 130 30 60 – 140
Ethylbenzene 4.3 30 70 – 130 30 60 – 140
M,p-xylene 4.3 30 70 – 130 30 60 – 140
o-Xylene 4.3 30 70 – 130 30 60 – 140
Styrene 4.2 30 70 – 130 30 60 – 140
1,1,2,2-Tetrachloroethane 6.9 30 70 – 130 30 60 – 140
Cumene 4.9 30 70 – 130 30 60 – 140
n-Propylbenzene 4.9 30 70 – 130 30 60 – 140
4-Ethyltoluene 4.9 30 70 – 130 30 60 – 140
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Revision 22.1, 09/2011 Page 6-72
Volatile Organic Compounds
Reporting
Limit (ng)
Acceptance Criteria
ICAL (%RSD) ICV (% R) CCV (%D) LCS (%R)
1,3,5-Trimethylbenzene 4.9 30 70 – 130 30 60 – 140
1,2,4-Trimethylbenzene 29 30 70 – 130 30 60 – 140
1,3-Dichlorobenzene 6.0 30 70 – 130 30 60 – 140
1,4-Dichlorobenzene 6.0 30 70 – 130 30 60 – 140
1,2-Dichlorobenzene 6.0 30 70 – 130 30 60 – 140
1,2,4-Trichlorobenzene 7.4 30 70 – 130 30 60 – 140
Hexachlorobutadiene 11 30 70 – 130 30 60 – 140
Naphthalene 0.5 30 70 – 130 30 60 – 140
2-Methylnaphthalene 0.5 30 70 – 130 30 60 – 140
1-Methylnaphthalene 0.5 30 70 – 130 30 60 – 140
Acenaphthylene 5.0 30 70 – 130 30 60 – 140
Acenaphthene 5.0 30 70 – 130 30 60 – 140
Fluorene 5.0 40 60 – 140 40 50 – 150
Phenanthrene 5.0 40 60 – 140 40 50 – 150
Anthracene 5.0 40 60 – 140 40 50 – 150
Fluoranthene 5.0 40 60-140 40 50 – 150
Pyrene 5.0 40 60-140 40 50 – 150
For low volume applications (< 1L) the following VOCs can also be measured:
Volatile Organic Compounds Reporting Limit (ng)
Acceptance Criteria
ICAL (%RSD ICV (%R) CCV (%D) LCS (%R)
Chloroethane 16 30 70 – 130 70 – 130 60 – 140
Isopropyl alcohol 49 30 70 – 130 70 – 130 60 – 140
Carbon Disulfide 3.1 30 70 – 130 70 – 130 60 – 140
MTBE 22 30 70 – 130 70 – 130 60 – 140
Methyl Ethyl Ketone 59 30 70 – 130 70 – 130 60 – 140
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Revision 22.1, 09/2011 Page 6-73
Table 6.16.2 Internal Standard Recovery Limits
Table 6.16.3 Field Surrogate Recovery
Limits
Analyte CCV IS (%R) Sample IS (%R)

Analyte Accuracy (%R)
Bromochloromethane 60 – 140 60 – 140 1,2-Dichloroethane-d4 50 – 150
1,4-Difluorobenzene 60 – 140 60 – 140 Toluene-d8 50 – 150
Chlorobenzene-d5 60 – 140 60 – 140 Naphthalene-d8 50 – 150
Bromofluorobenzene 60 – 140 60 – 140
Table 6.16.4 Summary of Calibration and QC Procedures for Method TO-17 VI
QC Check Minimum Frequency Acceptance Criteria Corrective Action
BFB Tune check Before initial and daily calibration. Check is
valid for 24 hours.
SW – 846 tune criteria. Correct problem then repeat tune.
5-Point Calibration Prior to sample analysis. %RSD < 30% with 2 VOCs exceeding up to 40%RSD and
2 PAHS exceeding criteria
Correct problem then repeat Initial Calibration Curve.
ICV After each initial
Calibration Curve.
See table 6.16.1. 10% of the
compounds are allowed to exceed criterion.
Determine if the exceedence is due to
an inaccurate calibration standard or inaccurate ICV standard. Recalibrate
with an accurate standard or reprepare the ICV as necessary.
Continuing
Calibration Verification
(CCV)
At the start of each 24-hour clock after the Tune Check.

70-130% for VOCs. See Table 6.16.1
If project specified risk drivers exceed
this criteria, more than 5% of the compounds exceed this criteria, or any
VOC exceeds 50-150% recovery, maintenance is performed and the CCV
test repeated. If the system still fails the CCV, perform a new 5-point Calibration Curve.
Laboratory
Blank
After the CCV and before
the samples and at end of sequence
Results less than the laboratory
RL for Lab Blank analyzed prior to samples.
Inspect the system and re-analyze the
Blank.
Laboratory Control Spike
(LCS)
Once per analytical batch. 60-140% or 50-150% as noted in Table 6.16.1. 10% of
compound list may exceed criteria before corrective action is required.
Verify accuracy of standard and dry purge procedure. Re-prepare LCS if
necessary.
If calibration curve and/or system is
found to be out of control, perform maintenance and re-calibrate
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Revision 22.1, 09/2011 Page 6-74
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Laboratory Control Spike
Duplicate (LCSD)
Once per analytical batch –(reanalysis of LCS) <20%RPD Narrate exceedences. Evaluate system if more than 5% of the compounds
exceed criterion. Perform maintenance as required and re-calibrate as needed.
Internal Standard
(IS)
As each QC sample and
sample are being loaded.
CCVs: area counts 60-140%,
RT w/in 20 sec of mid-point in ICAL.
Blanks and samples: Retention time (RT) must be
within ±0.33 minutes of the RT in the CCV. The IS area must
be within ±40% of the CCV’s IS area for the Blanks and
samples.
CCV: inspect and correct system prior
to sample analysis.
Blanks: inspect the system and re-
analyze the Blank.
Samples: Investigate the problem by
verifying the instrument is in control by running a Lab Blank. Re-analyze
recollected samples to verify recovery. Report the run with acceptable IS
recovery. If both runs are unacceptable, narrate and flag
associated data.
Field Surrogates Added to each tube prior to shipment to field.
Added to QC samples prior to analysis.
50-150%

For blanks: inspect the system and re-analyze the Blank.
For samples: Review data to
determine whether sample collection parameters or matrix interference resulted in the exceedence. If so,
narrate and flag recovery. If no cause is evident, verify the instrument is in control by running a Lab Blank. Re-analyze recollected sample to verify
recovery.
Field Blank Project dependent. Artifact levels should be less than the reporting limit or less
than 10% of the mass measured on the sampled tubes,
whichever is less.
Flag associated results and evaluate tube conditioning and storage
procedures.
Distributed Pairs Project dependent. %RPD < 25%. Narrate discrepancy.

Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-75 6.17 PASSIVE SAMPLING ANALYZED BY THERMAL DESORPTION - VOLATILE
ORGANIC COMPOUNDS
This method involves GC/MS analysis of VOCs collected using passive samplers. These samplers are
used to measure vapor-phase VOCs in a variety of gaseous matrices including indoor air, outdoor air and soil gas. VOCs in the sampling environment pass through a diffusive barrier or permeable membrane at a
controlled rate and adsorb to the sorbent bed of the sampler. The sorbent is transferred to an empty tube,
if needed, and the tubes are thermally desorbed by heating and purging with UHP Helium. The resulting gaseous effluent is transferred to secondary trap for re-concentration and desorption onto the gas chromatograph equipped with a mass spectrophotometer. The retention time and spectral pattern of a
compound are compared with that of a known standard. Concentrations of the analytes are calculated from the average relative response factors of calibration curves obtained from analysis of standard
solutions. Results are reported in ng/sample or ug/m3 if the sampling rate and duration are known.
The analysis is performed using the analytical protocols of EPA Method TO-17. The only deviation from the TO-17 method is that the samples are collected using passive samplers as opposed to the method
defined procedure of using a pump to actively pull vapors through the sorbent.
Table 6.17.1. Summary of Method TO-17 Modifications
Requirement TO-17 ATL Modifications
Sample collection Active Passive
Table 6.17.2. Radiello 145
Analytes
Reporting Limit
(ng)
Acceptance Criteria
ICAL
(%RSD)
LCS
(% R) CCV
1,1,1-Trichloroethane 5.5 30 70 – 130 30
Benzene 5.0 30 70 – 130 30
Ethyl Benzene 2.2 30 70 – 130 30
m,p-Xylene 2.2 30 70 – 130 30
o-Xylene 2.2 30 70 – 130 30
Tetrachloroethene 3.4 30 70 – 130 30
Toluene 1.9 30 70 – 130 30
Trichloroethene 2.7 30 70 – 130 30
1,1-Dichloroethene 4.0 30 70 – 130 30
Carbon Tetrachloride 6.3 30 70 – 130 30
cis-1,2-Dichloroethene 2.0 30 70 – 130 30
Styrene 4.2 30 70 – 130 30
trans-1,2-Dichloroethene 2.0 30 70 – 130 30
Vinyl Chloride 1.3 30 70 – 130 30
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Revision 22.1, 09/2011 Page 6-76
Analytes
Reporting
Limit (ng)
Acceptance Criteria
ICAL (%RSD) LCS (% R) CCV
1,1,2-Trichloroethane* 5.4 30 70 – 130 30
1,1-Dichloroethane* 2.0 30 70 – 130 30
1,2,4-Trimethylbenzene* 4.9 30 70 – 130 30
1,2-Dichloroethane* 2.0 30 70 – 130 30
1,3,5-Trimethylbenzene* 4.9 30 70 – 130 30
Chloroform* 4.9 30 70 – 130 30
Cyclohexane* 3.4 30 70 – 130 30
Heptane* 4.1 30 70 – 130 30
Tetrahydrofuran* 2.9 30 70 – 130 30
Internal Standards
Analyte CCV IS % Recovery Sample IS % Recovery
Bromochloromethane 60 – 140 60 – 140
1,4-Difluorobenzene 60 – 140 60 – 140
Chlorobenzene-d5 60 – 140 60 – 140
Analytical Surrogate
Analyte % Recovery
4-Bromofluorobenzene 70 – 130
Compounds in bold indicate that the associated Sampling Rate is calculated. A “C” flag will be applied to these results, as they should be considered as estimated.
*Compounds require prior approval as a Sampling Rate has not been determined and additional laboratory set-up is required.
Table 6.17.3. Ultra III and SKC Badge
Analytes
Reporting Limit (ng)
Acceptance Criteria
ICAL (%RSD) LCS (% R) CCV (%R)
1,1,1-Trichloroethane 2.7 30 60 – 140 70 – 130
1,1-Dichloroethene 2.0 30 60 – 140 70 – 130
1,2-Dichloroethane 2.0 30 60 – 140 70 – 130
Acetone 24 30 60 – 140 70 – 130
Benzene 16 30 60 – 140 70 – 130
Carbon Tetrachloride 3.1 30 60 – 140 70 – 130
Chloroform 2.4 30 60 – 140 70 – 130
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Revision 22.1, 09/2011 Page 6-77
Analytes
Reporting
Limit (ng)
Acceptance Criteria
ICAL (%RSD) LCS (% R) CCV (%R)
cis-1,2-Dichloroethene 2.0 30 60 – 140 70 – 130
Cyclohexane 17 30 60 – 140 70 – 130
Ethyl Benzene 2.2 30 60 – 140 70 – 130
Heptane 20 30 60 – 140 70 – 130
Hexane 18 30 60 – 140 70 – 130
m,p-Xylene 2.2 30 60 – 140 70 – 130
Methyl tert-butyl ether 18 30 60 – 140 70 – 130
Methylene Chloride 35 30 60 – 140 70 – 130
o-Xylene 2.2 30 60 – 140 70 – 130
Tetrachloroethene 4.0 30 60 – 140 70 – 130
Toluene 4.0 30 60 – 140 70 – 130
trans-1,2-Dichloroethene 2.0 30 60 – 140 70 – 130
Trichloroethene 2.7 30 60 – 140 70 – 130
1,1,2,2-Tetrachloroethane 3.4 30 60 – 140 70 – 130
1,1,2-Trichloroethane 2.7 30 60 – 140 70 – 130
1,1-Dichloroethane 2.0 30 60 – 140 70 – 130
1,2,4-Trichlorobenzene 7.4 30 60 – 140 70 – 130
1,2,4-Trimethylbenzene 2.5 30 60 – 140 70 – 130
1,2-Dichlorobenzene 3.0 30 60 – 140 70 – 130
1,2-Dichloropropane 2.3 30 60 – 140 70 – 130
1,3,5-Trimethylbenzene 2.5 30 60 – 140 70 – 130
1,3-Butadiene 2.2 30 60 – 140 70 – 130
1,3-Dichlorobenzene 3.0 30 60 – 140 70 – 130
1,4-Dichlorobenzene 3.0 30 60 – 140 70 – 130
1,4-Dioxane 18 30 60 – 140 70 – 130
2,2,4-Trimethylpentane 23 30 60 – 140 70 – 130
2-Hexanone 20 30 60 – 140 70 – 130
4-Ethyltoluene 2.5 30 60 – 140 70 – 130
Butane 12 30 60 – 140 70 – 130
Carbon Disulfide 32 30 60 – 140 70 – 130
Chlorobenzene 2.3 30 60 – 140 70 – 130
Chloroethane 5.3 30 60 – 140 70 – 130
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Revision 22.1, 09/2011 Page 6-78
Analytes
Reporting
Limit (ng)
Acceptance Criteria
ICAL (%RSD) LCS (% R) CCV (%R)
Cumene 2.5 30 60 – 140 70 – 130
Ethanol 9.4 30 60 – 140 70 – 130
Freon 11 2.8 30 60 – 140 70 – 130
Freon 113 3.8 30 60 – 140 70 – 130
Hexachlorobutadiene 11 30 60 – 140 70 – 130
Isopentane 15 30 60 – 140 70 – 130
Methylcyclohexane 20 30 60 – 140 70 – 130
Naphthalene 5.2 30 60 – 140 70 – 130
Propylbenzene 2.5 30 60 – 140 70 – 130
Vinyl Chloride 1.3 30 60 – 140 70 – 130
Internal Standards
Analyte CCV IS % Recovery Sample IS % Recovery
Bromochloromethane 60 – 140 60 – 140
1,4-Difluorobenzene 60 – 140 60 – 140
Chlorobenzene-d5 60 – 140 60 – 140
Analytical Surrogate
Analyte % Recovery
4-Bromofluorobenzene 70 – 130
Note: Compounds in bold indicate that the associated Indoor and/or Outdoor Sampling Rate is calculated. A “C” flag will be applied to these results, as they should be considered as estimated.
Table 6.17.4 WMS Samplers
Analytes
Reporting Limit (ng)
Acceptance Criteria
ICAL (%RSD) LCS (% R) CCV (% R)
1,1-Dichloroethene 2.0 30 70 – 130 70 – 130
Acetone 48 30 70 – 130 70 – 130
Methyl tert-butyl ether 1.8 30 70 – 130 70 – 130
trans-1,2-Dichloroethene 2.0 30 70 – 130 70 – 130
Hexane 18 30 70 – 130 70 – 130
1,1-Dichloroethane 2.0 30 70 – 130 70 – 130
2-Butanone (Methyl Ethyl Ketone) 59 30 70 – 130 70 – 130
cis-1,2-Dichloroethene 2.0 30 70 – 130 70 – 130
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Revision 22.1, 09/2011 Page 6-79
Analytes
Reporting
Limit (ng)
Acceptance Criteria
ICAL (%RSD) LCS (% R) CCV (% R)
Chloroform 2.4 30 70 – 130 70 – 130
1,1,1-Trichloroethane 2.7 30 70 – 130 70 – 130
Cyclohexane 1.7 30 70 – 130 70 – 130
Carbon Tetrachloride 3.1 30 70 – 130 70 – 130
Benzene 16 30 70 – 130 70 – 130
1,2-Dichloroethane 2.0 30 70 – 130 70 – 130
Heptane 20 30 70 – 130 70 – 130
Trichloroethene 2.7 30 70 – 130 70 – 130
4-Methyl-2-pentanone 20 30 70 – 130 70 – 130
Toluene 19 30 70 – 130 70 – 130
1,1,2-Trichloroethane 5.5 30 70 – 130 70 – 130
Tetrachloroethene 3.4 30 70 – 130 70 – 130
Chlorobenzene 2.3 30 70 – 130 70 – 130
Ethyl Benzene 2.2 30 70 – 130 70 – 130
m,p-Xylene 22 30 70 – 130 70 – 130
o-Xylene 22 30 70 – 130 70 – 130
Styrene 4.3 30 70 – 130 70 – 130
1,1,2,2-Tetrachloroethane 3.4 30 70 – 130 70 – 130
Propylbenzene 25 30 70 – 130 70 – 130
1,3,5-Trimethylbenzene 4.9 30 70 – 130 70 – 130
1,2,4-Trimethylbenzene 4.9 30 70 – 130 70 – 130
1,3-Dichlorobenzene 6.0 30 70 – 130 70 – 130
1,4-Dichlorobenzene 6.0 30 70 – 130 70 – 130
1,2-Dichlorobenzene 8.0 30 70 – 130 70 – 130
Naphthalene 20 30 70 – 130 70 – 130
Internal Standards
Analyte CCV IS % Recovery Sample IS % Recovery
2-Fluorotoluene 60 – 140 60 – 140
Surrogates
Analyte % Recovery
4-Bromofluorobenzene 70-130

Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 6-80 Table 6.17.5 Summary of Calibration and QC Procedures for Method TO-17 (Volatile Organic
Compounds)
QC Check
Minimum
Frequency
Acceptance
Criteria
Corrective
Action
BFB Tune Check Every 24 hours

SW - 846 tune criteria. Correct problem then repeat tune.
5-Point Calibration Prior to sample Analysis. %RSD < 30%, 2 allowed out up to 40%

Correct problem then repeat Initial Calibration Curve.
LCS After each initial
Calibration Curve and daily prior to analysis.
Recovery 70-130% or as noted
in Tables 6.17.2 through 6.17.5.
Check the system and reanalyze
the standard. Re-prepare the standard if necessary. Re-
calibrate the instrument if the criteria cannot be met.
LCSD Each analytical batch Recovery 70 – 130% or as
noted in Tables 6.17.2 through 6.17.5; %RPD < 25%
If more than 5% target compounds
exceed criteria, evaluate system and recollection process. Correct
problem and reanalyze.
Continuing
Calibration
Verification (CCV)
At the start of each analytical clock 70 – 130 % If project specified risk drivers
exceed this criteria, more than 5%
of the compounds exceed this criteria, or any VOC exceeds 50-
150% recovery, maintenance is performed and the CCV test repeated. If the system still fails the CCV, perform a new 5-point
Calibration Curve.
Laboratory Blank After the CCV and at the end of the analytical
batch.
Results less than the laboratory RL. Inspect the system and re-analyze the Blank. No corrective action
for Lab Blank at end of batch.
Internal Standard (IS) As each standard, Blank, and sample is being loaded.
CCVs: area counts 60-140%, RT w/in 20 sec of mid-point in ICAL.
Blanks and samples:
Retention time (RT) must be within ±0.33 minutes of the RT in the CCV. The IS area must be within ±40% of the CCV’s
IS area for the Blanks and samples.
CCV: inspect and correct system prior to sample analysis.
Blanks: inspect the system and re-analyze the Blank.
Samples: samples cannot be re-analyzed due to the nature of the
sorbent cartridges. However investigate the problem by reviewing the data. If necessary, run a Lab Blank to check the
instrument performance. Report the data and narrate.
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Revision 22.1, 09/2011 Page 6-81
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Field Surrogates Each clean sample tube used for pumped sample
collection and lab blank and QC samples
50 – 150%. For blanks: inspect the system and re-analyze the Blank.
For samples: If no obvious reason can be ascertained after
evaluation of the data and sample collection parameters, the sample
should be reanalyzed to verify out of control recovery. If recovery is
out of acceptance criteria in both the primary and recollected
sample, the primary sample is reported with the surrogate
flagged.

