#165_05_2014__FinalREVISED

INSPECTION REPORT ROUTING SHEET

To be attached to all inspection reports in-house only.

Laboratory Cert. #: 165

Laboratory Name: Meritech, Inc.

Inspection Type: Commercial Maintenance

Inspector Name(s): Jason Smith, Jeff Adams, Todd Crawford,
Gary Francies, Nick Jones,
Dana Satterwhite, Tonja Springer

Inspection Date: May 20 & 28, 2014

Date Report Completed: June 23, 2014

Date Forwarded to Reviewer: June 23, 2014

Reviewed by: Nick Jones

Date Review Completed: July 3, 2014

Cover Letter to use: Insp. Initial Insp. Reg.
Insp. No Finding Insp. CP
Corrected

Unit Supervisor/Chemist III: Gary Francies

Date Received: 7/16/2014

Date Forwarded to Linda: 8/18/2014

Date Mailed: 8/18/2014

_____________________________________________________________________

cc: Carrie Ruhlmann

At the request of the laboratory, a revision was made to the second paragraph in the General Comments. DBS

On-Site Inspection Report

LABORATORY NAME: Meritech, Inc.

ADDRESS: P.O. Box 27
Reidsville, NC 27320

CERTIFICATE #: 165

DATE OF INSPECTION: May 20 & 28, 2014

TYPE OF INSPECTION: Commercial Maintenance

AUDITOR(S): Jason Smith, Jeff Adams, Todd Crawford, Gary Francies, Nick Jones,
Dana Satterwhite, and Tonja Springer

LOCAL PERSON(S) CONTACTED: Kris Pawlak, David Merritt, and Ian Bailey

I. INTRODUCTION:

This laboratory was inspected by representatives of the North Carolina Wastewater/Groundwater Laboratory
Certification (NC WW/GW LC) program to verify its compliance with the requirements of 15A NCAC 2H .0800 for the
analysis of environmental samples.

II. GENERAL COMMENTS:

The laboratory was clean and well organized. The facility has all the equipment necessary to perform the analyses.
Analytical data pertinent to each certified analysis was filed in an orderly manner and was readily available for
inspection upon request. Laboratory personnel were accessible to answer questions that arose during the inspection.

Some laboratory documentation was incomplete, inaccurate and additional quality control procedures need to be
implemented. The laboratory must take steps to bring operations into compliance with changes in federal
regulations, particularly 40 CFR Part 136 Methods Update Rules; the most recent was published on May 18, 2012.
Many Standard Operating Procedures (SOPs) were in direct conflict with method and/or regulatory requirements,
did not describe in detail how procedures are performed and personnel were not always following the procedures
as described in the SOPs.

The laboratory is reminded that any time changes are made to laboratory operations; the laboratory must update
the Quality Assurance (QA)/Standard Operating Procedures (SOP) document(s). Any changes made in response
to the Findings, Recommendations or Comments listed in this report must be incorporated to insure the method is
being performed as stated, references to methods are accurate, and the QA and/or SOP document(s) is in
agreement with approved practice and regulatory requirements. In some instances, the laboratory may need to
create a SOP to document how new functions or policy will be implemented. The laboratory must also take steps
to insure that all personnel are aware of the changes made; that they have fully implemented those changes and
steps have been taken (e.g., detailed SOPs and guidance documents, documented training and demonstration of
proficiency with new procedures, etc.) to prevent recurrence of findings.

The requirements associated with Findings A, N, O, P, Q, T, HH, KK, YY, ZZ, LLL, MMM, and HHHH have been
implemented by our program since the last inspection.

III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:

Documentation

Recommendation: The laboratory currently maintains only the most recent SOP revision date. It is recommended
that SOP review dates, in addition to revision dates, be maintained. It is recommended that SOPs include a revision
and review history with relevant dates (e.g., effective, review and revision dates) and a brief description of the
change(s) made.

Recommendation: Copies of each reference method are included in each SOP. However, the introduction section,
which lists the approval year for Standard Methods methods, is not included to verify that the document is actually the
most recently approved version. This means that further research (comparing page numbers and text to the approved
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method) is required to verify that the approved method is provided. It is recommended that a copy of the introduction
page of the method be included to easily verify that it is a copy of the most recently approved method.

Recommendation: It is recommended that the initials of the analyst that prepared the calibration curve be recorded
on the daily benchsheet with the calibration curve date to unequivocally link the daily benchsheets to the curve used
for each subsequent set of data. This was specifically noted for Phenols where the analyst’s initials were documented
with the original curve data but not on subsequent benchsheets where only the calibration curve date was recorded.

Recommendation: In order to improve the quality of the data being reported, it is recommended that the laboratory
expand their data verification system to include a technical peer review process to check for accuracy and
completeness of data. Steps must be taken to minimize and correct errors in calculations and may include checks for
the following: transcription errors, calculation errors, correct application of dilution factors, appropriate reporting of dry
weight versus wet weight, correct application of conversion factors, etc. Whether a Laboratory Information
Management System (LIMS) or manual system is used to process laboratory data and generate analytical reports,
the review should include, at a minimum, a percentage of “raw data calculation verifications.” The data reviewer
should recalculate reported results using instrument outputs (e.g., peak area or absorbances) or recorded
measurements (e.g., volume of titrant) for samples and standards, along with sample-specific preparation information
(e.g., dilutions, percent moisture). The number of errors, as well as Quality Control (QC) and data omissions noted
during the inspection underscores the importance of a thorough data review process.

Recommendation: Some SOPs, such as MBAS and Phenols, use the term Method Detection Limit (MDL) in
reference to the reporting limit when it is adjusted for sample dilution or volume. They also state that the blank must
be <1/2 of the MDL, meaning that the blank must be <1/2 of the concentration of the lowest calibration standard. (The
blank acceptance criterion of <1/2 the concentration of the lowest calibration standard meets NC WW/GW LC
requirements.) This causes confusion because the MDL is defined differently in 40 CFR Part 136 Appendix B. It is
recommended that the laboratory adopt the Federal Register definition of MDL and change their terminology to
something like practical quantitation limit (PQL), minimum quantifiable level (MQL), minimum reporting level (MRL),
etc. It is recommended that the laboratory use consistent nomenclature in all SOPs.

Recommendation: Some SOPs (e.g., MBAS and Phenols) state “Samples should be chilled to 0-4 °C during
collection, for transport, and during holding”. Thermal preservation allows a temperature range of 0 -6 °C now, and
it is recommended that a statement be added with regards to the samples not freezing (e.g., “Samples must be
chilled to 0-6 °C without evidence of freezing.”).

Recommendation: As noted above, some SOPs state “Samples should be chilled…” rather than indicating that
they must be chilled. It is recommended that more diligence be used in all SOPs, and a thorough review of all
SOPs be conducted, to clearly indicate when items are a requirement and therefore “must” be done, and when
items are recommended and therefore “should” be done.

Recommendation: Samples are assigned sample identification numbers in the format of XXYYZZ, where X is the
month, Y is the day, and Z is the number of the sample that was received for the day. This format results in
different samples having the same sample number as a sample from previous years. It is recommended that the
year be incorporated into the sample number to prevent this from happening and to increase the legal defensibility
of the data.

A. Finding: The laboratory needs to increase the documentation of purchased m aterials and reagents, as
well as documentation of standards and reagents prepared in the laboratory.

Requirement: All chemicals, reagents, standards and consumables used by the laboratory must have the
following information documented: Date received, Date Opened (in use), Vendor, Lot Number, and
Expiration Date (where specified). A system (e.g., traceable identifiers) must be in place that links
standard/reagent preparation information to analytical batches in which the solutions are used.
Documentation of solution preparation must include the analyst’s initials, date of preparation, the volume
or weight of standard(s) used, the solvent and final volume of the solution. This information as well as the
vendor and/or manufacturer, lot number, and expiration date must be retained for primary standards,
chemicals, reagents, and materials used for a period of five years. Consumable materials such as pH
buffers, lots of pre-made standards and/or media, solids and bacteria filters, etc. are included in this
requirement. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy.
Comment: This traceability must also extend to distillation/digestion logs and computer print outs.
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B. Finding: Numerous instances of writing over a number as a means of error correction were observed.

Requirement: All documentation errors must be corrected by drawing a single line through the error so
that the original entry remains legible. Entries shall not be obliterated by erasures or markings. Wite-Out®,
correction tape or similar products designed to obliterate documentation are not to be used. Write the
correction adjacent to the error. The correction must be initialed by the responsible individual and the date
of change documented. All data and log entries must be written in indelible ink. Pencil entries are not
acceptable. Ref: North Carolina Wastewater/ Groundwater Laboratory Certification Policy.

Comment: Several examples of overwriting were noted on the Biochemical Oxygen Demand (BOD)
benchsheet dated 4/16/14. Other instances were observed and were made by various lab analysts.

