#402_2022_0321_MC_FINAL

NC Department of Environmental Quality | Division of Water Resources | Laboratory Certification Branch
4405 Reedy Creek Road | 1623 Mail Service Center | Raleigh, North Carolina 27699-1623
919-733-3908

July 1, 2022

402
Mr. Kyle Collins
Waypoint Analytical - Charlotte
P.O. Box 240543
Charlotte, NC 28224-0543

Subject: North Carolina Wastewater/Groundwater Laboratory Certification Branch (NC
WW/GW LCB) Maintenance Inspection

Dear Mr. Collins:

Enclosed is a report for the inspection performed on March 21, 2022 by Michael Cumbus, Beth
Swanson, Anna Ostendorff, Todd Crawford, Tom Halvosa, Jill Puff, Tonja Springer and Jason
Smith. 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, 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 02H .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 have questions or need additional information, please contact me at (919) 733-
3908 Ext. 259.

Sincerely,

Beth Swanson
Technical Assistance & Compliance Specialist
Division of Water Resources

Attachment
cc: Todd Crawford, Michael Cumbus, #402

On-Site Inspection Report

LABORATORY NAME: Waypoint Analytical - Charlotte
ADDRESS: 449 Springbrook Road
Charlotte, NC 28217
CERTIFICATE #: 402
DATE OF INSPECTION: March 21, 2022 – March 23, 2022
TYPE OF INSPECTION: Commercial Maintenance
AUDITOR(S): Michael Cumbus, Beth Swanson, Anna Ostendorff, Todd
Crawford, Tom Halvosa, Jill Puff, Tonja Springer, Jason Smith

LOCAL PERSON(S) CONTACTED:

Kyle Collins, McLayne Reese, Jeff Vogel, Jack Cattron, Jenelle
Kamienski, Kelly LaTour, Tyrese Williams, Elizabeth Vrapi,
Joseph Blydenburgh, Andrew Guptill, Taylor Lowe, Emily
McComiskey, Paula Blakeborough, Sarah Locklear, Zoe Vigilant,
Christopher Garcia, Stacy Ortiz, Sharol Wiley, Caroline Baratta,
David Morris

I. INTRODUCTION:

This laboratory was inspected by representatives of the North Carolina Wastewater/Groundwater Laboratory
Certification Branch (NC WW/GW LCB) to verify its compliance with the requirements of 15A NCAC 02H
.0800 for the analysis of compliance monitoring samples.

II. GENERAL COMMENTS:

The facility is neat, well maintained and has all the equipment necessary to perform the analyses. Staff
were forthcoming and responded well to suggestions from the auditors. The laboratory is highly organized,
and staff were able to rapidly supply additional information requests. The laboratory has undergone
significant personnel and organizational changes within the last 24 months and has recently transitioned
to a new Laboratory Information Management System (LIMS).

All required Proficiency Testing (PT) Samples for the 2022 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, 2022.

The laboratory is reminded that any time changes are made to laboratory procedures, QA/SOP document(s)
must be updated and relevant staff retrained. Staff must acknowledge that they have read and understand
the changes as part of the documented training program. The same requirements apply when changes are
made in response to Findings, Recommendations or Comments listed in this report, to ensure the methods
are being performed as stated, references to methods are accurate, and the QA and/or SOP document(s) is
in agreement with each approved practice, test, analysis, measurement, monitoring procedure or 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. Revisions to the SOPs, based on the
Findings, Comments and Recommendations within this report must be submitted to this office by
July 1, 2023.

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The laboratory is also reminded that SOPs are required to be reviewed at least every two years and 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.

Contracted analyses are performed by Waypoint Analytical LLC (Certification #415), Waypoint Analytical
Mississippi (Certification #694), Analytical Environmental Services, Inc. (Certification #562), Pace West
Columbia (Certification #329) and Environment 1 (Certification # 10).

Approved Procedure documents for the analysis of the facility’s currently certified Field Parameters were
provided at the time of the inspection.

III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:

Documentation

A. Finding: Error corrections are not always properly performed.

Requirement: All documentation errors shall be corrected by drawing a single line through
the error so that the original entry remains legible. Entries shall not be obliterated by erasures
or markings. Wite-Out®, correction tape, or similar products designed to obliterate
documentation shall not to be used; instead, the correction shall be written adjacent to the
error. The correction shall be initialed by the responsible individual and the date of change
documented. Ref: 15A NCAC 02H .0805 (a) (7) (E).

Comment: Multiple instances were noted throughout the laboratory where error corrections
were lacking the date and/or the initials of the person making the change.

B. Finding: SOPs have not been updated for all of the methods included on the laboratory’s
Certified Parameters Listing (CPL).

Requirement: Each laboratory shall have a documented analytical quality assurance and
quality control program. Each laboratory shall have a copy of each approved test, analysis,
measurement, or monitoring procedure being used in the laboratory. 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. 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).

Comment: Many instances were noted where the effective dates of the SOPs on file
exceeded the two year requirement. The laboratory submitted drafts of upcoming revisions
for many of the SOPs.

C. Finding: The laboratory does not document SOP revisions.

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Requirement: 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: There is not a summary sheet detailing dates and specific revisions completed.

D. Finding: Sample preservation verification is not always clearly documented in the laboratory
records.

Requirement: Sample preservation shall be verified and documented. If a laboratory receives
a sample subject to G.S. 143-215.1 and 143-215.63 that does not meet sample collection,
holding time, or preservation requirements, the laboratory shall document the incident, notify
the sample collector or client, and secure another sample that meets the regulatory
requirements, if possible. If another viable sample cannot be secured, the original sample may
be analyzed but the results reported shall be qualified with the nature of the sample collection,
holding time, or preservation infractions and the laboratory shall notify the State Laboratory of
the infractions. The notification shall include a statement indicating corrective action taken to
prevent future infractions. Ref: 15A NCAC 02H .0805 (a) (7) (M).

Comment: Documentation of sample preservation for each batch of client samples consisted
of a single checkmark on the chain of custody form. Sample preservation was documented
on the sample bottles, but this does not create a permanent (or lasting) record once the bottles
are discarded.

E. Finding: Units of measure are not consistently documented on the laboratory benchsheets.

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 that samples are analyzed. Ref: 15A NCAC
02H .0805 (a) (7) (F) (xii).

Comment: The laboratory benchsheet for Alkalinity was lacking the units of measure for the
“initial pH”, “pH prior to low level 0.3 unit titr.” and “results” columns.

Comment: The laboratory benchsheet for Cyanide by SM 4500 CN E-2011 was lacking the
units of measure for the “pH >12” column.

Comment: The columns on the Inorganic Phenols benchsheet by EPA 420.1, labeled “pH 4”
and “pH 10” are lacking units of measure.

Comment: The laboratory benchsheet for Hexavalent Chromium by SW-846 3060A/7196A
was lacking units of measure for pH.

Comment: The Quantitative Analysis Report benchsheets for Hexavalent Chromium (all
methods) do not have the correct units on the "Concentration" columns. The value in the
column is only "ug". On most of the results, the analyst then divides the value by 100 (mL of
sample reacted) and documents that value, which is correctly ug/mL at that point (i.e., mg/L
as reported).

Comment: The prep benchsheet for Total Phosphorus by SM 4500 P F-2011, has a column
labeled "Sample Amt (mL or g)" and nothing was circled or indicated which unit is correct.

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Comment: The laboratory benchsheet for pH is lacking units of measure for Temperature
(°C).

Recommendation: This list may not be exhaustive. It is recommended that the laboratory
review all benchsheets to ensure that they include the proper units of measure.

F. Finding: The COD benchsheet and the laboratory calibration log for the pH meter used in
BOD/CBOD analyses are lacking required documentation: instrument identification.

Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data
shall be traceable to the associated sample analyses and shall consist of: the instrument
identification. Each item shall be recorded each time that samples are analyzed. Ref: 15A
NCAC 02H .0805 (a) (7) (F) (iii).

Comment: The laboratory uses two COD reactors for an analytical batch. It is not clear which
samples were digested in each reactor.

G. Finding: The laboratory benchsheet for pH and Temperature is lacking required
documentation: the method or Standard Operating Procedure reference; the instrument
identification and the proper units of measure.

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; the instrument identification; the proper units of measure. Each item
shall be recorded each time that samples are analyzed. Ref: 15A NCAC 02H .0805 (a) (7) (F)
(i) (iii) (xii).

Comment: This Finding applies to Field pH and Temperature analyses.

Comment: Temperature and pH results are documented in a notebook in the field and
transferred to the Chain of Custody. The notebook is missing units of measure for
Temperature, and method reference and instrument identification for both parameters. There
is a log that includes all the required information, but it is no longer being used.

H. Finding: The laboratory benchsheet is lacking required documentation: the signature or
initials of the analyst.

Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data shall
be traceable to the associated sample analyses and shall consist of: the signature or initials
of the analyst. Each item shall be recorded each time that samples are analyzed. Ref: 15A
NCAC 02H .0805 (a) (7) (F) (v).

Comment: This Finding applies to the laboratory Field Benchsheet used to document
temperature and pH analyses.

I. Finding: The analysis end time of Paint Filter Liquids is not documented.

Requirement: Supporting records shall be maintained as evidence that these practices are
being effectively carried out. Ref: 15A NCAC 02H .0805 (a) (7).

Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data shall
be traceable to the associated sample analyses and shall consist of: the time of sample
analyses (when required to document a required holding time or when time-critical steps
are imposed by the method, a federal regulation, or this Rule). Each item shall be recorded
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each time that samples are analyzed. The date and time that samples are placed into and
removed from ovens, water baths, incubators and other equipment shall be documented if a
time limit is required by the method. Ref: 15A NCAC 02H .0805 (a) (7) (F) (viii).

Requirement: Allow sample to drain for 5 min into the graduated cylinder. Ref: EPA SW-
846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition,
Method 9095 B. Rev. 2, November 2004, Section 7.5.

J. Finding: The laboratory is not documenting all traceability information for purchased
materials, reagents and standards.

Requirement: 15A NCAC 02H .0805 (a) (7) (K) and (g) (7) requires laboratories to have a
documented system of traceability for the purchase, preparation, and use of all chemicals,
reagents, standards, and consumables. That system must include documentation of the
following information: Date received, Date Opened (in use), Vendor, Lot Number, and
Expiration Date (where specified). A system (e.g., traceable identifiers) must be in place that
links standard/reagent preparation information to analytical batches in which the solutions are
used. Documentation of solution preparation must include the analyst’s initials, date of
preparation, the volume or weight of standard(s) used, the solvent and final volume of the
solution. This information as well as the vendor and/or manufacturer, lot number, and
expiration date must be retained for primary standards, chemicals, reagents, and materials
used for a period of five years. Consumable materials such as pH buffers, lots of pre-made
standards and/or media, solids and bacteria filters, etc. are included in this requirement. Ref:
NC WW/GW LCB Policy.

Comment: Traceability information for the filters used for Color, Oil and Grease, Total
Suspended Residue and Total Dissolved Residue is not documented.

K. Finding: Some benchsheets and/or report summaries reference unapproved methods and/or
do 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: 15A
NCAC 02H .0805 (a) (7) (F) (i).

Requirement: Analytical methods, sample preservation, sample containers, and sample
holding times shall conform to the requirements found in: 40 CFR Part 136. Ref: 15A NCAC
02H .0805 (a) (1) (A).

Comment: Many laboratory benchsheets do not reference the method year. This may be
due to space constraints in transferring data from the LIMS.

Comment: The laboratory benchsheets for BOD/CBOD cite the revision year as 2011 instead
of 2015.

Comment: One Seal autoanalyzer printout (i.e., AA090121A) reviewed references SM 4500
NO3- I, which is not an approved method.

Comment: The client reports submitted in advance of the inspection did not always transfer
the correct method year from the LIMS. Client report 21-175-0010 dated June 24, 2021
omitted the method year reference for Ammonia Nitrogen (SM4500 NH3-G 2011) and Total
Phosphorus (SM4500 P-F 2011). Client report 21-302-0033 dated November 10, 2021
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omitted the method year for Ammonia Nitrogen (SM4500 NH3-G 2011) and listed the method
year for Total Dissolved Residue (SM2540 C-2015) as 2011.

