#10_08_2015_FINAL

INSPECTION REPORT ROUTING SHEET

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

Laboratory Cert. #: 10

Laboratory Name: Environment 1, Inc.

Inspection Type: Commercial Maintenance

Inspector Name(s): Nick Jones, Dana Satterwhite, Todd Crawford
Tonja Springer, Jason Smith, Beth Swanson

Inspection Date: August 11 and 12, 2015

Date Report Completed: September 30, 2015

Date Forwarded to Reviewer: October 12, 2015

Reviewed by: Jason Smith

Date Review Completed: 10/29/2015

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

Unit Supervisor/Chemist III: Gary Francies

Date Received: 11/17/2015

Date Forwarded to Linda: 12/16/2015

Date Mailed: 12/16/2015

cc: Jay Sauber, Carrie Ruhlman, Chris Goforth

On-Site Inspection Report

LABORATORY NAME: Environment 1, Inc.

ADDRESS: PO Box 7085
Greenville, NC 27835

CERTIFICATE #: 10

DATE OF INSPECTION: August 11 and 12, 2015

TYPE OF INSPECTION: Commercial Maintenance

AUDITOR(S): Nick Jones, Dana Satterwhite, Todd Crawford
Tonja Springer, Jason Smith, and Beth Swanson

LOCAL PERSON(S) CONTACTED: Mark Oliveira and Steve Jones

I. INTRODUCTION:

This laboratory was inspected by a representative 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 facility has all the equipment necessary to perform the analyses. Laboratory
personnel communicate well with sample collectors and coordinate sample analyses
effectively to manage workload and holding times.

Proficiency Testing (PT) samples have been analyzed for all certified parameters for the
2015 proficiency testing calendar year. The laboratory has fulfilled its PT requirements for
the 2015 calendar year.

Contracted analyses are performed by Meritech, Inc. (Certification #165) and Eurofins
Lancaster Laboratories Environmental, LLC (Certification #521).

Current quality assurance policies and Field Parameter Approved Procedures for the
analysis of the facility’s currently certified parameters were provided at the time of the
inspection.

Laboratory Fortified Matrix (LFM) and Laboratory Fortified Matrix Duplicate (LFMD) are
also known a Matrix Spike (MS) and Matrix Spike Duplicate (MSD) and may be used
interchangeably in this report.

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) documents. Any changes made in response to the Findings,
Recommendations or Comments listed in this report must be incorporated to insure the
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Method is being performed as stated, references to Methods are accurate, and the QA
and/or SOP documents are 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.

III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:

General Laboratory

Comment: The laboratory deleted the following parameter methods from their Certified
Parameters Listing on November 3, 2015:

 Chlorine, Total Residual – Standard Methods, 4500 Cl G-2000.
 Phosphorus, Total – EPA Method, 365.1, Rev. 2.0 (1993).
 Phosphate, Ortho – EPA Method, 365.3 (1978).
 Purgeable, Aromatics & Halocarbons – SW -846 8021 B (Aqueous)
 Chlorinated Acid Herbicides – Standard Methods, 6640 B-2006 (Aqueous)

Comment: The sample preservation and storage temperature requirements may be
changed in accordance with 40 CFR Part 136.3 Table II in all pertinent SOPs and in
practice. The current practice is to store “at 4°C”. 40 CFR Part 136.3 Table II allows ≤6°C
for most inorganic parameters and <10°C for bacterial tests, without evidence of freezing.

Recommendation: It is recommended that the lab 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.

A. Finding: The laboratory is reporting uncertified data without qualifying it as such.

Requirement: Commercial laboratories are required to obtain certification for
parameters which will be reported by the client to comply with State surface water
monitoring, groundwater, and pretreatment Rules. Ref: 15A NCAC 2H .0804 (a).

Comment: The lab was under the impression that being certified for the
parameter method included both aqueous and non-aqueous matrices. In the Fall
of 2012, the NC WW/GW LC program implemented certification by parameter
method matrix. Effective August 11, 2015, the following Parameter Methods have
been added to the labs certificate for Non-Aqueous matrix:

 Cyanide – Standard Methods, 4500 CN- E-1999
 Aluminum, Calcium, Chromium, Copper, Magnesium, Nickel, Potassium,
Sodium and Zinc - EPA 200.7, Rev. 4.4 (1994)
 Arsenic, Lead and Selenium – Standard Methods, 3113 B-2004

Data reported by the following Parameter Methods must be flagged as uncertified
for Non-Aqueous matrix. Certification is not offered for these parameter methods in
non-aqueous matrix because the methods only include procedures for preparation
and analysis of aqueous samples.
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 Chloride – Standard Methods, 4500 Cl- B-1997
 Fluoride – Standard Methods, 4500 F- C-1997
 Phenols, Inorganic – EPA Method, 420.1 Rev. (1978)
 Nitrogen, Ammonia – EPA 350.1, Rev. 2.0, 1993
 Nitrogen, NO2 + NO3 – EPA Method, 353.2, Rev. 2.0 (1993)
 Nitrogen, Total Kjeldahl – EPA Method, 351.2, Rev. 2.0 (1993)
 Total Phosphorus – EPA Method, 365.4 (1974)
 Sulfate - Standard Methods, 4500 SO42 E-1997
 Mercury – EPA Method, 245.1, Rev. 3.0 (1994)

Documentation

Recommendation: It is recommended that all records of maintenance performed on
analytical instrumentation be documented in an individual equipment maintenance log
book. All records of corrective action taken or minor troubleshooting and repair
performed should also be documented in the equipment maintenance log. The records
may include the following, as appropriate:

 The identity of the item of equipment and its software;
 The manufacturer’s name, type identification, and serial number or other unique
identifier;
 The current location;
 The dates, results and copies of reports and certificates or all calibrations,
adjustments, acceptance criteria, and the due date of the next calibration.
 The maintenance plan, where appropriate, and maintenance completed date.
 Documentation of any damage, malfunction, modification, or repair to the
equipment.
 Signature or initials of the person performing the maintenance or troubleshooting.

These records provide an historical reconstruction of the maintenance performed, a
reference for effective troubleshooting in the future, and can also serve as a valuable
training tool for new analysts.

Recommendation: It is recommended that labels be added to boxes on the benchsheets
to designate their content. Some benchsheets have boxes which are not labeled but are
used for data entry codes.

Recommendation: It is recommended to include calculation formulas on benchsheets.

Recommendation: It is recommended to include Quality Control acceptance criteria on
benchsheets.

Comment: There were several instances on benchsheets (i.e., benchsheets for Chemical
Oxygen Demand, Inorganic Phenols and Sulfate) where the analyst’s handwriting was
difficult to distinguish. This could pose issues with data defensibility or transcription errors.

B. Finding: The laboratory needs to increase the documentation of standards and
reagents prepared in the laboratory.
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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.
Ref: NC WW/GW LC Policy.

C. Finding: The analyst is not signing/initialing or dating electronically generated
laboratory benchsheets or data printouts. 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 02H .0805 (a) (7) (A).

Standard Operating Procedures

Recommendation: It is recommended that flow diagrams be included where applicable to
improve SOP utilization.

Recommendation: It is recommended that the SOPs for Nitrogen, Ammonia by EPA
Method, 350.1, Rev. 2.0 (1993), Phosphorus, Total by EPA Method, 365.4 (1974) and
Nitrogen, Total Kjeldahl by EPA Method, 351.2, Rev. 2.0 (1993) be revised to indicate that
the analyst actually recalibrates when curve standards fail QC criteria. It currently states to
only use curve points that are +10%.

Comment: The Total Coliform, MF SOP states that the pH of M-Endo Liquid Media must
be between 7.1 and 7.3 S.U. The reference method, Standard Methods, 9222 B-1997,
allows 7.2 + 0.2 S.U.

Comment: The Total Coliform, MF and MPN SOPs require preservation temperature of
<4°C and hold time requirements of 6 and 8 hours, respectively. 40 CFR Part 136, Table II
allows <10°C and 8 hours.

Comment: The laboratory did not have a Standard Operating Procedure (SOP) for
Thallium by EPA Method, 279.2 (Aqueous). The North Carolina Administrative Code, 15
NCAC 2H .0805 (a) (7) states: Each laboratory shall develop and maintain a document
outlining the analytical QC practices used for the parameters included in their certification.
Supporting records shall be maintained as evidence that these practices are being
effectively carried out. Acceptable corrective action [i.e., a SOP for Thallium by EPA
Method, 279.2 (Aqueous)] was received via email on 11/28/2015. No further response is
necessary for this Finding.