Analytical Surrogate Each passive sampler and Lab Blank and QC
samples during sample desorption
70-130%. For blanks: inspect the system and re-analyze the Blank.
For samples: If no obvious reason can be ascertained after
evaluation of the data, the sample should be reanalyzed to verify out
of control recovery. If recovery is out of acceptance criteria in both the primary and recollected sample, the primary sample is
reported with the surrogate flagged.

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Revision 22.1, 09/2011 Page 6-82 6.18 VOST SW-846 5041A/8260B
This method involves GC/MS full scan analysis of volatile organic compounds in air samples collected on Tenax/Charcoal (VOST) cartridges. Samples are collected using SW-846 Method 0030/0031 Volatile
Organic Sampling Train (VOST) protocols. The VOST cartridges are thermally desorbed by heating and purging with Ultra High Purity Helium. The resulting gaseous effluent is then bubbled through 5 ml of
organic free reagent grade water and trapped on the sorbent trap of the purge and trap system. The trap is
then thermally desorbed for GC/MS analysis. For condensate analysis, a 5 ml aliquot of condensate sample is placed directly in the sparge vessel of the purge and trap (P&T) system and analyzed in a similar manner.
Certain compounds are not included in ATL’s standard target analyte list. These compounds are communicated at the time of client proposal request. Unless otherwise directed, ATL reports these non-
standard compounds with partial validation. Validation includes a 3-point calibration with the lowest
concentration defining the reporting limit, no second source verification is analyzed, and no method detection limit study is performed unless previous arrangements have been made. In addition, stability of
the non-standard compound during sample storage is not validated. Full validation may be available upon
request.
Air Toxics Ltd. performs a modified version of this method. The method modifications, standard target
analyte list, Limit of Quantitation, QC criteria, and QC summary can be found in the following tables.
Table 6.18.1. Summary of Method Modifications
Requirement EPA Method 5041A/8260B Air Toxics Ltd. Modifications
Method Blank Cartridges from the same media batches as
the samples.
Media batch is certified prior to use in the field. Method Blank is from a different batch
unless requested by the client.
Connection between thermal
desorption apparatus & purge vessel.
PTFE 1/16” Teflon
tubing.
Heated, 1/16” silica lined stainless steel
tubing.
Calibration Criteria for non-CCCs. RSD ≤ 15 % for all non-
CCCs.
RSD ≤ 30 % for Acetone, Bromoform, Vinyl
Acetate, Bromomethane, Chloromethane, 1,1,2,2-Tetracholoroethane, & 1,2,3-
Trichloropropane.
Table 6.18.2 SW-846 Modified Method 5041A Standard Analyte List
Analytes RL (ng)
Acceptance Criteria
ICAL (%RSD) LCS (% R) CCV
1,1,1-Trichloroethane 10 15 70 – 130 -
1,1,1,2-Tetrachloroethane 10 15 70 – 130 -
1,1,2,2-Tetrachloroethane – SPCC 10 30 70 – 130 RF > 0.30
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Revision 22.1, 09/2011 Page 6-83
Analytes RL (ng)
Acceptance Criteria
ICAL (%RSD) LCS (% R) CCV
1,1,2-Trichloroethane 10 15 70 – 130 -
1,1-Dichloroethane – SPCC 10 15 70 – 130 RF > 0.10
1,1-Dichloroethene – CCC 10 30 70 – 130 %D ≤ 25% VOST tubes;
≤20% condensates
1,1-Dichloropropene 10 15 70 – 130 -
1,2,3-Trichlorobenzene 50 15 70 – 130 -
1,2,3-Trichloropropane 10 30 70 – 130 -
1,2,4-Trichlorobenzene 50 15 70 – 130 -
1,2,4-Trimethylbenzene 10 15 70 – 130 -
1,2-Dibromo-3-chloropropane 50 15 70 – 130 -
1,2-Dichlorobenzene 10 15 70 – 130 -
1,2-Dichloroethane 10 15 70 – 130 -
1,2-Dichloropropane – CCC 10 30 70 – 130 %D ≤ 25% VOST tubes;
≤20% condensates
1,3,5-Trimethylbenzene 10 15 70 – 130 -
1,3-Butadiene1 50 30 50 – 150 -
1,3-Dichlorobenzene 10 15 70 – 130 -
1,3-Dichloropropane 10 15 70 – 130 -
1,4-Dichlorobenzene 10 15 70 – 130 -
2,2-Dichloropropane 50 15 70 – 130 -
2-Butanone2 50 30 50 – 150 -
2-Chloropropane 10 15 70 – 130 -
2-Chlorotoluene 10 15 70 – 130 -
2-Hexanone2 50 30 50 – 150 -
3-Chloropropene 50 15 70 – 130 -
4-Chlorotoluene 10 15 70 – 130 -
4-Methyl-2-pentanone2 50 30 50 – 150 -
Acetone2 50 30 50 – 150 -
Acrylonitrile 50 15 70 – 130 -
Benzene 10 15 70 – 130 -
Bromobenzene 10 15 70 – 130 -
Bromochloromethane 10 15 70 − 130 -
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Revision 22.1, 09/2011 Page 6-84
Analytes RL (ng)
Acceptance Criteria
ICAL (%RSD) LCS (% R) CCV
Bromodichloromethane 10 15 70 − 130 -
Bromoform − SPCC 10 30 70 − 130 RF > 0.10
Bromomethane2 10 30 50 − 150 -
Butylbenzene 10 15 70 − 130 -
Carbon Disulfide 10 15 70 − 130 -
Carbon Tetrachloride 10 15 70 – 130 -
Chlorobenzene – SPCC 10 15 70 – 130 RF > 0.30
Chloroethane 10 15 50 – 150 -
Chloroform – CCC 10 30 70 – 130 %D ≤ 25% VOST tubes;
≤20% condensates
Chloromethane – SPCC 10 30 50 – 150 RF > 0.10
cis-1,2-Dichloroethene 10 15 70 – 130 -
cis-1,3-Dichloropropene 10 15 70 – 130 -
cis-1,4-Dichloro-2-butene 50 15 70 – 130 -
Cumene 10 15 70 – 130 -
Dibromochloromethane 10 15 70 – 130 -
Dibromomethane 10 15 70 – 130 -
Ethylbenzene – CCC 10 30 70 – 130 %D ≤ 25% VOST tubes;
≤20% condensates
Ethylene Dibromide 10 15 70 – 130 -
Freon 11 10 15 70 – 130 -
Freon 12 10 15 50 – 150 -
Freon 113 10 15 70 – 130 -
Hexachlorobutadiene 50 15 70 – 130 -
Hexane 10 15 70 – 130 -
Iodomethane 50 15 70 – 130 -
Methylene Chloride 10 15 70 – 130 -
Methyl t-butyl ether (MTBE) 10 30 70 – 130 -
Naphthalene 50 15 70 – 130 -
m,p-Xylene 10 15 70 – 130 -
o-Xylene 10 15 70 – 130 -
p-Cymene 10 15 70 – 130 -
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Revision 22.1, 09/2011 Page 6-85
Analytes RL (ng)
Acceptance Criteria
ICAL (%RSD) LCS (% R) CCV
Propylbenzene 10 15 70 – 130 -
sec-Butylbenzene 10 15 70 – 130 -
Styrene 10 15 70 – 130 -
tert-Butylbenzene 10 15 70 − 130 -
Tetrachloroethene 10 15 70 − 130 -
Toluene – CCC 10 30 70 – 130 %D ≤ 25% VOST tubes;
≤20% condensates
trans-1,2-Dichloroethene 10 15 70 – 130 -
trans-1,3-Dichloropropene 10 15 70 – 130 -
trans-1,4-Dichloro-2-butene 50 15 70 – 130 -
Trichloroethene 10 15 70 – 130 -
Vinyl Acetate1,2 50 30 50 – 150 -
Vinyl Bromide1 (Bromoethene) 50 30 50 – 150 -
Vinyl Chloride – CCC 10 30 50 – 150 %D ≤ 25% VOST tubes;
≤20% condensates
1 Independent source verification check not available for these compounds. 2 Due to nature of these compounds, recoveries outside of noted limits do not result in re-calibration.
Table 6.18.3 Matrix Spike/Matrix Spike Duplicate
Analyte %R
1,1-Dichloroethene 60 – 140
Benzene 60 – 140
Trichloroethene 60 – 140
Toluene 60 – 140
Chlorobenzene 60 - 140
Table 6.18.4 Internal Standards
Analyte CCV IS (%R) Sample IS (%)R
1,4-Dichlorobenzene-d4 50 – 200 60 – 140
Chlorobenzene-d5 50 – 200 60 – 140
Fluorobenzene 50 – 200 60 – 140

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Revision 22.1, 09/2011 Page 6-86 Table 6.18.5 Surrogates

Analyte %R
4-Bromofluorobenzene 70 – 130
Dibromofluoromethane 70 – 130
Toluene-d8 70 – 130
Table 6.18.6 Summary of Calibration and QC Procedures for SW-846 Modified Method 5041A Note: These criteria are used specifically for the standard list of analytes listed in Table 6.18.2.
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Tuning Criteria Prior to calibration and at the start of
every 12-hour clock.
Method 5041A tuning criteria. Correct problem then repeat tune.
Initial 5-Point
Calibration
Prior to sample
analysis.
SPCC criteria in Table
6.18.2, CCC and non-CCC compound criteria in Table
6.18.2.
Correct problem then repeat initial
calibration.
Laboratory Control Spike (LCS) Once per initial calibration, and with
each analytical batch (maximum of 20 samples).
See Table 6.18.2. Investigate the problem and if warranted, analyze a new analytical curve for the
out-of-limits compound. (except for compounds noted in Table 6.18.2.)
Continuing Calibration Verification (CCV)
At the start of every shift immediately after the BFB tune check.
For SPCCs: see "CCV criteria" column
For CCCs: %D ≤ 25% for
VOST tubes and ≤ 20% for condensates.
Investigate and correct the problem, up to and including recalibration if necessary.
Internal Standards
(IS)
As each standard,
blank, and sample is being loaded.
For CCVs: area counts
50% - 200%, RT w/in 30 sec of mid-point in ICAL.
For blanks, samples and non-CCV QC Checks: area counts 60 – 140%, RT w/in 20 sec. of RT in CCV.
CCV: inspect and correct system prior
to sample analysis.
For blanks: inspect the system and re-
analyze the blank.
For condensates: re-analyze; if out
again, flag data.
For VOST: flag the data, evaluate
system and correct problem before proceeding.
Surrogates With all samples and QC. See Table 6.18.5. Same as for Internal Standards.
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Revision 22.1, 09/2011 Page 6-87
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Laboratory Blanks Immediately after
the calibration standard or after
samples with high
concentrations (≥ 5000 ng).
Results less than laboratory
reporting limit
Inspect the system and re-analyze the
blank.
Laboratory Control Spike (LCSD) One/analytical batch. RPD ≤25% Inspect the system and re-analyze; if out again, narrate.

(MS/MSD) Once/batch of condensate samples. See Table 6.18.3. Q-flag and narrate.

Air Toxics Limited Quality Manual
Revision 22.1, 09/2011 Page 7-1
7.0 DATA COLLECTION, REVIEW, REPORTING, AND RECORDS
7.1 DATA COLLECTION
All analytical results are generated from the instrument software. Data is acquired using a PC/Windows based platform. Data processing occurs on a UNIX based network system. Desktop
PCs configured with HP Chemstation software acquire the sample analysis results. Once the
acquisition is complete, a post-run macro automatically transfers the raw data files from the hard drive of the acquisition PC to the UNIX server. The UNIX server is a HP D390 server with a full
RAID system. This fault tolerant server is configured to manage hot-swappable hard drives and
memory cards to avoid any serious downtime. This server is configured with HP-UX 10.2, Thermo Lab Systems Target Software, and Omniback software.

All sample data is stored and processed on the UNIX server. Access to this server is limited based on the privileges associated with the users’ passwords. Only the Systems Administrator and the IT
Manager maintain full access to the system (which includes exclusive privilege for the adjustment of
acquisition station clock times). The system servers are physically located in a secured office, which is locked during off-hours. The data stored on the UNIX server is backed up nightly, weekly, and
monthly using a modified grandfather-father-son (GFS) backup rotation. All permanent backup tapes are stored in a secure fireproof safe.
Data reduction of analytical files is accomplished using Thermo Lab Systems’ Target software, which allows for complete traceability of the data results. Additionally, multiple permanent records of the
data reduction files are maintained through the data back up procedures, minimizing the threat of any
lost data trail evidence. Chemists must login to the data reduction software using a unique password in order to access and work with the sample data files. Once the bench chemists have successfully
logged-in to the working environment, all of their activities are tracked and logged by the Target
software’s electronic assessment trail. The assessment trail file is a tamper proof record of each event that occurred with the data file. The assessment history for a data file contains:

• Date of Change
• Time of Change
• Name of User who made the Change
• Parameter Changed
• Old Value
• New Value
• Reason for Change (if applicable)
The assessment trail file is completely secure within the Target software and cannot be modified or
deleted by any user. A hardcopy of the sample assessment trail can be provided upon request for
specialized data validation packages. Whenever an electronic raw data assessment is requested, the assessment trail file is automatically included.
Once data reduction is complete, the Scientist or Analyst transfers a copy of the sample results file along with all associated batch QC results into the laboratory’s SQL database from which reports are
ultimately generated.
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7.2 DATA REVIEW
Following analysis, the chemist verifies that the computer generated data reduction is correct using the Data Review Checklist (Exhibit 7.2). There are four categories of data review performed in the
laboratory.
These categories include:
I Analytical review is performed by the chemist. This review includes a review of raw data,
verification of all method and project specific QC
requirements, the addition of data qualifier flags when needed, and documentation of any unusual circumstances on the Data Review Checklist.

II. Technical review is performed by the Scientist or designated personnel who have demonstrated proficiency. This is the same type of review performed in Category I, however, it may be
performed either by the same person that performed the analysis or by a second individual if
specified by the project profile.
III. Report review represents a 3rd level of review which is required for DoD and client specific projects only. This is a review to ensure the accuracy of the standard report in PDF format. Data integrity surveillance checks are performed at this level.
IV. QA review is performed by the quality assurance department.
7.3 FINAL REPORT PRODUCTION
This review is similar to that performed in Categories I and II, however is done with an emphasis on overall quality of the data
and verification that standard quality assurance systems are functioning. Data integrity surveillance checks are performed at this level.

Category I is performed on every data package. Some clients request that 100% of their final data packages undergo a Technical peer review. The review in this case is performed by the Laboratory
Manager, QA personnel, or designated personnel. Technical peer review (Category II), must be
performed by a different individual than the original analyst, even when that person has the classification of scientist or higher. A request for Technical peer review shall be documented in the
project profile. Report review (Category III) is performed for DoD and client specific projects.
Report review must be performed by a different individual than the original analyst. Clients requesting 100% QA review of their data packages receive category IV review.

7.3.1 Automatic Data Transfer (ADT) System
Most data reports are created using ADT from the analytical instrument to a custom-reporting
module. Approved Analysts/Scientists on each team review the raw data at the instrument and then
transfer a copy of the sample results file electronically through a network server to the main database. Once in the database, the data results are automatically formatted into pre-designed method templates
using the reporting module. The method templates are designed at by the Project Management Team, associated with the samples at sample login and a review copy is e-mailed for client approval prior to reporting. Analysts/Scientists on each analytical team, batch samples results with QC results and any
additional information for any sample duplicates or re-analysis.
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7.3.2 Manual Data Entry System
Results that cannot be reported using the ADT system are manually entered into a validated, pre-programmed EXCEL spreadsheet. The final report is thoroughly reviewed by an approved team
member. 7.3.3 Report Compilation
Data reports are designed to include all necessary information which would be required for
traceability including:

• Analytical laboratory name, address, and phone number
• Name and address of the client
• Project name or number (title)
• Total number of pages
• Sample field I.D. number
• Laboratory I.D. number
• Receipt pressure (if applicable)
• Dates of collection and receipt
• Date of extraction (if applicable)
• Date and time of analysis
• Applicable method reference
• Instrument number
• Analytical run file name
• Analyte list
• Dilution factor
• Reporting Limit
• Amount detected in units specified
• Surrogate percent recovery
• Laboratory Director signature
• Chain-of-Custody Record

Each report contains a comprehensive Laboratory Narrative which describes the number of samples received in that batch, any abnormal receipt conditions, any deviations from method specific hold
times, the analytical method used, any modifications taken by the lab to the referenced method, and
any deviations from standard protocol experienced during sample receiving and analysis. Expected and unexpected deviations that may occur during the analysis of the samples are contained in
template format. The Narrative is unambiguous and clearly defines both the nature and substance of the variation.
The QA Manager is responsible for creating, and publishing the templates on a secured and shared network drive. The laboratory staff copies appropriate portions of the template into the Laboratory Narrative document. This approach standardizes the language used in the narratives. The narrative is
reviewed using the check sheet in Exhibit 7.2.
The final report is compiled in such a fashion that each subsection is unambiguous and inseparable
from the body of the report. A unique page number appears on every page of the report. The
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estimated uncertainty of the test results may be included on the report at client request (see Section
8.4). After all QC results have been reviewed and any deviations from the acceptance criteria are noted in
the Laboratory Narrative section of the report, the Laboratory Director, Technical Director, Laboratory Manager or Scientists/Analysts who are approved by the QA Department for relevant
analytical procedures may apply an electronic signature to the final reports. The electronic signature
on the report cover page means that the signatory accepts responsibility for the accuracy and completeness of the data generated. The approved signatory corresponds to the Chief Executive
Officer/Technical Director. The QA Manager keeps a log of the approved applicators of electronic
signature to final reports, and ensures that each applicator has the necessary education and experience.

