#163_2016_1115_BS_FINAL

INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #:
163
Laboratory Name:
Wilkesboro Cub Creek WWTP Lab
Inspection Type:
Municipal Maintenance
Inspector Name(s):
Beth Swanson, Gary Francies, Dana Satterwhite and Jason Smith
Inspection Date:
November 15, 2016
Date Forwarded for Initial
Review:
January 13, 2017
Initial Review by:
Jason Smith
Date Initial Review
Completed:
January 13, 2017
Cover Letter to use:
❑ Insp. Initial ❑ Insp. Reg
❑Insp. No Finding ❑Insp. CP
❑Corrected
®Insp. Reg. Delay
Unit Supervisor/Chemist III:
Gary Francies
Date Received:
January 17, 2017
Date Forwarded to Admin.:
2/24/2017
Date Mailed:
2/24/2017
Special Mailing Instructions:
Copy George Smith, Katie Mills, Cyndi Karoly

Water Resources
ENV I RONMENT AL QU/1,L!T f
February 24, 2017
163
Ms. Kimberly Wiles
Wilkesboro Cub Creek WWTP Lab.
P.O. Box 1056
Wilkesboro, NC 28697
ROY COOPER
MICHEAL S. REGAN
S. JAY ZIMMERMAN
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Ms. Wiles:
Enclosed is a report for the inspection performed on November 15, 2016 by Beth Swanson, Dana
Satterwhite, Jason Smith and myself. I apologize for the delay in getting this report to you. Where
Finding(s) are cited in this report, a response is required. Within thirty days of receipt, please supply this
office with a written item for item description of how these Finding(s) were corrected. Please describe
the steps taken to prevent recurrence and include an implementation date for each corrective action. If
the Finding(s) cited in the enclosed report are not corrected, enforcement actions may be
recommended. For certification maintenance, your laboratory must continue to carry out the
requirements set forth in 15A NCAC 2H .0800.
A copy of the laboratory's Certified Parameter List at the time of the audit is attached. This list will reflect
any changes made during the audit. Copies of the checklists completed during the inspection may be
requested from this office. Thank you for your cooperation during the inspection. If you wish to obtain an
electronic copy of this report by email or if you have questions or need additional information, please
contact me at [phone].
Sincerely,
Gary Francies, Technical Assistance/Compliance Specialist
Division of Water Resources
Attachment
cc: master file
Beth Swanson
Water Sciences Section
NC Wastewater/Groundwater Laboratory Certification Branch
1623 Mail Service Center, Raleigh, North Carolina 27699-1623
Location: 4405 Reedy Creek Road, Raleigh, North Carolina 27607
Phone: [phone] FAX: [phone]
Internet: http:/Ideg.nc.gov/about/divisions/water-resources/water-resources•data/water-sciences-home-Pagellabo ratory-certification-branch

LABORATORY NAME:
NPDES PERMIT #:
ADDRESS:
CERTIFICATE #:
DATE OF INSPECTION:
TYPE OF INSPECTION:
AUDITOR(S):
LOCAL PERSON(S) CONTACTED:
I. INTRODUCTION:
Wilkesboro Cub Creek WWTP Lab
NC0021717
700 Snyder St.
Wilkesboro, NC 28697
163
November 15, 2016
Municipal Maintenance
Beth Swanson, Dana Satterwhite, Gary
Francies and Jason Smith
Kimberly Wiles
This laboratory was inspected by representatives of the North Carolina Wastewater/Groundwater
Laboratory Certification (NC WW/GW LC) program to verify its compliance with the requirements
of 15A NCAC 2H .0800 for the analysis of environmental samples.
II. GENERAL COMMENTS:
The laboratory is neat and clean with ample and organized space. The benchsheets and logs are
structured in ways that are easy to follow. The staff were forthcoming, answered questions in an
honest manner and were receptive to changes discussed as requirements or recommendations.
The inspection was performed at the request of the Division of Water Resources Winston-Salem
Regional Office.
All required Proficiency Testing (PT) samples have been analyzed and the laboratory has fulfilled
its PT requirements for the 2016 PT calendar year.
The laboratory submitted their Quality Assurance (QA) and/or Standard Operating Procedures
(SOP) document(s) in advance of the inspection. These documents were reviewed and editorial
and substantive revision requirements and recommendations were made by this program
outside of this formal report process. Although subsequent revisions were not requested to be
submitted, they must be completed by November 15, 2017.
The laboratory is reminded that any time changes are made to laboratory procedures, the
laboratory must update the QA/SOP document(s) and inform relevant staff. Any changes made
in response to the pre -audit review or to Findings, Recommendations or Comments listed in this
report must be incorporated to insure the method is being performed as stated, references to
methods are accurate, and the QA and/or SOP 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.

