NC0043176_Lab Certification_20071005

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October 5, 2007
115
Ms. Jessica Teague
Dunn Black River VV NTP Lab.
P.O. Box 1065
Dunn, NC 28335
Michael F. Easley, Governor
William G. Ross Jr., Secretary
North Carolina Department of Environment and Natural Resources
SUBJECT: Laboratory Certification Maintenance Inspection
Dear Ms. Teague :
Coleen H. Sullins, Director
Division of Water Quality
DENR_FRO
OCT ,1 O 2007
DWQ
Enclosed is a report for the inspection performed on August 30, 2007 by Mr. Jeff
Adams. 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. 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 questionsor need additional information, please
contact us at 919-733-3908.
Sincerely,
Dana Satterwhite
Certification Unit Supervisor
Laboratory Section
Enclosure
cc: Jeff Adams
Fayetteville Regional Office
NorthCarolina
Naturally
North Carolina Division of Water Quality 1623 Mail Service Center Raleigh, NC 27699-1623 Phone [phone] Customer Service
Internet: www.dwglab.org Location: 4405 Reedy Creek Rd Raleigh, NC 27607 . Fax [phone]
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On -Site Inspection Report
LABORATORY NAME:. Dunn Black River WWTP Laboratory
NPDES PERMIT-# NC0443176
ADDRESS: P.O Box 1065
Dunn, NC 28335
CERTIFICATE 115
DATE OF INSPECTION: August 30, 2007
TYPE OF INSPECTION: Municipal Maintenance
AUDITOR(S): Jeffrey R: Adams .
LOCAL PERSON'(s) CONTACTED: Donrie-Dukes and Jessica Teague
1. INTRODUCTION:
This laboratory was inspected to verify its compliance with the requirements of 15A NCAC 2H .0800 for
the analysis of environmental samples.
II. GENERAL COMMENTS:
The inspection consisted of reviewing data for NPDES compliance. The staff is congratulated for doing
a good job of maintaining the laboratory certification program. The laboratory is spacious and well
equipped. All facilities and equipment are well. maintained. Records. are well kept but some further
quality control procedures need to be implemented.
Comment: For all benchsh'eets,'it .is recommended that the lab indicate which edition of the method is
being referenced. This will aid the analysts, when method changesare promulgated by EPA, to
maintain adequate documentation of their data.
Comment: The laboratory is no longer performing the analyses for BOD, COD, TKN, NO2 + NO3 and
these parameters are currently being contracted out 'to a commercial laboratory for analysis. The
laboratory also has Specific Conductance. -on its certificate but is not required on its discharge permit.
Recommendation: It is recommended that since the laboratory is no longer analyzing the above stated
parameters that these parameters (including conductivity) be removed fromits certificate.
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS':
General Laboratory
' A. Finding: The analytical calibration weights were over 5 years old and need to be checked against
certified weights.
Requirement: Certified analytical weights, Class S, 1 or 2, must be recalibrated and recertified a
minimum of every 5 years. Ref: NC Wastewater/Groundwater Laboratory Certification . (NC
WW/GW LC) Policy.
Finding: The NIST thermometer (ERTCO S/N #5337) certification has expired. The certificate
listed a certification date of 5/25/95. This exceeds the 5 year period ending 5/25/2000.

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#115 Dunn Black River WWTP Laboratory
Requirement: NIST certified thermometers must be recertified, at a minimum, every five years.
NIST traceable thermometers must be recalibrated Within its expiration date. A new certificate
must be issued and maintained for inspection upon request. Ref:, NC Wastewater/Groundwater
Laboratory Certification Policy Statement February 2006.
Comment: The laboratory has another in-house NISI certified thermometer (Apple Scientific,
S/N 1998-ZZ2) that can be used for future NIST temperature sensor checks. This thermometer
was certified on 4/04/05. -
C. Finding: Some chemicals were used after the expiration date.
Requirement: Some standardized solutions alter slowly because of chemical or biological
changes. The practical life, required frequency of standardization, or storage precautions are
indicated for such standards. A laboratory should not consider a solution valid once the
practical life or expiration date has passed. Ref: Standard Methods 18th Edition - Method 1070
C p1-26.
Recommendation: It is recommended that the laboratory establish a -policy for disposal of
chemicals which do not have expiration dates assigned by the manufacturer.
Dissolved Oxygen (DO) - Standard Methods, 18th Edition, 4500 0 G
Comment: The laboratory is using a'YSI-52 meter to measure the DO of its effluent stream. The --
DO probe storage well was dirty. This can affect the membrane and promote algae growth, which
could -affect accurate calibration and measurement. =
Recommendation: It is recommended that the laboratory follow the manufacturer's instructions
on the proper cleaning and maintenance of the probe and to change the sponge and clean the
storage bottle at, least weekly. It is also recommended, to encourage the operator(s) to thoroughly ---
rinse the probe between samples and after each use and before placing into storage well.
Fecal Coliform - Standard Methods, 18th Edition, 9222D (MF)
Comment: The laboratory is recording the incubator temperatures on the bench sheets .but is .not
recording in a daily log book.
Recommendation: It is recommended that the laboratory maintain a daily log book for
recording the Fecal Coliform incubator temperatures. This will enable the laboratory to more
closely monitor any temperature changes that may occur and take preemptive corrective action
measures as required.
D. Finding: The laboratory is not checking and recording the pH of the MFC broth each time it is
prepared.
Requirement: "Check pH of a portionof each medium after sterilization and cooling." Ref:
Standard Methods 18th Edition; Method 9020 B. 3. h. Culture media: Page 9-9. "Final pH should
be 7.4." Standard Methods 18th Edition; Method 9222 D. 1. a.
E. , Finding: Thelaboratory is not calculating precision on its duplicate analyses.