Application of the electronic signature will automatically lock the Work Order thus preventing changes to the original report. If amendments are required due to omissions, errors or additional
requests a Work Order reissue is initiated. All reissues receive a unique Work Order number to distinguish them from the original issue. Reissued reports require a reason for the reissue and date of the reissue in the Laboratory Narrative. The laboratory maintains all supporting documentation for the
revision including corrections, additions, or deletions relative to the original report. 7.4 ELECTRONIC DATA REPORTING

ATL standard format Electronic Data Deliverables (EDD) are automatically created in the ATLAS database and sent with the final report. The ATL standard EDD format is delivered in Excel (.xls)
format and reports the same units as the final report. Examples of the fields for this EDD are summarized in Table 7.1.
The Lumen EDD software allows the user to create more complex custom/client-specific EDD formats. The Lumen EDD software uses the data from the SQL database for these deliverables, while allowing the users to add custom fields when necessary. The laboratory can produce ERPIMS,
GIS/Key, GeoTracker, and EQUIS deliverables, as well as other client-specific formats. 7.5 ECVP REPORTING IN ADOBE FORMAT
eCVP refers to the electronic conversion of laboratory data compiled as a Comprehensive Validation
Package in Adobe Acrobat Portable Document Format (.pdf) and archival onto a network drive. The
eCVP simultaneously meets the requirements of a Level III or IV Data Validation Package. Adobe Corporation’s .pdf documents are an exact replica of the original. Adobe Acrobat .pdf provides a
convenient way to view and print images at high resolution. The pdf is a compilation of data from
several internal systems including the raw data reports and the data reports created by Air Toxics Ltd, as well as client documents such as the COC. Each page is numbered and a table of contents given,
as well having each section bookmarked within the .pdf document. The .pdf document is archived on
a network drive and uploaded to a secure Web portal where the client will have access to it using a private username and password provided by ATL. Exhibit 7.1 is an example Table of Contents for an
eCVP package.
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Table 7.1. ATL DISKETTE DELIVERABLE STANDARD FORMAT
FIELD NAMES FORMAT WIDTH
LABSAMPLEID CHAR 15
LABCODE CHAR 3
MATRIX CHAR 3
METHOD CHAR 10
CLIENTSAMPID CHAR 15
SAMPDATE DATE 8
ANALDATE DATE 8
ANALTIME TIME 4
LABCTLID CHAR 8
DILUTION NUMBER 5
REPLMT NUMBER 5
UNITS CHAR 4
RESULTS NUMBER 5
DATAFLAGS CHAR 2
REPLMT (uG/m3) NUMBER 5
UNITS (uG/m3) CHAR 4
RESULTS (uG/m3) NUMBER 5
DATAFLAGS (uG/m3) CHAR 2
COMPOUND NAME CHAR 40
CAS# CHAR 12
COMMENTS CHAR 50

LABSAMPLEID: Sample identifier assigned by ATL.
LABCODE: Laboratory identifier (ATL). MATRIX: Sample Matrix.
METHOD: Analytical method of analysis.
CLIENTSAMPID: Sample identifier from Chain of Custody. SAMPDATE: The date the sample was collected.
ANALDATE: The date the sample was analyzed.
ANALTIME: The time the sample was analyzed. LABCTLID: Laboratory batch number.
DILUTION: Dilution factor.
REPLMT: Detection limit for sample. UNITS: Reporting units of measure.
RESULTS: Parameter value or result. DATAFLAGS: Data qualifiers. COMPOUND NAME: The name of each compound analyzed.
CAS#: The CAS registry number for each compound. COMMENTS: General comments field.

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Exhibit 7.1. Example eCVP Cover Page

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7.6 RECORDS OF METHOD CAPABILITY

Prior to sample analysis, the laboratory must demonstrate the ability to meet method accuracy and precision objectives. This is accomplished through an initial multi-point calibration, analysis of four
consecutive second source check standards, and completion of a Limit of Detection (MDL) study.
The mean recovery for each target analyte must be within current laboratory generated control limits with regard to test and compound. Following this initial set-up, there is a continuing requirement for
the demonstration of method capability any time the equipment undergoes significant change, such as different column phase and different concentrator design. Records of these tests are kept for a period of at least 5 years.
There is also a requirement for personnel involved with sample analysis to demonstrate capability for
both initial and continuing method proficiency in the specific test method. Analyst/Scientist
Demonstration of Capability for the initial method proficiency is accomplished by analyzing any of the following:
• Analysis of four replicate second source check standards either on the same day or on four
consecutive days.

• Successful completion of an independent PT sample.

Demonstration of method proficiency must occur at least once per year to be considered current. Personnel whose demonstration of method proficiency has surpassed the one year criteria may
proceed with sample analysis however; their work must be reviewed by the Laboratory Manager or a designated peer until they have completed the continuing method proficiency and received approval by the QA Department. Analyst/Scientist Demonstration of Capability for the continuing method
proficiency is accomplished by analyzing any of the following:
• Analysis of four consecutive LCS either on the same day or on four separate days.
• A duplicate analysis paired with another Analyst’s or Scientist’s results that demonstrate
acceptable %RPD will be acceptable.
• Successful completion of an independent PT sample. The Demonstration of Capability for the initial and continuing method proficiency is considered
acceptable if the accuracy and precision objectives of the test method are met. Documentation of method proficiency including the relevant raw data summary is kept in each analyst’s/scientist’s
training record. Documentation must be kept for a period of 5 years. The ‘Demonstration of
Capability Certification Statement’ is completed each time a demonstration of method proficiency study is completed. See ATL’s SOP #87 for further details.

7.7 RECORD STORAGE
The laboratory has a system for record storage such that historical reconstruction of all activities can
be made. Raw data includes:
• Instrument run logs
• Instrument calibrations
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• Data acquisition files
• Assessment trails
• Manual and spreadsheet calculations
• Date of analysis
• Instrument used
• Sample chain of custody
• Analyst initials and date
• Data review checklists
• Corrective action reports

The laboratory also maintains files dealing with client correspondence. The ATLAS Client Contacts database stores the date and time of the contact along with the email body or a brief summary of the
conversation, and any decisions made affecting sample status. When a decision is made to proceed
with analysis of compromised samples, the contact is logged into the database and a note is made on the Sample Discrepancy Report. The electronic files are maintained for a period of at least 5 years.
Additional project management information stored includes:

• The Project Profile
• ATLAS Client contact database
• Correspondence relating to sample disposition
• Contracts
• SOWs and/or QAPPs
The laboratory maintains electronic reports, as well as supporting information including calibrations,
Limit of Detection (MDL) studies, logbooks, and SOPs for a minimum of 5 years. Records stored on electronic media are supported by both hardware and software necessary for retrieval. If the laboratory changes ownership, then responsibility for file storage transfers to the new entity. If the
laboratory were to close its doors entirely, then allowance would be made to return files to those clients who contact the laboratory within 30 days of when notice is given. Under either scenario, the
transfer of ownership notice would be provided to clients through the NELAP national database and
on the ATL web page.
The record keeping system allows for historical reconstruction of all laboratory activities from sample
receipt to reporting. The record system includes:
• The identity of personnel involved in sample receiving, preparation, calibration, and analysis.
• A log of names, initials, and signatures for individuals who are responsible for signing or initialing any laboratory record.

• A unique identifier for each piece of equipment used.

• Initials and date for responsible staff at each step in the analytical process.
• Direct, prompt, and legible manual recording in bound logs using permanent black ink.
• Entries in logs that are not obliterated by erasures, over-writing, or markings. All corrections are made by single line strike out of the error followed by the correct entry if applicable. Each strike
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out is initialed and dated by the person making the correction and the reason for the correction is
documented for corrections due to reasons other than transcription errors. Any items, such as computer generated logs or spreadsheets that are pasted into the bound logbook, have initials and date appearing across the item boundary in such a fashion that removal is apparent.

• Records generated by a computer have either hardcopy or write protected back-up copy.

• The QA Department creates and tracks all logbooks throughout their lifetime. Each logbook
contains a new logbook request form which is filled out by laboratory personnel and submitted to
the QA Department. QA personnel create the logbook by first entering the new logbook into the Inventory Database. This database contains information such as the Book #, its Title, the
person’s initials and date that created the logbook, the start date, the date it was finished being used and the location of the logbook. Once the necessary information is entered into the database, the logbook is created and given to either the Laboratory Manager or the person that
submitted the request. When the logbook is completed or no longer in use, it is submitted to the QA Department. QA personnel update the Inventory Database with the finished date, the location and the logbook is archived.

7.8 CONFIDENTIALITY OF DATA
The data generated by analyzing a sample is considered to be the property of the entity appearing in
the “REPORT TO:” field of the Work Order request unless other contractual arrangements have
been made. Accordingly, that data is treated as confidential information and released only to that client, as identified by associated contractual agreements unless written permission is given to
proceed otherwise. All data generated under NELAP related fields of testing shall be made available to recognized agents of any laboratory accrediting authority for purposes of inspection and verification during an onsite visit. Clients will not be notified when the accrediting authority reviews
data during the normal course of the onsite assessment. Clients will be notified any time a request is made by the accrediting authority to remove copies of sample files, either electronic or hardcopy, from the laboratory. Client written approval must be arranged prior to removal of the files from the
laboratory unless the request is accompanied by appropriate court order. Both e-mail and facsimile data are treated as confidential by noting on the cover page:
“The information contained in this communication is confidential and intended only for the use of the individual or entity named above. Any other use, dissemination, distribution, or copying of this
communication is prohibited. If you have received this communication in error, please notify us by telephone and return the original message to us via US mail.”
Client confidentiality is observed in accordance with guidelines described in Section 5.10.7 TNI
Standard 2009 (EL-V1-2009):
“The laboratory shall ensure that, where clients require transmission of test results by telephone, telex, facsimile or other electronic or electromagnetic means, staff will follow documented procedures that ensure the requirements of this Standard are met and that confidentiality is preserved
as described in Section 5.4.7.”

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Exhibit 7.2. Data Review Checklist

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8.0 ESTABLISHING ACCEPTANCE CRITERIA
8.1 CONTROL CHART PROGRAM
Air Toxics Ltd. complies with guidance from ISO/IEC 17025:2005(E), Section 5.9, to determine quality control limits. This regulation suggests that statistical techniques may be used to detect trends,
but does not mandate acceptance or rejection of analytical results based on use of historically derived control limits. Additionally, NELAP does not address the issue of control charting. Therefore, in
accordance with ISO/IEC 17025:1999(E), Section 5.9, quality controls are in place to monitor
validity of tests and calibrations only.
Historically derived control limits are generated quarterly by the QA Department, or whenever a
procedure has been changed significantly. Control Limits may be updated less often (or not at all) for methods which are performed so infrequently that it is difficult or impossible to gather at least 20 data
points. These limits, however, are not used to validate data unless required by specific client request.
A complete description of the Control Chart program can be found in ATL’s SOP #48.
8.2 ESTABLISHING CONTROL LIMITS Control limits are generated from a minimum of 20 randomly chosen data points. The calculations
used to establish and update these investigative limits include:
Upper Control Limit = M +3S
Lower Control Limit = M -3S Upper Warning Limit = M +2S Lower Warning Limit = M -2S
Where:

M: The population mean recovery of at least 20 points, and S: The standard deviation of the population.

8.3 INTERPRETING CONTROL LIMITS
Calculated control limits based on historical data for Surrogate and LCS recoveries are used to demonstrate statistical control and display method variability, and are not used to qualify actual sample recoveries. Additionally, control limits may not be representative of the analytical process if
less than 20 points are generated for a given method. As a result, Air Toxics Ltd. uses the default
limits prescribed for each method in the corresponding SOP and Section 6.0 of this document. Historically derived control limits are used to evaluate LCS or Surrogate results only when requested
by clients or certifying agencies. 8.4 MEASUREMENT UNCERTAINTY
Upon request from a client (documented in the Project Profile), Air Toxics Limited will report measurement uncertainty for a given analyte reported by a specific method. Measurement uncertainty
is calculated as a function of historical LCS Control Limits (suggested by the American Association for Laboratory Accreditation Guide for Estimation of Measurement Uncertainty in Testing, July
2002). This policy is valid for environmental test methods in which measurement uncertainty is not
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defined. Uncertainty is estimated as a function of ± 2X the standard deviation (σ )of analyte percent
recovery derived from a minimum of 13 data points. Additional data points may be included in the calculation at the discretion of the laboratory. The data points may be Laboratory Control Sample
(LCS) results exclusively, or may be composed of a combination of Initial Calibration Levels (requantified as spikes), Initial Calibration Verification (ICV) and MDL replications (requantified as spikes). In practical application, 2X σ of the mean recovery is transformed into a percent of the
calculated mean. The calculated percentage representing 2X σ of the mean recovery is then applied to real sample results. For example, if 2X σ = 17% the limits of uncertainty would be represented on a
report as 0.83X to 1.17X (where X = the reported result).
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Exhibit 8.1. Control Chart

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9.0 PREVENTIVE MAINTENANCE
The best form of preventive maintenance is to have good, new stuff and a lot of it. If the customer expectations for quality, turn around time, and price are to be met, then the instrumentation must be
maintained in a fashion that supports the quality objective. The program is designed to adequately protect the laboratory from unexpected instrument failure and minimize scheduled instrument down
time. Preventive maintenance consists of an on-going program of routine maintenance, service
contracts, and a comprehensive inventory of spare parts.
All of the analytical instrumentation within the laboratory is serviced on a regularly scheduled
program. Preventative maintenance is performed at a minimum on a yearly basis.
9.1 ROUTINE MAINTENANCE
The Analyst/Scientist monitors instruments for potential failure on a daily basis. The analysis of
blanks and control standards at the start of the day and as analysis continues helps to provide real time
feedback to the Analyst/Scientist as well as the instrument support team on the condition of the instruments. Routine maintenance, specific to the various types of instruments, is covered in the
method SOPs. Any routine or major maintenance is documented in the bound maintenance logbook assigned to
each instrument. The date of the maintenance, work performed, and Analyst’s or Scientist’s initials are included.

If a malfunction occurs and control of the analytical system cannot be demonstrated using the QC parameters, discussed in section 4.3, the instrument is removed from production until analytical
control can again be demonstrated.
9.2 SERVICE CONTRACTS
Some analytical systems are covered under manufacturer service agreements. These agreements cover all forms of hardware failure and include regular hardware upgrades as needed. The response
time is guaranteed to be within 48 hours under the agreement and includes parts and labor.
Some contracts cover regularly scheduled routine maintenance. Leased instrumentation is similarly
covered by service agreements either through the leasing agency or directly with the manufacturer. In addition, the Technical Services group performs bi-annual (every six months) preventative
maintenance on the mass spectrometers. These records are kept in the individual instrument’s maintenance logbooks.
9.3 SPARE PARTS INVENTORY
A normal inventory of analytical consumable parts most frequently required is maintained in the
laboratory. These parts are typically not covered by the service agreements and may take several weeks to acquire on an as needed basis. An inventory is required to minimize instrument down time
and facilitate routine maintenance. An inventory of design parts is also maintained including:

• Stainless steel valves
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• Tubing
• Various connecting nuts and ferrules
• Tools
• Flow controllers
• Flow sensors
• Electrical connectors
• Sheet metal
• Miscellaneous items
• Multipliers and other MS source parts

The laboratory invests a significant amount of resources every year in lab/computer and research supplies.

9.4 CONTROL OF MISCELLANEOUS MONITORING, MEASURING, TESTING, AND DATA COLLECTION EQUIPMENT
In addition to the equipment used directly in the analysis of samples, ATL uses various other monitoring, measuring, testing, and data collection equipment. This equipment includes: analytical
balances and weight sets, pressure gauges, flow meters, fume hood testing devices, thermometers,
temperature and humidity recorders, mechanical volumetric devices, oven vacuum gauges, and sampling interface flow controllers. The procedures for ensuring the accuracy of the test equipment
are summarized in the following sections. Additional information can be found in ATL Certification of Test Equipment SOP, #34, and Refrigerator and Freezer Temperature Monitoring SOP #19.
9.4.1 Analytical Balances and Weight Sets
The analytical balances are certified and serviced once a year by an independent balance maintenance
company. A sticker is put on the side of the balance to indicate the date of certification and the company performing the certification. The certificates are maintained in the Quality Assurance (QA) Department. The certificate must indicate that the reference standards are traceable to NIST
standards and indicate the tolerances of the balance.
In addition, each time a balance is used; it is first checked with Class 1 weights. The weights used
must bracket the final amount being weighed. The result must be within acceptance criteria. If the acceptance criteria are not met, a Corrective Action Request (CAR) form is initiated and given to the
QA Department. The balance and/or weight set may require servicing to correct the problem.
Annually, all Class 1 weight sets are serviced and calibrated on-site against NIST-certified standards
by an independent calibration company. The certificate of calibration is maintained in the QA Department. The weights are kept in the manufacturer package that indicates the certification expiration date for the weight set. A sticker is put on the outside of the box to indicate the date of
certification and the company performing the certification.
9.4.2 Pressure Gauges
Pressure gauges are used to verify sample receipt pressures and for gaseous standard preparation. The measurement of pressure on the gauges used to pressurize canisters is relative. The readings are
used to assess the initial canister receipt vacuum/pressure and then pressurize the canister to a known
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pressure. The pressurization Technician compares the final vacuum/pressure recorded on the Chain-
of-Custody Record and/or sample tags by the field personnel with the receipt vacuum/pressure. If there is a discrepancy of more than 7"Hg/7psi a Sample Discrepancy Report is initiated and the client is notified.
In addition, the pressure gauges installed on the pressurization manifolds are re-calibrated and NIST certified on-site by an independent calibration company annually or as-needed. The certificates are
kept on file in the QA Department.
9.4.3 Fume Hood Testing Device
Quarterly, the Velocicheck Portable Air Velocity Meter is used by a member of the Safety Committee to check fume hood velocities. Velocities are checked in various quadrants of the hood at both full
open and half-open sash levels. Results of this check must be within specified limits and are recorded
in the Fume Hood Evaluation Logbook. If results are outside of these limits, the fume hood must be taken out of service until the problem is corrected.

Annually, the Velocicheck Portable Air Velocity Meter is calibrated on-site by an independent calibration company against NIST-traceable standards. The certificates of calibration are maintained
in the QA Department. 9.4.4 Thermometers
9.4.4.1 Reference Thermometers
ATL has NIST-traceable digital thermometers, which are used by the QA Department as reference devices. The thermometers are re-calibrated and certified annually by an independent calibration
company. A label indicating the date of calibration, the due date for the next calibration, and the
name of the company performing the certification is placed on the back of the thermometer itself. The reference thermometers are kept, along with certificates of calibration, in the QA Department.

