#12_2022_0516_MC_Revised_10_31_FINAL

INSPECTION REPORT ROUTING SHEET

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

Laboratory Cert. #: 12
Laboratory Name: Pace Analytical Services, LLC – Huntersville, NC
Date Mailed:
Special Mailing Instructions:

On-Site Inspection Report

LABORATORY NAME: Pace Analytical Services, LLC – Huntersville, NC
ADDRESS: 9800 Kincey Avenue, Suite 100
Huntersville, NC 28078
CERTIFICATE #: 12
DATE OF INSPECTION: May 16, 2022 – May 17, 2022
TYPE OF INSPECTION: Commercial Maintenance
AUDITOR(S): Michael Cumbus, Tom Halvosa, Jill Puff

LOCAL PERSON(S) CONTACTED:

Ross Simmons, Steven Saenz, Gregory Wellman, Brandon
Johnson, Patrick Sim, Sarah Marlowe, James Lalonde, Greg
Willman, Catalina Londono, Michael Damte, Leyna Brown,
Kimberly Frank; Haleigh Hill

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 and well organized and has all the equipment necessary to perform the analyses. Staff
were very forthcoming and responded well to suggestions from the auditor . The Laboratory Information
Management System (LIMS) makes traceability of s amples, standards and reagents easily accessible.
Most data is stored electronically. Laboratory personnel were able to accommodate additional data
requests quickly.

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 a pply
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 appr oved 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 October 1, 2023.

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
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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 Pace Analytical Services, LLC – Asheville, NC (Certification #40),
Pace Analytical Services, LLC – Atlanta, Ga (Certification #381) and Pace National Center for Testing &
Innovation (Certification #375).

III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:

Documentation

A. Finding: The autoclave temperature, pressure and cycle time are not being documented.

Requirement: Each day samples are placed into or removed from an incubator, oven, water
bath, refrigerator, or other temperature-controlled device, the temperature shall be checked,
recorded, dated, and initialed. If a method requires more frequent monitoring, the method shall
be followed. During each use of an autoclave, the temperature, pressure, cycle time, and
items autoclaved shall be checked, recorded, dated, and initialed. Ref: 15A NCAC 02H .0805
(a) (7) (I).

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/in2 (≥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).

Comment: The autoclave pressure is not documented on the autoclave log. The start time
and time removed from the autoclave are recorded, but the time that the autoclave reaches
temperature and end time at that temperature are not documented. Overexposure to high
temperatures can lead to the breakdown of carbohydrates in media, so it is critical to remove
autoclaved media within the time limit and document that this is being done.

QA/QC

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
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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 following, which may not be all-inclusive, lists SOPs that were noted as having
not been reviewed or updated within the last two years at the time of the inspection.
• ENV-SOP-HUN1-0038
• ENV-SOP-HUN1-0039
• ENV-SOP-HUN1-0040
• ENV-SOP-HUN1-0015
• ENV-SOP-HUN1-0016
• ENV-SOP-HUN1-0021
• ENV-SOP-HUN1-0023
• ENV-SOP-HUN1-0033
• ENV-SOP-HUN1-0034

C. Finding: Chromatograms generated by the data reduction software are not always on an
appropriate scale.

Requirement: 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. Ref: NC
WW/GW LCB Manual Integration Policy.

Comment: The electronic copies of the chromatograms submitted for review were not always
on the appropriate scale. This was noted in both manually integrated chromatograms as well
as chromatograms generated by the data reduction software. While the PDF file allows the
user to zoom in, it does not allow the user to expand the scale to ensure that peaks are not
flat topped. The analysts were able to retrieve the original files readily using the analytical
software, but the client reports which require copies of the chromatograms lose this option.
The laboratory may wish to reexamine the scale of the chromatograms to allow users viewing
a PDF to better examine the data.

Reporting

D. Finding: The laboratory is analyzing and reporting results for Total Petroleum Hydrocarbons
(TPH) by improper methods.

Requirement: This method is not applicable to measurement of materials that volatilize at
temperatures below approximately 85°C. Petroleum fuels from gasoline through #2 fuel oil
may be partially lost in the solvent removal operation. Ref: EPA Method 1664, Rev. B,
Section 1.3.

