#329_2020_0113_MC_FINAL

Laboratory Cert. #:
329
Laboratory Name:
Pace South Carolina — Analytical Laboratory
Inspection Type:
Commercial Maintenance
Inspector Name(s):
Michael Cumbus, Beth Swanson, Todd Crawford, Dana Satterwhite, Tonja
Springer, Tom Halvosa, Jason Smith, Anna Ostendorff
Inspection Date:
January 13, 2020 — January 16, 2020
Date Forwarded for Initial
February 10, 2020
Review:
Initial Review by:
Anna Ostendorff
Date Initial Review
February 27, 2020
Completed:
❑ Insp. Initial ® Insp. Reg
Cover Letter to use:
❑Insp. No Finding ❑Insp. CP
❑Corrected
❑Insp. Reg. Delay
Unit Supervisor/Chemist III:
Beth Swanson
Date Received:
February 27, 2020
Date Forwarded to Admin.:
3/19/2020
Date Mailed:
Special Mailing Instructions:
Michael to send a copy to Bill Gintert w/ Charlotte Water

ROY COOPER
Governor
MICHAEL. S. REGAN
Secretary
S. DANIEL SMITH
Director
NORTH CAROLINA
Environmental Quality
March 20, 2020
329
Ms. Stephanie Atkins
Pace South Carolina - Analytical Laboratory
106 Vantage Point Dr.
West Columbia, SC 29172-
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW
LC) Maintenance Inspection
Dear Ms. Atkins:
Enclosed is a report for the inspection performed on January 13-16, 2020 by Michael Cumbus,
Beth Swanson, Todd Crawford, Dana Satterwhite, Tonja Springer, Tom Halvosa, Jason Smith,
Anna Ostendorff. I apologize for the delay in getting this report to you. Where Finding(s)
are cited in this report, a response is required. Within thirty days of receipt, please supply this
office with a written item for item description of how these Finding(s) were corrected. Please
describe the steps taken to prevent recurrence and include an implementation date for each
corrective action. If the Finding(s) cited in the enclosed report are not corrected, enforcement
actions may be recommended. For Certification maintenance, your laboratory must continue to
carry out the requirements set forth in 15A NCAC 2H .0800.
A copy of the laboratory's Certified Parameter List at the time of the audit is attached. This list
will reflect any changes made during the audit. Copies of the checklists completed during the
inspection may be requested from this office. Thank you for your cooperation during the
inspection. If you wish to obtain an electronic copy of this report by email or if you have
questions or need additional information, please contact me at [phone] Ext. 259.
Sincerely,
rr
Beth Swanson
Technical Assistance & Compliance Specialist
Division of Water Resources
Attachment
cc: Michael Cumbus, Dana Satterwhite
- North Carolina Department of Environmental Quality I Division of Water Resources
4405 Reedy Creek Road ( 1623 Mail Service Center j Raleigh, North Carolina 27699-1623
NORTHCAR UNA
DWd t fEmlroame Ulwa; 919,733.3908

CERTIFICATE :
Pace South Carolina — Analytical Laboratory
106 Vantage Point Drive
West Columbia, SC 29172
329
January 13, 2020 — January 16, 2020
Commercial Maintenance
Michael Cumbus, Beth Swanson, Todd Crawford, Dana Satterwhite,
Anna Ostendorff, Tom Halvosa, Tonja Springer and Jason Smith
Stephanie Atkins, Kristina Bouknight, Tracy Fowler, Dan Wright and
Brad Belding
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 02H .0800 for the analysis of environmental samples.
II. GENERAL COMMENTS:
The laboratory was neat and well -maintained. Staff were very forthcoming, knowledgeable,
engaged and seemed eager to adopt any necessary changes. The laboratory retains records
electronically and was easily able to produce any required data or information needed. Laboratory
Standard Operating Procedures (SOPs) do a good job of describing method modifications. The
laboratory has a robust manual integration SOP and training program. The laboratory's system of
standard and reagent traceability is thorough and effective.
- - All required- Proficiency Testing (PT) Samples for the 2020 PT Calendar Year have not yet been -
analyzed. The laboratory is reminded that results must be received by this office directly from the
vendor by September 30, 2020.
The laboratory submitted their Quality Assurance (QA) documents and/or SOPs in advance of
the inspection. These documents were reviewed and editorial and substantive revision
requirements and recommendations were made by this program outside of this formal report
process. Although subsequent revisions were not requested to be submitted, they must be
completed by March 1, 2021.
The laboratory is reminded that any time changes are made to laboratory procedures, the
laboratory must update the QA document(s) and/or SOPs and inform relevant staff. Any
changes made in response to the pre -audit review or to 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 documents) is in
agreement with each approved practice, test, analysis, measurement, monitoring procedure or

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regulatory requirement being used in the laboratory. In some instances, the laboratory may
need to create an SOP to document how new functions or policies will be implemented.
The laboratory is also reminded that SOPs are intended to describe procedures exactly as they
are to be performed. Use of the word "should" is not appropriate when describing requirements
(e.g., Quality Control (QC) frequency, acceptance criteria, etc.). Evaluate all SOPs for the proper
use of the word "should".
Laboratory Fortified Matrix (LFM) and Laboratory Fortified Matrix Duplicate (LFMD) are also
known as Matrix Spike (MS) and Matrix Spike Duplicate (MSD) and may be used
interchangeably in this report.
Documentation
Comment: Prior to our rules being updated, Flash Point and Ignitability methods were listed under
the same parameter heading. They are now listed under separated parameter headings. The
laboratory currently holds certification for Flash Point by SW-846 1010 A (Pensky-Martens)
(Aqueous). The laboratory is not certified for Ignitability. The laboratory needs to update the
benchsheet to say Flash Point instead of Ignitability.
A. Finding: Chemical containers are not consistently dated when received and opened.
Requirement: Chemical containers shall be dated when received and when opened.
Reagent containers shall be dated, identified, and initialed when prepared. Chemicals and
reagents exceeding the expiration date shall not be used. The laboratory shall have a
documented system of traceability for the purchase,, preparation, and use of all chemicals,
reagents, standards, and consumables. Ref: 15A NCAC 02H .0805 (a) (7) (K).
Comment: During the walk-through of the laboratory, it was discovered that a bottle of
sodium sulfite (laboratory ID# 18-1850B) was lacking the date opened on the bottle.
B. Finding: Temperature measuring device documentation does not always include the
correct serial number.
Requirement: To check a temperature -measuring device, read the temperature of the
temperature -measuring device against a_ Reference Temperature -Measuring Device and
record the two temperatures, the serial number (or other unique identifier) of each device,
the date the calibration was verified and the signature/initials of the analyst. Ref: NC
WW/GW LC Policy.
Comment: For waterbath M10, the serial number on the back of the temperature -
measuring device is 17076882 and the verification sticker says 122403854. The
thermometer verification log shows waterbaths M10 and M8 as having temperature -
measuring devices with identical serial numbers.
C. Finding: The laboratory benchsheet does not clearly state when sample reduction is
performed for samples prepared by SW-846 Method 1311 and SW-846 Method 1312. This
is considered pertinent data.
Requirement: Weigh out a small subsample of the solid phase of the waste, reduce the
solid (if necessary) to a particle size of approximately 1 mm in diameter or less, and
transfer 5.0 g of the solid phase of the waste to a 500 mL beaker or Erlenmeyer flask. Ref:

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EPA SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd
Edition, Method 1311. Rev. 0, July 1992, Section 7.1.4.1.
Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data
shall be traceable to the associated sample analyses and shall consist of: sample
preparation, where applicable. Each item shall be recorded each time that samples are
analyzed. Ref: 15A NCAC 02H .0805 (a) (7) (F) (x).
Requirement: All analytical records, including original observations and information
necessary to facilitate historical reconstruction of the calculated results, shall be maintained
for five years. All analytical data and records pertinent to each certified analysis shall be
available for inspection upon request. Ref: 15A NCAC 02H .0805 (a) (7) (E).
Requirement: Prepare the solid portion of the waste for extraction by crushing, cutting, or
grinding the waste to a surface area or particle size as described in Section 7.1.3. When
the surface area or particle size has been appropriately altered, quantitatively transfer the
solid material into an extractor bottle. Include the filter used to separate the initial liquid from
the solid phase. Ref: EPA SW-846 Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods; 3rd Edition, Method 1311. Rev, 0, July 1992, Section 7.2.10.
Comment: Only one checkbox for each sample, indicating yes/no, is listed on the
benchsheet. This does not clearly demonstrate if the size reduction is performed during
fluid determination, extraction, or both.
D. Finding: Units of measure are not consistently documented.
Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data
shall be traceable to the associated sample analyses and shall consist of: the proper units
of measure. Each item shall be recorded each time samples are analyzed. Ref: 15 NCAC
02H .0805 (a) (7) (F) (viii).
Comment: This Finding applies to the units of measure for pH on the Analytical Batch
sheet for Oil & Grease. EPA Method 1664, Rev. B (Aqueous).
Comment: This Finding applies to the "PQL" column on the Analytical Batch sheet for the
following analyses:
® Nitrogen, Ammonia - EPA Method 350.1, Rev. 2.0, 1993 (Aqueous)
• Phosphorus, Total - EPA Method _365.1,_Rev. 2.0, 1993 (Aqueous)
® Fluoride - SW-846 9056 A (Aqueous & Non -Aqueous)
® Chloride - SW-846 9056 A (Aqueous & Non -Aqueous)
® Sulfate - SW-846 9056 A (Aqueous & Non -Aqueous)
® Nitrogen, Total Kjeldahl - EPA Method 351.2, Rev. 2.0, 1993 (Aqueous)
® Organic Carbon, Total - SM 5310 C-2011 (Heated Persulfate) (Aqueous)
® Organic Carbon, Total - SW-846 9060 A (Heated Persulfate) (Aqueous)
® Inorganic Phenols - EPA Method 420.4, Rev. 1.0, 1993 (Aqueous)
® Inorganic Phenols - SW-846 9065 (Aqueous)
® Cyanide - EPA Method 335.4, Rev. 1.0, 1993 (Total) (Aqueous)
® Cyanide - SW-846 9012 B (Total) (Aqueous & Non -Aqueous)
® Cyanide - SM 4500 CN- E-2011 (Total) (Aqueous)
® Cyanide - Lachat 10-204-00-1-X, Rev. 2.2, 2005 (SM 4500 CN E-2011 Automated)
(Total) (Aqueous)

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Comment: This Finding applies to the "PQL" and "TV" columns on the Analytical Batch
sheets for the following analyses:
® Residue, Total — SM 2540 B-2011 (Aqueous)
® Residue, Suspended — SM 2540 D-2011 (Aqueous)
® Residue, Dissolved 180 C — SM 2540 C-2011 (Aqueous)
Comment: This Finding applies to the "Instrument Reading" and "PQL" columns on the
"Turbidity Analytical Batch" benchsheet.
Comment: The laboratory benchsheet for Paint Filter Liquids includes a column for sample
amount. This column lists "Sample Volume (ml-) or Sample Weight (g)" but there is no
indication which units of measure are being used in the analytical batch.
E. Finding: The laboratory is not documenting the adjusted sample pH for Total Hardness.
Requirement: Add 1 to 2 mL buffer solution. Usually 1 mL will be sufficient to give a pH of
10.0 to 10.1. Ref: Standard Methods, 2340 C-2011. (3) (b).
Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data
shall be traceable to the associated sample analyses and shall consist of: sample
preparation, where applicable. Each item shall be recorded each time that samples are
analyzed. Ref: 15A NCAC 02H .0805 (a) (7) (F) (x).
Comment: The analyst is checking that the pH is adequately adjusted with pH strips but
does not document this.
F. Finding: The laboratory is not documenting the true value of QC standards on the
Ammonia Nitrogen and Anions Analytical Batch sheets.
Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data
shall be traceable to the associated sample analyses and shall consist of: all quality control
assessments. Each item shall be recorded each time samples are analyzed. Ref: 15 NCAC
02H .0805 (a) (7) (F) (xv).
G. Finding: The EPH laboratory benchsheets do not adequately differentiate between the
aliphatic and aromatic fractions.
Requirement: All laboratories shall use printable laboratory_ benchsheets._ Certified_ Data
shall be traceable to the associated sample analyses and shall consist of: sample
identification. Ref: 15A NCAC 02H .0805 (a) (7) (F) (ix).
Comment: Sample Preparation Batch sheets for batch numbers #96848/96849 and
#96888/96889 had separate batch numbers for each fraction, but there was nothing to
distinguish the fractions from each other.
H. Finding: The laboratory benchsheet for Inorganic Phenols does not fully reference the
approved methods.
Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data
shall be traceable to the associated sample analyses and shall consist of: the method or
Standard Operating Procedure. Each item shall be recorded each time samples are
analyzed. Ref: 15 NCAC 02H .0805 (a) (7) (F) (i).

