NCD003446721_19900423_Celeanse Corporation - Shelby Fiber_FRBCERCLA RA_60% Remedial Design Report and Draft Remedial Action Work Plan-OCR

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Westinghouse Environmental
and Geoteclmical Services. Inc.
4000 DeKalb Technology Parkway, NE
Suite 250
Atlanta. Georgia 30340
[phone]
FAX [phone]
OPERABLE UNIT 2
60% REMEDIAL DESIGN REPORT AND
DRAFT REMEDIAL ACTION WORK PLAN
HOECHST CELANESE/SHELBY, NORTH CAROLINA
WESTINGHOUSE PROJECT 4124-85-0S0N
DOCUMENT CONTROL 85050N-0227
Prepared For:
HOECHST CELANESE CORPORATION
Shelby, North Carolina
Prepared By:
WESTINGHOUSE ENVIRONMENTAL AND
GEOTECHNICAL SERVICES, INC.
April 1990
Madoly-rr-A. Stre:; Everett W. Glover, Jr., P.E.
Project Manager Staff Engineer
5050N013
A Westinghouse Electric Corporation subsidiary
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operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document Control 85050N-0227
Page i
TABLE OF CONTENTS
List of Figures
List of Tables
List of Appendices
EXECUTIVE SUMMARY
1.0 INTRODUCTION
1.1 site Description
1.2 Site History and Regulatory Status
1.3 Project Objective and Scope
2.0 REMEDIATION OBJECTIVES AND BASIS FOR DESIGN
2.1
2.2
2. 3
Remediation Objectives
Waste Characteristics
waste Volumes
3.0 REMEDIATION CRITERIA
3.1
3.2
3.3
3.4
3.5
3. 6
3.7
3.8
3.9
3.10
3.11
3.12
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Organization Responsibilities
Excavation Requirements
3.2.1 General Excavation and Site Preparation
3.2.2 stream Sediments
3.2.3 Source Materials
Solidification Criteria
Thermal Treatment criteria
water Treatment criteria
Spill Control and Emergency Procedures Criteria
Decontamination Criteria
Quality Assurance/Quality Control Criteria
Permitting Criteria
Health and Safety criteria
Sampling and Analysis Criteria
Project Schedule
V
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vii
ES-1
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1-3
1-7
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3-11
3-15
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Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document Control 85050N-0227
Page ii
4.0 QUALITY ASSURANCE/QUALITY CONTROL
4.1
4.2
4.3
4.4
4.5
4.6
4.7
4.8
4.9
4.10
Project Organization and Responsibilities
Quality Assurance Objectives for Measurement
Data
Sampling Procedures
sample Custody
Calibration Procedures and Frequencies
4.5.1 Field Equipment
4.5.2 Laboratory Equipment
Analytical Procedures
Data Reduction, Verification, and
Internal Quality Control Checks
Performance and System Evaluation
Preventive Maintenance
4.10.1 General
Reporting
4.10.2 Sampling and Analytical Equipment
4.10.3 Support Equipment
4.11 Specific Routine Procedures Used to Assess
Data Precision, Accuracy, and Completeness
4.12 Corrective Action
4.13 Quality Assurance Reports to Management
5.0 HEALTH AND SAFETY PLAN
5.1 Organization and Staff Responsibilities
5.1.1 Personnel
5.1.2 On-Site Personnel
5.1.3 Work Zones
5.2 Work Practice Controls
5.2.1 Standing Orders
5.2.2 Site Organization
5.3
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Site Control
5.3.1 Pit Excavation
5.3.2 stream Excavation
4-1
4-1
4-3
4-4
4-6
4-10
4-10
4-12
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Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document Control 85050N-0227
Page iii
5.4
5.5
5.6
5.7
Safety Precautions
5.4.1 Liquids/Sludges
5.4.2 Dusts
5.4.3 Vapors/Gases
5.4.4 Physical Hazards
5.4.5 Weather Conditions
Education and Training
Medical Surveillance
Ambient Field Monitoring
5.7.1 Excavating
5.7.2 Decontamination
5.7.3 Rotary Kiln Sampling
5.8 Levels of Protection
5.9 Safety Equipment List
5.9.l First Aid
5.9.2 Fire-Fighting
5.9.3 Communications
5.9.4 Decontamination Equipment
5.9.5 Sanitation/Hygiene
5.10 Decontamination Procedures
5.11 Contingency Plans
5.11.1 Local Sources of Assistance
5.11.2 National/Regional Sources of Assistance
5.12 Amendments to Site Specific Health and Safety
Plan
6.0 SAMPLING AND ANALYSIS PLAN
6.1 Sampling Handling
6.2 Sample Identification
6.3 Sampling Procedures
6.4 Specific Sampling Procedures
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6.4.1 Treated Scrubber and Storrnwater Samples
6.4.2 Solidified Material
6.4.3 Incinerator Ash
6.4.4 Stream Sediments
Page
5-8
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5-13
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5-18
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6.5
6.6
6.7
6.8
6.9
6.10
6.11
Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document Control 85050N-0227
Page iv
6.4.5 Stack Sampling
6.4.6 Waste Feed
Sample Custody
Equipment Decontamination
Calibration Procedures and Frequencies
Analytical Procedures
Data Reduction, Verification, and Reporting
Internal Quality Control Checks
Preventive Maintenance
6-16
6-16
6-17
6-19
6-20
6-20
6-20
6-21
6-22
7 • 0 REFERENCES 7-1
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Figure
1-1
2-1
2-2
3-1
3-2
4-1
4-2
5050N013
Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document Control 85050N-0227
Page v
List of Figures
Title
Site Location Map
GRU and Burn Pit Locations
Stream Segments Needing Remediation
Location of Treatment Equipment and
Excavation Areas
Operable Unit 2 Schedule
sample Tag
Chain-of-Custody Form
1-2
2-6
2-7
3-3
3-23
4-7
4-9
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Table
3-1
3-2
3-3
5-1
6-1
5050N013
Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-B5-O5ON
Document Control 85O5ON-O227
Page vi
List of Tables
Title
Maximum concentration of Contaminants
for the Toxicity Characteristics
Constituents and Concentrations Reported
in GRU Samples
organic Chemicals, Plastics and Synthetic
Fibers Effluent Guidelines
Precautionary Standards of Hazardous
Chemicals
3-9
3-14
3-16
5-9
Recommended Sample Containers, Preservation, 6-2
and Holding Times
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Appendix
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IV
5050N013
Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document Control 85050N-0227
Page vii
List of Appendices
Title
GDC Remedial Action Work Plan
GDC Trial Burn Plan
Metal Emissions from Hazardous Waste Incineration
Laboratory Quality Assurance/Quality Control
Manuals
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Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document control 85050N-0227
Page ES-1
EXECUTIVE SUMMARY
This remedial report describes the engineering services and
remedial action recommended at the Hoechst Celanese site in
Shelby, North Carolina. Westinghouse and GDC Engineering Inc.
have prepared the remedial design (RD) for the on-site
incineration remedial action alternative developed in the
feasibility study (FS). This alternative was selected and
summarized by the Environmental Protection Agency (EPA) in the
Record of Decision (ROD) for the Shelby site dated March 28,
1989.
The RD includes a discussion of the technical-aspects of the
project including the plans, design drawings, and performance
specifications needed to accomplish the remedial action
recommended in the ROD. The recommended remedial action
consists of:
o excavation of
plastic chip,
sediments
glycol recovery unit (GRU) sludges,
burn pit residuals, and selected stream
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on-site incineration of GRU sludges and associated contaminated soils
chemical fixation (solidification) of incinerator ash, plastic chip, burn pit residuals, and selected stream sediments
on-site disposal of inert, solidified material
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Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document Control 85050N-0227
Page ES-2
regrading and revegetation, where necessary
monitoring
This report presents the 60% design submittal and Draft Remedial
Action Work Plan prepared cooperatively by Westinghouse and GDC
Engineering Inc.
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1.1 site Description
Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0S0N
Document Control 85050N-0227
Page 1-1
1.0 INTRODUCTION
The Hoechst Celanese site is a 469-acre property occupied by a
polyester resin and fiber production facility (Figure 1-1). The
site is located in south-central Cleveland County east of North
Carolina Highway 198. It is approximately 1 mile north of
Earl, North Carolina and 6 miles south of Shelby. The nearest
major city is Charlotte, North Carolina, 35 miles east of
Shelby.
The plant facilities consist of the plant production area,
wastewater treatment area, former waste disposal areas, former
sludge landfarm area, and recreation and wooded areas. The
majority of the land surface reflects cultural modification by
construction, and by cutting and filling. The original soil
profile has probably been either truncated or covered across
much of the site, and was never conclusively identified as
undisturbed during the field investigations of the Remedial
Investigation (RI) (S&ME, 1987). The plant production area is
predominantly covered with buildings and paved or gravelled
areas. However, to the east, toward the wastewater treatment
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~ rao. 11..,cn11.ao ,1"11,i11. QIJfDWO.f 11n11
CCIIT'CUt IIIT[l¥Al.1 20 ,UT
~ Westinghouse Environmental '& and Geotechnical Services, Inc.
0 2000
SCALI. II FUT
FIGURE 1-1
SITE LOCATION MAP
HC/SHELBY
WESTINGHOUSE PROJECT 4124-85-OSON
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Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document Control 85050N-0227
Page 1-3
area, the site becomes more open, with the majority of the land
covered by impoundments, with grass and access roads in
between. The former sludge landfarm is north of the plant
production area and is overgrown with coarse grasses. The
recreation area and wooded area to the south have no facilities
related to the plant process.
Adjacent land use is rural; some residences are located within 1
mile of the site.
1.2 site History and Regulatory Status
Fiber Industries, Inc., a joint venture of Celanese Corporation
and Imperial Chemic~ls, Incorporated, (ICI), was the original
owner of the plant and operated it from 1960 until 1983 when the
Celanese Corporation bought out ICI's share of the facility.
American Hoechst and Celanese merged in 1987 to form Hoechst
Celanese. It is now operated as the Hoechst Celanese, Shelby
Facility. Operations at the Shelby facility began in April,
1960. Manufacturing operations included the production of
polyester polymer resin and filament yarn. The principal
chemicals involved in polymer production are dimethyl
terephthalate and ethylene glycol.
The Hoechst Celanese wastewater treatment plant was constructed
5050N013
Operable Unit 2 60% Remedial Design Report and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC Westinghouse Project 4124-85-0S0N
Document Control SS0S0N-0227
Page 1-4
in phases concurrent with the manufacturing plant, and became
fully operational in the mid-1960's. In 1973, the plant was
expanded with the addition of a polishing pond, two emergency
spill ponds, and an additional aeration basin. The treated
effluent from the wastewater treatment plant is piped to a
discharge point on Buffalo Creek.
Several areas around the plant have been used for waste
. disposal. Normal plant wastes (primarily polyester and
miscellaneous trash) were disposed of in old burn pits located
just north of the aeration basins. North and east of the burn
pits, glycol recovery unit (GRU) sludge was buried in trenches
during the early 1960 1 s.
Two other areas of buried waste are located to the north of the
main plant. The polymer and fiber landfill contains primarily
non-hazardous inert materials such as excavation spoil,
construction waste, and yarn. The construction debris landfill
contains items such as old cinder blocks and steel strapping
bands.
Investigation of the Hoechst Celanese site began in October 1981
when Hoechst Celanese contracted with Westinghouse to install 23
groundwater .monitor wells. In conjunction with the groundwater
monitor well installation program, Westinghouse also conducted a 5050N013
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Operable Unit 2 60% Remedial Design Report and Draft Remedial Action work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document Control 85050N-0227
Page 1-5
hydrogeologic evaluation. Subsequently, Hoechst Celanese
initiated a groundwater sampling and analysis program under the
supervision of Davis & Floyd Laboratories, Inc. Westinghouse
also conducted an electromagnetic survey and excavated test pits
at the site.
In October 1984, the Hoechst Celanese, Shelby Facility was
. proposed for EPA's National Priorities List (NPL), and
preparation of a Work Plan for a Remedial Investigation (RI) and
Feasibility Study (FS) was started by Hoechst Celanese's
contractor, Westinghouse. Concurrent with this, EPA's
contractor, Camp, Dresser & McKee, Inc. (COM); prepared a report
that included a review of the data collected during previous
site investigations and identified information deficiencies and
data gaps to provide a basis for development of Remedial
Investigation activities. These events resulted in the
submission of a draft Work Plan by Westinghouse, on behalf of
Hoechst Celanese, with the final Order on Consent to perform the
RI/FS on March 10, 1986. In June 1986, the EPA added the site
to the NPL.
The RI report for the site was final in July 1987 and determined
that the former glycol recovery unit waste pits and other
adjacent disposal pits, and groundwater contaminated by the
waste in those pits should be remediated. Because of the
5050N013
Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document Control 85050N-0227
Page 1-6
potential for contaminated groundwater to move off site, EPA
approved Westinghouse's proposal for a two-phased clean-up
action. The first phase was identified as Operable Unit l (OU
1) and focuses on remediating contaminated groundwater.
Operable Unit 2 (OU 2) addresses remediation of the sludges and
soils associated with the former glycol recovery unit trenches,
of the burn pit areas, and of specific stream sediments.
The Operable Unit FS for the groundwater was completed in
February 1988. The ROD for OU l Remedial Action was signed
March 23, 1988, and required extraction and treatment of
contaminated groundwater associated with the site. Hoechst
Celanese agreed to conduct the Remedial Action for OU 1 in a
partial Consent Decree dated June 30, 1988. Construction of the
extraction and treatment systems are complete, and they are
operational.
The FS for OU 2 Remedial Action was final in April 1989 (S&ME,
1989a), and addresses contaminant source control. A Consent
Decree on OU 2 was signed by Hoechst Celanese on June 19, 1989.
The selected remedial action for the Hoechst Celanese, Shelby,
Facility is outlined in the ROD (EPA, 1989) and includes the
following remediation activities:
o excavation of approximately 2000 cubic yards of glycol
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Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0S0N
Document Control 85050N-0227
Page 1-7
recovery unit (GRU) sludges. The 2000 cubic yards
includes a known GRU volume of 1500 cubic·yards plus an additional 1 foot of soil below the GRU/soil interface
excavation of approximately 1200 cubic yards of burn pit residuals
excavation of approximately 600 cubic yards of plastic chip
excavation of approximately 110 cubic yards of stream sediments
o incineration of GRU sludges and associated soils
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chemical fixation (solidification) of incinerator ash, plastic chips, burn pit residuals, and stream sediments
on-site disposal of solidified materials
o regrading and revegetating, where necessary
0 monitoring
1.3 Project Objective and Scope
The objective of this phase of the project is to prepare .. a
Remedial Design and Remedial Action Work Plan for the source
material that will remove and treat the major source of
contamination on the site, and thus, mitigate further
groundwater contamination. The remedial action addresses the
GRU material, burn pit materials, plastic chip, and stream
sediments.
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Operaole Unit 2 60% Remedial Design Report and Draft Remedial Design work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document control SSOSON-0227
Page 2-1
2.0 REMEDIATION OBJECTIVES AND BASIS FOR DESIGN
2.1 Remediation Objectives
The objectives of the remediation are to treat, through
incineration and/or solidification, the material identified as
the most probable source of contamination, and to excavate and
solidify stream sediments identified as containing some
plant-related organic contamination, primarily phthalates and,
in one area, polynuclear aromatic hydrocarbons. These
objectives will be accomplished by excavating the GRU waste and
1 foot of soil below the GRU waste-soil interface, and
incinerating it in a rotary kiln incinerator. The incinerator
residual, burn pit residuals, and plastic chip will be
solidified and reburied on site. The contaminated stream
sediments will be excavated, returned to the processing area,
and solidified and buried with the other solidified material.
The intent of this remediation is to remove the major source of
contamination from the GRU and burn pit area. Any trace
contaminants or residuals that may remain in the source area
will be collected and treated by the existing groundwater
treatment system.
The intent of the stream remediation is to remove the stream
5050N004
Opera~le Unit 2 60% Remedial Design Report
and Draft Remedial Design work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document control 85050N-0227
Page 2-2
sediment contaminated with plant-related organic compounds,
solidify them, and bury them in the primary source area with the
other solidified materials. After each stream segment is
remediated, sediment samples will be collected and analyzed to
verify that the organic compounds have been removed, or are
below a threshold level agreed upon between Hoechst Celanese and
EPA. The solidified stream sediments will be buried in the
primary source area, upgradient of the· groundwater extraction
system.
2.2 Waste Characteristics
The GRU sludges are predominately ethylene glycol distillation
bottoms (polyester oligimers) containing lesser concentrations
of other identified and unidentified organics. The sludges
typically contain some heavy metals with antimony being the
predominant element. Antimony is present up to 6,400 mg/kg. A
more complete description of the waste is included in the
Remedial Investigation (RI) (S&ME, 1987) and Operable Unit 2
Feasibility Study (FS) (S&ME, 1989a).
From testing done as part of the Operable Unit 2 Feasibility
study (S&ME, 1989a), the following information is estimated for
the GRU material:
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0 moisture
0 carbon -
0 hydrogen
0 oxygen
0 nitrogen
0 sodium -
0 chlorine
-
Operable Unit 2 60% Remedial Design Report
and Draft Remedial Design Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document Control 85050N-0227
Page 2-3
25% average range 6-40%
36.1%
-7.8%
-54.8%
-0.003%
0.004%
-0.024% average range 0.010-0.05%
o ash -1. 3%
0 antimony -0.332% average range 0.0087 -0.64%
0 lead -0.75 mg/kg average range <0.02-53 mg/kg
0 chromium -3. O mg/kg average range <1. 5-40 mg/kg
0 upper -5440 BTU/lb average range <2000-7700 BTU/lb heating
value.·
As part of the testing for the Operable Unit 2 FS (S&ME, 1989a),
IEA ashed a sample of the GRU Waste and performed EP Toxicity
testing on the ash. The results of that analysis show:
0 arsenic -O. 2 mg/kg
0 barium -< 0.1 mg/kg
0 cadmium -< 0.01 mg/kg
0 chromium -< 0.03 mg/kg
0 lead -< 0.005 mg/kg
0 mercury -< 0.0005 mg/kg
0 selenium -< 0. 005 mg/kg
0 silver -< 0.05 mg/kg
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Operable Unit 2 60% Remedial Design Report and Draft Remedial Design Work Plan Hoechst Celanese/Shelby, NC Westinghouse Project 4124-85-050N
Document Control 85050N-0227
Page 2-4
Other materials to be remediated include plastic chip, burn pit
residuals, and contaminated stream sediments.
From the Expanded Characterization study (S&ME, 1989a), the
following analyses results are expected to be representative for
the burn pit residuals:
o moisture -23% average
o antimony -26 mg/kg average
0 lead -32 mg/kg average
0 chromium -238 mg/kg average
range 21-26%
range <20-33 mg/kg
range 9-93 mg/kg
range 30-490 mg/kg
0 upper -2950 BTU/lb average range <2000-5800 BTU/lb heating value (4 of 5 samples <2000 BTU/lb)
Stream sediments were sampled and anaiyzed during Remedial
Investigation (RI) (S&ME, 1987). Phthalate concentrations in
the stream sediments range from 1,500 to 13,000 ug/kg.
Polynuclear aromatic hydrocarbon (PAH) compounds in the stream
sediments were measured at levels ranging from 1,400 to 10,000
ug/kg. The sediments also contain some other organic compounds
at lower concentrations.
2.3 Waste Volumes
Volume estimates of the GRU, burn pit materials, and plastic
chip (collectively known as the source material) were made based
on data obtained from the test drilling and trenching operations 5050N004
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Operable Unit 2 60% Remedial Design Report
and Draft Remedial Design Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document Control 85050N-0227
Page 2-5
(S&ME, 1989a). The volume estimates for the in-place materials
are 1500 cubic yards (cy) for GRU material, 1200 cy of burn pit
materials, 600 cy of plastic chip, 110 cy of stream sediments,
and 500 cy of underlying GRU soils. Figure 2-1 shows the
approximate locations of GRU and burn pit materials. Figure 2-2
shows the approximate locations of stream sediments requiring
remediation.
The EPA Record of Decision (ROD) (EPA, 1989) and subsequent
agreements (Westinghouse, 1989 and EPA, 1989a) require the GRU
material is to be removed and incinerated to the GRU-soil
interface on the sides and to the GRU~soil interface plus 1 foot
on the bottom. This results in approximately 2000 cubic yards
of GRU sludge and soil to be incinerated.
5050N004
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~ Westinghouse Environmental ~ and Geotechnical Services, Inc.
X ___ ...,
-= POt,JSHN:: == ::=. POtl) •2 :-, -
,,,:;:::::-------------
FIGURE 2-1
APPROXIMATE LOCATION OF GRU ANO BURN PIT MATERIAL HC/SHELBY
WESTINGHOUSE PROJECT 4124-85-0SON 5050N08
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( Pl.4.MT PROOUCTIQ\I AREA
0
CJ-c:::::::::::=,~..N
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a
~ Westinghouse Environmental ~ and Geotechnical Services, Inc.
□
!-+--PROPERTY
LINE
NOTE, DARKER STRE/IM SEGMENTS
INDICATE THOSE REQUIRING
REl.4EDIA TION
0 .., .,.
FIGURE 2-2
STREAM SEGMENTS NEEDING REMEDIATION
HC/SHELBY N.C.
WESTINGHOUSE PROJECT 4124-85-OSON
45050N04
, ...
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Operable Unit 2 60% Remedial Design Report and Draft Remedial Action work Plan Hoechst Celanese/Shelby, NC Westinghouse Project 4124-85-050N
Document control 85050N-0227
Page 3-1
3.0 REMEDIATION CRITERIA
This section contains the performance and general criteria that
the contractor is being asked to meet and assure with the
proposed remediation. At this time, drafts of most of the
contractor's proposed operations plans are available and are
incorporated into this document as Appendices I and II.
Packaged together with Section 4.0 -Quality Assurance/Quality
Control (QA/QC), Section 5.0 -Health and Safety (H&S), and 6.0
-Sampling and Analysis (S&A), these exhibits will constituent
the Remedial Action Work Plan for Operable Unit 2 remediation.
3.1 organization Responsibilities
The Hoechst Celanese Shelby facility (HC) is responsible for the
remediation. To assist in the project, HC has retained
Westinghouse Environmental and Geotechnical Services, Inc.
(Westinghouse) to develop the design report, maintain agency
liaison, and assist Hoechst Celanese in verification oversight.
HC has also retained GDC Engineering Inc. (GDC) to perform the
remediation activities. As the contractor, GDC has developed
the Project Operations Plan, which includes the materials
handling plan, surface water control plan, backfilling plan,
5050N018
Operable Unit 2 60% Remedial Design Report and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document Control 85050N-0227
Page 3-2
permitting plan, spill control plan, the Trial Burn Plan, and
the Health and Safety and Quality Assurance/Quality Control
Plans as they relate to their operations. To assist them, GDC
has retained York Research Consultants to perform and evaluate
the trial burn.
The analytical laboratories of Industrial and Environmental
Analysts, Inc. (IEA) and Davis and Floyd, Inc. (D&F) have been
retained by HC to provide analytical services as needed for
verification analysis during the remediation. York Research
consultants will provide the analytical services for the trial
burn.
3.2 Excavation Requirements
3,2,1 General Excavation and Site Preparation
The general areas to be disturbed during the source removal
operation and operations area preparation are shown on Figure
3-1. The disturbed area will be maintained as small as
practical at all times, and the contractor will use ditching,
temporary berms, and erosion control techniques to minimize the
amount of surface water encroaching on the active work areas and
the detrimental effects of channeling water around the work
area.
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'----= =
~ Westinghouse Environmental ~ and Geotechnical Services, Inc.
FIGURE 3-1
LEGEND
X
000
IIIIIIIl GRU MATERIAL
~ BURN PIT MATERIAL
(D INNER TIER WELLS
APPROXIMATE LOCATION OF TREATMENT
EQUIPMENT AND EXCAVATION AREAS
HC/SHELBY
WESTINGHOUSE PROJECT 4124-85-OSON 5O5ONO7
Operable Unit 2 60% Remedial Design Report and Draft Remedial Action work Plan Hoechst Celanese/Shelby, NC Westinghouse Project 4124-85-0SON
Document Control 85050N-0227
Page 3-4
Overburden materials stripped from above the waste pits will be
stockpiled for later reuse in backfilling the excavations and
regrading the site after the remediation. Since this material
may contain low levels of contamination from the invasive
techniques used during the RI/FS, it will be stockpiled inside
the active work area; however, since the intent of this
remediation is to remove the major source of contamination, the
overburden is not being considered for remediation, and will not
be tested before reuse.
During the time that the overburden is stockpiled, it will be
protected from wind and water erosion through use of a physical
cover of a non-contaminating foam, or of other techniques as
appropriate and approved by HC, Westinghouse, and EPA.
Details of the_general excavation and site preparation are
contained in Appendix I, Section 2.2.
J.2.2 stream sediments
Figure 2-2 illustrated the general areas of stream requiring
remediation. The small tributaries indicated are intermittent,
and only contain flow during the wetter season and after heavy
precipitation events. These areas will be excavated by hand if
dry at the time of remediation to minimize the potential
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and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0S0N
Document Control 85050N-0227
Page 3-5
disposal of contaminants and the amount.of water to be treated.
The remainder of the stream to be remediated is mapped as
intermittent, but contains flow a large portion of the year.
This stream section will be excavated by isolating segments of
the stream with temporary dams, pumping the water accumulating
behind the upstream dam around the isolated stream segment,
slurrying the sediment to be removed with a high-pressure water
jet to a collection area behind the downstream dam, and
collecting the resultant slurry and water. The slurry and water
mixture will be removed by vacuum, the solids separated for
solidification, and the water reused for cleaning in subsequent
sections downstreams.
Portions of the stream flows across a rock stream bed. In these
areas, there is little or no sediment, and will be eliminated
from the cleaning operations provided EPA concurrence can be
obtained to omit them.
Verification sampling will be performed immediately after an
area has been cleaned and before the temporary dams isolating a
section are removed. One composite sample will be collected for
each 40-foot segment or piece thereof cleaned, and will consist
of material from at least eight discrete points chosen by the
sampler to best represent the area being verified.
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Operable unit 2 60% Remedial Design Report and Draft Remedial Action Work Plan Hoechst Celanese/Shelby, NC Westinghouse Project 4124-85-0S0N
Document Control 85050N-0227
Page 3-6
Details of the stream remediation can be found in Appendix I,
section 2.2 and in· Section 6.4.4 of this document.
J.2.3 source Materials
The source materials (GRU sludge, burn pit materials, and
plastic chip) will be excavated to their lateral extent as
indicated by the visible contact between the waste and soil.
The excavation will extend vertically to the visible contact
between the burn pit materials and plastic chip, and the
underlying soil. Below the GRU sludge the excavation will
extend to the visible contact between the waste and s_oil, plus
an additional 1 foot as approved by EPA (EPA,·1989a) of
Wes.tinghouse' s request (Westinghouse,· 1989) . The excavations
will be sequenced to minimize the a·mount of excavation open at
any time. The excavated materials will be stockpiled for
processing in accordance with the contractor's plan.
Upon adequate removal of the source materials, the excavations
will be backfilled with soil or solidified materials. After
completing the backfilling, the area will be graded to drain and
blend with the adjacent topography.
No verification sampling will be performed in the excavations
since it is not the intent of the remediation to provide a clean 5050N018
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and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document Control 85050N-0227
Page 3-7
closure. The only verification of suitability of the
excavations is the conformation that the visual removal criteria
were attained, and that 1 foot of soil was removed below the GRU
sludge.
Details of the source material excavation plans are presented in
Appendix I, section 2.2.
3.3 Solidification Criteria
The incineration residuals, burn pit materials, plastic chip,
and stream sediments will be solidified prior to their
backfilling in the primary source area. The solidified
materials will be backfilled in the excavations where the source
materials were buried starting at the northernmost end of the
excavation area and filling southward. After placement, the
solidified material will be covered with at least 18 inches of
soil and graded to drain and blend with adjacent topography.
The solidified waste will will be placed in an area to be
designated as non-buildable for future plant construction.
Th.us, the strength criteria to be met is to have sufficient
strength to withstand equipment loading and to inhibit excessive
deflection of the original excavation sidewall under adjacent
loading. These criteria can be met with a compressive strength
5050N018
Operable Unit 2 60% Remedial Design Report and Draft Remedial Action work Plan
Hoechst Celanese/Shelby, NC Westinghouse Project 4124-B5-050N
Document Control B5050N-0227
Page 3-8
of the solidified matrix of about 7 pounds per square inch
(psi); however, to provide some safety factor, the solidified
matrix will have an unconfined compressive strength of at least
14 psi.
The solidification agent(s) will be selected so that the
solidified mass will not classify as a leachable waste using the
Toxicity Characteristic Leaching Procedure (TCLP) and evaluating
the leachate against the constituents listed in Table 3-1.
North Carolina has established the regulatory level for ethylene
glycol (EG) in groundwater at 7.0 mg/1. Thus, to inhibit
leaching of EG from the solidified material that may have been
solidified without the complete destruction of the EG, we have
established an acceptable EG concentration of l mg/1 in the TCLP
extract as the performance criteria for this compound.
The final criterion for the solidification process is that the
waste and solidifying agent(s) be mixed using a pug mill to
blend the material. Where non-soil components (debris) exist in
the burn pit, processing will be required prior to solidifica-
tion. Non-porous debris is to be surface decontaminated and
placed in the solidified matrix as it is placed. Porous debris
(wood, cardboard, etc.) is to be chipped or crushed and
solidified. Lab scale testing of the proposed solidification 5050N018
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Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0S0N
Document control SS0S0N-0227
Page 3-9
TABLE 3-1
MAXIMUM CONCENTRATION OF CONTAMINANTS
FOR THE TOXICITY CHARACTERISTICS
arsenic
barium
benzene
cadmium
contaminant
carbon tetrachloride
chlordane
chlorobenzene
chloroform
chromium
o-cresol+
m-cresol+
p-cresol+
2,4-D
1,4-dichlorobenzene
1,2-dichloroethane
1,1-dichloroethylene
2,4-dinitrotoluene
endrin ·
heptachlor (and its hydroxide)
hexachlorobenzene ·
hexachlorobutadiene
hexachloroethane
lead
lindane
mercury
methoxychlor
methyl ethyl ketone
nitrobenzene
pentachlorophenol
pyridine
selenium
silver
tetrachloroethylene
toxaphene
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Final Toxic Characteristic
Regulatory Level (mg/1)
5.0
100.0
0.5
1.0
0.5
0.03
100.0
6.0
5.0
200.0
200.0
200.0
10.0
7.5
0.5
0.7
0.13
0.02
0.008
0.13
0.5
3.0
5.0
0.4
0.2
10.0
200.0
2.0
100.0
5.0
1.0
5.0
0.7
0.5
Opera~le Unit 2 60% Remedial Design Report and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC Westinghouse Project 4124-85-0S0N
Document Control SS0S0N-0227
Page 3-10
TABLE 3-1
MAXIMUM CONCENTRATION OP CONTAMINANTS
FOR THE TOXICITY CHARACTERISTICS
(Continued)
contaminant
trichloroethylene
2,4,S-trichlorophenol
2,4,6-trichlorophenol
2,4,5-TP (Silvex)
vinyl chloride
Pinal Toxic Characteristic
Regulatory Level (mg/1)
0.5
400.0
2.0
1.0
0.2
+ o-,m-, and p-cresol concentrations are added together and compared to the threshold.
Reference: 40 CFR 261, pp 11798·118n, March 29, 1990
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Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document Control 85050N-0227
Page 3-11
agent(s) will be performed by GDC using representative samples
of the waste obtained during the early stages of the
remediation.
Details of the solidification program are contained in Appendix
I, Section 2.2.
3.4 Thermal Treatment Criteria
Rotary kiln incineration was chosen for destruction of the GRU
waste by the Operable Unit 2 FS (S&ME, 1989a) and identified in
the ROD (EPA, 1989). This technique was chosen becau.se of the
uniqueness of the GRU waste and the handling problems presented
by its varying consistency. The ROD identified that the
incinerator would be operated in accordance with 40 CFR 264
Subpart o on incineration. The criteria contained in Subpart o
for non-dioxin or similar waste is a Destruction and Removal
Efficiency (DRE) greater than 99.99% of all hazardous
constituents, particulate emissions (corrected to 7% oxygen in
gas) less than 180 mg/dscm (dry standard cubic meter) and
hydrogen chloride (HCl) emissions less than the greater of 4
lb/hr or 1% untreated at the stack gas level.
An additional restriction applies for metals control because of
the volatile metal antimony and non-volatile chromium, both of
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Operable Unit 2 60% Remedial Design Report and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC Westinghouse Project 4124-85-050N
Document Control 85050N-0227
Page 3-12
which are present in the GRU sludge and adjacent soil. Appendix
III to this report presents an analysis based on the EPA
guidance (EPA, 1989b) indicating that greater than 96% of the
antimony must be removed so that detailed monitoring and air
modeling of the incinerator operations are not required.
To establish the conditions under which the incinerator can
operate and attain the specific emissions criteria, Subpart O
requires performance of a trial burn under extreme operating
conditions to establish a conservative range of operational
conditions. During the trial burn, the incinerator is closely
monitored and DREs ar~ calculated for.the compounds designated
as the Principal Organic Hazardous Constituents (POHCs) in the
waste to be burned. The POHCs are typically selected from the
40 CFR 261 Appendix VIII constituents in the waste based on
their concentration and difficulty to adequately incinerate.
To select POHCs for this project, the data generated during the
Expanded Characterization Study (S&ME, 1989a) were reviewed.
This review indicated Appendix VIII constituents in the GRU
sludge at the maximum concentration shown in Table 3-2.
Examination of the list shows that most Appendix VIII
constituents are present at concentrations of less than 2 mg/kg
making them inappropriate for use as a POHC since it would be
impossible to calculate a DRE for the constituent.
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Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document control 85050N-0227
·page 3-13
Ethylene glycol is a 'principal constituent of the sludges, and
it was measured and found to range between 130 mg/kg and 3200
mg/kg in the sludge samples tested. Hence, we propose to use
ethylene glycol as the Principal organic Compound of Concern
(POCC) since it has the highest concentration measured in the
waste, and since it is present at a concentrations which will
allow the DRE calculations to be meaningful. However, the EG
concentrations are variable in the waste. Thus, a sufficiently
large sample will be homogenized to provide a "uniform"
concentration in the feed during'the test burn.
To demonstrate the incineration efficiency of the unit, a
surrogate POHC will be added to the waste used for the trial
burn. For the surrogate·PoHc, we propose using the Class 1
constituent naphthalene (EPA, 1989c) at a concentration of
20,000 mg/kg "uniformly" mixed throughout the feed for the trial
burn. This concentration should provide an adequate amount of
the surrogate in the waste to allow the DRE calculations to be
meaningful.
Detailed descriptions of the incinerator operation and trial
burn procedures are presented in the Trial Burn Plan in Appendix
II.
5050N018
Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document control 85050N-0227
Page 3-14
TABLE 3-2
APPENDIX VIII
*coNSTITOENTS AND CONCENTRATIONS
REPORTED IN GRO SAMPLES
CONSTITUENTS
benzene
chloroform
methylene chloride
bis(2-ethylhexyl)phthalate
trichloroethene
toluene
carbon disulfide
2-butanone
di-n-butyl phthatlate
diethyl phthatlate
1,4-dichlorobenzene
2-chlorophenol
2,4-dichlorophenol
pentachlorophenol
CONCENTRATION mg/kg
DOC BSOSOD-0138
0.30
0.008
0. 007.
1.4
DOC 850SOA-0056
0.006
0.004
0.043
1. 7
0.016
1.6
0.173
0.487
2.2
1.7
0.50
.. 0. 78
0.44
1. 50
* Complete Appendix VIII analyses were not run on the GRU samples. This table was compiled from analyses performed for the Hazardous Substance List (HSL), Target Compound List (TCL), and Tentatively Identified Compounds (TICs) reported by Contract Laboratory Program (CLP) protocols. Thus, additional Appendix VIII constituents may be present.
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Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0S0N
Document Control 85050N-0227
Page 3-15
3.5 Water Treatment criteria
Contaminated or potentially contaminated water will be generated
by the following:
o water separated from the sediments during stream
clean-up
0
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quench water form the air pollution control and ash
handling equipment
waters from decontamination of personnel and equipment
operating in the exclusion zone
storm water falling in the waste excavation or the
operations areas that may become contaminated
These waters will be treated in a portable treatment system set
up by GDC. The treatment system will have sufficient storage
and/or throughput to treat the volume of water anticipated to
the NPDES limits for the Shelby plant at the time that the
remediation is performed. It is anticipated that those
guidelines will be the Organic Chemicals, Plastics and Synthetic
Fibers (OCPSF) guidelines (Table 3-3) scheduled for implementa-
tion in 1991. After treatment in the contractor's water
treatment plant, the treated water will be discharged into
polishing pond B for ultimate discharge to Buffalo creek through
the Shelby Plant's permitted NPDES discharge point.
The planned water treatment system and its operation are
described in Appendix I Section 2.2.