L. Finding: The laboratory is not documenting the preparation of the combined reagent.

Requirement: 15A NCAC 02H .0805 (a) (7) (K) and (g) (7) requires laboratories to have a
documented system of traceability for the purchase, preparation, and use of all chemicals,
reagents, standards, and consumables. That system must include documentation of the
following information: Date received, Date Opened (in use), Vendor, Lot Number, and
Expiration Date (where specified). A system (e.g., traceable identifiers) must be in place that
links standard/reagent preparation information to analytical batches in which the solutions are
used. Documentation of solution preparation must include the analyst’s initials, date of
preparation, the volume or weight of standard(s) used, the solvent and final volume of the
solution. This information as well as the vendor and/or manufacturer, lot number, and
expiration date must be retained for primary standards, chemicals, reagents, and materials
used for a period of five years. Consumable materials such as pH buffers, lots of pre-made
standards and/or media, solids and bacteria filters, etc. are included in this requirement. Ref:
NC WW/GW LCB Traceability Documentation Requirements for Chemicals, Reagents,
Standards and Consumables Policy.

Comment: All components of the combined reagent are documented, but the separate
preparation time and directions for preparing (i.e., volume of each reagent used) the combined
reagent are not documented. The combined reagent has a very short expiration period (4
hours) so the preparation time is especially important.

Comment: This Finding applies to Total and Ortho-Phosphorus by SM 4500 P E-2011
(Aqueous) and Total Phosphorus by SM 4500 P F-2011 (Aqueous)

Equipment

M. Finding: The analytical balance level indicator bubble was outside the circle of accepted
range.

Requirement: Always check that the air bubble is in the center of the level indicator before
each weighing. Use the leveling feet to make adjustments. Once leveled, always perform an
internal adjustment. The exact procedure is described in the operating instructions for the
balance. Ref: Mettler Toledo, Weighing the Right Way, January 2015, Section 3.

Comment: The air bubble of the analytical balances in the wet chemistry weighing room and
the semivolatiles analysis room were outside of the level indicator.

General Laboratory

Comment: All currently approved methods are not readily accessible to all analysts. The wet
chemistry laboratory has online access to the 22nd Edition of Standard Methods as a reference, which
does not include all methods or QC chapters currently approved and in use.

Proficiency Testing

Comment: The PT sample for Organochlorine Pesticides had several dilutions run. While running
multiple dilutions on samples suspected or known to contain high levels of target analytes is
considered acceptable practice, the laboratory QA Program and/or SOPs must include this
information as part of the PT program and laboratory practice.

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QA/QC

Recommendation: The laboratory SOP for extraction by separatory funnel (SOP ORG-PRP007-02)
mentions that the procedure may be used for Polychlorinated Biphenyls (PCBs) and Organochlorine
Pesticides. However, the SOP does not provide any option for solvent exchange or the final volume
of 10 mL. It is recommended that the laboratory eliminate the references to the above parameters or
refer the reader to the appropriate analytical SOPs to complete the necessary steps.

Recommendation: Client reports use the phrase “Method Quantitation Limit” but the SOPs do not
define this term or explain how it is derived. It is recommended that the SOPs incorporate these terms
into the next revision in order to improve data review.

N. Finding: The laboratory QA Manual does not state the frequency of updates to all parameter
QC items that use control charts.

Requirement: Each laboratory shall have a documented analytical quality assurance and
quality control program. Each laboratory shall have a copy of each approved test, analysis,
measurement, or monitoring procedure being used in the laboratory. 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. Ref: 15A NCAC 02H .0805 (a) (7).

Comment: Currently, the QA manual only addresses the frequency of control chart updates
for MS/MSD pairs.

O. Finding: Thermometers in the Fecal Coliform and E. Coli incubators are not consistently
verified against a Reference Temperature-Measuring Device at least every three months.

Requirement: Digital temperature-measuring devices and temperature-measuring devices
used in incubators shall be verified at the temperature of use every three months against a
Reference Temperature-Measuring Device and their accuracy shall be corrected. Ref: 15A
NCAC 02H .0805 (a) (7) (N) (iii).

Comment: The thermometer in Bath #3 (T142) was verified on April 20, 2021, August 2,
2021, November 15, 2021, and February 22, 2022. The Micro (T140) thermometer was
verified on March 19, 2021, June 30, 2021, October 13, 2021, and February 22, 2022.

P. Finding: The laboratory is not correctly verifying the infrared (IR) temperature-measuring
device against a Reference Temperature-Measuring Device.

Requirement: Infrared temperature-measuring devices shall be verified every three months
at three different temperatures over the temperature range of use against a Reference
Temperature-Measuring Device and their accuracy shall be corrected. Each day of use,
infrared temperature-measuring devices shall be verified against a non-Reference
Temperature-Measuring Device that meets NIST specifications for accuracy. If the infrared
temperature-measuring device does not agree within 0.5 degrees Celsius during the daily
verification, the laboratory shall take corrective action. Ref: 15A NCAC 02H .0805 (a) (7) (N)
(iv).

Comment: The laboratory is verifying at two temperatures. Three temperatures are required.

Q. Finding: The laboratory is not verifying the infrared (IR) temperature-measuring device each
day of use.

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Requirement: Infrared temperature-measuring devices shall be verified every three months
at three different temperatures over the temperature range of use against a Reference
Temperature-Measuring Device and their accuracy shall be corrected. Each day of use,
infrared temperature-measuring devices shall be verified against a non-Reference
Temperature-Measuring Device that meets NIST specifications for accuracy. If the infrared
temperature-measuring device does not agree within 0.5 degrees Celsius during the daily
verification, the laboratory shall take corrective action. Ref: 15A NCAC 02H .0805 (a) (7) (N)
(iv).

R. Finding: The State Laboratory is not notified when samples are received out of holding time
or do not meet thermal and/or chemical preservation requirements. Cited Previously on July
21, 2016.

Requirement: Sample preservation shall be verified and documented. If a laboratory receives
a sample subject to G.S. 143-215.1 and 143-215.63 that does not meet sample collection,
holding time, or preservation requirements, the laboratory shall document the incident, notify
the sample collector or client, and secure another sample that meets the regulatory
requirements, if possible. If another viable sample cannot be secured, the original sample may
be analyzed but the results reported shall be qualified with the nature of the sample collection,
holding time, or preservation infractions and the laboratory shall notify the State Laboratory of
the infractions. The notification shall include a statement indicating corrective action taken to
prevent future infractions. Ref: 15A NCAC 02H .0805 (a) (7) (M).

S. Finding: The laboratory is not including both the original and manually integrated
chromatograms in the data package when manual integrations are performed.

Requirement: When manual integration is employed, the laboratory must clearly identify
manually integrated compounds, document the reason the manual integration was performed,
the date performed and who completed the work. A flag or qualifier code may suffice for simple
manual integrations. In addition, a hardcopy printout of the data displaying the manual
integration shall be included in the raw data package (i.e., both the original and manually
integrated chromatograms, of similar scale, must be present in the data package). All
information necessary for the historical reconstruction of data must be maintained by the lab.
Additionally, the laboratory must employ a systematic data validation procedure to check
manual integrations to assure integrations are technically sound and representative of the
response. Ref: NC WW/GW LCB Manual Integration Policy.

Comment: This Finding includes, but is not limited to, chromatograms generated for the
following parameter methods:
• Anions – EPA 300.0, Rev. 2.1, 1993 (Aqueous & Non-Aqueous)
• Anions – SW-846 9056 A (Aqueous & Non-Aqueous)
• Base Neutral/Acid, Organics – EPA 625.1, December 2016 (Aqueous)
• Base Neutral/Acid, Organics – SW-846 8270 E (Aqueous & Non-Aqueous)
• Extractable Petroleum Hydrocarbons – MADEP, December 2019, Rev. 2.1 (Aqueous
& Non-Aqueous)
• Pesticides, Organochlorine – EPA 608.3, December 2016 (Aqueous)
• Pesticides, Organochlorine – SW-846 8081 B (Aqueous & Non-Aqueous)
• Polychlorinated Biphenyls (PCBs) – EPA 608.3, December 2016 (Aqueous)
• Polychlorinated Biphenyls (PCBs) – SW-846 8082 A (Aqueous, Non-Aqueous & Oil)
• Purgeable, Organics – EPA 624.1, December 2016 (Aqueous)
• Purgeable, Organics – SW-846 8260 D (Aqueous & Non-Aqueous)
• TPH Diesel Range, Organics – SW-846 8015 C (Aqueous & Non-Aqueous)
• TPH Gasoline Range, Organics – SW-846 8015 C (Aqueous & Non-Aqueous)
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• Volatile Petroleum Hydrocarbons – MADEP, Feb 2018, Rev. 2.1 (Aqueous & Non-
Aqueous)

Comment: The laboratory Manual Integration SOP (QAU-GEN003-02) states in Section 6.0
that “If the QDEL function is used, the deletion should be marked as a “d” next to the
compound. The ion profile or peak must be printed, and an explanation of the deletion should
be documented.” The data reviewed did not include the peak that was deleted, nor an
explanation of the deletion.

T. Finding: The laboratory is not always examining computerized data reduction properly to
ensure that peaks are integrated correctly.

Requirement: All computerized data reduction must be reviewed carefully by the analyst to
determine the accuracy and appropriateness of the quantitation performed by the data
system. Any errors must be corrected using this document as a guideline to define appropriate
integration. The document must describe procedures for completing and documenting
corrections to analytical results. The failure of the software to appropriately integrate a peak
is usually obvious from visual inspection of the chromatogram (i.e., at an appropriate scale -
enlarged chromatograms must be used to discern baseline noise). Ref: NC WW/GW LCB
Manual Integration Policy.

Comment: Multiple instances were noted where the Chemstation software had improperly
integrated peaks. These errors were often caused by examining the chromatogram at an
inappropriate scale.

U. Finding: The laboratory manually integrates chromatograms without documenting the reason
why the manual integration was performed. Cited Previously on July 21, 2016.

Requirement: All data must be integrated consistently in standards, samples and QC
samples. Integration parameters (both automated and manual) must adhere to valid scientific
chromatographic principles. Manual integration is employed to correct an improper integration
performed by the data system and must always include documentation clearly stating the
reason the manual integration was performed and who completed the work. Under no
circumstances should manual integration be performed solely for the purpose of meeting
quality control criteria. Ref: NC WW/GW LCB Manual Integration Policy.

V. Finding: The laboratory was not able to demonstrate compliance with current ongoing
Method Detection Limit (MDL) requirements for all applicable parameter methods, where
required.

Requirement: During any quarter in which samples are being analyzed, prepare and analyze
a minimum of two spiked samples on each instrument, in separate batches, using the same
spiking concentration used in Section 2. If any analytes are repeatedly not detected in the
quarterly spiked sample analyses, or do not meet the qualitative identification criteria of the
method (see Section 2(c) of this procedure), then this is an indication that the spiking level is
not high enough and should be adjusted upward. Note that it is not necessary to analyze
additional method blanks together with the spiked samples, the method blank population
should include all of the routine method blanks analyzed with each batch during the course of
sample analysis. Ref: Code of Federal Regulations, Title 40, Part 136; Federal Register Vol.
82, No. 165, August 28, 2017; Appendix B–Definition and Procedure for the Determination of
the Method Detection Limit–Revision 2. (3) (a).

Requirement: Ensure that at least seven spiked samples and seven method blanks are
completed for the annual verification. If only one instrument is in use, a minimum of seven
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spikes are still required, but they may be drawn from the last two years of data collection. Ref:
Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 82, No. 165, August
28, 2017; Appendix B–Definition and Procedure for the Determination of the Method Detection
Limit–Revision 2. (3) (b).

Requirement: At least once every thirteen months, re-calculate MDLs and MDLb from the
collected spiked samples and method blank results using the equations in Section 2. Ref:
Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 82, No. 165, August
28, 2017; Appendix B–Definition and Procedure for the Determination of the Method Detection
Limit–Revision 2. (4) (a).

W. Finding: The laboratory has not established an acceptance criterion for the back-calculation
of the standard at the lowest reporting concentration.

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).

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: This Finding applies to TKN by EPA Method 351.2, Rev. 2.0.