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Comment: The reference year is not included on the benchsheet. Only "420.4" is included
for the EPA method.
I. Finding: The laboratory is not documenting the adjustment of the Inorganic Phenols
sample pH to 4 S.U. prior to distillation. This is considered pertinent data.
Requirement: Measure 500 mL sample into a beaker. Adjust the pH to approximately 4
with 1+9 NaOH (Section 7.9) or 1+9 H2SO4 (Section 7.10), and transfer to the distillation
apparatus. Ref: EPA Method 420.4, Rev. 1.0 (1993), Section 11.1.1.
Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data
shall be traceable to the associated sample analyses and shall consist of: sample
preparation, where applicable. Ref: 15 NCAC 02H .0805 (a) (7) (F) (x).
Comment: The laboratory is adjusting and checking the pH of the sample as required prior
to distillation but does not document this.
Quality Control
Comment: During the verification of the temperature -sensing devices performed on January 2,
2020, the device with serial number 170768875, used in fecal waterbath M10, was found to
have a correction factor of-0.3°C. North Carolina Administrative Code, 15A NCAC 02H .0805
(a) (7) (N) states: All temperature -measuring devices shall have accuracy that meets or exceeds
one-half the tolerance required for its intended use. NC WW/GW LC Policy states: Incubators
with an incubation temperature tolerance of ± 0.2 °C (e.g., fecal coliform incubators) must have
temperature measuring devices with a stated accuracy of ± 0.1 'C. If the temperature -measuring
device reading differs from the Reference Temperature -Measuring Device reading by more than
0.1 °C during subsequent verifications, the temperature -measuring device must be recalibrated
or replaced. A Notice of Finding for Immediate Response was issued and a response time of
three weeks was negotiated with the laboratory. Acceptable corrective action [i.e., the laboratory
located a thermometer (serial number 192621163) with a stated accuracy of ± 0.1°C and a
correction factor of 0.0°C, and put it into use on January 13, 2020] was witnessed by the auditor
during the inspection.
J. Finding: The laboratory is not analyzing or back -calculating a standard at the same
concentration as the lowest reporting concentration each day samples are analyzed.
Requirement: For analytical procedures requiring analysis of a series of standards, the
concentrations of these standards shall bracket the range of the sample concentrations
measured. One of the standards shall have a concentration equal to or less than the
laboratory's lowest reporting concentration for the parameter involved. All data sets shall
reference the corresponding calibration. Laboratories shall analyze or back -calculate a
standard at the same concentration as the lowest reporting concentration each day
samples are analyzed. Ref: 15A NCAC 02H .0805 (a) (7) (H).
Comment: This Finding was noted for the following parameter methods:
• Purgeable, Organics — SW-846 8260 D (Aqueous & Non -Aqueous)
• Purgeable, Organics — EPA Method 624.1 (Aqueous)
• Purgeable, Organics — SM 6200 B-2011 (Aqueous & Non -Aqueous)
• TPH Gasoline Range, Organics — SW-846 8015C (Aqueous & Non -Aqueous)
• Non -Halogenated Volatile, Organics — SW-846 8015 C (Aqueous & Non -Aqueous)
• Chlorinated Acid Herbicides — SW-846 8151 A (Aqueous & Non -Aqueous)

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® Volatile Petroleum Hydrocarbons — MADEP, February 2018, Rev. 2.1 (Aqueous &
Non -Aqueous)
® COD — SM 5220 D-2011 (Aqueous) (High Range Curve Only)
® Nitrogen, Nitrite — EPA 300.0, Rev. 2.1 (Aqueous & Non -Aqueous)
® Nitrogen, Nitrite — SW-846 9056A (Aqueous & Non -Aqueous)
® Nitrogen, Nitrite — EPA 353.2, Rev. 2.0 (Aqueous)
® Nitrogen, Nitrate — EPA 300.0, Rev. 2.1, 1993 (Aqueous & Non -Aqueous)
® Nitrogen, Nitrate — SW-846 9056A (Aqueous & Non -Aqueous)
® Nitrogen, Nitrate — (NO3+NO2 EPA 353.2, Rev. 2.0, 1993) — (NO2 EPA 353.2, Rev.
2.0, 1993) (Aqueous)
® Nitrogen, NO3 + NO2 — EPA 353.2, Rev. 2.0, 1993 (Aqueous)
® TPH Diesel Range, Organics — SW-846 8015C (Aqueous & Non -Aqueous)
® Base Neutral/Acid, Organics — EPA Method 625.1 (Aqueous)
® Base Neutral/Acid, Organics — SW-846 8270 E (Aqueous & Non -Aqueous)
® Pesticides, Organochlorine — EPA Method 608.3 (Aqueous)
® Pesticides, Organochlorine — SW-846 8081 B (Aqueous & Non -Aqueous)
® Polychlorinated Biphenyls — EPA Method 608.3 (Aqueous)
® Polychlorinated Biphenyls — SW-846 8082 A (Aqueous & Non -Aqueous)
® Extractable Petroleum Hydrocarbons — MADEP, May 2004, Rev. 1.1 (Aqueous &
Non -Aqueous)
K. Finding: Initial accuracies for temperature -measuring devices used in incubators with
tolerance of ± 0.2°C do not have a stated accuracy of ± 0.1 °C from the manufacturer.
Requirement: Incubators with an incubation temperature tolerance of ± 0.2°C (e.g., fecal
coliform incubators) must have temperature -measuring devices with a stated accuracy of ±
0.1 °C. Ref: NC WW/GW LC Policy.
Comment: The temperature -measuring devices in use at the time of the inspection had all
been verified by the laboratory since being put into use and were found to be within the
required accuracy limits. This Finding will apply to all temperature -measuring devices put
into use after the inspection.
L. Finding: The laboratory is not rotating the range of spike concentrations, where applicable.
Requirement: To prepare an LFM, add a known concentration of analytes (ideally from a
secondsource)_ to a_ randomly selected routine sample without increasing its volume by
more than 5%. Ideally, the new concentration should be at or below the midpoint of the
calibration curve, and for maximum accuracy, the spike should approximately double the
sample's original concentration. If necessary, dilute the spiked sample to bring the
measurement within the calibration curve. Also, rotate the range of spike concentrations to
verify performance at various levels. Ref: Standard Methods, 4020 B-2011. (2) (g).
Requirement: To prepare an LFM, add a known concentration of analytes (ideally from a
second source) to a randomly selected routine sample without increasing its volume by
more than 5%. Ideally, the new concentration should be at or below the midpoint of the
calibration curve, and for maximum accuracy, the spike should approximately double the
sample's original concentration. If necessary, dilute the spiked sample to bring the
measurement within the calibration curve. Also, rotate the range of spike concentrations to
verify performance at various levels. Ref: Standard Methods, 5020 B-2011. (2) (g).
Comment: The spike concentration was not found to be varied for the following parameter
methods:

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® Sulfide — SM 4500 S2- F-2011 (Aqueous)
® Cyanide — SM 4500 CN- E-2011 (Aqueous)
® COD — SM 5220 D-2011 (Aqueous)
® MBAS — SM 5540 C-2011 (Aqueous)
® TOC — SM 5310 C-2011 (Heated Persulfate) (Aqueous)
M. Finding: The laboratory is not adjusting the sample concentration in the percent recovery
calculation when the spike volume is >1% of the total sample volume.
Requirement: The volume of spike solution used in MS preparation must in all cases be <_
5% 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 must be adjusted by
calculation. Ref: NC WW/GW LC Policy.
Comment: For analysis of Total Phosphorus by EPA Method 365.1, Rev. 2.0, the
laboratory is diluting 1 mL of spiking solution to a final volume of 25 mL with sample,
yielding a volume of spike solution of 4%.
Comment: The laboratory is using 2% Metals spike solution per total volume to prepare
the LFM/LFMD by preparation methods SW-846 1311, 1312 and 3050, for analysis by SW-
846 Method 6020B (Aqueous).
Comment: For analysis of TKN by EPA Method 351.2, Rev. 2.0, the laboratory is spiking 1
mL of spike solution into 25 mL of sample. This volume of spike solution constitutes 4% of
the total sample volume.
Comment: For analysis of Nitrite Nitrogen, Nitrate Nitrogen and NO3 + NO2 Nitrogen, the
volume of spike solution used constitutes 2% of the total sample volume.
N. Finding: The matrix spike solution volume constitutes > 5% of the total sample volume.
Requirement: The volume of spike solution used in MS preparation must in all cases be <_
5% 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 must be adjusted by
calculation. Ref: NC WW/GW LC Policy.
Comment: The laboratory prepares the Ammonia Nitrogen MS/MSD by spiking 5 mL of
the Initial Calibration Verification (ICV)/Laboratory Control Sample (LCS) Intermediate
Standard into a final volume of 50 mL of sample. This constitutes 10% of the total MS
volume.
O. Finding: The laboratory is not calculating the MS percent recovery properly.
Requirement: If the sample concentration is below the reporting limit, use zero for amount
of target in the unspiked sample. Ref: NC WW/GW LC Policy.
Comment: The LIMS is subtracting actual calculated concentrations for the unspiked
sample from the spiked sample when the unspiked sample concentration is below the
reporting limit.

