#131_2016_0308_TS_FINAL

Water Resources
ENVIRONMENTAL QU.ALI"CY
June 27, 2016
131
Ms. Tammy Smith
City of Lumberton Environmental Utilities Laboratory
P.O. Box 1388
Lumberton, NC 28359
PAT MCCRORY
DONALD R. VAN DER VAART
,,
S. JAY ZIMMERMAN
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Ms. Smith:
Enclosed is a report for the inspection performed on March 8, 2016 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.
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] ext. 251.
Sincerely,
D ozr-o�
Todd Crawford
Technical Assistance & Compliance Specialist
NC WW/GW Laboratory Certification Branch
Attachment
cc: Dana Satterwhite, Tonja Springer, Master File
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] t FAX: [phone]
Internet' http://deg.nc.gov/aboutidivisions/water-resources/water-resources-data/water-sciences-home-page/laboratory-certification-branch

z, - • :if] Zia 'TeltAtime-
Wil
To be attached to all inspection reports in-house only.
Laboratory Cert. #:
Laboratory Name:
Inspection Type:
Inspector Name(s):
Inspection Date:
Date Report Completed:
Date Forwarded to Reviewer:
Reviewed by:
Date Review Completed:
Cover Letter to use:
Unit Supervisor/Chemist III:
Date Received:
Date Forwarded to Admin:
Date Mailed:
City of Lumberton Environmental Utilities Laboratory
Municiaal Maintenance
Tonia Springer, Dana Satterwhite, Anna Ostendorff
Gary Francies, and Todd Crawford
March 8, 2016
April 28. 2016
April 28, 2016
Jason Smith
5/12/16
❑ Insp. Initial ❑ Insp. Reg.
❑ Insp. No Finding ❑ Insp. CP
❑ Corrected ® Insp. Reg. Delay
Todd Crawford
5/17/2016
6/27/2016
6/27/2016

LABORATORY NAME:
NPDES PERMIT #:
ADDRESS:
CERTIFICATE :
DATE OF INSPECTION:
TYPE OF INSPECTION:
AUDITOR(S):
LOCAL PERSON(S) CONTACTED:
I. INTRODUCTION:
City of Lumberton Environmental Utilities Laboratory
NCO024571
P.O. Box 1388
Lumberton, NC 28359
131
March 8, 2016
Municipal Maintenance
Tonja Springer, Dana Satterwhite, Gary Francies, Anna Ostendorff,
and Todd Crawford
Tammy Smith and Kerdette Lowry
This laboratory was inspected by a representative 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 Was immaculate and well organized. The facility has all the equipment necessary to
perform the analyses. Analytical data pertinent to each certified analysis was filed in an orderly manner
and was readily available for inspection upon request. The organizational culture of this laboratory is one
that focuses on quality of data. Laboratory staff contacted during the audit were interested and willing to
adapt their processes to the required and recommended changes. Laboratory personnel were
knowledgeable and forthcoming and accessible to answer questions that arose during the inspection.
All required Proficiency Testing (PT) samples for the 2016 PT calendar year have not yet been analyzed.
The laboratory is reminded that results must be received by this office directly from the vendor by
September 30, 2016.
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 October 31, 2016.
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

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#131 City of Lumberton Environmental Utilities Laboratory
instances, the laboratory may need to create a SOP to document how new functions or policies will be
implemented.
The laboratory is also reminded that SOPs are intended to describeprocedures exactly as they are to be
performed. Use of the word "should" is not appropriate when describing requirements (e.g. 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 demonstrating
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) and Environment 1, Inc.
(Certification #10).
Current Quality Assurance Policies for Field Laboratories and Approved Procedure documents for the
analysis of the facility's currently certified methods were provided at the time of the inspection.
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
Quality Control
Comment: When verifying a factory set curve, all standards are considered second source. Additional
second source standards are not required. The laboratory currently verifies the curve daily with a second
source standard. When verifying a factory set curve, all standards are second source. -
Comment: Duplicate analyses are not required for Field parameters (i.e., pH, Total Residual Chlorine,
Dissolved Oxygen, Temperature, and Conductivity).
Comment: The sample preservation and storage temperature requirements may be changed in
accordance with 40 CFR Part 136.3 Table II in all pertinent SOPs and in practice. The current practice is
"at or below 4°C." 40 CFR Part 136.3 Table II allows :560C for most inorganic parameters and <10°C for
bacterial tests, without evidence of freezing. Additionally, the holding time for Fecal Coliform may be
extended from 6 hours to 8 hours.
Recommendation: It is recommended the laboratory follow The Division of Water Resources (DWR)
guidance for significant figures reporting. The North Carolina Division of Water Resources, Water
Quality Permitting Section has developed an NPDES Compliance Guidance Document titled,
Significant Figures and Their Use on Discharge Monitoring Reports (DMRs). This document
provides guidance to promote the consistent use of significant figures in preparing Discharge
Monitoring Reports (DMRs). If you have any questions about the guidance provided in this document,
please contact Mike Templeton, P.E. Water Quality Permitting Section, Wastewater Branch at
mike.tempietonCcDncdenr.. ov .
Proficiency Testing (PT)
Comment: The laboratory personnel had not reviewed the PT Guidance Document. A copy of the
document was provided at the time of the inspection.