X. 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 LCB Matrix Spiking Policy.

Comment: This Finding applies to TKN by EPA Method 351.2, Rev. 2.0.

Comment: The spike volume is 5%.

Y. Finding: Preservation acid is not being added to reagent (method) blanks.

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. Ref:
EPA Method 353.2, Rev. 2.0 (1993). Section 3.6.

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Requirement: A reagent blank (method blank) consists of reagent water (see Section 1080)
and all reagents (including preservatives) that typically are in contact with a sample during the
entire analytical procedure. The reagent blank is used to determine whether and how much
reagents and the preparative analytical steps contribute to measurement uncertainty. Ref:
Standard Methods 4020 B-2014. (5).

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. The reagent blank is used to determine whether and how
much reagents and the preparative analytical steps contribute to measurement uncertainty.
Ref: Standard Methods 5020 B-2017. (5).

Comment: This Finding applies to samples analyzed for COD and NO2+NO3 Nitrogen.

Comment: The laboratory needs to ensure that chemical preservatives are added to all
reagent blanks for all parameters where chemical preservation is required.

Reporting

Z. Finding: The laboratory is not properly qualifying all results on the client report. Cited
Previously on July 21, 2016.

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: Current laboratory practice for Base Neutral/Acid Organics samples that do not
have detections is that when a Continuing Calibration Verification (CCV) standard is biased
low, a reporting limit standard is analyzed and data is qualified on the client report. If a CCV
standard is biased high without sample detections, data is reported without qualification. Even
if the impact of a QC failure is minimal, the associated data must be qualified. This situation
must also be addressed in the next laboratory QA manual revision.

Comment: Samples for pH are sometimes analyzed at the bench out of holding time. The
client report includes a paragraph on the cover page stating the report contains pH sample
results that were analyzed out of holding time, but this is the only place the qualifier is
documented in the report. It is a general statement and does not specifically list the individual
sample that is out of holding time.

Recommendation: It is recommended that the laboratory qualifier code be placed adjacent
to the actual result.

AA. Finding: Data is not always qualified when quality control failures occur.

Requirement: If quality control results fall outside established limits or show an analytical
problem, the laboratory shall identify the Root Cause of the failure. The problem shall be
resolved through corrective action, the corrective action process documented, and any
samples involved shall be reanalyzed, if possible. If the sample cannot be reanalyzed, or if
the quality control results continue to fall outside established limits or show an analytical
problem, the results shall be qualified as such. Ref: 15A NCAC 02H .0805 (a) (7) (B).

Comment: Multiple samples analyzed on June 21, 2021 for Organochlorine Pesticides by
EPA 608.3 were affected by an ending CCV that failed low for a significant number of analytes.
Surrogates were also low. The analyst was aware of the failure and made a comment in the
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"Additional Text" field but failed to check a checkbox that would have flagged the associated
data. Consequently, the data was reported to clients without qualification. Revised reports
to the affected clients will be required as part of the Corrective Action.

BB. Finding: Values less than the established reporting limit are being reported on the client
report.

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. Ref: 15A NCAC 02H
.0805 (a) (7) (H).

Comment: The MDL is being used as the reporting limit for Base Neutral/Acid Organics and
ICP-MS metals, Mercury and Purgeable Organics, rather than the concentration of the lowest
standard. No qualifiers were noted in the case narratives regarding the MDL being used as
the reporting limit. The laboratory SOP and QA manual both require the reporting limit be set
at or above the concentration of the lowest standard.

Comment: A reporting limit of 1.14 mg/L for Total Hardness was observed for Client Report
21-307-0012. The SOP for Hardness (WET-GEN009-12) defines the reporting limit as 5 mg/L.

Comment: Client report 21-244-0017 dated September 20, 2021 reported an MDL for
Turbidity of 0.49 NTU and an MQL of 1.0 NTU. The laboratory SOP for Turbidity (WET-
GEN003-05) defines the reporting limit as 1.0 NTU. Sample results were reported as < 0.49
NTU.

CC. Finding: The laboratory does not report results of all tests on the characteristics of the effluent
when duplicate sample analyses are performed.

Requirement: The results of all tests on the characteristics of the effluent, including but not
limited to NPDES Permit Monitoring Requirements, shall be reported on monthly report forms.
Ref: 15A NCAC 2B .0506 (b) (3) (J).

Requirement: Any average for Fecal Coliform is to be calculated as a geometric mean. Ref:
Directions for Completing Monthly Discharge Monitoring Reports, Section II, (8).

Comment: When samples are duplicated for Fecal Coliform and E. Coli analyses, only the
value of the first sample is in the client report. The client report does not include the duplicate
result or the geometric mean of the results.

Comment: This Finding applies to Fecal Coliform and E. Coli samples analyzed by Standard
Methods, 9222 D-2015 (MF) (Aqueous), IDEXX Colilert-18® (Aqueous) and IDEXX Colilert®
(24 hr) (Aqueous).

Bacteria, Coliform Fecal – Standard Methods, 9221 E-2014 (MPN) (Aqueous & Biosolids)
Bacteria, Coliform Fecal – Standard Methods, 9222 D-2015 (MF) (Aqueous & Biosolids)

DD. Finding: The autoclave log does not include the time that media are withdrawn from the
autoclave to demonstrate that media are in the autoclave for 45 minutes or less after the
sterilization period has concluded. This is considered pertinent information.

Requirement: All analytical records, including original observations and information
necessary to facilitate historical reconstruction of the calculated results, shall be maintained
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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 each run cycle, record the items sterilized, sterilization temperature,
total run time (heat exposure), programmed/preset sterilization period, actual pressure
readings, and analyst initials. Ensure that the autoclave maintains 121°C with minimal
temperature variation at ≥15 lb/in.2 (≥103 kPa) for 15 min during the media sterilization
cycle and that media are withdrawn from the autoclave in 45 min or less. Ref: Standard
Methods 9020 B-2015. (4) (h).

Bacteria, Coliform Fecal – Standard Methods, 9221 E-2014 (MPN) (Biosolids)
Bacteria, Coliform Fecal – Standard Methods, 9222 D-2015 (MF) (Biosolids)

EE. Finding: An inconsistency was noted between the SOP and laboratory practice as follows:
The SOP states that samples analyzed by Standard Methods, 9221 E-2014 (MPN)
(Biosolids) and Standard Methods, 9222 D-2015 (MF) (Biosolids) have a 24-hour holding
time. Laboratory practice is to analyze them within 8 hours.

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. 86, No. 95, May 19, 2021;
Table II, Footnote 22.

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: The 24-hour holding time only applies to EPA Methods 1680 and 1681 and the
laboratory is not certified for these methods.

FF. Finding: The laboratory is not heating the evaporating dishes in a 103–105°C oven for ≥1
hour prior to sample analysis for percent solids.

Requirement: Preparation of evaporating dish - If only measuring total solids, heat dish for
≥1 hour in a 103–105°C oven. Cool in desiccator to ambient temperature and weigh. Store
in desiccator or 103–105°C oven until needed. Ref: Standard Methods, 2540 G-2015. (3)
(a) (1).

GG. Finding: The drying cycle is not repeated until a weight change of <50 mg is achieved.

Requirement: Repeat cycle (drying, cooling, desiccating, and weighing) until weight
change is <50 mg. Ref: Standard Methods, 2540 G-2015. (2) (b).

Alkalinity – Standard Methods, 2320 B-2011 (Aqueous)

HH. Finding: The volume analyzed for low-alkalinity samples is not between 100 and 200 mL.

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Requirement: Report alkalinity less than 20 mg CaCO3/L only if it has been determined by
the low-alkalinity method of 2320B.4d. Ref: Standard Methods, 2320 B-2011. (1) (d).

Requirement: Potentiometric titration of low alkalinity: For alkalinities less than 20 mg/L titrate
100 to 200 mL according to the procedure of ¶ c above, using a 10 mL microburet and 0.02N
standard acid solution. Ref: Standard Methods, 2320 B-2011. (4) (d).

Comment: Alkalinity is considered a method-defined parameter per the definition in the Code
of Federal Regulations, Part 136.6, Section (a) (5). This means the method must be followed
as written.

Comment: The laboratory analyzes 50 mL for low-alkalinity samples.

BOD – Standard Methods, 5210 B-2016 (Aqueous)
CBOD – Standard Methods, 5210 B-2016 (Aqueous)

II. Finding: The laboratory benchsheet for BOD/CBOD is lacking required documentation:
quality control assessments.

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: 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 that samples are analyzed. Ref: 15A
NCAC 02H .0805 (a) (7) (F) (xv).

Comment: Calibration buffer true values are documented in the columns for the true and
observed values of the check buffer, which are not documented elsewhere..

JJ. Finding: Calculated results of sample dilutions are not being evaluated to ensure ≤ 30%
difference between valid high and low values.

Requirement: Identify results in the test reports when any of the following QC conditions
occur: test replicates show >30% difference between highest and lowest values. Ref:
Standard Methods, 5210 B-2016. (7) (b).

KK. Finding: The laboratory is not analyzing a check standard buffer after calibration and prior to
sample analysis.

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. If the meter
response shows a difference greater than 0.1 pH unit from expected value, look for trouble
with the electrodes or potentiometer. Ref: Standard Methods, 4500 H+ B-2011. (4).

Comment: This Finding applies to the pH meter used in BOD/CBOD analyses.

Chromium, Hexavalent – Standard Methods, 3500 Cr- B-2011 (Aqueous)

Comment: On the benchsheet the column "drops Acid added" is not required, just the documented
verification of sample pH 2.0 ± 0.5 S.U. However, if the column is retained, the type of acid must be
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documented since it could be either H3PO4 or 0.2N H2SO4 depending which point in the procedure
this represents.

Chromium, Hexavalent – SW-846 7196 A (Non-Aqueous)

LL. Finding: The laboratory does not document that each sample pH has been adjusted to 7.5 ±
0.5 S.U. following digestion. This is considered pertinent information.

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: 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. If the pH of the
digest should deviate from the desired range, discard the solution and redigest. Ref: EPA SW-
846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition,
Method 3060A, Rev. 1, December 1996, Section 7.7.

COD – Standard Methods, 5220 D-2011 (Aqueous)
COD – Hach 8000 (Aqueous)

MM. Finding: The laboratory does not analyze low range samples correctly.

Requirement: For COD values between 100 and 900 mg/L, increase in Cr3+ in the 600-nm
region is determined. Higher values can be obtained by sample dilution. COD values of 90
mg/L or less can be determined by following the decrease in Cr2O72- at 420 nm. The
corresponding generation Cr3+ gives a small absorption increase at 420 nm, but this is
compensated for in the calibration procedure. Ref: Standard Methods 5220 D-2011 (1).

Comment: COD is considered a method-defined parameter per the definition in the Code
of Federal Regulations, Part 136.6, Section (a) (5). This means the method must be
followed as written.

Comment: The laboratory has a reporting limit of 50 mg/L and analyzes a reporting limit
standard with each batch.

Comment: The laboratory may either obtain the low-level reagent kit and have a separate
calibration curve for low range samples or raise the reporting limit to 100 mg/L.

NN. Finding: An inconsistency was noted between the SOP and laboratory practice as follows:
Personnel were not following procedures as stated in the Laboratory’s SOP. The SOP is in
direct conflict with method and/or regulatory requirements.

Requirement: Each laboratory shall have a documented analytical quality assurance and
quality control program. Each laboratory shall have a copy of each approved test, analysis,
measurement, or monitoring procedure being used in the laboratory. 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
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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).

Comment: The laboratory is drying KHP at 100°C. The laboratory SOP states the drying
temperature is 120°C, however, Standard Methods states to dry at 110 °C. COD is a method-
defined parameter, and therefore must be followed as written.

Color, PC – Standard Methods, 2120 B-2011 (Pt-Co) (Aqueous)

OO. Finding: The laboratory benchsheet is lacking required documentation: the proper units of
measure, all quality control assessments and any other data needed to reconstruct the final
result.

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, all quality control assessments and any other data needed to reconstruct the final
result. Each item shall be recorded each time that samples are analyzed. Ref: 15A NCAC
02H .0805 (a) (7) (F) (xii), (xv) and (xviii).

