#5342_2022_1103_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

December 8, 2022

5342
Mr. Ross Simmons
Pace Analytical Services LLC - Field Services NC
9800 Kincey Avenue - Suite 100
Huntersville, NC 28078-

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

Dear Mr. Simmons:

Enclosed is a report for the inspection performed on November 3, 2022 by Michael Cumbus, Todd
Crawford, Beth Swanson, Tonja Springer, Tom Halvosa, Jason Smith and Jill Puff. 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
not 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: Michael Cumbus, Todd Crawford, #5342

On-Site Inspection Report

LABORATORY NAME: Pace Analytical Services LLC – Field Services NC

NPDES PERMIT #:
NC0006564, NC0020591, NC0020737, NC0021971,
NC0023868, NC0023876, NC0024333, NC0024911,
NC0025071, NC0025534, NC0026051, NC0029033,
NC0043532, NC0050342, NC0084662, NC1117264
WATER QUALITY PERMIT #: WQ0000579

ADDRESS: 9800 Kincey Avenue - Suite 100
Huntersville, NC 28078
CERTIFICATE #: 5342
DATE OF INSPECTION: November 3, 2022
TYPE OF INSPECTION: Field Commercial Maintenance

AUDITOR(S): Michael Cumbus, Todd Crawford, Beth Swanson, Tonja
Springer, Tom Halvosa, Jason Smith and Jill Puff

LOCAL PERSON(S) CONTACTED: Ross Simmons, Colley Frank, Taylor Dodds, Anthony Maiorana,
Jesse Allred, Samuel Warlick, Nick Ausburn and Harley Amos

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 forthcoming and responded well to suggestions from the auditors.

All required Proficiency Testing (PT) Samples have been analyzed for the 2022 PT Calendar Year and the
graded results were 100% acceptable. The laboratory has a large number of analysts and is doing a good
job of rotating the PT samples among the analysts from year to year.

Any time changes are made to laboratory procedures, Quality Assurance (QA)/Standard Operating
Procedure (SOP) documents 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 June 15, 2023.
Page 2
#5342 Pace Analytical Services LLC – Field Services NC

The laboratory is 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”.

Contracted analyses are performed by Pace Analytical Services LLC – Huntersville NC (Certification #12)
and Pace Analytical Services LLC – Asheville NC (Certification #40).

Approved Procedure documents for the analysis of the facility’s currently certified Field Parameters were
provided prior to 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 are 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 (g) (1).

B. Finding: The laboratory benchsheet is lacking required documentation: the method or SOP
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. Each item shall be recorded each time
samples are analyzed. Analyses shall conform to methodologies found in Subparagraph (a)(1)
of this Rule. Ref: 15A NCAC 02H .0805 (g) (2) (A) (C) and (L).

Comment: Some Temperature results for NPDES samples are recorded solely on the Chain
of Custody, rather than on the laboratory benchsheets. The Chain of Custody lacks the
necessary documentation requirements.

Comment: During the data review, one field notebook was discovered that documents the
daily calibration verification and instrument ID for both the Hach Pocket II and Hach DR1900
meters, however, there is no indication on the data which meter is used for the TRC and FAC
compliance samples that were analyzed. Additionally, the proper units of measure are not
documented on the daily calibration or end of day calibration check of the Hach Pocket II (i.e.,
documented as µg/L instead of mg/L).

C. Finding: The laboratory does not document the date of the most recent Total Residual
Chlorine (TRC) or Free Available Chlorine (FAC) calibration curve verification on the
benchsheets.

Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref:
15A NCAC 02H .0805 (g) (4).

Requirement: The following must be documented in indelible ink whenever sample analysis
is performed: Date of most recent calibration curve generation or calibration curve verification.
Ref: NC WW/GW LCB Approved Procedure for the Analysis of Total Residual Chlorine (DPD
Page 3
#5342 Pace Analytical Services LLC – Field Services NC

Colorimetric by SM 4500 Cl G-2011) and NC WW/GW LCB Approved Procedure for the
Analysis of Free Available Chlorine (DPD Colorimetric).