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#131 City of Lumberton Environmental Utilities Laboratory
A. Finding: Preparation of PT samples that require vendor directed dilutions are not documented.
Requirement: PT samples received as ampules must be diluted according to the PT provider's
instructions. The preparation of PT samples must be documented in a traceable log or other
traceable format. The diluted PT sample becomes a routine environmental sample and is added
to a routine sample batch for analysis. Ref: Proficiency Testing Requirements, February 20,
2012, Revision 1.2.
Comment: Dating and initialing PT sample dilution instructions would satisfy the documentation
requirement.
D. Finding: The laboratory does not have a documented plan for analysis of PT samples.
Requirement: 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. Ref: 15A
NCAC 2H .0805 (a) (7).
Requirement: 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. Ref: Proficiency
Testing Requirements, February 20, 2012, Revision 1.2.
C. Finding: The laboratory is not analyzing PT samples in the same manner as compliance
samples.
Requirement: All PT samples are to be analyzed and the results reported in a manner
consistent with the routine analysis and reporting requirements of compliance samples and any
other samples analyzed according to the requirements of 15A NCAC 2H .0800. Ref: Proficiency
Testing Requirements, February 20, 2012, Revision 1.2.
Comment: The laboratory's common practice was to analyze PT samples on the same day as all
their quarterly QC standards. Since this is not performed with all environmental samples, it is
considered additional quality control. However, known samples are recommended when analyzing
remedial PT samples as part of the troubleshooting and corrective action process.
Documentation
D. Finding: The laboratory needs to increase the documentation of purchased materials,
consumable 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 standard(s) used, the solvent and final volume of

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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: Following are examples of traceability issues observed. This list may not be
complete.
® Traceability is needed for the calibration standards, calibration verification standards,
quarterly known standards and PTs for the Ammonia Nitrogen benchsheet. (e.g., stock
lot number and vendor, etc.)
® Date put in use, date opened, and occasionally the expiration date and the vendor is not
documented in the standards and reagent log.
® Traceability is needed for the pH buffers.
® Suspended Residue filter traceability information is not documented in a way to provide
linkage between the filters and the samples analyzed.
® Traceability is not being extended to the Suspended Residue and Total Residue
quarterly standards.
E. Finding: Error corrections are not always properly performed.
Requirement: 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. Wite-Out®, correction tape or similar products designed to obliterate documentation
are not to be used. Write the correction adjacent to the error. The correction must be initialed
by the responsible individual and the date of change documented. All data and log entries must
be written in indelible ink. Pencil entries are not acceptable. Ref: NC WW/GW LC Policy.
Comment: Some instances of overwriting errors and error corrections without initials and
dates were observed for Ammonia data for January 2016.
Bacteria — Coliform Fecal — IDEXX Colilert 0 18 (MPN) (Aqueous)
Comment: All values are not being reported on the Discharge Monitoring Report (DMR). Duplicates are
analyzed and only the first value is reported. The North Carolina Administrative Code, 15A NCAC 2B
.0506 (b) (3) (J) states: The results of all tests on the characteristics of the effluent, including but not
limited to NPDES permit monitoring requirements, shall be reported on the monthly report forms.
Notification 'of acceptable corrective action (i.e., an updated benchsheet which included space to
document the average of the duplicates and a statement that duplicates are averaged as part of the
reporting results, with an implementation date of 4/1/2016) was received by email on 4/6/2016. No
further response is necessary for this Finding.
Recommendation: It is recommended before analyzing samples, if sample is not already at 33-38°C,
place sample container in a 350C water bath for about 20 minutes or, alternatively, a 44.5°C water bath
for 7-10 minutes.
F. Finding: The laboratory is using a total immersion thermometer in the fecal water bath
improperly.

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Requirement: Thermometers with no indicated depth are the total immersion type. 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. When a total immersion thermometer is used, the bulb and the
entire portion of the stem containing liquid, except for the last 1 cm, are exposed to the
temperature being measured. If the thermometer is not used in this manner, the thermometer
immersion is incorrect. Ref: "Selecting Alternatives to Mercury -Filled Thermometers",
http:/I nn v.ep ov/mercu/alternatives.htm.
Comment: If the thermometer is not able to be properly submerged, an NIST traceable partial
immersion thermometer or the digital thermometer on the incubator (after acceptable verification
against a NIST traceable thermometer) must be used.
G. Finding: Samples are not consistently checked and documented for the presence of residual
chlorine.
Requirement: Dechlorinating agents used at the time of sampling must be documented to have
been effective upon receipt in the laboratory. A variety of field testing kits are considered to be
adequate for most chlorine interference checks and a maximum detection limit of 0.5 mg/L is
allowed. Ref: NC WW/GW LC Policy.
Comment: The benchsheet provides a box to check yes or no if chlorine is present but it is not
always checked. The box was not checked for January 4, 5, 7, 14, 15 and 22, 2016. Samples
must be checked for the presence of chlorine after an aliquot is taken for analysis to avoid
contamination.
BOD — Standard Methods, 5210 B-2001 (Aqueous)
Comment: Dilution water blank averages are routinely calculated correctly. On the 1/3/2016, the average
of -0.25 mg/L and -0.23 mg/L was incorrectly documented as 0.24 mg/L. The average should have been
documented as -.024 mg/L. No other instances of this type error were observed.
Recommendation: There were many instances of negative blanks. Negative blanks could be
contributed to meter calibration drift from day 1 to day 5, possible air bubbles, improper seal, etc. It is
recommended that the laboratory establish limits for acceptance and corrective actions for
exceedances for negative blanks.
Recommendation: It is recommended that negative blanks not exceed the blank acceptance criterion
on the negative side (e.g., -0.20 mg/L).
Comment: Sample volumes <3 mL were being measured without primary dilutions. The NC WW/GW
LC Policy states: For dilutions greater than 1:100 make a primary dilution before making final dilution.
This would be any measurements of less than 3 mL sample volume if diluting directly into BOD bottles.
Notification of acceptable corrective action (i.e., an updated benchsheet that included a statement saying
"Serial dilutions need to be done on any sample that uses less than 3 mL of sample. See SOP for Serial
Dilutions." with an implementation date of 4/1/2016) was received by email on 4/6/2016. No further
response is necessary for this Finding.
Comment: An inconsistency was noted between the Standard Operating Procedure (SOP) and
laboratory practice. Duplicates were evaluated using absolute difference criteria of <2.0 mg/L of
dissolved oxygen. The SOP states that duplicates with a Relative Percent Difference (RPD) >25% must
be reanalyzed. The North Carolina Administrative Code, 15 NCAC 2H .0805 (a) (7) states: Each