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The laboratory is also reminded that SOPs are intended to describe procedures exactly as they
are to be performed. Use of the word "should" is not appropriate when describing requirements
(e.g. Quality Control (QC) frequency, acceptance criteria, etc.). Evaluate all SOPs for the proper
use of the word "should".
Laboratory Fortified Matrix (LFM) and Laboratory Fortified Matrix Duplicate (LFMD) are also
known as Matrix Spike (MS) and Matrix Spike Duplicate (MSD) and may be used
interchangeably in this report.
Requirements that reference 15A NCAC 2H .0805 (a) (7) (A), stating "All analytical data
pertinent to each certified analysis must be filed in an orderly manner so as to be readily
available for inspection upon request", are intended to be a requirement to document
information pertinent to reconstructing final results and demonstrating method compliance. Use
of this requirement is not intended to imply that existing records are not adequately maintained
unless the Finding speaks directly to that.
Contracted analyses are performed by Meritech, Inc. (Certification # 165).
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
Documentation
Recommendation: It is recommended that a reference log be maintained which includes all
analyst's and operator's printed names and the initials and/or signature recorded on any
supporting records that fall under the scope of 15A NCAC .0800.
Recommendation: It is recommended that the laboratory document any sample condition
anomalies (e.g., unusual color, multiple phases present, container has more or less sample than
usual, etc.) that are observed upon receipt in the laboratory.
Comment: Error corrections were not always properly performed. Instances were found of
overwriting and corrections that were not initialed and/or dated. The incorrect error corrections did
not have concerning trends (i.e., they did not change results from non-compliance to compliance).
NC WW/GW LC Policy states: All documentation errors must 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. Write the correction adjacent to the error. The correction must be initialed
by the responsible individual and the date of change documented. Notification of acceptable
corrective action (i.e., a statement that the proper procedure for error correction was reviewed and
implemented by December 1, 2016 and 4 signs reading "Error Corrections: To correct an error,
draw 1 single straight line through it and write correction, then initial. Also include date." were
placed in areas where benchsheets are used on December 13, 2016) was received by email on
December 2 and 13, 2016. No further response is necessary for this Finding.
A. Finding: Some traceability documentation is lacking for purchased materials and
reagents, as well as documentation of standards and reagents prepared in the laboratory.
Requirement: All chemicals, reagents, standards and consumables used by the
laboratory must have the following information documented: Date received, Date Opened
(in use), Vendor, Lot Number, and Expiration Date (where specified): A system (e.g.,
traceable identifiers) must be in place that links standard/reagent preparation information
to analytical batches in which the solutions are used. Documentation of solution
preparation must include the analyst's initials, date of preparation, the volume or weight of

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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 LC
Policy.
Comment: The laboratory has a well -designed log in place for documenting purchased
materials and preparation of reagents and standards, however, there were a few items
missing:
® The log was not always updated to include the date opened and received.
(Corrected December 6, 2016)
® pH buffers currently in use were not entered into the log at all. (Corrected
December 6, 2016)
® Aliquots of the pH buffers were placed into separate containers that did not contain
the lot number for traceability. (Corrected December 6, 2016)
® The working standards and spike preparation for Ammonia Nitrogen analyses were
not documented.
B. Finding: The composite sampler temperature log does not include units of measure for
temperature.
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15A
NCAC 2H .0805 (a) (7) (A).
Quality Control
Recommendation: North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (0) requires
that thermometers be checked, at a minimum, annually against a NIST traceable thermometer;
however, it is recommended that digital type thermometers be calibrated more frequently (i.e.,
quarterly).
Comment: The laboratory is reminded that digital probes have manufacturer specified immersion
depths. Refer to the manufacturer's instructions to ensure these thermometers are immersed
appropriately.
Comment: QC results were not consistently evaluated and/or documented to demonstrate the
analytical process is in control and the established acceptance criteria are met. The Relative
Percent Difference (RPD) for Fecal Coliform sample duplicates was not documented on the
benchsheets. Ammonia standard recoveries, RPDs and MS/MSD recoveries were not consistently
calculated and documented. The analyst would evaluate visually whether the QC results appeared
to be within limits and only calculate and document the RPD and/or percent recovery if it appeared
they were close to the control limits. North Carolina Administrative Code, 15A NCAC 2H .0805 (a)
(7) states: Each laboratory shall develop and maintain a document outlining the analytical quality
control practices used for the parameters included in their certification. Supporting records shall
be maintained as evidence that these practices are being effectively carried out. North Carolina
Administrative Code, 15A NCAC 2H .0805 (a) (7) (F) states: Any time quality control results
indicate an analytical problem, the problem must be resolved and any samples involved must be
rerun if the holding time has not expired. Notification of acceptable corrective action (i.e.,
submission of Fecal Coliform and Ammonia benchsheets showing all QC results calculated and a
statement that as of November 15, 2016, the analysts will be diligent about calculating and