Comment: An inconsistency and/or omission was noted between the Standard
Operating Procedure (SOP) and laboratory practice as follows: personnel were not
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following procedures as stated in the Laboratory’s SOP, the Method reference in the
SOP was not correct, the SOP was in direct conflict with Method and/or regulatory
requirements, and the SOP did not describe in detail how the Method is performed
(observations are listed below ). The North Carolina Administrative Code, 15 NCAC 2H
.0805 (a) (7) states: Each laboratory shall develop and maintain a document outlining the
analytical QC practices used for the parameters included in their certification. Supporting
records shall be maintained as evidence that these practices are being effectively carried
out. Demonstration of acceptable corrective action (i.e., SOPs were revised) was observed
during the second day of inspection (i.e., August 12, 2015). No further response is
necessary for this Finding.

 Biochemical Oxygen Demand -SM 5210 B-2001
o The SOP did not state that the incubation temperature is 20+1°C.

 Phosphate, Ortho – Standard Methods, 4500 P E-1999
o The SOP did not describe the process of back–calculating each calibration
standard.

D. Finding: The laboratory does not have an Analytical QC Document or SOP for the
following:

 Pesticides, Organochlorine - EPA Method 608 (Aqueous)
 Purgeable, Organics - EPA Method 624 (Aqueous)
 Metals - EPA SW -846 Method 6020 B(Aqueous)
 Mercury - EPA SW -846 Method 7470 A (Aqueous)
 Mercury - EPA SW -846 Method 7471 B (Aqueous)
 Purgeable, Aromatics & Halocarbons - EPA SW -846 Method 8021 B
(Aqueous)
 Proficiency Testing Samples

Requirement: Each laboratory shall develop and maintain a document outlining the
analytical QC 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).

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
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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.

E. Finding: An inconsistency and/or omission was noted between the Standard
Operating Procedure (SOP) and laboratory practice as follows:

 General
o The SOPs do not describe in sufficient detail QC acceptance criteria
and/or corrective actions for unacceptable QC measures for all QC
elements. This was noted for the following parameters; however, this
list may not be all inclusive: Acidity, Nitrogen (Ammonia, Nitrite,
Nitrate and Nitrate + Nitrite), Total Phosphorus, Inorganic Phenols,
Salinity, Organochlorine Pesticides, 1,2-Dibromoethane, Alkalinity,
Hardness, Mercury, Purgeable Organics, Residues (Dissolved,
Suspended and Total), Metals, Chloride, Chlorinated Acid
Herbicides, Purgeables (Halocarbons & Aromatics), Fecal Coliform
MF, Total MPN &Total MPN Sludge, Cyanide, and Fluoride.
o SOPs are intended to describe procedures exactly as they are to be
performed. Evaluate all SOPS for the proper use of the word
“should”.

 Acidity – Standard Methods, 2310 B-1997
o The SOP does not state preservation / hold time requirements.
o .
o The SOP does not state that the sample is brought to room temperature
before analysis.
o The SOP does not state that the titrant is added in increments of 0.5 mL
or less, such that a change of less than 0.2 S.U. occur per increment.

 Alkalinity – Standard Methods, 2320 B-1997
o The SOP does not define the reporting limit.

 Biochemical Oxygen Demand – Standard Methods, 5210 B-2001 (Hach
10360-2011, Rev. 1.2) (LDO)
o The SOP does not state that samples and dilution water are warmed to
20+3°C (it states “approximately 20 °C”).
o The SOP does not state that the pH adjustment must not change the
sample volume by more than 5%.
o The SOP does not state the initial Dissolved Oxygen (DO) of the blank
must be 7.5-9.0 mg/L.
o The SOP does not state that the initial DO must be measured within 30
minutes of preparation.
o The SOP does not state how sample results are calculated and which
results are reported.
o The SOP does not state details of calculating and applying the seed
correction factor.
o The SOP does not define the reporting limit (i.e., 2 mg/L).

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 Chemical Oxygen Demand – Hach Method 8000
o The SOP does not state preservation / hold time requirements.
o The SOP does not state to wait 20 min for the vials to cool to 120°C or
less before inverting.
o The SOP does not state to invert the vials several times while still warm.
o The SOP does not state the reporting limit for the high range curve.
o The SOP does not include calculations for QC.

 Chloride - Standard Methods, 4500 Cl- B-1997
o The SOP section for preparation of the Aluminum Hydroxide Solution
states: Follow procedure in Standard Methods on page 4-67. The correct
reference is 4500 Cl- B-1997, (3) (d) (1).
o .
o The SOP does not state how the LFM/LFMD is prepared.

 Chlorophyll - EPA Method 445.0, Rev. 1.2 (Fluorometric)
o The SOP does not include the revision in the Method reference.
o The SOP does not include the units of the vacuum pressure in section
3.b.1.
o The SOP does not include the spectrophotometer calibration sheet.
o The SOP contains a section (i.e., section 1.h) which appears to be
irrelevant to the analysis.

 Coliform, Fecal - Standard Methods, 9222 D-1997 (MF)
o The SOP does not state a range for reagent storage temperature.

 Coliform, Total - Standard Methods, 9222 B-1997 (MF)
o The SOP states that the lab is to set two dilutions. Lab practice is to set
three dilutions.
o The SOP does not state the volume of sample to be analyzed.
o The SOP states that it is attached, but does not include the attachment
regarding the preparation of phosphate dilution water.
o The SOP does not state the specifications of the light source utilized for
counting colonies.

 Coliform, Fecal - Standard Methods, 9222 D-1997 (MF)
 Coliform, Fecal - Standard Methods, 9221 C E-2006 (MPN)
o The SOPs do not state to document the water bath temperature twice
daily.
o The SOPs do not describe the known culture positive.

 Coliform, Total - Standard Methods, 9221 B-2006 (MPN)
o The SOP states to shake the samples and observe for gas formation. The
method says to swirl the sample gently after incubation.
o The SOP does not state the size of the sterile loop or how much sample to
transfer to the confirmation phase.
o The SOP does not state the pH of the sterilized broth must be 6.8 + 0.2
S.U.
o The SOP does not state what is used to adjust the pH of the brilliant green
lactose bile broth.
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o The SOP does not state instructions for determining a reportable result.
o The MPN table is not included with the SOP.

 Color, PC – Standard Methods, 2120 B-2001
o The SOP does not state to document the pH adjustment.
o The SOP does not state that the pH of samples must be reported as well.

 Conductance, Specific – Standard Methods, 2510 B-1997
o The lab currently has three SOPs. Since this is a Field Parameter, not all
of the analyses are subject to the same QC requirements. Ensure that QC
is performed as required per individual SOP.
(a) Lab and Field SOP
(i) The SOP states to adjust meter to the proper scale, but does
not state how to determine which scale is proper.
(ii) Duplicates are not required, but if the lab continues to analyze
them, then the SOP needs to include acceptance criteria and
corrective actions for failures.
(iii) The SOP does not state that the Automatic Temperature
Compensator (ATC) check must be performed every twelve
months.
(b) Lab SOP
(i) The SOP does not state the proper units for the 1412
µmhos/cm standard (i.e., was only listed as µmhos).
(ii) The SOP does not state preservation and hold time
requirements (i.e., cool to ≤6°C and 28 days).
(iii) The SOP does not describe in sufficient detail how the
standards are prepared.
(iv) The SOP does not state the frequency, acceptance criteria or
corrective actions regarding Laboratory Fortified
Blanks/Second Source Standards.
(c) Field SOP
(i) The SOP does not state QC requirements for second source
laboratory fortified blank, associated acceptance criteria and
corrective actions for failures.
(d) River Basin Coalition SOP
(i) The SOP does not state directions for ATC verification.

 Cyanide – Standard Methods, 4500 CN- E-1999
o The SOP does not state that the calibration standards are back-calculated
against the curve and how acceptance criteria are applied.
o The SOP does not state the frequency that IDOCs or MDLs are
performed.
o The SOP does not state how the titrant is standardized.
o The SOP does not state that the blanks (i.e., calibration and method) and
calibration standards are analyzed at the beginning of the analytical
sequence.

 Dissolved, Oxygen – Standard Methods, 4500 O G-2001
o The SOP does not state sample hold time (i.e., 15 minutes).
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o The SOP does not describe a detailed operating procedure. It refers the
analyst to the manufacturer’s instructions for guidance, but instead the lab
has a document titled “YSI 556 MPS Calibration Instructions” which needs
to be the referenced document.
o The SOP does not state the amount of time needed for the instrument to
warm up.
o The SOP does not state that a post analysis calibration verification is
required.
o The SOP does not state acceptance limits (i.e., ±0.5 mg/L) for the post
analysis calibration verification.
o The SOP does not state the analysis of a mid-day check and acceptance
criteria.