5050N018
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and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document control 85050N-0227
Page 3-16
TABLE 3-3
ORGANIC CHEMICALS, PLASTICS AND SYNTHETIC FIBERS
EFFLUENT GUIDELINES
Effluent Characteristics
BOD
Total Suspended Solids
Effluent Characteristics
acenaphthene
acrylonitrile
benzene
carbon tetrachloride
chlorobenzene
1,2,4-trichlorobenzene
hexachlorobenzene
1,2-dichloroethane
1, 1·, 1-trichloroethane
hexachloroethane
1,2-dichloroethane
1,1,1-trichloroethane
chloroethane
chloroform
2-chlorophenol
1,2-dichlorobenzene
1,3-dichlorobenzene
1,4-dichlorobenzene
1,1-dichlorobenzene
1,2-trans-dichloroethylene
2,4-dichlorophenol
1,2-trans-dichloroethylene
1,3-dichloropropylene
2,4-dimethylphenol
2,4-dinitrotoluene
2,6-dinitrotoluene
ethylbenzene
flouranthene
Daily MaximWII
mq/1
48
115
MaximWII for
any day
ug/1
59
242
136
38
28
140.
28
211
54
54
59
54
268
46
98
163
44
28
25
54
112
230
44
36
285
641
108
bis (2-chloroisopropyl) ether
methylene chloride
68
757
89
190
49
methyl chloride
hexachlorobutadiene
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Monthly Average
mg/1
18
36
MaximWII for
monthly average
ug/1
22
96
37
18
15
68
15
68
21
21
22
21.
104
21
31
77
31
15
16
21
39
153
29
18
113
255
32
25
301
40
86
20
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Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document Control 85050N-0227
Page 3-17
TABLE 3-3
(continued)
ORGANIC CHEMICALS, PLASTICS AND SYNTHETIC FIBERS
EFFLUENT GUIDELINES
Effluent Characteristics
napthalene
nitrobenzene
2-nitrophenol
4-nitrophenol
2,4-dinitrophenol
4,6-dinitro-o-cresol
phenol
bis(2-ethylhexyl)
phthalate
di-n-butyl phthalate
diethyl phthalate.
dimethyl phthalate
benzo(a)anthracene
benzo(a)pyrene
3,4-benzofluoranthene
benzo (k) fluoranthene
chrysene
acenaphthylene
anthracene
fluorene
phenanthrene
pyrene
tetrachloroethylene
toluene
trichloroethylene
vinyl chloride
total chromium
total copper
total cyanide
total lead
total nickel
total zinc
Maxim\1111 for
any day
uq/1
59
68
69
124
123
277
279
279
57
203
47
59
61
61
59
59
59
59
59
59
67
56
80
54
268
2,770
3,380
1,200
690
3,980
2,610
Reference: 52 CFR 42522 -42584, Noventier 5, 1987
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Maxim\1111 for
monthly average
ug/1
22
27
41
72
71
78
15
103
27
81
19
22
23
23
22
22
22
22
22
22
25
22
26
21
104
1,110
1,450
420
320
1,690
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Hoechst Celanese/Shelby, NC Westinghouse Project 4124-85-0S0N
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3.6 Spill Control and Emergency Procedures Criteria
The contractor will develop spill control and emergency
procedures for all aspects of the planned remediation. Spill
control procedures will address of the waste handling,
incineration, and solidification operations, and are intended to
limit the spread of waste within or to non-contaminated areas of
the site. In addition, the contractor will develop contingency
plans to address potential physical and health-related emergency
situations that reasonably could be expected to occur.
Details of the contractor's plans are contained in the
appropriate sections of Appendix I, Section i .and section 4.
3.7 Decontamination criteria
The contractor will establish a decontamination area(s) suitable
for decontamination of both men and equipment. The decontamina-
tion area will be sufficiently large to decontaminate the
largest piece of excavation or hauling equipment planned for
site use, and have an area dedicated for decontamination of
personnel and small equipment such as sampling equipment and/or
health and safety equipment. The decontamination area will be
as close as practical to the operations area to minimize the
size of the exclusion zone. All decontamination solutions will 5050N018
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Operable Unit 2 60% Remedial Design Report and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC Westinghouse Project 4124-85-0SON
Document Control 85050N-0227
Page 3-19
be treated by the contractor's water treatment system prior to
discharge to polishing pond B.
Details of the construction and operation of the decontamination
area are contained in Appendix I, Section 4 and in Section 5.10
of this document.
J.8 Quality Assurance/Quality control criteria
Hoechst Celanese, Westinghouse, and the GDC will all have
Quality Assurance/Quality control (QA/QC) responsibilities for
various aspects of the project. HC and Westinghouse will
operate under the general.guidance set forth ·in section 4.0 of
this document for verification sampling and analysis, and
overall project management of the remediation.
GDC will be responsible for the QA/QC of the equipment necessary
for implementing the remediation including, but not limited to,
instrumentation for the incinerator, metering devices for the
solidification operation, scales or weight belts for determining
the amount of material remediated, etc. The GDC QA/QC plan will
be developed in accordance with the guidance document for
preparing a quality assurance manual (EPA, 1983) and the Region
IV Standard Operating Procedures and Quality Assurance Manual
(EPA, 1986).
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and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document Control 85050N-0227
Page 3-21
an initial review of the incineration system by EPA. No other
permits are required.
3.10 Health and Safety Criteria
HC, Westinghouse, and GDC will all have health and safety
responsibilities on the project. HC and Westinghouse will
operate under· the health and safety guidelines presented in
section 5.0 of this document. GDC has developed a H&S Plan in
accordance with 29 CFR 1910.120. Its purpose will be to
establish requirements for protecting the health and safety of
operating personnel during all activities at the site.
Details of GDC's Health and Safety Plan are contained in
Appendix B to the Trial Burn Plan in Appendix II.
3.11 sampling and Analysis Criteria
sampling and analysis will be the responsibility of Westinghouse
for verification of the stream sediment removal, verification
that the solidified matrix meets_ the design criteria,
verification of the discharge water quality, and possibly
sampling of the incinerator ash, waste feed, exhaust gas, etc.
Westinghouse sampling and analysis operations will be in
accordance with the guidelines in Section 6.0 and of the
5050N018
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Operable Unit 2 60% Remedial Design Report and Draft Remedial Action Work Plan Hoechst Celanese/Shelby, NC Westinghouse Project 4124-85-0S0N
Document Control BS0S0N-0227
Page 3-20
Details of the contractor's QA/QC program are contained in
Appendix I, section 6.
In addition to the field QA/QC provided by HC, Westinghouse, and
GDC, the laboratories providing analytical results have their
own QA/QC protocols. Copies of the QA/QC manuals for IEA, and
D&F are included in Appendix IV to this document. York
Research's QA/QC is included in Appendix A to the Trial Burn
Plan in Appendix II.
3.9 Permitting criteria
In accordance with 40 CFR 300.68 (a) (3), a federal Resource
Conservation and Recovery Act (RCRA) permit is not required for
an on-site Superfund remedial action pursuant to Section 106 of
the Superfund Amendments and Reauthorization Act (SARA).·
However, SARA does contain provisions which require remedial
actions to meet all legally applicable or relevant and
appropriate standards. Performance standards are specified
under RCRA for hazardous waste incinerators and these standards
will be achieved during the operation of the thermal treatment
unit. The North Carolina Department of Environment, Health, and
Natural Resources has requested that a state air quality permit
application be filled out and submitted even though a permit is
not required. GDC will prepare and submit an application after
5050N018
Operable Unit 2 60% Remedial Design Report and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC Westinghouse Project 4124-85-0SON
Document Control 85050N-0227
Page 3-22
laboratories used for analysis.
GDC will be responsible for waste feed sampling, ash sampling,
and incinerator exhaust gas sampling required for implementation
of the trial burn. In addition, GDC will be responsible for
continuous monitoring of certain incinerator operational
parameters. Details of their sampling and analysis plans are
contained in the relevant sections of Appendices I and II.
3.12 Project Schedule
Figure 3-2 illustrates the Operable Unit 2 schedule of events to
occur during remedial desigri and remedial action. The schedule
includes Westinghouse and GDC activities from present (60%
Design phase) through demobilization of the project.
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---------------- - --
SCHEDULE !MONTHS)
1990 1 991
ACTIVITIES -"" -JII.Y .... SlPT OCT ... DCC , .. "' ... .... "" ,..., , ... .... sm
• fflllN,'lWl'Jil'lr.T .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. • la£tlll111',1' .. 'fll...,T
~A.Mll'lf.foc.'°lt:...,,
• 1:r'J&'lll 'II', I'"' 'fll,...,
~A.Mll'lf.¥1.n...,
• =:::l 11s?'CN 1f!Wc.T
EPA Jl[VIU &IC> IIPf"ftOVAl
lHMm1-•T lllll!!!l!!l!ll
11 T[ NtlPAR.l Tl ON
rmll~tr::"T fACILITT -ffllt'~ll.!t_°'INO lW1'. l!lil8il ~11,WI/I'· .,.,,, .. -
r ,AM.~!il WT !0000000
I MC I Nl"ATOII 0,l 111111 lA JI 0911
TIIIAI. 11.191 mm • 1111::i.~.&..T V ' / ' ' / /
nuv.u ION MG ... ING / ' / / / / / / / / / / / / / / ' / A
P'MICl:SS STillMI SlDIIEfl'S -/ /// / / /
IMCIIEU.TION
SU. IDlf ICATlmil I/// / / / /// /// 7, / / / ;
1AC1Cr1u1-. V/ / / / // -, T -, / / / / / /1
SIT[ ,_$TCIUT_IOII 7// , Tl //, /
D[CmnAMINATION ,---, , ' r, ' / /
OC_..lllZATION
V ' / '
CONTIN.JWS AC Tl v IT I[$
I/ 2 Z 7 /I u•nllWJTT[Nl ACTIVITIES
• CCL I YUt,....ES
WESTINGHOUSE PROJECT 4124-85-0SON DATE (@) DESIGNED BY MAS 4/23/QI FIGURE 3-2
DRAWN BY cce 4/23/0I" Westinghouse Environmental OPERABLE UNIT 2 SCHEDULE
CHECKED BY and Geotechnical Services, Inc. HC/SHELBY
FLENN-E ,,,,,,0,10• 4/23/9( WESTINGHOUSE PROJECT 4124-85-050N
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and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document Control 85050N-0227
Page 4-1
4.0 QUALITY ASSURANCE/QUALITY CONTROL
4.1 Project organization and Responsibilities
Westinghouse Environmental and Geotechnical Services, Inc.
(Westinghouse) will be the engineers of record for the source
remediation design at the Shelby facility. The project will be
under the direction of Mr. Everett W. Glover, Jr., P.E., and he
will be supported by Ms. Madelyn Streng, Messrs. Alan M. Lubell,
P.E., and Philip Shipley of Westinghouse and Mr. William R.
Carter, P.E. of Hoechst Celanese (HC). Analytical services will
either be provided by Industrial and Environmental Analysts,
Inc., (IEA) or Davis and Floyd, Inc. Credentials for
Westinghouse, IEA, and Davis and Floyd, Inc., were submitted
with Westinghouse Document Control 85050H-0123, dated October
25, 1988, and the reader is referred to the referenced document
for details. Appendix IV to this report presents updated QA/QC
documents for IEA and Davis and Floyd, Inc.
The quality assurance auditing and monitoring will be conducted
by Westinghouse and HC. Overview of the field operations will
be performed by the Site Manager for Westinghouse and/or the
project engineer for HC. GDC is responsible for installation
and operation of the Thermal Treatment Unit (TTU) and has
5050N016
Operable Unit 2 60% Remedial Design Report and Draft Remedial Action work Plan Hoechst Celanese/Shelby, NC Westinghouse Project 4124-85-0S0N
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Page 4-2
provided a Quality Assurance Project Plan (Section 6.0 in
Appendix I) in general accordance with EPA's Interim Guidelines
and Specifications for Preparing Quality Assurance Project Plans
(EPA, 1983) .
The personnel assigned quality assurance responsibilities shall
be familiar with this Quality Assurance/Quality Control Plan for
the project and will be qualified to observe and evaluate
techniques. Westinghouse personnel shall be cognizant of the
requirements of the Westinghouse corporate quality assurance
program which is incorporated by reference, and also GDC's QA/QC
plan.
In carrying out their duties, the quality assurance personnel
shall have access to all work areas. They shall have the
freedom to identify potential quality problems; initi~te,
recommend, or provide solutions to quality problems through
designated channels; verify implementation of solutions; and
ensure that further processing or action is controlled until
proper disposition of unsatisfactory conditions has occurred.
Quality assurance personnel shall have access to HC project
management and to Westinghouse branch and corporate management
at all levels as required to resolve problems or coordinate
quality concerns.
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Operable Unit 2 60% Remedial Design Report
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Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document control 85050N-0227
Page 4-3
4.2 Quality Assurance Objectives for Measurement Data
The field work will require the use of equipment having
acceptable limits of accuracy and precision. These limits are:
0
0
0
0
0
0
0
portable pressure gages with a range of -10 inches of water column to+ 10 inches of water column. Duplicate analyses shall agree within± 10%. The pressure gages shall be calibrated with a U-tube manometer.
portable pressure gages with a range of o to 100 psi. Duplicate analyses shall agree within l psi. The pressure gages shall be calibrated with compressed air.
portable thermocouples with a range of 32°F to 2200°F. Duplicate analyses shall agree within 6°F. The thermocouples shall be calibrated with a thermal sand bath.
portable pH meters accurate to the hundredth place. Duplicate analyses shall agree within 0.1 pH units. Results shall be recorded to the nearest 0.1 pH unit.
portable specific conductance meters with an analog scale and with a maximum error of± 2.5% plus the probe error. Duplicate analyses shall agree within± 10%. Results shall be recorded to the nearest 10 units for readings under 1000 umhos/cm, and to the nearest 100 units for units for readings over 1000 umhos/cm.
thermometers reading in degrees Celsius or Fahrenheit with a range of -20 to 110 C or -30 to 120°F or
greater. Replicate readings should agree within ±1°. Results shall be recorded to the nearest degree.
engineer's
0.01 foot.
0.01 foot.
rule or tape, manufactured accurate to the
Results shall be recorded to the nearest
The calibration and maintenance of the field equipment will be
discussed further in the Calibration Procedures and Frequencies
5050N016
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Hoechst Celanese/Shelby, NC Westinghouse Project 4124-85-0SON
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Page 4-4
portion (Section 4.5) of this plan.
The laboratory work shall be done following the EPA Contract
Laboratory Program (CLP) Statements of Work for Organic and
Inorganic Analyses (EPA, 1988 and EPA, 1988a) and the
laboratory's own QA procedures.
4.3 Sampling Procedures
Samples may be taken of incinerator feed, stream sediments,
scrubber treatment waters, scrubber air emissions, ash, and
solidified materials at the Shelby Facility. The specific
sampling procedures to be used are included in the Sample and
Analysis Plan. The containers and preservatives to be used will
be supplied by the laboratory in accordance with their QC
manual, or by a qualified supplier such as I-Chem. Samples
containing high concentrations of contamination will be
separated from those with low concentrations.
Samples will be packaged and sent as environmental samples and
transported to the laboratory by courier (i.e. Federal
Express). Packaging requirements for environmental samples are:
1. Complete all documents, tags, and forms appropriate to the samples to be shipped.
2. Ensure that all bottles have the appropriate
labels affixed and all appropriate tags are securely fastened.
5050N016
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Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document Control 85050N-0227
Page 4-5
3. Mark the sample volume level on ·each container
with an indelible marker.
4. Secure container lids to prevent leaks. Tape the
lids for added leak protection, except for water
samples in VOA vials. Use custody seals on lids.
5. Secure the drain plug, if present, at the bottom
of the cooler or shipping carton used for sample
transport with duct tape.
6. Place approximately 1 inch of vermiculite or
equivalent in the bottom of the liner as a
cushioning material and as an absorbent in case of
leakage.
7. Seal each sample container in individual plastic
bags, and place upright in the lined cooler or
shipping carton.
8. Repackage ice in small, sealed plastic bags and
place loosely in the cooler or shipping carton.
Reusable, prepackaged ice packs may be used
instead of ice. Do not pack ice so tightly that
it may break glass bottles or prevent addition of
sufficient cushioning material.
9. Place small containers, such as 40 ml septum vials
for VOAs, in small sealed plastic bags. When
shipping these with larger containers, additional
cushioning material will be added to prevent them
from being crushed.
10. Fill the remaining space in the lined cooler or
shipping carton with cushioning material.
11. Place the documents accompanying the samples in a
sealed, large plastic bag attached to the inside
of the cooler or shipping carton lid.
12. Close the lid of the cooler or shipping carton and
fasten the latch.
13. Affix signed custody seals to both ends of the
cooler or shipping carton in such a manner that
they must be removed or broken in order to open
the cooler or shipping carton.
14. Wrap duct or fiber tape around both ends of the
cooler or shipping carton several times, each time
5050N016
Operable Unit 2 60% Remedial Design Report · and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC Westinghouse Project 4124-85-0SON
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Page 4-6
slightly overlapping the custody seal.
15. Mark the cooler or shipping carton on the outside with the following information: name and address of laboratory, return address, and arrows indicating the "This End Up" on all four sides.
4.4 Sample Custody
The sample custody and chain-of-custody procedures will
be:
1.
2 •
3.
4.
5050N016
Place the sample in an appropriate bottle and log the following information in the field notebook:
o sample number
0
0
0
0
0
date
name(s) of sampler(s)
time (military)
location or station identifier
comments
Fill in sample tag (Figure 4-1) or label with: o project name and number
o sample number
o date
o time (military)
o location or station identifier o type of preservative used, if any o parameters to be analyzed
o sampler's signature
Place samples in coolers or shipping cartons. Samples are to remain in the custody of the samplers until they are brought to the sample processing area.
Complete chain-of-custody forms (Figure 4-2) including:
o sample number(s)
o date
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Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document Control 85050N-0227
Page· 4-7
e
Figure 4-1
Sample Tag
0
Westlnghouae Envtronmental Servlcet
Preservative:
J Yea □ No □
-ANALYSES
§ BOO Anlana
Solldl ~(111111-
COO,TOC,Nutrtenll
l PNo!OIICI
Mera.y
Metall
I Cyanjde
OilandGI-.
°'VIIIICIOOMS
PnorltyPoltu1anll
Volattle °'VlnlCI
Peellcldlll
PCS
I Rena,a;
! ,_ .... ... -....
A 18011
5.
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Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document Control SSOSON-0227
Page 4-8
project name and number
o name(s) of sampler(s)
0
0
0
0
time (military)
type (grab or composite)
number of samples
volume of bottles
o parameters to be analyzed
0 sample tag numbers
0 signature of personnel releasing samples
Relinquish the samples to the person designated to receive them .and have the chain-of-custody form signed, and record the time and date of transfer.
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6. Log the name of the individual receiving the sample and I the time relinquished in the sampler's field notebook.
7. Tape the lids closed and affix custody seals over the I sample lids.
s. Prepare sample tags, signed by the sampler(s) and attach to the bottle. Record the tag numbers in the I remarks column on the appropriate chain-of-custody form.
9. Record the sample numbers, receipt of samples, tag I numbers, date and time samples were taken, etc., in the sample tracking log books (one for organic samples and 1 one for inorganic samples).
10. Package the samples and deliver according to the protocols described in this plan or store in a •. designated refrigerator until packed for shipping.
5050N016
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Proiec1 No
I
Proiect Name
Samplers: Is1gnatureJ
S1at1on 0 a E Dale T,me 0 • No. " a
.
AehnQutshed by. tsIgna1ure1 Oatw.
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AehnquIshed by: (signature) Date:
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Rehnq1.u1hed by: (s1gna1ure) Date:
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Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document control 85050N-0227
Page 4-9
Figure 4-2
chain of custody Form
CHAIN OF CUSTODY RECORD . • e jj e 0 " 0
i
Branch:
Department
REMARKS
E S1a11on Loca110n 0 z
nme· Aeca1 .... ed by:js1gna1ure) Aelmqu1ahed by: (aignetural Data: Time: Received by:(signaturel I Time: Received by:(11gnatura) Relil'IQursned by: (s1gnature1 Date Time: Aec01ved by:(signatura)
I Time: Rec:etved by:ts1gna1uraJ Cate: I Time: Aamarka
"' OISTRIBUT!ON: Wh119 and Canary copn accom~"'111,11mple t,h1~nt.
Pink copy ma1ntam.O WI Illa.
5050N016
Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document Control 85050N-0227
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4.5 calibration Procedures and Frequencies
4.5.1 Field Equipment
The time of calibration and serial number of each piece of
equipment should be recorded in a field equipment log book.
Equipment should be calibrated before sampling is started. All
field equipment will be maintained and calibrated per
manufacturers' instructions.
Portable pH meters will be checked before each use for
mechanical and electrical functions, weak batteries, and cracked
or fouled electrodes. The meter will be checked against buffer
solutions at pH 4 and 7 before sampling. The buffer solution
containers should be refilled each day of use from fresh
solution stock. Portable pH meters to be used will be accurate
to the hundredths place. Duplicate analyses shall agree within·
0.1 pH units. Results shall be recorded to the nearest 0.1 pH
unit.
Portable specific conductance meters will be checked before use.
Batteries will be checked and the internal calibration
procedures followed using the manufacturer's instruction guide.
Portable specific conductance meters to be used must be supplied
with an analog scale and with a maximum error of ±2.5 % plus the 5050N016
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Westinghouse Project 4124-85-050N
Document control 85050N-0227
Page 4-11
probe error. Duplicate analyses shall agree within'±lO %.
Portable Ecolyzer explosimeter/oxygen meter (or equivalent)
shall be accurate to within± 0.2 % concentration. Oxygen
readings will be recorded to 0.1 %. The portable
explosimeter/oxygen meter will be checked before use for the
battery charge. The instrument has a built-in, self-checking
system which checks the warning lamps and available alarms to
confirm operation, and will be checked before each day's use.
The oxygen sensor will be cleaned and/or replaced as needed. A
functional check will be performed by breathing on or placing a
hand over the probe (oxygen meter) and/or using a calibration
gas (explosimeter), per the .manufacturer's recommendations.
Portable photoionization detector (HNu or equivalent) must be
factory-calibrated in parts per million (ppm) by volume of
benzene. Range will be 0.1 to 2000 ppm with a lower detection
limit of 0.1 ppm. Values will be recorded to the nearest mark
on the scale times the multiplication factor. The HNu will have
the battery, lamp, and fan checked before each field use.
Isobutylene will be used as a field-calibration gas before each
day's field use to check the sensitivity of the lamp. The unit
will then be checked with organic vapor from a "magic marker" or
similar volatile substance. The probe will be cleaned and/or
replaced as needed.
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Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document Control 85050N-0227
Page 4-12
Portable Foxboro organic vapor analyzer (OVA) (or equivalent)
must have reporting values in ppm, with a range from o to 1000
ppm. The OVA must have a sensitivity to 0.1 ppm for methane.
Values will be recorded to the nearest mark on the scale times
the multiplication factor. The organic vapor analyzer (OVA)
will be checked before each field use. The battery charge,
probe/side pack assembly leakages, and possible cylinder
leakages will be checked. A step-by-step start-up procedure
from the instruction manual will be followed for the OVA, and
the OVA's response will be checked with organic vapor from a
"magic marker" or similar volatile substance.
Equipment su~h as thermometers, engi~eer's rules, surveyor's
tapes and other measuring devices will not be calibrated.
4.5.2 Laboratory Equipment
Industrial and Environmental Analysts, Inc. (IEA) is proposed as
the primary supplier of analytical services on this project.
IEA has a Quality Assurance/Quality Control program in place and
has been used on the Feasibility Study for OU 2 and Operable
Unit 1 remedial action portions of the project. The IEA Quality
Assurance Manual, dated August 1988 (Appendix IV), contains the
procedures and frequency of calibration for the type of
equipment used by the laboratory.
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Hoechst Celanese/Shelby, NC
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Page 4-13
4.6 Analytical Procedures
The analytical procedures to be used are those in the Contract
Laboratory Program Statement of Work for Organics, February
1988, and Statement of Work for Inorganics, July 1988, or those
modified for the project and approved by EPA for this project.
4.7 Data Reduction, Verification, and Reporting
Data reduction during the remedial action reporting task will be
the responsibility of the individual providing the evaluation
and/or writing the report, and verified by a second person for
completeness and needed corrections,. Checked and/or corrected
data will be initialed and dated by the individual performing
the task.
For the laboratory, internal data reduction and verification are
covered in the testing and QA procedures followed by the
laboratory.
4.8 Internal Quality Control Checks
Spikes, blanks, and duplicate samples will be analyzed to
provide a quality control check for the laboratory.
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Data packages can be submitted to EPA for review, if requested,
or the results of the QA checks can be addressed as part of the
submittal of routine monitoring reports. The QA samples will
include:
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Spiked samples: Selected samples will be spiked by the laboratory with surrogate compounds to check for analytical recovery.
Blank Samples: Distilled/deionized water and organic-free water will be used as a reagent or method blank. These samples will be submitted from the field along with other water samples taken from the site and numbered accordingly.
As a Westinghouse quality control check, the following samples
will be sent to the laboratory:
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Duplicate Samples: Selected samples will be duplicated simu·1taneously from .the same ·source ·under similar conditions, placed in separate containers, and sent to the laboratory for analysis.·
Equipment Blanks: Control samples will be selected after equipment decontamination to assess the thoroughness of the cleaning procedures.
The member of the Westinghouse field sampling crew designated as
the quality control officer will be responsible for collecting
and submitting duplicate samples and equipment blanks.
The QA/QC samples will comprise up to 10% of the total number of
samples. Internal laboratory QA/QC samples such as matrix
spikes and matrix spike duplicates will be in accordance with
the CLP protocols.
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Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0S0N
Document control SS0S0N-0227
Page 4-15
4.9 Performance and system Evaluation
In addition to the internal quality control checks, EPA
personnel or their oversight contractors may audit the project
and periodically split samples with the sampling team. EPA's
audit will also include the analysis of spiked and blank samples
submitted by EPA, or an EPA contractor, to Westinghouse for
analysis. Access will be provided for Agency personnel at
reasonable times, and the scheduling of the audit(s) will be at
the discretion of EPA.
4.10 Preventive Maintenance
4.10.1 General
Project team members need to be able to respond rapidly to a
variety of field and sampling situations, using both routine and
specialized equipment. This equipment will be maintained in
acceptable condition at all times, or will be noted as
unsuitable until repaired and/or recalibrated.
4.10.2 sampling and Analytical Equipment
The sampling and analytical equipment for air, soils, surface
water, sludges, and solidified material will be maintained to
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Document Control 85050N-0227
Page 4-16
manufacturer's specifications and in operational condition.
This equipment includes such items as samplers, spoons, buckets
and the field equipment listed in Section 4.5.1. Routine
preventive maintenance, inspections, and checkouts will be
conducted by the members of the field crew to assure proper
operation of the.various pieces of equipment. Stainless steel,
glass and/or teflon items will be inspected for excessive wear,
cracks, and scratches and will be replaced when necessary.
Field equipment will be calibrated and maintained according to
specifications. These items will be repaired and maintained
on-site when feasible or returned to the manufacturer for
extensive repairs. Back-up equipment will be available so that
tasks are not delayed.
4.10.3 Support Equipment
support equipment is defined as all equipment not previously
discussed that may, at some point, be required for completing an
environmental monitoring or measurements task. support
equipment will be periodically inspected by the person
responsible for its use to maintain the performance standards
for proper and efficient execution of tasks and
responsibilities. Appropriate and sufficient replacement parts
will be available for these categories of equipment so that
sampling and monitoring tasks are not substantially impeded or 5050N016
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4,11 Specific Routine Procedures used to Assess Data Precision, Accuracy, and completeness
The CLP methods and procedures incorporate the methods to
evaluate the data precision and accuracy of analyses, and
completeness of reporting required for each parameter. EPA
methods and procedures (EPA, 1983a) and/or (EPA, 1986a)
incorporate requirements to assure quality of the data.
4,12 Corrective Action
Each individual responsible,for specific or general tasks will
be knowledgable of the requirements of this Quality Assurance/
Quality Control Plan as they relate to that work task, and the
proper performance of the work according to those requirements.
The on-site Quality Assurance Officer will be responsible for
conducting routine work evaluations. If the QA officer
discovers that the requirements of this Quality Assurance/
Quality Plan are not being met, corrective measures will be
taken immediately to bring the work back into compliance with
the Plan.
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4.13 Quality Assurance Reports to Management
Quality assurance reports concerning field quality assurance
checks or audits will be periodically incorporated in the
progress reports. If necessary, separate quality assurance
reports will be written.
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Page 5-1
5.0 HEALTH AND SAFETY PLAN
5.1 Organization and Staff Responsibilities
s.1.1 Personnel
Lead organization Management
The lead organization for health and safety is Westinghouse,
whose management is responsible for providing the necessary
equipment, facilities, personnel, and support for field
activities. Aspects of field support may be delegated to HC for
implementation. Additionally, GDC is responsible for the
implementation of the Health and safety Plan for the operations
personnel. In these events, Westinghouse management is
responsible for quality assurance on the tasks.
GDC is responsible for providing the necessary equipment,
facilities, personnel, and support of their field activities.
GDC shall provide a health and safety officer who will direct
the development of their site health and safety plan, train
employees, and provide overall management of GDC's health and
safety requirements covered in the site health and safety plan.
The health and safety plan will be in conformance with the
requirements of 29 CFR 1910.120.
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Page 5-2
Certain aspects of field support may be delegated to HC
personnel for implementation. In this event, Westinghouse
management is responsible for quality assurance on the tasks.
Technical support
Off-site technical support will be provided by individuals with
specific expertise, as needed. This may include chemists,
engineers, industrial hygienists, toxicologists, etc.
Assignment of off-site technical personnel will be made by
Westinghouse. ·
Medical Support staff
The medical support staff includes company retained physicians,
medical personnel administering the medical monitoring programs,
in-house medical personnel, and medical services personnel near
the site who may be called upon in an emergency.
s.1.2 on-site Personnel
Site management duties for Westinghouse will be provided by
personnel designated by the Project Manager, and for HC by Mr. 5050N019
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Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document Control 85050N-0227
Page 5-3
Bill carter. The Westinghouse Site Manager is responsible for
Westinghouse activities, including coordinating health and
safety activities for the project, and reports to Westinghouse
management. The Site Manager will coordinate with Mr. Carter to
see that the appropriate level of health and safety precautions
are being taken.
Specific duties for the Westinghouse Site Manager include:
o assigning Westinghouse field teams to specific tasks and ensuring that all team members are qualified
o initiating the site safety program during a pre-mobilization site safety meeting
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conducting on-site health and safety meetings as required by changes in site activities, amendments to the• site safety plan, or other situations with the potential for impact on the health and safety of site personnel·
selecting and maintaining personal protective equipment
o enforcing compliance with the site safety plan
0 controlling entry and exit from limited access areas
o monitoring site personnel for signs and stress
Following employee training under the auspices of an acceptable
site health and safety plan, a site safety coordinator working
under the direction of the health and safety officer may be
utilized for the continued safety and health surveillance. The
site safety coordinator, along with the health and safety
officer, shall have authority to act on all health and safety
measures and to establish new-controls as needed. The duties of 5050N019
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Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0S0N
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GDC's health and safety personnel are included in the their site
health and safety plan, and will be subject to review by
Westinghouse. If it is determined that the personnel assigned
are not providing adequate controls, GDC shall be required to
obtain the services of other health and safety personnel.
The health and safety officer shall be a GDC representative,
with overall responsibility for the preparation, implementation,
and enforcement of the site health and safety plan. The health
and safety officer shall have specialized experience in the
hazardous waste or chemical industry with hazards similar to
those anticipated on this project. The health and safety
officer shall have a broad working knowledge of state and
federal occupational safety and health regulations. In
addition, the health and safety officer shall have demonstrable
expertise in air monitoring techniques and in the development of
respiratory protection programs. The name, qualifications, and
work experience of the health and safety officer is included in
the site health and safety plan.
The site safety coordinator shall be a GDC representative
assigned to the site on a full-time basis for the duration of
the project with functional responsibility for implementation
and.enforcement of the site health and safety plan. The site
safety coordinator shall have experience in the chemical or
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Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document Control 85050N-0227
Page 5-5
hazardous waste industry, a sound working knowledge of federal
and state occupational safety and health regulations, and
experience in air monitoring techniques and the administration
of respiratory protection programs. The site safety coordinator
shall also have current certification in CPR and multimedia
first aid.
The health and safety officer shall be qualified in first aid
and CPR. In addition other first aid and CPR qualified
personnel shall be available on-site. Certifications shall be
by the American Red Cross.
A site safety coordinator shall be present for each shift. The
health and safety officer shall conduct periodic inspections as
necessary to determine the overall effectiveness of the site
health and safety plan. Any deficiencies shall be submitted to
Westinghouse in writing, and the site health and safety plan
will be modified accordingly. Should the deficiencies be of a
nature to present an immediate danger, the health and safety
officer shall stop all work in the area, immediately initiate
changes as required, and notify Westinghouse and Hoechst
Celanese.
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s.1.J site security
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Site security will be provided by Hoechst Celanese Security.
s.2 work Practice controls
s.2.1 Standing Orders
The Site Manager shall develop and post a set of standing orders
governing work practices and shall ensure that each person
entering the site is aware of these standing orders. Standing
orders may be altered/amended based on the development of new
information. ··At a minimum, · standing :orders will include the
following:
o Activities which require hand-to-mouth contact such as eating, drinking, smoking, etc. are prohibited except in designated areas.
o All personnel on-site must be briefed on all known hazards associated with area prior to entry.
s.2.2 Work zones
The site project area will be divided into three distinct work
areas. The three separate classifications of zones for the
thermal treatment project site are the exclusion zone, the
contamination reduction zone, and the support zone. The areas
will be delineated through the use of barrier tape. Figure 2-4 5050N019
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Hoechst Celanese/Shelby, NC
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Document Control BSOSON-0227
Page 5-7
through 2-7 in Appendix I illustrate these areas.
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exclusion zone
The exclusion zone is the work area where contamination
does or could occur. This zone will encompass the feed
preparation area and existing contaminated area.
contamination reduction zone
The contamination reduction zone is located between the
exclusion and support zones and provides a transition
zone between contaminated and clean areas of site.
This zone shall be located directly outside and
adjacent to the exclusion zone. To prevent cross
contamination and for accountability purposes, all
personnel shall enter and leave the exclusion zone
through the contamination reduction zone where
decontamination procedures will occur.
support zone
The support zone shall be the uncontaminated.area from
which site activities shall be directed. Thermal
treatment system components, control facilities, and
other support facilities will be located in this area.
It is essential that contamination from the exclusion
zone be kept from this area.
5.3 Site Control
The following site control will be implemented during remedial
action at the Shelby Facility.
5.3.1 Pit Excavation
The areas to be excavated will be enclosed by the exclusion
zone. The exclusion zone will be clearly marked with barrier
tape to limit unauthorized entry. Located outside and adjacent
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to the exclusion zone is the contamination reduction corridor in
which field personnel and support equipment will be
decontaminated. The support zone will be located adjacent to
the contamination reduction zone.
5.3.2 stream Excavation
A corridor on either side of the stream, will be considered the
exclusion zone during the stream excavation task. Figure 2-2
depicts the layout of the streams requiring excavation.
5.4 safety Precautions
The waste types expected to be encountered during this phase of
work at the Shelby Facility may be in the form of liquids/
sludges, solids, dusts, and vapors/gases. Table 5-1 list·s
Appendix VIII compounds which were identified in GRU samples.
Included in the table are permissible exposure limits in air,
ceiling limits (air), and harmful effects and symptoms.
5.4.1 Liquids/Sludges
Liquids/sludges may be difficult to contain and are easily
splashed onto unprotected body surfaces. caution will be
exercised when working with or near suspected contaminant-
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CONSTITUENTS
ethylene glycol*
naphthalene*
benzene·
chloroform
methylene chloride
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TABLE 5-1
PRECAUTIONARY STANDARDS OF HAZARDOUS CHEMICALS
PERMISSIBLE
EXPOSURE
LIMIT IN AIR
CEILING LIMIT HARMFUL EFFECTS ANO SYMPTOMS (LOCAL)
no Federal Standard 50 ppn (for vapor) None
10 ppn TWA
10 ppn TWA
10 ppn TWA
500 ppn TWA
N.A.
25 ppn
50 ppn
1000 ppn
Naphthalene is a primary irritant and
causes erythema and dermatitis upon
repeated contact, It is also an allergen
and may produce dermatitis in hypersen·
sitive individuals. _Direct eye contact
with the dust has produced irritation and
cataracts.
Exposure to liquid and.vapor may produce
primary irritation to skin, eyes, and
upper respiratory tract. If the liQuid is
aspirated into the lung, it may cause
pulmonary edema and hemorrhage. Erythema,
vesiculation, and dry, scaly dermatitis
may also develop from defatting of the
skin.
May produce burns if left in contact with
the skin.
Repeated contact with methylene chloride
may cause a dry, scaly, and fissured
dermatitis. The lic:p.Jid and vapor are
CONSTITUENTS
bis(2-ethylhexyl)phthalate
trichloroethene
toluene
carbon disulfide
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TABLE 5-1
PRECAUTIONARY STANOAROS OF HAZAROQJS CHEMICALS
(Continued)
PERMISSIBLE
EXPOSURE
LIMIT IN AIR
5 rr,;tm3 TWA
100 ppn TWA
200 ppn
20 ppn TWA
CEILING LIMIT
N.A.