D. Finding: The laboratory does not document QC assessments.

Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data shall
be traceable to the associated sample analyses and shall consist of: the quality control
assessments. Each item shall be recorded each time samples are analyzed. Analyses shall
conform to methodologies found in Subparagraph (a)(1) of this Rule. Ref: 15A NCAC 02H
.0805 (g) (2) (O).

Comment: The laboratory is documenting the values of the QC checks, but the benchsheets
lack the acceptance criteria, as well as an evaluation that these criteria are being met. No data
were reviewed where the QC results were out of compliance.

E. Finding: The laboratory is not documenting all traceability information for purchased
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 Traceability Documentation Requirements for Chemicals, Reagents,
Standards and Consumables Policy.

Comment: The laboratory purchases bottles of Formazin at various concentrations for use
during the daily calibration of the turbidimeters. Aliquots of each standard are dispensed for
use by individual analysts. Several instances were noted where the Lot Number and
Expiration Date had not been updated on the individual analysts’ aliquots (stored in matching
sample cells) to reflect the lots currently in use. This can give the appearance of an analyst
using standards past their expiration date.

F. Finding: The laboratory is not documenting the default Salinity value of zero that is used to
calibrate the Dissolved Oxygen (DO) meters.

Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref:
15A NCAC 02H .0805 (g) (4).

Requirement: The following must be documented in indelible ink whenever sample analysis
is performed: Calibration variables (temperature, elevation or barometric pressure [in mmHg],
and salinity). Ref: NC WW/GW LCB Approved Procedure for the Analysis of Dissolved
Oxygen (DO).

Requirement: Per NC WW/GW LC Branch policy, facilities may use the Salinity default value
of zero when calibrating the DO meter unless it is known or suspected that the Salinity value
of the samples being analyzed is > 9 ppt. In those situations, actual Salinity values must be
Page 4
#5342 Pace Analytical Services LLC – Field Services NC

used. Regardless of which value is used, it must be documented. Ref: NC WW/GW LCB
Approved Procedure for the Analysis of Dissolved Oxygen (DO).

G. Finding: Some analytical results are not legible to all parties.

Requirement: All analytical records shall be legible to all parties and safeguarded against
unauthorized amendment, obliteration, erasures, overwriting and corruption. Ref: 15A NCAC
02H .0805 (g) (1).

Comment: The units of measure for TRC (Project #92627591), analyzed on September 20,
2022, were not legible. It is possible that these results were reported incorrectly due to the
illegible writing, because the reported units (mg/L) do not match the reporting limit units (µg/L).

Proficiency Testing

H. Finding: The laboratory is not documenting the preparation of PT Samples.

Requirement: PT Samples received as ampules are diluted according to the Accredited PT
Sample Provider’s instructions. It is important to remember to document the preparation of PT
Samples in a traceable log or other traceable format. The diluted PT Sample then becomes a
routine Compliance Sample and is added to a routine sample batch for analysis. No
documentation is needed for whole volume PT Samples which require no preparation,
however the instructions must be maintained. Ref: Proficiency Testing Requirements,
February 19, 2020, Revision 5, Section 3.6.

Comment: Dating and initialing the instruction sheet for each prepared PT Sample would
satisfy the documentation requirement.

I. Finding: The laboratory is not analyzing a PT Sample that corresponds with routine testing
of low-level compliance samples.

Requirement: For colorimetric procedures, TRC PT Samples must be analyzed on the same
spectrophotometric program using the same procedure that is used for routine Compliance
Sample analysis. There are two options for achieving this when you have a low-level permit
requirement:

1. If a facility having a low-level permit requirement analyzes a regular-level TRC PT Sample,
it must be diluted to the verified range of the low-level curve routinely used. The reported result
must then be calculated using the dilution factor and the TRC value obtained.