 Enterococci – Enterolert® IDEXX
o The SOP does not include the IDEXX MPN table.
o The SOP does not include instructions for opening the Quanti-Tray®
without contaminating the interior of the foil or tray.
o The SOP does not state the source of the culture positive control.
o The SOP does not state the source of the culture sterility control.
o The SOP does not state to allow any foam to settle before sealing.

 Fluoride - Standard Methods, 4500 F- C-1997
o The SOP does not specify how sample volumes are measured.
o The SOP states to wipe the electrode with a paper towel. The Method
states to blot dry and cautions that this may poison the electrode if not
done gently.
o The SOP does not state to verify the calibration after every ten samples
and at the end of an analysis run.
o The SOP does not state to bring all of the samples and standards to the
same temperature prior to buffer addition.
o The SOP instructions for preparing working standards produce
concentrations that are half of what is stated.
o The SOP does not include the distillation requirement or reference the
distillation SOP.
o The SOP does not include QC calculations.
o The laboratory is combining the standard preparation step with one of the
other procedural steps causing confusion regarding the concentration of
the standards. The method says add a volume of buffer equal to the
volume of standard or sample being analyzed prior to analysis. Each
working standard final volume is 100ml, however the stated concentration
of the standard is based on a final volume of 50 ml. Since only 50 ml of
sample is used for analysis and the adding of 50 ml of buffer to the
sample gives the sample volume proportion as that of the standard (i.e. 50
ml of standard plus 50 ml of buffer), the final sample results, based on the
stated standard concentrations, is correct. However, the description of the
standards preparation, by itself, is misleading in that it appears to
incorrectly state the final concentrations when based on the stated final
volume of 100 ml.

 Hardness – Standard Methods, 2340 C-1997
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o The SOP does not describe in sufficient detail how the Matrix Spike (MS)
is prepared.

 Nitrogen, Ammonia – EPA Method, 350.1, Rev. 2.0, 1993
o The SOP does not state EPA 350.1, Rev. 2.0, 1993 as the distillation
Method. It states SM 4500 NH3 B-1997.

 Nitrogen, NO2 – EPA Method, 353.2, Rev. 2.0, 1993
o The SOP does not state that NO2 is determined by bypassing the Cd
column.
o The SOP does not describe how to adjust samples with pH values outside
of 5-9 S.U. prior to analysis.
o The SOP does not state that matrix spikes must be analyzed at 10%
frequency with +10% recovery, as required by the method. The SOP
states matrix spikes are to be analyzed at a 5% frequency with +15%
recovery or 95% confidence interval.

 Nitrogen, NO2 + NO3 – EPA Method, 353.2, Rev. 2.0, 1993
o The SOP does not describe the preparation of all reagents used during
analysis (e.g., Na2S2O3, 2% CuSO4, 50% H2SO4, 0.5 N HCl).

 Nitrogen, NO2 – EPA Method, 353.2, Rev. 2.0, 1993
 Nitrogen, NO2 + NO3 – EPA Method, 353.2, Rev. 2.0, 1993
o The SOP contains typos in the color reagent section (i.e., the spellings of
naphthylethylenediamine and sulfanilamide).

 Nitrogen, Total Kjeldahl – EPA Method, 351.2, Rev. 2.0, 1993
o The SOP does not state the true value of the second source standard.
o The SOP does not include an equipment / supplies section.
o The SOP does not address interferences.

 Phosphorus, Ortho – Standard Methods, 4500 P E-1999
o The SOP does not state that MS/MSDs are analyzed daily.
o The SOP does not describe the analysis of MSDs.

 Phosphorus, Total – EPA Method, 365.4, 1974
o The SOP references a version of the Method which is not approved (i.e.,
revision 2.0, 1993).
o The SOP does not address all required QC elements (e.g., IDC MDL,
MS/MSD, trend analysis). Refer to 40 CFR 136.7 for all 12 QC elements.

 Phosphate, Ortho – Standard Methods, 4500 P E-1999
o The SOP does not describe actions taken if turbidity forms when making
the combined reagent.

 Nitrogen, Ammonia – EPA Method, 350.1, Rev. 2.0, 1993
 Nitrogen, NO2 – EPA Method, 353.2, Rev. 2.0, 1993
 Nitrogen, NO3 - (NO3 + NO2 EPA 353.2, Rev. 2.0, 1993) - (NO2 EPA 353.2,
Rev. 2.0, 1993)
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 Nitrogen, NO2 + NO3 – EPA Method, 353.2, Rev. 2.0, 1993
 Phosphorus, Total – EPA Method, 365.4, 1974
o The SOPs do not state the lab name.
o The SOPs do not state interferences.
o The SOPs do not state utilized equipment.
o The SOPs do not state the source of the reagent water.
o The SOPs do not document all calculations (e.g., results, percent
recovery, software regression and relative percent difference).
o The SOPs do not state reporting requirements (e.g., significant figures,
units, rounding, etc.).
o The SOPs do not state calibration curve acceptance criteria.
o The SOPs do not state preservation and hold time requirements.
o The SOPs do not describe the chemical preservation of samples.
o The SOPs do not state that blanks must be analyzed initially, after every
10 samples and at the end of an analysis batch.
o The SOPs do not describe matrix spike preparation.
o The SOPs do not describe glassware cleaning protocols.
o The SOPS do not describe what is done for over range samples.

 Nitrogen, Ammonia – EPA Method, 350.1, Rev. 2.0, 1993
 Nitrogen, NO2 – EPA Method, 353.2, Rev. 2.0, 1993
 Nitrogen, NO2 + NO3 – EPA Method, 353.2, Rev. 2.0, 1993
 Nitrogen, NO3 - (NO3 + NO2 EPA 353.2, Rev. 2.0, 1993) - (NO2 EPA 353.2,
Rev. 2.0, 1993)
 Nitrogen, Total Kjeldahl – EPA Method, 351.2, Rev. 2.0, 1993
 Phosphorus, Total – EPA Method, 365.4, 1974
o The SOPs do not state that the 2nd source standard acceptance criterion
must be ±10%.
o The SOPs do not state that the calibration standards be analyzed in order
of decreasing concentration.

 Organic Carbon, Dissolved – Standard Methods, 5310 C-2000
 Organic Carbon, Total – Standard Methods, 5310 C-2000
o The SOPs do not state the true value of the second source standard.
o The SOPs do not include the calculations for QC.

 Phenols, Inorganic – EPA Method, 420.1, Rev. 1978
o The SOP does not state that when the distillate is turbid, filter through a
prewashed membrane filter.
o In step five of the SOP, it does not state that the 50 mLs of deionized
water added be warm.
o In step twelve of the SOP, it does not state that after the additional ten
shakes to let chloroform settle again, then vent chloroform fumes into
hood.

 Residue, Suspended – Standard Methods, 2540 D-1997
o The SOP does not state the total maximum filtration time allowed for
samples (i.e., 10 minutes).
o The SOP does not state that the drying time utilized daily is the drying time
established from the annual study.
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o The SOP does not state QC acceptance criterion and corrective actions
for the dry blank.

 Residue, Dissolved – Standard Methods, 2540 C-1997
 Residue, Suspended – Standard Methods, 2540 D-1997
 Residue, Total – Standard Methods, 2540 B-1997
o The SOPs do not describe the annual drying study.
o The SOPs do not include all necessary equipment to perform the analysis.
o The SOPs do not state that weight 1 and weight 2 are in grams in the
utilized calculation.
o The SOP does not state how different sample volumes are measured (i.e.,
wide bore pipettes vs. graduated cylinders).

 Residue, Suspended – Standard Methods, 2540 D-1997
 Residue, Total – Standard Methods, 2540 B-1997
o The SOP does not state explicit QC acceptance criteria for duplicate
analyses. The total residue SOP stated the duplicates “should be ±5%”
and there was no criterion in the suspended residue SOP.

 Residue, Dissolved – Standard Methods, 2540 C-1997
 Residue, Total – Standard Methods, 2540 B-1997
o The SOP does not state that the given reporting limits are only
applicable when using sample volumes of 250 mL for Dissolved Solids
and 100 mL for Total Solids.
o The SOP does not describe how to adjust the PQL if different volumes
of sample are used and the minimum weight gain is not achieved.