C. Finding: Inconsistencies were noted between the Standard Operating Procedures (SOPs) and laboratory
practice as follows:

o Personnel were not following procedures as stated in the Laboratory’s SOP.
 Total Organic Carbon – The SOP states that samples are collected without preservation
and are preserved within two hours. However, sample bottles are sent out with preservative
in order to preserve samples upon collection as required.
 MBAS – The SOP states that a reporting limit standard is analyzed daily, but this is not
being performed consistently.
 Chlorophyll a – The SOP states the calibration curve is updated every six months, but the
curves in the log book are approximately 13 months apart.
 Turbidity – The laboratory was not following the SOP defined acceptance criterion for the
1.0 NTU standard.
 Oil & Grease – The laboratory is not following their SOP and analyzing a Quality Control
Standard (QCS) on a quarterly basis. A quarterly QCS is not required by the method and
this may be in the SOP in order to fulfill the rule requirement [15A NCAC 2H .0805 (a) (7)
(B)] to analyze a quarterly standard for Oil and Grease. Since the OPR fulfills this
requirement and is analyzed on a daily basis, a quarterly QCS sample is not required. The
SOP may be updated to reflect this.
 Metals – EPA Method 200.8, Rev. 5.4 (1994) - The SOP defines the CVS (called a
Continuing Calibration Verification (CCV) in the SOP) standard as mid-range, which would
be 50 µg/L based on the calibration curve, but the laboratory analyzes a 25 µg/L standard as
the CVS (CCV).
o The method reference in the SOP is not correct.
 Settleable Residue – The SOP references EPA Method 160.5, which has not been
promulgated by EPA in 40 CFR Part 136 since May, 2012. The laboratory is certified for
Standard Methods, 2540 F-1997.
 Cyanide – The SOP references EPA Method 335.2. The laboratory is certified for EPA
335.4.
 Total Coliform – The SOP does not include method reference year.
 Ignitability – The SOP references SW -846 1020 A. The laboratory is certified for SW -846
1010 A and 1030.
 Orthophosphate – The Orthophosphate SOP is titled to indicate that it also applies to Total
Phosphorus, which is not contained in this SOP.
o The SOP is in direct conflict with method and/or regulatory requirements.
 BOD – The BOD SOP states that all BOD samples must be composite samples. This is not
always the case since some small facility’s permits require grab samples for BOD analyses.
 Dissolved Residue – The SOP states that the balance is capable of measuring to 1 mg;
however, this is an error and should state that the balance is capable of measuring to 0.1
mg as required by the method.
o The SOP does not describe in detail how the method is performed.
 Inorganic Phenols – The SOP does not indicate the frequency of blank analyses.
 Metals – EPA Method 200.7, Rev. 4.4 (1994) - The SOP does not address standard
preparation and concentrations of standards or specify the source of the standards, i.e., the
Matrix Spike (MS), Calibration Verification Standard (CVS), etc.
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 Metals – EPA Method 200.8, Rev. 5.4 (1994) - The SOP does not address internal
standards.
 Organics Extraction SOPs – All standards used must be listed (not just “surrogate” or
“spike”).
 All applicable SOPs – The SOPs do not clearly show how to prepare the Matrix Spike
(MS). This is required in order to show that it is being prepared and calculated properly.
 All applicable SOPs - Individual parameter and/or QC SOPs must include all calculation
formulas (e.g., percent recovery, Relative Percent Difference (RPD), etc.).
o Standard Operating Procedures (SOPs) have not been developed and/or updated for all of the
parameters included on the laboratory’s certificate attachment.
 BOD – The criteria for flagging Quality Control failures has not been updated in the BOD
SOP. A copy of the policy document titled “Flagging BOD Quality Control Requirements”
was provided to the laboratory at the time of the inspection.
 Ammonia Nitrogen – The laboratory does not have a SOP for Standard Methods 4500
NH3 D-1997.
 All applicable Parameters (Inorganics and Organics) – The laboratory does not have
an SOP for manual integration and manual integration is not addressed in individual
parameter SOPs.
 Organics – The laboratory did not have SOPs for EPA 602, EPA 624, EPA 625, SW -846
8015 C (TPH Diesel and Gas), SW -846 8082 A, Standard Methods 6200 B-1997, MADEP,
May 2004, Rev. 1.1 (EPH and VPH).
 Organics Extraction SOPs – The SOPs are inadequate. They only contain a procedure
section, but nothing more. A typical SOP contains the following sections: 1) revisions
tracking, 2) description, 3) precautions/interferences, 4) sample preservation, 5) apparatus,
6) standards/ reagents, 7) procedure, 8) quality control, 9) references.
o The SOPs do not define acceptance criteria for QC.
 Inorganic Phenols – Blank acceptance criterion is not defined.
 Inorganic Phenols – Reporting limit acceptance criterion is not defined.
 Cyanide – Blank acceptance criterion is not defined.
 Chlorophyll a – High and low standard acceptance criteria are not defined.
 Chlorophyll a – Calibration curve acceptance criterion is not defined.

Requirement: Each laboratory shall develop and maintain a document outlining the analytical quality control
practices used for the parameters included in their certification. Supporting records shall be maintained as
evidence that these practices are being effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7). Please
submit updated SOPs with the items listed above addressed by December 31, 2014.

D. Finding: Several benchsheets were noted that referenced the wrong method or had not been updated to
include the method reference year. The following errors were noted:

 Settleable Residue – The benchsheet did not include method approval year.
 Total Residue – The benchsheet references EPA 160.3, which has not been promulgated by EPA
in 40 CFR Part 136 since May, 2012. The laboratory is certified for SM 2540 B-1997.
 Dissolved Residue – The benchsheet references EPA 160.1, which has not been promulgated by
EPA in 40 CFR Part 136 since May, 2012. The laboratory is certified for SM 2540 C-1997.
 Ignitability – No method reference is listed.
 Fecal Coliform – The benchsheet references 18th Edition of Standard Methods, which has not been
promulgated by EPA in 40 CFR Part 136 since May, 2012. The laboratory is certified for SM 9222
D-1997.
 Ammonia Nitrogen – The benchsheet references SM 4500 NH3 F-1997. The laboratory is certified
for SM 4500 NH3 D-1997.
 Fluoride – The method code is not documented on the benchsheet.
 Orthophosphate – The benchsheet has a check box to indicate if it is used for Orthophosphate or
Total Phosphorus. Since Total Phosphorus is no longer analyzed by this method, the check boxes
should be removed.
 Conductivity – The benchsheet references EPA 120.1. The laboratory is certified for SM 2510 B-
1997.
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 MBAS – The benchsheet references 18th Edition of Standard Methods, which has not been
promulgated by EPA in 40 CFR Part 136 since May, 2012. The laboratory is certified for SM 5540
C-2000.
 Turbidity – The benchsheet references Standard Methods 2130. The laboratory is certified for EPA
Method 180.1, Rev. 2.0 (1993).
 Total Coliform - The laboratory uses the same benchsheet for Total Coliform and Fecal Coliform.
The analyst marks out “Fecal” and writes “Total”. But the reference method is not changed and is
incorrect when the benchsheet is used to document Total Coliform analyses.

Requirement: Each laboratory shall develop and maintain a document outlining the analytical quality control
practices used for the parameters included in their certification. Supporting records shall be maintained as
evidence that these practices are being effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).

Recommendation: It is recommended that all benchsheets be reviewed to ensure proper method
references.

E. Finding: Benchsheets do not include the following information:

 Chlorophyll a – True value, acceptance criteria, and percent recovery of high and low standards
 Chloride – True value of standards
 Chloride – Normality of NaCl
 Oil & Grease – True value of standards
 Oil & Grease – Documentation on the sample log only shows sample date and filter date. Time of
collection and filtration must be documented in order to demonstrate that the sample is filtered within
48 hours.

Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as
to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A).

Recommendation: It is recommended that all benchsheets be reviewed to ensure that the required
information is properly documented.

F. Finding: Data qualifiers are not consistently reported on client reports.

Requirement: When quality control (QC) failures occur, the laboratory must attempt to determine the source
of the problem and must apply corrective action. Part of the corrective action is notification to the end user. If
data qualifiers are used to qualify samples not meeting QC requirements, the data may not be useable for
the intended purposes. It is the responsibility of the laboratory to provide the client or end-user of the data
with sufficient information to determine the usability of the qualified data. Where applicable, a notation must
be made on the Discharge Monitoring Report (DMR) form, in the comment section or on a separate sheet
attached to the DMR form, when any required sample quality control does not meet specified criteria and
another sample cannot be obtained. Ref: NC WW/GW LC Policy.

Comment: Examples of this include:

 4/3/14 – Chloride, SM 4500 Cl- C-1997 – Duplicate RPD was 40%. The average was reported to the
client with no qualifier.
 4/3/14 – Purgeable Organics, SW -846 8260 B – laboratory contamination for Acetone and
Methylene Chloride.
 4/2/14 – Turbidity, EPA 180.1, Rev. 2.0 (1993) – no check standard was analyzed (see Finding Z
below).
 3/6/14, 3/13/14, and 3/24/14 – pH, Standard Methods, 4500 H B-2000 – check buffer standards
were not acceptable (for WWTP operations, see Finding IIII below).
 Metals - EPA Method 200.7 - Copper contamination appears consistently in blank analyses (see
Finding SSS below).

G. Finding: Uncertified data is not documented as such on the benchsheets or final reports.

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Requirement: All uncertified data must be clearly documented as such on the benchsheet and on the
final report. Ref: 15A NCAC 2H .0805 (e) (3).

Comment: For example, a sample was analyzed for Color by SM 2120 B-2001; however, the laboratory is
not certified for this method. This was not documented on the benchsheet or the final report. The Client
Report was work order 11201351 for Anson County WWTP (NPDES permit #NC0041408). The Color result
was not reported on the Discharge Monitoring Report (DMR).