Comment: The pH meter used (ID#: pH0016) holds an internal calibration, but this calibration
information is not transferred to the LIMS or documented.

Comment: The benchsheet does not contain the units of measure.

PP. Finding: The laboratory needs to increase traceability of consumables used in the analysis
of Color.

Requirement: 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: The laboratory benchsheet is lacking the comparison standard reference ID and
the filter lot number.

Conductivity – EPA 120.1, Rev. 1982 (Aqueous)
Conductivity – Standard Methods, 2510 B-2011 (Aqueous)
Conductivity – SW-846 9050 A (Aqueous)

QQ. Finding: The Automatic Temperature Compensator (ATC) check is not being performed.

Requirement: The State Laboratory may develop Approved Procedures for Field
Parameters based upon the methods in any of the sources referenced in Parts(a)(1)(A)
through (F) of this Rule. Ref: 15A NCAC 02H .0805 (a) (1) (F).

Requirement: The Automatic Temperature Compensator (ATC) must be verified prior to
initial use and annually (i.e., 12 months) thereafter at two temperatures by analyzing a
standard or sample at 25°C (i.e., the temperature to which conductivity values are reported)
and a temperature(s) that brackets the temperature ranges of the environmental samples
routinely analyzed. This may require the analysis of a third temperature reading that is >
25°C. As the temperature increases or decreases, the value of the conductivity standard or
sample must be within ±10% of the true value of the standard or ±10% of the value of the
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sample at 25°C. If not, corrective action must be taken. Ref: NC WW/GW LCB Approved
Procedure for the Analysis of Specific Conductance (Conductivity).

Cyanide – Standard Methods, 4500 CN E-2016 (Aqueous)

RR. Finding: Sample preservation verification checks performed at the laboratory benchtop are
not consistently documented.

Requirement: Sample preservation shall be verified and documented. Ref: 15A NCAC 02H
.0805 (a) (7) (M).

Comment: A column on the laboratory benchsheet is provided to document that the sample
pH is > 12 S.U. but a check mark is not always recorded in this space. Data submitted prior
to the inspection for Project #V11119 and V804 were lacking the check mark to indicate that
the preservation requirement had been verified.

Comment: The preservation requirements listed in Code of Federal Register, Title 40, Part
136, Federal Register Vol. 86 No. 95 May 19, 2021, Table II, state that the pH be >10 S.U.
The laboratory may therefore choose to preserve samples to pH >10 S.U., rather than >12
S.U.

SS. Finding: The laboratory benchsheet occasionally lacks required documentation: the volume
of sample analyzed.

Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data
shall be traceable to the associated sample analyses and shall consist of: the volume of
sample analyzed, where applicable. Each item shall be recorded each time that samples
are analyzed. Ref: 15A NCAC 02H .0805 (a) (7) (F) (xi).

Comment: The laboratory digestion worksheet has a column to record the “aliquot sample”
final volume, but this column is not always filled out. Data reviewed prior to the inspection
lacked the final volume for Project #V11119 and V804.

pH – Standard Methods, 4500 H+B-2011 (Aqueous)

Comment: Duplicates are being analyzed for pH. Duplicates are not required for Field parameters.
This applies to bench and field analyses.

Comment: The method only requires that one buffer be analyzed as a Check Standard Buffer. The
laboratory’s current practice is to read back each calibration buffer as well as an outside source check
standard buffer.

Recommendation: The calibration check buffer is not clearly stated on the benchsheet. It is
recommended that the laboratory change "Readback" to "Check Buffer". This applies to bench and
Field analyses.

TT. Finding: The laboratory is not analyzing a post-analysis check standard buffer when analyses
are performed at multiple sample sites on a single day.

Requirement: The State Laboratory may develop Approved Procedures for Field Parameters
based upon the methods in any of the sources referenced in Parts(a)(1)(A) through (F) of this
Rule. Ref: 15A NCAC 02H .0805 (a) (1) (F).

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Requirement: When performing analyses at multiple sample sites, a post-analysis calibration
verification using the check standard buffer must be analyzed at the end of the run. It is
recommended that a mid-day check standard buffer be analyzed when samples are analyzed
over an extended period of time. The post-analysis check standard buffer(s) must read within
±0.1 S.U. or corrective actions must be taken. If recalibration is necessary, all samples
analyzed since the last acceptable calibration verification must be reanalyzed, if possible. If
samples cannot be reanalyzed, the data must be qualified. Ref: NC WW/GW LCB Approved
Procedure for the Analysis of pH.

Comment: This Finding applies to pH analyses performed in the field.

UU. Finding: The laboratory is not using fresh aliquots of standard buffers to calibrate the pH
meter each day.

Requirement: The State Laboratory may develop Approved Procedures for Field Parameters
based upon the methods in any of the sources referenced in Parts(a)(1)(A) through (F) of this
Rule. Ref: 15A NCAC 02H .0805 (a) (1) (F).

Requirement: The calibration and check standard buffers must bracket the range of the
samples being analyzed. A portion of the standard buffer is not to be used for more than one
calibration. Discard any used buffer portions. Do not pour unused portions back into the
original bottle. Ref: NC WW/GW LCB Approved Procedure for the Analysis of pH.

Comment: The buffers are poured into a plastic tube from the stock buffers in the main lab.
These are poured up at the beginning of the week and replaced weekly.

Comment: This Finding applies to pH analysis performed in the field.

VV. Finding: Values were reported that exceed the method specified accuracy of 0.1 units.

Requirement: By careful use of a laboratory pH meter with good electrodes, a precision of
±0.02 unit and an accuracy of ±0.05 unit can be achieved. However, ± 0.1 pH unit represents
the limit of accuracy under normal conditions, especially for measurement of water and poorly
buffered solutions. For this reason, report pH values to the nearest 0.1 pH unit. Ref: Standard
Methods, 4500 H+ B-2011. (6).

Comment: The laboratory currently reports pH sample results to two decimal places on client
reports.

Comment: This Finding applies to pH analyses performed in the laboratory and in the field.

Hardness – Standard Methods, 2340 C-2011 (Aqueous)

WW. Finding: Documentation does not demonstrate that the samples were titrated within five
minutes of the addition of the buffer. This is considered pertinent information.

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: Select a sample volume that requires less than 15 mL EDTA and complete
titration within 5 min, measured from time of buffer addition. Ref: Standard Methods, 2340
C-2011. (3) (b).
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Ignitability – SW-846 1030 (Non-Aqueous)

XX. Finding: A description of the material, the sample pre-test results, particle size, temperature
of the test material (°C), air velocity through the fume hood (m/s) and burn rate are not
documented. This is considered pertinent information.

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: The NC WW/GW Laboratory Certification Branch must confirm that
analytical data is valid by reviewing the QA/QC data generated during the sampling and
analysis procedures when implementing SW-846 methods in order to be assured that
scientifically sound decisions are made which will be protective of human health and the
environment. 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 LCB SW-846 Method Implementation Policy.

Comment: The laboratory only documents the preliminary screening for “Negative” or
“positive” and the burn time in seconds. Results of the pre-test to determine if the sample is
explosive or extremely flammable are not documented.

YY. Finding: An inconsistency was noted between the SOP and laboratory practice as follows:
the laboratory is not reporting results in the units of mm/sec and applying the “Positive” or
“Negative” qualifiers as required by the SOP.

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: The SOP (WET-GEN035-04) Section 9.1.6 states that if the result of the
preliminary screening test is negative, results are to be reported as 0 mm/sec and a qualifier
of “Negative” added. Section 9.3 states to calculate the average of the three results of the
burn rate portion of the test and add a qualifier to report the results as “Positive” or “Negative”.
The laboratory is reporting results as “Negative” without a numeric value for the burn rate. The
method only requires reporting the burn rate. The addition of “positive” or “negative” is not
required.

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MBAS – Standard Methods, 5540 C-2011 (Aqueous)

Comment: The reporting limit documented at the top left corner of the laboratory sample preparation
log for MBAS does not match the reporting limit on the client report. There is a column header on the
log captioned "Reporting Limit". In the column, the reporting limit is written in as 0.2 mg/L, which does
not match the lowest standard in the calibration curve and the client report, which is 0.1 mg/L. This
appears to be a copy and paste error.

Nitrogen, Ammonia – Standard Methods, 4500 NH3 G-2011 (Aqueous)
Nitrogen, Ammonia – Standard Methods, 4500 NH3 D-2011 (Aqueous)
Nitrogen, Ammonia – Standard Methods, 4500 NH3 C-2011 (Aqueous & Non-Aqueous)

ZZ. Finding: Samples are not checked for Total Residual Chlorine in the laboratory prior to
analysis.

Requirement: Residual Chlorine reacts with ammonia; remove by sample pretreatment. If a
sample is likely to contain residual chlorine, immediately upon collection, treat with
dechlorinating agent as in 4500-NH3.B.3d. Ref: Standard Methods, 4500 NH3 A-2011. (2).

Chromium Hexavalent - Standard Methods, 3500 Cr B-2011 (Aqueous)
Nitrogen, Ammonia - Standard Methods, 4500 NH3 G-2011 (Aqueous)
Nitrogen, Nitrite - Standard Methods, 4500 NO2- B-2011 (Aqueous)
Nitrogen, NO3 + NO2 - Standard Methods, 4500 NO3- F-2016 (Aqueous)
Phosphate, Ortho - Standard Methods, 4500 P E-2011 (Aqueous)
Phosphorus, Total - Standard Methods, 4500 P E-2011 (Aqueous)
Phosphorus, Total - Standard Methods 4500 P F-2011 (Aqueous)

AAA. 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 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: Compare each calibration point to the curve and recalculate its concentration.
If any recalculated values are not within the method's acceptance criteria -- up to twice the
MRL ±50%; between 3 and 5 times the MRL ±20%; or greater than 5 times the MRL ±10% --
unless otherwise specified in individual methods, identify the source of any outlier(s) and
correct before sample quantitation. Ref: Standard Methods, 3020 B-2017. (1) (b).

Requirement: Compare each calibration point to the curve and recalculate its concentration.
If any recalculated values are not within the method's acceptance criteria -- up to twice the
MRL ±50%; between 3 and 5 times the MRL ±20%; or greater than 5 times the MRL ±10% --
unless otherwise specified in individual methods, identify the source of any outlier(s) and
correct before sample quantitation. Ref: Standard Methods, 4020 B-2014. (1) (b).

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Nitrogen, Nitrite – Standard Methods, 4500 NO2- B-2011 (Aqueous)

BBB. Finding: The laboratory does not document that the sample pH is between 5-9 S.U. before
color reagent is added. This is considered pertinent information.

Requirement: If sample pH is not between 5 and 9, adjust to that range with 1N HCl or NH4OH
as required. Ref: Standard Methods, 4500 NO2- B-2011. (4) (b).

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).

Comment: The exact pH does not need to be recorded, but acknowledgment that the pH was
between 5 and 9 S.U. must be documented.

CCC. Finding: The MS/MSD are prepared with greater than 5% spike solution by 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 LCB Matrix Spiking Policy.

Comment: The benchsheet states that the laboratory uses 5mL of spike solution and 45mL
of sample. The SOP states that 0.5 mL of spike solution is used in a total volume of 50mL,
which is an acceptable volume and would not require sample concentration adjustment.

Nitrogen, NO3 + NO2 - Standard Methods, 4500 NO3- F-2016 (Aqueous)
Nitrogen, NO3 + NO2 - EPA Method 353.2, Rev. 2.0, 1993. (Aqueous)

DDD. Finding: Samples are not consistently chemically preserved within fifteen minutes.

Requirement: Except where noted in this Table II and the method for the parameter, preserve
each grab sample within 15 minutes of collection. For a composite sample collected with an
automated sample (e.g., using a 24-hour composite sample; see 40 CFR 122.21 (g)(7)(i) or
40 CFR Part 403, Appendix E), refrigerate the sample at ≤6°C during collection unless
specified otherwise in this Table II or in the method(s). For a composite sample to be split into
separate aliquots for preservation and/or analysis, maintain the sample at ≤6°C, unless
specified otherwise in this Table II or in the method(s), until collection, splitting, and
preservation is completed. Add the preservative to the sample container prior to sample
collection when the preservative will not compromise the integrity of a grab sample, a
composite sample, or aliquot split from a composite sample within 15 minutes of collection. If
a composite measurement is required but a composite sample would compromise sample
integrity, individual grab samples must be collected at prescribed time intervals (e.g., 4
samples over the course of a day, at 6-hour intervals). Ref: Code of Federal Regulations, Title
40, Part 136; Federal Register Vol. 86, No. 95, May 19, 2021; Table II, Footnote 2.