 Residue, Dissolved – Standard Methods, 2540 C-1997
o The SOP does not describe how the filters are washed.
o The SOP does not state that filters must be wrinkled side up on the
filtration apparatus.
o Step 9 states to repeat steps 7 and 8. The lab is performing a drying
time study instead of repeating steps 7 and 8.

 Residue, Settleable – Standard Methods, 2540 F-1997
o The SOP does not state to clean and dry the Imhoff cone.
o The SOP does not include a section for reporting results (i.e., units and
reporting limit).

 Salinity – Standard Methods, 2520 B-2010
o The SOP does not state the calculation that is utilized in the Microsoft
Excel® calculation spreadsheet to determine results
o The SOP does not describe the preparation and concentration of
calibration standards.

 Sulfate – Standard Methods, 4500 SO42- E-1997
o The SOP does not state the requirement to nor the instructions for back-
calculating the calibration standards.

 Sulfide – Standard Methods, 4500 S2- D-2000
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o The SOP states to document “required sample information”, but does not
specifically state what that includes.
o At the end of step two, the SOP does not state that it is inverted slowly
and only once.
o The SOP does not state to standardize the methylene blue solution each
day it is used.
o The SOP does not state to analyze a MS/MSD daily.

 Temperature – Standard Methods, 2550 B-2000
o The SOP does not state that the analysis must be in situ or immediate.

 Mercury – EPA Method, 1631 E
o The SOP does not state that the samples must be preserved within 48
hours (SOP states within 72 hours).
o The SOP states that 20 mL of standard is added to 20 mL of sample. In
practice, the laboratory adds 2 mL of standard to 38 mL of sample.

 Metals – EPA Method, 200.7, Rev. 4.4,1994
o The SOPs (i.e., digestion and analysis) do not describe preparation and
concentrations of all standards and QC.
o The SOP does not define all standard nomenclature (i.e., CCB, ICB, LRB,
CCV, etc.)

 Base Neutral / Acid Organics – SW846 Method, 8270 D
o The SOP skips sections three and four.
o The SOP states in section 2, subsections 1, 2 and 3 to continue to step
3C. There is no step 3C.

 1,2-Dibromoethane – EPA Method, 504.1
o The SOP does not include the second source confirmation.
o The SOP does not include the DBCM retention time standard.

 Pesticides, Organochlorine – SW846 Method 8081 B
o The SOP does not cite the complete method reference, only 8081 B.
o The SOP does not cite the extraction method.
o The SOP does not state that samples with pH values outside of 5-9 S.U.
will be adjusted and how.

 Pesticides, Organochlorine – SW846 Method, 8081 B
 1,2-Dibromoethane – EPA Method, 504.1
o The SOPs do not state the lab name.
o The SOPs do not state interferences and their mitigations.
o The SOPs do not state retention time windows.
o The SOPs do not state confirmation techniques.
o The SOPs do not state reagent preparation.
o The SOPs do not state utilized equipment (including columns).
o The SOPs do not state calculations (e.g., software regression, results,
percent recovery and relative percent difference).
o The SOPs do not state reporting requirements (e.g., significant figures,
units, rounding, etc.).
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o The SOPs do not state calibration curve acceptance criteria.
o The SOPs do not define all QC frequencies.
o The SOPs do not state preservation and hold time requirements.

 Purgeable, Aromatics – Standard Methods, 6200 C-1997
o The SOP does not state sample preservation requirements.

 Purgeable, Halocarbons – EPA Method, 601
 Purgeable, Aromatics – EPA Method, 602
o The SOPs do not include the complete method reference. It only
references 601 and 602.
o The SOPs do not state sample preservation requirements.
o The SOPs do not state that the prepared aqueous calibration standards
may be stored for up to 24 hours, if held in sealed vials with zero
headspace. If not stored, they must be discarded after one hour.
o The SOPs do not state the frequency of MS/MSDs.

Requirement: Each laboratory shall develop and maintain a document outlining the
analytical QC 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 respond in writing
stating that the SOPs will be revised to address the items in this Finding
within one year.

Comment: The inspectors left an example SOP review checklist for the lab’s
internal use during the audit.

Acidity – Standard Methods, 2310 B-1997

F. Finding: The lab has not established a reporting limit.

Requirement: Calculation
Acidity, as mg CaCo3/L = [(A x B) – (C x D)] x 50 000
mL sample

where:

A = mL NaOH titrant used,
B = normality of NaOH,
C = mL H2SO4 used (2310B.4a), and
D = normality of H2SO4 Ref: Standard Methods, 2310 B-1997. (5).

Comment: To determine the reporting limit with the above equation, “A” equals the
smallest measurement increment of the buret utilized.

G. Finding: The lab is not documenting the endpoint pH. This is considered pertinent
information.

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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).

Requirement: Consequently, use fixed end points of pH 3.7 and pH 8.3 for
standard acidity determinations via potentiometric titration in wastewaters and
natural waters where the simple carbonate equilibria discussed above cannot be
assumed. Ref: Standard Methods, 2310 B-1997. (1) (b).

Alkalinity – Standard Methods, 2320 B-1997

H. Finding: The lab is not standardizing the titrant monthly.

Requirement: Verify standardized titration reagents by periodically re-
standardizing. Method parameters in Part 2000 that are determined using
standardized titration reagents are acidity, alkalinity, and hardness. Typically, the
standardized reagents are stable for several months when sealed to avoid
evaporation and stored properly. Re-standardize reagents once a month or when
improper storage occurs. Ref: Standard Methods, 2020 B-2010. (2) (b).

I. Finding: The lab is not reporting results as “The alkalinity to pH ____=____ mg
CaCO3/L.”

Requirement: Report pH of end point used as follows: “The alkalinity to
pH____=____ mg CaCO3/L” and indicate clearly if this pH corresponds to an
inflection point of the titration curve. Ref: Standard Methods, 2320 B-1997. (5) (a).

Biochemical Oxygen Demand – Standard Methods, 5210 B-2001

Recommendation: It is recommended to not change the sample volume by more than
5% when neutralizing Total Residual Chlorine with sodium sulfite.

J. Finding: The laboratory was not seeding samples over six hours old.

Requirement: Some samples (for example, some untreated industrial wastes,
disinfected wastes, high-temperature wastes, wastes having pH values less than 6
or greater than 8, or wastes stored more than 6 h after collection) do not contain a
sufficient microbial population. Seed such samples by adding a population of
suitable microorganisms. Ref: Standard Methods 5210 B-2001. (4) (d).

K. Finding: Samples were not properly adjusted for pH.

Requirement: 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 or sodium hydroxide of such strength that the quantity of reagent does not
dilute the sample by more than 0.5%. The pH of dilution water should not be
affected by the lowest sample dilution. Always seed samples that have been pH
adjusted. Ref: Standard Methods, 5210 B-2001. (4) (b) (1).

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Comment: The laboratory adjusts all samples to a neutral pH if the sample pH is
less than 6.0 or greater than 8.5 units. Samples are adjusted to pH 6.5 to 7.5 units if
needed.

L. Finding: Incubation time is not always documented. This is considered pertinent
information.

Requirement: After 5 d + 6 h of incubation, determine DO in all sample dilutions,
and in all blanks and checks as in ¶ 6b–d, using the azide modification of the
titrimetric method or the membrane electrode method. Ref: Standard Methods,
5210 B-2001. (5) (i).

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: All incubation start times are not documented on the Biochemical
Oxygen Demand (BOD) benchsheets. Total incubation time cannot be verified
without start and end times. Samples are occasionally set up in both the morning
and afternoon. When they are, the time samples are incubated is documented in
the morning, but is not documented for the samples set up in the afternoon.

M. Finding: The units of measure for Dissolved Oxygen 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).

Chloride - Standard Methods, 4500 Cl- B-1997

Recommendation: Method Blank titrant volumes are typically 0.7-0.8 mLs. The method
states that 0.2 to 0.3 mLs is typical. It is recommended that the laboratory verify the purity
of the water source utilized for the analysis with regard to the high blank titrant volumes.

Chlorophyll  - EPA Method 445.0, Rev. 1.2 (Fluorometric)

N. Finding: The lab is not taking appropriate corrective action when QC failures
occur.

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. Ref: NC WW/GW LC Policy.

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Comment: Duplicate RPDs on 5/16/2015 and QCS standard comparisons in
June and July, 2015, failed acceptance criteria. The associated data was not
qualified on the client reports.