H. Finding: A sample was analyzed by one method but reported as another.

Requirement: Each laboratory shall develop and maintain a document outlining the analytical quality control
practices used for the parameters included in their certification. Supporting records shall be maintained as
evidence that these practices are being effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).

Comment: The final lab report indicated that the ADMI Color sample was analyzed by SM 2120 B-2001, but
reported as SM 2120 E-2001 on the Client Report. The Client Report was work order 11201351 for Anson
County WWTP (NPDES permit #NC0041408). The Color result was not reported on the DMR.

I. Finding: Sample preservation, including temperature, pH, and dechlorination is not consistently checked and
documented when samples are received by the laboratory.

Requirement: A record of date collected, time collected, sample collector, and use of proper preservatives
must be maintained. Each sample must clearly indicate the State of North Carolina collection site on all
record transcriptions. Ref: 15A NCAC 2H .0805 (a) (7) (M).

Comment: This was noted on Chains of Custody dated 4/1/13, 9/5/13, 4/2/14, and 5/6/14.

J. Finding: Computer print outs (e.g., Inorganic Phenols) are missing units of measure for items such as
concentration, absorbance, and volume.

Requirement: All laboratories must use printed laboratory bench worksheets that include a space to enter
the signature or initials of the analyst, date of analyses, sample identification, volume of sample analyzed,
value from the measurement system, factor and final value to be reported and each item must be recorded
each time samples are analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (H).

K. Finding: Many benchsheets do not have the year recorded on them, only month and day.

Requirement: All laboratories must use printed laboratory bench worksheets that include a space to enter
the signature or initials of the analyst, date of analyses, sample identification, volume of sample analyzed,
value from the measurement system, factor and final value to be reported and each item must be recorded
each time samples are analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (H).

Comment: Most laboratory notebooks have the applicable dates contained in the notebook written on the
front cover in full month, day, and year format. Often only the month and day were documented on the
enclosed benchsheets. Individual benchsheets must be dated in day, month, and year format in case of
separation from the notebook.

L. Finding: Units of measure for temperature upon receipt are not documented.

Requirement: All laboratories must use printed laboratory bench worksheets that include a space to enter
the signature or initials of the analyst, date of analyses, sample identification, volume of sample analyzed,
value from the measurement system, factor and final value to be reported and each item must be recorded
each time samples are analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (H).

Comment: Although the Chain of Custody (CoC) is not a benchsheet, units of measure are required due to
this being the method of documenting proper preservation of samples.

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Quality Control

Recommendation: It is recommended that the laboratory implement a temperature grid check of all block
digesters by alternating the well location of the thermometer each time samples are digested. This will document
heating uniformity and consistency of all sample wells in the block.

M. Finding: Quality Control acceptance is not consistently evaluated (calculated) for acceptance.

Requirement: Each laboratory shall develop and maintain a document outlining the analytical quality control
practices used for the parameters included in their certification. Supporting records shall be maintained as
evidence that these practices are being effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).

Comment: The following parameters were noted as having QC that was not evaluated:

 Total Suspended Solids - Relative Percent Difference (RPD) of duplicates
 Chloride – RPD of duplicates and percent recovery of standard(s)
 Ammonia Nitrogen – Percent recovery of MS and RPD of MS duplicate (MSD)
 Nitrate + Nitrite Nitrogen - Percent recovery of MS and RPD of MS duplicate
 Total Kjeldahl Nitrogen - Percent recovery of MS and RPD of MS/MSD
 Oil and Grease – Percent recovery of standards
 Alkalinity – RPD of duplicates
 Inorganic Phenols – RPD of duplicates
 Cyanide – Percent recovery of standards and RPD of duplicates
 Chlorophyll a - Percent recovery of standards.

Recommendation: It is recommended that a Quality Control (QC) cover sheet be added to each data pack
to document whether QC meets acceptance criteria and to document that it has been reviewed and who
performed the review.

Proficiency Testing

N. Finding: The laboratory is not analyzing Proficiency Testing (PT) samples in the same manner as
environmental samples.

Requirement: All PT samples are to be analyzed and the results reported in a manner consistent with the
routine analysis and reporting requirements of compliance samples and any other samples analyzed
according to the requirements of 15A NCAC 2H .0800. Ref: Proficiency Testing Requirements, February 20,
2012, Revision 1.2.

Comment: The laboratory’s common practice was to analyze a known standard along with the PT sample as
additional quality control. Since this is not performed with all environmental samples, it is considered
additional quality control. However, known samples are recommended when analyzing remedial PT samples
as part of the troubleshooting and corrective action process.

O. Finding: The preparation of Proficiency Testing (PT) samples is not documented.

Requirement: PT samples received as ampules must be diluted according to the PT provider’s
instructions. The preparation of PT samples must be documented in a traceable log or other traceable
format. The diluted PT sample becomes a routine environmental sample and is added to a routine sample
batch for analysis. Ref: Proficiency Testing Requirements, February 20, 2012, Revision 1.2.

P. Finding: The laboratory does not have a documented plan for PT procedures.

Requirement: Each laboratory shall develop and maintain a document outlining the analytical quality control
practices used for the parameters included in their certification. Supporting records shall be maintained as
evidence that these practices are being effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).

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Requirement: Laboratories must have a documented plan (this is usually detailed in the laboratory’s Quality
Assurance Manual) of how they intend to cover the applicable program requirements for proficiency testing
per their scope of accreditation. This plan shall cover any commercially available proficiency testing and any
inter-laboratory organized studies, as applicable. The laboratory must also be able to explain when
proficiency testing is not possible for certain parameters and provide a description of what the laboratory is
doing in lieu of proficiency testing. This shall be detailed in the plan. The plan must also address the
laboratory’s process for submission of proficiency testing results and related corrective action responses.
Laboratory Standard Operating Procedures (SOPs) must address how low level samples will be analyzed,
including concentration of the sample or adjustment of the normality of a titrant. These instructions shall be
followed when the concentration of a PT sample falls below the range of their routine analytical method.
Instructions shall also be included in the laboratory’s SOP for how high level samples will be analyzed,
including preparation of multiple dilutions of the sample. These instructions will be followed when the
concentration of a PT falls above the range of their routine analytical method. Ref: Proficiency Testing
Requirements, February 20, 2012, Revision 1.2.

Q. Finding: The laboratory was not entering the PT samples into the sample tracking system as an
environmental sample.

Requirement: Laboratories shall conduct proficiency tests in accordance with their routine testing, calibration
and reporting procedures, unless otherwise specified in the instructions supplied by the PT provider. This
means that they are to be logged in and analyzed using the same staff, sample tracking systems, standard
operating procedures including the same equipment, reagents, calibration techniques, analytical methods
and preparatory techniques such as digestions, distillations and extractions. Ref: Proficiency Testing
Requirements, February 20, 2012, Revision 1.2.

Fecal Coliform – Standard Methods, 9222 D-1997

R. Finding: Samples that were read on 4/23/14 and 4/24/14 did not have a time samples were removed from
the incubator documented.

Requirement: The date and time BOD and coliform samples are removed from the incubator must be
included on the laboratory worksheet. Ref: 15A NCAC 2H .0805 (a) (7) (H).

Alkalinity – Standard Methods, 2320 B-1997

S. Finding: The titrant is not being standardized monthly.

Requirement: Re-standardize reagents once a month or when improper storage occurs. If the titration
reagent’s normality (titer value) has changed, then use the measured value, adjust the normality as the
procedure describes, or prepare and standardize fresh titration reagent as needed. Ref: Standard Methods,
2020 B-2010. (2) (b).

Settleable Residue – Standard Methods, 2540 F-1997

T. Finding: The 45 minute stir time is not documented.

Requirement: The following must be documented in indelible ink whenever sample analysis is performed:
45 minute stir time (use of a check box is acceptable). Ref: NC WW/GW LC Approved Procedure for the
Analysis of Settleable Solids.

U. Finding: The reporting limit is not adjusted when less than 1 L of sample is analyzed.

Requirement: Fill an Imhoff cone to the 1-L mark with a well-mixed sample…record volume of settleable
solids in the cone as milliliters per liter. Ref: Standard Methods, 2540 F-1997 (3) (a).

Comment: A sample was analyzed on 4/9/14 using 425 mL and reported as <1 ml/L. If there is not enough
sample volume, the reporting limit must be adjusted based on the volume used. In this case, the sample
result should have been reported as <2.4 ml/L.
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Suspended Residue – Standard Methods, 2540 D-1997

V. Finding: Filters are not weighed to constant weight prior to sample analysis, nor is a dry filter blank analyzed
with each set of samples.

Requirement: If pre-prepared filters are not used, the method requires that filters must be weighed to a
constant weight after washing. Repeat cycle of drying, cooling, desiccating, and weighing until a constant
weight is obtained or until weight change is less than 4% of the previous weighing or 0.5 mg, whichever is
less. In lieu of this process, it is acceptable to analyze a single daily dry filter blank to fulfill the method
requirement of drying all filters to a constant weight prior to analysis. Ref: North Carolina
Wastewater/Groundwater Laboratory Certification Policy.

Total Residue – Standard Methods, 2540 B-1997

W. Finding: Samples are not dried at 98 °C initially.

Requirement: When evaporating in a drying oven, lower temperature to approximately 2 °C below boiling to
prevent splattering. Ref: Standard Methods, 2540 B-1997. (3) (b).

X. Finding: Many instances of samples yielding more than 200 mg of dried residue were noted.

Requirement: Choose a sample volume that will yield residue between 2.5 and 200 mg. Ref: Standard
Methods, 2540 B-1997. (3) (b).

