#114_2018_1212_TS_FINAL

Laboratory Cert. :
114
Laboratory Name:
Clinton -Norman H. Larkins WWTP Lab.
Inspection Type:
Municipal Maintenance
Inspector Name(s):
Tonja Springer, Todd Crawford and Tom Halvosa
Inspection Date:
December 12, 2018
Date Forwarded for Initial
Review:
January 18, 2019
Initial Review by:
Tom Halvosa
Date Initial Review
Completed:
January 22, 2019
Cover Letter to use:
❑ Insp. Initial ❑ Insp. Reg
❑Insp. No Finding ❑Insp. CP
❑Corrected ®Insp. Reg. Delay
Unit Supervisor/Chemist III:
Todd Crawford
Date Received:
January 23, 2019
Date Forwarded to Admin.:
February 1, 2019
Date Mailed:
February 4, 2019
Special Mailing Instructions:

CLOY t t.�t:il''`E
I.,, I D A CR I Na I 'PPE R
114
Ms. Lisa Osthues
Clinton -Norman H.
P.O. Box 199
Clinton, NC 28328
Larkins WWTP Lab.
N 0Ir":l i t CAR
Errvironrraer tat QrTaUxy
February 4, 2019
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection -
Dear Ms. Osthues:
Enclosed is a report for the inspection performed on December 12, 2018 by Tonja Springer. 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].
Attachment
cc: Dana Satterwhite, Tonja Springer, Master File #114
Sincerely,
Todd Crawford
Technical Assistance & Compliance Specialist
NC WW/GW Laboratory Certification Branch
r
North Carolina Department of Environmental Quality I Division of Water Resources
1623 Mail Service. Center I Raleigh, North Carolina 27699-1.623
Phone [phone]/Fax [phone]

LABORATORY NAME: Clinton -Norman H. Larkins WWTP Lab.
NPDES PERMIT : NC0020117
NC GENERAL PERMIT #: NCG590015
ADDRESS: 123 Mill Branch Road
Clinton, NC 28328
CERTIFICATE #: 114
DATE OF INSPECTION: December 12, 2018
TYPE OF INSPECTION: Municipal Maintenance
AUDITOR(S): Tonja Springer, Todd Crawford and Tom Halvosa
LOCAL PERSON(S) CONTACTED: Lisa Osthues, Patrick West and Barry Templin
INTRODUCTION:
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 compliance monitoring samples.
II. GENERAL COMMENTS:
The auditors found this lab to have excellent organization. This was evident from viewing records
and observing the layout and actions which help streamline the day to day activities of the lab.
The staff were very forthcoming and willing to make necessary changes.
All required Proficiency Testing (PT) Samples have been analyzed and the laboratory has fulfilled
its PT requirements for the 2018 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 January 31, 2020.
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

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#114 Clinton -Norman H. Larkins WWTP Lab.
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.
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 Environmental Chemists, Inc. (Certification # 94).
Approved Procedure documents for the analysis of the facility's currently certified Field
Parameters were provided at the time of the inspection.
Documentation
Recommendation: The Ammonia benchsheet has column headings for "LFM1" and "LFM2".
These represent the LFM and LFMD. However, there is no indication of which sample is being
spiked. It is recommended that the column header be revised to say "LFM" and "LFMD" and a
space be added to document which sample is being spiked to ensure effective traceability.
Recommendation: The Ammonia benchsheet states the acceptance criterion for the LFM is 0.8
to 1.2 mg/L. This assumes a sample concentration of <1.0 mg/L. It is recommended the
laboratory clearly document the required percent recovery instead of a concentration range.
A. Finding: The laboratory benchsheets for Total Residual Chlorine (TRC) and Specific
Conductance (Conductivity) are lacking pertinent data: meter calibration time.
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: The following must be documented in indelible ink whenever sample
analysis is performed: meter calibration time. Ref: NC WW/GW LC Approved Procedure
for the Analysis of Total Residual Chlorine and NC WW/GW LC Approved Procedure for
the Analysis of Specific Conductance (Conductivity).
B. Finding: The laboratory benchsheets for Dissolved Oxygen (DO) and Temperature are
lacking pertinent data: method reference.