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Comment: The following parameter methods were found to have MS percent recovery
improperly calculated:
® Nitrogen, Ammonia — EPA Method 350.1, Rev. 2.0, 1993 (Aqueous)
® Sulfide - Standard Methods, 4500 S2- F-2011 (Aqueous)
® Anions (Cl-, F-, Br, S042- , NO2 , NO3) — EPA 300.0, Rev. 2.1, 1993 (Aqueous &
Non -Aqueous)
® Anions (Cl-, F-, Br, S042-, NO2 , NO3) — SW-846 9056 A (Aqueous & Non -Aqueous)
® Nitrogen, Nitrite — EPA 353.2, Rev. 2.0, 1993 (Aqueous)
® Nitrogen, Nitrate — (NO3+NO2 EPA 353.2, Rev. 2.0, 1993) — (NO2 EPA 353.2, Rev.
2.0, 1993) (Aqueous)
® Nitrogen, NO3 + NO2 — EPA 353.2, Rev. 2.0, 1993 (Aqueous)
® Organic Carbon, Total — Standard Methods, 5310 C-2011 (Aqueous)
® Organic Carbon, Total — SW-846 9060 A (Aqueous)
® Inorganic Phenols — EPA Method 420.4, Rev. 1.0, 1993 (Aqueous)
® Inorganic Phenols — SW-846 9065 (Aqueous)
® Cyanide - EPA Method 335.4, Rev. 1.0, 1993 (Total) (Aqueous)
® Cyanide - SW-846 9012 B (Total) (Aqueous & Non -Aqueous)
® Cyanide — Standard Methods, 4500 CN E-2011 (Total) (Aqueous)
® Cyanide - Lachat 10-204-00-1-X, Rev. 2.2, 2005 (Standard Methods, 4500 CN E-
2011 Automated) (Total) (Aqueous)
P. Finding: Method blanks (MB) and Laboratory Fortified Blanks (LFB) are not being
prepared with the associated preservative.
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).
Requirement: A laboratory -fortified blank (laboratory control standard (LCS)) is a reagent
water sample (with associated preservatives) to which a known concentration of the
analyte(s) of interest has been added. Ref: Standard Methods, 1020 B-2011 (6).
Requirement: Laboratory Reagent Blank (LRB) - An aliquot of reagent water or other
blank matrices that are treated exactly as a sample including exposure to all glassware,
equipment, solvents, reagents, and internal standards that are used with other samples.
The LRB is used to determine if method analytes or other interferences are present in
the laboratory environment, reagents, or apparatus (Sections 7.6.2 and 9.3.1). Ref: EPA
Method 200.8, Rev. 5.4, 1994, Section 3.10
Requirement: Laboratory Fortified Blank (LFB) - An aliquot of LRB to which known
quantities of the method analytes are added in the laboratory. The LFB is analyzed
exactly like a sample, and its purpose is to determine whether the methodology is in
control and whether the laboratory is capable of making accurate and precise
measurements (Sections 7.9 and 9.3.2). Ref: EPA Method 200.8, Rev. 5.4, 1994,
Section 3.8
Requirement: Laboratory Fortified Blank (LFB) -- An aliquot of reagent water or other
blank matrices to which known quantities of the method analytes are added in the
laboratory. The LFB is analyzed exactly like a sample, and its purpose is to determine
whether the methodology is in control, and whether the laboratory is capable of making
accurate and precise measurements. Ref: EPA Method 365.1, Rev. 2.0 (1993), Section
3.4.

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Requirement: Laboratory Reagent Blank (LRB) -- An aliquot of reagent water or other
blank matrices that are treated exactly as a sample including exposure to all glassware,
equipment, solvents, reagents, internal standards, and surrogates that are used with
other samples. The LRB is used to determine if method analytes or other interferences
are present in the laboratory environment, the reagents, or the apparatus. Ref: EPA
Method 365.1, Rev. 2.0 (1993), Section 3.6.
Requirement: Method blank — Prepare by a processing either a volume of reagent
water equal to that used for actual aqueous samples, or, otherwise, a clean, empty
container, equivalent to that used for actual solid samples through all of the preparatory
and instrument determination steps used for making ICP-MS determinations in samples.
These steps may include, but are not limited to, pre -filtering, digestion, dilution, filtering,
and analysis (refer to Sec. 9.5). Ref: EPA SW-846 Test Methods for Evaluating Solid
Waste, Physical/Chemical Methods; 3rd Edition, Method 6020B, Rev. 2, July 2014, Section
7.22.2.
Requirement: The LCS consists of an aliquot of a clean (control) matrix similar to the
sample matrix and of the same weight or volume. The LCS should be spiked at the
same levels and using the same spiking materials as the corresponding MS/MSD (see
above Sec. 9.7.2). Ref: EPA SW-846 Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods; 3rd Edition, Method 6020B, Rev. 2, July 2014, Section 9.7.3.
Requirement: The LCS sample is prepared and analyzed in the same analytical batch
and in exactly the same manner as the other routine samples. Ref: EPA SW-846 Test
Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition, Chapter
One, Rev. 2, July 2014, Section 1.5.
Comment: The following analyses were found to have MB and LFB lacking the associated
preservative:
• COD — SM 5220 D-2011 (Aqueous)
• Hardness Total — SM 2340 C-2011 (Aqueous)
• Metals — EPA Method 200.8, Rev. 5.4, 1994 (Aqueous)
• Metals — SW-846 6020B (Aqueous & Non -Aqueous)
• Phosphorus, Total — EPA Method 365.1, Rev. 2.0, 1993 (Aqueous)
Comment: For Hardness samples, 40 CFR Part 136.6 states that samples may be
preserved- with either HNO3 or H2SO4. However, theChainof Custody (COC) observed -
documented preservation of a Hardness sample with H2SO4 (sample ID# UC13072-001).
The analyst stated that samples are typically preserved with HNO3. Care must be taken to
ensure the correct preservative is added to the MB and LFB, or analyze 2 MB, each
prepared with one preservative, if both acids are used routinely in samples.
Q. Finding: An acceptance criterion has not been established for the precision of duplicates.
Requirement: Unless specified by the method or this Rule, each laboratory shall establish
performance acceptance criteria for all quality control analyses. Each laboratory shall
calculate and document the precision and accuracy of all quality control analyses with each
sample set. When the method of choice specifies performance acceptance criteria for
precision and accuracy, and the laboratory chooses to develop laboratory -specific limits,
the laboratory -specific limits shall not be less stringent than the criteria stated in the
approved method. Ref: 15A NCAC 02H .0805 (a) (7) (A).

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Comment: This finding applies to the following parameter methods:
® 1,2-Dibromoethane (EDB) — EPA Method 504.1 (Aqueous)
® 1,2-Dibromoethane (EDB) — SW-846 8011 (Aqueous)
® Mercury — EPA Method 245.1, Rev. 3.0, 1994 (Aqueous)
® Mercury — SW-846 Method 7470 A (Aqueous)
® Mercury — SW-846 Method 7471 B (Non -Aqueous)
R. Finding: The Instrument Performance Check (IPC) standard is not at a mid -range
concentration, where required by the method.
Requirement: For all determinations the laboratory must analyze the IPC (a mid -range
check standard) and a calibration blank immediately following daily calibration, after every
tenth sample (or more frequently, if required), and at the end of the sample run. Analysis of
the IPC solution and calibration blank immediately following calibration must verify that the
instrument is within ±10% of calibration. Ref: EPA 420.4, Revision 1.0 (1993), Section
9.3.4.
Requirement: For all determinations, the laboratory must analyze the IPC (a mid -range
check standard) and a calibration blank immediately following daily calibration, after every
tenth sample (or more frequently, if required) and at the end of the sample run. Ref: EPA
Method 350.1, Rev. 2.0 (1993), Section 9.3.4.
Requirement: For all determinations, the laboratory must analyze the IPC (a mid -range
check standard) and a calibration blank immediately following daily calibration, after every
tenth sample (or more frequently, if required) and at the end of the sample run. Ref: EPA
Method 180.1, Rev. 2.0 (1993), Section 9.3.2.
Comment: Due to EPA Method 180.1 requirements, no standard or sample reading > 40
NTU is deemed valid. The laboratory is using calibration standards of 0.02, 10.0 and 1000
NTU. Based on those concentrations, the valid calibration range is 0.02 — 10 NTU. The
laboratory has two options to meet the concentration requirement for the IPC solution;
Replace the 1000 NTU calibration standard with a 20.0 NTU calibration standard. This
would make the current IPC (ICV) concentration mid -range; or replace the 1000 NTU
calibration with a 40.0 NTU calibration standard and prepare a second -source IPC (ICV)
solution at a concentration of 20.0 NTU to satisfy the requirement. Alternatively, the
laboratory may switch to Standard Methods 2130 B-2011, which does not require diluting
samples/standards with a turbidity greater than 40 NTU or the analysis of a mid -range
standard
Comment: For Ammonia Nitrogen by EPA Method 350.1, Rev. 2.0, 1993, the laboratory
analyzes a 1.0000 mg/L IPC Solution, which it calls the ICV and CCV. The range of the
calibration is 0.0000 - 5.0000 mg/L. A 2.5000 mg/L IPC Solution would be required.
Comment: For Inorganic Phenols by EPA Method 420.4, Rev. 1.0, 1993, the laboratory is
analyzing an ICV with a concentration of 0.08 mg/L. The range of the calibration is 0.005 —
0.10 mg/L. A 0.05 mg/L IPC solution would be required.
S. Finding: The laboratory is not evaluating the recoveries of the back -calculated standards.
Requirement: Each laboratory shall develop documentation outlining the analytical quality
control practices used for the Parameter Methods included in its Certification, including
Standard Operating Procedures for each certified Parameter Method. Quality assurance,
quality control, and Standard Operating Procedure documentation shall indicate the

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effective date of the document and be reviewed every two years and updated if changes in
procedures are made. Each laboratory shall have a formal process to track and document
review dates and any revisions made in all quality assurance, quality control, and Standard
Operating Procedure documents. Supporting Records shall be maintained as evidence that
these practices are implemented. The quality assurance, quality control, and Standard
Operating Procedure documents shall be available for inspection by the State Laboratory.
Ref: 15A NCAC 02H .0805 (a) (7).
Requirement: The back -calculated and true concentrations should agree within ± 10%,
unless different criteria are specified in an individual method. At the lower limit of the
operational range, acceptance criteria are usually wider. Such criteria must be defined in
the laboratory's QA plan. Ref: Standard Methods, 4020 B-2011. (2) (a).
Comment: The back calculation is being done by the software but no acceptance criteria
have been established.
Comment: This Finding applies to the following parameter methods:
® Cyanide - SM 4500 CN- E-2011 (Total) (Aqueous)
® Cyanide - Lachat 10-204-00-1-X, Rev. 2.2, 2005 (SM 4500 CN E-2011 Automated)
(Total) (Aqueous)
® Cyanide - SW-846 9012 B (Total) (Aqueous)
® Cyanide - EPA Method 335.4, Rev. 1.0, 1993 (Total) (Aqueous)
Reporting
T. Finding: Data that does not meet all QC requirements is not always qualified on the client
report.
Requirement: Reported data associated with quality control failures, improper sample
collection, holding time exceedances, or improper preservation shall be qualified as
such. Ref: 15A NCAC 02H .0805 (e) (5).
Comment: The laboratory qualifier "S", which is used to denote matrix spike recovery
failures, transfers to the client report only for Department of Defense (DOD) samples. It
does not transfer for any other programs. One SW-846 Method 7199 data pack that was
examined contained a sample with matrix spike recoveries of 71% and 73%, and the client
report was lacking the "S" qualifier.
Comment: The following samples from NC clients, found in TKN analytical batch #16489,
were bracketed by blanks that were not less than half the reporting limit: UE07063-002;
UE07090-001; UE08089-003 and UE09055-002.
Comment: For the analysis of Hexavalent Chromium, samples that did not meet the
conditions of Code of Federal Regulations, Title 40, Part 136.3; Federal Register Vol. 82,
No. 165, August 28, 2017; Table II, Footnote 2 and Footnote 20, were not qualified when
analyzed outside of the stated holding time of 24 hours.
U. Finding: It is unclear from the client report and Field Analysis benchsheet that Field
Parameter analyses for NC clients are performed by the laboratory's Field Commercial
facility in Charlotte, NC (Certificate #5639)
Requirement: If a certified laboratory refers or subcontracts analysis of samples to
another laboratory certified for the Parameter, the referring laboratory shall supply the