Comment: Excessive residue in the dish may form a water-trapping crust; subsequently imparting a high
bias to sample results.

Suspended Residue – Standard Methods, 2540 D-1997
Dissolved Residue – Standard Methods, 2540 C-1997

Y. Finding: A check standard is not analyzed quarterly.

Requirement: Analyze one suspended residue, one dissolved residue, one residual chlorine and one oil and
grease standard quarterly. Ref: 15A NCAC 2H .0805 (a) (7) (B).

Turbidity – EPA Method 180.1, Rev. 2.0 (1993)

Z. Finding: No standards were analyzed with samples on 4/2/14.

Requirement: Turbidimeter calibration: The manufacturer's operating instructions should be followed.
Measure standards on the turbidimeter covering the range of interest. If the instrument is already calibrated in
standard turbidity units, this procedure will check the accuracy of the calibration scales. At least one standard
should be run in each instrument range to be used. Ref: EPA Method 180.1, Rev. 2.0 (1993), Section 10.1.

Ignitability – SW-846 Method 1010 A

AA. Finding: The laboratory was not consistently recording the temperature of flash point.

Requirement: Record as the observed flash point the reading on the temperature measuring device at the
time ignition source application causes a distinct flash in the interior of the test cup. Ref: ASTM Method D 93-
80 Section 9.4 [SW -846 1010A].

Ignitability – SW-846 Method 1030

BB. Finding: Analysts signature or initials are not recorded on the benchsheet.

Requirement: All laboratories must use printed laboratory bench worksheets that include a space to enter
the signature or initials of the analyst. Ref: 15A NCAC 2H .0805 (a) (7) (H).
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CC. Finding: The laboratory is performing the test in a powder train mold prepared from aluminum foil.

Requirement: Apparatus and Materials: Low-heat conducting, non-combustible, impervious ceramic tile or
equivalent material, of approximate dimension of 25 cm X 25 cm X 2.5 cm (the tile must be at least 25 cm in
length to support a 250 mm test sample). Ref: SW -846 Method 1030, Section 4.1.

Requirement: Prepare the test material in its "as received" form by forming an unbroken strip or powder train
of sample 250 mm long by 20 mm wide by 10 mm high on the ceramic tile. Use the mold to form the material
as in 7.2.3 if appropriate. Ref: SW -846 Method 1030, Section 7.1.2.

Requirement: All tests for the burn rate test are performed on clean, ambient temperature, ceramic plates.
Ref: SW -846 Method 1030, Section 7.2.1.

BOD – Standard Methods, 5210 B-2001
BOD – Standard Methods, 5210 B-2001 (Hach 10360-2011, Rev. 1.2)

DD. Finding: The laboratory dedicates the same bottles to be used for blank analyses with each sample set.

Requirement: This dilution blank serves as a check on quality of unseeded dilution water and cleanliness of
incubation bottles. Ref: Standard Methods, 5210 B-2001. (6) (c).

Comment: The bottles used for the dilution water blank, seed blank, seed controls, and glucose-glutamic
acid (GGA) standard are never used for anything else (i.e., the bottle used for the dilution water blank is
always used for the dilution water blank, etc.). If nothing but dilution water is used in the same bottles each
time, the cleanliness of those bottles is never truly verified. Bottles must be randomly used for each purpose
in order to verify the presence/absence of any contamination issues.

EE. Finding: The seed correction was not correctly calculated on 4/16/2014.

Requirement: Determine BOD of the seed suspension as for any other sample. Ref: Standard Methods,
5210 B-2001. (6) (d).

Comment: When calculating the seed correction, the analyst was off by one line when determining the
Dissolved Oxygen depletions. This was the only instance of this noted in the data review and seemed to be
an anomaly. The seed correction was miscalculated to be 0.99 mg/L and was actually 1.23 mg/L when
calculated correctly. This caused all of the results to be reported greater than their actual values this day.

Recommendation: It is recommended that revised reports be sent for all samples affected by this error.

FF. Finding: The laboratory is not properly neutralizing chlorine in BOD samples.

Requirement: If residual chlorine is present, dechlorinate sample. Determine required volume of Na2SO3
solution on a 100- to 1000-mL portion of neutralized sample by adding 10 mL 1 + 1 acetic acid or 1 + 50
H2SO4, 10 mL potassium iodide (KI) solution (10 g /100mL) per 1000 mL sample and titr ating with Na2SO3
solution to the starch-iodine end point for residual. Add to neutralized sample the proportional volume of
Na2SO3 solution determined by the above test, mix, and after 10 to 20 min check sample for residual
chlorine. Ref: Standard Methods, 5210 B-2001. (4) (b) (2).

Comment: The laboratory was performing the titration as required. However, only 1 mL /100 mL of Na2SO3
was added to samples in order to avoid diluting the sample too much; even if more than 1 mL /100 mL of
Na2SO3 was required to neutralize the sample. Therefore, the chlorine was not fully neutralized in these
samples. In cases such as this, the laboratory is allowed to prepare a stronger concentration of Na2SO3 in
order to avoid excess dilution.

Recommendation: It is OK to prescreen samples visually with DPD powder. If no pink color is present;
document as no chlorine present. If pink color is present; sample aliquot must be titrated per method. TRC
test strips may be used for samples where interference with DPD precludes their use. Since dechlorination is
required for most NC wastewater facilities, there should rarely be any chlorine in samples. The method
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required titration may be showing other oxidizing agents which are not required to be neutralized.
Prescreening samples in this manner will show which samples truly have chlorine. The document titled
“Neutralizing Total Residual Chlorine in BOD Samples” was provided to the laboratory at the time of the
inspection, which more fully describes this process.

GG. Finding: The laboratory is not documenting the time that samples are put in the incubator in such a manner
that shows that the holding time is met and that they are incubated for five days ± six hours.

Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as
to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A).

Requirement: Biochemical Oxygen Demand. Maximum holding time: 48 hours. Ref: Code of Federal
Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012; Table II.

Requirement: After 5 d ± 6 h of incubation, determine DO in all sample dilutions, and in all blanks and
checks as in 5210B.6b-d. Ref: Standard Methods, 5210 B-2001. (5) (i).

Comment: The laboratory documents the time that BOD analyses begin and the time that the last of the
samples are put in the incubator. For example, on 4/21/14, the benchsheet indicates that samples were set
up at 8:00 AM and in put in the incubator at 7:35 PM. This creates the appearance that the BOD bottles were
left out all day, but the analyst stated that this was not the case. In order to demonstrate compliance with the
holding time and method requirements, document when each set of bottles are placed in the incubator.
Additionally, the holding time is not met by beginning analysis, but rather by putting the BOD bottles in the
incubator within 48 hours of collection.

HH. Finding: The laboratory is not setting three dilutions for all samples and the GGA standard.

Requirement: Using the dilution water prepared as in ¶ a above, make at least three dilutions of prepared
sample estimated to produce a residual DO of at least 1.0 mg/L and a DO uptake of at least 2.0 mg/L after a
5-d incubation. Five dilutions are recommended if experience with a particular sample does not produce at
least three bottles having acceptable minimum DO depletions and residual limits (5210B.6a). Ref: Standard
Methods, 5210 B-2001. (5) (c).

Requirement: Together with each batch of samples, check seed effectiveness and analytical technique by
using procedures in 5210B. (5) to make measurements on an equal weight mixture of glucose and glutamic
acid. Ref: Standard Methods, 5210 B-2001. (6) (b).

II. Finding: The initial DO readings are sometimes greater than 9 mg/L.

Requirement: The working range is equal to the difference between the maximum initial DO (7 to 9 mg/L)
and the minimum DO residual of 1 mg/L corrected for seed, and multiplied by the dilution factor. Ref:
Standard Methods, 5210 B-2001. (8) (b).

Requirement: Samples supersaturated with DO – Samples containing DO concentration above saturation at
20 °C may be encountered in cold waters or in water where photosynthesis occurs. To prevent loss of
oxygen during incubation of such samples, reduce DO to saturation by bringing sample to about 20 ± 3 °C in
partially filed bottle while agitating by vigorous shaking or by aerating with clean, filtered compressed air. Ref:
Standard Methods, 5210 B-2001. (4) (b) (4).

JJ. Finding: Sample results are not flagged when the blank is >0.20 mg/L.

Requirement: Identify results in the test reports when any of the following quality control parameters are not
met: Dilution water blank exceeds 0.20 mg/L (5210B.6c). Ref: Standard Methods, 5210 B-2001. (7) (b).

KK. Finding: Sample pH adjustment is not being correctly performed.

Requirement: All samples – Check pH; if it is not between 6.0 and 8.0, adjust sample temperature to 20 ± 3
°C, then adjust pH to 7.0 to 7.2 using a solution of sulfuric acid (H2SO4) or sodium hydroxide (NaOH) of such
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strength that the quantity of reagent does not dilute the sample by more than 0.5%. Ref: Standard Methods,
5210 B-2001. (4) (b) (1).

Comment: For example: sample 042372 was adjusted from 8.53 Standard Units (S.U.) to 7.45 S.U., sample
042373 was adjusted from 8.19 S.U. to 6.83 S.U., sample 032011 was adjusted from 4.83 S.U. to 6.05 S.U.,
and sample 032023 was adjusted from 9.39 S.U. to 6.38 S.U.