9.4.4.2 Working Liquid-Filled (Ref/Freezer and Receiving) Thermometers
Thermometers used to record the temperature of refrigerator/freezers as well as of Temperature
Blanks (received with samples shipped on ice), are re-certified every year by the QA Department using the NIST-traceable digital thermometer as reference. The certification test is performed by
comparison to the NIST-traceable digital thermometer. Both thermometers (working and reference) are placed in a Dual Well Dry Block Calibrator (Model 9009 Hart Scientific). This instrument allows accuracy checks at both low and high temperatures.
The temperature range tested must correspond to the temperature range that the thermometer is used
to measure (i.e. approximately 4 ± 2°C for Refrigerator and Receiving thermometers and ≤ –10° C ±
5°C for Freezer thermometers). The results of this test are recorded in the Thermometer Calibration Verification logbook. The difference between the temperatures of the working thermometers and the
reference thermometer should be within the specified accuracy limits. Any thermometer that fails this
certification test is discarded and new replacements are purchased as needed.
The manufacturer provides the newly purchased thermometers with a calibration certificate. The QA
Department checks the new thermometers for defects (i.e., air bubbles present in red liquid column) before placing the new thermometers into use. A table containing the exact location, serial numbers,
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calibration and re-calibration due dates of each thermometer is kept in the Thermometer Calibration
Verification Logbook. 9.4.4.3 Oven and IS Station Thermometers
Temperature controllers used in the Canister Cleaning and Tube Preparation areas are verified on a
yearly basis by the QA Department to ensure that the proper temperature range is being achieved. The
test is performed using the NIST-traceable digital thermometer as a reference. The test consists of comparing the temperatures displayed by the ovens temperature controllers versus the temperature
measured by the reference thermometer.
The temperature range tested must correspond to the temperature range the thermometer is used to
measure (i.e. approximately 65 - 125 °C for Can Cleaning ovens). The temperature readings are
recorded in the Thermometer Calibration Verification logbook, which is kept in the QA Department. The accuracy limits used to compare the two readings are ± 5°C.
If the readings are outside of acceptance limits, a correction factor may be applied to the temperature
readings and maintenance or replacement of the controller may be necessary.
Temperature control used for desorption at the Internal Standard (IS) Loading Station in the main lab
(used for VOST and TO-17 analysis) is verified for accuracy prior to analysis using a NIST-traceable digital thermometer as a reference.
The temperature range tested must correspond to the temperature range the thermometer is used to
measure (i.e. approximately 100 °C for the IS station). The temperature readings are recorded in the instrument logbook. The acceptance limits are ± 10°C.
If the readings are outside of acceptance limits, a correction factor may be applied to the temperature readings and maintenance or replacement of the thermometer may be necessary.

9.4.4.4 Non-Contact Thermometers Non-contact thermometers are used to verify the temperature of the desorption plate used in the
analysis of VOST and TO-17 samples as well as to take the temperature of chilled samples which arrive without a Temperature Blank. These thermometers are certified against NIST-traceable
standards on-site by an independent calibration company on a yearly basis. Certificates of calibration
are maintained in the QA Department. 9.4.5 Temperature/Humidity Recorders
A Temperature/Humidity Recorder is used to verify that conditions required for PM10/TSP analyses
of filters have been met in the Desicator unit. The required conditions are a temperature of 59 to 86°F
+ 5 °F and humidity at 20 to 45 %RH ± 5% RH (≤ 50% RH ± 5% RH for TSP) over a 24 hour period.
These conditions are graphed, and every 7 days a replacement graph card is placed into the recorder by designated personnel. The date range recorded, along with the analyst’s initials, is noted on the back of the graph and filed in a folder next to the instrument. The recorder is re-calibrated and
certified annually by an independent calibration company. The certificates of calibration are kept on file in the QA Department.

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The Refrigerator used for the storage of VOST samples uses a Temperature Recorder in order to
verify required temperature has been maintained over holidays when the regular temperature checks are not performed (see ATL SOP #19 Refrigerator/Freezer Temperature Monitoring and Documentation). The temperature is graphed, and every 7 days a replacement graph card is placed
into the recorder by designated personnel. The date range recorded, along with the analyst’s initials, is noted on the back of the graph and filed in a folder next to the instrument. The recorder is re-
calibrated and certified annually by an independent calibration company. The certificates of
calibration are kept on file in the QA Department.
9.4.6 Flow Meters
Flow meters are used in the Laboratory to check the flow rates for VOST/TO-17 and other analyses,
and in connection with sorbent tube preparation. Canister Cleaning also uses flow meters to calibrate
flow controllers. These instruments are re-certified annually on-site by an independent calibration company against NIST-traceable standards. The certificates of calibration are kept in the QA
Department.
9.4.7 Mass Flow Controllers
The Mass Flow Controllers on the sampling interfaces are used as part of the Initial Calibration. Therefore, measurements made using them are relative in nature. The samples are introduced through
the very same process; therefore any potential bias is self-correcting. In addition, the accuracy of the Mass Flow Controllers is verified in four ways:

1) Each time the daily CCV is analyzed, the recoveries document the accuracy of the Mass Flow Controller with respect to the most recent instrument Calibration.

2) The linearity of the Calibration Curve demonstrates the accuracy of the Mass Flow Controller because the curve is developed using a mixture of syringe and Flow Controller standard loadings.

3) The accuracy of the Mass Flow Controller is verified through comparison of the new Calibration Curve with the previous Curve
4) In addition, the Mass Flow Controllers on the sampling interfaces are calibrated in house using a NIST certified flow meter before each Initial Calibration. They are calibrated by trained Analysts
and/or Scientists. This action is documented in the instrument logbook the day of the calibration which includes flow controller serial number, NIST flow meter expiration date, nominal value, actual value, verified/set by initials and date. The Laboratory staff oversees the Mass Flow
Controller certification program. The certificate of calibration for the NIST flow meter is kept in the QA Department.

9.4.8 Mechanical Volumetric Devices Mechanical volumetric devices such as solvent dispensers are verified for accuracy against a known
volume approximately once per month and never less than four times per year.
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9.4.9 Oven Vacuum Gauges
Each oven used by the Support Services Department to clean stainless steel canisters is equipped with a CONVECTRON vacuum gauge and controller. The accuracy of these gauges is checked approximately every 6 months or as needed.
A NIST certified CONVECTRON gauge and controller is mounted onto an empty port on the evacuation manifold by a member of the Support Services Department. The controller readings are
compared to the oven vacuum gauges and recorded into to the comment line of the oven logbook.
The NIST gauge and the oven gauge should match within ± 6 % (± 1.2 mTorr for a 20 mTorr reading) based on the manufacturer’s accuracy limits. If the 2 gauges do not match, then the oven vacuum
gauge controller is adjusted until the readings are the same, or the oven gauge is replaced/repaired.
Documentation of changes or repair is noted in the Canister Cleaning Maintenance Logbook. The NIST gauge is re-certified annually on-site by an independent calibration company and the certificate
of calibration is kept in the QA Department.

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10.1 NELAP/DOD PT SAMPLE PROGRAM
Proficiency testing (PT) samples are used to measure analytical accuracy, precision, and report completeness. To be accredited under NELAP and DoD-ELAP, the laboratory contracts with an
outside approved PT sample provider in each field of testing. Testing is limited by availability of samples that meet NELAP and DoD-ELAP criteria (noted below). The provider must be a NIST
accredited PT provider. It may be necessary to participate in more than one proficiency testing
program to be evaluated for multiple interdependent analyte groups. Currently there is no NELAP or DoD-ELAP accredited PT provider for air samples therefore, ATL participates in a PT program for
EPA Method TO-15 which is ISO 17025 compliant. Performance samples are processed through the
laboratory in the same manner as project samples. In each calendar year, the certified lab will complete at least two separate proficiency testing samples for each analyte or interdependent analyte
group. The following policies apply to laboratory PT sample analysis and reporting:

• The samples shall be analyzed and reported to the PT provider within 45 calendar days of receipt
or the specific deadline specified by the PT provider.
• The PT sample is received and logged into an electronic sample receiving database in the same fashion as field samples.

• The laboratory must follow the PT provider’s instructions for preparing the PT sample.

• The laboratory management and bench chemist ensure that the PT samples are prepared, analyzed and reported in the same fashion as field samples using the same staff, equipment, and methods.
• Initial and continuing calibrations for the PT sample are analyzed at the same frequency of field samples.

• The PT sample is analyzed with the same quality control samples as routine field samples.

• The PT sample cannot undergo duplicate or replicate analyses that would not ordinarily be
performed on field samples. The PT sample result cannot be derived from averaging the results of
multiple analyses unless specifically called for in the reference method.
• The PT sample can only be analyzed on equipment leased or owned by the company and handled only by bona fide employees of the company.
• The analysis of PT samples by temporary or contract employees is explicitly forbidden.
• The laboratory shall not subcontract any PT sample or portion.
• The laboratory shall not knowingly receive any PT sample or portion from another lab.
• The laboratory shall not communicate in any fashion with another laboratory concerning the PT sample or results.
• The laboratory shall not attempt to obtain the PT sample result prior to reporting.
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• The PT sample reporting forms provided by the sample provider will be used to report the results and will be maintained in the laboratory’s record system.

• The laboratory shall maintain copies of all written, printed and electronic records relating the
analysis or reporting of the PT sample for a period of 5 years or as required by the applicable
regulatory program.
• A CAR form will be generated any time an analyte result fails the proficiency testing assessment. A copy of the PT results is sent to the NELAP and DoD-ELAP accrediting agencies and
associated corrective action summary will be sent upon request.

• The lab authorizes provider to release any PT assessment information to the accrediting agency.

• The QA Manager must sign the PT results form and by so doing, attests that the sample was
analyzed and reported in the same fashion as a field sample and followed the PT provider instructions for preparation.
• The lab must notify its primary accrediting agency and any other agencies under reciprocity that it has enrolled with a particular PT provider.

• The lab must notify its primary accrediting agency and any other agencies under reciprocity in the
event it wishes to change PT providers.

• For each analyte or interdependent analyte group for which proficiency is not available, the
certified lab will establish, maintain and document the accuracy and reliability of its procedures through a system of internal quality management.

• Results of any failed PT samples are summarized in the Quarterly QA Status Report.

10.2 EXTERNAL (NON-NELAP/NON-DOD-ELAP) PT SAMPLES Occasionally proficiency testing samples are submitted along with field samples by private clients.
The lab processes and reports the samples in the same fashion as field samples. When the client notifies the laboratory that one or more analytes appear to have failed, the report is processed through
the normal Client Inquiry Corrective Action Process. The QA Manager will carry out an assessment
and investigation into the circumstances surrounding the proficiency results including aspects relating to how the client prepared the sample for submission. The outcome of the assessment will be
documented as per (Section 3.3.2) and maintained on file for a period of 5 years. Results of any failed
external PT samples are summarized in the Quarterly QA Status Report.
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Revision 22.1, 09/2011 Page 11-1 11.0 MANAGEMENT OF COMPUTER AND SOFTWARE SYSTEMS
Data are electronically captured from virtually all analytical instruments used by Air Toxics Limited.
A network of computers and servers is used for the acquisition, processing, manipulation, recording, storage, and retrieval of test data. The laboratory uses a variety of both commercial as well as proprietary software applications to acquire, process, and report sample results. This network of
computers is also used to receive and process customer information regarding field activities, sample disposition, and quality assurance objectives. Quality systems relating to the management of the
computers and software are designed to incorporate the standards established in the EPA Document “2185-Good Automated Laboratory Practices (1995)” wherever possible given the size and resources available in the laboratory and IT groups.

11.1 SECURITY
The systems of Air Toxics Ltd. are protected from unauthorized access through the use of both
physical and programmatic security measures. All of the laboratory servers are housed in a locked office, which maintains favorable environmental conditions to allow for optimal server performance.
Access to the laboratory’s networks is granted by the Systems Administrator or IT Manager. Network access is tightly controlled for the entire company. Users maintain individual network accounts and are allowed to access specific areas of the network based on the privileges assigned to
them. A user is granted access to only those areas needed to fulfill his/her job function. All software used to reduce sample data or generate sample reports is password protected; users are granted rights to these systems based on a read/write/none privilege system.
11.2 BACK UP AND STORAGE OF DATA
All data systems are backed up on a daily, weekly, and monthly basis using a modified grandfather-father-son (GFS) rotation protocol. Specifically, these back ups are conducted on the servers
responsible for all laboratory production data files and databases (i.e., Project Management files,
analytical data, audit trails, quality assurance documents, etc.). A daily incremental back up is scheduled to run each night Monday through Saturday. The daily incremental back up is limited to
files modified the same day. On Sunday, a weekly full back up of all files on each server is
completed. At the end of each month, a full back up of each data system is conducted. This monthly back up tape is then placed in permanent storage. The permanent historical back-up tapes are stored
in a offsite data storage facility. Data is not removed from the server until at least three permanent monthly back-up tapes have been created. This ensures that no archived data will be lost due to corruption of the magnetic tape. A more comprehensive description of the electronic data archiving
system can be found in ATL SOP #55, Electronic Archival of GC/MS Analytical Instrument Data.
11.3 SOFTWARE AND ELECTRONIC DATA VALIDATION

The IT Department is responsible for the testing and verification of all internally developed software applications. This includes: Developer Testing, Non-Production Testing, Validation, and where
needed, User Acceptance Verification. Documentation of changes made and of the associated testing is located with c.Support incidents. It should be noted that every change is different, and thus
differing levels of testing are needed for different issues. A minor change, such as a typo can quickly
be tested, whereas major coding changes like flagging changes or a new module require much more in-depth testing. The developer and tester will need to determine the depth of testing needed based on
the requirements of each specific change.
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of the change in the development environment, ensuring the code meets specifications. When it is determined that the change meets the design specification,
the developer will update the c.Support incident to document their testing and with any notes that the tester will need. The developer will then re-assign the incident to the tester and change the status of the incident to “Review”.
11.3.2 Non-Production Testing: The tester will evaluate the change by installing a test build and testing in a non-production environment on a different computer than the
developer tested on. The specified test user must be familiar with the process being
tested. The tester will attach documentation of the testing to the c.Support incident. They will then write notes to the developer in the Resolution section of the incident
as to whether the tests passed or if further development is needed.
11.3.3 Validation: Once the code has been approved in the test environment, the pre-release build must be validated in the production environment. Typically, this will mean that
the validator will use the test version of ATLAS but choose to use the production
environment. Documentation of validation will be attached to the c.Support incident. The validator will then write notes to the developer in the Resolution section of the
incident as to whether the validation passed, if the software is ready to be deployed, if further development is needed or if further verification is required. The validator will re-assign the incident to the developer or to a user, if additional verification is
needed.
11.3.4 User Acceptance Verification: In some cases, further user acceptance is needed. (If the issue was something minor such as a typo, this step will not be performed.
However, for complex changes, such as flagging, user acceptance will be required. This step is performed at the discretion of the validator and with approval of the
developer.) In these cases, 1-2 persons who use the feature on a regular basis will be
given the pre-release build. They will perform their typical job function, but verify that this feature is working correctly every time. They will notify the developer via
the c.Support incident whenever they find an issue. Once verification is completed,
user acceptance notes will be attached to the incident and notes placed in the Resolution section of the incident as to whether they approve the code or if further
development is necessary. The incident will then be re-assigned back to the
developer.
11.3.4.1 If no further development is needed, the developer will move on to the
implementation phase. If more development is needed, the developer will make the changes and then repeat the above steps until all issues are resolved.
11.4 IMPLEMENTATION

11.4.1 After testing is successful, an “ATL Software Development Change Control” form
must be filled out and submitted for approval. The tester must sign the form and make any necessary notes. The developer must also sign the form. For Critical and High Risk SCRs one of the following must also sign approval of the change: CEO,
President, a Director or Lab Manager. Once the form is complete, the developer keeps a copy and another copy is given to the IT Manager to archive.