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date and time that samples were collected to insure holding times are met. All record
transcriptions of subcontracted samples shall state that the collection site is in North
Carolina. Laboratories may subcontract sample fractions, extracts, leachates, and other
sample preparation products provided that adherence to 15A NCAC 02H .0800 is
documented. The initial client requesting the analyses shall receive the original or a copy
of the report made by the laboratory that performs the analyses. Each reported result
shall be traceable to the laboratory that performed the analysis on the final report. Ref:
15A NCAC 02H .0805 (e) (2).
Comment: This was noted for sample ID# UK060107-003 (date of analysis: 11/6/2019).
Alkalini — Standard Methods, 2320 B-2011 (Aqueous)
Comment: Per the 22nd Edition errata, a method blank is not required to be analyzed. The
laboratory is currently analyzing one blank for every 10 samples.
Comment: Samples < 1000 mg/L are analyzed with an automated instrument. Samples >1000
mg/L are analyzed manually.
Comment: Alkalinity is a method -defined parameter, and therefore must be followed as written.
Recommendation: It is recommended that the laboratory not analyze a method blank. Analysis of
high-level samples causes all blanks to have a value > 1/2 the limit of quantitation (LOQ).
V. Finding: The laboratory is not titrating samples to a single endpoint.
Requirement: Potentiometric titration to preselected pH: Determine the appropriate end-
point pH according to 2320B.1b. Prepare sample and titration assembly (Section
2310B.4c). Titrate to the end -point pH without recording intermediate pH values and
without undue delay. As the end point is approached make smaller additions of acid and be
sure that pH equilibrium is reached before adding more titrant. Ref: Standard Methods,
232013-2011, (4) (c).
Comment: The current end point range of 4.5 ± 0.3 S.U. allows for multiple endpoints.
Recommendation: It is recommended that the laboratory tighten the acceptance range for
the final pH to 4.46-4.55 S.U. to ensure a consistent single end point.
W. Finding: The laboratory is not verifying the pH meter calibration for automated sample
analysis.
Requirement: Titrate at room temperature with a properly calibrated pH meter or
electrically operated titrator, or use color indicators. Ref: Standard Methods, 2320 B-2011.
(1) (d).
Requirement: Immerse in a third buffer below pH 10, approximately 3 pH units different
from the second; the reading should be within 0.1 unit for the pH of the third buffer. Ref:
Standard Methods, 4500 H+B-2011. (4) (a).
X. Finding: The laboratory is not performing the required boiling and cooling steps in the
titrant standardization process.

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Requirement: Prepare acid solution of approximately 0.1N and determine exact normality
as follows. Standardize against 40.00 mL 0.05N Na2CO3 solution, with about 60 mL water,
in a beaker by titrating potentiometrically to pH of about 5. Lift out electrodes, rinse into the
same beaker, and boil gently for 3 to 5 minutes under a watch glass cover. Cool to room
temperature, rinse cover glass into beaker and finish titrating to the pH inflection point. Ref:
Standard Methods, 2320 B-2011. (3) (b).
Comment: The laboratory is currently standardizing by titrating directly to the 4.5 S.U.
endpoint, rather than titrating to 5 S.U., boiling, cooling and then completing the titration.
Y. Finding: The laboratory is not properly reporting the results of analysis.
Requirement: Report pH of end point used as follows: "The alkalinity to pH ® = ® mg
CaCO3/U and indicate clearly if this pH corresponds to an inflection point of the titration
curve. Ref: Standard Methods, 2320 B-2011. (5) (a).
Comment: The laboratory is currently reporting only the results, and not including the pH to
which the samples are titrated and whether the pH endpoint corresponds to the inflection
point.
Z. Finding: The laboratory is not using the appropriate normality of acid for analyzing samples
with >1000 mg/L alkalinity.
Requirement: See Section 2310B.1 a for selection of size sample to be titrated and
normality of titrant, substituting 0.02N or 0.1 N sulfuric (H2SO4) or hydrochloric (HCI) acid for
the standard alkali of that method. Ref: Standard Methods, 2320 B-2011. (1) (e).
Comment: The laboratory is using 0.2N H2SO4 to titrate high-level samples. Alkalinity is a
method -defined parameter, and therefore must be followed as written.
AA. Finding: The laboratory is not properly standardizing the sulfuric acid titrant.
Requirement: Standardize against 40.00 mL 0.05N Na2CO3 solution, with about 60 mL
water, in a beaker by titrating potentiometrically to pH of about 5. Ref: Standard Methods,
2320 B-2011. (3) (b).
Requirement: Standardize by potentiometric_ titration of 15.00_ mL 0.05N Na2CO3,
according to the procedure of ¶ b above; 1 mL = 1.00 mg CaCO3. Ref: Standard Methods,
2320 B-2011. (3) (c).
Comment: The laboratory is standardizing the acid solutions against 0.02N Na2CO3.
Bacteria — Coliform Fecal — Standard Methods, 9221 C E-2006 (MPN) (Biosolids)
Bacteria — Coliform Fecal — Standard Methods, 9221 C E-2006 (MF) (Biosolids)
BB. Finding: Samples are not being incubated within 8 hours of collection.
Requirement: Sample analysis should begin as soon as possible after receipt; sample
incubation must be started no later than 8 hours from time of collection. Ref: Code of
Federal Regulations, Title 40, Part 136; Federal Register Vol. 82, No. 165, August 28,
2017; Table ll, Footnote 22.
Comment: The 24-hour holding time only applies to EPA Methods 1680 and 1681.

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CC. Finding: The laboratory is not always determining the appropriate three dilution series
correctly.
Requirement: The guidance provided in "Control of Pathogens and Vector Attraction in
Sewage Sludge" (EPA/625/R-92/013), more commonly known as the White House
document, is to be followed for setting up the series of sample dilutions. If the laboratory
is unfamiliar with the samples, it is recommended that a series of five dilutions, instead
of four, be set. Once the dilutions have been set, follow the procedure in Standard
Methods 9221E-2006 for incubation and interpretation of gas production. Follow the
procedure in Standard Methods 9221 C-2006 for narrowing the series of dilutions down
to three. Ref: NC WW/GW LC Policy
Comment: The laboratory has a spreadsheet detailing how the dilutions are narrowed
down to the appropriate three. The instructions are correct except for when the positive
tube combination in the determined appropriate dilutions does not appear in MPN Table
9221:IV. In that situation, Standard Methods 9221C-2006 says to use the highest dilution
with at least one positive tube and the two dilutions immediately lower as the three selected
dilutions. The laboratory spreadsheet in this situation says to "select the lowest dilution that
does not have all positive results, then select the highest dilution with at least one positive
dilution. Use all dilutions between them to perform calculation and report as estimated."
However, following those instructions, it would be possible to pick two dilutions that are next
to each other. In that case there is no dilution between them to select as the third dilution.
See the Technical Assistance Document at the end of the report for more information.
Bacteria — Coliform Fecal — Standard Methods, 9222 D-2006 (MF) (Aqueous)
Comment: The documented time samples are placed into the incubator is not clearly associated
with a date on the benchsheet.
DD. Finding: The time sample filtration begins is not recorded on the benchsheet to show that
no more than 30 minutes has passed before filters are placed into the incubator. This is
considered pertinent data.
Requirement: All analytical records, including original observations and information
necessary to facilitate historical reconstruction of the calculated results, shall be maintained
for five years. All analytical data and records pertinent to each certified analysis shall be
available for inspection upon request. Ref; 15 NCAC 02H .0805 (a)_(7) (E),__
Comment: Place all prepared cultures in the water bath within 30 min after filtration. Ref:
Standard Methods, 9222 D-2006. (2) (d).
EE. Finding: Single analyst plate count comparisons are not being performed.
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 for the same analyst should agree
within 5% (within analyst repeatability of counting) and those between analysts should
agree within 10% (between analysts reproducibility of counting). If they do not agree,
initiate investigation and any necessary corrective action. Ref: Standard Methods, 9020 B-
2005. (9) (a).
Comment: Multi -analyst plate count comparisons are being performed and documented.

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BOD — Standard Methods, 5210 B-2011 (Hach 10360-2011, Rev. 1.2) (LDO) (Aqueous)
CBOD — Standard Methods, 5210 B-2011 (Hach 10360-2011, Rev. 1.2) (LDO) (Aqueous)
Comment: An instance was observed on a client report where a sample was flagged for a Seed
Correction Factor (SCF) > 1.0 ppm. This is not required for NC samples.
FF. Finding: Documentation does not demonstrate that the initial Dissolved Oxygen (DO) is
measured within 30 minutes of sample preparation. This is considered pertinent data.
Requirement: All analytical records, including original observations and information
necessary to facilitate historical reconstruction of the calculated results, shall be maintained
for five years. All analytical data and records pertinent to each certified analysis shall be
available for inspection upon request. Ref: 15A NCAC 02H .0805 (a) (7) (E).
Requirement: After preparing dilution, measure initial DO within 30 minutes. Ref: Standard
Methods, 5210 B-2011. (5) (g).
Chromium, Hexavalent - SW-846 Method 7199 (Aqueous & Non -Aqueous)
Chromium, Hexavalent - EPA Method 218.6, Rev. 3.3, 1994 (Aqueous)
GG. Finding: The back calculations of the low-level standards are not being evaluated for
precision and accuracy.
Requirement: Unless specified by the method or this Rule, each laboratory shall establish
performance acceptance criteria for all quality control analyses. Ref: 15A NCAC 02H .0805
(a) (7) (A).
Requirement: For analytical procedures requiring analysis of a series of standards, the
concentrations of these standards shall bracket the range of the sample concentrations
measured. One of the standards shall have a concentration equal to or less than the
laboratory's lowest reporting concentration for the parameter involved. All data sets shall
reference the corresponding calibration. Laboratories shall analyze or back -calculate a
standard at the same concentration as the lowest reporting concentration each day
samples are analyzed. Ref: 15A NCAC 02H .0805 (a) (7) (H).
Comment: The laboratory software automatically calculates the difference from the
known value of the standard.
Chromium, Hexavalent — SW-846 Method 7196 A (Aqueous)
Chromium, Hexavalent — SW-846 Method 7199 (Aqueous & Non -Aqueous)
HH. Finding: The laboratory is not stirring the samples during digestion.
Requirement: Heating Device - capable of maintaining the digestion solution at 90-95 °C
with continuous auto stirring capability or equivalent. Ref: EPA SW-846 Test Methods for
Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 3060 A. Rev. 1,
December 1996, Section 4.6.
Requirement: An automated continuous stirring device (e.g. magnetic stirrer, motorized
stirring rod, etc.), one for each digestion being performed. Ref: EPA SW-846 Test Methods
for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 3060 A. Rev.
1, December 1996, Section 4.11.