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documenting the results of all QC evaluations) was received by email on December 6, 2016 and
fax December 13, 2016. No further response is necessary for this Finding.
Comment: The laboratory's NIST reference thermometer calibration had expired. The calibration
was due in February 2016 and had been used for thermometer verifications after that date. NC
WW/GW LC Policy states: NIST traceable thermometers used for temperature measurement
must be recalibrated in accordance with the manufacturer's recalibration date. Notification of
acceptable corrective action (i.e., documentation that the thermometer had been recalibrated on
November 21, 2016 and a statement that the laboratory would request a separate thermometer to
be kept only in the laboratory so the expiration date could be more closely monitored) was
received by email on December 6, 2016 and fax on December 7, 2016. No further response is
necessary for this Finding.
C. Finding: The laboratory has not checked all thermometers or temperature measuring
devices against an NIST traceable thermometer.
Requirement: All thermometers must meet National Institute of Standards and
Technology (NIST) specifications for accuracy or be checked, at a minimum annually,
against a NIST traceable thermometer and proper corrections made. Ref: 15A NCAC 2H
.0805 (a) (7) (0).
Requirement: Any temperature measuring device, used to measure temperature for
compliance monitoring, must be verified against a National Institute of Standards and
Technology (NIST) traceable temperature measuring device prior to initial use and re -
verified at least every 12 months and any time the instrument is serviced. Ref: NC
WW/GW LC Approved Procedure for the Analysis of Temperature.
Requirement: All thermometers and temperature measuring devices must be checked
every 12 months against an NIST certified or NIST traceable thermometer and the
process documented. Ref: NC WW/GW LC Policy.
Comment: The composite sampler thermometer and Dissolved Oxygen (DO) meter
temperature sensor used to report Temperature have not been verified.
D. Finding: The laboratory is not verifying all thermometers at their temperature of use.
Requirement: The verification must be performed at a temperature that corresponds to
the temperature used by the incubator, refrigerator, freezer, etc. Ref: NC WW/GW LC
Policy.
Comment: Laboratory thermometers are currently verified at three temperatures (i.e.,
44.5 °C, ice water, and room temperature). The temperature of use for the residue oven is
approximately 104 °C, which is not included in that range. This program only requires a
thermometer to be verified at its temperature of use.
E. Finding: The laboratory is not consistently checking in use thermometers every 12
months.
Requirement: All thermometers must meet National Institute of Standards and
Technology (NIST) specifications for accuracy or be checked, at a minimum annually,
against a NIST traceable thermometer and proper corrections made. Ref: 15A NCAC 2H
.0805 (a) (7) (0).

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Requirement: All thermometers and temperature measuring devices must be checked
every 12 months against an NIST certified or NIST traceable thermometer and the
process documented. Ref: NC WW/GW LC Policy.
Comment: The most recent verifications were conducted after approximately 16 months
(i.e., 6/30/15 to 10/25/16).
F. Finding: Data are not consistently flagged on the electronic Discharge Monitoring Report
(eDMR) for QC failures.
Requirement: When QC failures occur, the laboratory must attempt to determine the
source of the problem and must apply corrective action. Part of the corrective action is
notification to the end user. If data qualifiers are used to qualify samples not meeting QC
requirements, the data may not be useable for the intended purposes. It is the
responsibility of the laboratory to provide the client or end -user of the data with sufficient
information to determine the usability of the qualified data.
Where applicable, a notation must be made on the eDMR form, in the comment section or
on a separate sheet attached to the eDMR form, when any required sample quality control
does not meet specified criteria and another sample cannot be obtained. Ref: NC
WW/GW LC Policy.
Comment: The laboratory appeared to be consistent with BOD qualifications, but the data
review showed that Fecal Coliform, TSS and Ammonia results were not flagged for all QC
failures. Unacceptable duplicate RPD results for Fecal Coliform which were not qualified
include samples from January 6, February 19, April 13, May 11, June 2, 6 and 10, August
22 and 25, 2016. The Fecal samples analyzed on May 4, 2016 were removed from the
incubator and counted more than 26 hours (i.e., 29:50) after the incubation start time and
the results were not qualified. Ammonia results were not qualified on May 9, 2016 for an
unacceptable second source standard (i.e., 89% recovery) nor on June 3-10, 2016
samples where an MS/MSD was not analyzed. Specific TSS duplicate RPD failures that
were not qualified include April 25, May 6 and July 6, 2016.
Proficiency Testing
Comment: Additional QC was analyzed with PT samples. An extra known standard was analyzed
with Ammonia and the PT sample was duplicated for pH, Ammonia and Fecal Coliform. The
Proficiency Testing Requirements, February 20, 2012, Revision 1.2 document states:
Laboratories shall conduct proficiency tests in accordance with their routine testing, calibration
and reporting procedures, unless otherwise specified in the instructions supplied by the PT
provider. They shall not be analyzed with additional quality control or replicated beyond what is
routine for environmental sample analysis. Results from multiple analyses (when this is the routine
procedure) must be calculated in the same manner as routine environmental samples. Notification
of acceptable corrective action (i.e., a statement that beginning with the 2017 PT samples,
additional quality control in the form of duplication and extra known standards will not be
performed) was received by email on December 6, 2016. No further response is necessary for
this Finding.
Comment: The laboratory was not consistently documenting PT sample analyses in the same
manner as environmental samples. Specific instances of this were noted with the pH and Fecal
Coliform PT samples for 2016. The analyst acknowledged that there was not always room for the
extra PT analysis results, and so they would not be recorded on the benchsheets during those