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Revision 22.1, 09/2011 Page 11-3 11.4.2 Before putting a new application into production, the developer must make a copy of
the current version, append an original name with the built date and put the copy to the archive/backup folder.
11.4.3 The developer must also fill out the “Change Control Log”, located in the archival binder which resides with the IT Manager.
11.4.4 For the ATLAS2000 program, IT personnel will set-up the automatic update
procedure; for Lumen, and other programs, IT or designated personnel will install the new applications.
11.4.5 Once the application has been put into production, any issues found will be
documented in c.Support as Software Change Requests. It will determine if the issue is software or training related. If it is software related, the procedure in ATL SOP
#104, Software Change Control Procedures will be followed to correct the bug.
11.5 COMMERCIAL SOFTWARE DATA VALIDATION
Any commercial software application used for data reduction is verified for adequate performance before release to the production laboratory. The various testing stages and process for implementation
of internally developed software are described in ATL SOP #104, Software Change Control Procedures.
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Exhibit 11.1. ATLAS Incident Report

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Revision 22.1, 09/2011 Page 12-1 12.0 CONTROL OF PURCHASED ITEMS AND EXTERNAL SERVICES
The primary materials procured by the laboratory are computer hardware, analytical software,
standard office software, analytical instrumentation, certified standards, carrier gases and cryogens, miscellaneous laboratory supplies, NIST-traceable re-certifications, disposable sampling media (e.g., Tedlar bags), and service contracts.
Control of the purchase of these items and services is maintained using a standard purchase order
system detailed in SOP#105 that includes the following:

• A purchase request that is approved by a director or manager.
• An assigned purchase order (PO) number that is logged along with the date, vendor, and requester.
• A requirement that upon receipt or delivery of services, the product is inspected by the purchasing agent, and compared to the packing slip and/or request for services.
• An evaluation of the supplier against established performance criteria.
• Each PO is matched with invoices prior to payment to insure that purchased items or services
were delivered as expected. Critical vendors (those for whom a failure or lack of supply would cause irreparable damage to the
laboratory operations) are selected on the basis of either being the sole supplier of an item or as a result of reliable service over a several year period. A table of current critical suppliers is presented in Exhibit 12.1. An example of the criteria used to evaluate performance of critical vendors is
provided in SOP#105.
When reagents are purchased in bulk volume for laboratory use, each lot is certified for cleanliness
prior to use. A laboratory blank is prepared using the analytical reference method. The concentration of target species present must be less than the laboratory reporting limit for the lot to be certified
clean and approved for use. Once a lot is approved, the vendor will set aside stock sufficient for
several months for ATL use. The certificates of analysis are kept on file in the main analytical laboratory and each incoming shipment is monitored by the extractions area staff to verify that only
certified lot numbers are used in the processes. Solvent Certification Method
Methylene Chloride SW8270C Hexane TO-4 Water SW8260B/SW8270C
Each reagent is labeled with the date of receipt, date opened, and date of expiration. In the case of Methylene Chloride and Hexane, a 100 mL aliquot of the solvent is evaporated to 1 mL and analyzed
via method SW8270C or TO-4. In the case of reagent water, a reagent blank is prepared and analyzed via methods SW8260B (5 mL) and SW8270C (1 L). Only reagent grade water is used in the laboratory and is purchased in bulk lots as HPLC grade.
Cylinder gasses used as diluent gas for sample analyses are also certified for cleanliness. Each tank
of UHP Helium or Nitrogen is tested by filling a clean lab blank canister followed by analysis via
EPA method TO-14. All target species must be present at less than the reporting limit in order for the cylinder to be certified clean. Results of the analysis are posted on each cylinder and stored in
designated logbooks.
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NIST traceable standards are re-certified upon receipt. The standard is analyzed under the
appropriate method and compared to the existing inventory of standards. If the response of any target species is not within acceptance limits for a second source standard, the standard is considered to have failed. The vendor is then contacted to discuss the discrepancy and arrangements made to
replace the standard.
Exhibit 12.1 Critical Suppliers

VENDOR JUSTIFICATION
Air Liquide America Specialty Gases LLC Sole supplier/Reliable service over several years
Airgas Reliable service over several years
SKC West Inc. Sole supplier
Chromatography Research Supplies, Inc. Sole supplier
Scientific Instrument Services Reliable service over several years
Hamilton Reliable service over several years
Quantum Analytics, Inc. Reliable service over several years
R & D Glassware Reliable service over several years
Aldrich Chemical Company NIST Certified
Supelco Reliable service over several years
Valco Sole Supplier
VWR Reliable service over several years
Control Company Reliable service
Agilent Technologies Reliable service
Davis Calibration Laboratory Reliable service
Dickson Calibration Services Reliable service
Sierra Instruments Inc. Reliable service
Millipore/Mykrolis Reliable service over several years
Leco Corporation Sole Supplier

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Revision 22.1, 09/2011 Page 13-1 13.0 PROJECT MANAGEMENT SYSTEM
Any quality system, no matter how elaborate, and no matter how well documented, will fail unless the
customer expectation is effectively communicated. The ATL Project Management System describes
the critical pathways necessary to adequately ensure that the customer expectation is reviewed, committed to by top management, documented and communicated to the laboratory prior to sample
delivery. System elements include:

• Review of project specific documents
• Negotiations and variance requests
• Documentation of project requirements
• Documenting client discussions
• Project briefings
• Scheduling sampling media
• Tracking sample analysis and reporting
• Project follow-up
The Project Management System is defined in the ATL SOP #1. Following are brief descriptions of
the elements comprising project management systems.
13.1 REVIEW OF PROJECT SPECIFIC DOCUMENTS Clients document project requirements in requests for proposals, work plans, SOWs, or QAPPs. No matter how the details are documented, the project requirements must be reviewed to ensure that the
laboratory has sufficient staff, equipment, and capacity to meet project needs. Any document received from a client containing either contractual language, description of work, QA/QC criteria,
and/or deliverable requirements different from our Standard Terms and Conditions will be processed
as a proposal. When a proposal is received, an electronic Proposal File is started and routed through the Proposal Tracking System using the c.Support software. The Project Managers are provided with
technical support by the designated Project Chemist or personnel who review all relevant sections of
the proposals. The Laboratory Management is consulted for further information when needed.
Items to be reviewed include:
• Requested methods
• Adequate and documented training of appropriate personnel including Demonstration of
Capability
• Adequate instrumentation
• Target compound lists and reporting limits
• Quantity of samples
• Requested media and degree of preparation
• Media preservation requirements
• Holding time requirements
• Project specific QC
• Deliverable requirements
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• TAT requirements
• Insurance requirements
• Special billing and payment terms
• Data storage requirements
• Client financial status

The following flow chart (Exhibit 13.1) depicts how the proposal is distributed through the review process and project requirements are received and logged into a database. Each proposal is given a
unique identifier by the Project Manager. The Project Manager determines project feasibility, consulting with the Technical Director when necessary. The Project Manager reviews the document to determine whether or not the proposal contains methods, target compounds, or production demands
requiring additional review and delegates sections to the appropriate department. If necessary, the Project Chemist or designated personnel and IT Manager review the document for special project
requirements in the areas of:

• Quality assurance criteria
• Reporting criteria
• Unusual compounds
• Electronic deliverable criteria
• Unusual Media Requirements
• Unusual volume of samples

If the Project Chemist or designated personnel has any questions, which may affect production, then the Project Manager is notified and the proposal is sent to the Technical Director to determine the implications to the laboratory production throughput. If the proposal does not require method
development, and has unusual deliverables then it is sent to the Reporting team or designee to verify if ATL is able to meet client deliverable demands. The reviewer may suggest pricing adjustments
according to the client specific format difficulties. If the proposal does not require review by the
Reporting team, it is returned to the Project Manager. A variance table to be included with the proposal is created by the Project Chemist or designated personnel. The variance table may undergo
revision as per the result of discussion with the client.
The Contract specifications are reviewed by the Contract Administrator to evaluate the terms and
conditions of the proposal, including the following areas:

• Retention;
• Penalties;
• Sales and Use Tax Requirements;
• Insurance Requirements;
• Data Storage Requirements; and
• Payments Terms.
The Contract Administrator then reviews the proposal to determine the amount of credit to be established for the client. The amount will be based upon credit status (Dunn & Bradstreet) report, the
amount of the contract and past payment history with ATL.
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Revision 22.1, 09/2011 Page 13-3 Following review and comments, the proposal is returned to the Project Manager for final review and
pricing. The proposal is then entered into the ATLAS Quotes module for reference. If the bidding process is successful, the Project Manager will set up an active project, utilizing the proposal
documents and quote as references. Before media is shipped, a signed copy of the variance table must be scanned to the network. The Project Manager and Project Chemist or designated personnel are brought back at this time if negotiations of the variance table are necessary. The Project Manager
will complete the project profile, while the Project Manager creates a project requirement table using the approved variance table which is stored on the network drive. An example of project profile
appears in Section 3, Exhibit 3.3.
Before the final report is released a contract must be signed and filed. Once a contract is received, it is
documented in the contract log. The contract is then reviewed to compare the pricing and language to
the proposal. If there are exceptions made to the contract, these are noted and negotiated with the client. Once pricing and terms have been agreed upon, the contract is then executed and copies sent
back to the client. If the client needs to amend the contract after the project has started the contract
review process is performed for the amended contract. When changes to the contract affects any current procedures (i.e. invoicing, analysis, reporting) the appropriate personnel are notified via e-
mail and associated documents are updated. In addition, ATL will notify the client of any suspensions, revocations, or voluntary withdrawals of accreditation resulting from the amended contract.

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Revision 22.1, 09/2011 Page 13-5 Exhibit 13.1. Proposal Review Flow Chart (Continued)

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Revision 22.1, 09/2011 Page 13-6 13.2 NEGOTIATIONS AND VARIANCE REQUESTS
When the Project Chemist or designated personnel notes differences between the project request and laboratory standard protocol, the laboratory may request a variance from the requirements. Ideally,
variance requests occur during the proposal stage, but sufficient details regarding project
requirements are sometimes not known until sampling is about to begin. With the assistance of the QA team, the Project Chemist (or designee) notes all discrepancies in a variance table that is
submitted to the Project Manager. The assigned Project Manager communicates the discrepancies to
the client by submitting the variance table along with the proposal. Variance requests are most often handled directly between these parties. On occasion, a conference call may be held with an agency
representative or additional project and laboratory staff present. It is the responsibility of the Project Manager to coordinate the meeting.
Once an agreement has been reached and the variance table is approved by the client, the Project Manager will finalize the understandings concerning the discrepancies in a project requirement table,
which is used for sample login and analysis. The variance table and project requirement table are
given unique identifiers that reference the unique identifier assigned to the proposal. The tables are stored on a network-shared drive in read-only format until sample log in occurs.

13.3 DOCUMENTATION OF PROJECT REQUIREMENTS The Project Manager becomes the primary client contact following the project award. The Project
Manager will verify at that time that the client has been provided most recent version of the project plans. Any outstanding issues are discussed by phone and documented in the Client Contacts
database. At this time the project profile is updated to include:

• Shipping information
• Report To and Bill To information
• Pricing
• Reference method
• Requested media and degree of preparation
• Target compound list
• Special QA requirements
• Calibration criteria (if different from SOP)
• Deliverable requirements
• Account Information, including payment terms
• Variance table by reference
• Project Requirement table by reference
• Any special instructions
• Subcontracting (when relevant)
The project profiles are secured with read only privileges for all staff except the Project Managers and
Laboratory Management.
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Once a project has been awarded, the majorities of contacts occur via phone or e-mail and are documented in the Project Management software. The software can track contacts by client name,
project name, or date. Project Management team members may sort the database for summaries of
calls made on the basis of specific clients or sub-contracting entities.
13.5 DOCUMENTING CLIENT CONCERNS
Client concerns are documented in the Project Management software. Project Managers respond
quickly to address client concerns within 24 hours. Resolution of these concerns is also documented in the Project Management software. Concerns of a more serious nature are documented utilizing a Corrective Action Report procedure. These are maintained and by the QA Department. The Project
Manager will follow up with the client once the corrective action has been implemented and the report is closed.
13.6 SCHEDULING SAMPLING MEDIA
The ATL Project Managers work closely with clients to ensure that media is delivered according to
project schedule. Shipments for on-going projects are scheduled well in advance. The Project Managers are responsible for processing shipping requests through the Client Contacts database. This is the same database used to log phone contacts. Each shipping request is given a unique identifier.
Both laboratory staff and shipping staff monitor the database throughout the day for posted shipping requests.

Some media types (e.g., DNPH solutions, PUF/XAD cartridges, etc.) take time to prepare. Careful planning and scheduling on the part of both the Project Managers and the clients is necessary. Clients
are encouraged to provide as much lead-time as possible.
13.7 TRACKING SAMPLE ANALYSIS AND REPORTING
The sample tracking database is reviewed daily and provides the Project Manager with up-to-date information on sample status. Daily contact with the Team/Task Leaders or Laboratory Manager is
necessary when the rate of the production is less than desirable in any area. It is the responsibility of
the Project Manager to inform the client within 24 hours in the event that delays in analysis and reporting are anticipated and deviations from project requirement and/or contract agreements have
occurred. 13.8 PROJECT FOLLOW-UP
All contact with the client following reporting is handled by the Project Managers. This includes requests for re-issues, perceived problems with data, or further clarification. All discussions are
documented in the Client Contacts database within 24 hours. When a client desires a modification to a completed report, the Project Manager reviews the request. Commonly the Laboratory Manager
responsible for the work or the QA Manager may be consulted. If the request is considered to be
legitimate, the Project Manager initiates a request for report re-issue (per ATL SOP #68) in the Sample Tracking database. The database tracks the re-issue status to make sure that the report is
fixed and sent to the client. The reason for the re-issue is documented on the report cover along with
report re-issue date. It is the responsibility of the Project Manager to ensure that the correct reason and supporting documentation is provided in the report folder.

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14.0 DATA INTEGRITY PROCEDURES
14.1 TRAINING
Data integrity is the cornerstone of Air Toxics Limited. Our Mission Statement and Value Statement
define the goals and values which produce data of known and defensible quality. Everything from data reporting programs, employee retention programs to customer service programs evolve around
maintaining our core values above all else.

ATL Mission Statement
• To deliver high quality cost effective environmental analytical services
• That are profitable, on time and meet/exceed the expectations of our customers

How we go about accomplishing this mission is governed by our standards of conduct; the ability to discern right from wrong and proper from improper and the commitment to always do what is right, good and proper.
“We seek success in what we do, but not at the expense of integrity. Integrity is essential to establishing and maintaining the trust that allows us to work as a team and to foster confidence in
our customers and co-workers. Without integrity there can be no trust.”
Without integrity, our customers would not trust us to get the job done and would not hire us.
Employees would not trust management to set realistic goals and provide adequate resources. Without integrity, management would not trust employees with the ultimate form of empowerment…. direct
responsibility for customer satisfaction. All new employees are provided with introductory training which consists of:

Ethics and Integrity Training I The ATL Value Statement
The ATL Mission Statement Definition of Standards of Conduct and Ethics
ATL Strategic Goals Importance of Trust
Definition of Integrity Four basic enemies of integrity with workplace examples
Criminal ramifications for misconduct Benefits of Integrity Training
Role of the Employee (reporting systems) Role of Management (promote core values)
Where to find ATL Codes of Conduct Employee Handbook (employment standards)
Quality Manual (quality standards) SOPs (technical standards)
Chemical Hygiene Plan (safety standards)
A yearly refresher course is provided which reviews the basic information of Ethics and Integrity Training I but then goes on to define the critical steps in making ethical decisions:
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Ethics and Integrity Training II
1. Review relevant values and standards, devise a plan.
2. Question the plan, your motives and any consequences.
3. Resolve to address any ethical dilemmas by making touch choices.
Case studies are used in Ethics and Integrity Training II to encourage work group participation in
actual decision making scenarios. Following each training session, the employee is provided with a certificate for training and asked to sign the certificate indicating they have been informed of their obligations in the ATL integrity program and understand that legal ramifications may be imposed
upon them for failure to comply.
14.2 PERIODIC MONITORING

There are three parts to the ongoing periodic monitoring for inappropriate data manipulations following initial training. First, the IT Department has removed access to adjustment of data
acquisition and reporting computer clocks. Second, each new employee undergoes a training period in which all of their data is reviewed by a Scientist or Team/Task Leader until such time as basic knowledge and comprehension of method as well as data integrity procedures is demonstrated. A
development plan is provided to each new employee by their Manager or Team/Task Leader, which outlines goals, timelines and demonstration of understanding. The measurement of success may
include proficiency with a task as well as a verbal or written test demonstrating concept
comprehension.
When the Manager and/or Team/Task Leader determine the new employee is ready to produce data of
defensible quality, he/she is asked to provide several representative data packages to the Quality Assurance Manager for thorough review. If the QA Manager agrees that defensible data was
produced, the employee is released from the 100% review program.
The third and final part of the periodic monitoring program involves the use of proprietary in-house
data validation software to review every data point generated and to alert the reviewer when manual
integrations occur. The software is also programmed to report when an analyte in the initial calibration and QC samples does not meet established acceptance criteria. (Validation software
currently reviews all method TO-14A/TO-15, TO-17, ASTM D-5504, TO-3, TO-12 and SW8260B
results. Further software development is ongoing to bring more methods on line).
14.3 MECHANISMS FOR REPORTING INFRACTIONS
During Ethics and Integrity Training I, the new employee is informed how to go about
communicating any real or perceived infractions of the data integrity system. Open dialogue is
encouraged between the employee and any member of management or Senior Scientists they feel most comfortable with. It is management’s responsibility to relay the information to the Technical
Director(s) and follow-up with an inquiry or corrective action. The employee who desires to remain
anonymous is encouraged to report to the designated lab staff as ombudsman. The designated lab staff will meet separately with management and the employee involved to ensure anonymity. An
immediate inquiry by one of the Technical Directors will follow each and every reported incident.
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Documentation of the inquiry and subsequent disciplinary actions will be maintained by both the
Technical Director and the Human Resource Department for at least 5 years.
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Appendix A
DEFINITIONS AND TERMS
Accuracy: The degree of agreement between an observed value and an accepted reference value.
Analyte: The substance or thing for which a sample is analyzed to determine its presence or
quantity.
Approved: The determination by any state for federal accrediting agency that a certified laboratory
may analyze for an analyte under the specified method.
Assessment: The process of inspecting, testing and documenting findings for purposes of
certification or to determine compliance.
Batch: A group of analytical samples (≤ 20) of the same matrix processed together including extraction, concentration and analysis using the same process, staff and reagents.
Bag: Means an inert air-sampling container consisting of inert polymeric material.
Canister: A stainless steel spherical air-sampling device consisting of summa polished or glass lined
internal walls and a leak tight on/off valve.
Contamination: The effect caused by the introduction of the target analyte from an outside source into the test system.
Continuing Calibration Verification (CCV): A CCV is analyzed to verify instrument linearity with respect to the Initial Calibration. The CCV concentration may be identical to any given point contained within the initial calibration. A CCV is analyzed at the beginning of every analytical
sequence (all methods) and then once every ten or twenty samples depending on the method (GC and LC, GC/MS excluded). GC and LC methods also include a CCV in every analytical sequence as an
End Check.
Control Charts: These are statistical tools for monitoring the performance of a particular task on a
continuing basis. The control chart is prepared for each test parameter after 20 determinations have
been performed. The mean is plotted with the warning limits being ±2s and the control limits being
±3s. (s – standard deviation)
Corrective Action: An action taken to eliminate the causes of an existing nonconformity, defect, or
other undesirable situation in order to prevent recurrence. Data Reduction: A qualitative and quantitative evaluation of the documentation and procedures
associated with environmental measurements to verify that the resulting data are of acceptable quality.

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Appendix A (Continued)
DEFINITIONS AND TERMS
Detection Limit (DL): An estimate of the minimum amount of a substance that an analytical process can reliably detect. A DL is analyte and matrix-specific and may be laboratory dependent. The DL
may be determined by a Method Detection Limit study.
Duplicate Samples: Samples collected for checking the preciseness of the sampling process. These
samples are collected at the same time and from the same source as the study samples.
Equipment Blank: A sample that is known not to contain the target analyte that is used to check the
cleanliness of sampling devices, collected in a sampling container from a clean sample collection
device and retuned to the laboratory as a sample.
Field Blank: A sample that is known not to contain the target analyte and is used to check for
analytical artifacts or contamination introduced by sampling and analytical procedures, carried to the sampling site, exposed to sampling conditions and returned to the laboratory and treated as an
environmental sample. Field Duplicate: Samples collected at the same time from the same source, but submitted and
analyzed as separate samples.
Holding Time: The maximum time that a sample may be held prior to preparation or analysis.
Impinger: The glass vessel used to contain collection solution through which a stream of air is
bubbled for sampling purposes.
Initial Calibration: Demonstration of a linear response to different concentrations of calibration
standards within a defined range.
Initial Demonstration of Analytical Capability: The procedure described in the method 40 CFR
Appendix A, used to determine a laboratory’s accuracy and precision in applying an analytical
method.
Instrument Blank: A sample that is known not to contain the target analyte, processed through the instrumental steps of the measurement process used to determine the absence of instrument contamination prior to analysis of field samples.
Instrument Detection Limit (IDL): It is the concentration of the analyte that produces a signal
greater than five times the signal-to-ratio of the instrument.
Interference: The effect on the final result caused by the sample matrix.
Internal Standards (ISs): These are the measured amounts of certain compounds added after preparation or extraction of a sample.