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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. Notification of acceptable corrective action (i.e., an
updated benchsheet that included the method duplicate acceptance criteria of <30% RPD, with an
implementation date of 4/1/2016) was received by email on 4/6/2016. No further response is necessary
for this Finding.
Comment: The analysis start time was not documented to verify that initial DO measurements were
made within the 30-minute time requirement. Standard Methods 5210 B-2001 (5) (g) states: After
preparing dilution, measure initial DO within 30 min. The North Carolina Administrative Code, 15 NCAC
2H .0805 (a) (7) states: Supporting records shall be maintained as evidence that these practices are
being effectively carried out. Notification of acceptable corrective action (i.e., an updated benchsheet that
included setup start time, with an implementation date of 4/1/2016) was received by email on 4/6/2016.
No further response is necessary for this Finding.
Comment: Units of measure are not documented on the benchsheet for all the column headers
associated with measurements or on the space for the DO Meter calibration labelled Air Saturation. The
North Carolina Administrative Code, 15 NCAC 2H .0805 (a) (7) (H) states: All laboratories must use
printed laboratory bench worksheets that include a space to enter the signature or initials of the
analyst, date of analyses, sample identification, volume of sample analyzed, value from the
measurement system, factor and final value to be reported and each item must be recorded each time
samples are analyzed. The date and time BOD and coliform samples are removed from the incubator
must be included on the laboratory worksheet. Notification of acceptable corrective action (i.e., an
updated benchsheet that included all units of measure with an implementation date of 4/1/2016) was
received by email on 4/6/2016. No further response is necessary for this Finding.
H. Finding: Dilutions that did not deplete at least 2.0 mg/L DO and have at least 1.0 mg/L DO
remaining were being averaged for the final BOD results.
Requirement: Average the test results for all qualified bottles within each dilution series.
Standard Methods, 5210 B-2001. (7) (b).
Requirement: Only bottles, including seed controls, giving a minimum DO depletion of 2.0
mg/L and a residual DO of at least 1.0 mg/L after 5 d of incubation are considered to produce
valid data. Ref: Standard Method, 5210 B-2001. (7) (a).
Comment: Dilutions that did not meet the 2 and 1 rule were averaged in the final calculation on
the following dates: 1/6/2016, 1/7/2016, 1/12/2016, 1/14/2016, 1/18/2016, 1/19/2016 and
1 /24/2016.
Finding: The lab is measuring sample volumes <20 mLs without using wide tip pipets.
Requirement: Sample volumes less than 20 mLs must be measured using a wide -tip pipet.
Ref: NC WW/GW LC Policy.
COD — Standard Methods, 5220 D-1997 (Aqueous)
Comment: The laboratory is having each analyst verify the factory -set curve annually. The factory -set
curve can be verified annually by one analyst and used by all the analysts.
Comment: Units of measure were not documented in the "raw reading" and "reagent blank" column
headings. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (H) states: All
laboratories must use printed laboratory bench worksheets that include a space to enter the signature or