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instances. The Proficiency Testing Requirements, February 20, 2012, Revision 1.2 document
states: All PT sample analyses must be recorded in the daily analysis records as for any
environmental sample. Notification of acceptable corrective action (i.e., a statement that all PT
results will be recorded on the benchsheets starting with the 2017 PT samples) was received by
email on December 6, 2016. No further response is necessary for this Finding.
Comment: The laboratory does not have a documented plan for proficiency testing procedures.
North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) states: Each laboratory shall
develop and maintain a document outlining the analytical quality control practices used for the
parameters included in their certification. Supporting records shall be maintained as evidence that
these practices are being effectively carried out. The Proficiency Testing Requirements, February
20, 2012, Revision 1.2 document states: Laboratories must have a documented plan (this is
usually detailed in the laboratory's Quality Assurance Manual) of how they intend to cover the
applicable program requirements for proficiency testing per their scope of accreditation. This plan
shall cover any commercially available proficiency testing and any inter -laboratory organized
studies, as applicable. The laboratory must also be able to explain when proficiency testing is not
possible for certain parameters and provide a description of what the laboratory is doing in lieu of
proficiency testing. This shall be detailed in the plan. The plan must also address the laboratory's
process for submission of proficiency testing results and related corrective action responses.
Laboratory Standard Operating Procedures (SOPs) must address how low level samples will be
analyzed, including concentration of the sample or adjustment of the normality of a titrant. These
instructions shall be followed then the concentration of a PT sample falls below the range of their
routine analytical method. Instructions shall also be included in the laboratory's SOP for how high
level samples will be analyzed, including preparation of multiple dilutions of the sample. These
instructions will be followed when the concentration of a PT falls above the range of their routine
analytical method. Notification of acceptable corrective action (i.e., a statement that an SOP for
PT handling and analysis will be developed by November 15, 2017) was received by email on
December 13, 2016. No further response is necessary for this Finding.
Bacteria — Coliform Fecal — Standard Methods, 9222 D-1997 (MF) (Aqueous)
Recommendation: It is recommended that a "1" be consistently recorded in the dilution factor
column for blanks, which are all 100 mL in volume. All other dilutions are recorded.
Recommendation: It is recommended to document on the benchsheet which acceptance
criterion is used to evaluate each set of duplicates. The laboratory has tiered criteria.
Recommendation: Plate counts that are not used for reporting (i.e., not within 20-60 colonies)
are marked through on the benchsheet. It is recommended that instead of marking though plate
counts that are not used, the counts that are used for reporting have a check or other notation
placed next to it. This would help distinguish unreported results from error corrections.
Recommendation: PT samples are analyzed using two 50 mL dilutions. It is recommended that
multiple dilutions such as 5, 10, 25 and 50 mL be analyzed to cover the range of possible results.
Comment: The Fecal waterbath thermometer was not immersed to the specified immersion line.
The US EPA's User -Friendly Guidance on the Replacement of Mercury Thermometers,
https://www.e a, ov/sites/production/tiles/2015-10/documents/nistuserfriendly ide�df document
states: When a partial -immersion thermometer is used, the bottom of the thermometer up to the
immersion line should be exposed to the temperature being measured, with the remainder of the
thermometer exposed to ambient conditions. If the thermometer is not used in this manner, the
thermometer immersion is incorrect. Notification of acceptable corrective action (i.e., The
laboratory submitted a statement affirming that the waterbath was filled to the immersion line