2. Since the dilution factor in option 1 may introduce error, it is recommended that facilities
having a low-level permit requirement order and analyze a low-level TRC PT Sample. This
PT Sample should be within the range of your verified curve on the low-level program.

Ref. NC WW/GW LCB Proficiency Testing Requirements, February 19, 2020, Rev. 5, Section
3.7.1.

Comment: The laboratory analyzes regular-level (i.e., mg/L) compliance samples with a Hach
Pocket II colorimeter and low-level (i.e., µg/L) compliance samples with a Hach DR1900. Only
a regular-level PT Sample is analyzed.

Recommendation: It is recommended that the laboratory purchase both low-level and
regular-level TRC PT Samples. Regular TRC PT Samples require additional dilution to bring
Page 5
#5342 Pace Analytical Services LLC – Field Services NC

the concentration within the verified range of the low-level (i.e. µg/L) calibration program on
the DR 1900. This additional dilution of regular-level PT Samples may introduce error.

J. Finding: PT Samples are not analyzed in the same manner as routine Compliance Samples.

Requirement: Laboratories are required to analyze an appropriate PT Sample by each
parameter method on the laboratory’s CPL. The same PT Sample may be analyzed by one
or more methods. Laboratories shall conduct the analyses in accordance with their routine
testing, calibration and reporting procedures, unless otherwise specified in the instructions
supplied by the Accredited PT Sample Provider. This means that they are to be logged in and
analyzed using the same staff, sample tracking systems, standard operating procedures
including the same equipment, reagents, calibration techniques, analytical methods,
preparatory techniques (e.g., digestions, distillations and extractions) and the same quality
control acceptance criteria. PT Samples shall not be analyzed with additional quality control.
They are not to be replicated beyond what is routine for Compliance Sample analysis.
Although, it may be routine to spike Compliance Samples, it is neither required, nor
recommended, for PT Samples. PT sample results from multiple analyses (when this is the
routine procedure) must be calculated in the same manner as routine Compliance Samples.
Ref: Proficiency Testing Requirements, February 19, 2020, Revision 5, Section 3.6.

Comment: The PT Samples for TRC are only analyzed on the Hach Pocket II colorimeter.
PT Samples must be analyzed using the same instruments that are used for compliance
testing (i.e. the Hach Pocket II colorimeter and the Hach DR1900 spectrometer). The Hach
Pocket II colorimeter is not acceptable for compliance monitoring at permitted sites which have
a daily maximum limit (i.e. in µg/L).

Reporting

K. Finding: The laboratory does not report all characteristics of the pollutants analyzed from
permitted locations.

Requirement: If the Permittee monitors any pollutant more frequently than required by this
permit using test procedures approved under 40 CFR Part 136 and at a sampling location
specified in this permit or other appropriate instrument governing the discharge, the results of
such monitoring shall be included in the calculation and reporting of the data submitted on the
DMR. Ref: Standard Conditions for NPDES Permits, Rev. 11/09/2011, Section (E) (5) (b).

Comment: The laboratory sometimes analyzes pH samples in duplicate but does not report
both values to the client. Duplicates are not a required QC element for Field Parameters.

Chlorine, Total Residual – Standard Methods, 4500 Cl G-2011 (Aqueous)
Chlorine, Free Available – Standard Methods, 4500 Cl G-2011 (Aqueous)

L. Finding: Values less than the established reporting limit are occasionally being reported.

Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref:
15A NCAC 02H .0805 (g) (4).

Requirement: For all calibration options, the range of standard concentrations must bracket
the permitted discharge limit concentration, the range of sample concentrations to be analyzed
and anticipated PT Sample concentrations. One of the standards must have a concentration
less than the permitted Daily Maximum Limit. The lower reporting limit concentration is equal
to the lowest standard concentration. Sample concentrations that are less than the lower
Page 6
#5342 Pace Analytical Services LLC – Field Services NC

reporting limit must be reported as a less-than value. Ref: NC WW/GW LCB Approved
Procedure for the Analysis of Total Residual Chlorine (DPD Colorimetric by SM 4500 Cl G-
2011) and NC WW/GW LCB Approved Procedure for the Analysis of Free Available Chlorine
(DPD Colorimetric).