300 ppn
30 ppm
HARMFUL EFFECTS ANO SYMPTOMS (LOCAL)
irritating to the eyes ard upper
respiratory tract at higher
concentrations. If the liquid is held in
contact with the skin, it may cause skin
burns.
Irritation of the eyes and nucous
meri>ranes; nausea; diarrhea.
Exposure ·may cause i. r~.i tat ion of the
eyes; nose, and throat. The liquid, if
splashed·in the eyes, may cause burning
irritation and damage, Repeated or
· prolonged skin contact with· the liquid may
cause dermatitis.
May cause irritation of the eyes,
respiratory tract, and skin. Repeated or
prolonged contact with liquid may cause
removal of natural lipids from the skin,
resulting in dry, fissured dermatitis.
The liquid splashed in the eyes may cause
irritation and reversible damage.
Carbon disulfide vapor in sufficient
quantities is severely irritating to eyes,
skin, and nucous ment,ranes. Contact with
liquid may cause blistering with second
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CONSTITUENTS
2-butanone
di-n-butyl" phthalate
diethyl phthalate
1,4-dichloroebenzene
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TABLE 5-1
PRECAUTIONARY STANDARDS OF HAZAROOJS CHEMICALS
(Continued)
PERMISSIBLE
EXPOSURE
LIMIT IN AIR
200 -TWA
5 1!J3/m3 TWA
CEILING LIMIT
N.A.
N.A.
no Federal Standards N.A.
75 -
N.A.
HARMFUL EFFECTS AND SYMPTOMS (LOCAL)
and third degree burns. Skin
sensitization may occur. Skin absorption
may result in localized degeneration of
peripheral nerves which is most often
noted in the hands. Respiratory
irritation may result in bronchitis and
eff1)hysema, though these effects may be
overshadowed by systemic effects.
Irritation of eyes and nose; headaches,
dizziness, vomiting.
Irritation of nasal passages and upper
respiratory system; stomach irritation;
light sensitivity
Diethyl phthalate has few acute or
chronic toxic properties and seems to be
devoid of any major irritating or
sensitizing effects of the skin.
Headaches; eye irritation, periorbital
swelling, profuse rhinitis; anorexia,
nausea, vomiting weight loss, jaundice,
cirrhosis.
CONSTITUENTS
Operable Unit 2 60% Remedial Design Report and Draft Remedial Action work Plan
Hoechst Celanese/Shelby, NC Westinghouse Project 4124-85-0S0N
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TABLE 5-1
PRECAUTIONARY STANDARDS OF HAZARDClJS CHEMICALS
(Continued)
PERMISSIBLE
EXPOSURE
LIMIT IN AIR
CEILING LIMIT HARMFUL EFFECTS ANO SYMPTOMS (LOCAL)
2-chlorophenol no limits set N.A. N.A.
2,4-dichlorophenol no limits set N.A.
pentachorophenol N.A.
5O5ONO19
* All constituents, except ethylene glYcol and
naphthalene, are Appendix VIII ~onstituents
reported in GRU sa,rples. concentrations are
reported in Table 3-2.
N.A. Information not available in referenced
materials.
References:
Marshall Sittig, Handbook of Toxic and Hazardous
Chemicals and Carcinogens. 2nd ed., Noyes
Publications, New Jersey, 1985.
occupational Health Services, Inc., New Jersey.
N.A.
Irritation of eyes, nose, and throat,
sneezing and coughing, weakness, anorexia,
weight loss, sweating, headaches,
dizziness, nausea, ~om,iting, dyspnea,
chest pains, fever, dermatitis
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Page 5-13
containing liquids. Spillage of contaminated liquids or sludges
will be avoided. However, a spill contingency plan is provided
in the GDC operation plan.
5.4.2 Dusts
Dust or fugitive emissions are particulate in nature and, like
vapors, are readily inhaled into the respiratory system.
Particulates will become more pronounced during dry conditions,
particularly during the excavation and transport of waste
material. Methods such as covering and wetting will be
implemented, as necessary, to curtail fugitive emissions.
5.4.3 vapors/Gases
Vapors may displace oxygen in low-lying or enclosed areas; may
or may not excite the olfactory senses, and are readily inhaled
into the respiratory system. At sea level, ambient air must
contain at least 19.5 percent oxygen by volume. At lower
percentages, air-supplied respiratory protective equipment is
needed. To ensure personnel hea.lth and safety, areas where
vapors may be present will be monitored with an organic vapor
analyzer (OVA), and personnel positioned upwind of work
activities (whenever possible) until contamination levels are
established and appropriate personal protection levels are
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5.4.4 Physical Hazards
Excavation/construction may cause serious injury to fingers,
hands, and feet which may be inadvertently caught in moving
machinery. Extreme care should be taken to avoid contact with
moving parts. Loose clothing should also be secured (for
example, taping loose portions of Tyvek coveralls) to minimize
the potential for entanglement with moving machinery.
5.4.5 Weather conditions
Weather-related hazards may also occur during the excavation/
construction process.
Individuals working outdoors in temperatures at ·or below
freezing may be frostbitten. Extreme cold for a short time may
cause severe injury to the surface of the body or result in
profound generalized cooling, causing death. Areas of the body
that have a high surface-area-to-volume ratio, such as fingers,
toes, and ears are the most susceptible. The prevention of
systemic cold stress includes providing shelter where warmth is
available, the utilization of thermal clothing applied in
layers, and the availability of warm/hot liquids (coffee, cocoa, 5050N019
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Field operations during the summer months can create a variety
of hazards to the employee. Heat cramps, heat exhaustion, and
heat stroke can be experienced, and if not remedied, can be
health or life threatening. Therefore, it is important that all
employees be able to recognize symptoms representative of these
conditions as well as being capable of remedying the situation
as quickly as possible.
Heat cramps usually affect people who work in hot environments
and perspire a great deal. Loss of salt from the body causes
very painful cramps of the legs and abdominal muscles. Heat
cramps may also result from drinking ice water or other drinks
either too quickly or in too large a quantity. The most common
symptoms of heat cramps are muscle cramps in the legs and
abdomen, pain accompanying cramps, faintness, and profuse
perspiration. Heat exhaustion may be associated with heat
cramps. It is brought about by the pooling of blood in the
vessels of the skin. The heat is transported from the interior
of the body to the skin surface by the blood. The skin vessels
become dilated, and a large amount of blood is pooled in the
skin. This condition, plus the blood pooled in the lower
extremities when in an upright position, may lead to an
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physical collapse. The most common symptoms of heat exhaustion
are weak pulse, rapid and usually shallow breathing, generalized
weakness, pale, clammy skin, profuse perspiration, dizziness,
and unconsciousness. Heat stroke is a profound disturbance of
the heat-regulating mechanism, associated with high fever and
collapse. Sometimes this condition results in convulsions,
unconsciousness, and even death. The most common symptoms of
heat stroke are sudden onset, dry, hot, and flushed skin,
dilated pupils, early loss of consciousness, full and fast
pulse, breathing deep at first, later shallow and almost absent,
and body temperature reaching 105 and 106 degrees or higher.
In the case ·of_ heat cramps. or heat exhaustion, "Gatorade" or its
equivalent is suggested as part of the treatment regime. This
type of liquid refreshment will replace needed electrolytes to
the system. Without these electrolytes, body systems cannot
function properly, thereby enhancing the represented health
hazard. Therefore, when working in situations where the ambient
temperatures and humidity are high, the health and safety
officer must:
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assure that all employees drink plenty of fluids ("Gatorade" or its equivalent)
assure that frequent breaks are scheduled so overheating does not occur
revise work schedules, when necessary, to take advantage of the cooler parts of the day (i.e. 5:00 a.m. to 11:00 a.m. and 6:00 p.m. to nightfall)
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When protective clothing must be worn, the suggested guidelines
relating ambient temperature and maximum wearing time per
excursion are:
Ambient Temperature Maximum Wearing Time per Excursion
Above 90 degrees F 15 minutes
85 -90 degrees F 30 minutes
80 -85 degrees F 60 minutes
70 -80 degrees F 90 minutes
60 -70 degrees F 120 minutes
50 -60 degrees F 180 minutes
A method of measuring the effectiveness of an employee's rest-
recovery regime is by monitoring the heart rate. The "Brouha
guideline" is one such method.
o Count the pulse rate for the last 30 seconds of the
first minute of a 3-minute period, the last 30 seconds
of the second minute, and the last 30 seconds of the
third minute.
0 Double the count.
If the recovery pulse rate during the last 30 seconds of the
first minute is at 110 beats/minute or less and the deceleration
between the first, second, and third minutes is at least 10
beats/minute, then the work-recovery regime is acceptable. If
the employee's heart rate is above that specified, a longer rest
period will be required, accompanied by an increased intake of
fluids.
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s.s Education and Training
Westinghouse, HC, and GDC shall staff all work positions in the
exclusion and contamination reduction zones with personnel who
have successfully completed a classroom occupational hazards
training program that meets or exceeds the requirements of 29
CFR 1910.120. Certification shall be submitted for each person
assigned to such work indicating that he/she has successfully
completed an OSHA training program prior to entering the site.
Training shall include at a minimum:
o hazard communication to conform with 29 CFR 1910.1200
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acute and chronic effects of.toxic chemicals
routes of exposure (skin penetration, inhalation, and ingestion) and specific operations that could result in exposure
need for personal protection (effectiveness and limitations)
proper use and fitting of all types of respirators to be used on site (to include drills in donning an emergency respirator)
medical surveillance program
o on-site prohibitions including:
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facial hair which interferes with respirator seal
contact lenses
eating, smoking, chewing
personal articles such as watches, rings, etc.
working when ill
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Westinghouse Project 4124-85-0SON
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establishing on-site work zones
engineering controls and safety work practices associated with employee's work assignment, including dust control measures and use of buddy system
5.6 Medical surveillance
All Westinghouse HC, and GDC personnel will be enrolled and
current in the medical monitoring program meeting the following
minimum requirements:
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baseline physical examination prior to any hazardous waste site operations. Baseline physical to include respiratory certification for persons using air-purifying respirators or self-contained breathing apparatus
annual physical examination by anniversary of baseline examination. Annual physical to include respiratory certification for persons using air-purifying
respirators of self-contained breathing apparatus
exit physical examination for personnel terminating employment or exiting work associated with hazardous waste site activities
5.7 Ambient Field Monitoring
During field operations ambient air quality will be continuously
monitored with an OVA or other appropriate device. The follow-
ing procedures will be adhered to for the specific work task.
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5.7.1 Excavating
o establish air quality in background
0 monitor personnel breathing zones
o action levels/elevations in breathing zones will be initially maintained in Level D. If air quality exceeds 50 ppm over background on an OVA then Level C will be implemented.
5.7.2 Decontamination
o establish background air quality
o monitor breathing zone
o Level D protection will be required for decontamination operations
5.7.3 Rotary Kiln sampling
o establish background air quality
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maintain Level· D protection, if air quality exceeds 50 ppm over background, implement Level C protection.
5.8 Levels of Protection
Level D Protection consists of:
Dl -
D2 -
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Tyvek coverall, hard hats, inner surgical gloves, outer chemical resistant work gloves, steel toe and shank (chemical resistant) boots, safety glasses or safety goggles, hearing protection during noisy operations, and no jewelry worn on hands.
In consideration of site conditions, Level D2 may be enacted by the discretion of the site manager. This level includes all level Dl protection with the option to omit Tyvek coveralls and outer chemical gloves.
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Level c Protection consists of:
Cl -Saranax coverall or Tyvek coverall, hard hats, inner surgical gloves, outer chemical resistent work gloves, steel toe and shank (chemical resistant) boots, booties, hearing protection during noisy operations (if.applicable),
respirator, GMC-H or equivalent cartridges. This level will be invoked if breathing air in the working area exceeds background by 5 ppm on an OVA.
5,9 Safety Equipment List
5,9,1 First Aid
A first aid kit will be located in the support area. This
equipment will be used for minor injuries and for temporary
emergency care (prior to transport only). Any more serious
injuries will be reported to the site medical personnel.
5.9,2 Fire-Fighting
A 30 lb dry chemical fire extinguisher will be located in the
support area and on the excavation and treatment equipment
during field operations. In the event of a fire, the Hoechst
Celanese emergency response team will be notified by the plant
emergency alarm system or by calling 4200, then the fire
department.
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5.9.3 communications
Operable Unit 2 60% Remedial Design Report
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Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0S0N
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Page 5-22
verbal communications will be appropriate for Level D
operations. Hand signals may be necessary if Level c protection
is needed. In the event of an emergency situation, an air horn
will be sounded and health and safety personnel will further
direct actions as necessary.
5.9.4 Decontamination Equipment
Decontamination equipment will consist of water hoses, brushes,
polyethylene sheeting, trash cans, polyethylene trash bags,
aluminum foii; paper towels, and Alconox soap.
5.9.5 Sanitation/Hygiene
1. Hand, face, and arm washing. Potable water and soap will be provided and stored in the support area.
2. Latrines. Located on site.
5.10 Decontamination Procedures
sampling equipment will be decontaminated prior to its initial
use, between sampling at separate locations, and after
completion of the sampling event. The intent of the
decontamination effort is to minimize the potential for creating
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Page 5-23
false data responses in the sample analyses resulting from
cross-contamination, or from introducing contamination from
external sources. Decontamination procedures ~ill be:
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equipment:
1. Wash equipment thoroughly with laboratory
detergent and hot water using a brush to remove
any particulate matter or surface film.
2, Rinse equipment thoroughly with tap water.
3. Rinse equipment thoroughly with deionized water.
4.
5.
Rinse equipment twice with pesticide-grade
isopropyl alcohol and allow to air dry.
Wrap equipment completely with aluminum foil to
prevent contamination during storage and/or
transport to the field. ·
6. Rinse the stainless steel or metal sampling
equipment thoroughly with tap water in the field
as soon as possible after use.
miscellaneous equipment such as hoses or measuring
tapes:
1.
2.
3.
4.
Wash with laboratory detergent and tap water.
Rinse with tap water.
Rinse with deionized water.
Equipment should be placed in a polyethylene bag
or wrapped with polyethylene film to prevent
contamination during storage or transport.
Equipment potentially contaminated during source remediation
will require decontamination at specific points during
remediation. Generally, potentially contaminated equipment will
require decontamination when traveling from the contaminated
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area (exclusion zone) to the contamination reduction zone, and
prior to leaving the site. Potentially contaminated equipment
that will contact otherwise uncontaminated items or areas will
also require decontamination. All potentially contaminated
materials including disposable clothing will be collected for
on-site treatment or disposal. Controls implemented to prevent
spillage and discharge of decontamination solutions will be
inspected for condition and effectiveness.
Decontamination procedures for larger equipment used in
remediation will be:
o items will first be cleaned with a pressurized steam cleaner
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items will then be rinsed with tap water
water used for decontamination will be collected and treated to meet the NPDES limits prior to disposal
s.11 Contingency Plans
Contingency plans are implemented when a situation or event
occurs that cannot be handled at the site by field or plant
personnel. If an injury occurs and cannot be adequately treated
by on-site first aid, the injured person(s) will be promptly
transported to the local hospital by ambulance, car, or other
means of transportation. The local fire department will be 5050N019
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Page 5-25
contacted in the event of a fire or chemical emergency that is
potentially harmful to the human health and cannot be handled by
the plant facility. The police department will be contacted
when a situation occurs that cannot be handled by plant
security. National and regional sources of assistance are
included for obtaining information when deemed necessary.
s.11.1 Local sources of Assistance
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Hospital:
Address:
Directions:
Ambulance:
Fire Department:
Local Police:
State Police:
Job Site:
Name: Cleveland Memorial Hospital
201 Grover street
Shelby, North Carolina 28150
Turn right at plant entrance onto
Highway 198 North~ After 2 miles,
this roadmerges with Highway 226.
Follow 226 N for 6 miles (also
merges with Highway 74) to DeKalb
Street, entrance is immediately on
right.
Call 4200 for HC Security for HC
ambulance first. In the event the
HC ambulance is unavailable, call
482-4422.
HC, then 482-4422
HC, then 482-8311
HC, then 482-8311
Pull alarm or dial 4200 on HC
phones.
s.11.2 National/Regional sources ot Assistance
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Westinghouse Environmental and
Geotechnical Services, Inc.
GDC Engineering Inc.
1-404-458-9309
1-504-383-8556
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Westinghouse Project Manager (Everett W. Glover, Jr.) 1-404-458-9309
GDC Project Manager
(Clinton Twilley) 1-504-383-8556
EPA (RCRA-Superfund Hotline) 1-800-424-9346
chemtrec (24-hours) 1-800-424-9300
Bureau of Explosives (24-hours) 1-202-293-4048 (Association of American Railroads)
Communicable Disease Center 1-404-633-5313 (Biological Agents)
National Response center, NRC 1-800-424-8802 (Oil/Hazardous Substances)
DOT, Office of Hazardous 1-202-426-0656 Operations
DOT, (Regulatory Matters) 1-202-426-2075
u.s .. coast Guard 1-800-424-8802 (Major incidents). ·
Pesticide Health Hotline [phone]
Westinghouse Corporate Health & Safety 1-404-452-1911 Officer (Barbara Foster)
Georgia Occupational Medicine 1-404-458-7041 (Westinghouse Health Consultants)
s.12 Amendments to Site specific Health and Safety Plan
This site specific health and safety plan is based on
information available at the time of preparation. Unexpected
conditions may arise which require reassessment of site safety
procedures. It is important that personnel protective measures
be thoroughly assessed by the site manager and/or the designated
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Page 5-27
site safety officer prior to and during the site activities.
Unplanned activities and/or changes in the hazard status should
initiate a review of and may initiate changes in this plan.
Changes in the anticipated hazard status or unplanned activities
are to be submitted on "Amendments to site Specific Health and
Safety Plan". Amendments must be approved by the plan author
and the Corporate Health and Safety Officer prior to
implementation of the amendment.
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Page 6-1
6.0 SAMPLING AND ANALYSIS PLAN
The objective of the Sampling and Analysis Plan is to describe
the equipment, methodologies, shipping and handling, hygiene, and
analytical procedures to be used in collecting and analyzing
waste and verification samples for evaluating the effectiveness
of the incineration and solidification.
6.1 Sample Handling
The specific procedures for collecting samples are detailed in
Section 6.4. · Bottle selection for each sample will be based on
the analysis to be performed. If samples are to be analyzed
using Contract Laboratory Program (CLP) protocols, the guidelines
as outlined in Table 6-1 will be used to determine what bottles
are needed. The EPA Region IV Standard Operating Procedures and
Quality Assurance Manual (SOPQAM), April 1986, will be used in
all sampling and sample handling, including proper determination
of preservatives to be used, sampling procedures, and proper use
of tags and chain-of-custody forms. Bottle requirements for
samples to be analyzed through a subcontract laboratory will be
determined by the laboratory performing the analysis.
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Table 6· 1
RECCMHEMOEO SAMPLE CONTAINERS, PRESERVATIC:W, ANO HOLDING TIMES
Parameter
Holding
Container
Liquid -Low to Hediun Concentration Sanples
Alkalinity
Acidity
Biochemical oxygen
· Demand (BOO)
Chloride
Chlorine Residual
Color
Conductivity
5D50ND17
500-ml or 1-liter
polyethylene with
polyethylene or
polyethrlene lined
closure
500-ml or 1-liter
polyethylene with
polyethylene or
polyethrene lined
closure
. 1/2-gal.
polyethylene with
pol y·ethrene
closure .
SOO·ml or 1-liter
polyethylene with
polyethylene or
polyethrene lined
closure
In-situ, beaker or
bucket
500-ml or 1-liter
polyethylene with
polyethylene or
polyethrene lined
closure
500-ml or 1·liter
polyethylene with
polyethylene or
polyethrene lined
closure
Preservative
Cool, 4°C
cool, 4°c
cool, 4°c
None
None
Cool, 4°C
Cool, 4°c
Time
14 days
14 days
·4S·hrs.
28 days
Analyze
lnmecliately
48 hrs.
28 days
(determ;ne an
site 1f
possible)
Reference
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Page 6-3
Table 6-1, Contirued
REC~MENDED SAMPLE CONTAINERS, PRESERVATION, AND HOLDING TIMES
Holding
Parameter Container Preservative Time Reference
Liquid -Low to MedillTI Concentration Sa11ples (continued)
Chromiun, Hexavalent 1·liter polyethylene Cool, 4°C 24 hrs. C
with polyethylene
closure
Cyanide 1·liter or Ascorbic 14 days C
1/2-gallon Acii•3
polyethylene with Sodi un
polyethylene or Hydroxide pH>
polyethylene lined 12, Cool 4°c
closure
EP Toxicity 1-gal. glass c antler> Cool, 4°C ASAP · NS B
with Teflon liner
Fluoride 1-lfter polyethylene None-28 days C
or 1/2-gal.
polyethylene with
polyethylene or
polyethrene lined
closure
Metals 1·liter polyethylene SOX Nitri/ 6 months C
with polyethylene Acid, pH <2
lined closure
Metals, Dissolved 1-liter polyethylene Filter on 6 months C
with polyethylene site2 SO X
lined closure Nitric Acid,
pH <2
Ci l and grease 1-liter widemouth SOX 28 days C
glass with Teflon Sul furic2
lined closure Acid, pH <2
Cool, 4°c
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Hoechst Celanese/Shelby, NC Westinghouse Project 4124-85-0S0N
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Page 6-4
Table 6·1, Continued
RECOIMENDED SAMPLE CONTAINERS, PRESERVATIC».I, AND HOLDING TIMES
Parameter Container Preservative
Liquid -Low to Mediun Concentration Sarrples (continued)
Organic Corrpound
Extractable and
Pesticide Scan
No Residual Chlorine
Present
Residual Chlorine
Present
Organic Coopounds
Purgeable (VOA)
1-gal. anber glass
or 2 1/2-gal • .-r
glass with Teflon
lined closure
1-gal. anber glass
or 2 1/2-gal, arrber
glass with Teflon.
. l i ned closure
No Residual Chlorine 2 40-ml vials with
Present
Residual Chlorine
Present
Organic c~
Specified and
Pesticides
(Non-Priority
Pollutants such as
Herbicides)
Organic Halides
Total (TOX)
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caps
2 40-ml vials with
Teflon lined sept1.111
caps
1-gal. ~r glass
or 2 1/2•gel. llll'ber
glass with Teflon
lined closure
250-ml llll'ber glass
with Teflon lined
sept1.111 closure
Cool, 4°c
Add 3 ml 10X
Sodiun
Thiosulfate per
gal Lon, Cool,
4°.c
4 drops Cone.
Hydrochloric
Acid, Cool,
4°c
Footnote 6
Footnote 7
Cool, 4°c
Holding
Time
47 days5
47 days5
14 days
14 days
47 day/
ASAP • NS
Reference
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Page 6-5
Table 6-1, Continued
REC04MENOED SAAPLE CONTAINERS, PRESERVATICW, AHO HOLDING TIMES
Parameter Container Preservative
Holding
Time
Liquid Low to Mediun Concentration Sarrples (continued)
pH
Phenols
Phosphate·Ortho
.Phospho~us, Total
Dissolved
Solids, Settleable
Solids (Total and
Suspended, etc.)
Sul fates
Sulfides
In-situ, beaker or
bucket
1-liter ani:>er glass
with Teflon lined
closure
500-ml or 1·liter
polyethylene with
polyethylene or
polyethylene lined
closure
500-ml or 1-liter
polyethylene with
polyethylene or
polyethylene lined
closure
1/2-gal.
polyethylene with
polyethylene closure
500-ml or 1-liter
polyethylene with
polyethylene or
polyethrene lined
closure
500-ml or 1-liter
polyethylene with
polyethylene or
polyethrene I ined
closure
500-ml · or 1 ·liter
polyethylene with
polyethylene or
polyethrene lined
closure
None
SOX Sul turic
Acid, pH <2
Cool, 4°C
Filter-on-site
Cool, 4°c
Analyze
lnmediately
28 days
48 hrs.
Filter-on-site .. 28days
SOX ·sulfuric
Acid, pH <2
Cool, 4°C
Cool, 4°c 48 hrs.
Cool, 4°c
Cool, 4°C
2 ml Zinc
Acetate2 Cone.
Sod i iin Hydroxide
to pH >9 Cool,
4°c
7 days
28 days
7 days
Reference
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Westinghouse Project 4124-85-0S0N
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Page 6-6
Table 6-1, Contirt..1ed
RECCJ<MENOED S~PLE CONTAINERS, PRESERVATION, AND HOLDING TIMES
Parameter Container Preservative
Liquid· Low to Mediun Concentration Sanples (continued)
Terrperature
Turbidity
In-situ, beaker or
bucket
500-ml or 1-liter
polyethylene with
polyethylene or
polyethylene lined
closure 1
None
Cool, 4°C
Soil, Sediment or Sludge: Low to Medil.rn concentration
E.P. Toxicity
Metals
Nutrients Including:
Nitrogen,
Phosphorus, Chemical
Oxygen Demand4
Organics •
Extractable
Organics -Purgeable
(VOA)
Other Inorganic
c~-
Jncluding Cyanide
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8-oz. widemouth
glass with Teflon
'tined closure
8-oz. widemouth
glass with Teflon
lined closure
500-ml polyethylene
with polyethylene
closure or 8 oz.
widemouth glass with
Teflon lined closure
Cool, 4°c
cool, 4°c
Cool, 4°c
8-oz. widemouth cool, 4°c
glass with Teflon
lined closure
4-oz. (120 ml)
widemouth glass with
Teflon lined closure
Cool, 4°c
500-ml polyethylene Cool, 4°c
w;th polyethylene
closure or 8·oz.
widemouth glass with
Teflon lined closure
Holding
Time
Determine On
Site
48 hrs.
ASAP -NS
6 months
ASAP
ASAP
ASAP
ASAP
Reference
C
C
B
A
A
A
A
A
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Table 6-1, ContintJed
RECO!MENOEO SAMPLE CONTAINERS, PRESERVATIO., AND HOLDING TIMES
Parameter Container Preservative
Holding
Time
Soil, Sediment or Sludge -Low to Mediun Concentration (continued)
Toxicity
Characteristics
Leaching Procedure
(!CLP)
Air Quality
Principal Organic
Hazardous
Constituents
~articulates
Metals
Abbreviations:
Footnotes:
8-oz widemouth glass Cool, 4°c
with Teflon lined
Closure
Glass Container
containing Tenax
sorbent cartridge
Particulate·
Sa~l ing Train
Particulate·
Sa~l ing Train
N/A
N/A.
N/A
ASAP= As Soon As Possible
NS = Not Specified
ASAP -Holding
Times ·for
Extract Per
Protocols for
Analytical
Fraction
ASAP
ASAP
ASAP
Reference
E
G
H
1. Use indicated container for single parameter requests, 1/2 gallon polyethylene container
for lllJltiple parameter requests except those including BOO, or 1-gallon polyethylene
container for lllJL tiple parameter request which include BOO.
2. Must be preserved in the field at time of collection.
3. Use ascorbic acid only if the S8""le contains residual Chlorine. Test a drop of s001)le
with potassiun iodide-starch test paper; a blue color indicates need for treatment. Add
ascorbic acid, a few crystals at a time, until a drop of S001)le produces no color on the
indicator paper. The add an additional 0.6 g of ascorbic acid for each liter of S001)le
voll.ll'le.
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Table 6-1, Contin.1ed
RECCMMENDED SA14PLE CCNTAINERS, PRESERVATIOH, AND HOLDING TIMES
Footnotes: (Continued)
4. May include nitrogen series (amnonia, total Kjeldahl nitrogen, nitrate-nitrite), total
phosphorus, chemical oxygen demand and total organic carbon.
5. San-.,les ITIJSt be extracted within 7 days and extract ITIJSt be analyzed within 40 days.
6. Collect the sarrple in a 4 oz. soil VOA container which has been pre-preserved with four
drops of 10 percent sodiun thiosulfate solution. Gently mix the saq:,le and transfer to a
40 ml VOA vial that has been pre-preserved with four drops concentrated HCl, cool to 4°c.
7. See Organic C0111)0unds -Extractable. The Analytical Support Branch should be consulted
for any special organic C0111)0Urd analyses in order to check on special preservation
requirements and or s~le volune.
References:
A. US-EPA, Region IV, Envirormental Services Division, "Analytical ~upport Branch, Operatior'ls ·
and Quality Control Manual 11, June 1, 1985 or la~est version.
B. · EPA Method 1310, Extraction Procedures, 11S\J 84611, US-EPA, Office of Sol id \Jastes,
\Jashin9ton, DC, 1986.
C. 40 CFR Part 136, Federal Register, Vol. 49, No. 209, October 26, 1984.
D. EPA Interim Method 450.1, "Total Organic Halide", US-EPA, ORD, EMSL, Physical and Chemical
Methods Branch, cincimati, Ohio, Novenber 1980.
E. 40 CFR Part 261, Federal Register, Vol. 55, No. 61, March 29, 1990, pg. 11798·11877.
F. EPA Method 30, Volatile Organic S~Ung Train, 11S\I 84611, US-EPA, Office of Sol id \Jaste,
\Jashington, DC, 1986.
G. EPA Method 5, Determination of Particulate Emissions from StBtionary Sources, 40CFR 60
Appendix A.
H. EPA Modified Method 12, Determination of Particulate Emissions from Stationary Sources,
40CFR 60 Appendix A,
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Document Control 85050N-227
Page 6-9
6.2 sample Identification
Each sample collected at the site will be identified by a unique
sequence of numbers and letters. The identification number for
a given sample will be assigned in the field by the sampling
team and will be recorded in a field notebook and placed on the
sample tag. Additionally, the sample identification number will
be recorded on the chain-of-custody form. Sample identification
numbers will be assigned according to the following format:
SH-XX-YY-ZZ
where SH is an abbreviation for the site name
XX is a sample type identifier
YY is the sample location identifier
zz is the sequential sample from that location
Sample type identifiers to be used in the sequence are as
follows:
IA -incineration ash
SO -solidification sample
SS -stream sediment
WW -treated scrubber water, treated stormwater,
miscellaneous waters, etc.
SE -trial burn exhaust gases, operational exhaust gases
WF -waste feed, miscellaneous feed
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As an example, the identification sequence:
SH-S0-04-02
represents a solidification sample obtained from the Shelby
site. The sample associated with this identification sequence
represents the second solidification sample and the fourth
sampling location.
· 6.3 Sampling Procedures
samples shall be taken of waste feed, solidified materials,
stream sediments, treated scrubber water; stormwater runoff,
stack gases and incinerator ash. A thorough discussion of
sampling procedures for incinerator stack gases is in the Trial
Burn Plan (Appendix I) and is not detailed here; however,
routine stack monitoring is included in the following sections.
The containers and preservatives to be used by Westinghouse will
be supplied by the laboratory in accordance with the QC
procedures. Samples containing high concentrations of
contaminants will be separated from those with low
concentrations. General sampling and packaging protocols shall
include:
1.
2.
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Complete all documents, tags, and forms appropriate to the samples to be shipped.
Ensure that all bottles have the appropriate labels affixed.or all appropriate tags securely fastened.
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3 •
4 •
5.
6.
7.
8.
. 9.
10.
11.
12.
13.
14.
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Mark the sample volume level on each container with an indelible marker.
Secure container lids to prevent leaks. Use signed or initialed custody seals on lids.
Secure the drain plug at the bottom of the cooler or shipping carton used for sample transport with duct tape, if present.
Place approximately 1 inch of vermiculite (or other suitable material) in the bottom of the liner as a cushioning material and an absorbent in case of leakage.
Seal each sample container in individual plastic bags, and place upright in the lined cooler or shipping carton.
Repackage ice in small, sealed plastic bags and place loosely in the cooler or shipping carton. Prepackaged, reusable chemical ice (Blue Ice) can be used. Pack ice so that it will not break glass bottles and will allow addition of sufficient cushioning material.
Place small containers, such as 40 milliliter (ml) septum vials for VOAs, in small sealed plastic bags. When shipping these with larger containers, additional cushioning material will be added to prevent them from being crushed.
Fill the remaining space in the lined cooler or shipping carton with vermiculite or other suitable material.
Place the documents accompanying the samples in a sealed, large plastic bag attached to the inside of the cooler or shipping carton lid.
Close the lid of the cooler or shipping carton and fasten the latch.
Affix signed custody seals to both ends of the cooler or shipping carton in such a manner that they must be removed or broken in order to open the cooler or shipping carton.
Wrap duct or fiber tape around both ends of the cooler or shipping carton several times, each time slightly
Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document Control 85050N-227
Page 6-12
overlapping the custody seal.
15. Mark the cooler or shipping carton on the outside with the following information: name and address of laboratory, return address, arrows indicating the "This End Up" on all four sides, label cooler or shipping carton as "Environmental Samples" and as "Fragile".
6.4 Specific sampling Procedures
The specific sampling procedures are outlined in the following
paragraphs for treated scrubber and stormwater samples,
solidified materials, incinerator ash, stream sediments, stack
gases, and waste feed.
6.4.1 Treated scrubber and stormwater samples
The sample code for treated scrubber and stormwater samples is
WW. Sample numbers will start with 01 and progress
arithmetically to the highest number needed.
Sampling Method
The procedures for sampling treated scubber water, stormwater,
and other miscellaneous waters are as follows:
1.
2.
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Make sure the pH and conductivity meters have been calibrated before sampling begins. Check calibration of meters periodically during sampling. Record
information in sample notebook.
Measure and record pH, conductivity, and temperature.
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Collect the sample from the end of the treatment plant after the water is processed though the treatment devices.
Add the proper preservatives to the sample bottle. After placing the cap on the sample container, attach the completed sample tag or label to the container.
Record all required information in the field logbook, chain-of-custody form, and sample log sheet.
Sampling Frequency and Analyses
The treated scrubber and stormwater will be analyzed daily
during the trial burn and monthly thereafter. Analysis will be
for the parameters listed in the National Pollutant Discharge
Elimination system (NPDES) permit.
6.4.2 Solidified Material
The sample code for solidified material is so. sample numbers
will start with 01 and progress arithmetically to the highest
number needed.
Sampling Method
The procedures for sampling solidified samples are as follows:
1.
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Using a sampling device appropriate for the consistency of the solidified material, place sample material in a decontaminated stainless steel pan and mix thoroughly, fill the appropriate number of 8-oz glass jars 3/4 full with sample. sample depths may vary from Oto l foot.
2 •
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Attach an identifying label or tag to the bottle.
Mark the location with a numbered stake and locate the sample point on a sketch of the site.
Record all required information in the field logbook, chain-of-custody form, and sample log sheet.
sampling Frequency and Analyses
One sample will be taken for every 100 cubic yards of solidified
material, leached by the TCLP, and the extract analyzed for the
TCLP parameters and ethylene glycol.
6.4.3 Incinerator Ash
The sample code for incinerator ash is IA. Sample numbers will
start with 01 and progress arithmetically to the highest number
needed.
Sampling Method
The procedures for sampling incinerator ash samples are as
follows:
1. Using a stainless steel beaker, fill the appropriate number of a-oz glass jars 3/4 full with sample. Sample depths may vary from Oto 1 foot.
2. Attach an identifying tag or label to the bottle.
3. Record all required information in the field logbook, chain-of-custody form, and sample log sheet. 5050N017
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Sampling Frequency and Analyses
One sample of the ash will be taken for every 20 tons of
incinerator feed material and analyzed for ethylene glycol.
6.4.4 stream Sediments
The purpose of the stream sediment sampling is to establish
whether contaminants have been removed from the stream beds.
The sample code for stream sediments is ss. Sample numbers will
start with 01 and progress arithmetically to the highest number
rieeded.
Sampling Method
The procedures for sampling the stream sediments are as follows:
1
2.
3.
4.
5050N017
Sediment samples will be collected using stainless steel spoons or scoops. The collected sediment will then be composited in a stainless steel bowl, mixed, and placed into 8-oz glass jars. Sample depths may vary from o to 6 inches.
Attach an identifying label or tag to the bottle.
Mark the location with a numbered stake and locate the sample point on a sketch of the site.
Record all required information in the field logbook, chain-of-custody form, and sample log sheet.
Operable Unit 2 60% Remedial Design Report
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Hoechst Celanese/Shelby, NC Westinghouse Project 4124-85-0SON
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Sampling Frequency and Analyses
One composite sample will be collected for each 40-foot segment
or piece there of cleaned, and will consist of material from at
least eight discrete points chosen by the sampler to best
represent the area being sampled. Those stream segments
containing no sediment will not be sampled.
6.4.5 Stack Sampling
The purpose of the stack sampling is to establish whether POHCs,
particulates, or other contaminants have been emitted into the
atmosphere. stack gases will be monitored continuously for
oxygen, carbon dioxide, and carbon monoxide. Stack sampling
will be conducted during the trial burn and is addressed in the
Trial Burn P_lan prepared by GDC.
6.4.6 Waste Feed
The sample code for waste feed is WF. Sample numbers will start
with 01 and progress arithmetically to the highest number
needed.