Comment: Unpreserved samples are occasionally preserved at the bench within 48 hours of
collection and analyzed.

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EEE. Finding: The ICV standard is not properly identified on the benchsheet.

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: The standard preparation section of the benchsheet lists both an "ICV" and a
"CCV" standard preparation, however there is no standard labeled as "ICV" included in the
analysis run log. The analyst stated that the first standard labeled as "CCV" in the analysis
run log is the "ICV" standard.

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

FFF. Finding: The temperature of the block digestor is not checked and documented to be 160°C
prior to digestion. This is considered pertinent data.

Requirement: Place tubes in block digestor preheated to 160°C and maintain temperature
for one hour. Ref: EPA Method 351.2, Rev. 2.0 (1993), Section 11.4.

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).

GGG. Finding: The laboratory is not properly preparing matrix spike samples that are above the
calibration range.

Requirement: The concentration of the spiked samples must be bracketed by the calibration
range. If the spiked sample result is over the calibration range, the spiked sample must be
diluted and re-analyzed. It is not acceptable to dilute the sample first and then add the spike
solution so as not to affect bias attributed to matrix. Ref: NC WW/GW LCB Matrix Spiking
Policy.

Phosphorus, Ortho – Standard Methods, 4500 P E-2011 (Aqueous)

HHH. Finding: The laboratory is not consistently analyzing the LFM and LFMD at the required
frequency.

Requirement: The LFM is used to evaluate analyte recovery in a sample matrix. If an LFM is
feasible and the method does not specify LFM frequency requirements, then include at least
one LFM with each sample set (batch) or on a 5% basis, whichever is more frequent. Ref:
Standard Methods, 4020 B-2014. (7) and Table 4020:I.

Requirement: As a minimum, include one duplicate sample or one LFM duplicate with each
sample set (batch) or on a 5% basis, whichever is more frequent, and process it independently
through the entire sample preparation and analysis. Ref: Standard Methods, 4020 B-2014. (8)
and Table 4020:I.

Comment: No LFM or LFMD were included in batches V8393 and V11225.

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III. Finding: The laboratory is not qualifying results when samples are not filtered within 15
minutes of collection.

Requirement: Basic documentation requirements for the sample collector include: Chemical
and/or physical preservation/treatment(s) used where required (e.g., name of preservative,
pH<2, pH>9, field filtration, TRC neutralization, etc.). Ref: NC WW/GW LCB Sample
Collection, Preservation and Receipt Requirements Policy.

Comment: Benchsheets and Chain of Custody documents reviewed did not contain any
documentation that samples were filtered, so it cannot be assumed that field filtration is being
performed as required per Code of Federal Regulations, Title 40, Part 136; Federal Register
Vol. 82, No. 165, August 28, 2017; Table II.

Phosphorus, Total – Standard Methods, 4500 P F-2011 (Aqueous)

JJJ. Finding: The laboratory is not checking the pH of the digested sample and adjusting if
necessary.

Requirement: Cool, add 0.05 mL (1 drop) phenolphthalein indicator solution, and neutralize
to a faint pink color with NaOH. Ref: Standard Methods 4500 P B-2011. (5) (c).

Requirement: Add 0.05 mL (1 drop) phenolphthalein indicator solution to approximately 50
mL sample. If a red color develops, add H2SO4 (4500-P.F.3e) dropwise to just discharge the
color. Standard Methods 4500 P F-2011. (4).

Comment: Based on the two Requirements, it is understood that prior to sample analysis, the
pH of the sample is to be adjusted within a neutral pH.

Phosphorus, Total – EPA Method 365.1, Rev. 2.0, 1993 (Aqueous)

KKK. Finding: The laboratory does not analyze matrix spike samples at the required frequency.

Requirement: The laboratory must add a known amount of analyte to a minimum of 10% of
the routine samples. Ref: EPA Method 365.1, Rev. 2.0 (1993), Section 9.4.1

Comment: The SOP (WET-AA003-05) combines EPA Method 365.1, Rev. 2.0, 1993 and SM
4500 PF-2011 and only requires an MS/MSD pair per analytical batch of 20 samples, which
is a frequency of 5%. To combine the methods, the laboratory must use the strictest
requirement between the two methods.

LLL. Finding: The laboratory does not rerun samples whose computed value is less than 5% of its
predecessor.

Requirement: Any sample whose computed value is less than 5% of its immediate
predecessor must be rerun. Ref: EPA Method 365.1, Rev. 2.0 (1993), Section 12.2.

Comment: There were no instances of samples with concentrations <5% of the immediate
predecessor in the three data packs reviewed.

Oil & Grease – EPA 1664, Rev. B (Aqueous)

Comment: The laboratory analyzes the parameter using solid phase extraction.

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MMM. Finding: The laboratory benchsheet is lacking required documentation: sample preparation;
the proper units of measure; all manual calculations; all quality control assessments.

Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data shall
be traceable to the associated sample analyses and shall consist of: sample preparation, the
proper units of measure, all manual calculations and all quality control assessments. Each
item shall be recorded each time that samples are analyzed. Ref: 15A NCAC 02H .0805 (a)
(7) (F) (x) (xii) (xiv) (xv).

Comment: The data sheets do not include a post-analysis balance verification.

Comment: The data sheets were lacking the volume of acid used in the analysis, acceptance
criteria for the weight verification and units of measure for the temperature of the Speed Vap.

Residue, Dissolved 180 C – Standard Methods, 2540 C-2015 (Aqueous)
Residue, Suspended – Standard Methods, 2540 D-2015 (Aqueous)
Residue, Total - Standard Methods, 2540 B-2015 (Aqueous)

NNN. Finding: The laboratory benchsheet is lacking required documentation: the instrument
identification; the proper units of measure; all manual calculations; all quality control
assessments; and any other data needed to reconstruct the final calculated result.

Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data shall
be traceable to the associated sample analyses and shall consist of: the instrument
identification, the proper units of measure, all manual calculations, all quality control
assessments and any other data needed to reconstruct the final calculated result. Each item
shall be recorded each time that samples are analyzed. Ref: 15A NCAC 02H .0805 (a) (7) (F)
(iii) (xi) (xiv) (xv) (xviii).

Comment: The laboratory is not documenting that the weight change between drying cycles
is < 0.5 mg. No data was found that did not meet the weight change criterion.

Comment: The Dissolved Residue benchsheet for July 6, 2021 did not have the LCS ID#,
the balance ID and the filter lot ID documented. The Dissolved Residue benchsheet for
November 2, 2021 did not have the units of measure documented.

Comment: The Total Residue benchsheet for September 30, 2021 did not have the oven ID#
or the balance ID documented.

Residue, Dissolved 180 C – Standard Methods, 2540 C-2015 (Aqueous)

OOO. Finding: The laboratory is not properly evaluating the Method Blank.

Requirement: Using the same containers and glassware normally in contact with samples,
put 30 ml of DI water through the sample filter and proceed through the entire analytical
process. Acceptance criterion is <0.5 mg weight gain. Ref: NC WW/GW LCB Policy.

Comment: The laboratory was using a Method Blank acceptance criterion of < 25 mg/l.

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

Comment: It was noted during data review that the laboratory is diluting all digested samples and
standards to a final volume of 30 mL. This makes data reconstruction difficult without access to the
SOP or LIMS to view the preparation of individual standards, since standard preparation is recorded
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electronically. Section 8.2.3.1 of the SOP (MET-CVA001-12) lists concentrations of the calibration
standards at both a 20 mL volume (prior to digestion) and the 30 mL final volume. Calculations are
based on the concentration of the calibration curve standards at the 30 mL final volume. The SOP
does not include the concentration of calibration verification standards at the 30 mL final volume, and
this made data reproduction difficult. The analyst did not know why this was current practice but did
say it had been in place since before they started.

Comment: The laboratory is preparing the LFB and LFM by adding 2500 µL of a 0.075 mg/L standard
solution to 20 mL of reagent water and sample prior to digestion. After digestion, the sample is diluted
to a final volume of 30 mL. This yields a theoretical value of 6.25 µg/L. This is well above the midpoint
of the calibration curve. While this does not impact the final calculation and data quality, such a large
volume in the LFM may impact the identification of matrix interferences in the original sample. Adding
a smaller volume of a more concentrated standard solution with a theoretical value less than the
midpoint of the calibration curve would better evaluate potential interferences while maintaining
compliance with the analytical method.

Recommendation: It is recommended that the laboratory revise their digestion logs to eliminate
unnecessary columns and update preprinted headings to avoid strikethroughs.

PPP. 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 µg/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.

Comment: Section 11.2.2 states to process calibration standards as in 11.1.3 without heating.
EPA Region IV has given guidance that the reason this method does not include heating is
because the standards only include the inorganic form of Hg. Heating is meant to dissociate
organic or bound Hg and is therefore unnecessary. As such, EPA did not recommend
combining EPA 245.1 with SW-846 7470A since 7470A states that the standards are heated
like the samples. Laboratories may combine methods but would have to follow the EPA 245.1
requirements.

QQQ. Finding: The laboratory is not preparing the Laboratory Fortified Blank (LFB) at the correct
concentration.

Requirement: The LFB is prepared by fortifying a sample size volume of laboratory reagent
blank solution with mercury to a suitable concentration of >10X the MDL but less than the
midpoint concentration of the calibration curve. Ref: EPA Method 245.1, Rev. 3.0 (1994),
Section 7.11.

Comment: The laboratory is currently preparing the LFB at a concentration of 6.25 µg/L.
which is well above the midpoint of the calibration curve (4.6875 µg/L).

Metals – EPA 200.8, Rev. 5.4, 1994 (Aqueous)
Metals – SW-846 6020 B-2011 (Aqueous)

Recommendation: The laboratory is currently analyzing samples using both “Helium” and “No Gas”
modes. It is unclear from the data package review which elements are reported with which mode. It
is recommended that the data package document which mode is used for which elements.

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

RRR. Finding: An inconsistency was noted between the SOP and laboratory practice as follows:
the SOP does not mention filtering samples and standards post digestion.

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: When there are samples that need to be filtered post-digestion to eliminate high
solids content, the MS/MSD and an additional blank are filtered. The method does allow
filtration of samples after digestion. However, the process is not described in the SOP.

Metals – EPA 200.7, Rev. 4.4, 1994 (Aqueous)
Metals – SW-846 6010 D (Aqueous & Non-Aqueous)

SSS. Finding: An inconsistency was noted between the SOP and laboratory practice as follows:
The laboratory is not analyzing an ICS-AB at the end of the run.

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: Section 10.2.4 of the SOP states “At the end of the analytical run, a CCV, CCB,
an ICSA and ICS-AB are run and must pass the recovery requirements.”

Comment: Neither method require the spectral interference checks to be analyzed at the end
of the analytical sequence.

1,2-Dibromoethane (EDB) – SW-846 8011 (Includes DBCP) (Aqueous)

TTT. Finding: The laboratory is not using an acceptance criterion of less than 10% for the RSD of
the average calibration factor for the calibration curve.

Requirement: Analyze each calibration standard and tabulate peak height or area response
versus the concentration in the standard. Prepare a calibration curve for each compound.
Alternatively, if the ratio of response to concentration (calibration factor) is a constant over the
working range (< 10% relative standard deviation), linearity can be assumed and the average
ratio or calibration factor can be used in place of a calibration curve. Ref: EPA SW-846 Test
Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 8011
A. Rev. 0, July 1992, Section 7.2.2.

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Comment: The laboratory is using an acceptance criterion of less than or equal to 10%.

Base Neutral/Acid, Organics – SW-846 8270 E (Aqueous & Non-Aqueous)
Base Neutral/Acid, Organics – EPA 625.1, December 2016 (Aqueous)
TPH Diesel Range, Organics – SW-846 8015 C (Aqueous & Non-Aqueous)

UUU. Finding: The laboratory is not consistently calculating, evaluating and reporting detections in
the LRB.