MBAS – Standard Methods, 5540 C-2000

Comment: The SOP states that the correlation coefficient must be >0.995. While this is acceptable, Standard
Methods allows the correlation coefficient to be ≥0.995.

Recommendation: It is recommended that the benchsheet column header labeled “dilution” be relabeled as “dilution
factor” to clarify how the number is used to determine the final sample concentration.

LL. Finding: Standards are not consistently treated in the same manner as samples.

Requirement: Process the Laboratory Fortified Blank (LFB) through all sample preparation and analysis
steps. Ref: Standard Methods, 1020 B-2011. (6).

Requirement: Excessive agitation may cause emulsions formation. To break persistent emulsions add a
small volume of isopropyl alcohol (<10 mL); add same volume of isopropyl alcohol to all standards. Ref:
Standard Methods, 5540 C-2000. (4) (d) (2).

Comment: Isopropyl alcohol is added to some samples in order to break up emulsions. When this is done,
isopropyl alcohol is also added to standards. However, when an analytical batch contains samples without
isopropyl alcohol added, a corresponding standard is not analyzed without isopropyl alcohol added. If an
analytical batch has samples with and without isopropyl alcohol added to samples, standards must be
analyzed both with and without isopropyl alcohol added.

MM. Finding: There was no evidence to indicate that a new curve is prepared for each new lot of LAS stock.

Requirement: For analytical procedures requiring analysis of a series of standards, the concentrations of
these standards must bracket the concentration of the samples analyzed. The curve must be updated as set
forth in the standard procedures, each time the slope changes by more than 10 percent at mid-range, each
time a new stock standard is prepared, or at least every twelve months. Each analyst performing the
analytical procedure must produce a standard curve. Ref: 15A NCAC 2H .0805 (a) (7) (I).

Comment: The SOP does not indicate that a new curve is prepared for each new lot number of LAS stock
and this is not able to be confirmed due to a lack of traceability. See Finding A.

NN. Finding: Results are not reported in terms of LAS molecular weight on the benchsheet or final reports.

Requirement: Report as “MBAS, calculated as LAS, mol wt ____.” Ref: Standard Methods, 5540 C-2000.
(5).

OO. Finding: Units of measure for absorbance (i.e., nm) are not documented on the benchsheet.

Requirement: All laboratories must use printed laboratory bench worksheets that include a space to enter
the signature or initials of the analyst, date of analyses, sample identification, volume of sample analyzed,
value from the measurement system, factor and final value to be reported and each item must be recorded
each time samples are analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (H).

PP. Finding: Recent benchsheets (for example 4/30/14) were not fully filled out.

Requirement: Each laboratory shall develop and maintain a document outlining the analytical quality control
practices used for the parameters included in their certification. Supporting records shall be maintained as
evidence that these practices are being effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).
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Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as
to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A).

Comment: Undocumented information included curve date, time analyzed, sample volume, percent recovery
of standards, and RPD of duplicates.

Inorganic Phenols – EPA Method 420.1 (Rev. 1978)

Recommendation: Some samples were crossed out on the distillation log and an absorbance was not recorded. It
was determined that these were redistilled and analyzed due to being above the range of the curve and needing to be
diluted. In cases such as this, the absorbance obtained should be documented and a note added to explain why the
sample was redistilled.

QQ. Finding: The initial and final dilution volumes are not documented on the distillation log in order to determine
the dilution factor correctly.

Requirement: All laboratories must use printed laboratory bench worksheets that include a space to enter
the signature or initials of the analyst, date of analyses, sample identification, volume of sample analyzed,
value from the measurement system, factor and final value to be reported and each item must be recorded
each time samples are analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (H).

Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as
to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A).

RR. Finding: The method blank is not distilled.

Requirement: If the method lacks QA/QC procedures…refer to the appropriate QA/QC section(s) of an
approved Part 136 method from a consensus organization compendium. Ref: Code of Federal Regulations,
Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012, 136.7 (b).

Requirement: A reagent blank (method blank) consists of reagent water (see Section 1080) and all reagents
(including preservatives) that normally are in contact with a sample during the entire analytical procedure.
Ref: Standard Methods, 1020 B-2011. (5).

MBAS – Standard Methods, 5540 C-2000
Inorganic Phenols – EPA Method 420.1 (Rev. 1978)

SS. Finding: Data was not in sequential order in the bound notebooks.

Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as
to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A).

Requirement: Each laboratory shall develop and maintain a document outlining the analytical quality control
practices used for the parameters included in their certification. Supporting records shall be maintained as
evidence that these practices are being effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).

Comment: For example, the order of dates in the bound MBAS notebook was 4/30/14, 5/3/14, 5/2/14, and
5/7/14. The order of dates in the bound Phenols notebook was 4/29/14, 5/6/14, and 4/13/14. Additionally, the
Phenols distillation log was not always in sequential order. For example, 5/13/14 is before 5/8/14. Analyses
recorded in this manner may give the appearance of fraudulent results.

Recommendation: The analyst indicated that the pages were not in sequential order due to accidentally
skipping pages and then going back to them to use for later analytical batches. If a page is accidentally
skipped, it is recommended that the analyst mark through the blank page in a “z” pattern, initial and date it,
and not use the page for analytical results in order to keep the analyses in sequential order and avoid any
perception of improper practices.

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Cyanide – EPA Method 335.4, Rev. 1.0 (1993)

Comment: The SOP requires samples to be preserved to pH >12. The Federal Register has updated the pH
preservation criterion to pH >10. While the older criterion is still acceptable, the lower pH requirement may be
implemented.

TT. Finding: Calibration standards are not analyzed in descending order.

Requirement: Place appropriate standards in the sampler in order of decreasing concentration and perform
analysis. Ref: EPA Method 335.4, Rev. 1.0 (1993), Section 10.5.

Comment: Please note that SW -846 9012 B requires calibration standards to be analyzed in ascending
order.

Cyanide – EPA Method 335.4, Rev. 1.0 (1993)
Cyanide – SW-846 9012 B

Recommendation: Dilution factor is not documented on the benchsheet. It is recommended the benchsheet be
updated to include this.

UU. Finding: Analyst initials are not documented on the Cyanide printouts, sequence log, reading log, and curve
print outs.

Requirement: All laboratories must use printed laboratory bench worksheets that include a space to enter
the signature or initials of the analyst. Ref: 15A NCAC 2H .0805 (a) (7) (H).

Chloride – Standard Methods, 4500 Cl- C-1997

VV. Finding: The normality of the mercuric nitrate was not correctly calculated on 5/15/14.

Requirement: Calculation.

mg Cl-/L = (A-B) x N x 35450
mL sample

where:

A = mL titration for sample,
B = mL titration for blank, and
N = normality of Hg(NO3)2.

Ref: Standard Methods, 4500 Cl- C-1997 (5).

Comment: The normality was incorrectly calculated to be 0.0138 N, but was actually 0.0144 N. Since this
data was analyzed so recently, the laboratory stated that they would recalculate the results before reporting
any of the data.

WW. Finding: A Laboratory Fortified Matrix (LFM) and LFM Duplicate (LFMD), also known as Matrix Spike (MS)
and MS Duplicate (MSD), are not analyzed with each set of samples.

Requirement: When appropriate for the analyte (Table 4020:I), include at least one LFM/LFMD daily or with
each batch of 20 or fewer samples. Ref: Standard Methods, 4020 B-2009 (2) (g).

Requirement: LFM and LFMD analyses are required. Ref: Standard Methods, 4020 B-2009, Table 4020:I.

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Ammonia Nitrogen – Standard Methods, 4500 NH3 D-1997

Recommendation: The benchsheet is confusing when dilutions are made. It is recommended that the dilution
column be moved in front of the concentration column since the concentration is the final concentration after applying
the dilution factor.

XX. Finding: The result of the blank is not being converted from millivolts to mg/L on the benchsheet to
determine acceptance.

Requirement: For analyses requiring a calibration curve, the concentration of reagent, method and
calibration blanks must not exceed 50% of the reporting limit or as otherwise specified by the reference
method. Ref: NC WW/GW LC Policy.

Requirement: Each laboratory shall develop and maintain a document outlining the analytical quality control
practices used for the parameters included in their certification. Supporting records shall be maintained as
evidence that these practices are being effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).

Comment: The result of the blank is being recorded in millivolts.

YY. Finding: The volume of 10N NaOH used in the samples and calibration standards was not documented
on the benchsheet.

Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as
to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A).

Comment: When the volume of 10N NaOH used for the samples is different than that used for the
calibration standards this must be compensated for in the calculation.

Comment: A statement may be added to the benchsheet that “unless otherwise noted, 1 mL of NaOH is
added to all samples and standards” to fulfill this requirement.

ZZ. Finding: The laboratory does not document that the pH is raised to >11 S.U. This is considered pertinent
information.

Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as
to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A).

Ammonia Nitrogen – EPA Method 350.1, Rev. 2.0 (1993)
Ammonia Nitrogen – Standard Methods 4500 NH3 D-1997

Recommendation: It is recommended that the laboratory compile distilled vs. non-distilled data in order to more
easily show that the required comparison studies have been performed.

Total Kjeldahl Nitrogen – EPA 351.2, Rev. 2.0 (1993)

AAA. Finding: Digestion times are not documented.

Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as
to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A).