Coliform, Fecal – Standard Methods, 9221 C E-2006 24hr 503 (MPN)

O. Finding: The lab is not drying samples to a constant weight.

Requirement: The solids content of treated domestic sludge can be highly variable.
Therefore, an aliquot of each sample must be dried and the solids content
determined in accordance with procedure 2540 G. of the 18th edition of Standard
Methods for the Examination of Water and Wastewater (SM). Ref: Control of
Pathogens and Vector Attraction in Sewage Sludge, EPA/625/R-92/013, July 2003,
Appendix F, Section 1 (1.1).

Coliform, Fecal – Standard Methods, 9222 D-1997 (MF)

Comment: If the media is purchased pre-made, then NC requires only weekly known
culture positive verifications.

P. Finding: The lab is not always placing prepared cultures in the water bath within 30
min after filtration.

Requirement: Place all prepared cultures in the water bath within 30 min after
filtration. Ref: Standard Methods, 9222 D-1997. (d) (2) (d).

Comment: For the data reviewed during the inspection, the requirement was not
met on Fecal Coliform sample sets prepared on 5/4/2015, 5/5/2015, 6/2/2015 and
6/4/2015.

Coliform, Fecal – Standard Methods, 9221 C E-2006 (MPN) (Aqueous) & 24hr 503
(Non-Aqueous)

Q. Finding: Positive sample counts are not repeated by a different analyst on a
monthly basis.

Requirement: For routine performance evaluation, repeat counts on one or more
positive samples at least monthly, record results, and compare the counts with
those of other analysts testing the same samples. Replicate counts … should agree
within 10%. Ref: Standard Methods, 9020 B-2005. (9) (a).

R. Finding: The lab has not established duplicate acceptance criteria.

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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Comment: Acceptable options for determining acceptance criteria can be found in
Standard Methods, 9020 B-2005. (9) (e), Standard Methods, 9221 C-2006. Table
9221:IV or establish your own. If the lab chooses Table 9221:IV to determine
duplicate acceptance, then the 95% confidence windows of each sample must
overlap to be acceptable.

Fluoride – Standard Methods, 4500 F- C-1997

S. Finding: The lab is not analyzing a blank and calibration verification standard after
every ten samples.

Requirement: Verify calibration by periodically analyzing a calibration standard
and calibration blank during a run—typically, after each batch of ten samples and
at the end of the run. Ref: Standard Methods, 4020 B-2009. (2) (b).

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.

T. Finding: The lab is not analyzing laboratory fortified matrix duplicates.

Requirement: W hen 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).

Comment: The laboratory analyzes unspiked environmental sample duplicates.

U. Finding: The data does not accurately reflect the QC practices which are being
carried 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).

Recommendation: It is recommended that the duplicate result column on the
benchsheet be labeled as the average result, since the data in this column is the
average of the results.

Hardness – Standard Methods, 2340 C-1997

V. Finding: The lab is not diluting 25 mL of sample to 50 mL before titrating.

Requirement: Titration precautions: Conduct titrations at or near normal room
temperature. The color change becomes impractically slow as the sample
approaches freezing temperature. Indicator decomposition becomes a problem in
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hot water. The specified pH may produce an environment conducive to CaCO3
precipitation. Although the titrant slowly re-dissolves such precipitates, a drifting end
point often yields low results. Completion of the titration within 5 min minimizes the
tendency for CaCO3 to precipitate. The following three methods also reduce
precipitation loss. Dilute sample with distilled water to reduce CaCO3 concentration.
This simple expedient has been incorporated in the procedure. If precipitation
occurs at this dilution of 1 + 1 use modification 2) or 3). Using too small a sample
contributes a systematic error due to the buret-reading error. Ref: SM 2340 C-1997.
(1) (c) and SM 2340 C-1997. (1) (c) (1).

Requirement: Dilute 25.0 mL sample to about 50 mL with distilled water in a
porcelain casserole or other suitable vessel. Ref: SM 2340 C-1997. (3) (b).

Nitrogen, Ammonia – EPA Method, 350.1, Rev. 2.0, 1993

Recommendation: It is recommended to develop and implement a distillation log.

W. Finding: The lab is using ammonium sulfate as the stock solution.

Requirement: Stock solution: Dissolve 3.819 g of anhydrous ammonium chloride,
NH Cl 4 (CASRN 12125-02-9), dried at 105°C, in reagent water, and dilute to 1 L.
1.0 mL = 1.0 mg NH -N. Ref: EPA Method, 350.1, Rev. 2.0 (1993), Section 7.11.

Comment: The lab has not performed a validation study to show that ammonium
sulfate is equivalent to ammonium chloride. The lab is not reporting results as
having been acquired via a modified method.

X. Finding: The lab is not using the method prescribed sodium hypochlorite solution.

Requirement: Dilute 250 mL of a bleach solution containing 5.25% NaOCl
(CASRN 7681-52-9) (such as "Clorox") to 500 mL with reagent water. Available
chlorine level should approximate 2-3%. Since "Clorox" is a proprietary product,
its formulation is subject to change. The analyst must remain alert to detecting
any variation in this product significant to its use in this procedure. Due to the
instability of this product, storage over an extended period should be avoided.
Ref: EPA Method 350.1, Rev. 2.0, 1993, Section 7.8.

Comment: The lab uses a different formulation (i.e., not Clorox).

Y. Finding: The lab is not analyzing both MS/MSD distilled and un-distilled for the
distillation study.

Requirement: Commercial Laboratories shall analyze initially at least six samples
distilled and un-distilled, but at least two samples from all waste types. Analyze
one sample distilled and un-distilled yearly from all wastes types. Ref: NC
WW/GW Policy.

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
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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 Notes (6).

Nitrogen, NO2 + NO3 – EPA Method, 353.2, Rev. 2.0, 1993

Recommendation: It is recommended to decrease the curve range to alleviate the
possibility of having results which may be biased low on the upper 10% of the curve. The
curve is beginning to plateau on the upper end.

Recommendation: It is recommended to establish accuracy criteria for triplicate
measurements of calibration standards.

Phosphorus, Total – EPA Method, 365.4, 1974

Comment: The only data available for review was from PT samples.

Z. Finding: The lab was not sufficiently documenting spike preparation. 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 req uest.
Ref: 15A NCAC 2H .0805 (a) (7) (A).

Recommendation: The lab was not completely filling out the spike preparation
worksheet (i.e., ___ mLs of spike up to ___ mLs with sample). It was
recommended that the spike preparation worksheet be revised to read “_ml of _
mg/L spike solution added to the digestion tube” to more accurately describe the
laboratory’s spike preparation scheme.

AA. Finding: The lab is not documenting digestion times and temperatures. 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).

Requirement: Place tubes in digester and switch to automatic mode. Set low
temperature timer for 1 hour. Reset high temperature to 380°C and set timer for 2
1/2 hours. Ref: EPA Method, 365.4 (1974), Section 6.3.

Nitrogen, Ammonia – EPA Method, 350.1, Rev. 2.0, 1993
Nitrogen, NO2 + NO3 – EPA Method, 353.2, Rev. 2.0, 1993
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BB. Finding: The lab is not using +10% recovery as the acceptance criterion for matrix
spiking.

Requirement: Calculate the percent recovery for each analyte, corrected for
concentrations measured in the unfortified sample, and compare these values to
the designated LFM recovery range 90-110%. Ref: EPA Method, 350.1, Rev. 2.0
(1993), Section 9.4.2 and EPA Method, 353.2, Rev. 2.0 (1993), Section 9.4.2.

Nitrogen, Total Kjeldahl – EPA Method, 351.2, Rev. 2.0, 1993

Recommendation: It is recommended that the lab reanalyze samples known to have high
nitrate concentrations. High nitrate concentrations (10X or more than the TKN level) result
in low TKN values. If interference is suspected, samples should be diluted and reanalyzed.
Ref: EPA Method, 351.2, Rev. 2.0 (1993), Section 4.1.

Nitrogen, Ammonia – EPA Method, 350.1, Rev. 2.0, 1993
Nitrogen, NO2 + NO3 – EPA Method, 353.2, Rev. 2.0, 1993
Nitrogen, Total Kjeldahl – EPA Method, 351.2, Rev. 2.0, 1993

CC. Finding: The lab is not using +10% recovery as the acceptance criterion for the QC
Sample (QCS).

Requirement: If the determined concentrations are not within ±10% of the stated
values, performance of the determinative step of the method is unacceptable.
Ref: EPA Method, 350.1, Rev. 2.0 (1993), Section 9.2.3, EPA Method, 351.2,
Rev. 2.0 (1993), Section 9.2.3 and EPA Method, 353.2, Rev. 2.0 (1993), Section
9.2.3.