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Requirement: Stir the samples continuously (unheated) for at least five minutes using an
appropriate stirring device. Ref: EPA SW-846 Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods; 3rd Edition, Method 3060 A. Rev. 1, December 1996, Section
7.4
Requirement: Heat the samples to 90-95 °C, then maintain the samples at 90-95 °C for at
least 60 minutes with continuous stirring. Ref: EPA SW-846 Test Methods for Evaluating
Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 3060 A. Rev. 1, December
1996, Section 7.5
Requirement: Place an appropriate stirring device into the sample digest beaker, place the
vessel on a stirrer, and, with constant stirring, slowly add 5.0 M nitric acid solution to the
beaker dropwise. Adjust the pH of the solution to 7.5 ± 0.5 if the sample is to be analyzed
using Method 7196 (adjust the pH accordingly if an alternate analytical method is to be
used; i.e. 9.0 ± 0.5 if Method 7199 is to be used) and monitor the pH with a pH meter. Ref:
EPA SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd
Edition, Method 3060 A. Rev. 1, December 1996, Section 7.7.
Chromium, Hexavalent — Standard Methods, 3500 Cr R-2011 (Aqueous)
Chromium, Hexavalent — SW-846 Method 7196 A (Aqueous)
Chromium, Hexavalent — EPA Method 218.6, Rev. 3.3, 1994 (Aqueous)
II. Finding: The laboratory is not filtering samples prior to analysis.
Requirement: Filter sample through a 0.45 pm filter. Ref: Standard Methods, 3500 Cr 13-
2011. (4) (b).
Requirement: For dissolved metals, filter grab samples within 15 minutes of collection and
before adding preservatives. For a composite sample collected with an automated sampler
(e.g. using a 24-hour composite sampler; see 40 CFR 122.21 (g) (7) (i) or 40 CFR part 403,
appendix E), filter the sample within 15 minutes after completion of collection and before
adding preservatives. Ref: Code of Federal Regulations, Title 40, Part 136 ; Federal
Register Vol. 82, No. 165, August 28, 2017; Table II, Footnote 7.
Requirement: Method 7196 is used to determine the concentration of dissolved
hexavalent chromium [Cr(VI)] in EP/TCLP characteristic extracts and ground waters. This
method may also be applicable to certain domestic and industrial wastes, provided that no
interfering substances are present (see Paragraph 3,1 below). Ref: EPA SW-846 Test
Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 7196
A. Rev. 1, July 1992, Section 1.1.
Requirement: Dissolved Metals: The concentration of metals determined in an aqueous
sample after the sample is filtered through a 0.45 pm filter (see Method 3005). Ref: EPA
SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition,
Chapter 3, Rev. 6, December 2018, Section 3.1
Comment: Although method 7196 A does not specifically state to filter the sample in the
sample collection or preparation sections, the fact that it is a measure of dissolved
hexavalent chromium requires filtration by definition of Dissolved Metals.
Comment: Clean Water Act samples must be clearly documented to have been filtered
within 15 minutes of sample collection. When samples are filtered prior to preservation,
then the results must be reported as Dissolved Hexavalent Chromium.

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Chromium, Hexavalent — Standard Methods, 3500 Cr B-2011 (Aqueous)
Chromium, Hexavalent — SW-846 Method 7199 (Aqueous)
Chromium, Hexavalent — EPA Method 218.6, Rev. 3.3, 1994 (Aqueous)
JJ. Finding: The laboratory is not routinely allowing the sample to reach ambient temperature
prior to analysis.
Requirement: Bring samples to room temperature before analysis. Ref: Standard
Methods, 3500 Cr B-2011. (4) (b).
Requirement: Bring to ambient temperature prior to analysis. Ref: EPA Method 218.6,
Rev. 3.3 (1994), Section 8.3.
Requirement: Sample preparation. Allow pl-l-adjusted samples to equilibrate to ambient
temperature prior to analysis. Ref: EPA SW-846 Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods; 3rd Edition, Method 7199. Rev. 0, December 1996, Section
7.1.
Recommendation: It is recommended that the laboratory fill a sink with warm water to
raise the temperature of the sample if there are time constraints on sample analysis.
Chromium, Hexavalent — SW-846 Method 7196 A (Aqueous)
KK. Finding: The laboratory is not analyzing a matrix spike duplicate or sample duplicate for
every 10 samples.
Requirement: Run one matrix spike replicate or one replicate sample for every ten
samples. A duplicate sample is a sample brought through the whole sample preparation
and analytical process. Ref: EPA SW-846 Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods; 3rd Edition, Method 7196 A. Rev. 1, July 1992, Section 8.5.
Comment: The laboratory analyzes a matrix spike duplicate for every 15 samples.
Chromium, Hexavalent — EPA Method 218.6, Rev. 3.3, 1994 (Aqueous)
LL. Finding: The samples are not preserved within 15 minutes of collection in order to achieve
the 28-day holding time.
Requirement: To achieve the 28-day holding time, use the ammonium sulfate buffer
solution specified in EPA method 218.6. The allowance in this footnote supersedes
preservation and holding time requirements in the approved hexavalent chromium
methods, unless this supersession would compromise the measurement, in which case
requirements in the method must be followed. Ref: Code of Federal Regulations, Title 40,
Part 136.3; Federal Register Vol. 82, No. 165, August 28, 2017; Table II, Footnote 20.
Requirement: Except where noted in this Table II and the method for the parameter,
preserve each grab sample within 15 minutes of collection. Ref: Code of Federal
Regulations, Title 40, Part 136.3; Federal Register Vol. 82, No. 165, August 28, 2017;
Table II, Footnote 2.
MM. Finding: The laboratory does not analyze all prepared LFB standards.
Requirement: Laboratory Fortified Blank (LFB) - To an aliquot of Laboratory Reagent
Blank (LRB) add an aliquot of stock standard (Section 7.3) to produce a final concentration

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of 100 pg/L of Cr (VI). The LFB must be carried through the entire sample preparation and
analysis scheme. Ref: EPA Method 218.6, Rev. 3.3 (1994), Section 7.5.
Comment: The laboratory prepares an LFB (called LCS by the lab) with each preparation
batch. When multiple preparation batches are combined into a single analytical batch, only
one of the LCS samples are analyzed.
Chromium, Hexavalent — Standard Methods, 3500 Cr B-2011 (Aqueous)
NN. Finding: The laboratory does not use an acceptance range of 95-105% recovery for the
initial calibration verification (ICV).
Requirement: For regulatory compliance purposes, use acceptance criteria of between 95
and 105% of the expected value. If the ICV is not within acceptance limits, do not proceed
with analysis; take corrective action such as recalibrating or changing standards. Ref:
Standard Methods, 3020 B-2005. (2) (c).
Comment: The laboratory is using 90-110% recovery.
®O. Finding: The laboratory is not adding H3PO4 to the samples.
Requirement: Color development and measurement: Bring samples to room temperature
before analysis. Add 0.25 mL (5 drops) H3PO4 to samples. Use 0.2N H2SO4 and a pH
meter to adjust solution to pH 2.0 ± 0.5. Ref: Standard Methods, 3500 Cr B-2011 (4) (c).
PP. Finding: The laboratory is not calibrating with each batch of samples.
Requirement: Repeat calibration at the beginning of each batch of samples and whenever
calibration verification acceptance criteria are not satisfied. Ref: Standard Methods, 3020 B-
2005. (2) (a).
Comment: The laboratory is holding the curve in the instrument for up to six months.
QQ. Finding: The laboratory is not checking and documenting the pH of the sample to show
that pH adjustment is within the proper range.
Requirement: Use 0.2N H2SO4 and a pH meter to adjust solution to pH 2.0 ± 0.5. Ref:
Standard Methods, 3500 CrB2011. (4)_(c).
Requirement: Certified Data shall be traceable to the associated sample analyses and
shall consist of: sample preparation, where applicable. Ref: 15A NCAC 02H .0805 (a) (7)
(F) (x).
Comment: The pH adjustment is performed by the instrument. The final pH needs to be
documented.
Cyanide — EPA Method 335.4, Rev. 1.0, 1993 (Aqueous)
Cyanide — SW-846 9012 B (Total) (Aqueous)
Cyanide — Standard Methods, 4500 CN E-2011 (Aqueous)
Cyanide - Lachat 10-204-00-1-X, Rev. 2.2, 2005 (SM 4500 CN E-2011) (Aqueous)
Comment: The laboratory is checking and documenting that the pH of samples is >12 S.U. The
preservation requirements listed in Code of Federal Regulations, Title 40, Part 136; Federal
Register Vol. 82, No. 165, August 28, 2017; Table II, state that the pH be >10 S.U. Although the

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Lachat method states that the pH of samples be >12 S.U., in situations where the method
conflicts with the Code of Federal Regulations, the Code of Federal Regulations takes
precedence. The laboratory may therefore choose to preserve samples to pH >10 S.U.
Cyanide — EPA Method 335.4, Rev. 1.0, 1993 (Aqueous)
RR. Finding: The laboratory is not standardizing the Stock Cyanide Solution.
Requirement: Titrants prepared in the laboratory must be standardized initially and
monthly; thereafter, unless a different frequency is specified in the referenced method. All
certified titrants which are purchased, may be used initially without standardization. The
Certificate of Analysis must be kept on file. The certified titrant must be standardized
monthly; thereafter, for as long as it is used unless a different frequency is specified in the
referenced method. If the normality (titer value) changes, a new titrant at the specified
normality must be used, or the sample results must be calculated using the newly
determined normality. Quality Control standards do not take the place of titrant
standardization. Ref: NC WW/GW LC Policy.
Comment: A certified Stock Cyanide Solution is purchased but is not being standardized
monthly after opening.
Nitrogen, Ammonia — EPA Method 350.1, Rev. 2.0, 1993 (Aqueous)
Nitrogen, Total Kieldahl — EPA Method 351.2, Rev. 2.0, 1993 (Aqueous)
Phosphate, Ortho — EPA Method 365.1, Rev. 2.0, 1993 (Aqueous)
SS. Finding: Calibration standards are not analyzed in order of decreasing concentration.
Requirement: Place appropriate standards in the sampler in order of decreasing
concentration and perform analysis. Ref: EPA Method 350.1, Rev. 2.0 (1993), Section 10.5.
Requirement: Place appropriate standards in the sampler in order of decreasing
concentration and perform analysis. Ref: EPA Method 351.2, Rev. 2.0 (1993), Section 10.5.
Requirement: Place appropriate standards in the sampler in order of decreasing
concentration and perform analysis. Ref: EPA, Method 365.1, Rev. 2.0 (1993), Section
10.5.
-Comment:- The laboratory is -generating calibration curves in order of increasing -
standard concentration. EPA has stated that altering the order of calibration standards,
when specified, is not an allowable method modification.
Nitrogen, Ammonia — EPA Method 350.1, Rev. 2.0, 1993 (Aqueous)
Recommendation: It has been shown that chlorine test strips are often not reliable at extreme
pHs. It is recommended that the laboratory educate clients that chlorine testing of ammonia
samples should be done in the field, at the time of sample collection, and prior to acid preservation.
It is also recommended that the Chain of Custody (COC) be modified to include space to document
that chlorine testing is performed prior to any pH adjustments to the sample.
Nitrogen, Nitrate — SW-846 9056A (Aqueous & Non -Aqueous)
Nitrogen, Nitrate — EPA Method 300.0, Rev. 2.1, 1993 (Aqueous & Non -Aqueous)
Nitrogen, Nitrate — (NO3+NO2 EPA 363.2, Rev 2.0, 1993) — (NO2 EPA 353.2, Rev. 2.0, 1993)
(Aqueous)