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Appendix A (Continued)
DEFINITIONS AND TERMS
Key Personnel: The laboratory director, technical director, quality assurance manager, and team leader, all of whom meet the requirements of the NELAP rule.
Laboratory Control Sample: An independent second source reference standard which goes through he same pretreatment and preparation procedures as the samples. It validates the accuracy of the
initial calibration.
Laboratory Duplicates: Aliquots of the same sample that are prepared and analyzed at the same
time.
Limits of Quantitation (LOQ): the minimum levels, concentrations, or quantities of a target variable
(e.g., target analyte) that can be reported with a specified degree of confidence. Generally, the LOQ is
equal to the concentration of analyte(s) in the lowest point of a calibration (see Reporting Limit). Matrix: The component or substrate (e.g., surface water, drinking water, air, liquid waste) which
contains the analyte of interest. Matrix Spike: A sample prepared to determine the effect of the matrix on a method’s recovery
efficiency by adding a known amount of the target analyte to a specified amount of matrix sample for which an independent estimate of the target analyte concentration is available.
Matrix Spike Duplicate (MSD): Duplicates of the matrix spike sample.
Measurement Uncertainty: Measurement uncertainty is the estimation of potential errors in a
measurement process and is expressed as ± 2X (s) of the historical mean of LCS recoveries.
Method Detection Limit: The minimum concentration of a substance that can be measured and reported with 99% confidence that the analyte concentration is greater than zero as determined from
analysis of a sample containing the analyte in a given matrix (40 CFR Part 136, Appendix B, July
1995).
Practical Quantitation Limit (PQL): A synonym for the standard of lowest concentration contained
in the Initial Calibration. It is the smallest concentration of the analyte that can be reported with a specific degree of confidence.
Precision: The degree to which a set of observations or measurements of the same property, obtained under similar conditions, conform to themselves. Precision is usually expressed as standard
deviation, variance or arrange, in either absolute or relative terms. Preservation: The temperature control or the addition of a substance to maintain the chemical or
biological integrity of the target analyte.
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Appendix A (Continued)
DEFINITIONS AND TERMS
Proficiency Testing (PT) Assessment: The event including receiving, analyzing, and reporting of
results from a set of samples that a proficiency testing provider sends to a laboratory for the laboratory to demonstrate compliance with the proficiency testing requirements.
Proficiency Test (PT) Sample: A sample, the composition of which is unknown to the analyst and is provided to test whether the analyst/laboratory can produce analytical results within specified
acceptance criteria.
Quality Assurance: An integrated system of activities involving planning, quality control, reporting,
and quality assessment and improvement to ensure that the product meets defined standards of quality with a stated level of confidence. Quality Assurance Project Plan (QAPP): An orderly assemblage of detailed procedures designed to produce data of sufficient quality to meet the data quality objectives for a specific data collection
activity.
Reporting Limit: The smallest concentration of an analyte that can be measured with a stated
probability of significance. All Initial Calibrations contain a standard at the Reporting Limit. The
Reporting Limit is never less than the PQL.
Reporting Limit Verification: A re-quantification of the lowest concentration data point of an initial calibration to test the percent recovery of each component. Analyte recovery should be between 50-150% to verify detection limit accuracy.
Selectivity: The capability of a method or instrument to respond to the target analyte in the presence
of other substances or things.
Sensitivity: The capability of a method or instrument to discriminate between measurement responses representing different levels of a target analyte.
Standard Operating Procedures (SOP): A written document which details the steps of an
operation, analysis or action whose techniques and procedures are thoroughly prescribed, and is
accepted as the procedure for performing certain routine or repetitive tasks.
Surrogate: A substance which is unlikely to be found in the environment and which has properties
that mimic the target analyte and that is added to a sample to check for analytical efficiency. Target Analyte: The analyte that a test is designed to detect or quantify.
Technical Employee: A designated individual who performs the analytical method and associated techniques.
Trip Blank: A sample known not to contain the target analyte that is carried to the sampling site and
transported to the laboratory for analysis without having been exposed to the sampling procedures.

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Appendix B STANDARD OPERATING PROCEDURES

#1 Customer Support System
#2 Analysis of Volatile Organic Compounds in VOST Cartridges and Condensates by
Modified EPA SW-846 Method 5041A/8260B
#3 Analysis of Semi-Volatile Organic Compounds by Modified EPA SW-846 Method 8270C
#4 Preparation and Conditioning of VOST and CMS Tubes
#5 Analysis of Volatile Organic Compounds in Ambient Air Using Modified EPA Method
TO-17 with Modified EPA SW-846
#6 Analysis of Volatile Organic Compounds in SUMMATM Polished Canisters by Modified EPA Methods TO-14A/TO-15
#7 Preparation of SiloniteTM, SilcosteelTM, and SummaTM Canisters for Sampling
#8 Analysis of Oxygen, Nitrogen, Methane, Ethane, Ethene, Carbon Monoxide, Carbon
Dioxide, Hydrogen and NMOC by Modified ASTM Method D-1946
#10 Analysis of Semi-Volatile Organic Compounds Collected on PUF Cartridges by GC/MS Full Scan Modified EPA Method TO-13A
#11
Analysis of Aldehydes and Ketones by Modified EPA Methods TO-5 (Impingers), TO-
11A (Sep-Pak Cartridges), Modified SW-846 Method 0011/8315A (Impingers) and
Modified CARB 430 (Impingers)
#12 Extraction of Aldehydes and Ketones by Modified EPA Method TO-5 and Modified
CARB 430
#13 Analysis of Sulfur Compounds by ASTM Method D-5504
#14 Preparation of PUF and PUF/XAD-2 Media for Ambient Air Sampling and XAD-2
Media for MM5 Sampling
#15 Extraction of Ambient Air & MM-5 Samples for Semivolatile Analysis and
Pesticides/PCB Analysis by Modified EPA SW-846 Method 3542
#17 Safe Lifting Procedures
#19 Refrigerator/Freezer Temperature Monitoring and Documentation
#20 ATL GC Applications for Analysis of Organic Compounds in Air
#24 Storage and Disposal of Hazardous Wastes

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Appendix B (Continued) STANDARD OPERATING PROCEDURES
#25 Extraction of Aldehydes by Modified Methods 0011 and 8315A
26 Analysis of Pesticides and PCBs Collected on PUF Cartridges using Modified EPA Methods TO-4A/TO-10A
#27 Internal Audit Procedures
#30 Laboratory Security
#33 Standard Preparation, Validation, and Documentation
#34 Certification of Test Equipment
#36 Analysis of Non-Methane Organic Compounds (NMOC) Using Modified EPA Method
TO-12
#38 Analysis of Volatile Organic Compounds in SummaTM Polished Canisters by GC/MS Selective Ion Monitoring Modified EPA Methods TO-14A/TO-15
#39 Procedures to Perform an MDL Study
#42 Analysis of Air-Phase Petroleum Hydrocarbons (APH) in Ambient Air Using
Summa Polished Canisters
#43 Analysis of Benzene, Toluene, Ethylbenzene, Xylene and Total Petroleum
Hydrocarbons in Ambient Air Using Modified EPA Method TO-3
#44 Certification of Summa Polished or Glass-Lined Canisters used in the Analysis of
Volatile Organic Compounds
#45 Preparation and Review of Laboratory Narratives
#46 Writing and Updating Standard Operating Procedures
#48 Preparation and Review of Control Charts
#50 Receipt and Tracking of Samples
#52 Manual Peak Integration for GC/MS Analyses
#53 Tune Check Spectrum Generation
#54 Analysis of Natural Gases by Modified ASTM Method D-1945
#55 Electronic Archival of Analytical Instrument Data
#57 Manual Peak Integration - Gas Chromatography

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Appendix B (Continued) STANDARD OPERATING PROCEDURES

#59 Screening Samples Using GC/FID
#60 Canister Pressurization
#61 Corrective Action Procedure
#62 Preparation of 2,4-Dinitrophenylhydrazine (DNPH) Reagent for Use in Modified EPA
Methods 0011, TO-5, TO-11A, and CARB 430 Sampling Media
#63 Sample Custody Cage Logbook Documentation
#65 Extraction of Aldehydes by Modified EPA Method TO-11A
#66
Determination of Suspended Particulate Matter in the Atmosphere as Total
Suspended Particulates from Quartz Fiber Filters by 40 CFR Part 50 Appendix B;
Determination of Particulate Matter as PM10 from Quartz Fiber Filters by 40 CFR
Part 50 Appendix J
#68 Procedure to Reissue Finalized Data Reports
#69 Transfer of Sample Collected in a Tedlar Bag to a SummaTM Canister
#70 Preparation and Procedures for Flow Controller Assemblies
#71 Siloxanes in Air by GC/MS Direct Inject Analysis
#74 Analysis Of Polycyclic Aromatic Hydrocarbons by GC/MS Selective Ion
Monitoring (SIM) Modified EPA Method TO-13A
#78 Generation of Air Toxics Ltd. Data Deliverables, Electronic Conversion, and Archival
#79

Analysis of Volatile Organic Compounds in SMVOC Cartridges (Tenax®-GC and Anasorb® 747) and Condensates by Modified EPA SW-846 Method 5041A/8260B /0031
#83 Analysis Of Volatile Organic Compounds In SummaTM Polished Canisters by
GC/MS Low Level Modified EPA Methods TO-14A/TO-15
#87 Demonstration of Capability Procedure
#89 Media Management
#90 Subcontract Analysis
#91 Analysis Of Volatile Organic Compounds In SummaTM Polished Canisters by GC/MS
Modified EPA Methods TO-14A/TO-15 (5 & 20 ppbv)

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Appendix B (Continued) STANDARD OPERATING PROCEDURES
#92 Analysis Of Volatile Organic Compounds In Soil Gas Collected in Passivated
Canisters by EPA SW-846 Modified Method 8260B
#93 Method Editor Procedure
#94 Valid Values Editor and Compound Editor Procedure
#95 Client Canister Tracking System
#96 ATLAS ( Air Toxics Ltd. Automated System)
#97 Client Inquiry Procedure
#98 Instrument Set Up Procedure For New Gas Chromatography/Mass
Spectrometer(GC/MS) Or Relocating An Existing GC/MS
#99 Confidential Doucment Policy
#100 Analysis Of Volatile Organic Compounds Collected On Charcoal-Based Passive
Samplers
#101 Analysis of H2S, NO2, NH3, and O3 Collected on Radiello® Samplers
#103 The Determination of Aliphatic and Aromatic Volatile Petroleum Hydrocarbons (VPH) Fractions by GC/MS
#104 Software Change Control Procedures
#105 Purchasing
#106 Management Review System
#107 Initial Test Method Evaluation for Laboratory-Derived Methods and Modifications
#108 Procedural Use of Lumen
#109
Analysis of Volatile and Semivolatile Organic Compounds in Vapor by Thermal
Desorption GC/MS Full Scan/SIM Using EPA Method TO-17 - Vapor Intrusion
Application
#110 Measurement of Air-Phase Petroleum Hydrocarbons(APH) using Multibed Sorbent
Tubes and Thermal Desorption/GC-MS
#111 TPH, NMOC and Hydrocarbon Fractionation Calculation from Modified EPA Methods TO-14A/TO-15

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Appendix B (Continued) STANDARD OPERATING PROCEDURES

#112 Measurement of VOCs in Ambient Air Using Passive Samplers and Analysis by EPA
Method TO-17 TD-GC/MS
#114 TO-15 Sample Screening Using Sorbent Tubes and TD-GC/MS
#115 Dilution Operating Procedure For Vapor Samples

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REFERENCES

• Annual Book of ASTM Standards, American Society for Testing & Materials, 1991.

• EPA Compendium of Methods for the Determination of Toxic Organic Compounds in Ambient Air (First and Second Editions)

• EPA Compendium of Methods for the Determination of Air Pollutants in Indoor Air, Winberry et
al., Atmospheric Research and Exposure Assessment Laboratory, September 1989.

• Environmental Sampling and Analyses Lab Manual, Maria Csuros, Lewis Publishers, 1997.

• Test Methods for Evaluating Solid Waste, SW-846, Third Edition, Final Update III, Revision 1, December, 1996.

• Statement of Work for the Organic Superfund Contract Laboratory Program, OLM04.2 May, 1999.

• CLP Draft - Analytical Method for the Determination of VOCs in Air Collected in Summa Canisters and Analyzed by GC/MS, December 1991.

• Guidelines Establishing Test Procedures for the Analysis of Pollutants under the Clean Water Act 40 CFR (136) 1984.

• NIOSH Manual of Analytical Methods, Center for Disease Control, Fourth Edition, August, 1994.

• OSHA Analytical Methods Manual, U.S. Department of Labor, January, 1990.

• California Air Resources Board Stationary Source Test Manual, Monitoring and Laboratory Division, September, 1990.

• TNI Standard, Environmental Laboratory Sector, Volume I, Management and Technical Requirements for Laboratories Performing Environmental Analysis (EL-V1-2009).

• DoD Quality Systems Manual for Environmental Laboratories Version 4.2, October 25, 2010.
EMSL.FLAA.Lead Brief
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Controlled Document Confidential Business Information/ Property of EMSL Analytical, Inc
EMSL Analytical Brief
Determination of Environmental Lead by FLAA

_________________________________

Jeffrey W. Siria, Ph.D.
National Director of Lead
Summary of Method
The sample is digested with Nitric acid utilizing either a Hot Block™ or a hot plate. Depending upon the matrix,
Hydrochloric acid and/or hydrogen peroxide may also be utilized. The digestate is filtered and analyzed by
flame AA. This method provides procedures for the determination of lead by flame atomic absorption (FLAA)
in the following matrices:
• Dust Wipes. Only ASTM E 1792 approved dust wipes may be used for this method. This method is not
applicable to composite wipe analysis. The reporting limit for dust wipes by this method is 10µg; if area data is
provided, results may be reported in units of µg/ft.2. Note that reporting limits in units of µg/ft.2 are inversely
proportional to the wipe area; a wipe area of 36 in.2 will provide a reporting limit of 40 µg/ft.2.
• Paint Chips. When practical, paint chip samples should be isolated from substrate material. The reporting
limit for paint chips by this method is 0.010 % by wt. based upon a minimum sample wt. of 0.2 grams.
• Soils. This method is applicable to soils and some other solid materials such as construction debris. The
reporting limit for soils by this method is 40 mg/kg based upon a minimum dried sample wt. of 0.5 grams.
• Air. Only air samples collected on 0.8 µm mixed cellulose ester (MCE) membrane are applicable to this
method. The reporting limit (in total µg) for air samples by this method is 4µg; if air volume data is provided,
results may be reported in units of µg/m3. Note that reporting limits in units of µg/m3 are inversely proportional
to air volume; an air volume of 200 liters will provide a reporting limit of 20 µg/m3.
References
1. EPA Method SW 846-7420 Lead, Revision 0, September 1986.
2. Method for Chemical Analysis of Water and Wastes. EPA-600/4-79-020. Revised March 1983,
Section 200. EPA Methods 239.1 for Lead.
3. EPA Method SW846-3050B, Revision 2, December 1996
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Overview of
EMSL Analytical SOP
PLM Analysis
EPA 600/R-93/116

Method Description
This method is used to determine asbestos content in a variety of relatively
homogenous building materials. Subsequent to various prepping techniques, the
sample is analyzed by both a stereomicroscope and Polarized Light Microscope
(PLM). Asbestos is identified by measuring a number of optical properties
including refractive indices. Asbestos percent is determined by calibrated visual
estimate (CVE) or point counting.

Applicable Matrices
This method is applicable to friable, non-friable and non-friable organically bound
building materials. Sample should be of sufficient quantity to ensure reliable
quantitation through the use of required multiple preparations.

Interferences
Interferences for this method include but are not limited to:
- All non-asbestos particulate, fibrous or not, which can partially or wholly
obscure asbestos fibers.
- Non-regulated amphiboles or scrolled clay particles, such as richterite or
sepiolite, may have aspect ratios > 3:1 and possess similar physical and
optical properties.
- Non-asbestiform varieties of the amphibole asbestos minerals may form
cleavage fragments that are indistinguishable from asbestos by this
method.
- Coatings applied during sample manufacturing, or while the building
material application was in place, may obscure the optical properties of
fibers.

Test Method Summary Including Scope and Application
Bulk samples are examined under stereoscope to locate suspect fibers for
identification. After the initial identification samples are homogenized and
prepared for quantitation by CVE or point counting. This procedure should be
used to determine the asbestos content of bulk building materials and includes
procedures for various prep techniques and quantitation methods. Due to the
procedure's use of multiple preps and re-preps, as well as numerous preparation
options, bulk building materials are specified due to their inherent gross

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homogeneity that cannot be assumed in debris or other non-manufactured
materials.

Sample Collection, Preservation, Shipment and Storage
Samples are collected in a manner which produces no fiber release and are
commonly collected using strong ‘zip lock’ or ‘whirl pak’ bags. Only one sample
should be placed in each bag. No preservation is required. Bulk samples are
not to be shipped or stored with air samples. Samples are retained in an easily
retrievable manner for a minimum of 60 days.

Limit of Detection
Under normal conditions, the practical detection limit for this method is one (1)
percent. Detection limits can vary with sample type, amount of sample analyzed
or method of quantitation used. For example, the 1,000 point count method can
report values down to 0.1%. Similarly when EPA 600/R-93/116 is combined with
gravimetric matrix modification techniques the detection limit may be lowered.
.
Calibration and Standardization
Each major component of the method is calibrated and/or standardized entailing;
PLM alignment including proper illumination, objective centering, polarizer,
analyzer and ocular alignment, refractive index liquid calibration and analyst
calibration using known reference standards.

Sample Preparation
Bulk samples are examined under stereoscope to locate suspect fibers for
identification. Once identification is complete the sample is homogenized if
necessary and prepared for quantitation. Optionally at this point the use of
gravimetric matrix modification (NOB preparation) may be employed to better
identify and quantify the sample. Sufficient sample preps are prepared to
accurately quantify the sample, at least 2 for positive samples and 3 for samples
none detected for asbestos.

Sample Analysis – Interpretation and Calculations
Samples are analyzed using a PLM and suspect asbestos fibers are identified by
optical properties including refractive index, sign of elongation, pleochroism,
morphology, extinction, birefringence and fiber color. Quantitation takes place
using either CVE or Point Counting and the amount of each component present
is recorded. More slides are prepared and observed as needed. Each
component is reported as well as its quantity. Components below 1% are report
as <1% for CVE estimations, point counting reports discreet results below 1%.