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#114 Clinton -Norman H. Larkins WWTP Lab.
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: The following must be documented in indelible ink whenever sample
analysis is performed: meter calibration. Ref: NC WW/GW LC Approved Procedure for
the Analysis of Dissolved Oxygen and INC WW/GW LC Approved Procedure for the
Analysis of Temperature.
C. Finding: The laboratory needs to increase the traceability documentation of purchased
materials.
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. 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.
Requirement: Supporting records shall be maintained as evidence that these practices
are being effectively carried out. All analytical records must be available for a period of
five years. Ref: 15A NCAC 2H .0805 (a) (7) and (a) (7) (G).
Comment: TRC filter traceability information is not documented in a way to provide
linkage between the filters and the samples analyzed. Documenting lot numbers on the
benchsheet would satisfy this requirement.
Quality Control
Comment: Sample duplicates are not a required quality control element for Field Parameters
(i.e., Conductivity, Dissolved Oxygen, pH, Settleable Residue, Temperature and TRC). The
laboratory is currently analyzing duplicates on Conductivity and TRC samples.
D. Finding: The laboratory is not randomly selecting Ammonia samples to fortify.
Requirement: When appropriate for the analyte (Table 4020:1), include at least one
LFM/LFMD daily or with each batch of 20 or fewer samples. 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%. Ref: SM 4020 B-2011,
Table 4020:1 and (2) (g).
Comment: The laboratory routinely fortifies the Effluent sample only.
E. Finding: The laboratory is not rotating the range of Ammonia spike concentrations.
Requirement: To prepare an LFM, add a known concentration of analytes (ideally from a
second source) to a randomly selected routine sample without increasing its volume by
more than 5%. Ideally, the new concentration should be at or below the midpoint of the

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#114 Clinton -Norman H. Larkins WWTP Lab.
calibration curve, and for maximum accuracy, the spike should approximately double the
sample's original concentration. If necessary, dilute the spiked sample to bring the
measurement within the calibration curve. Also, rotate the range of spike concentrations to
verify performance at various levels. Ref: SM 4020 B-2011. (2) (g).
Recommendation: It is recommended that the frequency at which spike concentrations
are changed be at least quarterly.
F. Finding: Spike recovery is not being calculated correctly when sample concentrations are
less than the reporting limit.
Requirement: If the sample concentration is below the reporting limit, use zero for
amount of target in the unspiked sample. Ref: North Carolina Wastewater/Groundwater
Laboratory Certification Matrix Spiking Policy and Technical Assistance.
Comment: Percent Recovery = spiked sample result (A) — unspiked sample result (B)
divided by theoretical value (C) X 100. The unspiked sample concentration (B) displayed
on the meter is used to calculate the spiked sample recovery even when that
concentration is below the reporting limit (i.e., the actual sample result for B instead of
zero). Because of this, the recovered spike concentrations (A — B) in the LFM and LFMD
on December 4, 2018 were incorrectly calculated to be 1.17 mg/L and 1.19 mg/L. If
sample concentrations of zero had been used, the recovered spike concentrations in the
LFM and LFMD would have been 1.42 mg/L and 1.44 mg/L, which were outside the
acceptance criterion.
G. Finding: The Ammonia benchsheet incorrectly lists the blank acceptance criterion as 5
mg/L.
Requirement: 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. Ref: NC WW/GW LC Policy.
Comment: The acceptance criterion on the Ammonia benchsheet is 5 5 mg/L which
exceeds 50% of the reporting limit (i.e., 1.0 mg/Q. The correct acceptance criterion is <_
0.5 mg/L. None of the data reviewed exceeded 0.5 mg/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 (e.g., pH), but it is recommended that the instructions be
maintained. Ref: Proficiency Testing Requirements, May 31, 2017, Revision 2.0.
Comment: Dating and initialing the instruction sheet for the prepared PT Sample for
Ammonia and TRC would satisfy the documentation requirement.

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#114 Clinton -Norman H. Larkins WWTP Lab.
Bacteria — Coliform, Fecal — IDEXX Colilert 018 (MPN) (Aqueous)
Recommendation: It is recommended the laboratory remove the incubator temperature from the
benchsheet since it is not consistently documented in the space provided. The incubator
temperature is checked twice daily and documented in a temperature log.
Comment: The thermometer's immersion line was well above the water level when first checked
during the inspection. There were no samples in the bath at the time. The water level was
adjusted during the inspection and the proper immersion depth was discussed during the exit
interview.
Finding: The Quanti-Tray® sealer is not checked monthly for leaks.
Requirement: If the Quanti-Tray® or Quanti-Tray®/2000 test is used, the sealer must
be checked monthly by adding a dye (e.g., bromcresol purple) to a water blank. If dye is
observed outside the wells, either perform maintenance or use another sealer. Ref: NC
WW/GW LC Policy.
Comment: The Quanti- Tray® sealer was checked in May and June 2018.
Chlorine, Total Residual — Standard Methods, 4500 Cl G-2011 (Aqueous)
Recommendation: It is recommended the laboratory verify the factory -set calibration curve
annually using a 400 pg/L standard as the highest standard concentration. Currently, the highest
standard concentration verified is 200 pg/L. PT Sample concentrations can exceed 300 pg/L,
though all observed historical PT Samples analyzed by the laboratory were bracketed. Increasing
the highest standard concentration to 400 pg/L will ensure future PT Sample concentrations will
be within the verified range of the curve.
Conductivity —Standard Methods, 2510 B-2011 (Aqueous)
J. Finding: The Automatic Temperature Compensator (ATC) was not properly verified.
Requirement: The Automatic Temperature Compensator (ATC) must be verified prior
to initial use and annually (i.e., 12 months) thereafter at two temperatures by analyzing a
standard or sample at 25°C (i.e., the temperature to which conductivity values are
reported) and a temperature(s) that brackets the temperature ranges of the
environmental samples routinely analyzed. This may require the analysis of a third
temperature reading that is > 25°C. As the temperature increases or decreases, the
value of the conductivity standard or sample must be within ±10% of the true value of
the standard or ±10% of the value of the sample at 25°C. If not, corrective action must
be taken. Ref: NC WW/GW LC Approved Procedure for the Analysis of Specific
Conductance (Conductivity).
Comment: The ATC was verified at 15°C, 200C and 30°C. A standard or sample must be
verified at 25°C, which is the temperature that conductivity values are compensated to.
Anticipated temperatures can be obtained from a review of the Discharge Monitoring
Reports (DMRs) from the peak summer and winter months. Historical data should provide
a reasonably accurate estimation of ranges that will bracket the expected sample
temperatures.