5050N017
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Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0S0N
Document Control 85050N-227
Page 6-17
Sampling Method
The procedures for sampling waste feed samples are as follows:
1. Using a decontaminated, stainless steel scoop or
trowel, fill the appropriate number of a-oz glass jars
3/4 full with sample. Sample depths may vary from o to
1 foot.
2. Attach an identifying tag or label to the bottle.
3 Record all required information in the field logbook,
chain-of-custody form, and sample log sheet.
Sampling Frequency and Analyses
One sample of the waste feed will be taken for every .150 tons of
waste feed material and an_alyzed for ethylene glycol and
antimony.
6.5 Sample Custody
The sample custody and chain-of-custody procedures will be as
follows:
1.
5050N017
Place the sample in an appropriate bottle and log the
following information in the field notebook:
o sample number
o date
0
0
0
name(s) of sampler(s)
time (military)
location or station identifier
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Hoechst Celanese/Shelby, NC Westinghouse Project 4124-85-0SON
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Page 6-18
o comments
2. Fill in sample label or tag with:
o project name and number
o sample number
o date
o time (military) of collection
o type of preservative used, if any
o parameters to be analyzed
o samplers name(s)
o location or station identifier
3. Place samples in-coolers or shipping' cartons. Samples are to remain in the custody_of the samplers until they are brought to the decontamination area or the support area.
4. Complete chain-of-custody forms including:
0 sample number(s)
0 date
0 project name and number
0 name(s) of sampler(s)
0 time (military)
0 type (grab or composite)
0 number of samples
0 volume of bottles
0 parameters to be analyzed
0 sample tag numbers
5050N017
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9.
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Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0S0N
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signatures of personnel releasing samples
Relinquish the samples to the Site Manager, a person
designated by the Site Manager, or the sample
packager, with the chain-of-custody form signed with
the date and time noted.
Log the name of the individual receiving the sample and
the time relinquished in the sampler's field notebook
by the sampler.
Tape the lids closed and affix signed or initialed
custody seals over the sample lids.
Prepare sample label or tags, signed by the sampler(s)
and attached to the bottle. Record the tag numbers in
the remarks column on the appropriate chain-of-custody
form.
Record the sample numbers, receipt of samples, tag
numbers, date,. and time samples were taken, in the
field office sample tracking log books.
Package the samples and deliver according to the
protocols described in this plan. Samples may be
stored in a site refrigerator until packed for
shipping, if necessary.
6.6 Equipment Decontamination
The sampling equipment will be decontaminated prior to its
initial use, between sampling locations, and after completion of
the sampling event. The intent of the decontamination effort is
to minimize the potential for creating false data responses in
the sample analyses resulting from cross-contamination, or from
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introducing contamination from external sources.
6.7 calibration Procedures and Frequencies
The Quality Control Manual provided by the laboratory contains
the procedures and frequency of calibration for the equipment
used in the laboratory.
6.8 Analytical Procedures
The analytical procedures to be used by the laboratory will be
listed in their Laboratory Quality Control Manual. The
procedures listed will generally follow the Contract Laboratory
Program (CLP) Statments of Work for Organic and Inorganic
Analyses, US EPA 600-4-79-020 Methods for Chemical Analysis of
water and Waste, SW-846 Test Methods for Evaluating Solid Waste:
Physical and Chemical Methods, and American Society for Testing
Materials, Annual Book of ASTM Standards, Part 31, water
Atmospheric Analysis, Philadelphia, PA. 1974, p40-42. sample
analyses will be conducted within recommended EPA holding times.
6.9 Data Reduction, Verification, and Reporting
The laboratory data reduction and verification are covered in
the testing and QA procedures followed by the laboratory (i.e., 5050N017
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CLP methodologies, etc.).
6,10 Internal Quality Control Checks
Split samples of the waste feed, solidified material, stream
sediments, treated wastewater, and incinerator ash will be
analyzed to provide a quality control check for the laboratory.
As a quality control check, duplicate incinerator stack gases
will be analyzed during the trial burn phase of operation.
As a Westinghouse quality control check, the following QA checks
will be incorporated into the field samples being sent to the
laboratory:
Duplicate Samples: Samples will be duplicated simultaneously
from the same source under similar conditions, placed in
separate containers and assigned a non-sequential sample
number. One duplicate sample will be collected for every 20
sampling locations, per type of sample (e.g., one duplicate
per 20 solidification samples). If less than 20 of a
particular type of sample are collected, one duplicate will
be collected.
Equipment Blanks: Control samples will be selected after
equipment decontamination to assess the thoroughness of the
cleaning procedures. Equipment will be rinsed with
deionized water and the rinsate collected and analyzed for
the same parameters as the routine analyses.
Trip Blanks:
40 ml septum
analyzed for
Laboratory prepared deionized water samples in
jars will accompany each water shipment to be
volatiles.
Blanks: For treated water samples, laboratory prepared
sample containers with deionized water will be exposed to
the work site atmosphere.
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Matrix Spike/Matrix Spike Duplicate: Triple volumes will be collected for selected samples. Two of the samples will be spiked at the laboratory and analyzed to determine the effects the site specific matrix may have an analyses ..
The Westinghouse quality control samples will be submitted from
the field along with other samples taken from the site and
numbered accordingly.
6,11 Preventive Maintenance
Project team members must be able to respond rapidly to a
variety of incidents, using both routine and specialized
equipment. Due to the unpredictable nature of sampling programs
of this type, equipment must be in a continual state of
preparedness. Therefore, preventive maintenance is critical.
The sampling and analytical equipment for air, solidified
material ash, treated waters, and sediments will be maintained
to manufacturer's specifications and in operational condition.
Routine preventive maintenance, inspections, and checkouts will
be conducted by the members of the field crew, to assure proper
operation of the various pieces of equipment.
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Page 7-1
7.0 REFERENCES
EPA, 1983. Interim Guidelines and Specifications for Preparing
Quality Assurance Project Plans. February, 1983.
EPA, 1983a. Methods for Chemical Analysis of Water and Waste.
March, 1983.
EPA, 1986. Region IV Standard Operating Procedures and Quality
Assurance Manual. April, 1989
EPA, 1986a. Test Methods for Evaluating Solid Waste: Physical
and Chemical Methods. September, 1986.
EPA, 1988.
Organics.
EPA, 1988a.
Inorganics.
Contract Laboratory Program Statement of Work for
February, 1988.
Contract Laboratory Program Statement of Work for
July, 1988.
EPA, 1989. Declaration for the Enforcement Record of Decision,
Celanese Fibers Operations, Shelby, North Carolina.
EPA 1989a. Letter Accepting 1-Foot Excavation Depth. Incoming
Document Control Number 85050MIE-0080.
EPA, 1989b. Draft Guidance on Metals and Hydrogen Chloride
Controls for Hazardous Waste Incinerators. March, 1989.
EPA 1989c. Guidance on Setting Permit Conditions and Reporting
Trial Burn Results.
52 CFR, pp 42522-42584, November 5, 1987.
40 CFR 261, pp 11798-11877, March 29, 1990.
Occupational Health Services, Inc., New Jersey
S&ME, Inc., 1987. Remedial Investigation Report for Celanese
Fibers Operations, Shelby, North Carolina. Document Control
Number 85050A-0056.
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S&ME, Inc., 1989a. Operable Unit 2 Final Feasibility Study,
Celanese Fibers Operations, Shelby, North Carolina. Document
Control Number 85050D-0138.
Sittig, Marshall, 1985. Handbook of Toxic and Hazardous
Chemicals and Carcinogens, 2nd ed., Noyes Publications.
Westinghouse, 1989. Letter Proposing 1-Foot Excavation Depth,
Operable Unit 2. Document Control Number 85050D-0171.
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APPENDIX III
METAL EMISSIONS FROM HAZARDOUS
WASTE INCINERATION
(Will be revised for 90% Design Report)
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1. Tier
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2. Tier
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Westinghouse Project 4124-85-0S0N
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Appendix III-1
METALS CONTROLS FOR HAZARDOUS WASTE INCINERATIONS
I Approach
Sets limits based on feed rates
Assumes no removal of metals in bottom ash or by air
pollution devices
It passes the Tier I limits, no trial burn for metals
is required
II Approach
Sets emmisions limits based on health risks using
dispersion coefficients for worst-case facilities
Allows for removal of metals in bottom ash and by air
pollution devices
Compliance determined by stack emmissions tests
3. Tier III
0
0
5050N020
Allows higher emission rates than Tier III limits
without exceeding health risk numbers
Established using dispersion modeling
Stack Height
Feed Rate
Exhaust Flow Rate
Complex Terrain
Rural Area
Volatile Antimony
Volatile Chromium
Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document Control 85050N-0227
Appendix III-2
Assumptions
10 Meters
1 ton/hr
10 meters/sec
100%
5%
Air Pollution Controls Are Used
DATA FROM THE .REMEDIAL INVESTIGATION
Soil Antimony
Soil Chromium
5050N020
Range
50-25,000 mg/1
<1.5 -40 mg/1
Average
5,000 mg/1
10
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1. Feed Rate
Antimony
Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document Control 85050N-0227
Appendix III-3
TIER I ANALYSIS
5000 mg/kg x 10-6 x 2000 lb/ton x 1 ton/hr=
= 10 lb/hr
Chromium
10 mg/kg x 10-6 x 2000 lb/ton x 1 ton/hr=
= 0.02 lb/hr
2. Plume Rise
Flow Rate -10 meters/sec
Exhaust Temperature -600°K
Plume Rise -16 meters (Table B-1)
3. Effective Stack Height
4.
5.
Effective Stack Height= Stack Height+ Plume Rise
Effective Stack Height= 10 + 16 = 26 meters
Allowable Feed Rate
o Antimony
0 Chromium
Results
0.3 lb/hr (Table B-3)
7.9 x 10-6 (Table B-5)
o Antimony and Chromium fail Tier I analysis
5050N020
Air Pollution
Control Device
Wet Scrubber (WS)
Venturi Scrubber
Venturi Scrubber
Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document Control 85050N-0227
Appendix III-4
ESTIMATED REMOVAL EFFICIENCIES
Percent Removal
Antimony Chromium
40 50
(VS-20) 20 90
(VS-60) 40 98
Electrostatic Precipitator (ESP-1) 80 95
Electrostatic Precipitator (ESP-4) 90 99
Fabric Filer (Baghouse) 90 95
Proprietary Wet Scrubber 95 95
VS-20/WS 96 97
Combination of Devices 99 99
5050N020
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1. Assumptions
Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-050N
Document Control 85050N-0227
Appendix III-5
TIER II ANALYSIS
Adequate air pollution control devices (APCD) to meet
Tier II analysis
2. Feed Rates
0
0
Antimony
10 lb/hr x 454 gm/lb x 1 hr/60 minx 1 min/60 sec=
= 1.26 gm/sec
Chromium
0.02 lb/hr x 454 gm/lb x 1 hr/60 minx 1 min/60 sec=
= 0.0025 gm/sec
3. Stack Emissions
4.
5.
0
0
Antimony
1.26 gm/sec x 100% volatile -removal by APCD
= 1.26 gm/sec -removal by APCD
Chromium·
0.0025 x 5% volatile -removal by APCD
= 1.25 x 10-4 gm/sec -removal by APCD
Allowable Stack Emissions
o Antimony: 3.6 x 10-2 gm/sec (Table B-7)
o Chromium: 1.0 x 10-4 gm/sec (Table B-9)
Percent Removal Required to Meet Allowable Emissions
o Antimony: 96%
0 Chromium: 20%
5050N020
1.
2.
Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0SON
Document Control 85050N-0227
Appendix III-6
TIER III ANALYSIS
Computer Modeling
o use comprehensive data available to characterize
incinerator
o determine type of terrain -flat, rolling, and complex
0
0
0
detemine if rural or urban
develop site-specific meteorological data
model hypothetical incinerators as well as actual
incinerator
o use appropriate model(s)
EPA estimate on modeling time
0 50 to 100 hours
o may be more if more models are required
0
0
does not include itme for the development of
meteorological data or running of meteorological
preprocessor (RAMET)
Reference Air Concentration
Antimony -0.3 mg/m3 (Table I-3)
Chromium -1.2 x 10-2 mg/m3 (Table I-2)
SOSON020
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Operable Unit 2 60% Remedial Design Report
and Draft Remedial Action Work Plan
Hoechst Celanese/Shelby, NC
Westinghouse Project 4124-85-0S0N
Document Control 85050N-0227
Appendix III-7
REFERENCE
EPA, "Draft Guidance on Metals and Hydrogen Chloride
Controls for Hazardous Waste Incinerators," March 2, 1989.
5050N020
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5050N013
APPENDIX IV
LABORATORY QUALITY ASSURANCE/QUALITY CONTROL MANUALS
INDUSTRIAL & ENVIRONMENTAL ANALYSTS, INC
AND
DAVIS AND FLOYD, INC.
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I QUALITY ASSURANCE
MANUAL
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I AUGUST, 1988
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I SECTION
I A.
B.
I C.
I D.
E
I F.
G.
I H.
I.
I J.
I K.
L.
I M.
I N.
0.
I P.
Q.
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'
QUALITY ASSURANCE MANUAL
TABLE OF CONTENTS
DESCRIPTION
Quality Assurance Policy
Laboratory Organization
Quality Assurance Objectives
Sample Custody
Insttument Calibration
Analytical Procedures
Laboratory Quality Control Checks
Data Reduction and Reporting
Performance and System Audits
Preventive Maintenance
Specific Quality Control Procedures
Corrective Action for Data Inadequacy
Quality Assurance Performance Reports to
Management
Personnel Qualifications and Resumes
Facilities
Laboratory Instrumentation
Chemicals and Reagents
A. Quality Assurance Policy
!EA QA Manual
Section A
Page 1 of 1
Date: August, 1988
It is the policy of IEA to provide legally and scientifically defensible analytical data to clients. The
management and staff at !EA are committed to maintaining a carefully controlled analytical
environment which assures the consistent generation of accurate data.
Detailed written analytical procedures are used to ensure strict adherence to published analytical
methods throughout the laboratory. Bench-level quality control measures with well defined
acceptance criteria are included in each analytical procedure employed by the laboratory. Laboratory
records and quality control data are monitored by management on a regular basis.
This manual is a written description of the structures employed by !EA to ensure that all data
generated by the laboratory is accurate and defensible.
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-------------------
INDUSTRIAL & ENVIRONMENTAL ANALYSTS, INC.
AJANAGEAIENT STAFF
PRESIDENT
--(F. Doane)
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VICE PRESIDENT VICE PRESIDENT
Administration VT Operations
(R. Walker) (B. Eldred)
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,---7
MANAGER ADMINISTRATIVE I I Laboratory MANAGER MANAGER DIRECTOR nIRECTOR
Client OFFICER I Finance & I Director Field Technical Product Quality ·:omputer
Relations ' I Accounting I Operations Support Assurance Services
I I
(L. Treadaway) (F. Blair) I (R. Walker) I (M. Randall) (F. Stevens) (L. Mitchell) (P. Ragsdale (I'. Ragsdale)
L ___ _J
INDUSTRIAL & ENVIRONMENTAL ANALYSTS, INC.
LABORATORY OPERATIONS
DIRECTOR
..
(M. Randall)
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MANAGER
CHROMATOGRAPHY
(E. Niemi)
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SUPERVISOR SUPERVISOR CLP SUPERVISOR MANAGER Technical Instru"11entalion
G(:/MS GC COORDINATOR Metals Inorganics & Support
Sample Prep
(S. Grirfin) (K. S~tt) (M. Bero) (A. Lynch) (D. Johnson) (G. Folk) (M. 8arnes)
-------------------
-------------------
INDUSTRIAL & ENVIRONMENTAL ANALYSTS, INC.
ADMINISTRATION
..
ADMINISTRATIVE
OFFICER
(F. Blair)
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PURCHASING FACILITIES &
,------7 RECEPTIONIST ADMINISTRATIVE I PERSONNEL I
MAINTENANCE ASSISTANT
I I
(M. Dunn) (H. Amick) I (F. Blair) I (V. Seawell) (L. Core) L ______ _J
INDUSTRIAL & ENVIRONMENTAL ANALYSTS, INC.
I
CLIENT RELATIONS
COORDINATOR
(Megan Day)
CLIENT RELATIONS
ASSISTANTS
(S. Urownc)
(S. Roeber)
CLIENT RELATIONS STAFF
MANAGER
(L. Treadaway)
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MARKETING
REPRESENTATIVE
(M. Burns)
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MARKETING
REPRESENTATIVE
(Charlotte Office)
(A. Rue)
-------------------
- - - - - - - - - - --- - - - - --·
INDUSTRIAL & ENVIRONMENTAL ANALYSTS, INC.
SUPERVISOR
TECHNICAL SUPPORT
(J. Niemi)
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TECHNICAL SUPPORT
ASSISTANTS
( II. Tcismann)
(A. Hoffman)
TECHNICAL PRODUCT SUPPORT
MANAGER
(L. Mitchell)
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SUPERVISOR
SAMPLE
MANAGEMENT
(J. Ausley)
'
SUPERVISOR
LIMS
(B. Brown)
COMPUTER
OPERATORS
(L. Coodey)
(S. Bartee)
(M. Spencer)
C. Quality Assurance Objectives
IEA QA Manual
Section C
Page I of I
Date: August, 1988
The objectives of IEA are to supply precise accurate data repons to clients which are representative
of the sample supplied. All data reponed are generated and calculated according to published
methods which are recognized standards of the environmental laboratory industry. Thus, data
reponed by IEA are calculated and reponed in units which are consistent with data produced by
other organizations. IEA strives to ensure that each data report is 100% complete, containing all
data elements and supponing documentation for the type of repon requested by the client.
The precision and accuracy control limits employed by IEA are based primarily on limits contained
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in the published methods or required by the U.S. Environmental Protection Agency's Contract I
Laboratory Program (CLP). When warranted by IEA's historical data, more restrictive control
limits are set than those cited by the method or the CLP.
The precision and accuracy requirements for each analytical method are included in the individual
laboratory standard operating procedures (SOPs).
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-------------------·
INDUSTRIAL & ENVIRONMENTAL ANALYSTS, INC.
FIEW Ol'ERATIONS
MANAGER
(F. Stevens)
PROJECT ENGINEER FIELD TECHNICIANS
(B. Cole)
(W. Pascal)
D. Sample Custody
!EA QA Manual
Section D
Page I of lO
Date: August, 1988
Due to the critical nature of the samples analyzed, IEA maintains strict security within the
laboratory. Entrances to the laboratory are secured through the use of deadbolts and pushbutton
combination locksets. Visitors to IEA must enter through the lobby and sign in at the reception
desk. Visitors to the office and/or laboratory must be accompanied by an employee at all times.
Samples are received in the shipping and receiving department by the sample custodian or by an
authorized member of the depanment. Upon receipt, the shipping container and the individual
sample containers are inspected for damage. If any damage is present, a note is made in the project
file and the project manager or customer service department is notified. All sample information
supplied by the client is reviewed and checked against the samples received. The number and type
of samples received and the identity tags/labels are checked against the information supplied.
Each sample is assigned an !EA sample number. The !EA sample number is a combination of the
!EA Client Number, !EA Client Project Number and the Sample Sequence Number.
Example -Sample number 789-100-2 refers to the second sample in the one hundredth
project submitted by IEA client 789.
Each container is labelled with the assigned IEA sample number. If multiple containers are received
for a single sample a unique alpha character is added to the end of the sample number assigned to
each container. This prac:tice allows each analysis to be traced to a single sample container.
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IEA QA Manual
Section D
Page 2of 10
Date: August, 1988
Each sample received is listed in the !EA Sample Check-In Log with the !EA sample number, client
ID number, a complete description of each sample received, sample 1,ondition at the time of receipt,
date of receipt, sample numbers or identifiers and any problems encountered in the course of
receiving the samples. The receipt of chain-of-custody records with the sample shipment is also
noted on the check-in log.
A project Data Sheet is completed for each set of samples received. This form serves as the primary
source of information for the laboratory. The number and type of samples and sample containers
received for the project are listed on the Project Data Sheet as well as type of analysis required, type
of repon required, turn around time and degree of chain-of-custody documentation required.
In-lab chain-of-custody records are maintained for each sample when requested by the client. For
these samples, the in-lab chain-of-custody record is initiated upon sample receipt Each movement
of a sample or sample extract container into and out of the locked refrigerator system is recorded
with date, time, bottle number, action (check in or check out), and signature of the individual
accepting or relinquishing responsibility of the sample. The chain-of-custody records are kept in
the associated project folder.
After receipt, samples are housed in locked refrigerators. Samples are removed from the
refrigerators by authorized employees for analysis and returned to the locked refrigerator system
after completion of the analysis. Throughout the analytical process, each sample is either in the
!EA QA Manual
Section D
Page 3 of 10
Date: August, 1988
possession of authorized laboratory personnel or secured in a locked,refrigerator inside the secured
laboratory area.
Analytical data reports are kept in filing cabinets which are locked at the end of each business day.
Sensitive documents· are shredded prior to disposal.
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[t4•1
No. of Samples:
Date Needed
By Client:
P.O. Number:
Parameters
Requested
Comments:
. Shm To:
Client:
Client Rep:
Address:
Phone No:
Initiated By:
Shipped By:
TRANSPAK REQUEST ~ORM
IEA QA Manual
Section D
Page 4 of 10
Date: August, 1988
Type of Sample: lW•Scr, SgjJ. SJudgr, Other)
(Clrcu Oru,)
Ship By: CCust ridruo, IJPS, 2-Dat UPS, fcd·Erl
(Clrcu Oru,) ,
Label
I . I B111 To:
I I Qient:
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Address:
I Attention:
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Bottle
Type
-----_L· ------
.Date:
Date:
No. of
Bottles Preservative
1r. # TransPaks:
Large
Small
Coolers
SAMPLER TNSTRJJCTTQNS
IEA QA Manual
Section D
Page 5 of 10
Date: August, 1988
This sample package has been prepared for you with the objective of helping to maintain the
integrity of your samples. It is therefore vital that you read and follow these instructions.
I.
2.
3.
4.
5.
6.
Carefully open the sample package and check the contents. If any bottles are missing,
broken, or damaged, call the laboratory immediately at 9 I 9-467-99 I 9.
Remove and freeze the freezer packs included with the shipping container for at least eight
hours. They must be solidly frozen upon packing the samples for return shipment. The
freezer packs will maintain a sufficient cool temperature for approximately 72 hours.
Note the following before sampling:
3 .1 40 ml Vo)atiJe Vjals
3.2
3.3
40 ml volatile vials must not contain any air bubbles. Fill the vial ro just below
the point of overflow, until there is a convex meniscus (see picture at the left).
Carefully slide the teflon insert over the meniscus, teflon (stiff) side down
(against the sample). Screw the cap on the vial, and check for air bubbles. If
air bubbles are present, repeat the capping procedure, or draw another sample, if
necessary. Volatile bottles do not normally contain preservative chemicals.
Bacteria Sampling Bottles
-HJr.dle sterile bacteria s=pEng bottles carefully io avoid c0nt.2rn'.::e.'.'on. Do not
open the bottles until ready to sample. Fill to within half an inch of the top, and
tighten the cap securely.
Other Sampling Bottles
Some sample bottles contain strong acids or bases as preservatives. These bottles
have color coded cautionary labels. Handle with care. Do not pre-rinse or overfill
bottles having color coded cautionary labels. Tighten cap securely when filled. The
color code used is as follows:
Red:
Yellow:
Blue:
White:
Green:
Preserved with nitric acid
Preserved with sulfuric acid
Preserved with hydrochloric acid
No preservative
Preserved with sodium hydroxide
(basic) solution
Complete the sample tags and labels by filling in the sample l.D., sampling address, the
sampling point, date and time (24 hr. format; for example: 8:00 am = 0800 hours or 10:00
pm= 2100 hours). Indicate if the sample is a grab or composite. The sampler should initial
at the appropriate space.
Make sure all caps are secure, and attach labels and tags 'co correct bottles. Repack the
samples for return ·shipment to the laboratory, making sure to include the freezer packs. Ship
by a route which will ensure delivery within 72 hours.
If you have any questions, call IEA's sample receiving department, or our client
representative, at 919-467-9919 between 8:00 am and 4:30 pmMonday through Friday.
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lt?t· DAT A FOR PROJECT NO.
*Client
IEA QA Manual
Section D
Page 6 of 10
Date: August, 1988 ------~.:..;.___:
Telephone __________ _
Project I.D.
__________________ •Purchase Order No.
*Client Rep.
*Address
C
*Billing Address
lEA
ID
omments:
Client
ID
____ Same as Above __ _
•Parameter(s)
Requested
Sub-Client __________ _
Other (see below)
•Bottle Size &
Type Preservative •Location
•Turnaround Requirements
No. or Pricing
·Workday,;(Jl fatlo.r
Normal IS 1.0 X --
Rush X ----
Sampling Date _______ •oa1.e Samples Received<ll ______ •Date Project Duc<2)
.. rvtatrix ----------CUSIOmcr Signature
Lab Completion ---Fmal Review ---Date Shipped ___ _
//niliais) /lniliais) (lniliais)
(1) Samples l<Ceived after 2:00 pm will be assigned lhe dale of lhc following woricday.
(2) Rcprcscnts lhc dale lhat results arc shipped to lhc customer.
(3) Excludes wcclccnds and holidays.
----------------""-'---'----------------
~ lndurniol & Environmental Analy5t5, Inc. CHAIN OF CUSTODY RECORD
PRO_J. NO. PROJECT NAME
NO.
SAMPLERS: ,_...,.J Of
REMARKS CQH,
' ~ TAIN!RS
ITA. NO. CATI TIM! 5 IT ATION LOCATION
.
fwllnqullhed by: IS,,,,.._/ Dai. f Time RICllwd by: /$1f1Wrv,e/ Rttlnqullhld by; IS.,.ru,e/ Datt /Time R-l•ld by: is.wru,e/
Rollnqullhed by: /$Jp,a,,_/
Otte r·""' R-lwd by: /S.-rvre/ Rtllnqullhld by; /S.,.ru,e/
Otta ill""' R_I_, by: IS_ru,.J
Rollnqullhed by; /S.,0...,..1 D•• f Tlmt R-lvtd tor Llbonto,y by: Dote rim■ R■m1rk1
tsl,in.tvtW J
0611ribu1ion: Original Accomc,anl• Shipman&; Copy 10 field flln I
,....
"' 00
00
u,
~ " n ...
0 " t:,
0 ....,
,....
0
~ (IQ
" .. n -- - - - -- -------- -- - -
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-
PROJECT NO.
.
PROJECT FOLDER CHECK-OUT
ANALYST NAME ,DATE
-
IEA QA Manual
Section D
Page 8 of 10
Date: August, 1988
TIME RET.
-
l'ROJ. f'OLDER CllK.
:oject NUlllber:
,mple Katrix:
:ittle Type:
:EA Sample I
IEA
LABORATORY
CHAIN-OF-CUSTODY REPORT
Page
Sample Number: ___ _ Receipt Date:
f Received: Alpha Bottle ID:
Client ID Analysis Type
R E
R E
R E
R E
R E
R E
R E
R E
R E
Received by: ,,
Bottle Type: # Receive.d Alpha Bottle Iii:
Storage ----Sample In -----1----Sample Out ---
Location Signature Det~ Time Signature Date Time Comments:
--
,, --•
----
----
--
--
--
--
t:l ., ..
" .
C ..
~
n .
..,
00 00
i:
.,, "' ,..
" I? rt .. n ... ,0 .., !'! :,.
0 :,:
"' t:l " :!
0 " ,-.
--------------------
---
'roject Ku_;::b<er:
CHent IO
---·-~ .. --- - --
!EA
LABORATORY
CHA !ti-OF-CUSTODY REPORT
Sor,ple Number: ----Receipt Date:
Received by:
- - -
Page
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I Analpla Type
Storage ----Somple In -----1----Sample Out ---Location Signature Date Ti~e Signature Date Time Comments:
R E --
R E --
R E --
R ~ ----
R E
R E ---
R E • --• R E • --•
R E --
R E ----
R E ----
R E --
R E
R E --
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I --I --
i I ----
~
-
-. --
--
----
--
----
--
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' i
a .,, tn
" " " ,. .. n ;;!
" ... ..
~-= ;o
00
00
E. Instrument Calibration
IEA QA Manual
Section E
Page I of 7
Date: August, 1988
Because of the critical relationship between instrument calibration and the accuracy of the analytical
data generated, IEA maintains strict controls on calibration. Each type of instrumentation is
calibrated prior to sample analysis. Specific criteria for the instrument calibrations must be met
before samples may be processed. Deviations from the stated criteria are strictly forbidden.
Hardcopy records of all instrument calibrations are maintained in the individual laboratories. These
records are reviewed each week by the laboratory supervisors and are audited monthly by the QA
Officer.
Calibration requirements are instrument and analysis specific. The requirements for the analysis of
volatile, semivolatile, pesticide and inorganic compounds are described in the following sections
according to the instrumentation utilized for analysis.
GCIMS
!EA has elected to employ the calibration criteria of the CLP protocols f.or all GC/MS analyses
performed regardless of the method. Five-point calibrations are performed with continuing
calibration checks being performed at the beginning of every twelve (12) hour period of analysis
time. Designated calibration check compounds (CCC), system performance check compounds
(SPCC) and relative standard deivations (%RSD) are required to meet specified criteria for response
factors before samples are analyzed.
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Table E-1: Volatile Calibration Specifics
!EA QA Manual
Section E
Page 2 of?
Date: August, 1988
The multipoint calibration standards consist of solutions containing all analytes at 20, 50, 100, 120,
and 200 ug/1.
The continuing calibration standard contains all iinalytes at 50 ug/1.
The CCCs are vinyl chloride, 1,1-dichloroethene, chloroform, 1,2-dichloropropane, toluene and
ethylbenzene.
The SPCCs are chloromethane, 1,1-dichloroethane, bromoform. 1,1,2,2-tetrachloroethane and
chlorobenzene.
Table E-2: Acceptance Criteria for Volatile Calibrations
CCC
SPCC
Multipoint Cafibratjon
% RSD for all 5 standards
must be less than or equal
to 30%.
The average relative response
factor for bromoform must
be 0.250 or greater. The
average relative response factor
for all other SPCCs must be
0.300 or greater.
Contjnuiai:: Calibration
% difference when compared to the
average relative response in the
mulitipoint cannot exceed 25%.
The relative response factor for
bromoform must be 0.250 or greater.
The relative response factor for all
other SPCCs must be 0.300 or
greater.
IEA QA Manual
Section E
Page 3 of 7
Date: August, 1988
Table E-3: Semivolatile Calibration Specifics
The multipoint calibration standards consist of solutions containing" all analytes at 20, 50, 80, 120
and 160 ug/1.
The continuing calibration standards contains all analytes at 50 ug/1.
The CCCs are phenol, 1,4-dichlorobenzene, 2-nitrophenol, 2,4-dinitrophenol,
hexachlorobutadiene, benzo (a) pyrene, 4-chloro-3-methylphenol, 2,4,6-trichlorophenol,
acenaphthene, N-nitrosodiphenylatnine, pentachlorophenol, and di-n-octyphthalate.
The SPCCs are N-nitroso-di-n-propylamine, 4-nitrophenol, hexachlorocyclopentadiene, and
2,4-dinitrophenol.
Table E-4: Acceptance Criteria for Semivolatile Calibrations:
CCC
SPCC
Mu)ljpojnt Calibration
% RSD for all 5 standards
must be less than or equal
10 30%.
The average relative response
factor for all SPCCs must be
0.050 or greater.
Continuing raHbratjon
% difference when compared to the
average relative response in the multipoint
cannot exceed 25%.
The relative response factor for all SPCCs
must be 0.050 or greater.
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IEA QA Manual
Section E
Page 4 of 7
Date: August, 1988
IEA has elected to employ the calibration criteri1 of the CLP protocols for the complex pesticides
analyses. Three-point calibrations of aldrin,. endrin, p,p'-DDT and dibutylchlorendate are
performed at the beginning of each 72-hour period to verify linearity. The %RSD for each of these
compounds which will be quantitated in the subsequent sample analyses must be less than or equal
to 10%. After the linearity verification, single point calibrations are performed for each single
component pesticide and each multicomponent mixrure prior to sample analysis. All quantitations
are performed using the single point standarcl(s) analyzed in closest proximity to the sample
analysis.
The volatile analyses by GC are performed according to methods 601 and 602. Three-point
calibrations are performed for these analyses. The %RS Os obtained for each compound in the three
calibration analyses determine the type of quantitation performed. If all %RSDs are 10% or less,
the average response factor of each compound is used for quantitation. For any compound having a
%RSD greater than 10%, quantitation is performed using the calibration curve rather than the
average response• factor. At the beginning of each day of analysis, the current three-point
calibration is verfied through the analysis of a 20 ug/1 standard. If the calculated concentration for
each compound is within the acceptance range, sample analysis is performed using the current
multipoint calibration. If one or more analyte concentrations are outside the acceptance ranges, a
new three -point calibration is performed before any samples are analyzed. The acceptance ranges
are listed in Tables E-5 -E-6.
!EA QA Manual
Section E
Page 5 of 7
Date: August, 1988
Table E-5: Method 601 Continuing Calibration Acceptance Criteria
' Analyte Concentration % of True Value
Bromodichloromethane 15.2 -24.8 76% -124%
Bromoform 14.7 -25.3 74%-127%
Bromomethane 11.7 -28.3 59%-142%
Carbon Tetrachloride 13.7 -26.3 69% -132%
Chlorobenzene 14.4 -24.6 72% -123%
1,2-Chloroethylvinyl ether 15.4 -28.0 77% -140%
Chloroform 12.0 -25.0 60%-125%
Chloromethane 15.0 -28.1 75% • 141%
Dibromochloromethane 11.9 -26.9 60% -135%
1,2-DichloroiJenzene 13.1 -26.0 66% • 130%
1,3-Dichlorobenzene 14.0 -30.1 70% • 151%
1,4-Dichlorobenzene 9.9 -26.1 50% -131 %
1,1-Dichloroethane 13.9 · 23.2 70% -116%
1,2-Dichloroethane 16.8 · 25.7 84% -129%
I, 1-Dichloroethene 14.3 -27.4 72% -137%
trans-1,2-Dichloroethene 12.6 -27.2 63% -136%
1,2-Dichloropropane 12.8 · 25.2 64%: 126%
cis-1,3-Dichloropropene 14.8 -27.2 74% • 136%
a-ans-1,3-Dichloropropene 12.8 · 27.2 64% -136%
Methylene chloride 12.8 -24.5 64% • 123%
1, 1,2,2-Tetrachloroethane 15.5 · 30.2 78% -151%
Tetrachloroethene 9.8 · 26.0 49% -130%
1, I, I-Trichloroethane 14.0 -25.8 70% -129%
1, 1,2-Trichloroethane 15.7 -24.3 79% -122%
Trichlorofluoromethane 15.4 -24.6 77% · 123%
Trichlorofluoromethane 13.3 -26.7 67% · 134%
Vinyl chloride 13.7 -26.3 69% · 132%
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!EA QA Manual
Section E
Page 6 of 7
Date: August, I 988
Table E-6: :Vlethod 602 Continuing Calibration Acceptance Criteria
Aoalyte Concentration=-% of True Value
Benzene 15.4 -24.6 77% -123%
Toluene 16.1 -23.9 81%-119%
Ethylbenzene 13.6 -26.4 68% -132%
Chlorobenzene 14.5 -25.5 73% -128%
1,4-Dichlorobenzene 13.9 -26.1 70%-131%
1,2-Dichlorobenzene 12.6 -27.4 63% -137%
1,3-Dichlorobenzene 15.5 -24.5 78% -123%
:VJ eta ls
!EA QA Manual
Section E
Page 7 of 7
Date: August. 1988
The metals analvses are performed according to the procedures published in Test Methods for . ..
Eyajuatjng Sojjd Waste SW-846. Three point instrument calibrations are performed and two
additional standards in the analytical range are analyzed. A minimum correlation coefficient of
0.997 is required for each calibration curve. One of the additional standards must be close to the
quantitation limit (no more than 2-3 times the quantitation limit).
The calibration is verified using a standard obtained from a source other than that of the normal
calibration standards. The source for the verification standard may be a government agency such as
U.S. EPA or may be purchased from a commercial vendor. The calibration is verified after
calil:iration of the instrument and after every ten sample an'.!.!y~es.
Mjscenaneons Tnorganjcs
Calibration curves consisting of a minimum of three points are prepared for each miscellaneous
inorganics analysis. A minimum correlation coeficient of 0.997 is required for each calibration
curve. The calibration curves are verified through the analysis of a standard obtained from a source
other than that of the calibration standards. Each calibration curve must include a low level standard
which is no more than 2-3 times the quantitation limit. The standard curve is verified after the
initial calibration and after every ten samples analyses.
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F. Analytical Procedures
fEA QA Manual
Section F
Page l of 2
Date: August. I 938
The analytical methods employed by !EA for the analysis of environmental samples include
methods published in the following: Test for Eva)uarjncr Solid Waste, Physical/Chemical Methods.