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Nitrogen, Nitrite — EPA Method 353.2, Rev. 2.0, 1993 (Aqueous)
Nitrogen, Nitrite — EPA Method 300.0, Rev. 2.1, 1993 (Aqueous & Non -Aqueous)
Nitrogen, Nitrite — SW-846 9056 A (Aqueous & Non -Aqueous)
Nitrogen, NO3+NO2 — EPA Method 353.2, Rev. 2.0, 1993 (Aqueous)
Comment: The Sulfanilamide Color Reagent is being made with 10g of sulfanilamide per liter
instead of 40g per liter as required by the method. The analyst stated that the instrument
manufacturer says to prepare with 10g per liter.
Nitrogen, Nitrate — SW-846 9056 A (Aqueous & Non -Aqueous)
Nitrogen, Nitrate — EPA Method 300.0, Rev. 2.1, 1993 (Aqueous & Non -Aqueous)
Nitrogen Nitrate — (NO3+NO2 EPA 353.2, Rev 2.0, 1993) — (NO2 EPA 353.2, Rev. 2.0, 1993)
(Aqueous)
TT. Finding: The stated true value of the QC standard is incorrect.
Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data
shall be traceable to the associated sample analyses and shall consist of: all quality control
assessments; any other data needed to reconstruct the final calculated result. Each item
shall be recorded each time samples are analyzed. Ref: 15 NCAC 02H .0805 (a) (7) (F)
(xv) and (xviii).
Comment: The "Nitrate/Nitrite/Nitrate-Nitrite Analysis Cover Sheet" lists the "NO3 LCS/D or
MS/D" concentration as 0.8 mg/L. The true concentration is 0.4 mg/L.
UU. Finding: The laboratory is not properly evaluating the percent recovery of the LFM and
LFMD to demonstrate the established acceptance criterion is met.
Requirement: Unless specified by the method or this Rule, each laboratory shall establish
performance acceptance criteria for all quality control analyses. Each laboratory shall
calculate and document the precision and accuracy of all quality control analyses with each
sample set. When the method of choice specifies performance acceptance criteria for
precision and accuracy, and the laboratory chooses to develop laboratory -specific limits,
the laboratory -specific limits shall not be less stringent than the criteria stated in the
approved method. Ref: 15A NCAC 02H .0805 (a) (7) (A).
Comment: The MS and MSD concentrations listed on the Analytical Batch data sheets that
are used to calculate the NO3 MS/MSD recoveries are the concentrations of the NOx
spiked samples, not the NO3 spiked samples. Example: Sample UH23013-007 in
Analytical Batch 26935.
Nitrogen, Nitrite — EPA Method 353.2, Rev. 2.0, 1993 (Aqueous)
Nitrogen, Nitrite — EPA Method 300.0, Rev. 2.1, 1993 (Aqueous & Non -Aqueous)
Nitrogen, Nitrite — SW-846 9056 A (Aqueous & Non -Aqueous)
W. Finding: The laboratory is not evaluating the percent recovery of the LFM and LFMD to
demonstrate the established acceptance criterion is met.
Requirement: Unless specified by the method or this Rule, each laboratory shall establish
performance acceptance criteria for all quality control analyses. Each laboratory shall
calculate and document the precision and accuracy of all quality control analyses with each
sample set. When the method of choice specifies performance acceptance criteria for
precision and accuracy, and the laboratory chooses to develop laboratory -specific limits,

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the laboratory -specific limits shall not be less stringent than the criteria stated in the
approved method. Ref: 15A NCAC 02H .0805 (a) (7) (A).
WK Finding: The laboratory is not evaluating the Relative Percent Difference (RPD) of
duplicate analyses to demonstrate the analytical process is in control and the established
acceptance criterion is met.
Requirement: Unless specified by the method or this Rule, each laboratory shall establish
performance acceptance criteria for all quality control analyses. Each laboratory shall
calculate and document the precision and accuracy of all quality control analyses with each
sample set. When the method of choice specifies performance acceptance criteria for
precision and accuracy, and the laboratory chooses to develop laboratory -specific limits,
the laboratory -specific limits shall not be less stringent than the criteria stated in the
approved method. Ref: 15A NCAC 02H .0805 (a) (7) (A).
Nitrogen, Total Kieldahl — EPA Method 351.2, Rev. 2.0, 1993 (Aqueous)
XX. Finding: Samples are not being analyzed as soon as possible after digestion.
Requirement: The method does not provide for holding samples between digestion and
analysis. EPA has stated that once the process has initiated (digestion) it is the implied
expectation in the method to analyze ASAP after digestion. Ref: Email from EPA Region IV.
Comment: The laboratory SOP states that samples may be held up to 7 days after
digestion before being analyzed.
Comment: EPA also stated that a holding time study would be required for a laboratory to
establish a policy of holding digestates for analysis.
Oil & Grease — EPA Method 1664, Rev. B (Aqueous)
Recommendation: It is recommended that the laboratory add the acceptance criterion (RPD) for
the MSD to the review cover sheet (ME0023P-02).
Recommendation: It is recommended that the laboratory add the balance weight acceptance
criterion to the review cover sheet (ME0023P-02).
YY.. Finding The laboratory is not consistently weighing the aluminum pans to constant
weight.
Requirement: Continue to dry and cool the flask to room temperature in a desiccator for
30 minutes minimum. Remove with tongs and weigh immediately. While at room
temperature and without additional heating, repeat the cycle of desiccating and weighing
until the weight loss of the flask and dried residue is less than 4 % of the previous weight
or less than 0.5 mg, whichever is less. Ref: EPA Method 1664, Rev. B, Section 11.4.4.
Comment: The laboratory was weighing some pans to constant weight, but not all.
ZZ. Finding: The laboratory acceptance criterion for the method blank deviates from the
method -defined acceptance criteria.
Requirement: If material is detected in the blank at a concentration greater than the
minimum level (Section 1.6), analysis of samples is halted until the source of
contamination is eliminated and a blank shows no evidence of contamination. All

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samples must be associated with an uncontaminated method blank before the results
may be reported for regulatory compliance purposes. Ref: EPA Method 1664, Rev. B,
Section 9.4.2.
Comment: The laboratory review cover sheet states that the MB must be < PQL but if
sample results are >_ 10x the blank results, then the effect of contamination is considered
minimal and ignored. The method and SOP state that the MB must be < PQL.
Comment: The laboratory must drop the stipulation that the MB may be >PQL if the
sample result is >_10x the blank results unless it is a DOD requirement. In that case, the
clarification must be made that it only applies to DOD samples.
Oil & Grease — SW-846 9071 B (Non -Aqueous)
Comment: The laboratory blank acceptance criterion is < LOQ. Since the method does not
specify acceptance criteria for the blank, the laboratory must ensure that the acceptance criterion
will meet the client's site -specific cleanup requirements.
Paint Filter Liquids — SW-846 9095 B
Recommendation: It is recommended that the laboratory establish, implement and document a
routine holding time.
Phosphate, Ortho — EPA Method 365.1, Rev. 2.0, 1993 (Aqueous)
AAA. Finding: Samples are not being filtered within 15 minutes of collection.
Requirement: The immediate filtration requirement in orthophosphate measurement is to
assess the dissolved or bio-available form of orthophoshorus (i.e., that which passes
through a 0.45-micron filter), hence the requirement to filter the sample immediately upon
collection (i.e., within 15 minutes of collection). Ref: Code of Federal Regulations, Title 40,
Part 136; Federal Register Vol. 82, No. 165, August 28, 2017; Table II, Footnote 24.
Residue, Dissolved 180 C — Standard Methods, 2540 C-2011 (Aqueous)
Residue, Suspended — Standard Methods, 2540 D-2011 (Aqueous)
Residue, Total — Standard Methods, 2540 B-2011 (Aqueous)
Comment: The laboratory is analyzing a Method Blank with each analytical batch. Method Blanks
are not a required QC element of these methods per Standard Methods 2020 B-2010, Table 2020
II.
Residue, Suspended — Standard Methods, 2540 D-2011 (Aqueous)
Residue, Total — Standard Methods, 2540 B-2011 (Aqueous)
BBB. Finding: Drying Oven #3 is not able to consistently maintain an operational temperature of
103-105°C.
Requirement: Each laboratory requesting Certification shall be maintained so as to
ensure the security and integrity of samples. Samples shall be analyzed in such a
manner that contamination or error will not be introduced. Each facility shall contain or
be equipped with the following: Glassware, chemicals, supplies, and equipment required

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to perform all tests, analyses, measurements, or monitoring included in its Certification.
Ref: 15A NCAC 02H .0805 (a) (6) (B).
Requirement: Dry evaporated sample for at least 1 h in an oven at 103-105°C, cool dish in
desiccator to balance temperature, and weigh. Ref: Standard Methods, 2540 B-2011. (3)
(b).
Requirement: Dry for at least 1 In at 103-105°C in an oven, cool in a desiccator to balance
temperature, and weigh. Ref: Standard Methods, 2540 D-2011. (3) (c).
Comment: According to the Drying Oven Temperature Log, Oven #3 has been fluctuating
both above and below the required temperature range for several months.
CCC. Finding: Sample volumes greater than 1 liter are occasionally filtered.
Requirement: Choose sample to yield between 2.5 and 200 mg dried residue. If volume
filtered to meet minimum yield, increase sample volume up to 1 L. Ref: Standard Methods,
2540 D-2011. (3) (b).
Comment: Suspended Residue is a Method -Defined Parameter. Increasing the sample
volume to lower the reporting limit or to avoid reporting a "less than" value is not allowed.
Residue, Total — Standard Methods, 2540 B-2011 (Aqueous)
DDD. Finding: An inconsistency was noted between the SOP and laboratory practice as follows:
The analytical balance is being checked with a 2 g ICV weight; the SOP says to use a 10 g
weight.
Requirement: Each laboratory shall develop documentation outlining the analytical quality
control practices used for the Parameter Methods included in its Certification, including
Standard Operating Procedures for each certified Parameter Method. Quality assurance,
quality control, and Standard Operating Procedure documentation shall indicate the
effective date of the document and be reviewed every two years and updated if changes in
procedures are made. Each laboratory shall have a formal process to track and document
review dates and any revisions made in all quality assurance, quality control, and Standard
Operating Procedure documents. Supporting Records shall be maintained as evidence that
these practices are implemented. Ref: 15A NCAC 02H .0805 (a) (7).
Sulfide — Standard Methods, 4500 Sz- F-2011 (Aqueous)
EEE. Finding: The acceptance criterion of the LRB is < LOQ.
Requirement: Any constituent(s) recovered must generally be less than or equal to one-
half the reporting level (unless the method specifies otherwise). Ref: Standard Methods,
4020 B-2011. (2) (d)
Comment: The SOP states that the acceptance criterion for sulfide is either: < LOQ or <
5% of the measured concentration in the sample, whichever is greater. No acceptance
criteria are listed in SW-846 9030B or SW-846 9034. While the criteria listed in the SOP are
acceptable for SW-846 methods, they do not meet the requirements of Standard Methods,
4500 S2- F-2011.