Requirement: If quality control results fall outside established limits or show an analytical
problem, the laboratory shall identify the Root Cause of the failure. The problem shall be
resolved through corrective action, the corrective action process documented, and any
samples involved shall be reanalyzed, if possible. If the sample cannot be reanalyzed, or if
the quality control results continue to fall outside established limits or show an analytical
problem, the results shall be qualified as such. Ref: 15A NCAC 02H .0805 (a) (7) (B).

Requirement: The blank must meet the requirements in Section 8.5 before sample
extracts may be analyzed. Ref: EPA Method 625.1, December 2016, Section 13.6.

Requirement: If an analyte of interest is found in the blank: 1) at a concentration greater
than the MDL for the analyte, 2) at a concentration greater than one-third the regulatory
compliance limit, or 3) at a concentration greater than one-tenth the concentration in a
sample in the extraction batch, whichever is greater, analysis of samples must be halted,
and the problem corrected. Ref: EPA Method 625.1, December 2016, Section 8.5.2.

Requirement: Quality control procedures necessary to evaluate the GC system operation
are found in Method 8000 and include evaluation of retention time windows, calibration
verification and chromatographic analysis of samples. Ref: EPA SW-846 Test Methods for
Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 8015 C, February
2007, Section 9.3.

Requirement: Results of the method blank should be less than the lower limit of
quantitation (LLOQ) (Sec. 9.7) for the analyte or less than the level of acceptable blank
contamination specified in the approved QAPP or other appropriate systematic planning
document. Ref: EPA SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical
Methods; 3rd Edition, Method 8000 D, March 2018, Section 9.2.6.5.

Requirement: If the method blank results do not meet the acceptance criteria above, the
laboratory should take corrective action to locate and reduce the source of the
contamination and re-extract and reanalyze any samples associated with the contaminated
method blank. If the method blank results still do not meet the acceptance criteria in 9.2.6.5
and re-analysis is not practical, then the data user should be provided with the sample
results, the method blank results, and a discussion of the corrective actions undertaken by
the laboratory. Qualification of the samples may be needed. Ref: EPA SW-846 Test
Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 8000
D, March 2018, Section 9.2.6.6.

Requirement: The concentration of reagent, method, and calibration blanks shall not exceed
50 percent of the lowest reporting concentration or as otherwise specified by the reference
method. Ref: 15A NCAC 02H .0805 (a) (7) (H) (i).

Comment: During data review, it was noted that some LRBs for Diesel Range Organics
(DRO) had values that exceeded the requirement of ≤ ½ the concentration of the reporting
limit but were not qualified. The analysts noted that a linear regression was used as the
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calibration model. DRO results for the LRBs and samples were “zeroed out” if the response
from the instrument was less than the response of the lowest calibration standard, without
qualification or justification on the client report. The analyst also noted that a similar
approach was used for Benzoic Acid using EPA Method 625.1 and SW-846 8270 E. While
chromatographic analyses are heavily dependent on the judgement of the analyst, this is
not an acceptable justification. The auditor explained that bias on the low end of a
calibration curve is extremely likely with this calibration model, and that forcing the curve
through zero is permitted by the methods, which eliminates low bias, without using zero as
a calibration point.

Comment: Client reports associated with data that had been “zeroed out” lacked qualifiers
or discussion in the case narratives.

Comment: The analytical methods and NC WW/GW LCB Rules require corrective action
to be taken when a blank does not meet the acceptance criterion listed. Zeroing out a blank
is not listed as a possible corrective action in either. The blank acceptance criterion to follow
and corrective actions may be chosen from either the analytical method or NC WW/GW
LCB Rules but the SOP must clearly address what the acceptance criterion and corrective
action will be.

Comment: The analyst noted that after major equipment maintenance to both instruments,
calibration curves using a different model (the average calibration factor model) have been
successfully achieved and the practice has been discontinued.

Recommendation: It is recommended that this situation be addressed in the next revision
of the laboratory QA manual, as well as analyst training programs.

Base Neutral/Acid, Organics – SW-846 8270 E (Aqueous & Non-Aqueous)
Base Neutral/Acid, Organics – EPA 625.1, December 2016 (Aqueous)

VVV. Finding: Acceptance criteria for the surrogate compounds have not been updated.

Requirement: Once established, control limits should be reviewed regularly and updated
on a routine basis as established by the laboratory’s quality management plan. Reviewing
appropriateness of these criteria with respect to generated data is especially important for
newly implemented procedures or those not in continual use. The laboratory should monitor
trends in both analyte recovery performance and also in the control limits. Control limits
used to evaluate sample results should be those in place at the time of sample analysis.
Once control limits are updated, they should apply to all subsequent analyses of new
samples. Ref: EPA SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical
Methods; 3rd Edition, Method 8000 D. Rev. 5, March 2018, Section 9.6.5.

Requirement: The NC WW/GW Laboratory Certification Branch must confirm that
analytical data is valid by reviewing the QA/QC data generated during the sampling and
analysis procedures when implementing SW-846 methods in order to be assured that
scientifically sound decisions are made which will be protective of human health and the
environment. 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
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criteria for method performance but may not omit or use less stringent criteria than that
stated in SW-846 methods. Ref: NC WW/GW LCB SW-846 Method Implementation Policy.

Comment: The low and high control limits for each surrogate compound in the Chemstation
analytical software have not been updated to the most recent limits. The analyst did not know
when the last updates occurred but noted that the limits printed in the data packages were not
the current criteria. Without access to the laboratory LIMS, the data package cannot be
properly reviewed by a third party to determine if QC criteria have been met.

Pesticides, Organochlorine – EPA 608.3, December 2016 (Aqueous)
Polychlorinated Biphenyls (PCBs) – EPA 608.3, December 2016 (Aqueous)

Comment: Sample 89261 was collected as a composite sample and is supposed to be a grab
sample, per EPA 608.3. There was nothing on the Shipment Receipt Form mentioning that the sample
was improperly collected. The sample is for a pre-treatment agreement between Total Clean of North
Carolina, LLC and CMUD. The pretreatment agreement specifies the sample type as "Grab/Comp".
The project manager stated that they have always received composite samples from them for
organochlorine pesticides/PCB analyses. She stated that she would check with CMUD to ensure that
a composite sample is what they really want for those parameters.

Recommendation: It is recommended that the client report comment on the fact the sample type
was a composite instead of the method specified grab.

Pesticides, Organochlorine – EPA Method 608.3, December 2016 (Aqueous)
Pesticides, Organochlorine – SW-846 8081 B (Aqueous)

WWW. Finding: The laboratory is not documenting that samples are being checked and/or mitigated
for residual chlorine when samples are being tested for Aldrin.

Requirement: If aldrin is to be determined and residual chlorine is present, add 80 mg/L of
sodium thiosulfate but do not add excess. Any method suitable for field use may be employed
to test for residual chlorine (Reference 14). If sodium thiosulfate interferes in the determination
of the analytes, an alternative preservative (e.g., ascorbic acid or sodium sulfite) may be used.
Ref: EPA Method 608.3, Section 9.2.

Comment: Extractions personnel stated they always check samples for TRC but do not
document the result. They also stated that they have never seen a positive hit.

Pesticides, Organochlorine – EPA 608.3, December 2016 (Aqueous)
Pesticides, Organochlorine – SW-846 8081 B (Aqueous)
Polychlorinated Biphenyls (PCBs) – EPA 608.3, December 2016 (Aqueous)
Polychlorinated Biphenyls (PCBs) – SW-846 8082 A (Aqueous)

Recommendation: It is recommended that the laboratory begin including client instructions with
sample bottles shipped to clients stating not to pre-rinse bottles with sample prior to filling for
Organochlorine Pesticides and PCBs.

XXX. Finding: Samples are improperly transferred from the sample bottles to the separatory funnel.

Requirement: Mark the water meniscus on the side of the sample bottle for later
determination of sample volume. Pour the entire sample into the separatory funnel. Pipet the
surrogate standard spiking solution (Section 6.8.6) into the separatory funnel. Ref: EPA
Method 608.3, Section 10.2.2.

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Requirement: Using a 1-liter graduated cylinder, measure 1 liter (nominal) of sample.
Alternatively, if the entire contents of the sample bottle are to be extracted, mark the level
of sample on the outside of the bottle. Ref: EPA SW-846 Test Methods for Evaluating Solid
Waste, Physical/Chemical Methods; 3rd Edition, Method 3510 C. Rev. 3, December 1996,
Section 7.1.

Requirement: Add 60 mL of methylene chloride to the sample bottle, seal, and shake for 30
seconds to rinse the inner surface. Transfer the solvent to the separatory funnel and extract
the sample by shaking the funnel for two minutes with periodic venting to release excess
pressure. Ref: EPA Method 608.3, Section 10.2.3.

Requirement: Quantitatively transfer the sample from the graduated cylinder (or sample
bottle) to the separatory funnel. Use 60 mL of methylene chloride to rinse the cylinder (or
bottle) and transfer this rinse solvent to the separatory funnel. If the sample was transferred
directly from the sample bottle, refill the bottle to the mark made in Sec. 7.1 with water and
then measure the volume of sample that was in the bottle. Ref: EPA SW-846 Test Methods
for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 3510 C. Rev. 3,
December 1996, Section 7.4.

Comment: SOP and in-house practice is to pour samples into a 1-liter graduated cylinder and
then into the separatory funnel. The graduated cylinder is rinsed with methylene chloride but
the residue left in the original sample bottle is not being captured. The SOP and laboratory
practice must be revised to analyze the entire volume from the sample bottle, rinse the sample
bottle with methylene chloride, and eliminate the transfer of the sample to the graduated
cylinder.

Pesticides, Organochlorine – EPA Method 608.3, December 2016 (Aqueous)
Pesticides, Organochlorine – SW-846 8081 B (Aqueous & Non-Aqueous)

YYY. Finding: An inconsistency was noted between the SOP and laboratory practice as follows:
The laboratory extraction SOP requires an MS/MSD pair be prepared for Chlordane and
Toxaphene, but this is not being done.

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: The laboratory SOP (ORG-PRP006-03) for EPA 608.3 states in Section 7.2.2 to
prepare MS/MSD pairs for pesticides Toxaphene and Chlordane. This does not appear to be
a requirement of the analytical methods.

Comment: The laboratory SOP (ORG-GCS012-02) for EPA 608.3 states to analyze a
MS/MSD pair for Chlordane and Toxaphene at least once every two years. The laboratory
SOPs (ORG-GCS007-09 and ORG-GCS006-10) for SW-846 8081B lack the 2-year wording,
so it is understood that these be prepared with each analytical batch.

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Polychlorinated Biphenyls (PCBs) – SW-846 8082 A (Oil)

ZZZ. Finding: An inconsistency was noted between the SOP and laboratory practice as follows:
Section 10.1.3 of the laboratory SOP says to use Florisil column cleanup after sulfuric acid
cleanup but the Florisil column is not being used.

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: The title of the SOP (ORG-GCS010-01) is "ANALYSIS OF POLYCHLORINATED
BIPHENYLS (PCBs) IN OIL BY METHOD SW846-8082, WITH FLORISIL COLUMN
CLEANUP".

Purgeable, Organics – SW-846 8260 D (Aqueous & Non-Aqueous)

AAAA. Finding: The laboratory is not re-calculating all calibration points using the final calibration
curve.

Requirement: All calibration points, especially those equivalent to the LLOQ, should be
recalculated (not reanalyzed) using the final calibration curve in which this standard is used
(i.e., re-fitting the response from the calibration standard back into the curve). See Method
8000 for additional details. The recalculated concentration of the calibration standard
corresponding to the LLOQ, especially where linear regression fits are used, should be within
±50% of the standard's true concentration if it is the lowest point, and within ±30% for all others
(i.e. above the low standard). No refit criteria need be passed for calibration levels below the
LLOQ. Ref: EPA SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical
Methods; 3rd Edition, Method 8260 D. Rev. 4, June 2018, Section 11.3.5.4.

Requirement: The NC WW/GW Laboratory Certification Branch must confirm that analytical
data is valid by reviewing the QA/QC data generated during the sampling and analysis
procedures when implementing SW-846 methods in order to be assured that scientifically
sound decisions are made which will be protective of human health and the environment. 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 LCB SW-
846 Method Implementation Policy.