SW-846, USEPA 3rd Edition, I 986; Ulieriil Regjster. 40, CFR, Pan 136, Volume 49, No. 209,
October 26, I 984: Srandard Methods for the E:qminarjon of Water and Wastewater, 16th Edition,
1985; Methods for Chemiql Analvsjs of Water and Wastes. EPA 600/4-79-20, 1979, (revised
1983). Methods selected for use by the US EPA Contract Laboratory Program (CLP) and published
in the statement of work for each contract are also utilized by !EA.
Each datJ. report issued by !EA includes a reJ'erence to the exact method err.ployed for :he a~aJvsis.
The referenced methods are strictly adhered to by the laboratory. Occasionally, modifications of the
referenced method are necessary. All deviations from the published method must be approved by
the Laboratory Manager and are stated in the final report with the reason for the deviation. (See
Method Discrepancy/ Method Resolution report form on page 2 of this section 1
LE.A
IEA QA Manual I Section F
Page 2 of 2
Date:. August, 19,I
Project No. __
I
CUSTOMER PROJECT DISCREPANCY REPORT
,, !
DISCREPANCY:
By: ____ Date: __ Time: __
RESOLUTION:
By: Date: Time: ---------
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G. L:aboratory Quality Control Checks
!EA QA Manual
Section G
Page 1 of 6
Date: August, I 988
The analytical process is continually checked and verified through the analysis of method blanks,
instrument blanks, maoix spikes. duplicate maoix spikes and sample duplicates. The depamnent
supervisor is responsible for the administration of the quality control checks within each
depanment. The records associated with the administration of the quality control checks are
reviewed quanerly as part of the system and performance audits conducted by the QA Officer. The
data generated for each quality control sample are reviewed by the laboratory supervisor, laboratory
manager and a member of the senior technical staff as part of the normal data review process.
All analytes, except methylene chloride, ace1:one, toluene, 2-butanone. and the phthalate esters are
required to have concentrations of less than the quantitation limit in all method and instrument
blanks. Warning limits of two times the quantitation limits have been established for methylene
chloride, acetone, toluene, 2-butanone, and phthalate esters. Control limits for these compounds
have been set at five times the quantitation limits.
Maoix spike duplicates are prepared and analyzed for all organic analyses at a rate of one pair for
every twenty (20) samples. The data generated for each pair of maoix spike duplicates are used to
measure the precision and accuracy of the analysis. A blank spike containing all analytes is also
-prepared with each pair of duplicate maoix spikes. If the pecision or accuracy of the duplicate
spikes is outside the control limits. the blank spike mtist be analyzed. The analysis of the blank
spike is evaluated to detennine if the analytical failure was caused by the sample maoix or by the
laboratorv analyst. Acceptance criteria for the matrix spike duplicate pairs analyzed for the common . .,
organic analyses are listed in Tables G-1 and G-2 on pages 4 and 5 of this section.
!EA QA Manual
Section G
Pa!!e 2 of 6
Date: August, 1988
Surrogate compounds are routinely used for the organic analyses. Compounds similar to the
analytes of interest are added to each sample prior to initiation of the analytical process. The
recovery of the surrogate(s) in the final analysis is used to evaluate'the accuracy and precision of the
process in each sample. Acceptable surrogate data must be obtained for each set of reponed sample
data. A database of surrogate recovery data for all samples is maintained. This database is
reviewed at least once a month by the laboratory supervisor. The QA Officer evaluates the
surrogate recovery data quanerly. Current surrogate control limits for the common organic analyses
are listed in Table G-3 on page 6 of this section.
Internal standards are employed for all GC/MS analyses. The area of the internal standards in each
sample analysis must be within the range -50% to+ 100% of the corresponding area in the current
analytical standard. The internal standard areas are evaluated periodically to ensure the consistency
of the injection techniques used throughout the laboratory.
Duplicate sample analyses are performed for the metals and inorganic parameters at a rate of one
duplicate for every ten sample analyses. Warning and control limits have been established for each
parameter. The specific limits have been included in the individual SOPs. Typical limits for the
metals analyses are:
Analyte Concentration Range
0.03 -0.20 mgl'L
0.21 -2.00 mg/L
Relative Percent Difference <RPDl
Warning Limit
35%
15%
Control Limit
65%
20%
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lEA QA Manual
Section G
Page 3 of 6
Date: August, l 988
Spiked sample analyses are performed for the metals and inorganic parameters at a rate of one spike
for every ten sample analyses. Warning and conrrol limits have been established for each
parameter. The specific limits have been inc:luded in the individu'.11 SOPs. Typical limits for metals
analyses are:
Analyte Concent_ration Range
0.03 -0.20 mg/L
0.21 -2.00 mg/L
Warning Limit
% Recovery
±25%
± 15%
Control Limit
% Recovery
±40%
±20%
!EA QA Manual
Section G
Page 4 of 6
Date: August, l 988
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Table G-1: Spike Acceptance Criteria for Common Organic Analyses in Water I
Semjvnlatj)es hv GC/MS
BN
BN
BN
BN
BN
BN
A
A
A
A
A
% Bec2veu R£l2
'
l ,2,4-Trichlorobenzene 39 -98 28
l ,4-Dich!orobenzene 36 -97 28
N-nitroso-di-n-propylamine 41 -116 38
Acenaphthalene 46 -118 31
2,4-Dinitrotoluene 24-96 38
Pyrene 26 -127 31
Phenol 12 -89 42
2-Chlorophenol 27 -123 40
4-Chloro-3-methylphenol 23 -80 42
4-Nitrophenol 10 -80 50
Pentachlorophenol 9 -103 50
For acceptance, the majority of % recoveries and RPDs for each compound class
(acid or base-neutral) in .the duplicate spike pair must meet the % recoveries and RPDs
listed above.
V2Jatj!es hy GC/MS
I, 1-Dichloroethane
Trichloroethane
Benzene
Toluene
Chlorobenzene
% Bec2very
61 -145
71 -120
76 -127
76 -125
75 -I 30
R£l2
14
14
11
13
13
For acceptance, the majority of% recoveries and RPDs obtained for the duplicate
spike pair must meet the % recoveries and RPDs listed above.
Pestjcjdes hy GC
Lindane
Heptachlor
Aldrin
Dieldrin
Endrin
4,4'-DDT ',
% Recovery
56 -123
40-131
40 -120
52 -126
56 -121
38 -127
15
20
22
18
21
27
For acceptance, the majoriry of% recoveries and RPDs obtained for the duplicate spike pair
must meet the % recoveries and RPDs listed above.
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IEA QA Manual
Section G
Page 5 of 6
Date: August, 1988
Table G-2: Spike Acceptance Criteria for Common Organic Analyses in Soil
Semjvo!atj)es hv fiC/::\JS
BN
BN
BN
BN
BN
BN
A
A
A
A
A
% ReCOYfCY Rm
1,2,4-Trichlorobenzene 38 -107 23
1,4-Dichlorobenzene 28 -104 27
N-nitroso-di-n-propylamine 41 -126 38
Acenaphthalene 31 -137 19
2,4-Dinitrotoluene 28 -89 47
Pyrene 35 -142 36
Phenol 26-90 35
2-Chlorophenol 25 -102 50
4-Chloro-3-methylphenol 26 -103 33
4-Nitrophenol 11 -114 50
Pentachlorophenol 17 -109 47
For acceptance, the majority of % recoveries and RPDs for each compound class
(acid or base-neutral) in the duplicate spike pair must meet the % recoveries and
RPDs listed above.
Vo!atjles hy GC/MS
1,1-Dichloroethane
Trichloroethane
Benzene
Toluene
Chlorobenzene
% Recovery
59 -172
62 -137
66 -142
59 -139
60 -133
Rm
22
24
21
21
21
For acceptance. the majority of% recoveries and RPDs obtained for the duplicate
spike pair must meet the % recoveries and RPDs listed above ..
Pesticides bY c;c
Lindane
Heptachlor
Aldrin
Dieldrin
Endrin
4,4'-DDT
% Recovery
46 -127
35 -130
34 -132
31 -134
42 -139
23 -134
.8..Pl!
50
31
43
38
45
50
For acceptance. the majority of% recoveries and RPDs obtained for the duplicate spike
pair must meet the % recoveries and RPDs list_ed above.
Table G-3: Surrogate Control Limits
Sernjvoialj(es hy r;c/MS
Nitrobenzene-d5
2-Fluorobiphenyl
Terphenyl-dl4
Phenol-d6
2-Fluorophenol
2.4,6-Tribromophenol
YoJatiJes hv GC/MS
Toluene-d8
Bromofluorobenzene
l ,2-Dichloroethane-d4
Pesticides hy r.c
Dibutylchlorendate
-------% Recovery -------
Water SJili
35 -114 23 -123
43 -116 30-115
33 -141 18 -137
10 -94 24 -113
21 -100 25 -121
IO -123 19 -122
-------% Recovery ......•
Water
88 -110
86 -115
76 -114
SJili
81-117
74-121
70 -121
•······ % Recovery •••••••
Water SJili
!EA QA Manual
Section G
Page 6 of 6
Date: August, 1988
24-154* 20 -15.0*
*These control limits serve as warning limits not control limits per CLP. All
other limits arecontrol limits.
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H . Data Reduction and Reporting
!EA QA Manual
Section H
Page I of I
Date: August, 1988
The data associated with each analysis are hardcopied for pe~anent storage either through the
printing of computer files or through hand entry into bound laboratory notebooks. All notebook
entries are dated and signed by the analyst. Data reduction is performed either manually by the
analyst or by computer systems interfaced to the analytical instruments.
All data are subjected to a multilevel review. All data repons are reviewed by the department
supervisor prior to release for final repon generation. A cross section of data repons are reviewed
by the Laboratory Manager. All final data repons are reviewed by a member of the senior technical
staff prior to release 10 the client. The members of the senior technical staff are not members of the
analyt:cal ?~oduction \:J.boratories.
Out-of-conrrol conditions identified by the analyst, supervisor, manager or technical staff member
are investigated. corrected and documented. Out-of-conrrol conditions which are caused by the
sample itself. are addressed in the final report.
All elements of the quality conrrol program must be satisfied before a data repon may be released to
the client.
I. Performance and System Audits
!EA QA Manual
Section I
Page l of I
Date: August, 1988
Each quaner the overall performance of the laboratory staff is evaluated and compared to the
performance outlined in the quality assurance manual and the stfmdard operating procedures. The
QA officer conducts a laboratory audit to evaluate the performance of the laboratory staff and
compares that performance to the requirements of the quality assurance program. During this
process, the records, standard operating procedures and adherence to those standard operating
procedures are examined. The results of the audit process are summarized and issued to each
depanment supervisor and the Laboratory Manager.
Known intralaboratory performance samples are analyzed in the form of sample spikes, duplicates
and duplicate sample spikes on a continuing basis. Two (2) such samples are processed for every
twenty (20) production samples.
"Blind" intralaboratory.performance audits are conducted monthly. Samples containing known
analyte concentrations are introduced into the laboratory as client samples. These samples are
analyzed and reponed in the same manner as normal production samples. The results and the true
values of each sa_mple are reponed to the laboratory supervisors and the laboratory director upon
receipt of the data by the QA officer.
!EA panicipates in interlaboratory performance audits through the v·arious state and federal
cenification programs. IEA is an active participant in the U.S. Environmental Protection Agency's
Contract Laboratory Program (CLP), U.S. Army Corps of Engineers accreditation program,
Commonwealth of Virginia Contract Laboratory Program and the Nonh Carolina. Virginia. South .,
Carolina, Georgia, Alabama and Tennessee drinking water (SOW A), ground water and waste water
cenification programs. Each of these programs require the analysis of performance evaluation
samples which contain analytes at concentrations which are known only to the cenifying agency.
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J. Preventive Maintenance
!EA QA Manual
Section J
Page 1 of 3
Date: August, 1938
Schedules of required maintenance have been prepared for ~ach analytical instrument. By
scheduling routine preventive maintenance, instrUment downtime is minimized with regard to
critical analytical schedules. All repair work is recorded in instrUment maintenance logs with the
date, reason for the repair, action taken and name of the repair person.
Laboratory maintenance schedules for key instrUmentation is summarized below:
GC/MS
Extrel Instruments
1. Change septa
2. Change disc drive filter
3. Change mechanical pump oil
4. Grease turbo pumps
5. Change column
6. Change injection pon liner
7. Check gas cylinders
finnjgnn QWA Instruments
I. Change septa
2. Change card cage filter
3. Change disk drive filter
4. Change mechanical pump oil
5. Change turbo pump oil
6. Change tra\)s
7. Change columns
8. Change injection port liners
9. Check gas cylinders
Freauencv
daily
quanerly
quarterly
quarterly
monthly
daily
daily
Freanencv
daily -
quarterly
quarterly
quarterly
annually
monthly
monthly
weekly
daily
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!EA QA Manual
Section J I , Page 2 of 3
Date: August, 1988
G.£ I
Freauencv I
l. Change septa ~iweekly
2. Change injection pon liners monthly I 3. Change column as needed
4. Wipe test ECD's semiannually I 5. Check gas cylinders daily
-I,
Freouencv I
1. Check air and nitrogen tanks daily ,1
2. Check level in waste jug daily
3. C'ean nebulizer tips weekly I' 4. Rinse spray chamber weekly
5. Check drain tubing for air bubbles weekly
6. Clean torch assembly monthly I 7. Check purge extension windows monthly
8. Clean purge extension windows as needed I 9. Change vacuum pump intake trap 1000 hrs.
10. Change vacuum pump oil 1000 hrs. I 11. Clean computer ventillation slits semiannually
I Freouency
1. Check dials, panel lights and control u knobs for proper functioning daily
2. Check energy of deuterium background I corrector daily
3. Note AA !a'inp output daily
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(continued)
4. Check gas and water lines for leaks
5. Check graphite tube condition
6. Clean electrodes on furnace
7. Change electrodes on furnace
8. Clean burner head
9. Oean nebulizer and burner chamber
Analyzer
1. Sweep pyrolysis tube, check humidifer
water level, check gas supplies, check
furnace temperature, change injection pon
syst~m. b:Jance the totalizer.
2. Clean sample boat and push rod
3. Run system performance tests, lubricate
piston shaft, change septum, clean inlet tube
General Laboratory Areas
I. Clean laboratory
2. Check supply of consummable items
3. Inspect, clean and replace worn pans on
automatic pipes.
4. Calibrate automatic pipets
5. Calibrate thermometers
6. Record oven refrigerator temperatures
'(
7. Check fume hood air flow
8. Calibrate balances
Ecegueacv
.,monthly
daily
as needed
as needed
daily
daily
!EA QA Manual
Section J
Page 3 of 3
Date: August, 1988
Freouencv
biweekly
weekly
monthly
Fceouencv
weekly
weekly -
monthly
monthly
semiannually
daily
weekly
semiannually
K. Specific Quality Control Procedures for
Assessing Precision. Accuracy and Completeness
Precision
!EA QA Manual
Section K
Page l of 2
Date: August, 1988
Precision is a measure of the reproducibility among replicate analyses. Relative percent difference
(RPD) is calculated for duplicate sample spikes analyzed for the organic parameters and for all of
the duplicate sample analyses performed for the inorganic parameters. Data acceptance during
normal processing is based on the specific control limits for the common analyses which are listed
in Section G -Laboratory Quality Control Checks. Data obtained for all duplicates are evaluated
monthly by the QA Officer for developing trends.
(XI -X2) RPD= _____ _ ,c 100
(XI+ X2) /2
Accuracy
Accuracy is a measure of the degree of difference between the analytically obtained value and the
known or actual value for a sample. !EA assesses accuracy by determining the percent recovery
(o/oR) for analytes contained by designated quality controls samples. Acceptance criteria for spiked
samples processed by the laboratory are listed in Section G -Laboratory Quality Control Checks.
Data obtained for all laboratory spikes are evaluated monthly by the QA Officer for developing
trends.
Analytical Value
%R= ________ " 100
True Value
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Testior for QutHers
!EA QA Manual
Section K
Page 2 of 2
Date: August. 1988
The influence of "bad" data on the statistical data is controlled by discarding true outliers before the
statistical evaluations are performed. Outliers are discarded if the individual value (X) mulitiplied
by the average absolute deviation of all values from the mean (D) is greater than 2.3 times the
average absolute deviation of all values from the mean.
Completeness
Completeness is a measure of the valid data obtained from an analysis expressed as the percentage
of the total data that should have been obtained.
amount of valid data obtained
% Completeness= _____________ x 100
total amount of valid data expected
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IEA QA Manual
Section L I
Page 1 of I
Date: August, 1988
L. Corrective Action for Data Inadequacy
In the preceeding sections. IEA's data acceptance criteria have be!n presented. Failure to meet any
of the specified acceptance criteria requires correction of the failure before the analysis of reportable
sample data. Corrective action may consist of instrument maintenance, recalibration of the
equipment, reanalysis of a sample or re-extraction of a sample followed by analysis of the new
extract.
Occasional! y, a failure is caused by a panicular sample. In those cases, the department supervisor
or Laboratory Manager is responsible for the investigation and documentation of the problem as
well as documentation of the measures taken·to control the sample induced failure. A description of
the problem and the control measures are included in the sample data report as well as in the
laboratory records.
Problems identified during the quality control audit process are addressed in the Quality Assurance
Summary Repon with recommended corrective action(s). The implementation of the corrective
action( s) is recorded in the laboratory records with the results of each action.
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M. Quality Assurance Reports to Management
!EA QA Manual
Section M
Page l of I
Date: August. 1988
The primary objective of IEA is to provide legally and scientifically defensible data to clients in a
timely and cost effective manner. The achievement of this goal is dependent upon an active QNQC
program. The QA Officer is responsible for monitoring laboratory compliance with all elements of
the QA/QC program and communicating the starus of the program to the President and other
' '
members of the senior management.
The results of the monthly and quanerly quality assurance audits are summarized and distributed to
the President, Laboratory Manager, and department supervisors. The current surrogate recoveries,
spike recoveries, duplicate comparisons, method blanks results, recent blind QC sample results,
adherence of each department to the written quality control procedures, and any identified anomolies
in the quality control data or procedures are included in the summary report. Corrective actions
steps are included in the summary report as required by the audit results.
IEA QA Manual
Section N
Page l of 1
Date: August, 1988
N . Personnel Qualifications
General
All persons hired or assigned to key laboratory positions at !EA work closely with experienced
personnel. Their program and performance is closely supervised and evaluated. The principal
criterion for employment or assignment is demonstrated professional proficiency at IEA or at
previous places of employment
Laboratocv Stace 1\Jemhers
The qualifications of key laboratory staff members are summarized in the appended resumes. We
have developed an organization of technical specialists in all major disciplines of the environmental
sciences. Each person is througrJy t:ained and experienced in his;her respective field and qu;.ji£~J
to function with other staff members to form an integrated team.
Required educational and experience qualifications of key laboratory personnel are described below:
Laboratory Manager:
B.S. degree in Chemistry, with a minimum of 10 years of environmental
laboratory experience.
Customer Service Manager:
B.S. degree. with a minimum of 10 years of laboratory e-xperience.
Quality Assurance Orficer:
B.S. degree in Chemistry, with a minimum of 10 years of laboratory experience.
Laboratory Department Supervisors:
Bachelors degree in scientific discipline. with minimum of 3 years of
envirqnmental laboratory experience or equivalent.
Technical Reviewer:
B.S. degree in scientific discipline with a minimum of 2 years of environmental
laboratory experience.
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Responsibility:
Education:
Experience:
Mark Randall
Manager Analytical Services
Mr. Randall is responsible for the overall administration and management of
the production laboratories. His duties include facilities planning, evaluation
and selection of analytical instrumentatiOI\, training and development of the
laboratory staff, and the assignment and evaluation of laboratory personnel.
Mr. Randall is also responsible for overseeing the administration of the
quality assurance protocols within the production laboratories.
Mr. Randall received a B.S. degree in Biology from the University of
Rhode Island in Kingston, Rhode Island in I 977.
From February 1987 to December 1987 Mr. Randall was responsible
for the supervision of the second shift staff. In addition to his super-
visory responsibilities, he was responsible for the operation and main-
tenance of two GC/MS instruments and the review of GC/MS data.
From October 1985 to February 1987 Mr. Randall served as IEA's
Shift Supervisor and GC Chemist. He also was responsible for all
identified special projects. In this capacity, he operated and maintained
the GC instrumentation, evaluated all gas chromatography data gener-
ated, developed and validated all new methods for the GC Department
and wrote the final repons for all special projects.
Grainger Laboratories, Inc.
Raleigh, North Carolina
From November 1984 to October I 985 Mr. Randall was employed as
a GC Chemist. In that capacity he was responsible for the operation
and maintenance of the GC instrumentation and evaluation of
chromatographic data.
Exxon Chemicals
Baytown, Texas
From November 1981 to October 1984 Mr. Randall was employed as
a Research Analyst In that capacity he was responsible for the super-
vision of the research laboratory. He was also responsible for the
operation of the developmental pilot units, and development and valida-
. tion of new methods and procedures. ,,
Experience:
(continued)
Affiliations:
NUS
Mark Randall
Manager Analytical Services
(continued)
Oearlake, Texas
From October 1978 to September 1981 Mr. Randall was employed as
a Chemical Analyst. In that capacity he served as a shift supervisor
with responsibility for organic extractions, metals analysis and inorganic
analysis and data interpretation.
American Industrial Hygiene Association
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Patty L. Ragsdale
Manager Technical Product Support
Manager Quality Assurance
Responsibility: Ms. Ragsdale is responsible for overseeing all phases of interaction between
!EA and clients after the sale of a product including technical assistance in
product selection and consultations on final data repons. Her departmental
responsibilities include Customer Service and Repon Generation. Ms.
Ragsdale is also responsible for the management of identified special projects.
Education: Ms. Ragsdale received a B.S. degree in Chemistry from Furman
University in Greenville, South Carolina in 1973.
Experience: CompuChem Laboratories
Research Triangle Park, North Carolina
From 1986 to 1987 Ms. Ragsdale served as Director of Technical
Affairs, in that capacity she was responsible for overseeing the dev-
lopment processes involved in the introduction of new products to the
product line. She was responsible for the technical oversight and
review of impact of new methods and products on the production
laboratory, evaluation of laboratory capacities with regard to special
projects and newly developed products. She made recommendations
for product development and improvement to ensure that the laboratory
has the ability and flexibility to respond to client needs. She also
assisted the Sales and Marketing staff in matching product line elements
with client needs.
From 1984 to 1986 she was Manager Semi-Volatile Analyses. In this
position she was responsible for the management of the preparation and
analysis of each semi-volatile sample in a timely, accurate and cost
effective manner. A custom tracking system designed and implemented
by Ms. Ragsdale allowed this laboratory to systematically process
samples according to priority from assignment of GC/MS instruments
through the data review process.
From 1983 to 1984, Ms. Ragsdale managed the Sample Preparation
Laboratory. As Manager of this section she was responsible for the
accurate and timely preparation of each sample for analysis.
From 1980 to I 983, Ms. Ragsdale was responsible for_the establish-
ment and management of the Quality Control Department As Manager
Quality Control she was responsible for ensurring that the quality of the
laboratory analyses performed and the data reponed to clients were of
the best quality possible.
From 1979 to 1980, Ms. Ragsdale operated a variety oflaboratory in-
stru~ents, including GC/MS, AutoAnalyzer and gas and liquid chroma-
tographs in her position as Senior Chemist.
Patty L. Ragsdale
Manager Technical Product Support
(continued)
Southern Analytical, Inc.
From 1978 to 1979, Ms. Ragsdale was employed by Southern Analyti-
cal Inc. She was involved in the sales and service of gas and liquid
chromatographic systems.
South Carolina Deparunent of Health & Environmental Control
Columbia, South Carolina
From 197 4 to 1978 Ms. Ragsdale was employed by the South Carolina
Deparnnent of Health and Environmental Services. As a Chemist I, she
served as a group leader for AutoAnalyzer analyses from 1974 to
1976. During that time she worked extensively on the development of
a quality assurance program for that laboratory and six regional labora-
tories. Following promotion to Chemist II, she served as group leader
of chromatographic analyses, reviewing all chromatograms and work
associated with GC and GC/MS analyses.
South Carolina Department of Mental Health
Columbia, South Carolina
From 1973 to 197 4 Ms. Ragsdale was employed by the South Carolina
Department of Mental Health as a Laboratory Specialist Her work
involved the separation of various drugs and their relative metabolites
from biological tissues and the quantitative analysis of the separated
compounds.
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Toivo E. Niemi
Supervisor GC/MS and GC Department
Responsibility: Mr. Niemi is responsible for the timely, accurate and efficient analysis of
client samples by GC/MS. His duties include maintenance of the GC/MS
instrumentation, training of staff members and evaluation of generated
sample data. In addition to his production responsibilities, Mr. Niemi is
responsible for the administration of the quality control requirements defined
for the GC/MS analyses.
As supervisor of the GC department, Mr. Niemi is responsible for the
timely, accurate and efficient analysis of clients samples for organic content
by GC. He is responsible for sample analysis scheduling, review of the data
generated, development of new analytical methods and training of staff
members. In addition to his production responsibilities, Mr. Niemi is
responsible for the administration of the quality control requirements which
have been defined for GC analyses.
Education: Mr. Niemi received a B.A. degree in Chemistry from Cornell Uni-
versity. He received a M.S. degree in Environmental Chemistry
from the University of Virginia in 1985.
Experience: IEA
From September 1984 to August 1985 Mr. Niemi was employed as
Staff Chemist. In that capacity he was responsible for the operation
and maintenance of the GC and GC/MS instruments, review of the
generated data and the preparation of the data reports.
University of Virginia
Charlottesville, Virginia
:-From 1981 to 1984 Mr. Niemi was a Graduate Research Assistant. His
responsibilities included the development of field and laboratory
methods. This work was pursuant to his advanced degree in Environ-
mental Chemistry.
From May 1979 to August 1979, Mr. Niemi was a Technical Assistant
for Dr. Fred W. Mclafferty. His responsibilities included calibration
and operation of an experimental MS/MS instrument designed
specifically for research.
Toivo E. Niemi
Supervisor GC/MS and GC Department
(continued)
Publications: · McLaffeny, Fred W., Peter J. Todd, Donald G. McGilvery, Michael
A. Baldwin, Frank M. Brockhoff, Gregory J. Wendel, Michael R.
Wixom and Toivo E. Niemi. "MS/MS: A New Separation/Identi-
fication Technique for Complex Organic Mixtures." Advances in~ Specrromea:y. 8B, 1589-96.
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Juliana K. Niemi
Technical Support Supervisor
Responsibility: Ms. Niemi is responsible for the final technical review of data reports
and for issuing release approval for those reports. Her technical
review encompasses all elements of the analytical process affecting
the integrity of the data repons from sample receipt and log-in to the
analysis and the final typing of the report In addition to the technical
review function, Ms. Niemi provides technical assistance to clients and
to the laboratory staff in the selection of analytical methods for unusual
or difficult sample matrices.
Education: Ms. Niemi received a B.S. degree in Floriculture/Horticulture in 1983
from North Carolina State University in Raleigh, North Carolina. She
has continued her education in chemistry at the University of North
Carolina at Chapel Hill.
Experience: IEA
From June 1987 to September 1987 Ms. Niemi reviewed data produced
by the GC Department. During that time she also assisted in the im-
. plementation of more complete documentation of the quality control
program within the laboratory.
From September 1985 to June 1987 Ms. Niemi was employed as a
GC/MS operator. In that capacity she operated 2 GC/MS instruments,
reviewed data produced within the GC/MS laboratory for accuracy
and viability, prepared laboratory data repons and assisted in the
rraining of six (6) other GC/MS operators. She also served as the
Second Shift Supervisor from March 1986 until February 1987.
From March 1985 to September 1985 Ms. Niemi performed metals
analyses by atomic absorption, TOX analyses, ion chromatography,
·-11J1d organic analyses·using infrared spectroscopy and HPLC. She also
assisted with bacteriological analyses, extractions, and the classical
wet chemistry analyses on an as needed basis.
From October 1984 to March 1985 Ms. Niemi was primarily responsible
for bacteriological analyses, TOX and the analysis of certain inorganic
components using selective ion electrodes. ·
From June 1984 to October 1984 Ms. Niemi was employed as an
Extractionist. In that capacity she was responsible for the preparation
of liquid and solid samples for analysis of pesticides, herbicides,
base-neutral and acid extractable compounds by GC and GC/MS.
Juliana K. Niemi
Technical Support Supervisor
(continued)
Nonh Carolina State University
Raleigh, Nonh Carolina
From September 1982 to April 1984 Ms. Niemi was employed as a
Laboratory Technician working on a research project funded by the
U.S. Department of Agriculture. She analyzed sweet potatoes for
total Kjeldahl nitrogen, metals and mineral content as part of the
research project.
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Responsibility:
Education:
Experience:
Edgar E. Folk IV
Technical Officer
As Technical Officer for !EA, Mr. Folk is responsible for troubleshooting
instrumentation and methodology to promote efficient sample analysis. He
is also responsible for method development and the refinement of current
instrumentation and methodology. In addition to his technical duties, Mr.
. Folk is responsible for personnel training of new products.
Mr. Folk received a B.A. degree in Chemistry from Wake Forest
University in Winston-Salem, North Carolina in 1981.
!EA
From August 1985 to September 1988 Mr. Folk was employed as a GC
OtemisL He implemented the use of standard operating procedures
in the GC Laboratory and was responsible for the development,
validation and implementation of new methods and procedures
in the laboratory. He also was responsible for the routine analysis
of environmental samples for pesticide, herbicide, PCB, and volatile
content using gas chromatographic techniques and the evaluation of
the resulting data.
Grainger Laboratories, Inc.
Raleigh, Nonh Carolina
From 1983 to 1985 Mr. Folk was employed as the GC Department
Supervisor. In that capacity he was responsible for the analysis of
environmental samples for pesticide, herbicide, PCB, and volatile
compounds.
Webb Food Lab, Inc.
Raleigh, Nonh Carolina
From 1982 to 1983 Mr. Folk was employed as the GC Laboratory
Supervisor. In that capacity he was responsible for the development and
implementation of methods required by a contract with U.S. Department
of Agriculture for pesticide analyses.
Edgar E. Folk IV
Technical Officer
(continued)
Nonh Carolina Depamnent of Natural Resources and
Community Development
Raleigh, Nonh Carolina
From 1981 to I 982 Mr. Folk was employed as a Chemist Analyst I.
He was responsible for the analysis of environmental samples for
pesticides, herbicides and priority pollutants by GC and GC/MS.
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Res ponsi bili ty:
Education:
Experience:
Keith B. Scott
Assistant Supervisor GC Department
As assistant supervisor of the GC Laboratory, Mr. Scott is responsible
for assisting in the scheduling of sample anlllyses, review of data
generated, development of new analytical methods and training of staff
members. He is responsible for ensuring that each sample is screened/
analyzed within allowable timeframes. He is also responsible for
ensuring that the necessary extraction preparation information is pro-
vided to the Extractions Department in time for each extraction to be
performed with specified holding times.
Mr. Scali received a B.S. degree in Ecology from the University of
Nonh Carolina in Wilmington. Nonh Carolina in 1986.
IE.A
From October 1986 to April 1987 Mr. Scoll was employed as a GC
Analyst In that capacity he performed analyses of samples for
volatile organic, pesticide, herbicide, polychlorinated biphenyl (PCB)
and fuel oil content using gas chromatographs.
From July 1986 10 October 1986 he was employed as an Organic
Extracrionist. In that capacity he prepared water and solid samples for
analysis by GC, GC/MS and IR. Gel permeation chromatography was
employed as necessary 10 "clean up" the extracts of complex sample
matrices.
Institute of Marine Biomedical Research
Wilmington. Nonh Carolina
From July 1985 to Spetember 1985 Mr. Scali was employed as a Labora-
tory Technician. In that capacity he performed experiments on the effects
of pressure and temperature on fresh water and marine fish.
Nonh Carolina Marine Resources Center
Fon Fisher, Nonh Carolina
From September 1983 to May l 984 Mr. Scali was employed as an
Aquariums Department Technician. He assisted in the maintenance of the
aquariums for fresh and saltwater organisms. His duties included
verification of pH, salinity, temperature and performing growth
studies.
Responsibility:
Education:
Experience:
Affiliations:
Darrell P. Johnson
Supervisor Inorganic Department
Mr. Johnson is responsible for the timely, accurate and efficient analysis
of client samples for inorganic content. He is responsible for scheduling
the various sample analyses, reviewing the analytical results and train-
ing his staff. In addition to his production responsibilities, he is re-
sponsible for the administration of the quality conaul requirements de-
fined for the inorganic analyses.
Mr. Johnson received a B.S. degree in Textile Chemistry in I 978 and
a second B.S. degree in Chemistry in 1987. Both degrees were
awarded by North Carolina State University in Raleigh, North Carolina.
Cannon Mills
Kannapolis, North Carolina
From June 1978 to September 1985 Mr. Johnson was employed as
Technical Manager for Cannon Mill's Print Department. In that
capacity he was responsible for the management of the laboratory
and the associated staff. He also was responsible for product develop-
ment and the investigation of production problems arrising from
technical difficulties.
American Chemical Society
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Responsibility:
Education:
Experience:
Affiliations:
Darrell P. Johnson
Supervisor Sample Preparation Department
Mr. Johnson is responsible for supervising and perfonning extractions for
organic analysis according to EPA protocol. Supervision and perfonning
EP-Toxicity Leaching Procedure and TCLP procedures for all analysis
types.
Also responsible for maintaining work flow for extractions to ensure
protocol and to make sure that production deadlines are met
Must ensure that all quality control guidelines are strictly adhered to and
documented.
Must maintain a trained technical staff for the Sample Prep Department.
Mr. Johnson received a B.S. degree in Textile Chemistry in 1978 and a
second B.S. degree in Chemistry in 1987. Both degrees were awarded by
N.C. State University in Raleigh, NC
Cannon Mills
Kannapolis, NC
·From June 1978 to September 1985, Mr. Johnson was employed as
Technical Manager for Cannon Mills' Print Department. In that capacity he
was responsible for the management of the lab and the associated staff. He
also was responsible for product development and the investigation of
production problems arising from technical difficulties.
American Chemical Society
Responsibility:
Education:
Experience:
Alan T. Lynch
SuperYisor Metals Department
As Metals Analysis Supervisor. Mr. Lynch is responsible for the timely,
accurate and efficient analysis of client samples for metals content. In
addition to production responsibilities, he is responsible for the
adminisrration of the quality conrrol requirements defined for the metals
depanment.
Master of Science -Analytical Chemisrry -May of 1986
Minor -Chemical Oceanography
North Carolina State University, Raleigh, NC
GPA -3.0 I 4.0
B.A. -Marine Chemisrrv -Mav 1983
University of North Carolina at Wilmington
Wilmington, NC
GPA -3.3 I 4.0 Dean's Honor List
IEA -August 1988 -Present
Technology Applications, Inc. c/o EPA College Station Road
Athens, GA -Analytical Chemist -May 1986 to August 1988
. Responsibilities:
Managed laboratory that conducted experiments on the thermodynamic
and kinetic aspects of metal sorption and speciation on environmental
surfaces.
Developed and pen·ormed atomic spectromerry techniques for the
Chemical Research Division of the Athens EPA.
Supervised 3 other laboratory employees
Nonh Carolina State University -Depanment of Chemisrry
September 1983 -May 1986
Teaching Assistant -Instructed senior level Quantitative Analysis and
General Chemisrry Laboratories
General Electric -Nuclear Division
', Wilmington. NC
Research Assistant
May 1983 -September 1983
Research in waste water rrearrnent and analvsis
(Summer employment -full time) ·
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Areas of
Expertise:
Areas of
Experience:
Alan T. Lynch
Supervisor Metals Department
(continued)
Plasma. Flame, and Electrotherrnal atomic abso_rption and emission
spectrometry . ,
UV-Vis and molecular absorption and emission spectrometry
Waste water analysis and treatment
GC, HPLC, NMR, electrochemical methods, computer interfacing, ion
chromatography, knowledge of neutron activation analysis, mass
spectrometry, isotopic daring and organic geochemistry
0. Facilities
!EA QA Manual
Section 0
Paee 1 of 2
Date: August, 1988
!EA occupies a 15.300 square foot building of which approximately 70% is dedicated to the
analytical laboratories. Separate laboratory areas are dedicated to GC instrumentation. GC/MS
instrumentation. organic extractions, sample preparation for volatile analysis, metals analysis by
atomic absorption, metals analysis by inductively coupled plasma (ICP), standards preparation, and
preliminary sample screening.
The laboratory is divided into seven (7) temperature controlled zones. The heating and air condition
control for these areas is provided by 62 tons of heating/air conditioning equipment. The overall
building air flow sweeps from its entry in the trace level GC and GC/MS laboratories through the
other analytical laboratories and exits the building in the extractions laboratory areas which are at the
opposite end of the building.
The laboratory has eleven ( 11) fume hoods strategically located for a total of over 60 linear feet of
hood capacity. 110/220 volt circuits power the instrumentation. Critical instrumentation such as
GC/MS units, data systems and selected gas chromatographs are equipped with uninterruptable
power supplies (UPS). Other instruments, such as atomic absonion spectrometer, ICP and gas
chromatographs used for routine analyses are protected with Topaz power conditioners.