Requirement: Method 9071 is not recommended for measuring materials that volatilize at
temperatures below 85°C. Petroleum fuels from gasoline through #2 fuel oil may be partially
lost during the solvent removal process. Ref: EPA SW-846 Test Methods for Evaluating
Solid Waste, Physical/Chemical Methods; 3rd Edition , Method 9071, Rev. B, Section 1.3.

Requirement: Some crude oils and heavy fuel oils may contain materials that are not soluble
in n-hexane, and recovery of these materials may be low. Ref: EPA SW-846 Test Methods
for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 9071, Rev. B,
Section 1.4.
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Requirement: Some crude oils and heavy fuel oils contain a significant percentage of
materials that are not soluble in n -hexane. Accordingly, recoveries of these materials may
be low. Ref: EPA Method 1664, Rev. B, Section 1.4.

Requirement: TPH is defined as the concentration of petroleum fuel contamination present
as carbon chains in the range of C6 through C35. TPH is a mixture of chemicals and they are
all composed mainly from hydrogen and carbon, called hydrocarbons. Some chemical
constituents of concern that may be found in TPH are benzene, ethylbenzene, toluene and
xylene. Ref: DEQ, UST Section “Guidelines for North Carolina Action Limits for Total
Petroleum Hydrocarbons” document, July 26, 2016.

Comment: The laboratory was analyzing and reporting TPH Oil & Grease by SW-846 9071B
and EPA 1664B at the client’s request. While the laboratory holds certification for Oil & Grease
by these methods, TPH is not a certifiable parameter by these methods. The Division of Waste
Management, UST section, stated in an email dated May 13, 2022 that they no longer accept
or require Oil & Grease, but instead use Extractable Petroleum Hydrocarbons (EPH) and
Volatile Petroleum Hydrocarbons (VPH). The laboratory must report all data generated by
EPA 1664, Rev. B, and SW-846 9071 B as Oil & Grease. The laboratory must also
communicate with clients the necessity of verifying that the requested analyses will meet the
needs of any applicable data receiver.

Comment: This Finding applies to Projects #92559526 analyzed September 10, 2021, and
#92569928 analyzed November 4, 2021. There may be more projects affected than the ones
listed above.

Comment: The laboratory needs to inform clients that TPH and Oil & Grease for NC
compliance purposes are two separate parameters that employ separate methods.

Bacteria, Coliform Fecal – Standard Methods, 9222 D-2015 (Aqueous)

E. Finding: The laboratory is using media prepared in-house past the expiration dates
established in the method.

Requirement: Prepare media in amounts that will be used within holding time limits given.
Ref. Standard Methods, 9020 B-2015. (5) (j) (4) Table 9020 V.

Comment: The LTB and EC media being prepared are stored in loose-cap tubes and kept
for 3 months. Table 9020 V lists the holding time for loose cap tubes as 2 weeks. Laboratory
prepared media stored in tightly-closed screw-cap tubes may be stored for up to 3 months.

Oil and Grease – SW-846 9071 B (Non-Aqueous)

F. Finding: The laboratory is not properly preparing the samples for analysis.

Requirement: Method 9071 may be used to quantify low concentrations of oil and grease
in soil, sediments, sludges, and other solid materials amenable to chemical drying and
solvent extraction with n-hexane. “Oil and grease” is a conventional pollutant under 40 CFR
401.16 and generally refers to substances, including biological lipids and mineral
hydrocarbons, that have similar physical characteristics and common solubility in an
organic extracting solvent. As such, oil and grease is an operationally defined parameter,
and the results will depend entirely on the extracting solvent and method of extraction.
Method 9071 employs n-hexane as the extraction solvent with Soxhlet extraction and the
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results of this method are appropriately termed “n -hexane extractable material (HEM).” Ref:
EPA SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd
Edition, Method 9071, Rev. B, Section 1.1.

Comment: The laboratory is preparing samples by microwave extraction. Samples have
been prepared utilizing this technique since prior to February 2015.

Base Neutral/Acid, Organics – SW-846 8270 E (Aqueous)

G. Finding: Some sample extracts are not properly protected from light.

Requirement: Store the sample extracts at ≤ 6°C (protected from light) in sealed vials (e.g.,
screw-cap vials or crimp-capped vials) equipped with unpierced PTFE -lined septa. Ref:
EPA SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd
Edition, Method 8270 E. Rev. 6, June 2018, Section 8.2.