Requirement: Place tubes in block digestor preheated to 160 °C and maintain temperature for one hour.
Reset temperature to 380 °C and continue to heat for one and one half hour. (380 °C must be maintained for
30 minutes). Ref: EPA 351.2, Rev. 2.0 (1993), Sections 11.4 and 11.5.

Comment: Due to the digestion requiring two different temperatures with different time requirements it is
necessary to document all start and end times to show method requirement is met.

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Ammonia Nitrogen – EPA Method 350.1, Rev. 2.0 (1993)
Ammonia Nitrogen – Standard Methods 4500 NH3 D-1997
Total Kjeldahl Nitrogen – EPA 351.2, Rev. 2.0 (1993)
Nitrate + Nitrite – EPA 353.2, Rev. 2.0 (1993)

BBB. Finding: For low level nutrient samples analyzed for the Monitoring Coalition, the laboratory analyzes one
Matrix Spike with each batch of samples, even when the sample batch includes more than 20 samples.

Requirement: Unless the referenced method states a greater frequency, spike 5% of samples on a
monthly basis. Laboratories analyzing less than 20 samples per month must analyze at least one matrix
spike each month samples are analyzed. Ref: NC WW/GW LC Policy.

Orthophosphate – Standard Methods, 4500 P E-1999

CCC. Finding: The computer printouts do not include analyst initials.

Requirement: All laboratories must use printed laboratory bench worksheets that include a space to enter
the signature or initials of the analyst. Ref: 15A NCAC 2H .0805 (a) (7) (H).

Total Organic Carbon – Standard Methods 5310 C-2000

Recommendation: It is recommended that the laboratory maintain the certificate of analysis that is provided with
each lot number of purchased sample bottles for traceability.

DDD. Finding: An inorganic carbon standard is not analyzed to check for removal of inorganic carbon.

Requirement: Check efficiency of inorganic carbon removal for each sample matrix by splitting a sample into
two portions; to one of the portions, add inorganic carbon to a level similar to that of the sample. The TOC
values should agree. If the values do not agree, adjust conditions such as sample container, sample volume,
pH, purge-gas flow rate, and purge time to obtain complete removal of inorganic carbon. Ref: Standard
Methods, 5310 C-2000. (4) (b).

Sulfate – SW-846 Method 9038
Sulfide – Standard Methods, 4500 S2- D-2000

EEE. Finding: Blank concentrations are not consistently documented.

Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as
to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A).

Requirement: For analyses requiring a calibration curve, the concentration of reagent, method and
calibration blanks must not exceed 50% of the reporting limit or as otherwise specified by the reference
method. Ref: NC WW/GW LC Policy.

Inorganic Phenols – EPA Method 420.1 (Rev. 1978)
Sulfide – Standard Methods, 4500 S2- D-2000

FFF. Finding: A second source standard is not analyzed whenever a new initial calibration curve is prepared.

Requirement: If the method lacks QA/QC procedures…refer to the appropriate QA/QC section(s) of an
approved Part 136 method from a consensus organization compendium. Ref: Code of Federal Regulations,
Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012, 136.7 (b).

Requirement: If the LFB is not prepared from second source to confirm method accuracy, the laboratory
must also verify the accuracy of its standard preparation by analyzing a mid-level second-source calibration
standard whenever a new initial calibration curve is prepared. Results must agree within 15%, unless
otherwise specified in a method. Ref: Standard Methods, 4020 B-2011. (2) (b).

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Sulfate – SW-846 Method 9038

GGG. Finding: An independently prepared check standard is not analyzed every 15 samples.

Requirement: Verify calibration with an independently prepared check standard every 15 samples. Ref: SW-
846 Method 9038, Section 8.5.

Fluoride – Standard Methods, 4500 F- C-1997

HHH. Finding: The laboratory has not performed a comparison of distilled vs. non-distilled samples.

Requirement: Manual distillation is not required if comparability data on representative effluent samples are
on file to show that this preliminary distillation step is not necessary: however, manual distillation will be
required to resolve any controversies. In general, the analytical method should be consulted regarding the
need for distillation. If the method is not clear, the laboratory may compare a minimum of 9 different sample
matrices to evaluate the need for distillation. For each matrix, a matrix spike and matrix spike duplicate are
analyzed both with and without the distillation step. (A total of 36 samples, assuming 9 matrices). If results
are comparable, the laboratory may dispense with the distillation step for future analysis. Comparable is
defined as <20% RPD for all tested matrices). Alternatively the two populations of spike recovery
percentages may be compared using a recognized statistical test. Ref: Code of Federal Regulations, Title 40,
Part 136; Federal Register Vol. 77, No. 97, May 18, 2012; Table IB Footnote 6. Please submit a distillation
comparison study summary with the response to this report.

Oil and Grease – EPA 1664 Rev. B

Recommendation: It is recommended that the nomenclature used in the method be used on benchsheets and
SOPs for Initial Precision and Recovery (IPR) standards and Ongoing Precision and Recovery (OPR) standards. The
laboratory currently calls the daily standard an IPR, but it is an OPR by method definition.

III. Finding: A blank appears to be analyzed, but results are not documented on the benchsheet and no flask
identification is recorded on the benchsheet.

Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as
to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A).

Requirement: Extract and concentrate a laboratory reagent water blank initially (i.e. with the tests in Section
9.2) and with each analytical batch. The blank must be subjected to the same procedural steps as a sample.
Ref: EPA Method 1664 Rev. B, Section 9.4.1.

JJJ. Finding: The laboratory uses various concentrations for the OPR standard (10, 20, and 40 mg/L).

Requirement: Precision and recovery (PAR) standard - Using a pipet, spike 10.0 ± 0.1 mL of the
hexadecane/ stearic acid spiking solution (Section 7.10) into 950 - 1050 mL of reagent water to produce
concentrations of approximately 20 mg/L each of hexadecane and stearic acid. The PAR standard is used
for the determination of initial (Section 9.2.2) and ongoing (Section 9.6) precision and recovery. Ref: EPA
Method 1664 Rev. B, Section 7.11.

KKK. Finding: The method required weights are not being checked for the balance.

Requirement: Calibrate the analytical balance at 2 mg and 1000 mg, using class “S” or ASTM E 617-1997
Class 1 weights. It is recommended that the balance should also be calibrated with an additional class “S” or
ASTM E 617-1997 Class 1 weight that will bracket the final expected weighing value. Ref: EPA Method 1664
Rev. B, Section 10.1.

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Chloride – Standard Methods, 4500 Cl- C-1997
COD – EPA Method 410.4, Rev. 2.0 (1993)
Cyanide – EPA Method 335.4, Rev. 10.0 (1993)
Cyanide – SW-846 9012 B (Total)
Fluoride – Standard Methods, 4500 F- C-1997
Inorganic Phenols – EPA Method 420.1 (Rev. 1978)
Oil and Grease – EPA 1664 Rev. B
Orthophosphate – Standard Methods, 4500 P E-1999
Sulfate – SW-846 Method 9038
Sulfide – Standard Methods, 4500 S D-2000

LLL. Finding: Matrix Spike (MS) analyses are not performed.

Requirement: Unless the referenced method states a greater frequency, spike 5% of samples on a
monthly basis. Laboratories analyzing less than 20 samples per month must analyze at least one matrix
spike each month samples are analyzed. Ref: NC WW/GW LC Policy.

Ammonia Nitrogen – Standard Methods, 4500 NH3 D-1997
Chloride – Standard Methods, 4500 Cl- C-1997
COD – EPA Method 410.4, Rev. 2.0 (1993)
Fluoride – Standard Methods, 4500 F- C-1997
Inorganic Phenols – EPA Method 420.1 (Rev. 1978)
MBAS – Standard Methods, 5540 C-2000
Mercury – EPA Method 245.1, Rev. 3.0 (1994)
Sulfate – SW-846 Method 9038
Sulfide – Standard Methods, 4500 S D-2000
Purgeable Organics – EPA Method 624
Purgeable Organics – SW-846 8260 B
Purgeable Organics – Standard Methods, 6200 B-1997
Polychlorinated Biphenyls (PCBs) – SW-846 8082 A
Extractable Petroleum Hydrocarbons – MADEP, May 2004, Rev. 1.1
Volatile Petroleum Hydrocarbons – MADEP, May 2004, Rev. 1.1

MMM. Finding: A blank and/or calibration verification standard are not analyzed after every tenth sample and/or at
the end of each sample group.

Requirement: The calibration blank and calibration verification standard (mid-range) must be analyzed
initially (i.e., prior to sample analysis), after every tenth sample and at the end of each sample group to
check for carry over and calibration drift. If either fall outside established quality control acceptance
criteria, corrective action must be taken (e.g., repeating sample determinations since the last acceptable
calibration verification, repeating the initial calibration, etc.). Ref: NC WW/GW LC Policy.

Chlorophyll a – EPA Method 445.0, Rev. 1.2 (Fluorometric)

Recommendation: Samples filtered on 10/23/13, 11/1/13, 12/19/13, and 12/20/13 had no sample collection date
recorded on the log sheet; however, the collection date was documented on the Chain of Custody form. It is
recommended that the sample collection date be consistently documented on the log sheet.

NNN. Finding: The standard curve is not updated every 12 months.

Requirement: For analytical procedures requiring analysis of a series of standards, the concentrations of
these standards must bracket the concentration of the samples analyzed. The curve must be updated as set
forth in the standard procedures, each time the slope changes by more than 10 percent at mid-range, each
time a new stock standard is prepared, or at least every twelve months. Each analyst performing the
analytical procedure must produce a standard curve. Ref: 15A NCAC 2H .0805 (a) (7) (I).