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#131 City of Lumberton Environmental Utilities Laboratory
initials of the analyst, date of analyses, sample identification, volume of sample analyzed, value from the
measurement system, factor and final value to be reported and each time must be recorded each time
samples are analyzed. Notification of acceptable corrective action (i.e., an updated benchsheet which
included proper units of measure in the "raw reading" and "reagent blank" column headings with an
implementation date of 4/1/2016) was received by email on 4/6/2016. No further response is necessary
for this Finding.
Comment: A calibration verification curve is not prepared for each new lot of tubes. Standard
Methods, 5220 D-1997 (4) (c) states: Prepare calibration curve for each new lot of tubes or ampules or
when standards prepared in ¶ a above differ by > 5% from calibration curve. Notification of acceptable
corrective action (i.e., an updated benchsheet which included a statement, "Run a 5-point curve on
each method (LR and HR) when you use a new lot # of vials. To verify the manufacturers curve." with
an implementation date of 4/1/2016) was received by email on 4/6/2016. No further response is
necessary for this Finding.
Comment: A LFM is not analyzed. Standard Methods, 5020 B-2011 (2) (g) states: 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%. Note that the analysis of an LFMD is not necessarily required for
this method. Table 5020: I, Footnote 2 states that either an LFMD or sample duplicate may be analyzed.
Notification of acceptable corrective action (i.e., an updated benchsheet which included a LFM with an
implementation date of 4/1/2016) was received by email on 4/6/2016. No further response is necessary
for this Finding.
Comment: Sample selection for duplicate analysis is not being randomized. Only the effluent sample
was duplicated. Standard Methods, 5020 B-2011 (2) (f) states: When appropriate (Table 5020: 1),
randomly select routine samples to be analyzed twice. Process duplicate sample independently through
the entire sample preparation and analysis procedure. Notification of acceptable corrective action (i.e., a
statement that the lab is now randomly rotating duplicate samples for COD between Effluent and Influent
samples and benchsheets have been changed to reflect this matter with an implementation date of
6/8/2016) was received by email on 6/23/2016. No further response is necessary for this Finding.
Recommendation: The COD reactor's thermometer is verified annually by a thermometer in the range
of 100 'C. It is recommended to use a thermometer in the range of the temperature in use.
J. Finding: A calibration blank and calibration verification standard is not analyzed after every tenth
sample and at the end of the sample group.
Requirement: The calibration blank and calibration verification standard (mid -range) must be
analyzed initially (i.e., prior to sample analysis), after every tenth sample and at the end of each
sample group to check for carry over and calibration drift. If either fall outside established
quality control acceptance criteria, corrective action must be taken (e.g., repeating sample
determinations since the last acceptable calibration verification, repeating the initial calibration,
etc.). Ref: NC WW/GW LC Policy.
K. Finding: The calibration verification standards are being evaluated with an acceptance criteria of
±10% acceptance criteria.
Requirement: Prepare calibration curve for each new lot of tubes or ampules or when
standards prepared in 4 a above differ by > 5% from calibration curve. Ref: Standard Methods,
5220 D (4) (c).

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#131 City of Lumberton Environmental Utilities Laboratory
Comment: Due to the incorrect acceptance criteria being used, on the following dates:
January 3, 5, 10, 24 and 31, 2016 the QC standards were outside the acceptance criteria.
L. Finding: The laboratory is not analyzing five standards when verifying the instrument's factory -
set calibration.
Requirement: For analytical Procedures requiring analysis of a series of standards, the
concentrations of these standards must bracket the concentration of the samples analyzed. One
of the standards must have a concentration equal to the laboratory's lower reporting concentration
for the parameter involved. For metals by AA or ICP, a series of three standards must be
analyzed with each group of samples. For colorimetric analyses, a series of five standards for a
curve prepared annually or three standards for curves established each day or standards as set
forth in the analytical procedure must be analyzed to establish a standard curve. The curve must
be updated as set forth in the standard procedures, each time the slope changes by more than 10
percent at midrange, each time a new stock standard is prepared, or at least every twelve months.
Each analyst performing the analytical procedure must produce a standard curve. Ref: 15A NCAC
2H .0805 (a) (7) (1).
Requirement: Prepare at least five standards from potassium hydrogen phthalate solution with
COD equivalents to cover each concentration range. Ref: Standard Methods 5220 D-1997 (4) (c).
Comment: Each analyst has been analyzing three standards when verifying the instrument's
factory -set calibration.
Nitrogen, Ammonia — Standard Methods, 4500 NH3 D-1997 (Aqueous)
Comment: The laboratory was not analyzing a calibration blank and calibration verification standard
(mid -range) at the end of the sample group. Only a calibration blank is analyzed initially. The sample sets
are small therefore only need to analyze initially and at the end of the sample group. NC WW/GW LC
Policy states: The calibration blank and calibration verification standard (mid -range) must be analyzed
initially (i.e., prior to sample analysis), after every tenth sample and at the end of each sample group to
check for carry over and calibration drift. If either fall outside established quality control acceptance
criteria, corrective action must be taken (e.g., repeating sample determinations since the last
acceptable calibration verification, repeating the initial calibration, etc.). Notification of acceptable
corrective action (i.e., an updated benchsheet which includes a calibration blank and calibration
verification standard initially and at the end of the sample group, with an implementation date of
4/1/2016) was received by email on 4/9/2016. No further response is necessary for this Finding.
Comment: The volume of 10N NaOH (ISA solution) added to the samples, blanks and calibration
standards was not documented on the benchsheet. The 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. Notification of acceptable
corrective action (i.e., an updated benchsheet which included a column to document the volume of 1ON
NaOH with an implementation date of 4/1/2016) was received by email on 4/6/2016. No further
response is necessary for this Finding.
M. Finding: The laboratory is not correctly evaluating the blank against the required acceptance
criterion.
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.