Comment: It was noted during the inspection that some sample extracts that did not reduce
to 1 mL final volume were stored in 12.5 mL clear glass screw cap vials. Clear glass may
cause sample or analyte degradation from light sources. Wrapping clear glass vials in foil
or switching to amber vials would adequately protect extracts from light.

H. Finding: The laboratory is not properly determining the amount of sample used during
microextraction.

Requirement: Working with a single field or QC sample at a time, remove the cap from the
VOA vial, and use a disposable pipette to remove approximately 5 mL of water . Ref: EPA
SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition,
Method 3511. Rev. 1, July 2014, Section 11.5.

Requirement: After removing the 5 mL, weigh the capped VOA vial for each field and QC
sample. Record the weight to the nearest 0.1 grams. Ref: EPA SW-846 Test Methods for
Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 3511. Rev. 1, July
2014, Section 11.6.

Requirement: Reweigh the capped vial, and record the weight to the nearest 0.1 g. The
difference between this weight, and the weight determined in Sec. 11.6 is equal to the
volume of water extracted, in mL. Ref: EPA SW-846 Test Methods for Evaluating Solid
Waste, Physical/Chemical Methods; 3rd Edition, Method 3511. Rev. 1, July 2014, Section
11.13.

Comment: The laboratory is currently using a graduated cylinder to measure 40 mL of
reagent water into conical extraction vials. Personnel then compare filled extraction vials
to empty ones and use the meniscus on the filled vials as a guide to draw a line on empty
extraction vials. Empty vials are then filled with sample to the line drawn. This practice
introduces the potential for significant variation in volume used during sample preparation.

Extractable Petroleum Hydrocarbons – MADEP, Rev. 2.1 (Aqueous & Non-Aqueous)
TPH Diesel Range, Organics – SW-846 8015 C (Aqueous & Non-Aqueous)

I. Finding: The laboratory is not performing the Retention Time (RT) study over the correct time
period.

Requirement: Before establishing retention time (Rt) windows, optimize the GC system’s
operating conditions. Make three injections of the Aromatic Hydrocarbon and Aliphatic
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Hydrocarbon Standard mixtures over the course of a 72 -hr period. Serial injections over
less than a 72-hr period may result in Rt windows that are too restrictive . Ref: MADEP,
Method for the Determination of Extractable Petroleum Hydrocarbons (EPH), December
2019, Rev. 2.1, Section 9.6.1.

Requirement: Make three injections of all single component st andard 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. 5, March 2018, Section
11.6.1.

Comment: The laboratory sometimes performs the Retention Time study over a period of
24 hours rather than 72 hours as mentioned in the methods. SW-846 Method 8000D,
Section 11.6.4 allows a default of ±0.03 minutes to be used if the RT windows are too
restrictive, until further data is gathered. If the laboratory cannot perform the RT study over
the 72-hour time frame, then the default of ±0.03 minutes must be used until data from 3
injections over 72 hours has been acquired.

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

Comment: The laboratory is using acetone as an eluting solvent during the fractionation step, per
the manufacturer's instructions. The acetone is then solvent exchanged to methylene chloride and
concentrated prior to analysis. This is considered an allowable modification per Section 1.13 and
Section 11.3.1.1 of the method.

J. Finding: Samples are not consistently 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). Ref: MADEP, Method for the Determination of Extractable Petroleum Hydrocarbons
(EPH), December 2019, Rev. 2.1, Section 9.8.6.

Requirement: All data must be integrated consistently and appropriately in standards,
samples and quality control samples. It must be a laboratory’s routine operating procedure to
report automated peak integration results. Exceptions include situations where an obvious
error in the determination of the peak area has been made, when the analytical method has
specific integration requirements or when a regulatory program has specific integration
requirements. Ref: NC WW/GW LCB Manual Integration Policy.

Comment: Sample ID #92558719-003x20, analyzed September 13, 2021, was not
properly integrated for the second Aliphatic range. The integration was performed valley -
to-valley rather than projecting a baseline. Valley-to-Valley integration is required for
surrogates, Target PAHs (if analyzed), and the individual peaks comprising the calibration
standards.

K. Finding: The laboratory is not using a stopcock during fractionation.

Requirement: Hexane should be added in 1 -2 mL increments or dropwise using a pipet,
with additions occurring when the level of solvent drops to the point just prior to exposing
the column frit to air. The use of a stopcock is mandatory. Ref: MADEP, Method for the
Determination of Extractable Petroleum Hydrocarbons (EPH), December 2019, Rev. 2.1,
Section 9.2.3.3.