Requirement: Analytical Quality Control Program. Each laboratory shall develop and maintain a document
outlining the analytical quality control practices used for the parameters included in their certification.
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Supporting records shall be maintained as evidence that these practices are being effectively carried out.
Ref: 15A NCAC 2H .0805 (a) (7).

Comment: The SOP states that a new curve is prepared every six months or more frequently, but the curves
in the log book are approximately 13 months apart. The most recent curve was prepared 9/3/13.

Recommendation: Since Chlorophyll a samples are generally submitted during the summer months, it is
recommended that a new calibration curve be prepared when sampling begins rather than rely on a much
older curve.

OOO. Finding: The vacuum pressure of the filtration is not documented.

Requirement: Assemble the filtration apparatus and attach the vacuum source with vacuum gauge and
regulator. Vacuum filtration should not exceed 6 in. Hg (20 kPa). Higher filtration pressures and excessively
long filtration times (>10 min) may damage cells and result in loss of chlorophyll. Ref: EPA Method 445.0,
Rev. 1.2, Section 8.1.

Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as
to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A).

Mercury – EPA Method 1631 E

PPP. Finding: The lab is not subtracting the mean peak height or area of the bubbler blanks from the peak height
or area for each standard.

Requirement: For each calibration point, subtract the mean peak height or area of the bubbler blanks from
the peak height or area for each standard. Calculate the calibration factor (CFx) for Hg in each of the five
standards using the mean bubbler-blank subtracted peak height or area. Ref: EPA Method 1631 E, Section
10.2.2.4.

QQQ. Finding: The laboratory is not analyzing equipment blanks.

Requirement: Equipment blanks—Before any sampling equipment is used at a given site, the laboratory or
cleaning facility is required to generate equipment blanks on all sampling equipment that will be used to
demonstrate that the sampling equipment is free from contamination. Ref: EPA Method 1631 E, Section
9.4.6.

Metals – EPA Method 200.7, Rev. 4.4 (1994)

RRR. Finding: The laboratory’s acceptance criterion of the method blank is “less than the reporting limit”.

Requirement: For analyses requiring a calibration curve, the concentration of reagent, method an d
calibration blanks must not exceed 50% of the reporting limit or as otherwise specified by the reference
method. Ref: NC WW/GW LC Policy.

SSS. Finding: The rinse blank does not appear to be used for an adequate amount of time for copper.

Requirement: Memory interferences result when analytes in a previous sample contribute to the signals
measured in a new sample. Memory effects can result from sample deposition on the uptake tubing to the
nebulizer, and from the buildup of sample material in the plasma torch and spray chamber. The site where
these effects occur is dependent on the element and can be minimized by flushing the system with a rinse
blank between samples (Section 7.10.4). The possibility of memory interferences should be recognized
within an analytical run and suitable rinse times should be used to reduce them. The rinse times necessary
for a particular element must be estimated prior to analysis. This may be achieved by aspirating a standard
containing elements corresponding to either their LDR or a concentration ten times those usually
encountered. The aspiration time should be the same as a normal sample analysis period, followed by
analysis of the rinse blank at designated intervals. The length of time required to reduce analyte signals to
within a factor of two of the method detection limit, should be noted. Until the required rinse time is
established, this method requires a rinse period of at least 60 seconds between samples and standards. If a
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memory interference is suspected, the sample must be reanalyzed after a long rinse period. Ref: EPA
Method 200.7, Rev. 4.4 (1994), Section 4.4.

Comment: Copper contamination above the NC WW/GW LC Policy criterion of <50 % of the reporting limit
appears consistently in blank analyses. Sample results are not qualified when this happens. The laboratory
may also need to assess whether the reporting limit for copper has been established at a concentration that
is not achievable or whether the reagent water is not of adequate purity to support the current reporting level.

TTT. Finding: The upper limit of the Linear Dynamic Range has not been established.

Requirement: Linear dynamic range (LDR) - The upper limit of the LDR must be established for each
wavelength utilized. It must be determined from a linear calibration prepared in the normal manner using the
established analytical operating procedure for the instrument. The LDR should be determined by analyzing
succeedingly higher standard concentrations of the analyte until the observed analyte concentration is no
more than 10% below the stated concentration of the standard. Determined LDRs must be documented and
kept on file. The LDR which may be used for the analysis of samples should be judged by the analyst from
the resulting data. Determined sample analyte concentrations that are greater than 90% of the determined
upper LDR limit must be diluted and reanalyzed. The LDRs should be verified annually or whenever, in the
judgment of the analyst, a change in analytical performance caused by either a change in instrum ent
hardware or operating conditions would dictate they be redetermined. Ref: EPA Method 200.7, Rev. 4.4
(1994), Section 9.2.2.

UUU. Finding: The laboratory only dilutes samples that are >10% above the highest calibration standard.

Requirement: For analytical procedures requiring analysis of a series of standards, the concentrations of
these standards must bracket the concentration of the samples analyzed. Ref: 15A NCAC 2H .0805 (a) (7)
(I).

Metals – EPA Method 200.8, Rev. 5.4 (1994)

Comment: The metals digestion log references EPA Method 200.7 and several methods for which the laboratory is
not certified, but does not reference EPA Method 200.8.

Comment: The generic digestion log has a “log #”, but the corresponding log calls it a “run #”.

VVV. Finding: The laboratory is using concentrated HCl and HNO3 for sample digestion.

Requirement: Add 2 mL (1+1) nitric acid and 1.0 mL of (1+1) hydrochloric acid to the beaker containing the
measured volume of sample. Ref: EPA Method 200.8, Rev. 5.4 (1994), Section 11.2.3.

WWW. Finding: The correlation coefficient is not documented with the calibration curve. This is considered pertinent
information.

Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as
to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A).

Purgeable Organics – Standard Methods, 6200 B-1997

XXX. Finding: A Matrix Spike Duplicate (MSD) (also known as Laboratory Fortified Matrix Duplicate or LFMD) is
not analyzed.

Requirement: Prepare at least one LFM/LFMD each day samples are prepared or with each preparation
batch of 20 or fewer samples. Ref: Standard Methods, 6020 B-2011. (2) (f) and Table 6020 I.

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Purgeable Organics – EPA Method 624
Purgeable Organics – SW-846 8260 B
Purgeable Organics – Standard Methods, 6200 B-1997

YYY. Finding: Non-aqueous blanks are spiked with calibration standards, extracted and subsequently analyzed as
a calibration curve for non-aqueous samples.

Requirement: Prepare at least five concentration levels for each compound by adding appropriate amounts
of secondary standard solution to reagent water and inverting water sample twice. Ref: Standard Methods,
6200 B-1997. (3) (j).

Requirement: The following are the recommended gas volumes spiked into 5 mL of water to produce a
typical 5-point calibration… Ref: SW -846 8260B. 5.7.6.10.

Requirement: The following are the recommended gas volumes spiked into 25 mL of water to produce a
typical 5-point calibration… Ref: SW -846 8260B. 5.7.6.11.

Requirement: Prepare calibration standards at a minimum of three concentration levels for each parameter
by carefully adding 20.0 L of one or more secondary dilution standards to 50 mL, 250 mL, or 500 mL or
reagent water. Ref: EPA Method 624. 7.3.1.

Comment: A calibration curve is always aqueous from start to finish. After a non-aqueous sample is
extracted to a liquid form, it is an aqueous sample; and is to be treated as such. The purpose of the surrogate
spike in the extraction is to verify this matrix conversion.

Comment: If multiple methods are analyzed as a combined run, the most stringent QC criteria must be
followed.

Extractable Petroleum Hydrocarbons – MADEP, EPH, May 2004, Rev. 1.1
Volatile Petroleum Hydrocarbons – MADEP, VPH, May 2004, Rev. 1.1

Comment: The laboratory did not have a copy of the approved method. A copy was provided to the laboratory at the
time of the inspection.

Extractable Petroleum Hydrocarbons – MADEP, May 2004, Rev. 1.1

ZZZ. Finding: The extraction log did not have a date for fractionation of the samples.

Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as
to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A).

AAAA. Finding: The percent difference of the lowest calibration point was regularly unacceptable.

Requirement: At a minimum, the calibration factor must be verified on each working day, after every 20
samples or every 24 hours (whichever is more frequent), and at the end of the analytical sequence by the
injection of a mid-level continuing calibration standard to verify instrument performance. If the percent
difference (%D) for any analyte varies from the predicted response by more than ±25%, as determined using
Equation 4, a new five-point calibration must be performed for that analyte. Ref: MADEP, May 2004, Rev.
1.1, Section 9.7.2.5.

Comment: The percent difference regularly exceeded > 25% and sometimes up to 200%.

BBBB. Finding: The laboratory is not using an approved EPH soil/sediment extraction method.

Requirement: Approved EPH Extraction Methods: 3540C - Soil/Sediment - Soxhlet Extraction, 3541 -
Soil/Sediment - Automated Soxhlet Extraction, 3545A - Soil/Sediment - Pressurized Fluid Extraction (PFE),
3546 - Soil/Sediment - Microwave Extraction, 3570 - Soil/Sediment - Microscale Solvent Extraction (MSE),
3550C - Contaminated Solids* - Ultrasonic Extraction. * Sonication may only be used for the extraction of
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highly contaminated (free product) non-soil/sediments (debris). Any other use of ultrasonic extraction is
considered a “significant modification” of the EPH Method. Ref: MADEP, May 2004, Rev. 1.1, Table 4.