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indicated on the thermometer on November 15, 2016 and since then is observed daily to ensure
that it remains at this line. In order to prevent future recurrence, another statement was submitted
saying that a note was placed near the waterbath by December 2, 2016 instructing that the water
must be level with the immersion line on the thermometer) was received by email on December 2,
2016. No further response is necessary for this Finding.
Comment: The Fecal Coliform incubator temperature was not checked twice daily during use.
The temperature was checked once daily. Standard Methods, 9020 B-2005. (4) (n). states: When
incubator is in use, monitor and record calibration -corrected temperature twice daily. Notification
of acceptable corrective action (i.e., a statement that beginning November 15, 2016 the waterbath
temperature is being checked and documented twice daily) was received by email on December
6, 2016. No further response is necessary for this Finding.
Comment: The sterility of laboratory sterilized bottles was not being verified. NC WW/GW LC
Policy states: Minimally test for sterility one sample bottle per batch sterilized in the laboratory, or
at a set percentage such as 1 to 4%. This is performed by adding sterile dilution/rinse water to the
bottle after sterilization and then subsequently analyzing it as a sample. Document results.
Notification of acceptable corrective action (i.e., a statement that beginning November 15, 2016,
one bottle per batch is tested for sterility and documented on the benchsheet) was received by
email on December 13, 2016. No further response is necessary for this Finding.
Comment: No expiration date was assigned to the laboratory prepared phosphate buffer. It had
last been prepared in 2010. NC WW/GW LC Policy states: If no expiration date is given, the
laboratory must have a policy for assigning an expiration date. If no date received or expiration
date can be determined, the item should be discarded. Notification of acceptable corrective action
(i.e., a statement that a new phosphate buffer will be prepared before the next dilution water batch
is made and that each batch will have a documented expiration date of 12 months after
preparation, which is recorded on the bottle) was received by email on December 13, 2016. No
further response is necessary for this Finding.
G. Finding: The use test for consumables is not properly conducted.
Requirement: Standard Methods requires that before a new lot of consumable materials
are used for the Fecal Coliform MF method, those materials be tested to ensure they are
reliable. At a minimum, make single analyses on five positive samples. North Carolina
policy requires the testing of the following consumable materials before they can be used
for sample analyses: membrane filters and/or pads (often packaged together) and media.
It is recommended that only one consumable be tested at a time. Ref: NC WW/GW
LC Policy.
Comment: The laboratory only includes 4 replicates for consumable testing. Additionally,
dilutions are of different volumes and some are not able to be used for comparison
because they are outside the ideal 20-60 colony range. Technical assistance documents
were provided to the laboratory at the time of the inspection for properly performing the
consumables test to result in five plates yielding 20-60 colonies.
H. Finding: The laboratory has not established an acceptance criterion to document the
precision of sample duplicates for plates with >60 colonies (when countable) or when one
plate has 20-60 colonies and the duplicate plate count is outside the 20-60 colony range.
Requirement: Each laboratory shall develop and maintain a document outlining the
analytical quality control practices used for the parameters included in their certification.

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Supporting records shall be maintained as evidence that these practices are being
effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).
Requirement: Any time quality control results indicate an analytical problem, the problem
must be resolved and any samples involved must be rerun if the holding time has not
expired. Ref: 15A NCAC 2H .0805 (a) (7) (F).
I. Finding: The time plates are placed into the water bath is not documented.
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15A NCAC
2H .0805 (a) (7) (A).
Requirement: Incubate for 24 ± 2 h at 44.5 ± 0.2 °C. Ref: Standard Methods 9222 D-
1997. (2) (d).
Comment: The time samples are placed into the water bath is necessary to document
that the required total incubation time is met.
J. Finding: The autoclave operating temperature is not checked weekly with a maximum
registering thermometer.
Requirement: For routine use, verify the autoclave temperature weekly by using a
maximum registering thermometer (MRT) to confirm that 121 °C has been reached. Ref:
Standard Methods, 9020 B-2005. (4) (h).
Comment: The laboratory's previous mercury MRT broke and has not been replaced.
Currently, the autoclave temperature is checked using the instrument dial and
documented and heat sensitive autoclave tape is used with each cycle.
K. Finding: The laboratory is not monitoring the quality of the reagent water used in Fecal
Coliform analysis.
Requirement: Reagent water used to prepare buffered dilution/rinse water or media must
be analyzed at least every twelve months for the following parameters: Specific
Conductance, Total Organic Carbon, Cadmium, Chromium, Copper, Nickel, Lead, and
Zinc.
Maximum Acceptable Limits are:
Specific Conductance < 2 pmhos/cm
TOC < 1.0 mg/L
Heavy Metals, single element < 0.05 mg/L
Heavy Metals, Total of cited elements < 0.10 mg/L
If the facility is using vendor purchased dilution/rinse water this testing is not required as
long as the Certificate of Analysis from the manufacturer is kept on file. Ref: NC WW/GW
LC Policy.
L. Finding: The laboratory is not testing a culture positive with each batch of media
prepared.
Requirement: A culture positive must be analyzed with each batch of prepared media and
once per week for purchased ready -to -use media. A sample volume that yields a