Comment: The TRC reporting limit is 10 µg/L and the FAC reporting limit is 0.1 mg/L, based
on the lowest standard concentration analyzed in the most recent calibration curve
verifications. Results below those values for NPDES permit #NC0004774 (Buck Steam)
analyzed on September 20, 2022 were reported as 0 mg/L for TRC and 0.02 mg/L for FAC.

Chlorine, Total Residual – Standard Methods, 4500 Cl G-2011 (Aqueous)

Recommendation: The laboratory verifies the factory set calibration curve with standards of 10, 50,
100, 200 and 400 µg/L. It is recommended that the laboratory analyze a standard between the 10 and
50 µg/L (e.g., 25 µg/L) and eliminate the 100 µg/L standard.

Chlorine, Free Available – Standard Methods, 4500 Cl G-2011 (Aqueous)

M. Finding: The Annual Factory-set Calibration Curve Verification does not bracket the
concentration of the annual Proficiency Testing (PT) Samples.

Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref:
15A NCAC 02H .0805 (g) (4).

Requirement: For all calibration options, the range of standard concentrations must bracket
the permitted discharge limit concentration, the range of sample concentrations to be analyzed
and anticipated PT Sample concentrations. One of the standards must have a concentration
less than the permitted Daily Maximum Limit. The lower reporting limit concentration is Ref:
NC WW/GW LCB Approved Procedure for the Analysis of Free Available Chlorine (DPD
Colorimetric).

Comment: The standards analyzed for the annual factory-set calibration curve verification
performed on October 29, 2022 ranged in concentration from 0.1 mg/L to 0.5 mg/L and the
2022 PT Sample assigned value was 0.675 mg/L. The laboratory reported a value of 0.60
mg/L.

Conductivity – EPA 180.1, Rev. 1982 (Aqueous)
Conductivity – Standard Methods, 2510 B-2011 (Aqueous)

N. Finding: The laboratory is not analyzing a second-source calibration verification check
standard.

Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref:
15A NCAC 02H .0805 (g) (4).

Requirement: Analyze and document a second-source calibration verification check
standard prior to compliance sample analysis. It is recommended that this standard value
approximate (may be higher or lower than the calibration standard, as applicable) the
expected range of sample values measured. The value obtained for the calibration verification
check-standard must read within 10% of the true value of the calibration verification check
standard. If the obtained value is outside of the ±10% range, corrective action must be taken.
Ref: NC WW/GW LCB Approved Procedure for the Analysis of Specific Conductance
(Conductivity).
Page 7
#5342 Pace Analytical Services LLC – Field Services NC

Comment: The majority of the analysts calibrate with a 1000 NTU standard, then verify the
calibration by analyzing another aliquot of the 1000 NTU standard as well as analyzing a 100
NTU standard, which is acceptable. However, several analysts were calibrating their meters
with both standards, then verifying the calibration with those same standards. One analyst
noted that they did perform second-source verifications for South Carolina samples but not
North Carolina samples.

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

O. Finding: Some pH probes are not consistently stored in the recommended storage solution.

Requirement: The pH probe must be stored in the solution recommended by the probe
manufacturer between analyses. A solution with a conductivity greater than 4000 µhos/cm is
recommended. Tap water is a better substitute than distilled water, but pH 4 buffer is best for
the single glass electrode and saturated KCl is preferred for the calomel and Ag/AgCl
reference electrode. Saturated KCl is preferred for a combination electrode. Keep electrodes
wet by returning them to the storage solution whenever the pH meter is not in use. Ref:
Standard Methods, 4500-H+ B-2011. (4) (a).