A standard preparation area equipped with an enclosed negative pressure bio-hazard
hood with interlock is used for the preparation of standards from highly hazardous pure
compounds. Less hazardous standards and dilutions of prepared standards are prepared in a
separate laboratory area.
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!EA QA Manual
Section 0
Page 2 of 2
Date: August. 1988
Laboratory reagent water is produced by a Millipore reverse osmosis unit which feeds a 30 gallon
' storage tank which in tum feeds a Barnstead deionized water system. A pair of 5 gallon tanks of
the resulting reagent grade water are heated and purged with nitrogen to generate the organic-free
reagent water required for the volatile analyses. Each 5 gallon tank is purged for a minimum of 24
hours and tested for volatile organic content prior to use. A second deionized water system capable
of producing 18 Megohm water provides cleaning and rinse water for the glassware preparation
area.
The glassware preparation area is equipped with a 24 cubic foot muffle furnace. All extraction and
sample preparation glassware is treated at 45Q<>C for 4 hours immediately prior to each usage.
Four locked commercial refrigerator units are used to house samples waiting for analysis. Twelve
locked laboratory refrigerators. located throughout the laboratory, are used to maintain sample
extracts or laboratory reagents. Each laboratory refrigerator is dedicated to sample (extract) storage
or reagent storage.
Access to the laboratory is carefully controlled through the use of key locked and combination
locked entry doors. All visitors are escorted while inside the building.
P. Laboratory Equipment
Gas Chromatography/Mass Spectrometry Instrumentation
2 Extrel EQL-400 MS equipped with
Hewlett Packard 5890
Hewlett Packard 7673A Auto Sampler
Pericom Montery MQ600 Terminal
160 Mb CDC Disk Drive
Cipher 9-ttack Magnetic Tape System
1 Finnigan OW A -1020 equipped with
Tekmar LSC-2000
Tekmar ALS-2016
Graph On GO-230 Terminal
CDC 32 Mb Disk Drive
WangCo 10 Mb Disk Drive
!EA QA Plan
Section P
Page I of 8
Date: January, 1989
Perkin Elmer Mod 10 NRZI 9-track Magnetic Tape Transport
Printronix P-300 Printer
1 Finnigan OW A -1020 equipped with
Tekmar LCS-2
Tekmar Automatic Heated Sampler Module Model 4200
Graph On GO-230 Terminal
160 Mb CDC Disk Drive
CDC 32 Mb Disk Drive
WangCo 10 Mb Disk Drive
Perkin Elmer Mod 10 NRZI 9-track Magnetic Tape Transport
Printronix P-300 Printer
1 Finnigan Stand Alone Data System equipped with
Data General NOV A 4C/5 Computer
CDC 32 Mb Disk Drive
Graph-On GC-230 Terminal
Kennedy 9600 9-track Magnetic Tape System
Printronix P-300 Printer
-------·----------
Total GC/MS Instrumentation:
4 GC/MS Instrumentation
I Additional Stand Alone Data System
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Gi15 Cbc!lmill!ll:CilllbX Ioslcum,olilli!lD (C11oliou,dl
1 Hewlett Packard 5890 GC equipped with
2 Flame Ionization Detectors
7673 Dual Tower Autosampler
2 Hewlett Packard 3396A Integrators
1 Hewlett Packard 5890 GC equipped with
2 Electron Capture Detectors
7673A Dual Tower Autosampler
Hewlett Packard 3392A Integrator
Spectra-Physics SP-4290 Integrator
1 Perkin Elmer Sigma 300 GCs equipped with
Photo Ionization Detector
Electrolytic Conductivity Detector
Tekmar LSC-2 Purge & Trap Unit
Tekmar ALS Auto Sampler
Spectro-Physics SP-4290 Integrator
1 Perkin Elmer Sigma 300 GCs equipped with
Photo Ionization Detector
Electrolytic Conductivity Detector
Tekmar LSC-2 Purge & Trap Unit
Spectra-Physics SP-4290 Integrator
Tekrnar ALS Auto Sampler
1 Perkin Elmer Sigma 2 GC equipped with
Flame Ionization Detector
· . -Nitrogen Phosphorus Detector
Tekrnar LSC-2 Purge & Trap Unit
LCI-100 Integrator
1 Perkin Elmer Sigma 300 GC equipped with
Electron Capture Detector
Flame Photomeaic Detector
Perkin Elmer AS-300 Auto Sampler
Spectra-Physics SP-4290 Integrator
1 Tracor 540 GC equipped with
Electron Capture Detector
Flame Photomeaic Detector
Spectra-Physics SP-4290 Integrator
Tracor 771 Auto Sampler
IEAQAP!an
Section P
Page 2 of 8
Date: January, 1989
Gas Chromatogcaohv Instrumentation (Continued)
1 Perkin Elmer Sigma 38 GC equipped with
Electron Capture Detector
Aame Ionization Detector
Spectro-Physics SP-4290 Integrator
Perkin Elmer AS-300 Autosampler
1 Perkin Elmer Sigma 1B GC equipped with
Electron Capture Detector
Connected to Sigma 18 Data System
1 Perkin Elmer Sigma 300 GC equipped with
2 Flame Ionization Detectors ·
Perkin Elmer AS-300 Auto Sampler
Spectra-Physics SP-4290 Integrator
1 Perkin Elmer Sigma 300 GC equipped with
2 Flame Ionization Detectors
Connected to Sigma 15 Data System
1 Tracor S40 GC equipped with
2 Flame Ionization Detectors
Spectra-Physics SP-4290 Integrator
1 Tracor 540 GC equipped with
Flame Ionization Detector
Spectra-Physics SP-4290 Integrator
Hall 1000 Electrolytic Conductivity Detector
Hewlett Packard HP 19395A Headspace Sampler
1 Perkin Elmer 910 GC equipped with
Thermal Conductivity Detector
Shimadzu CR3A Integrator
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IEAQAP!an
Section P I Page 3 of 8
Date: January, 1989
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G"s Chromato~canhv Instrumentation <Continued)
1
2
1
1
Perkin Elmer Sigma 18 GC equipped with
2 Flame Ionization Detectors
Thermal Conductivity Detector
Hewlett Packard 3390A Integrator
Connected to Sigma 18 Data System
Spectra-Physics ChromStation Data System
Perkin Elmer Sigma Data Station
Perkin Elmer Sigma 15 Data Station
Total Gas Chromatography Instrumentation
15
15
4
GC Instruments
Integrators
Stand Alone Data Systems
IEAQAP!an
Section P
Page 4 of 8
Date: January, 1989
!EA QA Plan
Section P
Page 5 of 8
Date: January, 1989
Atomic A hsorptioo/ICP Instrumentation
1
1
1
2
Perkin Elmer Plasma II Inductively Coupled Argon
Plasma Emission Spectrometer equipped with
Perkin Elmer Model 7500 Computer System Controller
Perkin Elmer PR-210 Color Printer
AS-51 Autosampler
Perkin Elmer Zeeman 5100 Atomic Absorbtion
Specctrophotometer equipped with
EPSON EX-800 Printer
Graphite Furnace
AS-60 Autosampler
EPSON Equity III plus Computer System
Perkin Elmer Zeeman/3030 Atomic Absorption
Spectrophotometer equipped with
HGA-600 Power Unit
PR-100 Printer
AS-60 Autosampler
Flame Unit
Perkin Elmer Model 5000 Atomic Absorption
Spectrophotometer equipped with
Atomic Spectroscopy Data System 10
PR-100 Printer
AS-40 Autosampler
Graphite Furnace
AS-50 Autosampler
Automatic Burner Control
Total Atomic Absorption/lCP Instrumentation
4 Atomic Absorption Instruments
1 Inductively Coupled Argon Plasma Instrument
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Elemental Analvsis Instrumentation
1 Kevex 8000 Elemental X-Ray Analyzer
IEAQAP!an
Section P
Page 6 of 8
Date: January, 1989
1 JOEL Model 35C Scanning Electron Microscope with 3-Axis
Automated Image Analyzer
1 JSM-840A Scanning Electron Microscope
--------
Total Elemental Analysis Equipment
1
2
Elemental X-Ray Analyzer
Scanning Electron Microscopes
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IEAQAP!an
Section P I Page 7 of 8
Date: January, 1989
I
Miscellaneous Laboratory Equipment I
1
2
3
4
5
6
7
8
9
10
11
Milton_ Roy Spectronic 1201 Spectrometer
Xertex Dohrman TOC Analyzer with Sample Conditioning Module
Dohrman Envirotech TOX Analyzer
Waters Lambda Max Model 481 LC Spectrometer Model 510 Solvent
Delivery System Differential Refractometer
IEC HN-SII Centrifuge
Tekmar Sonic Disrupter (For Sample Preparation)
Perkin Elmer No. 1430 Ratio Recording Infrared Spectrometer
Dughi Rotovapor Rll0
Bausch & Lomb Spectronic 21 Spectrometer
YSI Model 32 Conductance Meter
Fisher Model 447 Coulomatic K-F Titrimeter
12 Fisher Model 2200 Analytical Balance
13
14
15
16
17
18
19
20
21
22
Fisher XT Analytical Balance
Two Fisher Model 805 MP pH/Mv Meter
Fisher Model 825 MP pH/Mv Meter
ABC Laboratories Gel Permeations Chromatography.
Fisher ISOTEMP 200 Series 255G Oven
Fisher ISOTEMP 200 Series Oven
Fisher ISOTEMP 300 Series Oven Fisher
ISOTEMP 230F Oven
Fisher ISOTEMP 501 Oven .,
Market Forge Sterilmatic Autoclave
Millipore/Barnstead 18 Megohm RO/DI Water System
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Miscellaneous I.ahocatorv Eauiomeot CContiunedl
2 3 Labconco Protector 4 Ft. Fume Hood
2 4 Labconco Protector 6 Ft. Fume Hood
IEAQAP!an
Section P
Page 8 of 8
Date: January, 1989
2 5 Labconco Protector 5 Ft. Fume Hood with outside air make-up
26 Labconco 4 Ft. Glove Box
2 7 Fisher 5 Ft. Fume Hood with outside air make-up
28 Fisher 6 Ft. Fume Hoods withoutside air make-up
2 9 Perlick Stainless Three Door Commercial Cooler
30 Howard Stainless Three Door Commercial Cooler
31 Howard Stainless Single Door Commercial Cooler
3 2 Three Single Door Laboratory Refrigerators
3 3 Eight Single Door Laboratory Refrigerators
3 4 Four Topaz Power Conditioners
3 5 Three Uninterruptible Power Supplies for GC/MS
Systems (49 KV a Total)
36 Cannon NP-8570 High Speed Copier
Q. Chemicals and Reagents
!EA QA Manual
Section Q
Page 1 of 2
Date: August, 1988
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The chemicals and reagents used by !EA are selected with extreme care. Solvents, chemicals and I
analytical standards are purchased in large quantities to minimize the number of reagent lots.
Reagent lot numbers are recorded for every analytical batch processed.
"Analytical reagent grade" is the minimum quality used within the !EA laboratory. Ultra pure acids
are employed for low detection limit metals analyses. Pesticide grade solvents are used for all
organic extractions.
Each new lot solvent is tested prior to acceptance for use in sample analysis. The extraction
solvents are concentrated to duplicate the concentration employed by the extraction process and
analyzed. Solvents used for the analysis of volatiles are analyzed using the same solvent volume
and analytical technique used for samples. The acceptance criteria for new solvent lots are:
1. No analyte present at concentrations equal to or greater than one-half the reponed quantitation limit
2. No non-analyte peak present in the test chromatogram which is greater than 10% of the closest internal standard for GC/MS analyses or which would interfere in the identification and quantitation process for GC analyses.
Each lot of acid is tested prior to acceptance for use in sample analysis. A blank water sample is
prepared for analysis using the new acid Jot in the same manner used for sample analyses. For
acceptance, a new acid11ot must be proved to be free of all analytes at the reponed quantitation limit.
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!EA QA Manual
Section Q
Page 2 of 2
Date: August, 1988
Records showing the exact reagent lots employed are maintained for all analyses. The method
blanks prepared for each set of samples serve as continual verification of the quality of the reagents
as well as the quality of the total analytical environmental.
All analytical standards are traceable to EPA certified standards. Each new lot of analytical
standards is analyzed versus a corresponding standard obtained from the EPA. Both standards
must be within 20% of each other for the new analytical standard to be accepted for use by the
laboratory. Relative response of the analytes in the standards is monitored by the production staff
and by the QA Officer to ensure that the integrity of each analytical standard is maintained.
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I DAVIS AND FLOYD, INC.
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I 5050N013
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DAVIS & FLOYD, INC.
I LABORATORY QUALITY CONTROL MANUAL
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I JANUARY, 1980
REVISED FEBRUARY, 1983
I SECOND REVISION OCTOBER, 1985
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DAVIS & FLOYD, INC.
LABORA~ORY QUALITY CONTROL MANUAL
REVIEWED B y·,..,:::::-:::::::j.-:J_}.~-:;4~(4_'.Jk,~~-tj:_:=..._..Q.l.:_-~,2~-.1f32,L:__
APPROVED B Y.....:::~~,;..4~~-!.f.(.!UL~~~-....,:0:::!1~-::.!L:...-=.g..z_ ___ _
REVIEWED BY L
AP PROV ED By \_/ J-'eme? ~ fl
REVIEWED BY ____________________ _
APPROVED BY ____________________ _
REVIEWED BY ____________________ _
APPROVED BY ____________________ _
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IV.
V.
TABLE OF CONTENTS
APPROVED METHODOLOGY
A. Chemical/Physical
B. Microbiology
C. Aquatic Biology
D. Table of Approved Test Procedures
QUALITY CONTROL FOR ANALYTICAL PERFORMANCE
A. Standard Curves
B. Reagent Standardization
C. Gravimetric Analysis
D. Quality Control Checks
E. Quality Control Charts
F. Interlaboratory Quality Control
G. Microbiology Quality Control Checks
H. Quality Control for Organic Analysis
CHAIN OF CUSTODY
A. Sample Collection.
B. Laboratory Custody
LABORATORY PURE WATER
LABORATORY EQUIPMENT
A. Analytical Balance
B. pH Meter.
C. Spectrophotometer
D. Atomic Absorption
E. Organic Carbon Analyzer
F. Gas Chromatograph
G. Conductivity Meter
H. Turbidimeter
I. Drying Oven
J. Refrigerator
K. Incubators
L. Autoclave
M. Microscope
N. Atomic Absorption o. Gas Chromatograph-Mass Spectrometer
Page
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17
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19. l
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29
32
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35
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38
38
TABLE OF CONTENTS (Continued)
VI. GLASSWARE
A. General
B. Types of Glassware
C. Volumetric Analysis
D. Federal Specifications
E. Cleaning of Glass and Porcelain
F. Special Cleaning
G. Disposable Glassware
H. Specialized Glassware
I. Fritted Ware
VII. REAGENTS, SOLVENTS, AND GASES
A. Introduction
B. Reagent Quality
C. Elimination of Detenninate Errors
VIII. LABORATORY SAFETY
A. Infectious Materials
B. Corrosive Chemicals
C .. Toxic Materials
D. · Explosive or Inflammable Matei:ials
E. Broken Equipment ·
F. Miscellaneous.
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50 I 52
52
54 I 59
59 I 59
66
74 I
74 I 74
76.
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77 I 78
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I.
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APPROVED METHODOLOGY
A. Chemical/Physical
1. Federal Register -Monday, December 3, 1979
Part III, Environmental Protection Agency
Guidelines establishing test procedures for the
analysis of pollutants; proposed regulations.
2. NIOSH Manual of Analytical Methods
Second Edition -Volume 1-4
3. standard Methods for the Examination of Water and
Waste -14th Edition.
4. Methods for Chemical Analysis of Water and Waste
I Environmental Protection Agency, 1974 and 1976.
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B.
c.
5. ASTM
6. Manual of Analytical Quality Control for Pesticides
in Human and Environmental Media -Environmental
Protection Agency.
7. USEPA Contract Lab Program, Inorganics Analysis,
sow 787 of July, 1987 as amended (#1) in July,
1987.
Microbiology
1. Standard Methods for the Examination of Water and
waste, 14th Edition.
2. Microgiological Methods for Monitoring the Environ-
ment, Environmental Protection Agency.
Aquatic Biology
1. Standard Methods for the Examination of Water and
Waste.
2. Methods for Measuring the Acute Toxicity of
Effluents to Aquatic Organisms -Environmental
Protection Agency.
2
D. Table of Approved Test Procedures
PARAMETER & UN ITS
l. Acidity, as Caco 3 mg/1
2. Al ka l in i ty, as Ca CO 3, mg/l
3. Arrmonia (as N), mg/1
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
23.
Bacteria
Colifonn (Fecal),
Col ./100 mls.
Colifonn (Total),
Col ./100 mls.
Fecal streptococci,
Col ./100 mls.
8005, mg/1
Bromide, ·mg/1
COO,· mg/1
Chloride, mg/1
Chlorine-Total
Residual, mg/1
Color, Platinum Cobalt Units.
Cyanide, Total, mg/1
Cyanide, Amenable to
Chlorination, mg/1
Dissolved Oxygen, mg/1
Fluoride, mg/1
Hardness-Total as
CaC03, mg/1 .
Hydrogen Ion (pH),
pH Units
Kjeldahl Nitrogen (as N),
mg/l
Nitrate (as N), mg/1
Nitrite (as N), mg/1
Organic Nitrogen, mq/1
Oil & Grease, mg/1
METHOD REFERENCE
Electrometric Titration
(pH 8.2)
Electrometric Titration
(pH 4.5) 1
Microdistil lation (at
pH 9.5) followed by
nesslerization or
titration 2
Ment>rane Filter
Ment>rane Filter
Membrane Fi 1 ter
Winkler·(azide mod.)
Titrimetric, iodide-iodate
Dichromate Reflux
Mecuric Nitrate
Iodometric titration
DPD Colorimetric
Colorimetric
Distillation followed by
titration·or pyridine
pyrazolone colorimetric
Distillation followed by
titration.or pyridine
pyrazolone colorimetric
Winkler (Azide wod.)
Distillation followed by
SPADNS
AA-Calculation of Ca+ Mg
Electrometric
1
1
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2
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1
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1
2 & 7
2 & 7
1
1
1
1
t-licrodigestion and 2
distillation followed by
nesslerization and titration
Brutine Sulfate 2
Manual diazotization 2
·.colorimetric
TKN mi nus NH3 2
Freon Extraction-gravimetric l
PAGE
273
278
159
937
928
947
543
14
550
304
318
332
64
· 40
49
553
389
202
460
175
197
215
179 , 159
515
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I PARAMETER & UNITS ~:ETHOD REFERENCE PAGE
24. Organic Carbon, Total , m9/l . Combustion-infrared l 532
25. Phenols, mg/ l Distillation followed 1 582
I by colorimetric (4AAP)
26. Phosphorus, a 11 fonns, mg/1 Persulfate digestion 2 249
manual ascorbic acid
I 27. Specific conductance Wheatstone bridge 1 71
micromhos/cm
28. Sulfate (as so 4) mg/1 Turbidimetric 1 493
29. Sulfide (as S) mg/1 Titrimetric-iodine & 1 505
I methylene blue
photometer
30. Sulfiate (as so 3) mg/1 Ti trimetri c, iodine-l 508
I iodate
31. MBAS, mg/1 Colorimetric, methylene l 600
blue
I 32. Temperature, oc Calibrated glass l 125
. thennometer
33. Turbidity, NTU . Nephelometric l 132
34. Total Sol ids , m<J/1 Gravimetric, 103-105°C l 91
I 35. Total Dissolved Solids, mg/1 Glass fiber filtration, 1 92
180°C
36. Total Suspended Solids, Glass fiber filtration l 94
I mg/1. 103-105°C
37. Total Volatile Solids, mg/1 Gravimetric 550°C 1 95
38. Settleable Solids, mg/1 Volumetric l 95
I METALS
39. A 1 umi num-Tota 1 , mg/1 Di9estion~·ICP 2 & 7 92
I 40. Antimony-Total, mg/1 Digestion-AA 94
41. Arsenic-Total, mg/1 Digestion-AA gaseous 2 & 7 95
hydride
I 42. Barium-Total, mg/1 Digestion-AA -ICP 2 & 7 97
43. Beryllium-Total, mg/1 Di gestion-M -ICP 2 & 7 99
44. Cadmium-Total, mg/1 Digestion-AA 2 & 7 101
45. Ca 1 ci um-'T ota l , mg/1 Digestion-AA -ICP 2 & 7 103
I 46. Chromium VI , mg/1 Extraction-AA 2 & 7 89, 105
Col ori metric 1 & 7 192
47. Chromium-Total, mg/1 Digestion-AA 2 & 7 105
I 48. Cobalt-Total, mg/1 Digestion-AA -ICP 2 & 7 107
49. Copper-Total, mg/1 Digestion-AA -ICP 2 & 7 108
50. Iron-Total, mg/1 Digestion-AA -ICP 2 & 7 110
51. Lead-Total, mg/1 Digestion-AA 2 & 7 112
I 52. Magnesium-Total, mg/1 Digestion-AA -ICP 2 & 7 114
53. Manganese-Total, mg/1 Digestion-AA -ICP 2 & 7 116
54. Mercury-Total, mg/1 flameless-Al\ 2 & 7 118
I 55. Molybednum-Total, mg/1 Digestion-AA 2 & 7 139
56. Nickel-Total, mg/1 Digestion-AA·-ICP 2 & 7 141
57. Potassium-Total, mg/1 Digestion-AA 2 & i 143
I 58. Selenium-Total, mg/1 Digestion-AA 2 & 7 145
59. Silver-Tota 1 , mg/1 Digestion-AA 2 & 7 146
60. Silica-Dissolved, mg/1 0.45 micron filtration 2 & I 274
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colorimetric
-
4
PAIWiETER & UN ITS METHOD REFEREiKE PAGE
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61. Sodium-Total, mg/1 Di fies ti on-AA 2 & 7 147
62. Th a 11 i um-To ta l , mg/1 Digestion-AA 2 & 7 149
63. Tin-Total, m9/l Digestion-AA -ICP 2 & 7 150
64. Titanium-Total, mg/1 Digestion-AA -ICP 2 & 7 151
65. Vanadium-Total, mg/1 Di ges ti on-AA -ICP 2 & 7 155
(NOTES: l. Dissolved r.ietals (all) -.45 micro filtration-AA
Reference No. l -14th Ed. Standard Metals
Reference No. 2 -EPA Methods 1974)
2.
3.
ORGANIC COMPOUNDS
67.
68.
69.
70.
71.
72.
73.
74.
75.
76.
77.
78.
79.
80.
81.
82.
83.
84.
85.
86.
87.
88.
89.
90.
91.
92.
93.
94.
95.
96.
Chlorophenoxy Acid Herbicides -Interim EPA 1978
Acenaphthene, micrograms per 1 iter -GC method ( 610) GC/MS Method {625)
Ancenaphthylene micrograms per liter -GC Method (610) GC/MS Method (625)
Acrolein, micrograms per 1 iter -GC Method (603), GC/MS Method (624)
Acrylonitrite, micrograms per liter -GC Method {603), GC/MS Method (624)
Aldrin, micrograms per liter -GC Method (608), GC/MS Method (625)
Anthracene, micrograms per liter -GC Method (610), GC/MS Method (625)
I
Benzene, micrograms per 1 iter -GC Method (602), GC/MS Method (624) I
Benzidine milligrams per liter, micrograms per liter -GC/MS Method (625)
Benzo(a)anthracene, micrograms per liter -GC (610), GC/MS Method (625)
·senzo(a)pyrene, micrograms per liter -GC (610), GC/MS Method (625)
Benzo(b)fluroanthene, micrograms per liter -GC (610), GC/MS Method (625) I
Benzo{-g,H,l)perylene, micrograms per liter -GC Method (610), GC/MS Method (625)
Benzo(k)fluoranthene, .micrograms per liter -GC Method (610) GC/MS Method (625)
a-BHC, microgram per liter~ GC Method (608) I I,
b-BHC, micrograms per liter -GC Method (608), GC/MS Method (625)
d-BHC, micrograms per 1 iter -GC Method (608), GC/MS Method (625).
<J-BHC, micrograns per liter -GC tlethod (608), GC/MS Method (625)
Bis(2-chloroethyl) ether, micrograms per liter -GC Method (611), GC/MS Method (61
Bis(2-chloroethoxy) Methane, micrograms per liter -GC Method (611),
GC/MS Method (625)
Bis(2-chlorisopropyl) ether, micrograms per liter -GC Method (611),
GC/f.1S Method (625)
Bis(2-ethylhexyl )phth.alate, micrograms per liter -GC Method (606,
GC/MS Method (625)
Bromodi chloromethane, mi crograr.is per liter -GC Method (601),
GC/MS Method (624)
Bromofonn, micrograms per liter -GC Method (601)
Bromomethane, micrograms per 1 iter -GC Method (601), GC/MS Method (624)
4-Bromophenyl plienyl ether, micrograms per liter, ci crograms per liter -
GC Method (611), GC/MS Method (625)
Burylbenzyul phthalate, micrograms per liter -GC Method (606),
GC/MS Method (625)
Carbon tetrachloride, micrograms per liter -GC Method (601),
GC/MS ~iethod (624)
Chlordane, micrograms per liter -GC Method 603, GC/MS Method (625)
4-Chloro-3-methylphenol, microflrams per liter -GC Method (604),
GC/MS Method (625)
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PARAMETER & UNITS METHOD REFERENCE
97. Chlorobenzene, nicrograms per liter -GC Methods (601) (602),
GC/MS Method (624)
5
PAGE
98. 2-Chloroethylvinyl ether, micrograms per liter ~ GC Method (601),
GC/t1S Method ( 624)
99. Chloroform, micrograms per liter -GC Method ( 60 l), GC/MS Method ( 624)
100. Chloromethane, micrograms per liter -GC tlethod (601), GC/MS Method (624)
101. Chloromethane, micrograms per liter -GC Method (612), GC/MS Method (625)
l 02. 1-Ch l oropheno l, microgram per liter -.GC Method (604), GC/MS Method ( 625)
103. 4-Chlorophenylphenyl ether, micrograms per liter -GC Method (611)
GC/MS r,,ethod ( 625)
104. Chrysene, micrograms per liter -GC or HPLC Method (610), GC/t-1S
Method (625)
105. 4,4'-DDD, micrograms per liter -GC Method (608), GC/MS Method (625)
106. 4,4'-DDE, micrograms per liter -GC Method (608), GC/MS Method (626)
107. 4,4'-DDT, micrograms per liter -GC Method (608), GC/MS Method (625)
108. Dibenzo(a,h)anthracene, micrograms per liter -GC or HPIC Method (610),
GC/MS Method (625)
109. Dibromochloramethane, micrograms per liter -GC Method (610,
GC/MS Method (624)
110. 1,2-Dichlorobenzene, micrograms per liter -GC Methods (601) (602)
( 612) , GC/MS Method ( 626) .
111. 1,3-Dichlorobenzene, micrograms per liter -GC Methods (601), (602),
(612), GC/MS Method (625)
112. 2,4-Dichlorobenzene, micrograms per liter -GC Methods (601), (602), (612),
GC/MS Method (625) . . .
113. 3,3'Dichlorobenzidine, micrograms per liter -GC/MS Method (625)
114. Dichlorodifluoromethane, micrograms per liter-GC Method (601)
115. l, 1-Dichloroethane, micrograms per liter -GC Method (601), GC/MS Method (624)
116. 1,2-Dichloroethane, micrograms per liter -GC Method (601), GC/MS Hethod (624)
117. l,2-Dichloromethane, micrograms per liter -GC 1·1ethod (601), GC/MS Method (624)
118. trans-1,2-Dichloromethane, micrograms per liter -GC Method (601),
GC/t1S Method (624) .
119. 2,4-Dichlorophenol, micrograms per liter -GC t:ethod (604), GC/MS Method (625)
120. 1,2-Dichlorpropane, micrograms per liter -GC Method (601), GC/MS Method (624)
121. cis-1,3-Dichloropropene, micrograms per liter -GCC Method (601)29,
GC/MS Method (624)
122. trans-1,3-Dichlorpropane, micrograms per liter -GC Method (601),
GC/MS Method (624)
123. Dieldrin, micrograms per liter -GC Method (608), GC/MS Method (625)
124. Diethyl phthalate, micrograms per liter -GC Method. (606), GC/MS Method (625)
125. 2,4-Dimethylphenol, micrograms per liter -GC Method (604), GC/MS Method (625)
126. Dimethyl phthalamate, micrograms per liter -GC ·Method (606), GC/MS Method (625)
127. Din-butyl phthalate -GC Method (606, GC/MS Method (625)
128. Di-n-octyl phthalate, micrograms per liter -GC t1ethod (606), GC/MS Method (625)
129. 4,6-Dinitro-2-methylphenol, micrograms per liter -GC Method (604),
GC/t-1S Method ( 625)
130. 2,4-Dinitrophenol, micrograms per liter -GC Method (604), GC/MS Method (625)
131. 2,4-Dinitrotoluene, micrograms per liter -GC Method (609), GC/MS Method (625)
132. 2,6-0initrotoluene, micro9rams per liter -GC Method (609), GC/MS Method (625)
6 I
I
PARAMETER & UNIT METHOD REFERENCE PAGE
133.
134.
135.
136.
137.
138.
139.
140.
141.
142.
143.
144.
145.
146.
147.
148.
149.
150.
151.
152.
153.
154.
155.
156.
157,
158.
159.
160.
161.
162.
163.
164.
165.
166.
167.
168.
169.
170.
171.
172.
173.
1,2-Diphenylthydrazine, r;iicrograms per liter -GC/t1S Method (625)
Endosulfan I, micrograms per liter -GC Method (60!3), GC/MS Method (625)
Endosulfan II, micrograms per liter -GC Method (608), GC/MS Method (625)
Endo so lfan sulfate, micrograms per liter -GC Method ( 608), GC/MS Method ( 625)
Endrin, micrograms per liter -GC t1ethod (608), GC/MS Method (625)
Endrin aldehyde, micrograms per liter -GC Method (608), GC/MS Method (625)
Ethyl benzene, micrograms per liter -GC Method (602), GC/MS Method (624) I
Fl uoranthene, micrograms per liter -GC Method ( 610); GC/f.1S Method 625)
Fluorene, micrograms per liter -GC Method (610), GC/NS Method (625)
Heptachlor, micrograms per liter -GC Method (608), GC/MS Method (625) I
Heptachlor epoxide, micrograms per liter -GC Method (608), GC/!-1S Method (625)
Hexachl orobenzene, micrograms per liter -GC Method (612), GC/MS Method (625)
Hexach l orobutadi ene, · micrograms per liter • ,Ge Method ( 612) , GC/MS Method ( 625) 1 Hexachlorocyclopentadiene, micrograms per liter -GC Method (612),
GC/MS Method ( 625) .
Hexachloroethane, micrograms per liter -GC Method (612), GC/MS Method (625)
Indeno (a,3,3-od) pyrene, micrograms per liter -GC Method (610), GC/MS
Method (625)
Isophorone, micrograms per liter -GC Method (609), GC/MS t-1ethod (625)
Methylene chloride, micrograms per lij:er -GC Method (601), GC/MS Method (624)
Naphtha 1 ene, micrograms per liter -GC Method (610), GC/MS Method ( 625)
Nitrobenzene, micrograms per liter -GC Method (609), GC/MS Method (625)
2-Nitrophenol, micrograms per liter -. GC Method (604), GC/MS Methods (625)
4-Nitrophenol, micrograms per liter -GC Method (607), GC/MS Method (625)
N-Nitrosodimethylamine, micro')rams per liter -GC Method (607),
GC/MS Method (625)
N-Ni trosodi propyl amine, mi crograrns per 1 iter -GC Method (607),
GC/MS Method (625)
N-Ni trosodi phenyl amine, micrograms per liter ~ GC Method ( 607),
GC/MS Method (625)
PCB-1016, micrograms per liter -GC Method (608), GC/MS Method (625)
PCB-1221 , micrograms per 1 iter -GC Method ( 608), GC/MS Method ( 625)
PCB-1232, micrograms per liter -GC 11ethod (608), GC/MS Method (625)
PCB-1242, micrograms per liter -GC Method ( 608), GC/MS Method ( 625)
PCB-1248, micrograms per liter -GC Method (608), GC/MS Method (625)
PCB-1254, micrograms per 1 i ter -GC Method ( 608), GC/MS Method ( 625)
PCB-1260, micrograms per liter -GC 1-lethod ( 608), GC/HS Method (625)
Phenanthrene, micrograms per 1 iter -GC Method (608), GC/MS Method (625)
Phenanthrene, micrograms per liter -GC Method (608), GC/MS Method (625)
Phenol, micrograms per liter --GC Method (604), GC/MS Method (625)
Pyrene, micrograms per liter -GC Method (610), GC/MS Method 625)
1,1,2,2-Tetrachloroethane, micrograms per liter -GC Method (601),
GC/MS Method ( 624)
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I Tetrachloroethene, micrograms per liter -GC Method (601 ), GC/MS Method (624)
Toluene, micrograms per liter -GC Method (602), GC/MS Method (624)
Toxaphene, micrograms per liter -GC Method ( 608), GC/11S Method ( 625)
1,2,4-Trichlorobenzene, micrograms per liter -GC Method (612), GC/MS Method (62-
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PARAMETER & UNITS METHOD REFERENCE
174. l, l, 1-Trichloroethane, micrograms per liter -GC 1·1ethod (601),
GC/MS Method (624)
PAGE
175. l, 1,2-Trichloroethane, micrograms per liter -GC tlethod (601),
GC/MS Method (624)
176. Trichloroethene, micrograms per liter -GC Method (601), GC/MS Method (624)
177. Trichlorofluromethane, micrograms per liter -GC Method {601 ),
GC/MS Method (624)
178. 2,4,6-Trichlorophenol, micrograms per liter -GC Method (601),
GC/MS Method (625)
179. Vinyl Chloride, micrograms per liter -GC Method (601), GC/1-1S Method (624)
180. Orthophosphate (as P), r:iilligrams per liter -Manual or automated
ascorbic acid reduction
I I.
8
QUALITY CONTROL FOR ANALYTICAL PERFORMANCE
A. Standard Curves
B.
C.
A new standard curve must be established with each new
batch of reagents, using at least seven concentration levels
(Reagent blank and six standards). New curves must be
labeled, numbered, dated, and initialed by analyst.
Subsequent curves must be verified by use of at least a
Reagent blank and one standard at or near the maximum contami-
nant level (MCL). Daily checks must be within +10 percent
of the original curve.
Reagent Standardization
Unless otherwise specified in the procedure, all reagent
titrants must be standardized monthly or as frequency of
analysis demands. Reagent must be labeled as to date,
nonnality, and initial of analyst.
Gravimetric Analysis
All weighing vessels (beakers, flasks, dishes and
crucibles) are to be weighed to a consistant weight before
and after use to insure accuracy. This can be accomplished
by placing the vessel in an oven at l03-l05°C to drive off the
moisture and then desiccating for a minimum of one hour before
obtaining a weight. Repeat the drying cycle until weight
loss is less than 0.5 mg. Exception to the drying cycle is oil
and gr-ease for which this might result in loss of volatile
organics.
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D.
9
Quality Control Checks -For each analytical run
At least one reagent blank and one standard at or near
the MCL must be run with each set of samples. Checks must
agree within UCL and LCL (See charts).
At least one duplicate sample must be run every
10 samples or with each set of samples. Checks must be
within the UCL of the control charts. This detennines the
precision of the test.
At least one spiked sample must be run every 10 samples or
with each set of samples. Checks must agree within UCL and
LCL of the control charts. This detennines the accuracy of
the test.
E.
10
Quality Control Charts -For accuracy
Accuracy of testing must be evaluated indirectly through
the recovery of Standards and Spikes.
l.
2.
% Recovery: Standards
Spikes
Average% Recovery: n
P = EPi
i=l -n
P = 100 observed
known
P = 100 observed-background
spike
3. Standard Deviation for% Recovery:
Sp=
n-
4. Upper Control Limit:
5. Lower Control Limit:
UCL = P" + 3 Sp.
LCL = P -3. Sp.
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CONTROL CHART
140
______________________ U,CL
120
t' ~,oo - - - - - - - - - - - - - - - - - - -~ - - - - - - -l"
0 u Q)
"" .._
80
LCL ------------------------
60
0 5 10 15 20 25
SAMPLE NUMBER
In applying the control chart, either of the following two
conditions would indicate an out-of-control situation:
1, Any point beyond the control limits
2. Seven successive points on the same side of the value P of the
central line,
If an out-of-control situation exist, data must be rejected.
The problem must be identified and resolved.
12
QUALITY CONTROL CHARTS -For precision
Precision of testing must be evaluated through the analysis
of duplicate samples.
R = The absolute value of the difference between each set
of duplicate samples.
Average Range: R = Sum of R values divided by the number
of duplicate sets.
if = ER
n
l. Ueeer Control Limit: UCL -3. 27lf
2. Upper Warning Limit: UWL = 2. 511<
UWL corresponds to 95% confidence level.
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0.3
0.2
0. 1
0
COtlTROL CHART
_______________________ U,CL
_______________________ U.WL
--- - -- - --- ---- - -- -- ---- - ----[
ORDER OF RESULTS
An out-of-control situation exist if any point is beyond
the control limits, at which time the problem must be resolved and
corrected.