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#115 Dunn Black River WWTP Laboratory
Requirement: Calculate precision of duplicate analyses for each different type of sample
examined, for example, drinking water, ambient water, wastewater, etc., ... Ref: Standard
Methods 18th Edition, pg. 9-10, 5b,.
Temperature - Standard Methods, 18th Edition, 2550B
F. Finding: The laboratory is bringing, the sample back to the lab for the effluent sample
temperature measurement.
Requirement: All temperature measures must be taken immediately i.e., at the site of collection.
The Federal Register states the maximum holding' time as "analyzed" which is defined by our
program as "in situ". Ref: 40CFR Vol. 72, March 12, 2007 Table II.
Comment: If the sample is being collected from a location that makes in -stream analysis
impractical such as .a manhole or from' a high traffic highway over pass, then analyze the sample
as quickly as possible after collection. A footnote or cover statement should be included in the log
or on the bench sheet. For Example: The temperature sample point is in a high traffic area. For
safety reasons, samples are collected then analyzed on a road shoulder about 50 yards from the
collection point. If this is a permanent situation, the cover statement can be recorded in the front of
the analysis book, or printed on the bench sheet. It need not be written every time a sample is
analyzed.
Total Residual Chlorine - Standard Methods, 18th Edition, 4500 CI G.
Comment: The laboratory is using a HACH DR4000 spectrophotometer using the pre-
programmed analytical number 1460 for, Total Residual Chlorine. The laboratory is analyzing the
total residual chlorine of its effluent in mg/L and reporting results on the DMR in pg/L. The
standards beingused to verify the calibration curve are 0.02, 0.025, 0.50, 0.75 and 1.00 mg/L
Total Residual Chlorine. The laboratory appears to be reporting its data correctly, within the
required permit limit of 28pg/L. The concentrations of the calibration curve verification standards
are much too high for the required ultra -low level analytical range. When converted to pg/L these
concentrations are 20, 25, 500, 750 and 1000 pg/L total residual chlorine, far exceeding the
recommended ultra -low level calibration curve and the ultra low level dynamic range of the
instrument.
Recommendation: It is recommended that in order to analyze within the ultra -low level range
that the laboratory use program ULR 1490 for its ultra -low level chlorine analyses. It is also
recommended using the following concentrations in verifying the ultra -low level curve: 20, 50, 100,
200 and 400 pg/L and using a 200 pg/L_ midrange check or continuing calibration verification
(CCV) standard and a 40 or 50 pg/L second source laboratory control standard (LCS). These
concentrations will be much closer to the true analytical range of the samples and the dynamic
range of the instrument. Instructions on the preparation of the ultra -low level curve are attached.
G. Finding: The laboratory is not, making corrections , to the data''(in an ''approved manner. The
laboratory is writing over data results. • •
Requirement: If a mistake is made in data recording, the mistake must be corrected by
making asingle, line through the incorrect entry so it remains legible, recording the correct entry'
beside the mistake, and initialing and dating the error correction. Ref: SW 846 Sept 1994 Test
Methods for Evaluating Wastes, Chapter 1, pg. 13.

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#115 Dunn Black River WWTP Laboratory
IV. PAPER TRAIL INVESTIGATION:
A paper trail consisted of comparing laboratory bench. data and contracted data of several parameters
with monthly Discharge Monitoring Report (DMR) reports for November and December, 2006 and
January, March, May and July, 2007. The following error was noted:
Date
Parameter
Location
Value on Benchsheet
Value on DMR
11/07/06
Dissolved Oxygen
Effluent
7.67 mg/L
7.68 mg/L
In order to avoid questions of legality, it is recommended that an amended DMR be submitted to this
Division.
It appears the facility is doing a good job of accurately transcribing data.
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
their assistance in the inspection and data review process. Please respond to all findings.
Report prepared by: Jeffrey R. Adams . Date: September 19, 2007
Report reviewed by: Todd Crawford Date: September 20, 2007

TOTAL RESIDUAL CHLORINE CURVE PREPARATION
Prepare a stock solution by adding 891 mg KMnO4 (potassium permanganate) to a 1 liter volumetric
flask. Dissolve and dilute to 1 liter with distilled or,deionized water. Prepare the stock solution fresh
daily.
Dilute 10 mL of stock solution to 100 ml, with DI or distilled water in a volumetric flask. This is the
Intermediate standard.
Dilute 1 mL of the Intermediate standard to 100 mL with DI or distilled water. A chlorine equivalent
of 1.00 mg/L will be produced in the DPD reaction. This is the Working standard.
From this Working standard you will make up your annual curve.
Since your permit limit is 28pg/L, I would recommend a lower reporting limit of 20 pg/L and the top of
your curve at 400 pg/L.
Take 40 mL of working standard to 100 mL with distilled water in a volumetric flask.
This is your 400 pg/L standard.
Take 20 mL of working standard to 100 mL with distilled water in a volumetric flask.
This is your 200 pg/L standard.
Take 10 mL of working standard to 100 mL with distilled water in a volumetric flask.
This is your 100 pg/L standard.
Take 5 mL of working,standard to 100 mL with distilled water in a volumetric flask.
This is your.50 pg1L standard. _..
Take 2 mL of working standard to 100 mL with distilled water in a volumetric flask.
This is your 20 pg/L standard.
The concentrations stated are just recommendations and you can choose the curve points and the
range you choose to cover. Just remember this, you have to have a standard below your permitted limit
of 28 pg/L and anything that is above your highest standard must be diluted into range.