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#114 Clinton -Norman H. Larkins WWTP Lab.
Nitrogen, Ammonia - Standard Methods, 4500 NH3 D-2011 (Aqueous)
Comment: The laboratory analyzes a sample duplicate in addition to the LFM/LFMD. Analysis of
the LFMD, at the required frequency, is acceptable to satisfy the sample duplicate requirement
listed in North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (C).
K. Finding: The laboratory is not consistently chemically preserving the Influent samples to a
pH <2 S.U. within 15 minutes of collection.
Requirement: Cool, <_6 °C, H2SO4 to pH <2. Ref: Code of Federal Regulations, Title 40,
Part 136; Federal Register Vol. 82, No. 165, August 28, 2017; Table II.
Requirement: Except where noted in this Table II and the method for the parameter,
preserve each grab sample within 15 minutes of collection. For a composite sample
collected with an automated sample (e.g., using a 24-hour composite sample; see 40 CFR
122.21 (g)(7)(i) or 40 CFR Part 403, Appendix E), refrigerate the sample at :560C during
collection unless specified otherwise in this Table II or in the method(s). For a composite
sample to be split into separate aliquots for preservation and/or analysis, maintain the
sample at <-6°C, unless specified otherwise in this Table II or in the method(s), until
collection, splitting, and preservation is completed. Add the preservative to the sample
container prior to sample collection when the preservative will not compromise the integrity
of a grab sample, a composite sample, or aliquot split from a composite sample within 15
minutes of collection. If a composite measurement is required but a composite sample
would compromise sample integrity, individual grab samples must be collected at
prescribed time intervals (e.g., 4 samples over the course of a day, at 6-hour intervals).
Ref: Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 88, No. 165,
August 28, 2017; Table Il, Footnote 2.
Comment: Samples were not preserved on November 28, 2018 and November 29, 2018.
Residue, Suspended - Standard Methods, 2540 D-2011 (Aqueous)
Comment: A quarterly check standard is being analyzed at three different volumes and one of the
volumes is duplicated. Only one volume is required.
Comment: The annual drying time verification study was performed for 1 hour but samples are
dried for 2 hours. Samples can be dried for 1 hour since a 1-hour drying time has been verified.
Recommendation: It is recommended the laboratory change the column heading "Dilution
Factor" to 1000,000/ mL sample".
L. Finding: The laboratory is not analyzing a volume of sample to yield a minimum of 2.5 mg
dried residue.
Requirement: Choose sample volume to yield between 2.5 and 200 mg dried residue. If
volume filtered fails to meet minimum yield, increase sample volume up to 1 L. If complete
filtration takes more than 10 minutes increase filter diameter or decrease sample volume.
Ref: Standard Methods, 2540 D-1997 (3) (b).
Comment: The laboratory routinely filters only 500 mLs of sample.

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#114 Clinton -Norman H. Larkins WWTP Lab.
Temperature — Standard Methods, 2550 5-2010 (Aqueous)
Recommendation: Unless greater precision is required by the permit or data receiving agency, it
is recommended that all temperatures reported for compliance monitoring, be reported in whole
numbers as recommended by the Precision in Discharge Monitoring Reports document found
here:htt .1� rCr�( ncderi?r r� �'/docE,4 r`en' ' hbrar /qet l ljL,�i^d `,' 07b3-''O e84 45.,�' 9i/��J
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The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks,
etc.) and contract lab reports to Discharge Monitoring Reports (DMRs) submitted to the North
Carolina Division of Water Resources. Data were reviewed for Clinton -Norman H. Larkins
WWTP Lab (NPDES #NC0020117) for January, July and October 2018. No transcription errors
were observed. The facility appears to be doing a good job of accurately transcribing data.
Correcting the above -cited Findings and implementing the Recommendations will help this
laboratory to produce quality data and meet Certification requirements. The inspector would like
to thank the staff for their assistance during the inspection and data review process. Please
respond to all Findings and include supporting documentation, implementation dates
and steps taken to prevent recurrence for each corrective action.
Report prepared by: Tonja Springer Date: January 18, 2019
Report reviewed by: Tom Halvosa Date: January 22, 2019

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