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Quality Control
Each laboratory must adhere to the quality control and quality assurance
procedures described in EMSL’s Quality Assurance Manual. Instrument and
analyst calibration is performed prior to analysis as listed above. Sample
analysis is subjected to 10% total QC. This QC includes re-preparation and
reanalysis of samples by both the same and different analysts as well as the
analysis of known standards.

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4.0 PASSIVE SAMPLING - VOLATILE ORGANIC COMPOUNDS
This method involves GC/MS analysis of VOCs collected using charcoal-based passive samplers. These
samplers are used to measure vapor-phase VOCs in a variety of gaseous matrices including indoor air, outdoor air, extracted soil gas, and emissions from materials. VOCs in the sampling environment pass
through the diffusive barrier or permeable membrane of the sampler at a known, controlled rate (defined
as the sampling rate) and adsorb to the charcoal-based sorbent pad of the sampler. The sorbent is extracted using a volume of carbon disulfide, and the extract is directly injected into a gas chromatograph
equipped with a mass spectrometer. The retention time and spectral pattern of a compound are compared with that of known standard. Concentrations of the analytes are calculated from the average relative response factors of calibration curves obtained from analysis of standard solutions. The results are
reported in units of µg/sample or µg/m3 if the sampling rate and duration is known.
There are no regulatory methods for the preparation and analysis of the Radiello and WMS samplers, and
OSHA methods are available for workplace exposure measurements for several of the VOCs using 3M
OVM 3500 and SKC 575 series samplers. The OSHA methods and the recommended procedures published by Radiello (FSM) and 3M serve as the basis for this standard operating procedure for the
analysis of environmental samples. Additionally, QC elements outlined in EPA SW-846 8260 and 8270
are incorporated as applicable. One variance of note that ATL has taken to the OSHA, Radiello, and the OVM 3500 methods is the use of GC/MS instead of GC/FID.
Table 4.1 Target Analytes * Acceptance limits based on Desorption efficiency studies. ** 60 – 130% for WMS
Analytes
Reporting
Limit (µg/mL )
Acceptance Criteria
ICAL (%RSD) ICV (% R) LCS (% R) CCV
Chloromethane 0.2 30 70 – 130 50 – 140 %D ≤40%
Vinyl Chloride 0.2 30 50 – 140 50 – 140 %D ≤40%
Ethanol 0.5 30 70 – 130 50 – 130* %D ≤30%
1,1-Dichloroethene 0.2 30 70 – 130 70 – 130 %D ≤30%
Acetone 0.1 30 70 – 130 70 – 130 %D ≤30%
2-Propanol 0.1 30 50 – 130 50 – 130 %D ≤30%
MTBE 0.05 30 70 – 130 70 – 130 %D ≤30%
trans-1,2-Dichloroethene 0.1 20 80 – 120 70 – 130 %D ≤20%
Hexane 0.05 30 70 – 130 70 – 130 %D ≤30%
1,1-Dichloroethane 0.05 20 80 – 120 70 – 130 %D ≤20%
Ethyl Acetate 0.2 30 70 – 130 70 – 130 %D ≤30%
2-Butanone 0.05 30 70 – 130 70 – 130 %D ≤30%
cis-1,2-Dichloroethene 0.1 20 80 – 120 70 – 130 %D ≤20%
Chloroform 0.05 20 80 – 120 70 – 130 %D ≤20%
Air Toxics Limited Methods Manual
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Analytes
Reporting
Limit (µg/mL )
Acceptance Criteria
ICAL (%RSD) ICV (% R) LCS (% R) CCV
Cyclohexane 0.05 20 80 – 120 70 – 130 %D ≤20%
1,1,1-trichloroethane 0.05 20 80 – 120 70 – 130 %D ≤20%
Carbon Tetrachloride 0.05 20 80 – 120 70 – 130 %D ≤20%
Benzene 0.1 30 70 – 130 70 – 130 %D ≤30%
1,2-Dichloroethane 0.05 20 80 – 120 70 – 130 %D ≤20%
Heptane 0.05 20 80 – 120 70 – 130 %D ≤20%
Trichloroethene 0.05 20 80 – 120 70 – 130 %D ≤20%
4-Methyl-2-pentanone 0.1 30 70 – 130 70 – 130 %D ≤30%
Toluene 0.05 20 80 – 120 70 – 130 %D ≤20%
1,1,2-Trichloroethane 0.05 20 80 – 120 70 – 130 %D ≤20%
Tetrachloroethene 0.05 20 80 – 120 70 – 130 %D ≤20%
Chlorobenzene 0.05 20 80 – 120 70 – 130 %D ≤20%
Ethylbenzene 0.05 20 80 – 120 70 – 130 %D ≤20%
m,p-Xylene 0.05 20 80 – 120 70 – 130 %D ≤20%
o-Xylene 0.05 20 80 – 120 70 – 130 %D ≤20%
Styrene 0.05 30 70 – 130 20-100* %D ≤30%
1,1,2,2-Tetrachloroethane 0.05 30 70 – 130 60 – 130 %D ≤30%
Propylbenzene 0.05 20 80 – 120 70 – 130 %D ≤20%
1,3,5-Trimethylbenzene 0.05 20 80 – 120 70 – 130 %D ≤20%
1,2,4-Trimethylbenzene 0.05 20 80 – 120 70 – 130 %D ≤20%
1,3-Dichlorobenzene 0.05 30 70 – 130 50 – 110** %D ≤30%
1,4-Dichlorobenzene 0.05 30 70 – 130 50 – 110** %D ≤30%
1,2-Dichlorobenzene 0.05 30 70 – 130 50 – 110** %D ≤30%
Naphthalene 0.05 30 70 – 130 5-80* %D ≤30%
Table 4.2 Internal Standard
Analyte CCV IS (%R) Sample IS (%)R
2-Fluorotoluene 50 – 200 50 – 200
Table 4.3 Surrogate
Analyte %R
Toluene-d8 70-130
Air Toxics Limited Methods Manual
Revision 18.1, 11/2011 Page 11 Table 4.4 Sampling Rates for “Standard” target compounds (RAD 130)
Analytes
Reporting Limit (µg/mL )
Reporting Limit (µg/sampler) Sampling Rates for Radiello 130 Sampler
Chloromethane 0.2 0.4 Estimated
Vinyl Chloride 0.2 0.4 Estimated
Ethanol 0.5 1.0 102
1,1-Dichloroethene 0.2 0.4 Estimated
Acetone 0.1 0.2 77
2-Propanol 0.1 0.2 52
MTBE 0.05 0.1 65
trans-1,2-Dichloroethene 0.1 0.2 Estimated
Hexane 0.05 0.1 66
1,1-Dichloroethane 0.05 0.1 Estimated
Ethyl Acetate 0.2 0.4 78
2-Butanone 0.05 0.1 79
cis-1,2-Dichloroethene 0.1 0.2 Estimated
Chloroform 0.05 0.1 75
Cyclohexane 0.05 0.1 54
1,1,1-trichloroethane 0.05 0.1 62
Carbon Tetrachloride 0.05 0.1 67
Benzene 0.1 0.2 80
1,2-Dichloroethane 0.05 0.1 77
Heptane 0.05 0.1 58
Trichloroethene 0.05 0.1 69
4-Methyl-2-pentanone 0.1 0.2 67
Toluene 0.05 0.1 74
1,1,2-Trichloroethane 0.05 0.1 Estimated
Tetrachloroethene 0.05 0.1 59
Chlorobenzene 0.05 0.1 68
Ethylbenzene 0.05 0.1 68
m,p-Xylene 0.05 0.1 70
o-Xylene 0.05 0.1 65
Styrene 0.05 0.1 61
1,1,2,2-Tetrachloroethane 0.05 0.1 Estimated
Air Toxics Limited Methods Manual
Revision 18.1, 11/2011 Page 12
Analytes
Reporting
Limit (µg/mL )
Reporting
Limit (µg/sampler) Sampling Rates for Radiello 130 Sampler
Propylbenzene 0.05 0.1 57
1,3,5-Trimethylbenzene 0.05 0.1 Estimated
1,2,4-Trimethylbenzene 0.05 0.1 50
1,3-Dichlorobenzene 0.05 0.1 Estimated
1,4-Dichlorobenzene 0.05 0.1 51
1,2-Dichlorobenzene 0.05 0.1 Estimated
Naphthalene 0.05 0.1 25
Table 4.5 Sampling Rates for “Standard” target compounds (OVM)
Varied sampling rates for each compound (1 to 8hr) see the OVM Technical bulletin
Analytes
Reporting Limit
(µg/mL )
Reporting Limit
(µg/sampler)
Sampling Rates for
OVM Sampler
Chloromethane 0.2 0.30 Estimated
Vinyl Chloride 0.2 0.30 41
Ethanol 0.5 0.75 44
1,1-Dichloroethene 0.2 0.30 Estimated
Acetone 0.1 0.15 40
2-Propanol 0.1 0.15 39
MTBE 0.05 0.075 38
trans-1,2-Dichloroethene 0.1 0.15 Estimated
Hexane 0.05 0.075 32
1,1-Dichloroethane 0.05 0.075 33
Ethyl Acetate 0.2 0.3 34
2-Butanone 0.05 0.075 36
cis-1,2-Dichloroethene 0.1 0.15 Estimated
Chloroform 0.05 0.075 34
Cyclohexane 0.05 0.075 32
1,1,1-trichloroethane 0.05 0.075 31
Carbon Tetrachloride 0.05 0.075 30
Benzene 0.1 0.15 80
1,2-Dichloroethane 0.05 0.075 33
Air Toxics Limited Methods Manual
Revision 18.1, 11/2011 Page 13
Analytes
Reporting Limit
(µg/mL )
Reporting Limit
(µg/sampler)
Sampling Rates for
OVM Sampler
Heptane 0.05 0.075 29
Trichloroethene 0.05 0.075 31
4-Methyl-2-pentanone 0.1 0.15 30
Toluene 0.05 0.075 31
1,1,2-Trichloroethane 0.05 0.075 30
Tetrachloroethene 0.05 0.075 28
Chlorobenzene 0.05 0.075 29
Ethylbenzene 0.05 0.075 27
m,p-Xylene 0.05 0.075 27
o-Xylene 0.05 0.075 27
Styrene 0.05 0.075 29
1,1,2,2-Tetrachloroethane 0.05 0.075 28
Propylbenzene 0.05 0.075 Estimated
1,3,5-Trimethylbenzene 0.05 0.075 Estimated
1,2,4-Trimethylbenzene 0.05 0.075 Estimated
1,3-Dichlorobenzene 0.05 0.075 Estimated
1,4-Dichlorobenzene 0.05 0.075 27.8
1,2-Dichlorobenzene 0.05 0.075 27.8
Naphthalene 0.05 0.075 25
Chloromethane 0.2 0.30 Estimated
Vinyl Chloride 0.2 0.30 41
Ethanol 0.5 0.75 44
1,1-Dichloroethene 0.2 0.30 Estimated
Acetone 0.1 0.15 40
2-Propanol 0.1 0.15 39
MTBE 0.05 0.075 38
trans-1,2-Dichloroethene 0.1 0.15 Estimated
Hexane 0.05 0.075 32
1,1-Dichloroethane 0.05 0.075 33
Ethyl Acetate 0.2 0.3 34
2-Butanone 0.05 0.075 36
Air Toxics Limited Methods Manual
Revision 18.1, 11/2011 Page 14
Analytes
Reporting Limit
(µg/mL )
Reporting Limit
(µg/sampler)
Sampling Rates for
OVM Sampler
cis-1,2-Dichloroethene 0.1 0.15 Estimated
Chloroform 0.05 0.075 34
Cyclohexane 0.05 0.075 32
1,1,1-trichloroethane 0.05 0.075 31
Carbon Tetrachloride 0.05 0.075 30
Benzene 0.1 0.15 80
1,2-Dichloroethane 0.05 0.075 33
Heptane 0.05 0.075 29
Trichloroethene 0.05 0.075 31
4-Methyl-2-pentanone 0.1 0.15 30
Toluene 0.05 0.075 31
1,1,2-Trichloroethane 0.05 0.075 30
Tetrachloroethene 0.05 0.075 28
Chlorobenzene 0.05 0.075 29
Ethylbenzene 0.05 0.075 27
m,p-Xylene 0.05 0.075 27
o-Xylene 0.05 0.075 27
Styrene 0.05 0.075 29
1,1,2,2-Tetrachloroethane 0.05 0.075 28
Propylbenzene 0.05 0.075 Estimated
1,3,5-Trimethylbenzene 0.05 0.075 Estimated
1,2,4-Trimethylbenzene 0.05 0.075 Estimated
1,3-Dichlorobenzene 0.05 0.075 Estimated
1,4-Dichlorobenzene 0.05 0.075 27.8
1,2-Dichlorobenzene 0.05 0.075 27.8
Naphthalene 0.05 0.075 25

Air Toxics Limited Methods Manual
Revision 18.1, 11/2011 Page 15 Table 4.6 Sampling Rates for “Standard” target compounds (SKC Badge)
Analytes
Reporting
Limit (µg/mL )
Reporting
Limit (µg/sampler)
Sampling Rates for Indoor Air
Applications ‘Zero Face velocity’
Sampling Rates for
Outdoor/worker exposure (ml/min)
Chloromethane 0.2 0.4 Estimated Estimated
Vinyl Chloride 0.2 0.4 17.4 Estimated
Ethanol 0.5 1.0 Estimated 20.9*
1,1-Dichloroethene 0.2 0.4 9.74 12.3
Acetone 0.1 0.2 12.6 15.2
2-Propanol 0.1 0.2 Estimated 17.8*
MTBE 0.05 0.1 9.84 13.6
trans-1,2-Dichloroethene 0.1 0.2 10.2 14.8
Hexane 0.05 0.1 9.59 14.3
1,1-Dichloroethane 0.05 0.1 13.14 Estimated
Ethyl Acetate 0.2 0.4 9.26 13.1
2-Butanone 0.05 0.1 6.27 16.88
cis-1,2-Dichloroethene 0.1 0.2 11.10 14.8
Chloroform 0.05 0.1 Estimated 13
Cyclohexane 0.05 0.1 7.76 15.6
1,1,1-trichloroethane 0.05 0.1 9.40 14.1
Carbon Tetrachloride 0.05 0.1 10.41 14.1
Benzene 0.1 0.2 10.69 16
1,2-Dichloroethane 0.05 0.1 11.79 14.2
Heptane 0.05 0.1 9.38 13.9
Trichloroethene 0.05 0.1 11.47 14.9
4-Methyl-2-pentanone 0.1 0.2 Estimated 13.62
Toluene 0.05 0.1 8.90 14.5
1,1,2-Trichloroethane 0.05 0.1 Estimated 12.5
Tetrachloroethene 0.05 0.1 10.02 13.1
Chlorobenzene 0.05 0.1 Estimated 14.2*
Ethylbenzene 0.05 0.1 9.02 12.9
m,p-Xylene 0.05 0.1 8.1 12.65
o-Xylene 0.05 0.1 8.11 11.9
Styrene 0.05 0.1 9.04 13.7
1,1,2,2-Tetrachloroethane 0.05 0.1 Estimated 11.8
Air Toxics Limited Methods Manual
Revision 18.1, 11/2011 Page 16
Analytes
Reporting Limit
(µg/mL )
Reporting Limit
(µg/sampler)
Sampling Rates for
Indoor Air Applications ‘Zero
Face velocity’
Sampling Rates for Outdoor/worker
exposure (ml/min)
Propylbenzene 0.05 0.1 Estimated 11.69*
1,3,5-Trimethylbenzene 0.05 0.1 Estimated 12.1*
1,2,4-Trimethylbenzene 0.05 0.1 9.92 12.1*
1,3-Dichlorobenzene 0.05 0.1 Estimated 12.7*
1,4-Dichlorobenzene 0.05 0.1 10.74 12.7*
1,2-Dichlorobenzene 0.05 0.1 Estimated 12.6*
Naphthalene 0.05 0.1 Estimated 12.2*
Table 4.7 Summary of Calibration and QC Procedure Note: These criteria are used specifically for the standard list of analytes listed in Table 4.1.
QC Check Minimum Frequency Acceptance Criteria Corrective Action
Tuning Criteria Prior to calibration and at the start of every 12-
hour clock.
Method 8260B tuning criteria.

Correct problem then repeat tune.
Initial 5-Point Calibration Prior to sample analysis. Compound criteria in Table 4.1 Correct problem then repeat initial calibration. Analysis
may proceed if no more than 2 VOCs exceed criteria or 5%
of VOCs if short list is used. Narrate exceedences.
Initial Calibration
Verification (ICV)
Once per initial
calibration.
See Table 4.1 Verify concentrations and
standard preparation. Analysis may proceed if no more than 2
VOCs exceed criteria or 5% of VOCs if short list is used.
Narrate exceedences.
Continuing Calibration Verification (CCV) At the start of every shift immediately after the
BFB tune check.
See "CCV criteria" column in Table 4.1

Investigate and correct the problem, up to and including
recalibration if necessary. Analysis may proceed if no
more than 2 VOCs exceed criteria or 5% of VOCs if
short list is used. Associated results are flagged.
Air Toxics Limited Methods Manual
Revision 18.1, 11/2011 Page 17
QC Check
Minimum
Frequency
Acceptance
Criteria
Corrective
Action
Internal Standards (IS) IS is added at the time of extraction to all samples
and QC samples.
For CCVs: area counts 50% - 200%, RT w/in
30 sec of mid-point in ICAL.
For blanks, samples and non-CCV QC Checks:
area counts 50 – 200%, RT w/in 20 sec. of RT
in CCV.
CCV: inspect and correct system prior to sample
analysis.
For blanks: inspect the
system and re-analyze the blank.
For samples: re-analyze; if out again, flag data.
Surrogate Surrogate is added at the
time of extraction to all samples and QC
samples.
See Table 4.3. Same as for Internal
Standards.
Solvent Blanks Immediately after the calibration standard or
after samples with high concentrations
Results less than laboratory reporting
limit (see Table 4.1).
Re-aliquot and re-analyze solvent blank. If detections
remain, flag concentrations in associated samples.
Extracted Laboratory Blank Each set of up to 20
samples
Results less than the
reporting limit.
Flag sample concentrations in
associated extraction batch.
Extracted LCS Each set of up to 20 samples. See Table 4.1 Re-aliquot and re-analyze the extract. If within limits,
report the re-analysis. Otherwise, narrate.
Extracted LCSD Each set of up to 20
samples.
%RPD < 25% Analysis may proceed if no
more than 2 VOCs exceed criteria (or 5% for short list
exceed criteria). Run a 3rd time, perform corrective
action or narrate as appropriate.