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FFF. Finding: The laboratory is exceeding the method -specified holding time for the solid
sodium sulfide nonahydrate reagent.
Requirement: Prepare sulfide standards from sodium sulfide nonahydrate (Na2S * 9 H2O)
crystals. These crystals usually have excess water present on the surface, in addition to a
layer of contamination from oxidation products (polysulfides, polythionates, and sulfate) of
sulfide reacting with atmospheric oxygen. Further, solutions of sulfide are prone to ready
oxidation by dissolved and atmospheric oxygen. Use reagent water to prepare sulfide
standards and sample dilutions. Degas the water with either argon or nitrogen. Purchase
the smallest amount of solid standards possible and keep no longer than 1 year. Ref:
Standard Methods, 4500 S2- A-2011. (6).
Comment: The laboratory is keeping the solid sulfide standard until the end of the
manufacturer's designated expiration date.
GGG. Finding: The stock solution is not being stored in a container with minimal headspace.
Requirement: Store stock solution with minimum headspace for no more than 1 week.
Ref: Standard Methods, 4500 S2- A-2011. (6).
Sulfite — Standard Methods, 4500 S032- B-2011 (Aqueous)
HHH. Finding: The holding time for Sulfite analysis is routinely exceeded.
Requirement: Analyze within 15 minutes. Ref: Code of Federal Regulations, Title 40, Part
136; Federal Register Vol. 82, No. 165, August 28, 2017; Table II.
Comment: The laboratory noted two clients reporting to North Carolina had requested
Sulfite analysis for a total of 22 samples in 2019. The laboratory is appropriately qualifying
the results on client reports.
Comment: It is not acceptable to routinely analyze a sample out of hold time, which
would always be the case due to the distance of the lab from North Carolina clients.
Sulfite is defined as a Field Parameter in NC WW/GW LC rules and would be more
appropriate for the Pace South Carolina - Field Laboratory and Service Center
(Certificate #5639), which operates out of Charlotte.
TCLP — SW-846 Method 1311 (Non -Aqueous)
III. Finding: The laboratory is improperly preparing a sub -sample of the solid phase for pH
analysis during the extraction fluid determination step.
Requirement: Add 96.5 mL of reagent water to the beaker, cover with a watchglass, and
stir vigorously for 5 minutes using a magnetic stirrer. Ref: EPA SW-846 Test Methods for
Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 1311. Rev. 0,
July 1992, Section 7.1.4.2
Comment: The laboratory is using 95 mL of reagent water instead of 96.5 mL.
Metals — EPA Method 200.8, Rev. 5.4, 1994 (Aqueous)
Metals — SW-846 Method 6020 B (Aqueous)
Metals — EPA Method 200.7, Rev. 4.4, 1994 (Aqueous)

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JJJ. Finding: Samples analyzed for dissolved metals are not being filtered within 15 minutes of
sample collection.
Requirement: For dissolved metals, filter grab samples within 15 minutes of collection and
before adding preservatives. For a composite sample collected with an automated sampler
(e.g. using a 24-hour composite sampler; see 40 CFR 122.21(g)(7)(i) or 40 CFR part 403,
appendix E), filter the sample within 15 minutes after completion of collection and before
adding preservatives. Ref: Code of Federal Regulations, Title 40, Part 136.3; Federal
Register Vol. 82, No. 165, August 28, 2017; Table II, Footnote 7.
Mercu — EPA Method 245.1, Rev. 3.0, 1994 (Aqueous)
KKK. Finding: The laboratory digests the calibration standards.
Requirement: Prepare calibration standards by transferring 0.5, 1.0, 2.0, 5.0, and 10 mL
aliquots of the 0.1 pg/mL CAL (Section 7.6) to a series of sample containers (Section
6.5.2). Dilute the standard aliquots to 100 mL with reagent water (Section 7.2) and process
as described in Sections 11.1.2, 11.1.3 (without heating), and 11.1.5. Ref: EPA Method
245.1, Rev. 3.0 (1994), Section 11.2.2.
Silica - Metals — EPA Method 200.7, Rev. 4.4, 1994 (Aqueous)
LLL. Finding: Samples are not properly preserved.
Requirement: Cool, <_ 6 'C. Ref: Code of Federal Regulations, Title 40, Part 136; Federal
Register Vol. 82, No. 165, August 28, 2017; Table II.
Comment: The laboratory is obtaining a sample for silica analysis from the sample
container for other metals analyses. Other metals do not require refrigeration as a
preservative, but instead use acidification to pH < 2 S.U. However, silica may precipitate
out in acidic solutions, so proper thermal preservation without acidification is necessary for
accurate results.
Recommendation: Metals samples do not require immediate chemical preservation, as
long as the samples are acidified at least 24 hours prior to analysis. It is recommended that
the laboratory send an unpreserved sample bottle solely for Silica sample collection.
Base Neutral/Acid, Organics — SW-846 8270 E_(Aqueous &_ Non -Aqueous)
Base Neutral/Acid, Organics — EPA Method 625.1, December 2016 (Aqueous)
Comment: It was noted during data review that a Base Neutral/Acid Extractables sample was
diluted by a factor of 10, though the sample had no detections for any target analytes. However,
the sample had a Tentatively Identified Compound at a concentration of 1000, well above the linear
range of the calibration for the instrument. Based on this information, the laboratory is doing a good
job of diluting samples when appropriate to protect the instrumentation from matrix effects.
MMM. Finding: An inconsistency was noted between the SOP and laboratory practice as follows:
The laboratory is not consistently preparing an MS/MSD with each batch of samples for
EPA Method 625.1 and SW-846 8270E. The Base Neutral/Acid Organics SOP (Document
Number ME0014Q-10) requires an MS/MSD be prepared with each batch. If insufficient
sample remains, the SOP allows for an MS and sample duplicate or an LCSD to be
prepared. Extraction Batch numbers #13996, 14131 and 14781 were lacking spiked
environmental samples, sample duplicates and an LCSD.

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Requirement: Each laboratory shall develop documentation outlining the analytical quality
control practices used for the Parameter Methods included in its Certification, including
Standard Operating Procedures for each certified Parameter Method. Quality assurance,
quality control, and Standard Operating Procedure documentation shall indicate the
effective date of the document and be reviewed every two years and updated if changes in
procedures are made. Each laboratory shall have a formal process to track and document
review dates and any revisions made in all quality assurance, quality control, and Standard
Operating Procedure documents. Supporting Records shall be maintained as evidence that
these practices are implemented. Ref: 15A NCAC 02H .0805 (a) (7).
Comment: An MS/MSD is required per batch by EPA Method 625.1, Section 8.3.
Analyses are often performed as combined runs. In the case of combined batches and/or
runs, the laboratory must adhere to the strictest QC element requirements.
Chlorinated Acid Herbicides — SW-846 Method 8151 A (Aqueous & Non -Aqueous)
NNN. Finding: The laboratory is not consistently adding cold (4°C) H2SO4 to all extracts when the
pH was adjusted to < 2 S.U.
Requirement: Adjust the pH of the solution to < 2 with cold (4°C) sulfuric acid (1:3) and
extract once with 40 mL of diethyl ether and twice with 20-mL portions of ether. Ref: SW-
846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; V Edition,
Method 8151A, Revision 1, December 1996, Section 7.2.3.3.
Requirement: Adjust the pH of the solution to < 2 with cold (4°C) sulfuric acid (1:3) and
extract once with 40 mL of diethyl ether and twice with 20-mL portions of ether. Ref: SW-
846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition,
Method 8151A, Revision 1, December 1996, Section 7.2.4.2.
Requirement: Add 17 mL of cold (4'C) 12 N sulfuric acid to the sample (or hydrolyzed
sample), seal, and shake to mix. Check the pH of the sample with pH paper. If the
sample does not have a pH less than or equal to 2, adjust the pH by adding more acid.
Ref: SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd
Edition, Method 8151A, Revision 1, December 1996, Section 7.3.4.
Comment: The laboratory was acidifying the soil extracts with H2SO4 but the acid was
not consistently at 4°C at the time of addition to the sample. The addition of sulfuric acid is
an exothermic reaction. The sulfuric acid solutions must be kept cooled until the addition to
the sample in order to minimize loss of target analytes.
TPH Diesel Range, Organics — SW-846 Method 8015 C (Aqueous & Non -Aqueous)
Comment: The DRO ICV is dual labelled as an LCS to generate a recovery sheet for quality
control purposes. It is not a true LCS in the sense of having gone through extraction processes.
Comment: The analyst completing the DRO checklist indicated that they believed the percent
recovery acceptance criterion for the DRO second source standard is 70-130%. The laboratory's
SOP and the method both set the acceptance criterion at 80-120%. The data examined had a
percent recovery of 111 %, which does meet the criterion.
Recommendation: It is recommended that prior to recalibrating, the laboratory add an additional
1-minute hold to the initial temperature of the DRO instrument before beginning the temperature
increase program. This will allow n-Decane to fully resolve from the solvent peak.

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Recommendation: It was noted during data review that ICV# SVGC 1170.5 had a dilution factor
of 5X. It is recommended that the laboratory not dilute the standard, but change the value in the
LIMS or use a different standard so standards and samples are treated the same. Alternatively, the
laboratory may wish to address the reason for the dilution in the SOP.
OOO. Finding: An inconsistency was noted between the Diesel Range Organics SOP (document
number ME00138-05) and laboratory practice as follows: The SOP states that the CCV
true value is the mid -point of the calibration curve (i.e. 5000 pg/L). Examination of the data
showed that the CCV true value is 500 pg/L, which is the median value, not the mid -point
(mean) value.
Requirement: Each laboratory shall develop documentation outlining the analytical quality
control practices used for the Parameter Methods included in its Certification, including
Standard Operating Procedures for each certified Parameter Method. Quality assurance,
quality control, and Standard Operating Procedure documentation shall indicate the
effective date of the document and be reviewed every two years and updated if changes in
procedures are made. Each laboratory shall have a formal process to track and document
review dates and any revisions made in all quality assurance, quality control, and Standard
Operating Procedure documents. Supporting Records shall be maintained as evidence that
these practices are implemented. Ref: 15A NCAC 02H .0805 (a) (7).
Comment: SW-846 8015C does not state that the CCV must have a concentration at the
mid -point of the calibration curve. If the SOP were revised to state the current true value of
the CCV, the concentration would be considered acceptable.
Extractable Petroleum Hydrocarbons — MADEP, May 2004, Rev. 1.1, (Aqueous & Non -
Aqueous)
Recommendation: The laboratory is currently calculating breakthrough by a spreadsheet, which is
archived after a period of time. It is recommended that the laboratory retain a copy of the
spreadsheets with the raw data or note in the SOP where the spreadsheet for each extraction
batch is stored, so that the calculation is more easily accessible.
Recommendation: It is recommended that the laboratory use the same weight of sand in QC
samples as it does for routine samples. Currently, the lab uses 30g of soil for analysis, but the MB,
LCS, and LCSD use only 10g sand.
Recommendation: It is recommended that the laboratory adjust the scale of the EPH
chromatogram. Currently the target analytes are not visible due to the scale of the Y-axis being
affected by the size of the solvent peak.
PPP. Finding: The laboratory is not consistently preparing an LCSD with each batch of samples.
Requirement: At a minimum, for each analytical batch (up to 20 samples of similar
matrix), a Laboratory Method Blank, a Laboratory Control Sample (LCS), and an LCS
Duplicate must also be analyzed and results analyzed as part of the laboratory's
continuing quality control program. The blank and quality control samples fortified with
known concentrations and volumes of analytical standards should be carried through the
complete sample preparation and measurement processes. Ref: MADEP, Method for
the Determination of Extractable Petroleum Hydrocarbons (EPH), May 2004, Rev. 1.1,
Section 10.1.3.2.
Nonhalogenated Volatile, Organics — SW-846 Method 8015 C (Aqueous & Non -Aqueous)