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Recommendation: It is recommended that blank concentrations be documented to the same
number of decimal places as samples to demonstrate that the blank acceptance criterion is being
met. It is also recommended that the blank acceptance criterion be documented on the
benchsheet. The laboratory's reporting limit is 0.1 mg/L therefore the blank acceptance criterion
would be :50.05 mg/L. In order to make sure that the blank meets the requirements, wait until
the reading has stabilized (at least 2 to 3 minutes) before reading.
N. Finding: The difference in volume of 10N NaOH used in the samples versus the calibration
standards was not compensated for in the sample results calculation.
Requirement: The following formula must be used in the calculation:
mgNH3—N/L=AXBX 10( 0+D)
(100 + C)
A= Dilution Factor
B= Concentration of NH3-N/L, mg/L, from calibration curve
C= Volume of 10N NaOH added to the calibration standards, mL
D= Volume of 10N NaOH added to sample, mL
Ref: Standard Methods, 4500 NHs D-1997. (5).
®. Finding: The laboratory is not analyzing a Laboratory Fortified Matrix (LFM) and Laboratory
Fortified Matrix Duplicate (LFMD).
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 analyte (ideally from a second source) to a randomly selected routine sample without
increasing its volume by more than 5%. Ref: SM 4020 B-2009, Table 4020: 1 and (2) (g).
Comment: The laboratory submitted an updated benchsheet by email on 4/6/2016 with an
implementation date of 4/1/2016. The update benchsheet included space for an LFM but a space
for the LFMD was not included.
Comment: The laboratory was analyzing sample duplicates, which are not required by the
method. Analysis of the LFMD is required by the method and is acceptable to satisfy the sample
duplicate requirement listed in the North Carolina Administrative Code, 15A NCAC 2H .0805 (a)
(7) (C).
P. Finding: The distillation comparison study results were not within the acceptance criterion of
<20% RPD and no corrective action was taken.
Requirement: Samples must be spiked according to the NC WW/GW LC Matrix Spike Policy,
in duplicate, to allow for a meaningful statistical comparison. It is recommended that samples
are spiked to yield a value within the verified calibration range so that sample dilution is not
needed. Comparisons between the matrix spike and matrix spike duplicate, as well as between
distilled and undistilled samples must meet a 20% RPD acceptance criterion. Ref: NC WW/GW
Policy.
Requirement: As corrective action, analyze a minimum of 2 samples, spiked in duplicate both
with and without the distillation step (a total of 8 samples) to demonstrate that that distillation is
still not required. Submit documentation of study results with your response to this report.

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#131 City of Lumberton Environmental Utilities Laboratory
Comment: The requirements for the distillation study were revised subsequent to the
inspection. The requirements listed here reflect those revisions. Additional information can be
found in the Ammonia/Fluoride Distillation Technical Assistance document attached to this
report.
Comment: The distilled results were higher than the undistilled results for the study performed on
6/12/2015. The laboratory suspected that the study was invalid due to the use of a questionable
PT sample as the spiking solution. Based upon failure of the acceptance criterion, the distillation
study should have immediately been repeated with a reliable spiking solution or the routine
compliance samples should have all been distilled. Distillation is not required for the Ammonia
electrode method, however if a study is performed the results must meet NC WW/GW policy
requirements.
Residue, Suspended — Standard Methods, 2540 D-1997 (Aqueous)
Recommendation: It is recommended that an acceptance criterion for duplicates be split into two tiers.
The method recommends that duplicates agree within 5% of their average weight. However, low
concentration samples may need a separate low-level acceptance criterion which could be based upon
calculated recoveries or a ± mg/L criterion.
Comment: Units of measure were not documented over the "weight difference" (i.e., grams) column
and in the calculations (i.e., mLs, grams). The North Carolina Administrative Code, 15A NCAC 2H .0805
(a) (7) (H) states: All laboratories must use printed laboratory bench worksheets that include a space to
enter the signature or initials of the analyst, date of analyses, sample identification, volume of sample
analyzed, value from the measurement system, factor and final value to be reported and each time must
be recorded each time samples are analyzed. Notification of acceptable corrective action (i.e., an updated
benchsheet which included proper units of measure with an implementation date of 4/1/2016) was
received by email on 4/27/2016. No further response is necessary for this Finding.
Comment: Filters were not weighed to constant weight prior to sample analysis, nor is a dry filter blank
analyzed with each set of samples. The lab is analyzing a water blank which is not required. NC WW/GW
LC Policy states: If pre -prepared filters are not used, the method requires that filters must be weighed to
a constant weight after washing. Repeat cycle of drying, cooling, desiccating, and weighing until a
constant weight is obtained or until weight change is less than 4% of the previous weighing or 0.5 mg,
whichever is less. In lieu of this process, it is acceptable to analyze a single daily dry filter blank to fulfill
the method requirement of drying all filters to a constant weight prior to analysis. Notification of
acceptable corrective action (i.e., an updated benchsheet which included a statement, "A filter shall be
weighed and carried through with the other filters with each run and must not exceed 0.5 mg between the
initial and final weight. The filter shall be known as the Blank.", with an implementation date of 4/1/2016)
was received by email on 4/27/2016. No further response is necessary for this Finding.
Comment: The laboratory was not documenting the percent recovery of quality control standards on
laboratory benchsheets to demonstrate the analytical process is in control and the established
acceptance criteria are met. The 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 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., an updated benchsheet which included percent recovery of quality
control standards with an implementation date of 4/1/2016) was received by email on 4/27/2016. No
further response is necessary for this Finding.