Oil & Grease – EPA Method, 1664 Rev. B

DD. Finding: The method defined balance weights are not checked.

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.

Comment: The balance is only checked with a 100 mg weight daily.

EE. Finding: The Practical Quantitation Limit (PQL) is not being adjusted when less
than 1L of sample is being analyzed.

Requirement: Determine the original sample volume (Vs) in liters by filling the
sample bottle to the mark with water and measuring the volume of water in a 1- to
2-L graduated cylinder. If the sample weight was used (Section 11.1.4), weigh the
empty bottle and cap and determine Vs by difference, assuming a sample density
of 1.00. Ref: EPA Method 1664 Rev. B, Section 11.4.5.

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Comment: Three instances of incorrect PQLs were observed in the data reviewed
on 6/30/2015, 7/2/2015 and 7/7/2015 on samples from Carolina Seafood,
CRSWMA Interim Regional and Captain Neill’s Seafood, respectively.

Recommendation: It is recommended that the lab evaluate reported data to
determine whether amended reports are needed to demonstrate compliance.

pH – Standard Methods, 4500 H+ B-2000 – Field

Comment: Only one buffer is required for the mid-day and post analysis calibration
verification. Both the 4 S.U. and 7 S.U. buffers are currently being analyzed.

Specific Conductance – Standard Methods, 2510 B-1997 – Field and Lab
pH – Standard Methods, 4500 H+ B-2000 – Field and Lab

Comment: Duplicates are not required.

Specific Conductance – Standard Methods, 2510 B-1997 – Field and Lab

FF. Finding: The benchsheet for Specific Conductance does not include meter
calibration time. 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).

Requirement: The following must be documented in indelible ink whenever
sample analysis is performed: Meter Calibration Time. Ref: NC WW/GW LC
Approved Procedure for the Analysis of Specific Conductance (Conductivity).

Dissolved Oxygen - Standard Methods, 4500 O G-2001
Specific Conductance – Standard Methods, 2510 B-1997 – Field and Lab
pH – Standard Methods, 4500 H+ B-2000 – Field and Lab

GG. Finding: The units of measure are not all documented on the calibration logs.

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).

HH. Finding: The laboratory benchsheets and field log notebooks were lacking
pertinent data: Laboratory Name, Instrument identification.

Requirement: The following must be documented in indelible ink whenever
sample analysis is performed: Sample site including facility name and location,
ID, etc., Instrument Identification. Ref: NC WW/GW LC Approved Procedure for
the Analysis of Dissolved Oxygen, NC WW/GW LC Approved Procedure for the
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Analysis of pH, NC W W/GW LC Approved Procedure for the Analysis of Specific
Conductance (Conductivity).

Phenols, Inorganic – EPA Method, 420.1, Rev. 1978

II. Finding: The benchsheet does not have a space for the adjusted pH value or the
initial and final sample volumes. 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).

Requirement: Measure 500 mL sample into a beaker. Lower the pH to
approximately 4 with 1 + 9 H PO (7.1), add 5 mL CuSO solution (7.2) and transfer
to the distillation apparatus. Ref: EPA Method, 420.1, Rev. (1978). Section 8.1.1.

Requirement: Distill 450 mL of sample, stop the distillation, and when boiling
ceases add 50 mL of warm distilled water to the flask and resume distillation until
500 mL have been collected. Ref: EPA Method, 420.1, Rev. (1978). Section 8.1.2.

Residue, Dissolved – Standard Methods, 2540 C-1997

Recommendation: It is recommended to rinse the filter with a small portion of deionized
water just before sample introduction to ensure the filter is properly seated.

Residue, Total – Standard Methods, 2540 B-1997
Residue, Dissolved – Standard Methods, 2540 C-1997

Comment: Blanks are not required.

JJ. Finding: Sample drying times and temperatures cannot be verified. 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).

Requirement: Dry evaporated sample for at least 1 h in an oven at 103 to 105°C,
cool dish in desiccator to balance temperature, and weigh. Ref: Standard Methods,
2540 B-1997. (3) (b).

Requirement: Dry evaporated sample for at least 1 h in an oven at 180 + 2°C, cool
in a desiccator to balance temperature, and weigh. Ref: Standard Methods, 2540 C-
1997. (3) (d).

Comment: After the evaporation cycles at 98°C, the temperatures of the ovens are
increased to 105 and 180°C for the drying cycles. The lab is documenting the time
at which the ovens reach the drying cycle temperatures on a document which is not
retained.
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KK. Finding: The length of time samples are dried during the drying time study is not
documented.

Requirement: Constant weights must be documented. The approved Methods
require the following: “Repeat the cycle of drying, cooling, desiccating, and
weighing until a constant weight is obtained or until the weight change is less than
4% of the previous weight or 0.5 mg, whichever is less.” In lieu of this, an annual
study documenting the time required to dry representative samples to a constant
weight may be performed. Verify minimum daily drying time is greater than or
equal to the time used for the initial verification study drying cycle. Drying cycles
must be a minimum 1 hour for verification. Ref: NC WW/GW LC Policy.

Comment: The document which contains the drying time study does not include
the length of time samples were in the oven at the proper temperature. This makes
it impossible to determine the minimum amount of time verified by the drying time
study.

Comment: North Carolina allows for an annual drying study in lieu of the
requirement above to repeat the drying cycle for every sample. A random full set
of samples should be used for the drying study. The repeated drying time in the
oven should be at least 1 hour long. The time used for the annual drying study is
the minimum time that samples are to be dried until a new drying study is
performed.

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

Recommendation: It is recommended that duplicate samples agree within 5% of their
average weight.

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

Comment: The laboratory was analyzing duplicates at 5% frequency. Standard Methods,
2540 C-1997 (3) (d), 2540 B-1997 (3) (b), and 2540 D-1997 (3) (c) state: Analyze at least
10% of all samples in duplicate. Demonstration of acceptable corrective action (i.e., the
LIMS system was updated to require a duplicate analysis with every 10 samples with an
implementation date of 8/13/2015) was observed by the inspector on 8/12/2015. No
further response is necessary for this Finding but the laboratory is reminded to
make any applicable SOP revisions.

Comment: Incorrectly calculated results were observed on benchsheets / client reports for
Suspended Residue on 5/11/2015 [i.e., reported 107 mg/L (due to calculating with an
incorrect sample volume) but the correct result was 81.5 mg/L] and for Dissolved Residue
on 6/8/2015 (i.e., reported 290 mg/L (due to miscalculating the initial average weight) but
the correct result was 261 mg/L) and 7/7/2015 [i.e., reported 261 mg/L (due to calculating
with an incorrect sample volume] but the correct result was 522 mg/L). Standard Methods,
2540 D-1997. (4) and Standard Methods, 2540 C-1997. (4) state: Calculations:
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mg total dissolved solids/L = (A - B) x 100
Sample volume, mL

Where: A= weight of dried residue + dish, mg, and
B= weight of dish, mg.

mg total suspended solids/L = (A - B) x 100
Sample volume, mL

Where: A= weight of filter + dried residue, mg, and
B= weight of filter, mg.

Demonstration of acceptable corrective action (i.e., results were recalculated and
corrected reports were submitted to clients on 8/12/2015) was observed by the inspector
on 8/12/2015. No further response is necessary for this Finding.

Sulfate – Standard Methods, SO42 E-1997

LL. Finding: The lab is not analyzing a standard every three or four samples.

Requirement: Check reliability of calibration curve by running a standard with every
three or four samples. Ref: Standard Methods, SO42- E-1997. (4) (c).

MM. Finding: The lab is not analyzing a MSD.

Requirement: W hen 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).

Sulfide – Standard Methods, 4500 S²ˉ D-2000

Recommendation: It is recommended to document the wavelength used to analyze the
samples on the benchsheets (i.e., 664 nm).

Turbidity – Standard Methods, 2130 B-2001

NN. Finding: The lab is not retaining the documentation of the gel standard verification.
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).

Requirement: Not all secondary standards have to be discarded when comparison
with a primary standard shows that their turbidity value has changed. In some
cases, the secondary standard should be simply relabeled with the new turbidity
value. Ref: Standard Methods, 2130 B-2001. (3) (d).
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Comment: The verification of the Gel standard against prepared standards is
documented on an index card that is taped to the wall and the concentration is
written on the cap of the gel standard.