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Recommendation: It is recommended that instrument maintenance be performed when 2-
Propanol and Ethanol peak resolution deteriorates.
Pesticides, Organochlorine — EPA Method 608.3 (Aqueous)
Pesticides, Organochlorine — SW-846 8081 B (Aqueous & Non -Aqueous)
Recommendation: The toxaphene LCS is manually integrated, but some peaks are not well
defined. Toxaphene is a multi -component pesticide whose composition may vary by vendor.
Currently the laboratory uses separate vendors for their primary and secondary source standards
which have dissimilar peaks. It is recommended that separate lot numbers from the same vendor
be used to ensure that integration would not be called into question for dissimilar peaks.
Polychlorinated Biphenyls (PCBs) — EPA Method 608.3 (Aqueous)
Polychlorinated Biphenyls (PCBs) — SW-846 8082 A (Aqueous & Non -Aqueous)
QQQ. Finding: The laboratory is not consistently preparing the LCS, MS and MSD at the required
frequency.
Requirement: The laboratory must, on an ongoing basis, spike at least 5% of the samples
in duplicate from each discharge being monitored to assess accuracy (recovery and
precision). Ref: EPA Method 608.3, December 2016, Section 8.3
Requirement: A QC check sample (laboratory control sample, LCS; on -going precision
and recovery sample, OPR) containing each single -component analyte of interest
(Section 1.4) must be extracted, concentrated, and analyzed with each extraction batch
of up to 20 samples (Section 3.1) to demonstrate acceptable recovery of the analytes of
interest from a clean sample matrix. If multi -peak analytes are required, extract and
prepare at least one as an LCS for each batch. Alternatively, the laboratory may set up a
program where multi -peak LCS is rotated with a single -peak LCS. Ref: EPA Method
608.3, December 2016, Section 8.4.
Requirement: The laboratory must also have procedures for documenting the effect of
the matrix on method performance (precision, accuracy, method sensitivity). At a
minimum, this should include the analysis of QC samples including a method blank, a
matrix spike, a duplicate, and a laboratory control sample (LCS) in each analytical batch
and the addition of surrogates to each field sample and QC sample when surrogates are
used. Any method blanks, matrix spike samples, and replicate samples should be
subjected to the same analytical procedures (Sec. 11.0) as those used on actual
samples. Ref: EPA SW-846 Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods; 3rd Edition, Method 8082 A. Rev. 1, February 2007, Section
9.6.
Requirement: To promote consistency with the use of SW-846 methods and to assure
generation of data of known quality, the minimum recommended quality control
benchmarks in the methods will be considered the minimum QA/QC requirements. For
example, where a method states, "Documenting the effect of the matrix on target analyte
measurements should include the analysis of at least one matrix spike and one duplicate
unspiked samples or one matrix spike/matrix spike duplicate pair.", the laboratory must
analyze at least one matrix spike and one duplicate unspiked sample or one matrix
spike/matrix spike duplicate pair. Laboratories may adopt more stringent QC acceptance
criteria for method performance but may not omit or use less stringent criteria than that
stated in SW-846 methods. Ref: NC WW/GW LC Policy

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Comment: Data was examined for Client Report UF27061 and Sample Prep Batch
21370. The Sample Prep Batch was lacking an LCS, MS, and MSD spiked with PCBs.
Data submitted prior to the inspection for EPA 608.3/ SW-846 8082A did include Sample
Prep Batches with appropriately spiked samples.
Purgeable, Organics — EPA Method 624.1 (Aqueous)
RRR. Finding: Sample vials are not properly preserved for the analysis of some target
compounds.
Requirement: The ethers listed in Table 2 are prone to hydrolysis at pH 2 when a heated
purge is used. Aqueous samples should not be acid preserved if these ethers are of
interest, or if the alcohols they would form upon hydrolysis are of interest and the ethers are
anticipated to present. Ref: EPA Method 624.1, Section 9.6
Comment: 1,4-Dioxane was noted to be a target analyte. This compound is an ether and is
listed in Table 2 of the method.
SSS. Finding: The LCS is not being analyzed in the same manner as samples.
Requirement: Laboratory control sample (LCS; laboratory fortified blank (LFB); on -going
precision and recovery sample; OPR) — An aliquot of reagent water spiked with known
quantities of the analytes of interest and surrogates. The LCS is analyzed exactly like a
sample. Its purpose is to assure that the results produced by the laboratory remain
within the limits specified in this method for precision and recovery. Ref: EPA Method
624.1, December 2016, Section 19.2
Comment: The laboratory was not adding the anti -foaming agent, mentioned in the SOP
(Document Number: ME0012X-13) to an LCS when analyzing a batch of samples to which
the reagent had been added. The laboratory was adding the reagent to an additional
Method Blank. Adding the anti -foaming agent is considered part of the analysis.
Volatile Petroleum Hydrocarbons — MADEP, February 2018, Rev. 2.1 (Aqueous & Non -
Aqueous)
TTT. Finding: More than one C9-Cjo Aromatic component is being used in the calibration.
Requirement: Calculate a CF for the C9-Cjo aromatic hydrocarbon range using the
following steps. Use the individual PID peak area of the one VPH component that is
used to establish an average range CF for C9-Cjo aromatic hydrocarbons, as designated
in Table 2b. It is important to note that integration must be performed using a valley -to -
valley approach for the one peak that comprises this range. This area is used in the
subsequent calculation. Note: Do not include the area of any surrogate standard in
calculating a hydrocarbon range CF. Do not include the area of naphthalene when
determining the CF for C9-Cjo aromatic hydrocarbons. Ref: MADEP, Method for the
Determination of Volatile Petroleum Hydrocarbons (VPH), February 2018, Rev. 2.1, Section
9.4.2.9.
Requirement: Using the PID chromatogram, calculate an average collective CF for the
total concentration of C9-C10 Aromatic Hydrocarbons. This value is the value for 1,2,4-
trimethylbenzene, the only aromatic standard within this range. Ref: MADEP, Method for
the Determination of Volatile Petroleum Hydrocarbons (VPH), February 2018, Rev. 2.1,
Section 11.1.5.

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Comment: The analyst was adding more peaks in the Cs-Clo Aromatics PID range other
than 1,2,4-Trimethylbenzene.
UUU. Finding: The laboratory was analyzing and evaluating 4 LCSs when performing Initial
Demonstrations of Capability (IDOC).
Requirement: Prepare and analyze seven (7) replicate Laboratory Control Samples
(LCSs) fortified at a concentration of 50% of the highest calibration curve standard (100
pg/L for aqueous samples and 5 mg/kg for soil/sediment samples). Ref: MADEP, Method
for the Determination of Volatile Petroleum Hydrocarbons (VPH), February 2018, Rev. 2.1,
Appendix 7, Section 3.0.
The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks,
etc.) COCs and client reports. Base Neutral/Acid Extractables and Organochlorine
Pesticides/PCBs data were reviewed for sample ID UF27061-002. Mercury data were reviewed
for project number UA28038-001. CBOD data were reviewed for sample ID UD25044-001. COD
data were reviewed for sample ID UB27037-002. No transcription errors were observed. The
facility appears to be doing a good job of accurately transcribing data.
Correcting the above -cited Findings and implementing the Recommendations will help this
laboratory to produce quality data and meet Certification requirements. The inspector would like
to thank the staff for their assistance during the inspection and data review process. Please
respond to all Findings and include supporting documentation, implementation dates
and steps taken to prevent recurrence for each corrective action.
Report prepared by: Michael Cumbus Date: February 10, 2020
Report reviewed by: Anna Ostendorff Date: February 27, 2020

Page 31
#329 Pace South Carolina
Fecal Sludge MPN ® How to Determine the Appropriate Dilutions when Referencing SM 9221 C E-2006
Standard Methods states that when more than three dilutions are used in a decimal series of dilutions, use the
guidelines in SM 9221 C-2006 (2) to select the three most appropriate dilutions and refer to Table 9221:IV. We have
found that the language there can be confusing because it is interlaced with comments relevant only when using
specific dilution schemes. For example, in one place SM states, "If no dilution has all positive tubes (Example F),
select the lowest two dilutions, corresponding to 10 and 1 mL sample". This does not mean that your particular
dilution scheme must have tubes that contain 10 and 1 mL of sample. Your dilution scheme may be different. This
technical assistance document uses the instructions in Standard Methods but does not include those type examples
and simply provides the steps that one would go through to narrow the dilutions down to the appropriate three.
Also, be aware that the steps and conditional questions in Standard Methods are being asked with the assumption
that you have 5 dilutions. While having 5 dilutions is recommended, a minimum of 4 dilutions is required.
The black text below is language as it appears in Standard Methods with the example references removed. Yellow
highlighted text is intended to help explain or clarify what the conditional questions and instructions in black mean.
Proceed through the numbered steps below until you have identified the appropriate three dilutions to use in the
final MPN determination. Once you have your three appropriate dilutions, determine the MPN Index/100 mL value
from Table 9221:IV. If the three dilutions selected are not found in Table 9221:IV, use the highest dilution with at
least one positive tube and the two dilutions immediately lower as the three selected dilutions.
1. First, remove the highest dilution (the most dilute, with the least amount of sample) if it has all negative
tubes and at least one remaining dilution has a negative tube.
2. Next, remove the lowest dilution (the least dilute, largest sample volume) if it has all positive tubes and at
least one remaining dilution has a positive tube.
3. If the lowest dilution does not have all positive tubes, and several of the highest dilutions have all
negative tubes, then remove the highest negative dilutions.
4. More than three dilutions may remain after removal of the lowest dilution with all positive tubes and high
dilutions with all negative tubes.

Page 32
#329 Pace South Carolina
In this case, if the highest dilution with all positive tubes is within two dilutions of the highest dilution with any
positive tubes, then use the highest dilution with any positive tubes and the two immediately lower dilutions.
Remember, in Step 4, you are only looking at the dilutions that remain after having gone through steps '1
3.
5. If, after removal of the lowest dilution with all positive tubes, no dilution with all positive reactions
remains, then select the lowest two dilutions and assign the sum of any remaining dilutions to the third
dilution.
From there, use the formula in Appendix F, Section 1.1 (6) of Control of Pathogens and Vector Attraction in
Sewage Sludge, EPA/625/R-92/013, (July 2003), more commonly known as the White House book, to determine
the final MPN/gram result. See below.
mL
MPN Fecal CGhl'GrWg �.10 x hn9Pt� lip i 1 +
I e 1 vd,,unie x % dry Aids
NOTE: % dry solids is not in decimal form.
NOTE: "largest volume" refers to the volume of the original mixture (30 mL in 300, mL for aqueous samples;
30g in 270 mL, for non -aqueous samples) that is in 1 mL of the lowest dilution of the three used to determine
the MPN value.
03/18/2020

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