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Comment: During the inspection, the sample extraction staff expressed concern that the
stopcocks previously in use did not appear to provide consistent drip ra tes, and
discontinued their use. However, the use of a stopcock is mandatory to stop the flow of
eluent before exposing the frit to air, not control the drip rate of the eluent.

Purgeable, Organics – EPA 624.1, December 2016 (Aqueous)
Purgeable, Organics – SW-846 Method 8260 D (Aqueous & Non-Aqueous)
Purgeable, Organics – Standard Methods, 6200 B-2011 (Aqueous & Non-Aqueous)
TPH Gasoline Range, Organics - SW-846 8015 C (Aqueous & Non-Aqueous)

L. Finding: The laboratory is improperly preparing dilutions of matrix spike samples.

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.

Comment: Current laboratory practice is to dilute the source sample prior to addition of the
spiking solution.

M. Finding: The laboratory does not dilute and reanalyze matrix spike samples when they
measure over 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.

Comment: The laboratory removes the MS/MSD results from the analytical batch if the
original sample chosen for the MS/MSD was over the calibration range. The rest of the
acceptable sample results and QC in the batch are reported without the MS/MSD results
included. The original out of calibration range sample is then diluted and analyzed in the
next analytical batch but is not spiked.

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

N. Finding: Samples for analysis of 1,4-Dioxane are improperly preserved.

Requirement: Alcohols, ketones, ethers and other water-soluble compounds will have low
responses. Elevated sample equilibration temperatures may be necessary during
preparation. Elevated sample temperatures may be necessary during purges as heated
samples will exhibit better performance of these analytes. However, ethers such as diethyl
ether and MTBE hydrolyze more readily when heated in acid-preserved water. Acid
preservation is not recommended for analysis of these target analytes at elevated sample
temperature. Ref: EPA SW-846 Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods; 3rd Edition, Method 8260 D, June 2018, Section 1.3.3.

Requirement: 1,4-Dioxane is classified as an ether in EPA Method 624.1 and as such are
prone to hydrolysis at pH 2 when a heated purge is used. For this reason, volatile organic
compound (VOC) samples collected for 1,4 -Dioxane analysis are not to be acid-preserved.
Sodium thiosulfate is used to neutralize oxidizers such as total residual chlorine. Ref: NC
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DWR/WSS Sample Collection, Preservation, and Handling Instructions for Collecting
Aqueous Volatile Organic Compound Samples for 1,4 -Dioxane, November 14, 2017.

Comment: Samples are preserved with HCl to a pH of <2 S.U. then analyzed with a 90°C
heated purge.

O. Finding: The laboratory does not spike the LCS at the same concentrations as the MS .

Requirement: The LCS is spiked with the same analytes at the same concentrations as
the matrix spike, when appropriate. Ref: EPA SW-846 Test Methods for Evaluating Solid
Waste, Physical/Chemical Methods; 3rd Edition, Method 8260 D, June 2018, Section 9.6.2.

Comment: The laboratory spikes the LCS to a concentration twice that of the MS.

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

P. 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, December 2016, Section 8.5.1.

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

Purgeable, Organics – Standard Methods, 6200 B-2011 (Aqueous)

Q. Finding: The laboratory is not varying the concentration of their CCVs.

Requirement: Vary actual concentration of continuing calibration standard over calibration
range, with a minimum concentration greater than two times the reporting limit. Ref:
Standard Methods, 6200 A-2011. (5) (b) (2).

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

R. Finding: The laboratory is not defining the retention time (RT) window correctly for the C5-
C8 aliphatic hydrocarbon range.

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 C 9-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: The laboratory is incorrectly identifying the end of the C5 - C8 Aliphatic range
as the maxima of the n-Nonane peak. The end of the C5 - C8 Aliphatic range is defined by
the method as 0.01 minutes before the start of the n -Nonane.

IV. PAPER TRAIL INVESTIGATION:
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The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks, etc.) and
client reports. Data were reviewed for the following project numbers: #92551533, #92559064, #92557374,
#92557694, #92559526, #92569747, #92569860, #92570469, #92580295 and #92581514. No
transcription errors were observed. The facility appears to be doing a good job of accurately transcribing
data.

V. CONCLUSIONS:

Correcting the above-cited Findings 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: June 2, 2022
Report reviewed by: Tonja Springer Date: June 2, 2022