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countable plate must be analyzed so that individual colonies may be verified to have
proper morphology (e.g., color, shape, size, surface appearance). Ref: NC WW/GW LC
Policy.
M. Finding: Plate comparison counts are not being conducted.
Requirement: For routine performance evaluation, repeat counts on one or more positive
samples at least monthly, record results, and compare the counts with those of other
analysts testing the same samples. Replicate counts for the same analyst should agree
within 5% (within analyst repeatability of counting) and those between analysts should
agree within 10% (between analysts reproducibility of counting). If they do not agree,
initiate investigation and any necessary corrective action. Ref: Standard Methods, 9020 B-
2005. (9) (a).
N. Finding: Results were reported on the eDMR for a sample that was not analyzed.
Requirement: Frequency and Location. Except as otherwise provided herein, all industrial
establishments and units of government shall take influent, effluent and stream samples at
such locations and with such frequency as shall be necessary to conduct the tests and
analyses required by Rule .0508 of this Section. Ref: 15A NCAC 2B .0505 (c) (1).
Requirement: "Falsified data or information" means data or information which has been
made untrue by alteration, fabrication, omission, substitution, or mischaracterization. Ref:
15A NCAC 02H .0803 (6).
Comment: A sample result was reported on the eDMR for July 26, 2016; however, no
sample was collected and analyzed that day. The laboratory reported >600 #/100mL to
show that this would have been the worst case scenario had a sample been analyzed. The
result was also reported without qualification.
BOD —Standard Methods, 5210 B-2001 (Aqueous)
Comment: The location of the mid -analysis drift check was not clearly documented. While a mid -
analysis drift check is not required, when it is performed, the location during analysis needs to be
documented to assure any necessary corrective action is applied to the appropriate samples. NC
WW/GW LC Policy states: If the meter drifts more than 0.20 mg/L, recalibrate meter and
reanalyze all samples since the last drift check. Notification of acceptable corrective action (i.e.,
an updated benchsheet and statement that a procedure has been implemented as of November
30, 2016 to place a check mark next to the sample bottle read just after the drift check and next
to the drift check result) was received by email on December 6, 2016. No further response is
necessary for this Finding.
O. Finding: The documentation does not demonstrate that initial DO readings are measured
within 30 minutes of sample dilution. This is considered pertinent information.
Requirement: After preparing dilution, measure initial DO within 30 min. Ref: Standard
Methods, 5210 B-2001. (5) (g).
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15A NCAC
2H .0805 (a) (7) (A).

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Comment: Currently, only "start time" is documented. In order to show that 30 minutes or
less have passed from preparing the dilution to measuring the initial DO, a second time is
required. This is often achieved by documenting the time when all samples are placed into
the incubator.
P. Finding: The sample duplicate is not randomly selected.
Requirement: When appropriate (Table 5020:1), randomly select routine samples to be
analyzed twice. Standard Methods, 5020 B-2010. (2) (f).
Comment: The influent #2 sample was always selected for duplication.
Nitrogen, Ammonia — Standard Methods, 4500 NH3 D-1997 (Aqueous)
Comment: The inspector noted during data review that only the Thursday effluent sample was
used for the MS/MSD samples. Standard Methods, 4020 B. (2) (g). states: To prepare an LFM,
add a known concentration of analytes (ideally from a second source) to a randomly selected
routine sample without increasing its volume by more than 5%. Notification of acceptable
corrective action (i.e., a statement that while it was not necessarily the case that only the
Thursday effluent sample was used for the MS/MSD, that beginning November 15, 2016, they will
make sure that the sample used for the MS/MSD each day is more randomized) was received by
email on December 6, 2016. No further response is necessary for this Finding.
Comment: A laboratory reagent blank (method blank) was not being prepared with the
preservative. The analyst was only analyzing DI water, without preservation acid. Standard
Methods, 4020 B-2009, Rev. 2011. (2) (d). states: Include at least one method blank daily or with
each batch of 20 or fewer samples, whichever is more frequent. Standard Methods, 1020 B-2011.
(5) states: A reagent blank (method blank) consists of reagent water and all reagents (including
preservatives) that normally are in contact with a sample during the entire analytical procedure.
Notification of acceptable corrective action (i.e., a statement that preservation acid is added to a
DI water blank and analyzed as a sample beginning with the December 13, 2016 analysis) was
received by email on December 13, 2016. No further response is necessary for this Finding.
Comment: A laboratory fortified blank (LFB) was not being prepared with the preservative. A
second source standard was analyzed, but no preservation acid was added. Standard Methods,
4020 B-2009, Rev. 2011. (2) (e). states: Include at least one LFB daily or per each batch of 20 or
fewer samples. Standard Methods, 1020 B-2011. (6). states: A laboratory -fortified blank is a
reagent water sample (with associated preservatives) to which a known concentration of the
analyte(s) of interest has been added. Notification of acceptable corrective action (i.e., a
statement that preservation acid is added to the second source standard and analyzed as a
sample beginning with the December 13, 2016 analysis) was received by email on December 13,
2016. No further response is necessary for this Finding.
Comment: Blank results were not documented in a manner that demonstrates they meet the
acceptance criterion. The analyst would only record <0.1 mg/L, which is the reporting limit.
Documenting <0.1 mg/L does not demonstrate whether the blank met the acceptance criterion of
<_50% of the reporting limit. North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7)
states: Each laboratory shall develop and maintain a document outlining the analytical quality
control practices used for the parameters included in their certification. Supporting records shall
be maintained as evidence that these practices are being effectively carried out. NC WW/GW LC
Policy states: For analyses requiring a calibration curve, the concentration of reagent, method
and calibration blanks must not exceed 50% of the reporting limit or as otherwise specified by the
reference method. Notification of acceptable corrective action (i.e., a statement that as of