Mercury – EPA Method, 1631 E

OO. Finding: The lab is not recalibrating the instrument when more than 12 hours
have elapsed since verification of system performance.

Requirement: If system performance is verified at the end of an analytical batch
using the OPR, analysis of samples and blanks may proceed without recalibration,
unless more than 12 hours has elapsed since verification of system performance.
Ref: EPA 1631 E, Section 10.1.

Mercury – EPA Method, 245.1, Rev. 3.0, 1994 (Aqueous)

PP. Finding: The lab is not analyzing laboratory reagent blanks.

Requirement: Laboratory reagent blank (LRB) - The laboratory must analyze at
least one LRB (Section 7.11.2) with each batch of 20 or fewer samples of the same
matrix. Ref: EPA Method, 245.1, Rev. 3.0 (1994), Section 9.3.1.

Hardness – Standard Methods, 2340 C-1997
Mercury – EPA Method, 1631 E
Mercury – EPA Method, 245.1, Rev. 3.0, 1994 (Aqueous)
Metals – EPA Method, 200.7, Rev. 4.4, 1994

QQ. Finding: The laboratory is exceeding 1% sample volume with spiking solution
when preparing matrix spikes and is not using the proper correction factor when
calculating the final result.

Requirement: The volume of spike solution used in matrix spike preparation
must in all cases be ≤ 10% of the total matrix spike volume. It is preferable that
the spike solution constitutes ≤ 1% of the total matrix spike volume so that the
matrix spike can be considered a whole volume sample with no adjustment by
calculation necessary. If the spike solution volume constitutes >1% of the total
sample volume, the sample concentration or spike concentration must be
adjusted by calculation. Ref: NC WW/GW LC Policy.

Comment: See the NC WW/GW LC Matrix Spiking Technical Assistance
Document for further information, attached.

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

RR. Finding: The laboratory is using an acceptance criterion of ≤ the reporting limit
for the reagent, method and calibration blanks.

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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.

SS. Finding: The lab is not consistently analyzing matrix spikes at a frequency of
10%.

Requirement: The laboratory must add a known amount of each analyte to a
minimum of 10% of the routine samples. Ref: EPA Method, 200.7, Rev. 4.4 (1994),
Section 9.4.2.

Comment: For example, the data from April 6, 2015 contained 2 matrix spikes for
45 samples.

TT. Finding: The lab is not always waiting 24 hours after chemical preservation to
digest samples.

Requirement: However, acid must be added at least 24 hours before analysis to
dissolve any metals that adsorb to the container walls. Ref: Code of Federal
Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012;
Table II. Footnote 19.

UU. Finding: The lab is not using 5% as the acceptance criterion for the daily
Instrument Performance Check (IPC).

Requirement: Analysis of the IPC solution immediately following calibration must
verify that the instrument is within ±5% of calibration with a relative standard
deviation <3% from replicate integrations ≥4. Ref: EPA Method, 200.7, Rev. 4.4
(1994), Section 9.3.4.

Comment: The laboratory is using an acceptance criterion of ± 10%. The lab refers
to the IPC as ICV.

VV. Finding: The lab is not using 5% as the acceptance criterion for the quarterly QCS.

Requirement: To verify the calibration standards the determined mean
concentrations from three analyses of the QCS must be within ±5% of the stated
values. Ref: EPA Method, 200.7, Rev. 4.4 (1994), Section 9.2.3.

Comment: The laboratory is using an acceptance criterion of ± 10%.

WW. Finding: The lab is not using the method-defined acceptance criterion for Spectral
Interference Check (SIC) analyses.

Requirement: If the SIC solution confirms an operative interference that is ≥10% of
the analyte concentration, the analyte must be determined using a wavelength and
background correction location free of the interference or by another approved test
procedure. Ref: EPA Method, 200.7, Rev. 4.4 (1994), Section 7.14.

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XX. Finding: The lab is not adding the correct volume of (1+1) hydrochloric acid (i.e.,
1mL/100 mL of sample) to the sample.

Requirement: For the determination of total recoverable analytes in aqueous
samples (other than drinking water with <1 NTU turbidity), transfer a 100 mL (±1
mL) aliquot from a well-mixed, acid preserved sample to a 250 mL Griffin beaker
(Sections 1.2, 1.3, 1.6, 1.7, 1.8, and 1.9). (When necessary, smaller sample
aliquot volumes may be used.) Ref: EPA Method, 200.7, Rev. 4.4 (1994), Section
11.2.2.

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, 200.7,
Rev. 4.4 (1994), Section 11.2.3.

Comment: 5 mL of (1+1) hydrochloric acid is added to 50 mL of sample.

YY. Finding: Watch glasses are not being utilized during evaporation or reflux.

Requirement: The beaker should be covered with an elevated watch glass or other
necessary steps should be taken to prevent sample contamination from the fume
hood environment. Ref: EPA Method, 200.7, Rev. 4.4 (1994), Section 11.2.3.

Requirement: Cover the lip of the beaker with a watch glass to reduce additional
evaporation and gently reflux the sample for 30 minutes. Ref: EPA Method, 200.7,
Rev. 4.4 (1994), Section 11.2.5.

ZZ. Finding: The lab benchsheet does not document digestion start time. 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).

Requirement: However, acid must be added at least 24 hours before analysis to
dissolve any metals that adsorb to the container walls. Ref: Code of Federal
Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012;
Table II. Footnote 19.

AAA. Finding: The lab benchsheet does not document digestion end time. 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).

Requirement: Heat the sample and gently reflux for 30 minutes. Ref: EPA Method,
200.7, Rev. 4.4 (1994). Section 11.3.4.

Metals - Standard Methods, 3111 B-1999

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Recommendation: It is recommended that the lab periodically analyze field blanks.

BBB. Finding: The lab is not carrying standards through the same digestion procedure
used for samples.

Requirement: If digestion is used, carry standards through the same digestion
procedure used for samples. Ref: Standard Methods, 3111 A-1999. (5).

CCC. Finding: The lab is not adding a known amount of the metal of interest
approximately equal to the amount found in the sample after initial analysis and
reanalyzing to confirm recovery to one sample out of every ten.

Requirement: To one sample out of every ten (or one sample from each group of
samples if less than ten are being analyzed) add a known amount of the metal of
interest and reanalyze to confirm recovery. The amount of metal added should be
approximately equal to the amount found. If little metal is present add an amount
close to the middle of the linear range of the test. Recovery of added metal should
be between 85 and 115%. Ref: Standard Methods, 3111 A-1999. (7).

Mercury – EPA Method, 1631 E

DDD. Finding: The lab is not analyzing 10% of samples as MS/MSDs.

Requirement: To assess the performance of the Method on a given sample matrix,
the laboratory must spike, in duplicate, a minimum of 10% (1 sample in 10) from a
given sampling site or, if for compliance monitoring, from a given discharge.
Therefore, an analytical batch of 20 samples would require two pairs of MS/MSD
samples (four spiked samples total). Ref: EPA 1631 E, Section 9.3.

Metals – EPA Method, 200.8, Rev. 5.4, 1994
Nitrogen, Ammonia – EPA Method, 350.1, Rev. 2.0, 1993
Nitrogen, NO2 + NO3 – EPA Method, 353.2, Rev. 2.0, 1993

EEE. Finding: The lab is not analyzing 10% of samples as MSs.

Requirement: The laboratory must add a known amount of analyte to a minimum
of 10% of the routine samples. Ref: EPA Method, 200.8, Rev. 5.4, (1994), Section
9.4.2.

Requirement: The laboratory must add a known amount of analyte to a minimum
of 10% of the routine samples. Ref: EPA Method, 350.1, Rev. 2.0 (1993), Section
9.2.3 and EPA Method, 353.2, Rev. 2.0 (1993), Section 9.2.3.

Comment: The lab was analyzing 5% of samples as MSs.

Phosphorus, Total – EPA Method, 365.4, 1974
Chloride – Standard Methods, 4500 Cl- B-1997
Fluoride – Standard Methods, 4500 F- C-1997
Purgeable, Aromatics – Standard Methods, 6200 C-1997
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FFF. Finding: The lab is not analyzing MSDs.

Requirement: Incorporate the following twelve quality control elements, where
applicable, into the laboratory’s documented standard operating procedure (SOP)
for performing compliance analyses when using an approved part 136 method
when the method lacks such QA/QC procedures. One or more of the twelve QC
elements may not apply to a given method and may be omitted if a written rationale
is provided indicating why the element(s) is/are inappropriate for a specific method.
Ref: Code of Federal Regulations, Title 40, Part 136.7; Federal Register Vol. 77,
No. 97, May 18, 2012. (c) (1).