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#131 City of Lumberton Environmental Utilities Laboratory
Comment: The outdated minimum weight gain criteria (1.0 mg) is being used. NC WW/GW LC Policy
states: The minimum weight gain allowed by any approved method is 2.5 mg. Choose sample volume
to yield between 2.5 and 200 mg dried residue. This establishes a minimum reporting value of 2.5 mg/L
when 1000 mL of sample is analyzed. If complete filtration takes more than 10 minutes, increase filter
diameter or decrease sample volume. In instances where the weight gain is less than the required 2.5
mg, the value must be reported as less than the appropriate value based upon the volume used. The
reporting limit of 2.5 mg/L is based on 1000 mL sample. If sample volume is less than the 1000 mL and
the dried residue obtained is less than 2.5 mg, the reporting limit will need to be adjusted. For example, if
100 mL sample is analyzed, and less than 2.5 mg of dried residue is obtained, the value reported
would be <25 mg/L. Notification of acceptable corrective action (i.e., updated benchsheet which
included a statement, "Filtered sample volume shall be sufficient to yield at least 2.5 mg of dried
residue." With an implementation date of 4/1/2016) was received by email on 4/27/2016. No further
response is necessary for this Finding.
Q. Finding: The serial number or some other form of identification of the thermometer is not
documented on the oven temperature daily log to provide linkage to the annual thermometer
calibrations. This is considered pertinent information.
Requirement: 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. Ref: 15A
NCAC 2H .0805 (a) (7).
R. Finding: Samples chosen to be duplicated are not being randomly selected.
Requirement: When appropriate (Table 2020: II), randomly select routine samples to be
analyzed twice. Independently prepare and analyze duplicate samples. Ref: SM 2020 B-2011.
(2) (fl•
Comment: The effluent is always duplicated.
Residue, Total — Standard Methods, 2540 B-1997 (Aqueous)
Comment: No compliance samples are being reported. The laboratory is only analyzing samples for
process control but would like to retain certification.
pH —Standard Methods, 4500 H+13-2000 (Aqueous)
Comment: Values were reported that exceed the method specified accuracy of 0.1 units. Sample
results were reported to two decimal places. Standard Methods, 4500 H+ B-2000. (6) states: By careful
use of a laboratory pH meter with good electrodes, a precision of ±0.02 unit and an accuracy of ±0.05
unit can be achieved. However, ± 0.1 pH unit represents the limit of accuracy under normal conditions,
especially for measurement of water and poorly buffered solutions. For this reason, report pH values to
the nearest 0.1 pH unit. Notification of acceptable corrective action (i.e., an updated benchsheet which
included a statement on the bottom "pH shall be reported to 1 decimal place on the daily bench sheets
and on the DMR's." with an implementation date of 4/1/2016) was received by email on 4/6/2016. No
further response is necessary for this Finding.
Comment: The pH meter calibration log sheet did not contain all of the necessary labeling information.
No units of measure (i.e., s.u.) were associated with the buffers on the calibration log sheet. The North
Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (H) states: All laboratories must use printed
laboratory bench worksheets that include a space to enter the signature or initials of the analyst, date of

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#131 City of Lumberton Environmental Utilities Laboratory
analyses, sample identification, volume of sample analyzed, value from the measurement system, factor
and final value to be reported and each time must be recorded each time samples are analyzed.
Notification of acceptable corrective action (i.e., updated pH meter calibration log sheet which included
proper units of measure for buffers with an implementation date of 4/1/2016) was received by email on
4/27/16. No further response is necessary for this Finding.
Comment: The pH meter calibration log sheet used for pretreatment samples, did not contain all of the
necessary labeling information. No units of measure are associated with some of the data values listed on
the calibration log sheet. The North Carolina Administrative Code, 15A NCAC 2H .0805 (7) (H) states: All
laboratories must use printed laboratory bench worksheets that include a space to enter the signature
or initials of the analyst, date of analyses, sample identification, volume of sample analyzed, value from
the measurement system, factor and final value to be reported and each item must be recorded each
time samples are analyzed. Notification of acceptable corrective action (i.e., updated pH meter
calibration log sheet which included proper units of measure for pH with an implementation date of
4/1/2016) was received by email on 4/27/16. No further response is necessary for this Finding.
Comment: For pretreatment samples, instances were observed where the pH 10.0 calibration check
buffer exceeded ± 0.1 SU from the true value and no corrective action was taken. The NC WW/GW LC
Approved Procedure for the Analysis of pH states: For routine work, use a pH meter accurate and
reproducible to 0.1 pH unit with a range of 0 to 14, equipped with a temperature compensation device.
Follow all manufacturers' recommendations for the calibration of the meter each analysis day. In all
cases, the meter must be calibrated with at least two buffers. The calibration; however, must bracket
the range of the samples being analyzed. Notification of acceptable corrective action (i.e., updated pH
Meter Calibration Log that included a statement, "Recalibrate meter if Check Standard is not within its
respective limits of 9.9 -10.1 SU", with an implementation date of 5/13/2016) was received by email on
5/13/2016. No further response is necessary for this Finding.
Comment: For pretreatment samples, instrument identification is not documented on the calibration log
to link it to the benchsheet. The laboratory has two meters. One is solely used in the field and the other is
used on the bench. The instrument identification needs to be on the calibration log to link the instrument
to the samples analyzed by that instrument. The NC WW/GW LC Approved Procedure for the Analysis
of pH documents states: The following must be documented in indelible ink whenever sample analysis is
performed: Instrument identification. Notification of acceptable corrective action (i.e., revised calibration
log that includes instrument identification with an implementation date of 4/1/2016) was received by
email on 4/27/2016. No further response is necessary for this Finding.
Temperature — Standard Methods, 2550 B-2000 (Aqueous)
Dissolved Ongen — Standard Methods, 4500 O G-2001 (Aqueous)
S. Finding: All original records were not maintained.
Requirement: Data pertinent to each analysis must be maintained for five years. Ref: 15A NCAC
2H .0805 (g) (1).
Comment: The testing data is initially written on a piece of paper, transported back to the
laboratory and transferred to the field benchsheet. This original paperwork is then discarded. All
analytical records, including original observations, must be retained so as to facilitate historical
reconstruction of the reported results.