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Method: EPA Method TO-14A/TO-15 Volatile Organic Compounds (Standard)
Eurofins Air Toxics SOP#6 Revision 27 Effective Date: March 2, 2012 Methods Manual Summary
Description: This method involves full scan GC/MS analysis of whole air samples collected in evacuated stainless steel canisters. Samples are analyzed for volatile organic compounds using EPA
Method TO-14A/TO-15 protocols. An aliquot of up to 0.5 liters of air is withdrawn from the canister
utilizing a volumetric syringe, volumetric loop, or mass flow controller. This volume is loaded onto a hydrophobic multibed sorbent trap to remove water and carbon dioxide and to concentrate the vapor
sample. The focused sample is then flash heated to sweep adsorbed VOCs onto a secondary trap for further concentration and/or onto a GC/MS for separation and detection.
Eurofins Air Toxics maintains a suite of TO-14A/TO-15 methods, each optimized to efficiently meet the
data objectives for a wide range of targeted concentration ranges. The methods, their reporting limits and typical applications are summarized in the table below. This method summary (6.27) describes TO-14A/TO-15 (Standard or Quad).
Eurofins Air Toxics Method Base Reporting Limits Typical Application
TO-14A/TO-15 (5&20) 5 – 20 ppbv Soil Gas & ppmv range vapor
matrices
TO-14A/TO-15 (Standard or Quad) 0.5 – 5.0 ppbv Ambient Air, Soil Gas & ppbv level vapor matrices
TO-14A/TO-15 (Low-level) 0.1 – 0.5 ppbv Indoor and Outdoor Air
TO-14A/TO-15 SIM 0.003 – 0.5 ppbv Indoor and Outdoor Air

Certain compounds are not included in Air Toxics’ standard target analyte list. These compounds are
communicated at the time of client proposal request. Unless otherwise directed, ATL reports these non-routine compounds with partial validation. Validation may include a 3-point calibration with the lowest
concentration defining the reporting limit, no second source verification analyzed, and no method detection limit study performed unless previous arrangements have been made. In addition, stability of the non-standard compound during sample storage is not validated. Full validation may be available upon
request.
Eurofins Air Toxics takes no modifications of technical significance to Method TO-15 for the ‘Quad’ configurations. Since Air Toxics applies TO-15 methodology to all Summa canisters regardless of
whether TO-14A or TO-15 is specified by the project, Air Toxics performs a modified version of method TO-14A as detailed in Table 1. Please note that Methods TO-14A and TO-15 were validated for specially treated canisters. As such, the use of Tedlar bags for sample collection is outside the scope of the method
and not recommended for ambient or indoor air samples. It is the responsibility of the data user to determine the usability of TO-14A and TO-15 results generated from Tedlar bags.

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Table 1. Summary of TO-14A Method Modifications
Requirement TO-14A ATL Modifications
Sample Drying System Nafion Drier Multibed hydrophobic sorbent
Blank acceptance criteria < 0.2 ppbv < RL
BFB ion abundance criteria Ion abundance criteria listed in Table 4 of TO-14A Follow abundance criteria listed in TO-15
Daily CCV 70-130% for listed 39
VOCs.
70-130%. ATL’s 62 standard compound list exceeding this
criterion and associated data will be flagged and narrated.

Initial Calibration ≤ 30% RSD for listed 39 VOCs ≤ 30% RSD with 2 of ATL’s 62 standard compounds allowed out to ≤ 40%.
The standard target analyte list, Reporting Limit (RL) also referred to as Limit of Quantitation, QC
criteria, and QC summary can be found in Tables 2 through 5.
Table 2. Method TO-14A/TO-15 Analyte List (Standard Quad)
Analyte RL†
(ppbv)
ICAL %RSD
Acceptance Criteria
ICV/LCS (%R)
Precision Limits (Max. RPD)
1,1,2,2-Tetrachloroethane 0.5 30% 70 - 130 ≤ 25
1,1,2-Trichloroethane 0.5 30% 70 - 130 ≤ 25
1,1-Dichloroethane 0.5 30% 70 - 130 ≤ 25
1,1-Dichloroethene 0.5 30% 70 - 130 ≤ 25
1,2,4-Trichlorobenzene 2.0 30% 70 - 130 ≤ 25
1,2,4-Trimethylbenzene 0.5 30% 70 - 130 ≤ 25
1,2-Dibromoethane (EDB) 0.5 30% 70 - 130 ≤ 25
1,2-Dichlorobenzene 0.5 30% 70 - 130 ≤ 25
1,2-Dichloroethane 0.5 30% 70 - 130 ≤ 25
1,2-Dichloropropane 0.5 30% 70 - 130 ≤ 25
1,3,5-Trimethylbenzene 0.5 30% 70 - 130 ≤ 25
1,3-Dichlorobenzene 0.5 30% 70 - 130 ≤ 25
1,4-Dichlorobenzene 0.5 30% 70 - 130 ≤ 25
Benzene 0.5 30% 70 - 130 ≤ 25
Bromomethane* 5.0 30% 70 - 130 ≤ 25
Carbon Tetrachloride 0.5 30% 70 - 130 ≤ 25
Chlorobenzene 0.5 30% 70 - 130 ≤ 25
Chloroethane 2.0 30% 70 - 130 ≤ 25
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Analyte RL†
(ppbv)
ICAL
%RSD
Acceptance Criteria
ICV/LCS (%R)
Precision
Limits (Max. RPD)
Chloroform 0.5 30% 70 - 130 ≤ 25
Chloromethane 5.0 30% 70 - 130 ≤ 25
α-Chlorotoluene (Benzyl Chloride) 0.5 30% 70 - 130 ≤ 25
cis-1,2-Dichloroethene 0.5 30% 70 - 130 ≤ 25
cis-1,3-Dichloropropene 0.5 30% 70 - 130 ≤ 25
Dichloromethane 5.0 30% 70 - 130 ≤ 25
Ethylbenzene 0.5 30% 70 - 130 ≤ 25
Freon 11 (Trichlorofluoromethane) 0.5 30% 70 - 130 ≤ 25
Freon 113 (Trichlorotrifluoroethane) 0.5 30% 70 - 130 ≤ 25
Freon 114 0.5 30% 70 - 130 ≤ 25
Freon 12 (Dichlorodifluoromethane) 0.5 30% 70 - 130 ≤ 25
Hexachlorobutadiene 2.0 30% 70 - 130 ≤ 25
m,p-Xylene 0.5 30% 70 - 130 ≤ 25
Methyl Chloroform (1,1,1-
Trichloroethane) 0.5 30% 70 - 130 ≤ 25
o-Xylene 0.5 30% 70 - 130 ≤ 25
Styrene 0.5 30% 70 - 130 ≤ 25
Tetrachloroethene 0.5 30% 70 - 130 ≤ 25
Toluene 0.5 30% 70 - 130 ≤ 25
trans-1,3-Dichloropropene 0.5 30% 70 - 130 ≤ 25
Trichloroethene 0.5 30% 70 - 130 ≤ 25
Vinyl Chloride 0.5 30% 70 - 130 ≤ 25
1,3-Butadiene 0.5 30% 70 – 130 ≤ 25
1,4-Dioxane 2.0 30% 70 – 130 ≤ 25
2-Butanone (Methyl Ethyl Ketone) 2.0 30% 70 – 130 ≤ 25
2-Hexanone 2.0 30% 70 – 130 ≤ 25
4-Ethyltoluene 0.5 30% 70 – 130 ≤ 25
4-Methyl-2-Pentanone (MIBK) 0.5 30% 70 – 130 ≤ 25
Acetone 5.0 30% 70 – 130 ≤ 25
Bromodichloromethane 0.5 30% 70 – 130 ≤ 25
Bromoform 0.5 30% 70 – 130 ≤ 25
Carbon Disulfide 2.0 30% 70 – 130 ≤ 25
Cyclohexane 0.5 30% 70 – 130 ≤ 25
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Analyte
RL†
(ppbv)
ICAL
%RSD
Acceptance Criteria
ICV/LCS (%R)
Precision
Limits (Max. RPD)
Dibromochloromethane 0.5 30% 70 – 130 ≤ 25
Ethanol 2.0 30% 70 – 130 ≤ 25
Heptane 0.5 30% 70 – 130 ≤ 25
Hexane 0.5 30% 70 – 130 ≤ 25
Isopropanol (2-Propanol) 2.0 30% 70 – 130 ≤ 25
Methyl t-Butyl Ether (MTBE) 0.5 30% 70 – 130 ≤ 25
Tetrahydrofuran 0.5 30% 70 – 130 ≤ 25
trans-1,2-Dichloroethene 0.5 30% 70 – 130 ≤ 25
2,2,4-Trimethylpentane 0.5 30% 70 – 130 ≤ 25
Cumene 0.5 30% 70 – 130 ≤ 25
Propylbenzene 0.5 30% 70 – 130 ≤ 25
3-Chloroprene 0.5 30% 70 – 130 ≤ 25
Naphthalene** 2.0 40% 60 – 140 ≤ 25
TPH (Gasoline) or NMOC (Hexane/Heptane)*** 25 One Point Calibration NA ≤ 25
Table 3. Internal Standards Table 4. Surrogates
Analyte
Accuracy
(% R) Analyte
Accuracy
(% R)
Bromochloromethane 60 - 140 1,2-Dichloroethane-d4 70 – 130
1,4-Difluorobenzene 60 - 140 Toluene-d8 70 – 130
Chlorobenzene-d5 60 - 140 4-Bromofluorobenzene 70 – 130
†Reporting Limits are subject to change and require confirmation from the laboratory.
*Bromomethane recovery can be variable due to moisture/sorbent interactions specifically on the 2-trap concentration system. Data may require qualifier flags.
**Due to its low vapor pressure, Naphthalene does not meet TO-15 performance requirements. The
wider QC limits reflect typical performance. Although Naphthalene is not on Air Toxics ‘standard’ TO-15 list, it is commonly requested and included in Table 1.
***TPH and NMOC are not on Air Toxics’ standard TO-15 list, and are included in Table 1 due to
common requests.

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Table 5. Summary of Calibration and QC Procedures for Methods TO-14A/TO-15
Continued on next page
QC Check Minimum
Frequency Acceptance Criteria Corrective Action
Tuning Criteria Every 24 hours, TO-15 ion abundance criteria Correct problem then repeat tune.
Minimum 5-Point
Initial Calibration
(ICAL)
Prior to sample analysis. % RSD ≤ 30 with two compounds
allowed out to ≤ 40% RSD.

Note: Bromomethane and alpha-Chlorotoluene may exceed 40%RSD.
All associated data is flagged as estimated.
Correct problem then repeat Initial Calibration Curve.
Initial
Calibration
Verification and Laboratory Control Spike
(ICV and LCS)
After each initial
calibration curve,
and daily, prior to sample analysis.
Recoveries for 85% of Standard
compounds must be 70-130%. No
recovery may be <50%.

* If specified by the client in-house generated control limits may be used.
Check the system and reanalyze the
standard. Re-prepare the standard if
necessary to determine the source of error. Re-calibrate the instrument if the primary standard is found to be in error.
Initial
Calibration Verification and
Laboratory Control Spike
(ICV and LCS) for Non-
Standard Compounds
Per client request
or specific project requirements only.
Recoveries of compounds must be
60-140%. No recovery may be <50%.

Check the system and reanalyze the
standard. Re-prepare the standard if necessary to determine the source of
error. Re-calibrate the instrument if the primary standard is found to be in error.
Continuing
Calibration Verification (CCV)
At the start of each
24-hour clock.
70-130%.

Compounds exceeding this criterion and
associated data will be flagged and narrated with the exception of high bias
associated with non-detects.
If more than two compounds from the
standard list recover outside of 70-130%, corrective action will be taken. If any
compound exceeds 60-140%, samples are not analyzed unless compound is not a
risk driver and/or data meets project needs. Check the system and reanalyze
the standard. Re-prepare the standard if necessary. Re-calibrate the instrument if
the criteria cannot be met.
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QC Check Minimum
Frequency Acceptance Criteria Corrective Action
Laboratory Blank After analysis of standards and prior
to sample analysis, or when
contamination is present.
Results less than the laboratory reporting limit (Table 1). Inspect the system and
Re-analyze the blank. B-flag data for
common contaminants.
Internal
Standard (IS)
As each standard,
blank, and sample is being loaded.
Retention time (RT) for blanks and
samples must be within ±0.33 min of the RT in the CCV and within
±40% of the area counts of the daily CCV internal standards.
For blanks: inspect the system and
reanalyze the blank.
For samples: re-analyze the sample. If
the ISs are within limits in the re-analysis, report the second analysis. If
ISs are out-of-limits a second time, dilute the sample until ISs are within
acceptance limits and narrate.
Surrogates As each standard,
blank, and sample is being loaded.
70 - 130%.

* If specified by the client in-house
generated control limits may be used.
For blanks: inspect the system and
reanalyze the blank.
For samples: re-analyze the sample
unless obvious matrix interference is documented. If the %Rs are within
limits in the re-analysis, report the second analysis. If %Rs are out-of-
limits a second time, report data from first analysis and narrate.
Laboratory
Duplicates - Laboratory
Control Spike Duplicate
(LCSD)
One per analytical
batch. RPD ≤25%. Narrate exceedances. If more than 5%
of compound list outside criteria or if compound is >40%RPD, investigate the
cause and perform maintenance as required. If instrument maintenance is
required, calibrate as needed.
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Method: ASTM D1946 – Atmospheric Gases
Eurofins Air Toxics SOP#8 Revision 20 Effective Date: April 10, 2012 Methods Manual Summary
Description: This method involves GC analysis of soil gas, landfill gas, ambient air, or stack gas collected in SummaTM canisters, Tedlar bags, or any vessel that has been demonstrated to be clean and
leak free. Samples are analyzed for Methane, fixed gases, and Non-Methane Organic Carbon (NMOC) using modified ASTM D1946 protocols. Because the sample is withdrawn from the vessel by positive pressure, rigid containers are first filled to positive pressure using UHP Helium or Nitrogen. Samples are
then analyzed using a GC equipped with a FID and a TCD.
Certain compounds are not included in Eurofins Air Toxics’ standard target analyte list. These
compounds are communicated at the time of client proposal request. Unless otherwise directed, the
laboratory reports these non-standard compounds with partial validation. Validation includes a 3-point calibration with the lowest concentration defining the reporting limit, no second source verification is analyzed, and no method detection limit study is performed unless previous arrangements have been
made. In addition, stability of the non-standard compound during sample storage is not validated. Full
validation may be available upon request.
Since the protocols in the ASTM D1946 standard were designed for the analysis of Reformed gas, the
laboratory has taken modifications to apply the method to environmental samples covering a wide concentration range and to implement standard NELAP and EPA calibration criteria. The method
modifications, standard target analyte list, RL, QC criteria, and QC summary can be found in the
following tables.
Table 1. Summary of Method Modifications for ASTM D1946
Requirement ASTM D1946 Eurofins Air Toxics Modifications
Calibration A single point calibration is performed
using a reference standard closely matching the composition of the unknown.
A minimum 3-point calibration curve is
performed. Quantitation is based on a daily calibration standard, which may or may not resemble the composition of the associated samples.
Reference Standard The composition of any reference standard must be known to within 0.01 mol % for any component.
The standards used by AT are blended to a ³
95% accuracy.
Sample Injection Volume Components whose concentrations are in excess of 5 % should not be analyzed by
using sample volumes greater than 0.5 mL.
The sample container is connected directly to a fixed volume sample loop of 1.0 mL.
Linear range is defined by the calibration curve. Bags may be loaded by vacuum or by
positive pressure.
Normalization Normalize the mole percent values by
multiplying each value by 100 and dividing by the sum of the original values.
The sum of the original values should not differ from 100% by more than 1.0%.
Results are not normalized. The sum of the
reported values can differ from 100% by as much as 15%, either due to analytical
variability or an unusual sample matrix.
Precision Precision requirements established at each
concentration level.
Duplicates should agree within 25 % RPD.
for detections >5 X’s the RL
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Table 2. Method Compound List and QC Limits
Compound
Reporting
Limit
(%)
ICAL
Criteria
(%RSD)
ICV/LCS
Criteria
(%R)
CCV
Criteria
(%D)
Precision
Limits
(RPD)**
Carbon Dioxide 0.010 £ 15% 85 – 115 ± 15% ± 25%
Carbon Monoxide 0.010 £ 15% 85 – 115 ± 15% ± 25%
Methane 0.00010 £ 15% 85 – 115 ± 15% ± 25%
Ethene 0.0010 £ 15% 85 – 115 ± 15% ± 25%
Ethane 0.0010 £ 15% 85 – 115 ± 15% ± 25%
Nitrogen 0.10 £ 15% 85 – 115 ± 15% ± 25%
NMOC 0.010 £ 15% 85 – 115 ± 15% ± 25%
Oxygen 0.10 £ 15% 85 – 115 ± 15% ± 25%
Helium 0.050 £ 15% 85 – 115 ± 15% ± 25%
Hydrogen 0.010* £ 15% 85 – 115 ± 15% ± 25%

* RL is 1.0 % when sample is pressurized with He.
** For detections greater than 5 times the reporting limit.

Note: Results are reported in units of mol %. If required to report volume % or ppmV, a
compressibility factor of 1 for all gases will be assumed. As a result, mol % is assumed
to be equivalent to volume %. This assumption may result in a bias for highly
compressible gases at high concentrations and pressures.
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Table 3. Summary of Calibration and QC Procedures for Mod. ASTM Method D1946
QC Check Minimum
Frequency
Acceptance
Criteria Corrective Action
Initial Calibration Curve (ICAL) Prior to Sample analysis. RSD £ 15%. Correct problem then repeat Initial Calibration.
Second Source Verification
(LCS)
All analytes - once per
Initial Calibration, and with each analytical batch.
%R between 85
– 115 %.
Check the system and re-analyze the
standard. Re-calibrate the instrument if the criteria cannot be met.
Continuing Calibration Verification (CCV) Daily prior to sample analysis and after every
20 reportable samples.
%D± 15% Check the system and re-analyze
the standard. Re-calibrate the instrument
if the criteria cannot be met.
Laboratory Blank (He)
(N2 for He and H2 analysis)
After each daily check standard and prior to sample
analysis, or when contamination is present.
Results below the RL. Inspect the system and re-analyze the Blank.
End Check At the end of analytical sequence. It can be primary
(CCV) or Independent Source (LCS).
%R between 85 – 115 %. Check system and re-analyze the standard. If the 2nd analysis fails, identify
and correct the problem. Samples analyzed after the last acceptable CCV
are re-analyzed.
Sample Duplicates - Laboratory Control Spike Duplicate (LCSD)
One per analytical batch. RPD £ 25 %. Narrate exceedances. Investigate the cause and perform maintenance as required and re-calibrate as needed.