Comment: The laboratory uses a modified version of the soil/sediment extraction process from the MADEP
VPH method, substituting acetone for methanol.

Comment: The complete list of approved EPH extraction procedures for water and soil/sediment samples is
presented in Table 4. Alternative extraction procedures other than those listed are acceptable, provided that
the laboratory can document acceptable matrix- and petroleum product-specific performance. However, use
of an alternative extraction procedure is considered a “significant modification” of the EPH method pursuant
to Section 11.3.1.1 and as such would preclude obtaining “presumptive certainty” status for any analytical
data produced using an alternative EPH extraction procedure. Ref: MADEP, May 2004, Rev. 1.1, Section 9.1.

Comment: Any method modification approval must come from the data receiving agency (i.e., the Division of
Waste Management, UST Section).

CCCC. Finding: Units of measure were not documented on the EPH extraction log in the column for fractionation.

Requirement: All laboratories must use printed laboratory bench worksheets that include a space to enter
the signature or initials of the analyst, date of analyses, sample identification, volume of sample analyzed,
value from the measurement system, factor and final value to be reported and each item must be recorded
each time samples are analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (H).

Field Parameters

Comment: The laboratory performs two types of field parameter analyses. They have one certified WWTP operator
that operates Crown MHP (NPDES permit #NC0055255), Burlington Mfg. Services (NPDES permit #NC0001384),
Cornerstone Conference Center (NPDES permit #NC0046809), Stone Highway (NPDES permit #NC0060623), Quail
Acres (NPDES permit #NC0059251), Countryside Manor (NPDES permit #NC0073571), and Haw River Park
(NPDES permit #NC0046019). Other laboratory employees collect river basin samples for the North Carolina
Monitoring Coalition Program. The WWTP operator and Monitoring Coalition samplers use different benchsheets.
The Findings for Field Parameters will individually indicate to which category they apply (i.e., NPDES or Monitoring
Coalition).

Comment: The laboratory was not using the proper equipment for Total Residual Chlorine analyses. The North
Carolina Administrative Code, 15A NCAC 2H .0805 (a) (6) (H) states: Facilities and equipment. Each laboratory
requesting certification must contain or be equipped with the following: Glassware, chemicals, supplies, and
equipment required to perform all analytical procedures included in their certification. A Division letter dated August
14, 2001 states: “This letter serves as notification to facilities with effluent permit limits for Total Residual Chlorine
(TRC) that effective July 1, 2002, the Division of Water Quality expects these facilities to utilize an instrument or
method that will detect and measure TRC concentrations to levels that are below the permit discharge requirements.
Please note that if a facility has no effluent limit for TRC (just a monitoring requirement), then use of a hand-held
meter, sometimes described as a pocket colorimeter, and the reporting of <100 µg/L as a TRC value is acceptable.
The Environmental Protection Agency (EPA) and the State have determined that in the interest of overall program
equity, to ensure water quality protection, and to comply with 15A NCAC 2B .0505 (e) (4), the Division will require all
facilities with TRC limits to utilize instruments or methods that will produce detection and reporting levels that are
below the permit discharge requirements for TRC.” The laboratory was using a pocket colorimeter at all of the
NPDES permit facilities listed in the above comment and they all have low level TRC limits. It was determined that the
laboratory initially purchased a meter capable of low level TRC analysis, but returned to using the pocket colorimeter
when the meter did not work well. The laboratory has been using the pocket colorimeter since approximately 2009. A
Notice of Finding for Immediate Response (NOFIR) was issued to the laboratory regarding this issue and a copy was
provided to the Winston-Salem Regional Office staff. The laboratory replied to the NOFIR with an acceptable curve
verification on an approved meter and indicated that the approved meter would be put into use beginning June 9,
2014. No further response is necessary for this finding.

Recommendation: The inconsistencies between the benchsheets used by the two field units are the cause of
several of the Field Parameters Findings. Merging the existing benchsheets into one or creating a new benchsheet
(to be used by both units) that will encompass all of the needs for both units is recommended.

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DDDD. Finding: Monitoring Coalition benchsheets – Units of measure were not documented on the calibration sheet
for pH buffer true values and values obtained or for the Conductivity check standard true value and value
obtained.

Requirement: Data pertinent to each analysis must be maintained for five years. Certified Data must
consist of date collected, time collected, samples site, sample collector, and sample analysis time. The
field benchsheets must provide a space for the signature of the analyst, and proper units of measure for
all analyses. Ref: 15A NCAC 2H .0805 (g) (1).

EEEE. Finding: Monitoring Coalition and NPDES permit facility benchsheets - Temperature is analyzed
immediately, but is not documented as such.

Requirement: Data pertinent to each analysis must be maintained for five years. Certified Data must
consist of date collected, time collected, samples site, sample collector, and sample analysis time. The
field benchsheets must provide a space for the signature of the analyst, and proper units of measure for
all analyses. Ref: 15A NCAC 2H .0805 (g) (1).

Comment: A statement that Temperature samples are analyzed immediately upon collection and the
documented time is both collection and analysis time, may be added to the benchsheet.

FFFF. Finding: NPDES permit facility benchsheets – The benchsheets did not include units of measure for pH,
Total Residual Chlorine (TRC), and Dissolved Oxygen (DO).

Requirement: Data pertinent to each analysis must be maintained for five years. Certified Data must
consist of date collected, time collected, samples site, sample collector, and sample analysis time. The
field benchsheets must provide a space for the signature of the analyst, and proper units of measure for
all analyses. Ref: 15A NCAC 2H .0805 (g) (1).

GGGG. Finding: NPDES permit facility benchsheets – The meter calibration time is not documented for TRC and
DO.

Requirement: The following must be documented in indelible ink whenever sample analysis is performed:
Meter calibration and meter calibration time(s). Ref: NC WW/GW LC Approved Procedure for the Analysis
of Total Residual Chlorine and NC WW/GW LC Approved Procedure for the Analysis of Dissolved
Oxygen.

HHHH. Finding: NPDES permit facility benchsheets – No instrument identification is documented on the
benchsheets.

Requirement: The following must be documented in indelible ink whenever sample analysis is performed:
Instrument identification. Ref: NC WW/GW LC Approved Procedure for the Analysis of Total Residual
Chlorine, NC WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen, Ref: NC WW/GW
LC Approved Procedure for the Analysis of pH, Ref: NC WW/GW LC Approved Procedure for the Analysis
of Temperature.

Recommendation: NPDES permit facility benchsheets – Temperature is recorded on the Total Residual
Chlorine (TRC) benchsheet, but is obtained using the Dissolved Oxygen (DO) meter. In order to accurately
reflect the meter used to obtain Temperature, it is recommended that it be moved to the DO benchsheet.

IIII. Finding: NPDES permit facility benchsheets – pH buffer checks are not always acceptable and the meter
was not recalibrated.

Requirement: When quality control (QC) failures occur, the laboratory must attempt to determine the
source of the problem and must apply corrective action. Part of the corrective action is notification to the
end user. If data qualifiers are used to qualify samples not meeting QC requirement s, the data may not be
useable for the intended purposes. It is the responsibility of the laboratory to provide the client or end -user
of the data with sufficient information to determine the usability of the qualified data. Ref: North Carolina
Wastewater/Groundwater Laboratory Certification Policy.

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Requirement: The check standard buffer must read within ±0.1 S.U. to be acceptable. If the meter
verification does not read within ±0.1 S.U., the meter must be recalibrated before any samples are
analyzed. Ref: NC WW/GW LC Approved Procedure for the Analysis of pH.

Comment: In the data reviewed, the 4 and 10 S.U. buffers were occasionally unacceptable, but the 7 S.U.
buffer was acceptable. Sample results were not qualified on the final report (see Finding F).

Recommendation: Only one buffer is required to be checked after calibration. It is recommended that
this be the buffer closest to sample values, which is most often the 7 S.U. buffer.

JJJJ. Finding: NPDES permit facility analyses – A post analysis check is not performed for pH.

Requirement: When performing analyses away from the certified laboratory’s primary location, a post
analysis calibration verification using the check standard buffer must be analyzed at the end of the run. It is
recommended that a mid-day check standard buffer be analyzed when samples are analyzed over an
extended period of time. The post analysis check standard buffer(s) must read within ±0.1 S.U or corrective
actions must be taken. Ref: NC WW/GW LC Approved Procedure for the Analysis of pH.

Comment: Since the TRC and DO meters are recalibrated at each sample site, the operator indicated that
he would begin recalibrating the pH meter at each sample site as well. This will be an adequate response to
this finding.

IV. PAPER TRAIL INVESTIGATION:

The paper trail consisted of comparing laboratory benchsheets and chain of custody forms to client reports. Data
were reviewed for the following project numbers: 04011403, 05061403, and 09051384. No transcription errors
were detected. The facility appears to be doing a good job of accurately transcribing data.

V. CONCLUSIONS:

Correcting the above-cited findings and implementing the recommendations will help this lab to produce quality
data and meet certification requirements. A follow-up inspection will be performed after the laboratory has
corrected all findings in this report and submitted updated SOPs. The inspectors would like to thank the staff for its
assistance during the inspection and data review process. Please respond to all findings.

Report prepared by: Jason Smith Date: June 23, 2014
Report reviewed by: Nick Jones Date: July 3, 2014