It may be necessary to construct separate control charts for
various ranges of concentration within the same parameter.
1 3
ACCURACY CONTROL DATA
STMIDARDS
PARAMETER: ________ _
POINT KNOWN OBTAINED DIFFERENCE Pi Pi 2
. .
.
14
AtlAL YST DATE COMMENTS
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ACCURACY CONTROL DATA
SPIKES
PARAMETER: _________ _
POIIH KNOWN OBTAINED BACKGROUND Pi Pi 2
.
.
15
ANALYST DATE COMMENTS
PRECISION CONTROL DA TA
DUPLICATES
PARAMETER: _______ _
POINT 01 02 R Ir ANALYST
.
.,
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DATE
, ' ..
..
. .
•, . -
16
COMMENTS
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l 7
F. lnterlaboratory Quality Control
During the year, samples are received from various Federal and State
Agencies for laboratory quality control and laboratory certification
purposes. As of this date, (February, 1983), samples are received
as follows:
l. U.S.E.P.A., E.M.S.L., (voluntary) .for analyses of trace
metals, minerals, nutrients, demand, organics and other
parameters as are available from E.P.A.
2. National Institute of Health, American Industrial Hygiene
Association, Performance Audit Testin9 {PAT) Program, quarterly
samples for metals, organics and asbestos.
3. U.S.E.P.A., N.P.D.E.S., Industrial Client Laboratory Audit/
Certification, parameters are specific for the industrial client
and NPDES permit in question.
4. U.S.E .. P.A., Water Quality Survey Perfomance Standards for
Interim Primary Standards and Trihalomethanes.
5. U.S.E.P.A. Source Performance Audit Program-Method 6 (SOz);
Method 7 (NDx); Method 5 (Particulates)
6. South Carolina Department of Health and Environmental Control,
Laboratory Certification Performance, audit/samples, on-site audit
of personnel and equipment for analyses of unknowns
7. North.Carolina Department of Natural Resources and Community
Development, Laboratory Certification Performance, audit/samples,
on-site audit of personnel and equipment for analyses of unknowns
8. State of Tennessee, Department of Health, Laboratory Audit
and Certification-reciprocal with South Carolina
G.
18
Microbiology Quality Control Checks
In total colifonn tests using the membrane filter (MF}
technique, at least five sheen or borderline sheen colonies
when present must be verified. The verification procedures
should be conducted by transferring colonies into lauryl tryptose
broth (TB) tubes and brilliant green lactose bile (BGLB) tubes.
Negative LTB tubes must be reincubated a second day and
confinned if gas is produced.
A start and finish MF control test (rinse water, medium,
and supplies) must be conducted for each filtration series.
If sterile control indicates contamination, all data on affected
samples must be rejected and retested immediately.
At least once per month duplicate analyses must be run
on a known positive sample. Duplicates are to be run as a
split sample (50 ml. ea.) by two analysts.
At least once per month, each analyst involved in colifonn
analysis must count the sheen colonies from a positive sample.
Colonies must be verified and compared to the analyst's counts.
A known positive sample must be tested with each
filtration series.
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DAVIS & FLOYD INC
ENVIRONMENTAL SERVICES DIVISION
GREENWOOD SC
STERLIZATION OF
MEDIA, SUPPLIES, AND EQUIPMENT
BATCH NUMBER. _________ _ ANALYST ____________ _
DATE: ____________ _
AUTOCLAVE THERMOMETER READING _______ _
TIMER CHECK (HIN) _____________ _
I GIRGLE THE ITEMS
PREPARED
INDICATE NUMBER. I STERILIZATION ! LENGTH OF !
SIZE AND/OR VOL. I CONDITIONS I CYCLE I
+----------------------------------------------------------------------+
I SAMPLE BOTTLES I I +----------------------------------------------------------------------+
I FILTRATION ASSEMBLY I I I I +---------------------------------------------------------------------+
. !MISC GLASS. & FIPETS I I I i +-------------~----------------------------------------------------+
I RINSE/DILUT. WATER I I I I +----------------------------------------------------------------------+
MEDIA PREPARATION
TYPE OF MEDIA I BRAND-,---_____ STERILIZATION FINAL pH
I LOT tlO.______ CONDITIONS I WGT /VOL _____ _
I # TUBES ______ ! I
+----------------------------------------------------------------------+ I ! _______ I I
I _______ !
I _______ J
I i ________ ! I
+----------------------------------------------------------------------+
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+----------------------------------------------------------------------+
DAVIS &
ENVIRONMENTAL
FLOYD INC.
SERVICES DIVISION
GREENWOOD SC.
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NO SAMPLE WILL BE ACCEPTED ON FRIDAY UNLESS PRIOR ARRANGEMENTS ARE MADE I
TO GUARANTEE THAT RESULTS WILL REACH SCDEHEC ON TIME.SAMPLES
MUST BE RECEIVED BY THE 25th OF EACH MONTH.
BACTERIOLOGIC;i.l 2J1AI.YSIS FORM
Ha.me of V:!.ter Syst-em
!:2.ck .=..nd
, .. ,ount.y
Samele ID :;nalT;is Date/Time Analyst·; Coliform col/lOOml
Non-Coliform col/100ml
********************************************************************************
DIREGTIONS FOR S.:..11PLING DRINKING l'".'\TER FOR BACTERIOLOGICAL TEST
'!'his s-:mc,le bottle has been sterilized and contains a declhlorinating agent
DO NOT ooen the bottle i..:.n. til the mower. t it i·; t.o be filled. '-later oumos O!."
faucets -;hould be treed irom si:.anding ,.,ater by oumoing or ailoi.,ing vater to fl,:,i..•
£or about five minutes.) The faucet. sho1Jld be flamed, using a propane torch ,:,r a.
Y3.d ,:,£ cotton s.~tur-3.ted 1,•ith ::i.lcohol ~.nd the ~ater r1.mning until the f.3.ucet 2-=
,::::1Ja!. ~eW0'/2 cao from. ::.ot.tle, fill :,.:::;ttle to neck. :-eplace cac c:1i.cklr· ..,,.i.thc:..:t
i:,::iucOing the inside ·=,ur!::i.ce oi ,:..3.0 ,::01' bor~tle neck. Reolace botr~le in •=ontainer.
It i·; es;,ential that a.li information be recorded on the report ·⇒heet i...:hich
.;,:ccmoanies the sa.mpl~ bottle. THE ~:EFORT SHEET MUST HAVE THE c,.:..rs ,Zi,tfD TIME c,
~.::.JfPLING, RETURN .!..DO RESS, .u.N[r THE lt:iJ~lE . .;DD RESS ( OR LOC.9. TION) AND PH1)NE NUMBER
TOE '·:"E:LL 1)"-,~f~R IH C•RDEF-li) C:-E ,;ccC:Fi'~L• FOR .;H.;LY3I3. iHE s.:.JiFLC: 1-:;_;37 BE C•EL:i:'-,." :=.t:U
11=1 T:-lE [,AVIS .~t Fl(i.:lD r;;c. L.~.EC:~;_;:._l(iR'i ;.,'ITHIH 30 HVURS. After thi-=: time c,eric,j
b~c~eriological results sr2 unreliable ~nd ~ill not be scceoted by state 3nd
~~d~r;l agenci~;.
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DAVIS & PLOYD INC
ENVIRONMENTAL SERVICES DIVISION
GREENWOOD SC
EENC:!-! SHEET
TOTAL COLIFORM ANALYSIS
r-'i.EMBRANE FILTER
REF. MID. _________________ ANALYST: _________ _
DATE BEGUN: _____ TIME: ___ _ MEDIA LOT NO.: _________ _
DATE COMP.: _____ TIME: ___ _ EXPIRATION DATE: ________ _
********************************* ..... **** ..... *******************************
ISAMP. ID
I
SFV DIL FAC
SFV SAMPLE FILTRATION VOLUME
COLONY COUNT
COLI ! NON-COLI
COL/100 ml
COLI ! NON-COLI
DILUTION FACTOR= DECIMAL EQUIVALENT ( EX. 1/10 = 0.10 )
CALCULATION= COL/100mls = COLONY COUNT* 100
,-,,-,J...o..A't:"UTC· • '._,;,__;;.·i..i.iLH.i..J.
SFV * DILUTION fAG
=n
DAVIS~ FLOYD IN::
ENVIRONMENTAL SERVICES DIVISION
D r:"t..t,-•u C"'U!."::;""'!"' ......... ,i-_, ••• .=.a. • ..:...:..;.
TOTAL COLIFORM ANALYSIS
REF. 11.1.!...' ·------------------ANALYST: _________ _
DATE BEGUN: ____ _ ~IXE: ___ _
I SAMP. ID COLONY DESCRIPTION
INITIAL COUNT: ----
DATE COMP. : ____ _ TIME: ----
LAURLY TRYPTOSE
48hr
j.
BRILLIANT GREEN
24hr I 48hr
ADJUSTED COUNT: ___ _
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DAVIS & FLOYD INC
ENVIRONMENTAL SERVICES DIVISION
GREENwOOD SC
BENCH SHEET
FECAL COLIFORM ANALYSIS
MEMBRANE FILTER
REF. MID. __________________ ANALYST: _________ _
DATE BEGUN: _____ TIME: ___ _ MEDIA LOT NO. : -----------
DATE COMP. : ____ _ TIME: ___ _ EXPIRATION DATE:__,_ _______ _
************************************************************************
!SAMP. ID SFV OIL FAG COLONY COUNT ADJUSTED! COL/100MLI
I TYPICAL I ATYPICAL COUNT I I
SFV = SAMPLE FILTRATION VOLUME
DILUTION FACTOR = DECII'-'~ EQUIVALENT
I ' I
1/10 =
CALCULATION= COL/tOOmls = COLONY COUNT ... too
SFV * DILUTION FAC
COMMENTS:
REF. MTD.
DAVIS & FLOYD INC
ENVIRONMENTAL SERVICES DIVISIO~
BENCH SHEET
FECAL COLIFORM ANALYSIS
VERIFICATION
ANALYST: ----------------------------
BEGUN: TIME: ---------
SAMP. ID COLONY DESCRIPTION
T\.lT'T'T:,.. T .1.n-1. ..i. .i.tt.u GOUNT:
-rvnT,-•AT .1. 1 ~ .1.•-_,r-• .:....
]i.TYPICJ:..L
----
DATE COMP.: _____ TIME: ___ _
. i
' '
LAURYL TRYPTOSE
24 HR I 48 HR
E.C.BROTH
24 HR
AD.JUSTED COUNT: ----
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DAVIS & FLOYD INC
ENVIRONMENTAL SERVICES DIVISION
GREENWOOD SC
COMMERCIALLY PREPARED
MEDIA
***********************************************************************
I TYPE & BRAND I QUANT/SIZE I LOT NO. (DATE EXP IDATE REC !DATE USED I +---------------------------------------------------------------------+
I i I I I I I +---------------------------------------------------------------------+
i I I I I i +---------------------------------------------------------------------+
I I I I +---------------------------------------------------------------------+
! +---------------------------------------------------------------------+
! I I I l +---------------------------------------------------------------------+
l I I I I ! I +---------------------------------------------------------------------+
I I I I ! +---------------------------------------------------------------------+
! I . I . . I . . I i I +---------------------------------------------------------------------+
I I I i +---------------------------------------------------------------------+
I I I I I I +---------------------------------------------------------------------+
! I I I ! I I +---------------------------------------------------------------------+
I I I I I i I +---------------------------------------------------------------------+
I I I I i I i +---------------------------------------------------------------------+
i I i i i I i +---------------------------------------------------------------------+
I I I +---------------------------------------------------------------------+
I I I +---------------------------------------------------------------------+
! I I I ,
+---------------------------------------------------------------------+
I i I i I +---------------------------------------------------------------------+
I I I I I ; ! +---------------------------------------------------------------------+
! I i I ,
+---------------------------------------------------------------------+
H.
19. 1
Quality Control for Organic Analysis
The following quality control sections are surrmaries of
the QC requirements specified in the EPA Federal Register,
October 26, 1984. Any specific details of these procedures
can be found in the publication.
1. Quality Control for Start-Up or Method Modifications
A check sample study must be perfonned when a laboratory
is establishing new parameters or making any method changes.
Method modifications that are expressly pennitted (including
the use of non-specified columns or detectors) are acceptable
for organic analysis as long as the method detection limit
(MDL) is at or below the acceptable MDL given for each para-
meter in the Federal Register. The quality control must also
be demonstrated to be acceptable according to the procedure
described in this section.
A check sample contains each parameter of interest at a
specific concentration. They can be obtained from U.S.EPA,
Environmental Monitoring and Support Laboratory, Cincinnati,
Ohio or an external source or from independently prepared
stock samples.
A laboratory must analyze four aliquots of the diluted QC
check sample and use the data to calculate the average recovery
(X) in ug/L, and the standard deviation of the recovery (s) in
ug/L. Compare (X) and (s) to the corresponding acceptance
criteria (found in the appropriate tables in the Federal
Register). The perfonnance must fall within the range or the
system perfonnance is unacceptable for the parameter and a QC
check must be repeated.
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19.2
This quality control data must be made available to the
laboratory certification personnel at an on-site inspection or
submitted for review to that office for each method.
2. Daily Quality Control For Organic Analysis
Section 1: Each day a reagent water blank must be
analyzed. A laboratory must spike and analyze a minimum of
10% of all samples. For compliance monitoring, the concen-
tration of a specific parameter in the spike should be at that
limit of l to 5 times higher than the background concentration.
Compare the percent recovery (P) for each parameter with the
corresponding QC acceptance criteria. If any (P) falls
outside the designated range for recovery, a check sample for
that parameter must be analyzed as described in Section 2.
After the analysis of 5 spiked wastewater samples, a
laboratory must calculate the average percent recovery (P) and
the standard deviation of the percent recovery (s). Express
the accuracy (P -2s) to P + 2s). Update the accuracy assess-
ment for each parameter on a regular basis (after each 5 to 10
new accuracy measurements).
Additional precision quality control charts are required.
This data can be generated from duplicate spiked analyses.
Section 2: If any parameter fails the acceptance criteria
for recovery for 10% spikes, a QC check standard containing
each parameter that failed must be prepared and analyzed.
Analyze the QC check standard to determine the concentration
measured (A) of each parameter. Calculate each percent
recovery (P) as lOO(A/T)%, where (T) is the true value of the
19.3
standard concentration. Compare the percent recovery (P) with
the QC acceptance criteria. If the recovery of any such
parameter falls outside the designated range, the laboratory
performance for that parameter is unacceptable.
After an instrument has been down for any reason; eg.
repaired or new detectors, columns, or electronics, the
instrument should meet the manufacturer's start-up specifica-
tions and a quality control spike must be analyzed successfully
before any samples can be analyzed. Records indicating this
must be available to the laboratory certification per·sonnel.
A working standard notebook is required for all analytical
standards. This notebook should contain a list of al.l standard
compounds, date of preparation, initials of preparer, initial
volume or weight of stock, purity of stock, dilution volumes,
solvent used to prepare and final concentration. Standards
should be stored only for the recommended period of time and
according to individual standard requirements as discussed in
the U.S.EPA Federal Register, October 26, 1984. Generally,
calibration standards are stored, refrigerated in small
containers with little or no head space for no more than one
year.
Field duplicates and blanks, confinnatory techniques, and
the use of standard reference material when available are all
reco0111ended additional quality control parameters.
3. Quality Control for GC-MS Organic Analysis
All of the above QC procedures are required for GC-MS
analysis with the following additions:
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4.
19.4
a) The laboratory must spike and analyze 5% of all
samples.
b) QC check standard analysis frequency is 5% of all
samples.
c) The laboratory must spike all samples with a surrogate
standard solution.
Laboratory Records for Organic Samples
In addition to these requirements all chromatograms and
data system print-outs should contain the following information.
Sample or standard name, amount injected, concentration if
standard, dilution volume of sample, date, analyst's initials,
column ID, attenuation setting, and chart speed. These
records must be maintained and stored for a minimum of five
years for Clean Water Act Monitoring·and ten years for Safe
Drinking Water Act Monitoring.
20
Ill. CHAIN OF CUSTODY
The objective of this section is to create a written record
on samples from collection to analysis to report and disposal of sample.
A. Sample Collection, Handling and Identification
B.
It is the responsibility of the field crew chief to
insure that sampling is representative of the total
environment under investigation. Samples must be collected
and preserved in accordance with Table l. Samples must be
properly identified with sample numbe~ and site location, including
date, time, initial of collector, and preservative. If samples
are to be transported to the laboratory other than by field
crew (bus, mail, air, etc.), field data sheets should accompany
samples. The field crew chief must keep a written log of field
activities and pertinent sampling data.
Laboratory Custody
The laboratory supervisor shall be designated data manager
and an alternate designated to act as data manager in his or
her absence. All incoming samples must be logged in by data
manager and pennanent records kept on file. The data manager will
then post analysis ass_ignment sheets. The data manager shall
ensure that samples are properly stored and maintained through
analysis and until results are reviewed and approved. All
calculations and results must be recorded in laboratory
notebooks by the analyst at the time of analysis.
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Client:
Location:
Contact:
Job No.:
Comments:
Lab. Collector's No.
No. & Descri otion
Relinquished by:
Affiliation:
Relinquished By:
Affiliation:
Relinquished By:
Affiliation:
Relinquished By:
Affiliation:
Dispatched By:
Method of Shipment:
21
CHAIN OF CUSTODY
Sample Site:
Collector:
Date: Page_ Of
Affiliation of Collector:
Time Sample Container Analysis
Collected Type Tvoe Preservative Reaui red
Rec'd By: Date/Time
Affiliation: I
Rec'd By: Date/Time
Affiliation: I
Rec'd By: Date/Time
Affiliation: I
Rec'd By: Date/ I 1me
Affiliation: I
Date/Time Rec'd By Lab. Date/Time
I I
DAVIS & FLOYD, INC.
1::· I. .. C) ...... ,..,. :()
ENVIRONMENTAL '.3ERUICES
:i: i"-1 c:
DI 1v' IS I UN
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JOB LAB SP ------------------LAB BD □K DATE ----~~~~:: ___________ :~::~: ___ :~::~: ___ :::~---:~:~ ___ :: ___ :~:::~:~:---~~: ___ I I I I I I I I I I -I I I I I I I l ---------------------------------------------------------------------------1 I I I I I I I -----------------------------------------------------------------------------
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--------------- -
· MICROBIOLOGY SN1PLE IIANAGEIIENT
RECEIVEO .!'_NALYS IS B[GUH ANALYSIS C011PLETE
SAMPLE NO. OESCRJPTION Di\TE T !ME BY TEST /METl!OO ,/fA'fE -Ul'tE -w DATE TiflE BY RESULTS
.
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H[PO !.!__ .. OATE UY
---
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LADORA TOR y SAMPLE MAI/AG [ME/IT
""'PL £7 ITT jffJTTcil i' /Oil /i:ACY>t> AfiALYS£S APPIW'IEO...-i:~ i·5ffr--~:.::r-rruLII---,iril l (l(o·r:-
SAMPLE 110. RECEIVED PROJECT NO. COO£ 110. , DATE, TIM£, £TC. REPORT TO BEGUN COll?LEIE BY OUT \,;:Pl[ our 000>:, P,\G(
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I 25
I
i I TABLE I
I RECOMMENDATION FOR SAMPLING AND PRESERVATION
OF SAMPLES ACCORDING TO MEASUREMENT'>
I Vol.
I Req.· Holding
Measurement (ml) Container 2 Preservative3•4 Time5
I 100 Ph~ical Pro~nies
I Color 50 P,G Cool, 4'C 48 Hrs.
Conductance 100 P,G Cool, 4"C 28 Days
I Hardness 100 P,G HNO3 to pH <2 6 Mos.
I Odor 200 G only Cool, 4•c 24 Hrs.
pH 25 P,G None Req. Analyze C Immediately I Residue
Filterable 100 P,G Cool, 4'C 7 Days
I Non•
Filterable 100 P,G Cool, 4'C 7 Days
I Total 100 P,G Cool, 4'C 7 Days
Volatile 100 P,G Coo~ 4•c 7 Days
I Settlcable Matter 1000 P,G Cool. 4°C 48 Hrs.
Temperature 1000 P,G None Rcq. Analyze
Immediately I · Turbidity 100 P,G Cool, 4'C 48 Hrs.
200 Metals
I Dissolved ·200 P,G Filter on site 6 Mos.
HNO3 to pH <2
I Suspended 200 Filter on site 6 Mos_1a1
Total 100 P,G HN03 to pH <2 6 Mos.
I e·
XVI
I
26 I
TABLE 1 (CONT) I
C I Vol.
Req. Holding
Measurement . (ml) C . 2 on tamer · 3 4 Preservauve · Time5 I
Chromium+e 200 P,G Cool. 4°C 24 Hrs.
Mercury I Dissolved 100 P,G filter 28 Days
Total 100 P,G
HNO3 to pH<2
HNO, to pH<2 28 Days I
300 lnorganics, Non-Metallics I Acidity 100 P,G Cool,4°C 14 Days
Alkalinity 100 P,G Cool, 4'C 14 Days I
Bromide 100 P,G NoneReq. 28 Days
Chloride 50 P,G None Rcq. 28Days I
Chlorine 200 P,G None Req. Analyze
Immediately I C Cyanides 500 P,G Cool, 4'C 14 Days 7
NaOH to pH >12
0.6g a_scorbic acid' I Fluoride 300 P,G . None Rcq. 28 Days
Iodide 100 P,G Cool, 4'C 24 Hrs. I Nitrogen
Ammonia 400 P,G eoo1,4•c 28 Days I H,so, to pH< 2
Kjeldahl, Total 500 P,G Coo~ 4•c 28 Days
H,so, to pH< 2 I Nitrate pl':"' Nitrite 100 P,G Coo~ 4•c 28 Days
H,so, ·10 pH< 2 I Nitrate8 100 P,G Coo~ 4•c 48 Hrs.
Nitrite 50 P,G Cool, 4"C 48 Hrs. I
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I 27
I TABLE 1 (CONT)
I
(
\_
Vol.
Req. Holding
I Measurement (ml) Container 2 · 3 4 T. s Preservall ve · 11ne
I Dissolved Oxygen
Probe 300 G ho11le and top None Req. Analyze
[mmediately
Winkler 300 G bottle and top Fix on site 8 Hours
I and store
Phosphorus in dark
Onho-
phosphate, 50 P,G Filter on site 48 Hrs.
I Dissolved Cool, 4"C
Hydrolyzable 50 P,G Cool, 4"C 28 Days
I H2SO, to pH< 2
Total 50 P,G Cool, 4"C 28 Days
H2SO, to pH< 2
I Total, 50 P,G · Filter on site 24 Hrs.
Dissolved Cool, 4•c
H,so, to pH< 2
I Silica 50 P only Cool, 4"C 28 Days C
Sulfate 50 P,G c::oo,. 4•c 28 Days I Sulfide 500 P,G Cool. 4°C 7 Days
acid 2 ml zinc
I acetate plus NaOH
to pH >9
Sulfite so P,G None Req. Analyze
I I_mmediately
400 Organics
BOD 1000 P,G Cool, 4"C 48 Hrs.
I COD 50 P,G Cool, 4°C 28 Days
H,SO, to pH< 2
I Oil & Grease 1000 G only Cool, 4"C 28 Days
H,so, to pH< 2
Organic carbon 25 P,G Cool, 4'C 28 Days
I H,SO, or HCI to pH< 2
Phenolics 500 G only Cool, 4°C 28 Days
I H,.SO, to pH <2
I XVlll ' ~ I
(
C
C
Vol.
. Req.
Measurement (ml)
MBAS 250
NTA 50
. TABLE 1 (CONT)
Container 2 · 3 4 Preservauve ·
P,G Cool, 4•c
P,G Cool, 4"C
28
Holding
T . 5 1me
·18 Hrs.
24 Hrs.
I. More specific instructions for preservation and sampling are found with each procedure as
detailed in this manual. A general discussion on sampling water and industrial wastewater may
be found in ASTM, Part 31, p. 72-82 (1976) Method D-3370.
2. Plastic (P) or Glass (G). For metals, polyethylene with a polypropylene cap (no liner) is
preferred.
3. Sample preservation should be performed immediately upon sample collection. For
composite samples each aliquot should be preserved at the time of collection. When use of
an automated sampler makes it impossible to preserve each aliquot, then samples may be
preserved by maintaining at 4°C until compositing and sample spliuing is completed.
4. When any sample is 10 be shipped by common carrier or sent through the United States
Mails, it must comply with the Department of Transportation Hazardous Materials
Regulations (49 CFR Part 172). The person offering such material for transportation is
responsible _for ensuring such compliance. For the preservation requirements of Table I,
the OHice of ·Hazardous Materials, Materials Transportation Bureau, Department of
Transportation has determined that the Hazardous Materials Regulations do not apply to
the following materials: Hydrochloric acid (HCI) in water solutions at concentrations of
· 0.04% by weight or less (pH about 1.96 or greater); Nitric acid (HNO3) in water solutions at
concentrations of0.15% by weight or less (pH about 1.62 or greater); S'ulfuric acid ( H,SO,)
in water solutions at concentrations of 0.35% by weight or less (pH about I. 15 or greater);
Sodium hydroxide (NaOH) in water solutions at concentrations of 0.080% by weight or
less (pH about 12.30 or less).
5. Samples should be analyzed as soon as possible after collection. The times listed are the
maximum times that samples may be held before analysis and still con'sidered valid.
Samples may be held for longer periods only if the permiuee, or monitoring laboratory,
has data on file 10 show that the specific types of sample under study are stable for the
longer time, and has received a variance from the Regional Administrator. Some samples
may not be stable for the maximum time period given in the table. A permiuee, or
monitoring laboratory, is obligated to hold the sample for a shorter time if knowledge
exists to show this is necessary 10 maintain sample stability.
6, Should only be used in the presence of residual chl<,irine.
XIX
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28.1
7. i\laximum holding time is21 hours when sulfide is present. Optionally, all samples may be tested with lead acetate paper bdore the pH adj us, ment in order 10 determine if sulfide is present. If suliic.Je is present. it GIil be removed by the addition of cadmium nitrate powder until a negative spot cest is obtained. The sample is filtered and chen NaOH is added co pH 12. .
8. Samples should be filcered immediacely on-sice before adding preservative for dissolved mecals.
9. For samples from non-chlorinated drinking water supplies cone. H:,SO, should be added to lower sample pH to less chan 2. The sample should be analyzed before 14 days.
x.x
(
C
e
TABLE l
Vol.
Req.
Container(Z) Measurement ~
TOX 250 ml Glass, amber
Teflon
Volatile 2x40 ml Glass, Teflon
Organics Septa
Semi-Volatile l 000 ml Glass, Teflon
Organics
Pesticides, PCB's
Herbicides
Radiological ½ Gal. Plastic
(Continued)
Preservative
Cool 4 Degrees C
Cool 4 Degrees C
Cool 4 Degrees C
HN03 to pH <2
28.2
H~ldi~~ Time
14 Days
7 Days
Til Extraction
40 Days
After Extraction
6 Months
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IV. LABORATORY PURE WATER
On a monthly basis, laboratory pure water must be analyzed
for conductance, pH, chlorine residual, and standard plate count.
29
If it does not meet the requirements listed below, corrective action
must be taken and the water retested.
TEST
Conductivity
pH
Free Chlorine Residual
Standard Plate Count
Trace metals
A single metal
Total metals
REQUIREMENTS
Less than 5.0 micromhos/cm @25°C or
greater than 0.2 megohm as resistivity
5.5 -7.5
0.0
Less than 10,000/ml
Not greater than 0.05 mg/1
Equal to or less than 1.0 mg/1
The above monthly tests are performed during the first week
of each month. All data is to be recorded in the appropriate book.
On an annual basis, laboratory pure water is to be tested
for bactericidal properties. Use either "Standard Methods,"
or the procedure outlined in the South Carolina "State Environmental
Laboratory Certification Manual."
On the first day of each week, the glass still is to be
disassembled and cleaned with chromic acid solution. It must be rinsed
thoroughly with water to remove any traces of chromium and the first
liter of distilled water produced must be discarded.
Cartridges in the Millipore Mill-Q water systems must be changed
when the Meg-a-meter fails to indicate the desired resistivity within
5 minutes.
All glass carboys used in storing distilled water are to be
cleaned before each use with chromic acid solution. They must be
thoroughly rinsed with water to remove any traces of chromium,
followed by a final rinse with distilled water.
All storage vessels containing distilled water are to be
30
properly sealed to minimize contamination. If any visible growth or slime
develops in storage vessels due to prolonged storage or contamination,
the water must be discarded.
11
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Jate
Analyst
Ini t.
FORM
LABORATORY QUALITY CONTROL
PURE WATER ANALYSIS
pH Conductivity Res.
Uni ts Mi cromhos/CM
.'1:5. 5-7. 5 < 5.o @ 2s0 c
31
Chlorine Std. Plate
mg/1 Count
0 <10.000/ml Remarks
..
DAVIS & FLOYD INC
ENVIRONMENTAL SERVICES DIVISION
GREENWOOD SC
BENCH SHEET
LABORATORY PURE WATER
STANDARD PLATE COUNT
REF. HTD . _________________ ANALYST: ________ _
DATE BEGUN: _____ TIME: ___ _ MEDIA LOT NO.: _________ _
DATE COMP.: _____ TIME: ___ _ PREPARATION DATE: _______ _
****************** ..... ******************************-11-4-..... ******************
I DILUTION I COLONY COUNT
I I PLATE #1
COLONY COUNT
PLATE #2
RESULTS COL./ML
+----------------------------------------------------------------------+
! I I I I
I CONTROL I I I I +-------------------· --------------------------------------------------+
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I 1 I I I I +----------------------------------------------------------------------+
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I 1 0-1 I I . I I
+-----------------------------------------------------------------+
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I 10-2 I I I ! +----------------------------------------------------------------------+
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I 10-3 I I I I +----------------------------------------------------------------------+
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I 10-4 I I I I +----------------------------------------------------------------------+
!
10-5 I +----------------------------------------------------------------------+
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V. LABORATORY EQUIPMENT (Major)
A. Analytical Balance -Sartorius Model 2402 (2 ea.)
200 gram capacity 0. l mg sensitivity
The analytical balance must be checked for proper
calibration with a set of Class S weight monthly by the
laboratory supervisor.
The balance must be kept clean at all times.
be checked for level and tare prior to each use.
edges must be fully arrested when not in use.
It must
The knife
B. pH Meter -Beckman SS-3, Beckman 72, Beckman Chem-Mate.
Accuracy, _!9.05 units. Scale readability, :::_0. l units.
pH meters must be cleaned and calibrated each
use period with pH 7.0 buffer or other appropriate buffer.
Buffer aliquot may be used only once.
32
The temperature compensator must be set to match sample
temperature. The electrodes must be rinsed thoroughly with
distilled water after immersion into samples. When not in
use, electrodes must be immersed in distilled water.
Reference and combination electrodes must be checked
regularly for proper filling solution.
FORM
ANALYTICAL BALANCE CALIBRATION
Balance Calibration
Date By No. Wt.
33
Co111Tients
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METER NO.: ______ _
)ate Time
'
.
FORM
pH Calibration
pH CALI BRAT ION
Analvst
'
34
pH Buffer Corrrnents
-
-
-·
--·
---
-··
-
-··
C. Spectrophotometers. B & L Spectronic 21 MV wavelength
range 340-1000 nm
Spectral slitwidth 10 nm
B & L Spectronic 20
wavelength range 340 to 950 nm
Spectral slitwidth 20 nm, constant
Beckman DB-G
Wavelength range 190 to 700 mn
Spectral slit -Programmed or adjustable 0.01-2.0 mm
Sample cells must be handled with extreme care.
35
All cells must be kept scrupulously clean, free of scratches,
fingerprints, smudes, and evapoarted film residues. (See
Chapter VI for cleaning.)
Wavelength alignment must be checked monthly with
calibration standards.
D. Atomic Absorption -Perkin-Elmer Model 360
Hollow cathode lamp source
Flameless mercury analyzer
Gaseous hydride generator
Refer to owner's manual for proper operation.
E. Organic Carbon Analyzer -Beckman Model 915 with 215A
IR analyzer.
Refer to owner's manual for proper operation.
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)ate Bv
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FORM
SPECTROPHOTOMETER CALI BRA TIO!,
Instrument Calibration
.
36
Comments
.
.
F. Gas Chromatograph -Beckman GC-72.5 with dual flame
ionization
Varian Model 3700 with FIO, ECO, TSO
COS 111-C Data System
10 in recorder
Refer to owner's manuals for proper operation.
G. Conductivity Meter -HACH Model 16300 ranges 0-2,
0-20, 0-200, 0-2000, 0-20,000 micromhos/cm
Refer to owner's manual for operation.
H. Turbidimeter -HACH 2100A ranges 0-1, 0-10, 0-100,
0-1000 NTU
Refer to owner's manual for operation.
I. Drying Oven -Thelco Model 16 -gravity convection.
Thermometer must be immersed in a beaker of sand and
calibrated against NBS thermometer temperature must be
recorded daily.
J. Refrigerator -Precision Scientific Model 805
Reference inside must be calibrated against NBC
thermometer. It must be immersed in a beaker of water.
Temperature must be recorded daily (4°C).
K. Incubator -B005 -Precision Scientific Model B005
Reference thermometer inside must be calibrated
against NBS thermometer. It must be immersed in a beaker
of water. Temperature must be recorded daily. (20°C :!:{).5)
Total coli form -The l co Model 20
37 I
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Thennometer must be calibrated against NBS thennometer.
It must be in111ersed in a beaker of sand. Temperature
must be recorded daily (35°C 29.5).
Fecal Colifonn -Water bath incubator -
Thennometer must be calibrated against NBS thennometer.
Temperature must be recorded daily (44.5°C :!:().2)
L. Autoclave -National 704-90000
Refer to owner's manual for operation.
M. Microscope -American Optical 42RT
-Uni tron BMLK
-

B

& L Gallen II -Phase contrast & polarized light
Refer to owner's manual for operation.
N. Atomic Absorption -Varian Model 475
Hollow Cathode and Electrodless Discharge Lamps
Vapor Generation Accessory
Flameless Mercury Analyzer
Graphite Furnace
Refer to Owner's manual for operation.
0. Gas Chromatograph-Mass Soectrometer -
Hewlett Packard Model 5992
Purge & Trap Accessory
Dual Flexible Disk Drive
Refer to Owner's manual for operation.
FORM
DAILY EQUIPMENT CHECK LIST
DATE: _________ _
tquipment Description Specifications
Required Actua 1.
Refri oera tor No. 1 4°c
Refri a era tor No. 2 4°c
BOD Incubator 20°c+1
lrvina Oven No. 1 103-105°C
lrvi na Oven No. 2
·otal Coliform Incubator 35°c+.2
Fecal Coliform Bath 44.5°c+.2
.
39
BY: __________ _
Corrments
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VI
40
GLASSWARE
A. General
The measurement of trace constituents in water demands
methods capable of maximum sensitivity. This is especially
true for metals and trace organics such as pesticides, as well
as for the detennination of a1m1onia and phosphorus. In addition
to sensitive methods, however, there are other areas that
require special consideration. One such area is that of the
cleanliness of laboratory glassware. Obviously, the very
sensitive analytical systems are more sensitive to errors
resulting from the improper use or choice of apparatus, as
well ·as to contamination effects due to an improper method of
cleaning the apparatus. The purpose of this chapter is to
discuss the kinds of glassware. available, the use of volumetric
glassware and various cleaning requirements.
B. Types·of Glassware
Laboratory vessels serve three functions: storage of
reagents, measurement of solution volumes, and confinement
of reactions. For special purposes, vessels made from
materials such as porcelain, nickel, iron, aluminum, platinum,
stainless steel, and plastic may be employed to advantage.
Glass, however, is the most widely used material of construction.
There are many grades and types of glassware from which to
choose, ranging from student grade to others possessing
specific properties such as super strength, low boron content,
41
and resistance to thennal shock or alkali. Soft glass
containers are not recolTITiended for general use, especially
for storage of reagents because of the possibility of dissolving
of the glass (or of some of the constituents of the glass}.
The mainstay of the modern analytical laboratory is a highly
resistant borosilicate glass, such as that manufactured by
Corning Glass Works under the name "Pyrex" or by Kimble Glass
Co. as "Kimax." This glassware is satisfactory for all
analyses included in reference l.
Depending on the particular manufacturer, various trade
names are used for specific brands possessing special properties
such as resistance to heat, shock, and alkalies. Examples of
some of these special brands follow:
l. Kimax-or Pyrex-brand glass is a relatively inert all-
purpose borosilicate glass.
2. Vycor-brand glass is a silica glass (96 percent} made
to withstand continuous temperatures up to 900°C and can
be down-shocked in ice water without breakage.
3. Corning-brand glass is claimed to be 50 times more
resistant to alkalies than conventional ware and
practically boron-free (maximum 0.2 percent}.
4. Ray-Serb-or Low-Actinic-brand glass is used when the
reagents or materials are light sensitive.
5. Corex-brand labware is harder than conventional bore-
silicates and therefore better able to resist clouding
and scratching.