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#163 Wilkesboro Cub Creek WWTP Lab
November 15, 2016, the practice was implemented to record the first value obtained from the
meter after the blank reading reached < '/ the reporting limit and submission of a benchsheet
verifying implementation) was received by email on December 6, 2016 and fax on December 13,
2016. No further response is necessary for this Finding.
Comment: The samples were not always brought to room temperature prior to analysis. Sample
temperatures were documented to be occasionally as low as 9 °C. Standard Methods, 4500 NH3
D-1997. (4) (b). states: Maintain the same stirring rate and a temperature of about 25 °C
throughout calibration and testing procedures. Notification of acceptable corrective action (i.e., a
statement that beginning November 15, 2016, all samples will be brought to room temperature for
analysis) was received by email on December 6, 2016. No further response is necessary for
this Finding.
Q. Finding: The volume of NaOH added to samples and standards is not being documented.
This is considered pertinent information for result calculation.
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. 15A NCAC 2H
.0805 (a) (7) (A)
Requirement: Calculation
C 100 + D
1-ng NHS-N L= A X R x
1t10+C
Where:
A = dilution factor,
B = concentration of NH3-N/L, mg/L, from calibration curve,
C = volume of 10N NaOH added to calibration standards, mL,
and
D = volume of 10N NaOH added to sample, mL.
Ref: Standard Methods, 4500 NH3 D-1997. (5).
Comment: A benchsheet with data analyzed on November 29, 2016 was submitted on
December 13, 2016 which had a handwritten note "Added 1 mL Sodium Hydroxide to all
samples." This corrective action is not adequate. There must be a record of the amount of
NaOH added to both samples and standards to correctly document and reconstruct the
result calculation.
R. Finding: The laboratory is not preserving all samples within 15 minutes of collection.
Requirement: 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. Ref:
Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May
18, 2012; Table II.
Comment: The composite sample is brought into the laboratory to pour into individual
sample bottles containing H2SO4 preservative. Occasionally this is not completed within 15
minutes of collection.

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#163 Wilkesboro Cub Creek WWTP Lab
S. Finding: Sample pH is not consistently checked to verify proper preservation and the
process is not documented. This is considered pertinent information.
Requirement: Cool, <6 °C, H2SO4 to pH <2. Ref: Code of Federal Regulations, Title 40,
Part 136; Federal Register Vol. 77, No. 97, May 18, 2012; Table II.
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15A NCAC
2H .0805 (a) (7) (A).
T. Finding: The H2SO4 used to preserve ammonia samples was expired.
Requirement: Adherence to manufacturer expiration dates is required. Chemicals/
reagents/ consumables exceeding the expiration date can no longer be considered
reliable. Ref: NC WW/GW LC Policy.
Comment: The manufacturer's expiration date was February 18, 2016.
Nitrogen, Ammonia — Standard Methods, 4500 NH3 D-1997 (Aqueous)
BOD — Standard Methods, 5210 B-2001 (Aqueous)
U. Finding: New employees are not performing an Initial Demonstration of Capability before
beginning analytical testing.
Requirement: Initial demonstration of capability (IDC): Before new analysts run any
samples, verify their capability with the method. Run a laboratory -fortified blank (LFB)
(4020B.2e) at least four times and compare to the limits listed in the method. Ref:
Standard Methods, 4020 B-2009, Rev. 2011. (1) (a).
Requirement: Initial demonstration of capability (IDC): Before new analysts run any
samples, verify their capability with the method. Run a laboratory -fortified blank (LFB)
(5020B.2e) at least four times and compare to the limits listed in the method. Ref:
Standard Methods, 5020 B-2010. (1) (a).
Residue, Suspended — Standard Methods, 2540 D-1997 (Aqueous)
Comment: The following requirement was discussed during the inspection and this comment
serves as a reminder. No instance was found during data review. The analyst was unaware that
any time less than 1000 mL of sample is analyzed, and the weight gain is <0.0025 g, the reporting
limit is to be elevated and the sample reported appropriately to that reporting limit. For instance, if
500 mL of sample is analyzed and <0.0025 g of weight gain is achieved, the elevated PQL is 5
mg/L and the result would be reported as <5 mg/L. The elevated reporting limit = 2.5mg/volume
sample analyzed (in Liters).
Comment: The times samples were placed into and taken out of the oven were not consistently
documented. This is considered pertinent information to document proper drying time. North
Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (A) states: All analytical data pertinent
to each certified analysis must be filed in an orderly manner so as to be readily available for
inspection upon request. Standard Methods, 2540 D-1997. (3) (c). states: Dry for at least 1 h at
103 to 105 °C in an oven, cool in a desiccator to balance temperature, and weigh. Notification of
acceptable corrective action (i.e., a statement that a sign was posted on the oven by December 1,
2016 reading "Always record time in and out of oven on benchsheet" and a benchsheet with data