Requirement: Matrix spike (MS) and matrix spike duplicate (MSD), or laboratory
fortified matrix (LFM) and LFM duplicate, may be used for suspected matrix
interference problems to assess precision. Ref: Code of Federal Regulations,
Title 40, Part 136.7; Federal Register Vol. 77, No. 97, May 18, 2012. (c) (v).

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

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, Table 6020:I and (2) (f).

1,2-Dibromoethane – EPA Method, 504.1

Recommendation: TCMX surrogate calculation is based on a single point estimation.
Although surrogate analysis is not required by the method, it is recommended that
surrogate recovery be based upon a multi-level calibration curve.

Recommendation: It is recommended to optimize the temperature program of the oven.
This may alleviate the co-elution of 1,2,3-TCP with other analytes. The current resolution
requires either a qualifier to accompany the data or subcontracting of the analysis. There
are currently no laboratory clients under our program that require the reporting of this
analyte.

GGG. Finding: The lab is not weighing standard preparation flasks or sample bottles for
actual volume determination for standard preparation or samples.

Requirement: Allow the flask to stand, un-stoppered, for about 10 minutes and
weigh to the nearest 0.1 mg. Calculate the concentration in micrograms per
microliter from the net gain in weight. Replace the container cap and weigh the
container with contents to the nearest 0.1 g and record this weight for subsequent
sample volume determination (Section 11.3). Ref: EPA Method, 504.1, Sections
7.3.1, 7.3.3 and 11.1.2.

Pesticides, Organochlorine – SW846, 8081 B

Comment: The only data available for review was from PT samples.

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HHH. Finding: The lab is not preparing a surrogate calibration curve.

Requirement: For each analyte and surrogate of interest, prepare calibration
standards at a minimum of five different concentrations by adding volumes of one
or more stock standards to volumetric flasks and diluting to volume with an
appropriate solvent. Ref: EPA SW -846 Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods; 3rd Edition, Method 8000 B. Rev. 2, December 1996,
Section 7.4.1.1.

III. Finding: The use of manual integration is not properly documented.

Requirement: When manual integration is employed, the laboratory must clearly
identify manually integrated compounds, document the reason the manual
integration was performed, the date performed and who completed the work. A
flag or qualifier code may suffice for simple manual integrations. Ref: NC
WW/GW Policy.

Comment: The lab does not document the following when manual integrations are
performed for Organochlorine Pesticides by SW846 8081 B: the reason the
manual integration was performed, the date performed and who completed the
work.

JJJ. Finding: The laboratory is referencing an unapproved method on the extraction
log.

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: The extraction log references SW -846 Method 8080.

1,2-Dibromoethane – EPA Method 504.1
Purgeable, Halocarbons – EPA Method 601 & SW-846 8021 B
Purgeable, Aromatics – EPA Method 602 & SW-846 8021 B
Purgeable, Organics – EPA Method 624 & SW-846 8260 B
Base Neutral/Acid, Organics – EPA Method 625 & SW-846 8270 D
Pesticides, Organochlorine – SW-846 8081 B

KKK. Finding: Quality Control standards do not always contain all of the analytes of
interest.

Requirement: Quality Control Sample (QCS) -- A solution of method analytes of
known concentrations that is used to fortify an aliquot of LRB or sample matrix. Ref:
EPA Method 504.1, Rev. 1.1 (1995), Section 3.11.

Requirement: A quality control (QC) check sample concentrate is required
containing each parameter of interest at a concentration of 10 μg/mL in methanol.
Ref: EPA Method 601, Section 8.2.1 and EPA Method 602, Section 8.2.1.

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Requirement: Prepare the QC check sample as described in Section 8.2.2. EPA
Method 624, Section 7.4.1.

Requirement: A quality control (QC) check sample concentrate is required
containing each parameter of interest... Ref: EPA Method 625, Section 8.2.1.

Requirement: The solution used to fortify a sample and/or an LCS should contain
all of the target analytes and their concentration levels should be determined as
described in Secs. 9.4.1 and 9.4.2. Ref: EPA SW -846 Test Methods for Evaluating
Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 8000 D. Rev. 4,
July 2014, Section 9.4.2.

Requirement: Except where the determinative method contains alternative
calibration verification criteria, if the % Drift or % Difference is >± 20%, the initial
calibration relationship may no longer be valid. Ref: EPA SW -846 Test Methods for
Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 8000 D.
Rev. 4, July 2014, Section 11.7.

Requirement: It is the intent of the Environmental Protection Agency (EPA or the
Agency) that all target analytes for a particular analysis be included in the initial
calibration and calibration verification standard(s). These target analytes may not
include the entire list of analytes (Sec. 1.1) for which the method has been
demonstrated. However, the laboratory must not report a quantitative result for a
target analyte that was not included in the calibration standard(s). Ref: EPA SW -
846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd
Edition, Method 8021 B. Rev. 3, July 2014, Section 7.7.3.

Requirement: The initial calibration curve (Sec. 7.3) for each compound of interest
should be verified once every 12 hours prior to sample analysis, using the
introduction technique used for samples. This is accomplished by analyzing a
calibration standard at a concentration near the midpoint concentration for the
calibrating range of the GC/MS. Ref: EPA SW -846 Test Methods for Evaluating
Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 8260 B. Rev. 2,
December 1996, Section 7.4.2.

Requirement: The initial calibration (Sec. 11.3) for each compound of interest
should be verified once every twelve hours prior to sample analysis, using the
introduction technique and conditions used for samples. This is accomplished by
analyzing a calibration standard (containing all the compounds for quantitation) at a
concentration either near the midpoint concentration for the calibrating range of the
GC/MS or near the action level for the project. The results must be compared
against the most recent initial calibration curve and should meet the verification
acceptance criteria provided in Secs. 11.4.5 through 11.4.7. Ref: EPA SW -846
Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition,
Method 8270 D. Rev. 5, July 2014, Section 11.4.3.

Comment: Proficiency Testing samples do not contain all target analytes. The lab
is utilizing left over Proficiency Testing samples as Quality Control standards (i.e.,
calibration verification standards, second source standards, etc.)

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PAPER TRAIL INVESTIGATION:

The paper trail consisted of comparing original records (e.g., laboratory benchsheets,
logbooks, chain of custodies, etc.) and client reports. Data were reviewed for the
following project numbers: Client #s 1400 and 1001 for the parameters of Color, PC and
Inorganic Phenol on 5/6/2015 and 6/9/2015, respectively. 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. The inspector would
like to thank the staff for its assistance during the inspection and data review process.
Please respond to all Findings and include an implementation date for each
corrective action.

Report prepared by: Nick Jones Date: September 30, 2015
Report reviewed by: Jason Smith Date: October 29, 2015
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Matrix Spiking (NC WW/GW LC Policy 05/11/2012)

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 (MS) each month samples are analyzed. If MS results are out of control, the results must be
qualified or the laboratory must take corrective action to rectify the effect, use another method, or
employ the method of standard additions. When the method of choice specifies MS performance
acceptance criteria for accuracy, and the laboratory chooses to develop statistically valid,
laboratory-specific limits, the laboratory-generated limits cannot be less stringent than the criteria
stated in the approved method.

When spiking with multi-component standards, if the method does not specify the spiking
components, the Laboratory Control Spike (LCS) and MS must contain all analytes that are
reported.

If the unspiked sample result is in the top 40% of the calibration range, the sample should be
diluted and the MS prepared using the diluted sample. The recovery of the MS samples must be
bracketed by the calibration range.

The volume of spike solution used in MS preparation must in all cases be ≤ 10% of the total MS
volume. It is preferable that the spike solution constitutes ≤ 1% of the total MS volume so that the
MS can be considered a whole volume sample with no adjustment (i.e., volume correction) by
calculation necessary. If the spike solution volume constitutes >1% of the total sample volume,
the sample concentration or spike concentration must be adjusted by calculation.

Parameters Excluded from MS Requirements

Acidity Alkalinity
BOD/CBOD Aquatic Humic Substances
Chlorophyll All Bacteriological Parameters
Color – ADMI Color - PtCo
Conductivity Dissolved Oxygen
Ignitability All Residues
Paint Filter Test Turbidity
pH Temperature
Salinity Sulfite
Total Residual Chlorine Vector Attraction Reduction (All Options)

(Field Laboratories and Field Setting analyses are exempt.)