Comment: The analyst indicated that this had previously been routine practice but had been
discontinued at some point prior to the inspection.

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Purgeable, Organics – EPA 624.1, December 2016 (Aqueous)

BBBB. Finding: An inconsistency was noted between the SOP and laboratory practice as follows:
The laboratory is not evaluating all the parameter results for the BFB m/z Abundance Criteria.

Requirement: Each laboratory shall have a documented analytical quality assurance and
quality control program. Each laboratory shall have a copy of each approved test, analysis,
measurement, or monitoring procedure being used in the laboratory. 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. 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).

Comment: The laboratory is not documenting and evaluating the results of the m/z 50 and
m/z 75 abundance criteria. EPA Method 624.1, Table 4, Footnote 1 states: “Alternative tuning
criteria from other published EPA reference methods may be used, provided method
performance is not adversely affected.” The criteria used are those listed in SW-846 8260 D.
While this does not impact data quality, the SOP must document the criteria used.

CCCC. Finding: The laboratory is not always analyzing a reagent blank immediately after the LCS.

Requirement: Spike the internal standards and surrogates into the blank. Analyze the blank
immediately after analysis of the LCS (Section 8.4) and prior to analysis of the MS/MSD and
samples to demonstrate freedom from contamination. Ref: EPA Method 624.1, Section 8.5.1.

Comment: The laboratory sometimes analyzes a MS/MSD after the LCS but before the
reagent blank.

TPH Diesel Range, Organics – SW-846 8015 C (Aqueous & Non-Aqueous)

DDDD. Finding: The retention time check standard is not being properly evaluated.

Requirement: All target analytes, surrogates, and/or n-alkanes in the calibration verification
analyses need to fall within previously established retention time windows. If the retention time
of any analyte does not fall within the established window, then corrective action must be
taken to restore the system or a new calibration curve must be prepared for that compound.
Ref: EPA SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods;
3rd Edition, Method 8015 C. Rev 3, February 2007, Section 11.5.3.

Requirement: For the analysis of DRO, sum the area of all peaks eluting between C10 and
C28. This area is generated by projecting a horizontal baseline between the retention times
of C10 and C28. Ref: EPA SW-846 Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods; 3rd Edition, Method 8015 C. Rev 3, February 2007, Section
11.11.1.

Comment: Multiple instances were noted where the established retention time window did
not include the entire peak for Decane. After talking with the Semivolatiles Supervisor, it was
explained that during a previous audit, analysts were informed that the only requirement was
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that the mean retention time be at the apex of the peak. This led to some early portions of the
peak not being included in the area response.

EEEE. Finding: The retention time study is not performed over the correct time frame.

Requirement: Make three injections of all single component standard mixtures and multi-
component analytes (such as PCBs) over the course of a 72-hour period. Serial injections or
injections over a period of less than 72 hours may result in retention time windows that are
too tight. Ref: EPA SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical
Methods; 3rd Edition, Method 8000 D. Rev 6, March 2018, Section 11.6.1.

Comment: The analytical run on 6/21/21 lists current and past studies for the DRO retention
time. In 2020, injections were made over a 72-hour period (3/31-4/3). Later studies have been
performed on the same day in the same analytical batch.

FFFF. Finding: The retention time study is not being performed for the DRO surrogate, o-terphenyl
(OTP).

Requirement: Make three injections of all single component standard mixtures and multi-
component analytes (such as PCBs) over the course of a 72-hour period. Serial injections or
injections over a period of less than 72 hours may result in retention time windows that are
too tight. Ref: EPA SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical
Methods; 3rd Edition, Method 8000 D. Rev 6, March 2018, Section 11.6.1.

Comment: The laboratory includes OTP in the retention time check standard but is not
performing the study for OTP.

GGGG. Finding: The retention time window width is not properly evaluated.

Requirement: Width of the retention time window for each analyte, surrogate and major
constituent in multi-component analytes is defined as ± 3 times the standard deviation of the
mean absolute retention time established during the 72-hour period or 0.03 minutes,
whichever is greater. Ref: EPA SW-846 Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods; 3rd Edition, Method 8000 D. Rev 6, March 2018, Section 11.6.4

Comment: The laboratory is currently using 3 times the standard deviation, which is often
less than the 0.03 minute requirement. Too narrow a retention time window may result in low
bias for early and late eluting components.

Extractable Petroleum Hydrocarbons – MADEP, December 2019, Rev. 2.1 (Aqueous & Non-
Aqueous)

Comment: The laboratory analyzes samples utilizing dual autosamplers, columns and detectors.
Each autosampler, column, detector and calibration curve is specific to a particular hydrocarbon
fraction. The next revision of the method SOP needs to include this information.

Recommendation: The laboratory is performing multiple CCV analyses from the same vial, rather
than using fresh aliquots from non-punctured vials. This can cause bias due to loss of solvent and/or
more volatile compounds. It is recommended that fresh aliquots be used to avoid potential QC failures.

HHHH. Finding: The laboratory is not consistently preparing a Laboratory Control Standard Duplicate
(LCSD) with each batch.

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Requirement: At a minimum, for each extraction batch (up to 20 samples of similar matrix),
an LMB, LCS and an LCS Duplicate must also be prepared and results analyzed as part of
the laboratory’s continuing QC program. Ref: MADEP, Method for the Determination of
Extractable Petroleum Hydrocarbons (EPH), December 2019, Rev. 2.1, Section 10.1.3.2.

Comment: The laboratory is preparing and analyzing an MS/MSD pair as part of the routine
QC. These are optional QC elements for this parameter.

IIII. Finding: Samples are not being spiked with the recommended surrogates at the correct
concentration during extraction.

Requirement: Prepare a surrogate spiking solution which contains the surrogate standards
at a concentration of 40 ng/µL in acetone or methanol. Each sample, LMB, LCS, and matrix
spike is fortified with a specified volume of the surrogate spiking solution in order to yield a
final concentration of 40 µg/mL (on column, prior to correction for preparation factors). The
use of higher concentrations is permissible and advisable when spiking highly contaminated
samples. Ref: MADEP, Method for the Determination of Extractable Petroleum Hydrocarbons
(EPH), December 2019, Rev. 2.1, Section 7.5.5.

Comment: The laboratory is currently fortifying samples and extracted QC samples with the
surrogate solution at a final concentration of 20 µg/mL (on column, prior to correction for
preparation factors).

JJJJ. Finding: The laboratory is not analyzing a Continuing Calibration Standard (called CCV by
the laboratory) for the breakthrough compounds at the proper frequency.

Requirement: At a minimum, for each analytical batch (up to 20 samples) or every 24 hours,
whichever comes first, a beginning and ending Continuing Calibration Standard must be
analyzed. Ref: MADEP, Method for the Determination of Extractable Petroleum Hydrocarbons
(EPH), December 2019, Rev. 2.1, Section 10.1.3.1.

Comment: The laboratory is only analyzing a CCV for naphthalene and 2-methylnaphthalene
at the beginning of the analytical run.

KKKK. Finding: The laboratory is not properly preparing and evaluating the fractionation efficiency
of each lot of silica gel cartridges.

Requirement: For each analyte included in the Fractionation Check Solution (FCS),
excluding n-nonane, the mean percent recovery for four (4) replicate samples, expressed as
a percentage of the true value, must be between 40 and 140%. Lower recoveries are
permissible for n-nonane. If recovery of n-nonane is < 30%, the source of the problem should
be found and the fractionation check repeated. Ref: MADEP, Method for the Determination of
Extractable Petroleum Hydrocarbons (EPH), December 2019, Rev. 2.1, Appendix 5, Section
5.2.

Comment: Current laboratory practice is to prepare a single silica gel cartridge with the FCS
and proceed with the fractionation process. The extract is then analyzed. The hydrocarbon
ranges and breakthrough compounds are then evaluated, but the individual hydrocarbons are
not evaluated. Insufficient hexane volumes will cause low bias in the aliphatic fraction, while
excess hexane will cause breakthrough of the aromatic compounds into the aliphatic fraction.

Comment: It will be necessary to include each hydrocarbon analyte in the calibration curve
for the associated hydrocarbon range in order to properly evaluate the fractionation efficiency.
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The laboratory may include naphthalene and 2-methylnaphthalene in the aliphatic curve
rather than establishing a separate calibration curve for those analytes.

LLLL. Finding: Surrogate compounds are not always integrated properly.

Requirement: In samples, collective peak area integration for the hydrocarbon ranges, or
TPH, must be from baseline (i.e., must include the unresolved complex mixture “hump” areas).
For the integration of individual Target PAH analytes, surrogate compounds, and internal
standards, a valley-to-valley approach should typically be used, though this approach may be
modified on a case-by-case basis by an experienced analyst. In any case, the unresolved
complex mixture “hump” areas must not be included in the integration of individual Target PAH
Analytes, surrogate compounds, and internal standards. Ref: MADEP, Method for the
Determination of Extractable Petroleum Hydrocarbons (EPH), December 2019, Rev. 2.1,
Section 9.8.6.

Comment: Current laboratory practice is to integrate surrogate compounds by projecting a
baseline horizontally from the first valley to the end of the peak. With samples that have high
concentrations due to the unresolved complex mixture areas, this practice includes area under
the peak that is not part of the actual surrogate peak. Manually integrating the surrogate peaks
from valley to valley will ensure that surrogate recovery will not be improperly biased high due
to the matrix of the sample.

Volatile Petroleum Hydrocarbons – MADEP, Feb 2018, Rev. 2.1 (Aqueous & Non-Aqueous)

MMMM. Finding: The laboratory analyzes and evaluates four (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 µg/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.

NNNN. Finding: The laboratory is not within the acceptance criteria for some of the hydrocarbon
range retention time (RT) window markers.

Requirement: The RT window of the C5-C8 aliphatic hydrocarbons is defined as beginning
0.1 minutes before the elution of n-pentane and ending 0.01 minutes before the elution of
nonane. The C9-C12 aliphatic hydrocarbon range begins 0.01 minutes before the elution of
nonane; therefore there is no overlap of the two ranges and the nonane peak is only included
in the C9-C12 aliphatic hydrocarbon range. The C9-C12 aliphatic hydrocarbon range ends
0.1 minutes before the elution of naphthalene. The Rt window for the C9-C10 aromatic
hydrocarbons is defined as beginning 0.1 minutes after the elution of o-xylene and ending 0.1
before the elution of naphthalene. Ref: MADEP, Method for the Determination of Volatile
Petroleum Hydrocarbons (VPH), February 2018, Rev. 2.1, Section 9.3.6.

Comment: One of the recent chromatograms examined during the inspection had the C5 -
C8 Aliphatic RT marker greater than 0.01 minutes before the n-Nonane peak. Also, the RT
marker for the end of the C9 - C10 Aromatic range was greater than 0.1 minutes from the
Naphthalene peak.

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IV. PAPER TRAIL INVESTIGATION:

The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks, etc.),
chain of custodies and client reports. Representative data and associated client reports were submitted
prior to the inspection for all parameters analyzed during the months of July, September and November
2021. No transcription errors were observed. The facility appears to be doing a good job of accurately
transcribing data.