Page 13
#163 Wilkesboro Cub Creek WWTP Lab
from November 28 through December 2, 2016 verifying implementation) was received by email on
December 6, 2016 and fax on December 13, 2016. No further response is necessary for this
Finding.
Comment: The annual drying study in lieu of weighing to constant weight was not properly
performed. The study only included one sample type (i.e., the effluent), which is not fully
representative of the laboratory's routine samples and the drying times used were not
documented. NC WW/GW LC Policy states: Constant weights must be documented. The
approved methods require the following: "Repeat the cycle of drying, cooling, desiccating, and
weighing until a constant weight is obtained or until the weight change is less than 4% of the
previous weight or 0.5 mg, whichever is less." In lieu of this, an annual study documenting the
time required to dry representative samples to a constant weight may be performed. Verify
minimum daily drying time is greater than or equal to the time used for the initial verification study
drying cycle. Drying cycles must be a minimum 1 hour for verification. Notification of acceptable
corrective action (i.e., a statement that a drying study which includes all routine samples and will
clearly document drying times will be completed in January 2017) was received by email on
December 2 and 13, 2016. No further response is necessary for this Finding.
V. Finding: The sample duplicate is not randomly selected.
Requirement: When appropriate (Table 2020:11), randomly select routine samples to be
analyzed twice. Ref: Standard Methods, 2020 B-2010. (2) (f).
Comment: Only the Influent #2 sample is being duplicated. The Effluent, Influent #1 and
Influent #2 all need to be periodically duplicated.
Dissolved Oxygen — Standard Methods, 4500 O G-2001 (Aqueous)
Recommendation: It is recommended that the correction factor used to determine the post -
analysis meter calibration verification be documented. Since DO is analyzed on site, a post -
analysis meter calibration verification is not required. The easiest factor to use and document is
correction by elevation since that will remain constant.
Dissolved Oxygen — Standard Methods, 4500 O G-2001 (Aqueous)
Temperature — Standard Methods, 2550 B-2000 (Aqueous)
Comment: Only one time for sample collection and analysis was documented on the
benchsheet, without noting samples are analyzed in situ. The NC WW/GW LC Approved
Procedure for the Analysis of Temperature document states: Alternatively, since EPA requires
samples to be analyzed immediately, one time may be documented for collection and analysis
with the notation that samples are measured in situ or immediately at the sampling site (i.e.,
immediately following collection at a location as near to the collection point as possible). When
this `one time' option is used, state that the documented time is both collection and analysis time.
The NC WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen document states:
Alternatively, one time may be documented for collection and analysis with the notation that
samples are measured in situ or immediately at the sample site. Notification of acceptable
corrective action (i.e., a copy of the updated benchsheet implemented by December 1, 2016
which includes the blanket statement "All measurements are done in stream") was received by
email on December 6, 2016. No further response is necessary for this Finding.

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#163 Wilkesboro Cub Creek WWTP Lab
pH — Standard Methods, 4500 H+113-2000 (Aqueous)
Recommendation: The pH benchsheet lists the reference method as Standard Methods Part
4500 H-2000. It is recommended that it be updated to the full reference (including Section letter)
listed on the laboratory's Certified Parameters Listing (i.e., Standard Methods, 4500 H+B-2000).
pH — Standard Methods, 4500 H+B-2000 (Aqueous)
Temperature — Standard Methods 2550 B-2000 (Aqueous)
Dissolved Oagen — Standard Methods, 4500 O G-2001 (Aqueous)
Comment: The benchsheets did not contain the facility name and instrument identification. The
NC WW/GW LC Approved Procedure for the Analysis of pH, NC WW/GW LC Approved
Procedure for the Analysis of Temperature and NC WW/GW LC Approved Procedure for the
Analysis of Dissolved Oxygen documents state: The following must be documented in indelible ink
whenever sample analysis is performed. Sampling site including facility name and location, ID,
etc. Thermometer/instrument identification. Notification of acceptable corrective action (i.e., copies
of the updated pH and DO/Temperature benchsheets which were implemented by December 1,
2016 with the instruments identified and Wilkesboro Cub Creek WWTP Lab added to each) was
received by email on December 6, 2016. No further response is necessary for this Finding.
IV. PAPER TRAIL INVESTIGATION:
The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks,
etc.) and contract lab reports to eDMRs submitted to the North Carolina Division of Water
Resources. Data were reviewed for Wilkesboro Cub Creek WWTP (NPDES permit #
NC0021717) for February, June and September 2016. The following errors were noted:
Date
Parameter
Location
Analytical Result
*Contract Lab Data
Value on eDMR
2/12/2016
TSS
Effluent
16.7 mg/L
25 mg/L
6/8/2016
Zinc
Effluent
*0.027 mg/L
0.029 mg/L
7/16/2016
DO
Effluent
6.7 mg/L
6.73 mg/L
In order to avoid questions of legality, it is recommended that you contact the appropriate
Regional Office for guidance as to whether an amended eDMR will be required. A copy of this
report will be made available to the Regional Office.
V. CONCLUSIONS:
Correcting the above -cited Findings and implementing the Recommendations will help this
laboratory to produce quality data and meet Certification requirements. The inspectors 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 and implementation
dates for each corrective action.
Report prepared by: Beth Swanson Date: January 13, 2017
Report reviewed by: Jason Smith Date: January 17, 2017

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