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42
The use of plastic vessels, containers, and other
apparatus made of Teflon, polyethylene, polystyrene, and
polypropylene has increased markedly over recent years ..
Some of these materials, such as Teflon, are quite expensive;
however, Teflon stopcock plugs have practically replaced
glass plugs in burets, separatory funnels, etc., because
lubrication to avoid sticking or "freezing" is not required.
Polypropylene, a methylpentene polymer, is available as
laboratory bottles, graduates, beakers, and even volumetric
flasks. It is crystal clear, shatterproof, autoclavable, and
chemically resistant.
The following are some points to consider in choosing
glassware or plasticware:
l. The special types of glass listed above, other than
Pyrex or Ki max, generally are not required to perform
the analyses given in "Methods for Chemical Analysis
Water and Wastes" (l ) .
2. Unless instructed otherwise, borosilicate or·polyethylene
bottles may be used for the storage of reagents and
standard solutions.
3. Dilute metal solutions are prone to plate out on
container walls over long periods of storage. Thus,
dilute metal standard solutions must be prepared fresh
at the time of analysis.
C.
43
4. For some operations, disposable glassware is entirely
satisfactory. One example is the use of disposable
test tubes as sample containers for use with the
Technicon automatic sampler.
5. Plastic bottles of polyethylene and Teflon have been
found satisfactory for the. shipment of water samples.
Strong mineral acids (such as sulfuric acid) and
organic solvents will readily attack polyethylene and
are to be avoided.
6. Borosilicate glassware is not completely inert, particularly
to alkalies; therefore, standard solutions of silica, boron,
and the alkali metals are usually stored in polyethylene
bottles.
For additional infonnation, the reader is· referred to the
cata 1 ogs of the various glass and p 1 as tic manufacturers. These
catalogs contain a wealth of infonnation such as specific
properties, uses, and sizes.
Volumetric.Analyses
By corrrnon usage, accurately calibrated glassware for
precise measurements of volume has become known as volumetric
. glassware. This. group includes volumetric flasks, volumetric
pipets, and accurately calibrated burets. Less accurate types
of glassware including graduated cyliners and serological and
measuring pipets also have specific uses in the analytical
laboratory when exact volumes are unnecessary.
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Volumetric pipets are calibrated to deliver a fixed
volume. The usual capacities are 1 through 100 ml although
micropipets are also available. Micropipets are most
useful in furnace work and are available in sizes ranging from
1 to 100 u 1.
In emptying volumetric pipets, they should be held in a
vertical position and the outflow should be unrestricted. The
tip of the pipet is kept in contact with the wall of the
receiving vessel for a second-or two after the free flow has
stopped. The liguid remaining in the tip is not removed;
this is most important.
Measuring and serological pipets should also be held in
a vertical position for dispensing liquids; however, the tip
of the pipet-is only touched to the wet surface of the
receiving vessel after the outflow has ceased. For those
pipets where the small amount of liquid remaining in the tip
is to be blown out and added, indication is made by a frosted
band near the top.
Burets are used to deliver definite volumes. The
more co11111on types are usually of 25-or 50-ml capacity,
graduated to tenths of a millilter, and are provided with
stopcocks. For precise analytical methods in microchemistry,
microburets are also used. Microburets generally are of S-
or 10-ml capacity, graduated in divisions of hundredths
of a milliliter. Automatic burets with reservoirs are
also available ranging in capacity from 10 to 100 ml.
Reservoir capacity ranges from 100 to.4,000 ml.
45
General rules in regard to the manipulation of a buret
are as follows: Do not attempt to dry a buret that has been
cleaned for use, but rinse it two or three times with a
small volume of the solution with which it is to be filled.
Do not allow alkaline solutions to stand in a buret because
the glass will be attacked, and the stopcock, unless made of
Teflon, will tend to freeze. A 50-ml buret should not be
emptied faster than 0.7 ml/s, otherwise too much liquid will
adhere to the walls and as the solution drains down, the
meniscus will gradually rise, giving a high false reading.
It should be emphasized that improper use or reading of
. burets can result in serious calculation errors.·
In the case of all apparatus for delivering liquids,
the glass must be absolutely clean so that the film of
liquid never breaks at any point. Careful attention must
be paid to this fact or the required amount of solution will
not be delivered. The various cleaning agents and their
use are described later.
D. · Federal ·specifications for Volumetric Glassware
Reference 2 contains a description of Federal specifi-
cations for volumetric glassware. The National Bureau of
Standards no longer accepts stock quantities of volumetric
apparatus from manufacturers or dealers for certification
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46
and return for future sale to consumers. This certification
service is still available, but apparatus will be tested only
when submitted by the ultimate user, and then only after an
agreement has been reached.with the Bureau concerning the work
to be done.
Consequently, the various glass manufacturers have
discontinued the listing of NBS-certified ware. In its place
catalog listings of volumetric glass apparatus that meet the
Federal specifications are designated as Class A and all such
glassware is pennanently marked with a large "A". These
NBS specifications are listed in Table 1. The glassware in
question includes the usual burets, volumetric flasks, and
volumetric pipets.
In addition to the "A" marking found on calibrated
glassware and the temperature at which the calibration was
made, other markings also appear. These include the type
of glass such as Pyrex, Corex, or Kimax; the stock number of
the particular item; and the capacity of the vessel. If the
vessel contains a ground-glass connection, this will also be
included along with the TD or TC symbol.
Class A glassware need not be recalibrated before use. However,
if it should become necessary to calibrate a particular piece
of glassware, directions may be found in text on quantitative
analysis.
TABLE 1
Tolerances for Volumetric Glassware 1
Type of Glassware
Graduated fl ask
Transfer pipet
Buret3
]Abridged from reference 3.
2Less than and including.
Capacity2 (ml)
25
50
100
200
250
300
500
1,000
2,000
2
5
10
25
30
50
100
200
5
10
30
50.
100
3Limits of error are of total or partial capacity.
47
Limit of Error(ml)
0.03
0.05
0.08
0. l 0
0. 11
0. 12
0. 15
0.30
0.50
0.006
0.01
0.02
0.025
0.03
0.05
0.08
0. 10
0.01
0.02
0.03
0.05
0.10
Customary practice is to test the capac!tY at five intervals.
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48
E. Cleaning of Glass and Porcelain
The method of cleaning should be adapted to both
the substances that are to be removed, and the determination
to be performed. Water-soluble substances are simply washed
out with hot or cold water, and the vessel is finally rinsed
with successive small amounts of distilled water. Other
substances more difficult to remove may require the use of
a detergent, organic solvent, dichromate cleaning solution,
nitric acid, or aqua regia (24 percent by volume concentrated
HN03 in concentrated NCl ). In all cases it is good practice
to rinse a vessel with tap water as soon as possible after use.
Material allowed to dry on glassware is much more difficult
to remove.
Volumetric glassware, especially burets, may be thoroughly
cleaned by a mixture containing the following: 30 g of sodium
hydroxide, 4 g of sodium hexametaphosphate (trade name, Calgon),
8 g of trisodium phosphate, and 1 1 of water. A gram or two
of sodium 1 auryl sulfate or other surfactant wi 11. improve its
action in some cases. This solution should be used with a
buret brush.
Dichromate cleaning solution (chromic acid) is a powerful
agent; however, because of its destructive nature upon clothing
and upon laboratory furniture, extreme care must be taken
when using this mixture. If any of the solution is spilled, it
49
must be cleaned up immediately. Chromic acid solution may
be prepared in the laboratory by adding l l of concentrated
sulfuric acid slowly, with stirring, to a 35-ml saturated sodium
dichromate solution. This mixture must be allowed to stand for
approximately 15 minutes in the vessel that is being cleaned
and may then be returned to a storage bottle. Following the
chromic acid wash, the vessels are rinsed thoroughly with tap
water, then with small successive portions of distilled water.
The analyst should be cautioned that when chromium is included
in the scheme of analysis, it is imperative that the last
traces of dichromate be removed from the appartus. To this end,
a substitute for dichromate cleaning solution, called Nochromix,*
is available and may be used to advantage. Fuming nitric acid
is another powerful cleaning agent, but is disagreeable to handle.
As with dichromate, when the acid becomes dilute, the cleaning
mixture is no longer effective. A mixture of concentrated
sulfuric and fuming nitric acids is even more efficient but
is also hazardous to use. A persistent greasy layer or spot
may be removed by acetone or by allowing a warm solution of
sodium hydroxide, about lg per 50 ml of water, to stand in
the vessel for 10 to 15 min; after rinsing with water, dilute
hydrochloric acid, and water again, the vessel is usually clean.
Alcoholic potassium hydroxide is also effective in removing
grease. To dry glass apparatus, rinse with acetone and blow
or draw air through it.
*Available from Godax Laboratories, 6 Varick Street, New York, NY
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F.
50
Special Cleaning Requirements
Absorption cells, used in spectrophotometers, should
be kept scrupulously clean, free of scratches, fingerprints,
smudges, and evaporated film residues. The cells may be
cleaned with detergent solutions for removal of organic residues,
but should not be soaked for prolonged periods in caustic
solutions because of the possibility of etching. Organic
solvents may be used to rinse cells in which organic materials
have been used. Nitric acid rinses are pennissible, but
dichromate solutions are not reco1TJTiended because of the
adsorptive properties of dichromate on glass. Rinsing and
drying of cells with alcohol or acetone before storage is a
preferred practice. Matched cells should be checked to see
that they are equivalent by placing portions of the same
solution in both cells and taking several readings of the
transmittance (T, percent) or optical density (OD) values.
For certain detenninations, especially trace metals, the
glassware should also be rinsed with a 1:1 nitric• acid-water
mixture. This operation is followed by thoroughly rinsing with
tap.water and successive portions of distilled water. This may
require as many as 12 to 15 rinses, especially if chromium is
being detennined. The nitric acid rinse is also especially
important if lead is being detennined.
51
Glassware to be used for phosphate detenninations should
not be washed with detergents containing phosphates. This
glassware must be thoroughly rinsed with tap water and distilled
water. For ammonia and kjeldahl nitrogen, the glassware must
be rinsed with arrmonia-free water.
Glassware to be used in the detennination of trace
organic constituents in water, such as chlorinated pesticides,
should be as free as possible of organic contaminants. A
chromic acid wash followed by a detergent wash is necessary to
destroy these organic residues. Rinse thoroughly with tap
water, distilled water and finally, with acetone followed by
hexane. Glassware may be dried for irrmediate use by rinsing
with redistilled acetone. Otherwise glassware may be oven
dried or drip-dried. Glassware should be stored immediately
after drying to prevent any accumulation of dust and stored
inverted or with mouth of glassware cover with foil.
Bottles to be used for the collection of samples for
semi-volatile organic analyses should be washed successively
with chromium acid cleaning solution detergent, tap water,
distilled water, and finally, several times with a redistilled
solvent such as acetone followed by hexane. Caps are washed
with detergent, rinsed with tap water, distilled water and
solvent. Liners are treated in the same way as the bottles
and are stored in a sealed container.
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51.1
Bottles to be used for the collection of volatile organics
should be washed with chromium acid cleaning solution or
detergent, rinsed with tap water followed by distilled water.
Note that organic solvents should not be used as they may
introduce contamination. Bottles should then be dried in an
oven at 105 degrees Ca minimum of 1 hour. Teflon-faced septa
for the VOA bottles should be processed as above except no
chromic acid should be used.
Bottles to be used for total organic halogen (TOX)
analysis should be new amber glass with teflon-lined closures.
These bottles are to be washed thoroughly with methanol,
rinsed with tap water followed by distilled water. The ,
bottles should then be dried in an oven at 150 degrees C for a
minimum of 1 hour .. Teflon closures can be processed as VOA's
above.
52
G. Disposal Glassware
When the risk of washing a pipet for reuse becomes
too great, as in the case of use with toxic materials, or when
the cost of washing glassware becomes prohibitive, disposable
vessels may be the answer, provided they meet the necessary
specification. Various types are available including bacterio-
logical, serological, and microdilution pipets. Disposable
glassware generally is made of soft glass although plastic
vessels and pipets are also available.
H. Specialized Glassware
The use of vessels and glassware fitted with standard-
taper, ground-glass, and ball-and-socket joints has increased
because of certain advantages such as less leakage and fewer
freezeups. Standard-taper, interchangeable ground joints
save time and trouble in assembling apparatus. They are
precision-ground with tested abrasives to insure an accurate
fit and freedom from leakage. Ball and socket joints increase
flexibility of operation and eliminate the need for exact
alignments of apparatus. Symbols and their meaning as applied
to standard joints, stoppers, and stopcocks are shown below.
l. Standard Taper(~)
The symbol Tis used to designate interchangeable s
joints, stoppers, and stopcocks that comply with the
requirements of reference 5. All mating parts are
finished to a l :10 taper.
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53
The size of a particular piece appears after the
appropriate symbol. Primarily because of greater variety
of apparatus equipped with T.fittings, a number of
s
different types of identifications are used:
a. For joints - a two-part number as T 24/40, with s
24 being the approximate diameter in millimeters
at the large end of the taper and 40 the axial
length of taper, also in millimeters.
b. For stopcocks-a single number, as T 2, with 2 mm s
being the approximate diameter of the hole or holes
through the plug.
c. For bottles-a single number, as Tl9, with 19 mm s
being the appropriate diameter at top of neck.
However, there are differences in dimensions between
the bottle and fl ask steppe.rs.
d. For flasks and similar containers, a single number
as T 19, with 19 mm being the appropriate diameter
s
of the opening at top of neck.
2. Spherical Joints (S)
J
The designation Sis for spherical (semiball)
J
joints complying with reference 5. The complete desig-
nation of a spherical joint also consists of a two-part
number, as 12/2, with 12 being the approximate diameter
of the ball and 2 the bore of the ball and the socket,
also in millimeters.
3. Product Standard (P) s
The symbol Pis used for stopcocks with Teflon s
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54
plugs, the mating surfaces being finished to a 1:5 taper.
As with T stopcocks, a single number is used. Thus, s
P 2 means a Teflon stopcock with a hole of approximately s
2-mm diameter in the plug.
Fritted Ware
For certain laboratory operations, the use of fritted
ware for filtration, gas dispersion, absorption, or extrac-
tions may be advantageous.
There are six different porosities of fritted ware
available, depending on its intended use. Porosity is
controlled in manufacture, and disks are individually
tested and graded into these classifications. The extra-
coarse and coarse porosities are held toward the maximum pore
diameter as listed. The medium, fine, very fine, and ultra-
fine are held toward the minimum pore diameter as listed
in Table 2.
Pore sizes are determined by the method specified
in reference 3.
1. Rec011JTiended·Procedures for Maximum Filter Life
a. New Filters. Wash new filters by suction with hot
hydrochloric acid, followed by a water rinse.
b. Pressure Limits. The maximum, safe, diff_erential
pressure on a disk is 15 lb/in2.
c. Thermal Shock. Fritted ware has less resistance
to thermal shock than nonporous glassware. Hence,
excessive, rapid temperature changes and direct
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55
exposure to a flame should be avoided. Heating in
a furnace to 500°C may be done safely, provided
the heating and cooling are gradual. Dry ware may
be brought to constant weight by heating at 105°C
to 110°c.
Never subject a damp filter of ultrafine porosity
to a sudden temperature change. Steam produced in the
interior may cause cracking.
Paras i ty Grade
Extra Coarse
Coarse
Medium
Fine
Very Fine
Ultra fine
TABLE 2
Fritted-Ware Porosity
Designation Pore Size (um)
EC
C
M
F
VF
UF
170-220
40-60
10-15
4-5.5
2-2.5
0.9-1.4
56
Principal Users
Coarse filtration; gas
dispersion, washing,
and absorption
Coarse filtration; gas
dispersion, washing,
and absorption
Filtration and extraction
Filtration and extraction
General bacterial filtration
General bacterial filtration
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2.
Material
Albumen
57
Cleaning of Used Filters
In many cases, precipitates can be removed
by rinsing with water, passed through from the under-
side, with the pressure not exceeding 15 lb/in2. The
suggestions that follow wjll be helpful in dealing
with material that will not be removed by such a
reverse water-wash:
Removal Agent
Aluminous and siliceous residues
Hot arrmonia or hydrochloric acid
Hydrofluoric acid (2 percent) followed
by concentrated sulfuric acid; rinse
i111llediately with water until no trace
of acid can be detected.
Copper or iron oxides
Fatty materials
Mercuric sulfide
Organic matter
Silver chloride
Hot hydrochloric acid plus potassium
chlorate
Carbon tetrachloride
Hot aqua regi a
Hot, concentrated cleaning solution,
or hot, concentrated sulfuric acid
with a few drops of sodium nitrite
Arrmonium or sodium hyposulfite
58
J, References
1. Methods for Chemical Analysis of Water and Wastes,
U. S. EPA, Office of Research and Development,
EMSL ( 19 78).
2. Hughes, J. C., Testing of Glass Volumetric Apparatus,
NBS Circular 602, National Bureau of Standards (1959).
3. Peffer, E. L., and Mulligan, G. C., Testing of Glass
Volumetric Apparatus, NBS Circular 434, National
Bureau of Standards (1941).
4. Willard, H. H., and Funnan, N. H., Elementary
Quantitative Analysis-Theory and Practice, D. Van
Nostrand Co., Inc., New Yrok (1947).
5. Interchangeable Ground Glass Joints, Corrmercial
Standard CS-21-30, National Bureau of Standards
(Aug. 25, 1930).
6. Maximum Pore Diameter and Penneabil i ty of Rigid
Porous Filters for Laboratory Use, E-128, American
Society for Testing and Materials, Philadelphia
(19681.
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V 11
59
REAGENTS, SOLVENTS, AND GASES
A. Introduction
B.
The objective of this chapter is to provide general
infonnation and suggestions that will serve to keep the
analyst conscious of his responsibilities in analytical
quality control, as they relate to reagents, solvents, and
gases. While the material presented here will assist the
analyst in producing high quality data, it is by no means
complete. It is incumbent on the analyst to obtain details
of special precautions required to insure proper selection,
preparation, and storage of reagents, solvents, and gases
from the descriptions of individual methods.
Reagent Quality
Chemical reagents, solvents, and gases are available
in a wide variety of grades of purity, ranging from technical
grade to various ultrapure grades. The purity of these materials
required in analytical chemistry varies with the type of analysis.
The parameter being measured and the sensitivity and specificity
of the detection system are important factors in determining
the purity of the reagents required. For many analyses, including
most inorganic analyses, analtyical reagent grade is satisfactory.
Other analyses, such as trace organic and radiological,
frequently require special ultrapure reagents, solvents, and
gases. In methods where the purity of reagents is not specified,
it is intended that analytical reagent grade be used. Reagents
60
of lesser purity than that specified by the method should not
be used. The labels on the container should be checked and the
contents examined to verify that the purity of the reagents
meets the needs of the particular method involved. The
quality of reagents, solvents, and gases required for the
various classes of analyses-inorganic, metals, radiological,
and organic-are discussed in this section.
Reagents must always be prepared and standardized with the
utmost of care and technique against reliable primary standards.
They must be restandardized or prepared fresh as often as required
by their stability. Stock and working standard solutions must
be checked regularly for signs of deterioration; e.g.,
discoloration, fonnation of precipitates, and change of
-concentration .. Standard solutions should be properly labeled
as to compound, concentration, solvent, date, and preparer.
Primary standards must be obtained from a reliable source,
pretreated (e.g., dried, under specified conditions), accurately
prepared in calibrated volumetric glassware, and stored in
containers that will not alter the reagent. A large number
of primary standards are available from the National Bureau
of Standards (NBS). A complete listing of available standards
is given in reference 1. Primary standards may also be obtained
from many chemical supply companies. Suppliers for special
quality reagents, solvents, and gases are noted in later
discussions of the various classes of analyses. Reagents and
solvents of all grades are available from many chemical supply
houses.
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There is some confusion among chemists as to the definition
of the te1111s "Analytical Reagent Grade," "Reagent Grade," and
"ACS Analytical Reagent Grade". A review of the literature
and chemical supply catalogs indicates that the three te1111s
are synonymous. Hereafter, in this document, the te1111 "Ana lyti cal
Reagent Grade" (AR) will be used. It is intended that AR-grade
chemicals and solvents shall confo1111 to the current specifications
of the Committee on Analytical Reagents of the American Chemical
Society2.
References 3 through 5 devote several chapters to problems
related to preparation, standardization, and storage of reagents.
The info1111ation provided therein is particularly appropriate
to inorganic dete1111inations. The type of volumetric glassware
to be used, the effect of certain reagents on glassware, the
effect of temperature on volumetric measurements, purity of
reagents, absorption of gases and water vapor from the air,
standardization of solutions, instability, and the need for
frequent standardization of certain reagents are among the
topics discussed. It is recorrrnended that the analyst become
thoroughly familiar with these publications.
l. General Inorganic Analyses
In general, AR-grade reagents and solvents are
satisfactory for inorganic analyses. Primary standard
reagents must, of course, be used for standardizing all_
volumetric solutions. Corrrnercially prepared reagents
62
and standard solutions are very convenient and may be
used when it is demonstrated that they meet the method
requirements. All prepared reagents must be checked
for accuracy.
The individual methods specify the reagents that
require frequent standardization, or other special
treatment, and the analyst must follow through with
these essential operations. To avoid waste, the analyst
should prepare a limited volume of such reagents, depending
on the quantity required over a given period of time.
Examples and brief discussions of the kind of problems
that occur are given in section (3).
As far as possible, distilled water use for preparation
of reagent solutions must be free of measurable amounts of
the constituent to be determined. Special requirements for
distilled water are given in Chapter IV. of this manual and
in individual method descriptions.
Compressed gases, such as oxygen and nitrogen, used
for total organic carbon determination may be of commercial
grade.
2. Metals Analyses
All standards used for atomic absorption and emission
spectroscopy should be of spectroquality. It is recommended
that other reagents and sol vents al so be of spectroqua l ity,
although AR grade is sometimes satisfactory. Standards may
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be prepared by the analyst in the laboratory, or
spectrographically standardized materials may be
purchased coITTTiercially. Standards required for deter-
mination of metals in water are not generally available
from the National Bureau of Standards.
Analytical-reagent-grade nitric and hydrochloric
acids must be specially prepared by distillation in
borosilicate glass and diluted with deionized distilled
water. All other reagents and standards are also
prepared in deionized water.
In general, fuel and oxidant gases used for atomic
absorption can be of c0111Tiercial grade. Air supplied
by an ordinary laboratory compressor is quite satisfactory,
if adequate pressure is ma.intained and necessary precautions
are taken to filter oil; water, and possible trace metals
from the line. For certain detenninations such as
aluminum, AR-grade nitrous oxide is required.
3. Radiological Analyses
The great sensitivity of radioactive counting
instruments requires that scintillation-grade reagents
and solvents, or equivalent, be used for all radioactivity
: detenninations. Some of the reagents, for example,
strontium carbonate and yttrium oxide carriers used for
the detennination of strontium-90 and yttrium-90, must be
stable, that is, free of radioactivity. Barium sulfate,
used for coprecipitation of radium, must be free from
all traces of radium. These reagents and solvents are
commercially available from chemical supply houses.
64
Calibrated standard sources of specific radioactive
materials with known count and date of counting are
available from various suppliers. tlo single company
supplies all standards.
Gases used for radioactive counting must be of high
purity and extra dry. Bases such as helium and air are
aged for about 30 days to allow radioactive background
to decay. All gases are checked for background before
use. Some cylinders contain inherent radioactivity that
is imparted to the gas. When this background is above
normal, the gas should not be used for radioactivity
determinations.
4. Organic Chemical Analyses
The minimum purity of reagents that can be used for
organic analyses is AR grade. Reference-grade standards
should be used whenever available. Special note should
be taken of the assay of standard materials. Owing to the
great sensitivity (nanogram and subnanogram quantities)
of gas chromatography (GC), which is often used to
quantitate organic results, much greater purity is
frequently required 6. The specificity of some GC
detectors requires that reagents and solvents be free of
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certain classes of compounds. For example, analyses by
electron capture require that reagents and solvents be
free of electronegative materials that would interfere
with the determination of specific compounds in the sample.
Similarly, use of the flame photometric dector requires
that reagents and solvents be free from sulfur and
phosphorus interference. Pesticide-quality solvents,
available from several sources, are required when doing
low-level work. AR-grade solvents are permissible when
analyzing industrial waste samples.
However, the contents of each container must be
checked to assure its suitability for the analyses.
Similarly, all analytical reagents and other chemicals
must also be checked routinely.
The quality of gases required for GC determination
varies somewhat with the type of detector. In general,
the compressed gases are a prepurified dry grade. Grade
A helium from the U. S. Bureau of Mines has always been
satisfactory. The Dohrmann nitrogen detection system
requires the use of ultrapure hydrogen for satisfactory
results. Nitrogen used for electron-capture work
:should be oxygen free and should have an oxygen trap in
the supply line. The use of molecular-sieve, carrier-gas
filters and drying tubes is required on combustion gases
and is reconmended for use on all other gases. It is
C.
66
recollillended that the analyst familiarize himself with an
article by Burke? on practical aspects of GC.
All reagents, solvents and adsorbents used for thin-
layer chromatography must be checked to be certain that there
are no impurities present that will react with the
chromogenic reagent or otherwise interfere with subsequent
qualitative or quantitative detenninations. Glass-backed
layers prepared in the laboratory or precoated layers
supplied by a manufacturer may be used; however, precoated
layers are more difficult to scrape.
Elimination of Detenninate Errors
Procedures for eliminating or at least minimizing
impurities that produce specific interferences or high general
background vary with the reagent and method involved. These
procedures may include the following: recrystallization,
precipitation, distillation, washing with an appropriate solvent,
or a combination of these. Examples of procedures used for
various types of analyses are given below. For complete
infonnation, the analyst should consult the individual
methods.
l. General Inorganic Analyses
Analytical-reagent-grade chemicals and solvents
usually present no •interference problems in inorganic
analyses. However, some reagents do not always meet methods
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requirements. An example is potassium persulfate used in
phosphorus and nitrogen detenninations. This reagent
is frequently contaminated witJi ammonia. Therefore, it
is routinely purified by passing air through a heated
water solution of the reagent. The purified potassium
persulfate is recovered by recrystallization.
A problem more conrnonly encountered in inorganic
analyses is the rapid deterioration of the standard
reagents and other ingredients. To minimize or eliminate
this problem, some reagents, for example, ferrous anrnonium
sulfate, must be standardized daily. Others, such as
sodium thiosulfate used for dissolved oxygen detennination,
may require a substitute reagent such as phenylarsine
oxide. · Solid phenol, which readily oxidizes and acquires
a reddish color, can be.purified by distillation. Starch
indicator used for idiometric titrations may be prepared
for each use or preserved by refrigeration or by
addition of zinc chloride or other suitable compounds.
Metals Analyses
In general, spectrograde chemicals, solvents, and
gases present no interference problems in atomic absorption
or emission spectrographic detenninations. However,
standards that do not meet the requirements of the method
are sometimes obtained. Ordinarily, no effort is made
to purify them. They are simply replaced by new reagents of
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sufficient purity. Some reagents may form precipitates
on standing. Such reagents will reduce the accuracy of
quantitative analyses and should not be used.
3. Radiological Analyses
In general, reagents that do not meet the purity
requirements for radiological detenninations are replaced
with reagents that are satisfactory. However, in some
instances (for example, barium sulfate used for copreci-
pitation of radium) it may be necessary to perfonn
repeated recrystallization to remove all fonns of radium,
and reduce the background count to a usable level. In
some instances, solvents that do not meet requirements may
be di sti 11 ed to produce adequate purity. In some cases,
gases having background counts may be usable after aging
as described earlier. If not, they should be replaced
with gases that are satisfactory.
4. Organic Analyses
Many AR-grade chemicals and solvents, and.at times
pesticide-quality solvents, do not meet the specifications
required for the detennination of specific organic
compounds. Impurities that are considered trace, or
insignificant, for many analytical uses are often present
in greater quantities than the organic constituents being
measured. Coupled with the several-hundred-fold concen-
tration of the sample extract that is usually required,
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such impurities can cause very significant interferences
in trace organic analyses. Reagents and solvents found
to be unsatisfactory, under the conditions of the analyses,
must be replaced or cleaned up so that they are usable.
Some useful clean-up procedures are:
a. Washing the inorganic reagents with each solvent
that the reagents contacts during the analysis.
b. Washing the absorbents, such as silical gel G
and Florisil, with the solvents that are used for
a specified column or thin-layer chromatographic
procedure, or reactivating the Florisil by firing
to 630°C.
c. Pre-extracting distilled water with solvents used
for the particular analysis involved.
d. Pre-extracting aqueous reagent solutions with the
solvents involved.
e. Redistilling solvents in all-glass systems using an
efficient fractionating column.
f. Recrystallizing reagents and dyes used in
colorimetric or thin-layer detenninations.
If the reagents and solvents thus produced are not of
sufficient purity, they should be replaced.
Dirty gases (quality less than specified) are parti-
cularly troublesome in gas chromatographic analyses.
They may reduce the sensitivity of the detector, and
71
It is important that all containers be properly cleaned and
stored prior to use. (Refer to Ch. 4 for details.)
Standard reagents and solvents must always be stored
according to the manufacturer's directions. Reagents or
solvents that are sensitive to the light should be stored
in dark bottles and in a cool, dark place. It is particularly
important to store matierals used for radiological deter-
minations in dark bottles, because photoluminescence will
produce high background if .light-sensitive detectors are
used for counting. Some reagents require refrigeration.
Adsorbents for thin-layer and column chromatography
are stored in the containers that they are supplied in, or
according to the requirements of individual methods.
When new stock solutions are necessary, dilutions of the
old and new standard shou.ld be compared to detennine
their accuracy.
The analyst should pay particular attention to the
stability of the standard reagents. Standards should not
be kept longer than reconmended by the manufacture or in
the method. Some standards are susceptible to changes in
nonnality because of absorption of gases or water vapor
from the air. Provisions for minimizing this effect are
given in reference 4.
The concentration of the standards will change as a
result of evaporation of solvent. This is especially
true of standards prepared in volatile organic solvents.
Therefore, the reagent bottles should be kept stoppered,
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except when in actual use. The chemical composition of
certain standards may change on standing. Certain pesticides,
for instance, will degrade if prepared in acetone that
contains small quantities of water. Thus, it is essential
that working standards be frequently checked to determine
changes in concentration or composition. Stock solutions
should be checked before preparing new working standards
from them.
References
l. Catalog of Standard Reference Materials, NSB Special
Publication 260, National Bureau of Standards (June
19 75).
2. "Reagent Chemicals," American Chemical Society
Specifications, 5th Edition, American Chemical
Society; Washington, D .C. (1974).
3. Manual on Industrial Water and Industrial Waste Water
2nd Edition, ASTM Special Publication 148-H, American
Society for Testing and Materials(l965), p. 869.
4. "Standard Methods for Preparation, Standardization,
and Storage of Standard Solutions for Chemical
Analysis," from Part 31 of 1976 Book of ASTM Standards,
American Society for Testing and Materials,
Philadelphia(l977).
5. Standard Methods for the Examination of Water and
Wastewater, 13th Edition, American Public Health
Association, New York(l971).
73
6. Methods for Organic Pesticides in Water and
Wastewater, U.S. EPA, Environmental Research
Center, Cincinnati (1971 ).
7. Burke, J., ''Gas Chromatography for Pesticide Residue
Analysis; Some Practical Aspects," J. Assoc. Off.
Anal. Chem., 48, 1037(1~65).
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VIII. LABORATORY SAFETY
Safety is important in the laboratory .. Therefore, each employee
working in a laboratory should be thoroughly familiar with this section.
Personnel working in a laboratory must realize that a number of
hazardous materials and conditions exist. PREVENT ACCIDENTS. Be alert
and careful. Be aware of potential dangers at ·all times. The major threats
to you are listed for your safety.
A. Infectious Materials
B.
Wastewater and sludge contain millions of bacteria,
some of which are infectious and dangerous, and can cause
diseases such as tetanus, typhoid, dysentery, poliomelytis,
and hepatitis. Personnel handling these materials should
thoroughly wash their hands with soap and water, particularly
before handling food. Do not pipette wastewater or polluted
samples by mouth. Use a rubber bulb. Though not mandatory,
inoculations by your County Health Department are recommended
for each employee.
Corrosive Chemicals
1 . Acids
a. Examples: Sulfuric, hydrochloric, nitric, glacial
acetic, Pomeroy solutions Nos. 1 and 2, and
chromic acid cleaning solutions.
b. Acids are extremely corrosive to human tissue,
metals, clothing, wood, cement, stone, and concrete.
2.
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Use glassware or polyethylene containers.
c. In case of accidental spills, immediately dilute with
large portions of water and neutralize the acid with
sodium carbonate or bicarbonate until bubbling and
foaming stops. Clean-up neutralized material.
If spills occur on bench tops, dilute, neutralize, and
squeeze into sink. If spills occur on person,
inmediately wash off with water. If spills occur
on face (spills of concentrated acid), inmediately
flood with large quantities of cold water. Notify
supervisor. Remember to add acid to water, but
Bases
not reverse. Pour and pipette carefully to prevent
spilling and dropping. Prevent contact with metals,
particularly equipment.
a. Examples: Sodium hydroxide, potassium hydroxide,
anmonium hydroxide, alkaline iodide--sodium azide
solution.
b. Handle with extra care and respect. They are
extremely corrosive to skin, clothing, and leather.
Use glassware and polyethylene containers.
Anmonium hydroxide is extremely irritating to
the eyes and respiratory system. Pour anmonium
hydroxide under a laboratory hood with fan in
operation.
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C.
76
c. In case of accident, wash with large quantities
of water and use saturated boric acid solution to
neutralize.
3. Miscellaneous
a. Chlorine gas solution--avoid inhalation. Handle
in hood. Secure cover to prevent escape of vapors.
b. Ferric salts, Ferric chloride--very corrosive to
metals. Avoid body contact and wash off immediately.
c. Strong oxidants--avoid body contact. Wash off
immediately. Use of perchloric acid by untrained
personnel must be prohibited.
Toxic Materials
Avoid ingesting or inhaling.
1. Solids: Cyanides, chromium, cadmium, and other
heavy metals compounds.
2. Liquids: Use in vented hood. Carbon tetrachloride,
ammonium hydroxide, nitric acid, bromine, chlorine
water, aniline dyes, formaldehyde, chloroform, and
carbon disulfide. Carbon tetrachloride is absorbed
into skin on contact; its vapors will damage the lungs;
and it will·build up in your body to a dangerous level.
3. Gases: Use in vented hood. Hydrogen sulfide, chlorine,
ammonia, nitric, hydrochloric acid.
D.
E.
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4. Most laboratory chemicals have toxicity warnings and
antidotes on their labels. Learn about the materials
you use. Do not breathe, eat, or drink them; and if they
come in contact with your body, quickly apply large
quantities of water to wash the substances away.
Explosive or Inflamnable Materials
l. Gases: Acetylene, hydrogen.
2. Liquids: Carbon disulfide, benzene, ethyl ether,
petroleum ether, acetone, gasoline.
Store these materials according to fire regulations to
prevent fire hazards. If large quantities must be stored,
they should be located in a separate storage building.
Do not use near open flame or exposed heating elements.
Use under a vented laboratory hood. Do not distill to
dryness or explosive mixtures may result. Use face mask.
Do not throw flarrmable liquids into sinks. Cigarette discard
may cause fire. Do not let gas cylinders fall.
Broken Equipment
l. Inexpensive Items--Beakers and flasks should be
discarded, except for minor chips which can be
flame polished easily.
2. Expensive Items--Should be set aside for salvage if
possible. Discard i.f damaged beyond repair.
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F. Miscellaneous
l. Use safety goggles or face mask in any experiment in
which there is danger to the eyes. Never look into the
end of the test tube during reaction or heating.
Use care in making rubber-to-glass connections.
Lengths of glass tubing should be supported while they
are being inserted into rubber. The ends of the glass
should be flame polished, and either wetted or covered
with a lubricating jelly for ease in joining connections.
Never use grease or oil. Gloves or grippers should be
worn when making such connections, and the tubing should
be held as close to the end being inserted as possible to
prevent bending or breaking.
Never try to force rubber tubing or stoppers from
glassware'. Cut the rubber or material off.
2. Always check labels on bottles to make sure that the
chemical selected is correct. All chemicals and bottles
should be clearly labeled. Never handle chemicals with
bare hands. Use spatula, spoon or tongs.
3. .Never work in a poorly ventilated area. Toxic fumes even
in mild concentrations can knock you out. Be sure you
·have adequate ventilation before you start work in the
laboratory.
4.
5.
6.
79
Smoking and eating should be avoided when working with
infections materials such as wastewater and sludge.
Never use laboratory glassware for serving the food.
Always use the proper type of equipment for handling hot
containers, such as protective gloves, tongs, clothing,
glasses, etc.
Where cylinders of oxygen or other compressed gases
are used in the laboratory, they should be stored in
separated and ventilated sections. They should be
chained or clamped in an upright position while being
used. The protective caps should never be removed
until the cylinder is set and clamped in place, ready
for attachment of valve gage and connections. Always
use fittings approved for the cylinder being used and
carefully follow instructions.
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