V. CONCLUSIONS:

We are concerned with the Findings that were cited previously and not corrected. 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: April 14, 2022
Report reviewed by: Jill Puff Date: April 18, 2022

Certificate Number:402
Effective Date:1/1/2022
Expiration Date:12/31/2022
Lab Name:Waypoint Analytical - Charlotte
Address:449 Springbrook Road
Charlotte, NC 28217
North Carolina Wastewater/Groundwater Laboratory Certification
Certified Parameters Listing
Date of Last Amendment:2/2/2022
The above named laboratory, having duly met the requirements of 15A NCAC 2H.0800, is hereby certified for the measurement of the parameters listed below.
CERTIFIED PARAMETERS
INORGANIC
ACIDITY
SM 2310 B-2011(Aqueous)
ALKALINITY
SM 2320 B-2011 (Aqueous)
BACTERIA - COLIFORM FECAL
IDEXX Colilert ®18 (MPN) (Aqueous)
SM 9221 E-2014 (MPN) (Aqueous)
SM 9221 E-2014 (MPN) (Biosolids)
SM 9222 D-2015 (MF) (Aqueous)
SM 9222 D-2015 (MF) (Biosolids)
BACTERIA - E. coli
IDEXX Colilert® (24 hr) (MPN) (Aqueous)
IDEXX Colilert-18® (MPN) (Aqueous)
BOD
SM 5210 B-2016 (Aqueous)
BROMIDE
EPA 300.0, Rev. 2.1, 1993 (Aqueous)
CBOD
SM 5210 B-2016 (Aqueous)
CHLORIDE
EPA 300.0, Rev. 2.1, 1993 (Aqueous)
EPA 300.0, Rev. 2.1, 1993 (Non-Aqueous)
SW-846 9056 A (Aqueous)
SW-846 9056 A (Non-Aqueous)
CHLORINE, TOTAL RESIDUAL
SM 4500 Cl G-2011 (Aqueous)
COD
SM 5220 D-2011 (Aqueous)
Hach 8000 (Aqueous)
COLOR, PC
SM 2120 B-2011 (PtCo) (Aqueous)
CONDUCTIVITY
EPA 120.1, Rev. 1982 (Aqueous)
SM 2510 B-2011 (Aqueous)
SW-846 9050 A (Aqueous)
CYANIDE
SW-846 9014 (Total) (Colorimetric) (Aqueous)
SW-846 9014 (Total) (Colorimetric) (Non-Aqueous)
SM 4500 CNˉ E-2016 (Total) (Aqueous)
DISSOLVED OXYGEN
Hach 10360-2011, Rev. 1.2 (Aqueous)
SM 4500 O G-2016 (Aqueous)
FLUORIDE
EPA 300.0, Rev. 2.1, 1993 (Aqueous)
EPA 300.0, Rev. 2.1, 1993 (Non-Aqueous)
SW-846 9056 A (Aqueous)
SW-846 9056 A (Non-Aqueous)
HARDNESS TOTAL - METALS
SM 2340 B-2011 (Ca EPA 200.7, Rev. 4.4, 1994 + Mg EPA 200.7, Rev. 4.4, 1994) (Aqueous)
HARDNESS TOTAL - WET CHEM
SM 2340 C-2011 (Aqueous)
IGNITABILITY
SW-846 1030 (Non-Aqueous)
INORGANIC PHENOLS
EPA 420.1, Rev. 1978 (Aqueous)
SW-846 9065 (Aqueous)
MBAS
SM 5540 C-2011 (Aqueous)
NITROGEN, AMMONIA
SM 4500 NH3 G-2011 (Aqueous)
SM 4500 NH3 D-2011 (Aqueous)
SM 4500 NH3 C-2011 (Aqueous)
SM 4500 NH3 C-2011 (Non-Aqueous)
NITROGEN, NITRATE
(NO3 + NO2 EPA 353.2, Rev. 2.0, 1993) - (NO2 SM 4500-NO2ˉ B-2011) (Aqueous)
EPA 300.0, Rev. 2.1, 1993 (Aqueous)
EPA 300.0, Rev. 2.1, 1993 (Non-Aqueous)
This certification requires maintance of an acceptable quality assurance program, use of approved methodology, and satisfactory performance on evaluation samples. Laboratories are subject to civil penalties and/or decertification for infractions
as set forth in 15A NCAC 2H.0807.
Certificate Number:402
Effective Date:1/1/2022
Expiration Date:12/31/2022
Lab Name:Waypoint Analytical - Charlotte
Address:449 Springbrook Road
Charlotte, NC 28217
North Carolina Wastewater/Groundwater Laboratory Certification
Certified Parameters Listing
Date of Last Amendment:2/2/2022
The above named laboratory, having duly met the requirements of 15A NCAC 2H.0800, is hereby certified for the measurement of the parameters listed below.
CERTIFIED PARAMETERS
SW-846 9056 A (Aqueous)
SW-846 9056 A (Non-Aqueous)
NITROGEN, NITRITE
SM 4500-NO2ˉ B-2011 (Automated) (Aqueous)
EPA 300.0, Rev. 2.1, 1993 (Aqueous)
EPA 300.0, Rev. 2.1, 1993 (Non-Aqueous)
SW-846 9056 A (Aqueous)
SW-846 9056 A (Non-Aqueous)
NITROGEN, NO3 + NO2
SM 4500 NO3ˉ F-2016 (Aqueous)
EPA 353.2, Rev. 2.0, 1993 (Aqueous)
EPA 300.0, Rev. 2.1, 1993 (Aqueous)
EPA 300.0, Rev. 2.1, 1993 (Non-Aqueous)
SW-846 9056 A (Aqueous)
SW-846 9056 A (Non-Aqueous)
NITROGEN, TOTAL KJELDAHL
EPA 351.2, Rev. 2.0, 1993 (Aqueous)
OIL & GREASE
EPA 1664 Rev. B (Aqueous)
SW-846 9071 B (Non-Aqueous)
PAINT FILTER LIQUIDS
SW-846 9095B
pH
SM 4500 H+B-2011 (Aqueous)
SW-846 9040 C (Aqueous)
SW-846 9045 D (Non-Aqueous)
PHOSPHATE, ORTHO
SM 4500 P E-2011 (Aqueous)
PHOSPHORUS, TOTAL
SM 4500 P F-2011 (Aqueous)
SM 4500 P E-2011 (Aqueous)
EPA 365.1, Rev. 2.0, 1993 (Aqueous)
RESIDUE, DISSOLVED 180 C
SM 2540 C-2015 (Aqueous)
RESIDUE, SETTLEABLE
SM 2540 F-2015 (Aqueous)
RESIDUE, SUSPENDED
SM 2540 D-2015 (Aqueous)
RESIDUE, TOTAL
SM 2540 B-2015 (Aqueous)
SILICA - METALS
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SULFATE
EPA 300.0, Rev. 2.1, 1993 (Aqueous)
EPA 300.0, Rev. 2.1, 1993 (Non-Aqueous)
SW-846 9056 A (Aqueous)
SW-846 9056 A (Non-Aqueous)
SULFIDE
SM 4500 S²ˉ F-2011 (Aqueous)
TEMPERATURE
SM 2550 B-2010 (Aqueous)
TURBIDITY
EPA 180.1, Rev. 2.0, 1993 (Aqueous)
SM 2130 B-2011 (Aqueous)
METAL
ALUMINUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
ANTIMONY
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
This certification requires maintance of an acceptable quality assurance program, use of approved methodology, and satisfactory performance on evaluation samples. Laboratories are subject to civil penalties and/or decertification for infractions
as set forth in 15A NCAC 2H.0807.
Certificate Number:402
Effective Date:1/1/2022
Expiration Date:12/31/2022
Lab Name:Waypoint Analytical - Charlotte
Address:449 Springbrook Road
Charlotte, NC 28217
North Carolina Wastewater/Groundwater Laboratory Certification
Certified Parameters Listing
Date of Last Amendment:2/2/2022
The above named laboratory, having duly met the requirements of 15A NCAC 2H.0800, is hereby certified for the measurement of the parameters listed below.
CERTIFIED PARAMETERS
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
ARSENIC
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
BARIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
BERYLLIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
BORON
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
CADMIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
CALCIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
CHROMIUM HEXAVALENT
SM 3500-Cr-B-2011 (Aqueous)
SW-846 7196 A (Aqueous)
SW-846 7196 A (Non-Aqueous)
CHROMIUM TOTAL
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
COBALT
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
COPPER
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
IRON
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
This certification requires maintance of an acceptable quality assurance program, use of approved methodology, and satisfactory performance on evaluation samples. Laboratories are subject to civil penalties and/or decertification for infractions
as set forth in 15A NCAC 2H.0807.
Certificate Number:402
Effective Date:1/1/2022
Expiration Date:12/31/2022
Lab Name:Waypoint Analytical - Charlotte
Address:449 Springbrook Road
Charlotte, NC 28217
North Carolina Wastewater/Groundwater Laboratory Certification
Certified Parameters Listing
Date of Last Amendment:2/2/2022
The above named laboratory, having duly met the requirements of 15A NCAC 2H.0800, is hereby certified for the measurement of the parameters listed below.
CERTIFIED PARAMETERS
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
LEAD
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
MAGNESIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
MANGANESE
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
MERCURY
EPA 245.1, Rev. 3.0, 1994 (Aqueous)
SW-846 7470 A (Aqueous)
SW-846 7470 A (Non-Aqueous)
SW-846 7471 B (Non-Aqueous)
MOLYBDENUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
NICKEL
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
POTASSIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
SELENIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
SILVER
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
SODIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
This certification requires maintance of an acceptable quality assurance program, use of approved methodology, and satisfactory performance on evaluation samples. Laboratories are subject to civil penalties and/or decertification for infractions
as set forth in 15A NCAC 2H.0807.
Certificate Number:402
Effective Date:1/1/2022
Expiration Date:12/31/2022
Lab Name:Waypoint Analytical - Charlotte
Address:449 Springbrook Road
Charlotte, NC 28217
North Carolina Wastewater/Groundwater Laboratory Certification
Certified Parameters Listing
Date of Last Amendment:2/2/2022
The above named laboratory, having duly met the requirements of 15A NCAC 2H.0800, is hereby certified for the measurement of the parameters listed below.
CERTIFIED PARAMETERS
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
STRONTIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
THALLIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
TIN
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
TITANIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
VANADIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
ZINC
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SW-846 6020 B (Non-Aqueous)
ORGANIC
1,2, DIBROMOETHANE (EDB)
SW-846 8011 (Includes DBCP) (Aqueous)
BASE NEUTRAL/ACID, ORGANICS
EPA 625.1 (Aqueous)
SW-846 8270 E (Aqueous)
SW-846 8270 E (Non-Aqueous)
EXTRACTABLE PETROLEUM HYDROCARBONS
MADEP, December 2019, Rev. 2.1 (Aqueous)
MADEP, December 2019, Rev. 2.1 (Non-Aqueous)
NONHALOGENATED VOLATILE, ORGANICS
SW-846 8015 C (Aqueous)
SW-846 8015 C (Non-Aqueous)
PESTICIDES, ORGANOCHLORINE
EPA 608.3 (Aqueous)
SW-846 8081 B (Aqueous)
SW-846 8081 B (Non-Aqueous)
POLYCHLORINATED BIPHENYLS (PCBs)
EPA 608.3 (Aqueous)
SW-846 8082 A (Aqueous)
SW-846 8082 A (Non-Aqueous)
SW-846 8082 A (Oil)
This certification requires maintance of an acceptable quality assurance program, use of approved methodology, and satisfactory performance on evaluation samples. Laboratories are subject to civil penalties and/or decertification for infractions
as set forth in 15A NCAC 2H.0807.
Certificate Number:402
Effective Date:1/1/2022
Expiration Date:12/31/2022
Lab Name:Waypoint Analytical - Charlotte
Address:449 Springbrook Road
Charlotte, NC 28217
North Carolina Wastewater/Groundwater Laboratory Certification
Certified Parameters Listing
Date of Last Amendment:2/2/2022
The above named laboratory, having duly met the requirements of 15A NCAC 2H.0800, is hereby certified for the measurement of the parameters listed below.
CERTIFIED PARAMETERS
PURGEABLE, ORGANICS
EPA 624.1 (Aqueous)
SM 6200 B-2011 (Aqueous)
SW-846 8260 D (Aqueous)
SW-846 8260 D (Non-Aqueous)
TPH DIESEL RANGE, ORGANICS
SW-846 8015 C (Aqueous)
SW-846 8015 C (Non-Aqueous)
TPH GASOLINE RANGE, ORGANICS
SW-846 8015 C (Aqueous)
SW-846 8015 C (Non-Aqueous)
VOLATILE PETROLEUM HYDROCARBONS
MADEP, Feb 2018, Rev. 2.1 (Aqueous)
MADEP, Feb 2018, Rev. 2.1 (Non-Aqueous)
This certification requires maintance of an acceptable quality assurance program, use of approved methodology, and satisfactory performance on evaluation samples. Laboratories are subject to civil penalties and/or decertification for infractions
as set forth in 15A NCAC 2H.0807.