Requirement: The cable assembly is supplied with a sensor storage container, or sleeve,
that attaches to the cable. The container is used for short-term storage (less than 30 days).
Be sure to keep a small amount of moisture (tap water) in the container during storage.
This is done to maintain a 100% saturated air environment which is ideal for short-term
sensor storage. The sensors should not be submersed in water. The intent is to create a
humid air storage environment. Ref: YSI Professional Plus User Manual, Rev. D, 2009, pg.
(66).

Requirement: To store the sensor, remove it from the cable and seal the vacant port with
a port plug. Fill the original shipping/storage vessel (plastic boot or bottle) with buffer 4
solution and then submerge the sensor into the solution. The sensor should remain
submerged in the solution during the storage period; therefore, make certain that the vessel
is sealed to prevent evaporation and periodically check the vessel to ensure the sensor
does not dry out. Ref: YSI Professional Plus User Manual, Rev. D, 2009, pg. (67).

Comment: During the audit, it was noted that one pH probe was stored dry, though the analyst
noted that this was not the normal procedure. Another analyst noted that their probe was
stored in a bag overnight and in pH 4 S.U. buffer for longer storage.

Turbidity – Standard Methods, 2130 B-2011 (Aqueous)

Comment: Several sample cells were observed to have a significant yellow color. However, no
scratches or markings that might scatter the light beam were observed.

IV. PAPER TRAIL INVESTIGATION:

The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks, etc.),
chain of custodies and contract laboratory reports. Data were reviewed for Project No. 92599960, Project
No. 92585905, Project No. 92622513 and Project No. 92622514. The following errors were noted.

Date

Parameter

Location Value on
Benchsheet
Value on
Client Report
Page 8
#5342 Pace Analytical Services LLC – Field Services NC

08/11/2022 Chlorine, Total
Residual1
Duke Energy –
Cliffside Outfall 005

< 10 µg/L

< 10 mg/L

08/25/2022 Chlorine, Total
Residual2
Duke Energy –
Cliffside Outfall 005

14 µg/L

14 mg/L

09/20/2022 Chlorine, Total
Residual3
Duke Energy –
Buck Outfall 001A

0 µg/L

0 mg/L

1. The laboratory benchsheet lists the date and time of analysis as 08/11/2022 at 11:07 am. The
client report lists the date and time of analysis as 08/25/2022 at 16:36.
2. The laboratory benchsheet lists the date and time of analysis as 08/25/2022 at 11:21 am. The
client report lists the date and time of analysis as 08/25/2022 at 16:31.
3. The reporting limit for TRC as determined by the calibration curve verification is 10 µg/L. See
Finding G about possible transcription error due to illegible documentation.

V. CONCLUSIONS:

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: November 28, 2022
Report reviewed by: Jason Smith Date: November 30, 2022

CERTIFIED PARAMETERS
North Carolina Wastewater/Groundwater Laboratory Certification
Certified Parameters Listing
Lab Name: Pace Analytical Services LLC - Field Services NC Certificate Number: 5342
Address: 9800 Kincey Avenue - Suite 100 Effective Date: 1/1/2022
Huntersville, NC 28078- Expiration Date: 12/31/2022
Date of Last Amendment: 9/28/2021

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.

INORGANIC
CHLORINE, FREE AVAILABLE
SM 4500 Cl G-2011 (Aqueous)
CHLORINE, TOTAL RESIDUAL
SM 4500 Cl G-2011 (Aqueous)
CONDUCTIVITY
EPA 120.1, Rev. 1982 (Aqueous)
SM 2510 B-2011 (Aqueous)
DISSOLVED OXYGEN
SM 4500 O G-2016 (Aqueous)
pH
SM 4500 H+B-2011 (Aqueous)
TEMPERATURE
SM 2550 B-2010 (Aqueous)
TURBIDITY
SM 2130 B-2011 (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.