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#131 City of Lumberton Environmental Utilities Laboratory
Conductivity —Standard Methods, 2510 R-1997 (Aqueous)
Comment: The incorrect value was documented for the calibration standard on the calibration log.
The value documented was 1413 limhos/cm instead of 1408.8 pmhos/cm. The NC WW/GW LC
Approved Procedure for the Analysis of Specific Conductance (Conductivity) states: The following must
be documented in indelible ink whenever sample analysis is performed: True value of the calibration
verification check standard. Notification of acceptable corrective action (i.e., updated calibration log which
included the correct calibration standard value of 1408.8 Nmhos/cm with an implementation date of
4/1/2016) was received by email on 4/6/2016. No further response is necessary for this Finding.
T. Finding: The acceptance criterion used for the calibration check standards is ± 25%.
Requirement: 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 LC Approved
Procedure for the Analysis of Specific Conductance.
Comment: The laboratory is analyzing a 10, 100, 1000 and 10,000 Nmhos/cm for the
calibration check standards with an acceptance criterion of ± 25%. Most of the samples are in
the range of 1,000 Nmhos/cm standard. Some of the standards exceeded the required
acceptance criteria of ± 10%.
Comment: An updated calibration log was submitted on 4/6/2016 with the 1000 limhos/cm and
10,000 Nmhos/cm standards used as the calibration verification standards but the acceptance
criteria was documented as ± 25%.
U. Finding: The Automatic Temperature Compensator (ATC) has not been verified.
Requirement: The ATC must be verified annually (i.e., every twelve months) and the process
documented. The ATC must be verified by analyzing a standard at 25 °C (the temperature that
conductivity values are compensated to) and a temperature(s) that brackets the temperature
ranges of the samples to be analyzed. This may require the analysis of a third temperature
reading that is > 25 'C. Ref: NC WW/GW LC Approved Procedure for the Analysis of Specific
Conductance (Conductivity).
Comment: 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.
Comment: At the time of the inspection, a copy of the Approved Procedure for the Analysis of
Specific Conductance (Conductivity) was provided that includes directions on how to verify the
ATC.
IV. PAPER TRAIL INVESTIGATION:
The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks, etc.)
and Discharge Monitoring Reports (DMRs) submitted to the North Carolina Division of Water
Resources. Data was reviewed for City of Lumberton Environmental Utilities Laboratory (NPDES #
NC0024571) for the months of December 2015, January and February 2016. COD data were
reviewed for Pre-treatment for International Paper for January 1, 2016 and City of Lumberton
Environmental Utilities Laboratory for January 2016. No transcription errors were detected. The facility
appears to be doing a good job accurately transcribing data.

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#131 City of Lumberton Environmental Utilities Laboratory
V. CONCLUSIONS:
Correcting the above -cited Findings and implementing the recommendations will help this lab to produce
quality data and meet Certification requirements. The inspector would like to thank the staff for its
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: Tonja Springer Date: April 28, 2016
Report reviewed by: Jason Smith Date: May 12, 2016

AMMONIA/FLUORIDE DISTILLATION TECHNICAL ASSISTANCE (5/31/2016)
Background
40 CFR Part 136.3, Table IB — List of Approved Inorganic Test Procedures, requires manual distillation or gas
diffusion (pH>11) followed by any of the approved reference methods for Ammonia Nitrogen and manual
distillation followed by any of the approved reference methods for Fluoride analyses. This requirement is
footnoted.
Footnote 6 reads:
Manual distillation is not required if comparability data on representative effluent samples are on file to show
that this preliminary distillation step is not necessary; however, manual distillation will be required to resolve
any controversies. In general, the analytical method should be consulted regarding the need for distillation. If
the method is not clear, the laboratory may compare a minimum of 9 different sample matrices to evaluate the
need for distillation. For each matrix, a matrix spike and matrix spike duplicate are analyzed both with and
without the distillation step. (A total of 36 samples, assuming 9 matrices). If results are comparable, the
laboratory may dispense with the distillation step for future analysis. Comparable is defined as <20% RPD for
all tested matrices). Alternatively, the two populations of spike recovery percentages may be compared using
a recognized statistical test.
Ammonia/Fluoride Distillation (NC WW/GW LC Policy 05/31/2016)
It is the responsibility of the permittee to ensure that monitoring is conducted according to test procedures
approved under 40 CFR Part 136 even if the permittee does not operate the laboratory that performs the
analytical testing on the waste stream. In terms of Ammonia Nitrogen and Fluoride monitoring, this means that
the permittee must ensure that their effluent is appropriately characterized as to whether distillation is required.
Methods that specifically state that distillation is not required may only require distillation to resolve
controversies. Additionally, manual distillation may not be required if comparability data on representative
effluent samples are on file to show that this preliminary distillation step is not necessary; however, manual
distillation will be required to resolve any controversies. A comparison study may be performed in-house or
contracted to another certified laboratory. Permittees that do not perform the analyses in-house, and contract
the analyses or the distillation study to a NC WW/GW LC certified commercial laboratory must obtain a copy
of the initial comparison data and all subsequent comparison data, keep it on file at their facility and make
these records available to the Department upon request.
Samples must be spiked according to the NC WW/GW LC Matrix Spike Policy, in duplicate, to allow for a
meaningful statistical comparison. It is recommended that samples are spiked to yield a value within the
verified calibration range so that sample dilution is not needed. Comparisons between the matrix spike and
matrix spike duplicate, as well as between distilled and undistilled samples must meet a 20% RPD acceptance
criterion. Both the distilled and undistilled samples must be analyzed using the same method technology used
to report compliance data for the permitted facility. It is recommended that both the distilled and undistilled
portions of the sample be analyzed by the same laboratory. Per 15A NCAC 2H .0805 (e) (2), it would be
permissible to have a contract lab distill the samples and send the distillates back to the permittee for analysis
within the prescribed holding time. It is the responsibility of the permittee to ensure that when only the
distillation portion is contracted, that samples are distilled into the proper receiving solution required by the
analytical method to be used. That means when the titration method will be employed, samples must be
distilled into a boric acid solution. When the phenate method will be employed, samples must be distilled into a
sulfuric acid solution.
The following frequencies are required:
Initially, compare a minimum of 9 samples, spiked in duplicate, both with and without the distillation step (a
total of 36 samples), to evaluate the need for distillation.

Subsequently each year analyze a minimum of 2 samples, spiked in duplicate, approximately 6 months apart,
both with and without the distillation step (a total of 8 samples). If effluent characteristics change (e.g.,
contributing industries are added or lost, major change in plant processes, etc.), or if the laboratory changes to
another analytical method that requires the comparison, a minimum of two additional samples must be spiked
in duplicate and analyzed, both with and without the distillation step, to demonstrate that that distillation is still
not required.
Refer to the tables below to determine if distillation studies are allowed. NOTE: By following the previous NC
WW/GW LC Ammonia/Fluoride Distillation Studies policy, a laboratory may have historical data on file that
meets these requirements.
Ref: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) Policy, 05/31/2016;
based upon Code of Federal Regulations, Title 40, Part 136.3; Federal Register Vol. 77, No. 97, May 18,
2012: Table IB, Footnote 6.
TABLE 1: Ammonia Nitrogen Methods
Ammonia Nitrogen
Distillation
Study
Method
Required
Allowed
Comment
The distillation study option is not allowed. All
SM 4500 NH3 C-1997
samples must be distilled. Method states in
(Titration)
Yes
No
Section (1): The titrimetric method is used only
on samples that have been carried through
preliminary distillation.
SM 4500 NH3 D-1997
No
N/A
Method states in Section (1) (b): Sample
(Electrode)
distillation is unnecessary.
SM 4500 NH3 E-1997
No
N/A
Method refers you SM 4500 NH3 D 1., which
(Electrode)
states that sample distillation is unnecessary.
SM 4500 NH3 F-1997
Method states in Section (1) (b): Remove
(Manual Phenate)
Yes
Yes
interfering turbidity by distillation or filtration.
SM 4500 NH3 G-1997
(Automated Phenate)
Yes
Yes
SM 4500 NH3 H-1997
(Automated Phenate)
Yes
Yes
Method states in Section 2.1: The sample is
EPA 350.1, Rev. 2.0
buffered at a pH of 9.5 with a borate buffer in
(1993)
Yes
Yes
order to decrease hydrolysis of cyanates and
(Automated Phenate)
organic nitrogen compounds, and is distilled into
a solution of boric acid.
ASTM D1426-08 (A)
(Nesslerization)
Yes
Yes
ASTM D1426-08 (B)
(Electrode)
Yes
Yes
Method states in Section 2.1: Ammonia is distilled
USGS 1-3520-85
Yes
No
from the buffered solution, and an aliquot of the
(Nesslerization)
distillate then is nesslerized.
USGS 1-4523-85
(Automated Phenate)
Yes
Yes
* For requirements of methods not listed, contact us.
TABLE 2: Fluoride Methods

Fluoride Method
Distillation
Study
Comments
Required
Allowed
SM 4500-F- C-1997
Refer to Table 4500E-:I for interferences that may
(Electrode, Manual)
Maybe
y
Yes
require distillation.
Refer to Table 4500E-:I for interferences that may
require distillation. Method states in Section (1) (b):
whenever any one substance is present in sufficient
SM 4500-F- D-1997
Maybe
Yes
quantity to produce an error of 0.1 mg/L or
(Colorimetric)
whenever the total interfering effect is in doubt,
distill the sample. Also distill colored or turbid
samples.
Distillation is performed inline with the automated
method setup. Method states in Section (1) (b):
SM 4500-F- E-1997
Yes
No
Interferences normally associated with the
(Automated Complexone)
determination of fluoride are removed by
distillation.
SM 4110-F- B-2000
(Ion Chromatography)
Yes
Yes
SM 4110-F- C-2000
(Ion Chromatography)
Yes
Yes
SM 4140 B-1997
Yes
Yes
(CIE/UV)
EPA 300.0, Rev. 2.1 (1993)
(Ion Chromatography)
Yes
Yes
EPA 300.1, Rev. 1.0 (1997)
(Ion Chromatography)
Yes
Yes
ASTM D1179-04 (B)
No laboratories currently certified by this method.
(Electrode, Manual)
Yes
Yes
Standard has not been purchased.
ASTM D1179-04 (A)
No laboratories currently certified by this method.
(Colorimetric)
Yes
Yes
Standard has not been purchased.
Method states in Section 2.3: The method includes
USGS 1-4327-85
a distillation step to decompose organic fluoride
(Electrode, Automated)
Yes
Yes
compounds and attack minerals such as fluorspar in
water suspended sediment.
* For requirements of methods not listed, contact us.