NC0043176_Lab Certification Maintenance_20010822

Michael F. Easley, Governor rJ L
William G. Ross Jr., Secretary [J
North Carolina Department of Environment and Natural Resources j .—
Gregory J. Thorpe, Ph.D. DR!?
Acting Director
Division of Water Quality
August 22, 2001
115
Mr. Mark Brantley
Dunn Black River WWTP Lab.
r--1
P.O. Box 1065
Susan Tart -Road
Dunn, NC 28335
SUBJECT: Laboratory Certification Maintenance Inspection
Dear Mr. Brantley:
AUG 2 4 2001
Enclosed is a report for the inspection performed on August 14, 2001 by Mr.
Frederick L. Bone. Within thirty days, please supply this office with a written item for item
description of how these deficiencies were corrected. A response is not required for
comments or recommendations unless specifically requested. If the deficiencies cited
in the enclosed report are not corrected, enforcement actions will be recommended. For
certification maintenance, your laboratory must continue to carry out the requirements set
forth in 15A NCAC for 2H .0800.
Copies of the checklists completed during the inspection may be requested from
this office. Thank you for your cooperation during the inspection. Please contact us at
919-733-3908, if you have questions or need additional information.
Enclosure
cc: Frederick L. Bone
Fayetteville Regional Office
Sincerely,
ap.",,,
James W. Meyer
Laboratory Section
Laboratory Section N. C. Division of Water Quality 1623 Mail Service Center
FAX: [phone] Internet: www.esb.enr.state.nc.us/lab
Raleigh, NC 27699-1623
NCDENR
[phone]

On -Site Inspection Report
LABORATORY NAME: Dunn Black River \MNTP
ADDRESS:
P.O. Box1065
Susan Tart Road
Dunn, NC 28335
CERTIFICATE NO: 115
DATE OF INSPECTION: August 16, 2001
TYPE OF INSPECTION: Maintenance
EVALUATOR: Frederick L. Bone
LOCAL PERSON(S) CONTACTED: Mark Brantley
I. 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 laboratory is spacious and well equipped. All facilities and equipment are well maintained. Records are
well kept and most data looked good. Some further quality control procedures need to be implemented.
III. DEFICIENCIES, RECOMMENDATIONS, REQUIREMENTS, AND COMMENTS:
General:
A. COMMENT: The laboratory Togs for the preparation of standards and reagents does not contain all of
the necessary information for the laboratory to be able too precisely document how each standard and
reagent was prepared.
REQUIREMENT: The laboratory must have a written record of all standards and reagents on file for a
period of at least three years. A standard and reagent logbook will help the laboratory to meet this
requirement. A complete standard logbook enables the laboratory to document exactly when, by whom,
and how each standard or reagent was prepared.
B. COMMENT: The thermometer in the drying oven is currently reading the internal air temperature and
not the sample matrix temperature.
RECOMMENDATION: The thermometer in the drying oven should be placed in a beaker of sand or other
solid matrix. This ensures that the proper matrix temperature is measured as well as providing a more
stable temperature environment for the thermometer readings.

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C. COMMENT: Some of the daily logs and benchsheets used by the laboratory, do not contain all of the
necessary labeling information. No units of measure are associated with some of the data values listed in
the logbooks and benchsheets.
REQUIREMENT: The laboratory should review all of their bench sheets and log booksto make sure that
every entry is marked with the appropriate unit of measure. Every number recorded on a benchsheet or
logbook must have an appropriate unit assigned to it.
D. COMMENT: The laboratory is not analyzing a second source QC standard daily.
REQUIREMENT: Analyze one known standard in addition to calibration standards each day samples are
analyzed to document accuracy. This LCS (laboratory control standard) must be from a second source.
For held curves for colorimetric methods, it must be analyzed after the initial CCV (continuing calibration
verification standard) is analyzed. It is recommended that this laboratory control standard, like the CCV,
have a mid -range concentration and not vary by more than ± 10%. If it does, the analysis is out of control.
The analysis must be terminated and the problem corrected. Ref: 15A NCAC 2H .0805 (a) (7) (B), (F),
and Standard Methods, 18th Edition - Method 1020 B.3.
Fecal Coliform:
E. COMMENT: The majority of the samples analyzed in the laboratory have "0" (zero) colony counts.
RECOMMENDATION: The laboratory has few samples that yield plate counts in the 20 - 60 range. A
culture positive sample should be analyzed as a quality control measure to ensure that positive samples
are counted and reported properly.
F. COMMENT: The laboratory includes values from dilutions that do not meet the 20-60 colonies per plate
method criteria. The laboratory analyzes a 100ml-sample volume. Data should be reported from the 100m1
sample unless it is outside of the desired counting range or other dilutions yield results in the accepted
range. All results that meet the method acceptance criteria must be averaged to obtain a final value to be
reported.
Note: The only time that a laboratory may report data as < 1 colony/ 100m1 is if a whole volume 100 ml
sample is analyzed. All other data must either meet the 20 — 60 colony . count rule or be qualified and
reported as an' estimated value.
REQUIREMENT: Compute the density from the sample quantities that produced MF counts within the
desired range of 20 to 60 fecal coliform colonies. Ref: Standard Methods, 18th Edition 9222D. (3) p. 9-61.
Total Suspended Solids:
G. COMMENT: The laboratory lists process control samples on the same benchsheet as the reportable
data. Some of the process control data does not meet the requirements of the cited methodology.
RECOMMENDATION: The laboratory must either clearly label all non -certified work on the laboratory
benchsheet or have separate benchsheets for process control (non -certified) and reportable (certified)
data. This will allow the laboratory to demonstrate that all data used for reporting purposes has meet all
method requirements.

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BOD:
H. COMMENT: The laboratory is not analyzing a seeded blank daily.
RECOMMENDATION: It is strongly recommended that the laboratory analyze a seeded blank daily. The
results of this blank should closely approximate (within 0.2 mg/L ) the seed correction factor.
COD:
I. COMMENT: The laboratory has not analyzed a HACH low range'(1-150mg/L) COD curve. Samples are
routinely reported in the low region of a HACH high range curve. This curve has a calibration range of 10
—1000 mg/L.
REQUIREMENT: The laboratory must analyze the HACH low -range curve (1 - 150 mg/L).
The COD vials that bracket the range of the samples analyzed must be used for sample reporting.
Note: When the analytical curves are adjusted, the mid -point check standards must be adjusted as well.
As was discussed at the time of the audit the mid -range is to be defined as one half the concentration of
the high standard. The mid -range check standard must be prepared from the same stock standards as the
analytical curve. A second source laboratory control standard (LCS) must be analyzed in addition to the
mid -range check standard daily. A second source LCS sample does not constitute daily mid -range
verification.
Residual Chlorine:
1. DEFICIENCY: The laboratory is not analyzing a blank daily for the residual chorine analysis.
REQUIREMENT: Analyze reagent blanks whenever new reagents are used and as often as required in
specific methods: Analyze a minimum of 5% of the sample load as reagent blanks; this monitors purity of
reagents and the overall procedural blank. Analyze a reagent blank after any sample with a concentration
greater than that of the highest standard or that might result in carryover from one sample to the next. Ref:
Standard Methods 18th Edition 1020B Quality Control (4) p 1-5.
2. DEFICIENCY: The laboratory is not analyzing any duplicate samples.
REQUIREMENT: Excluding oil and grease, 10% of all samples must be analyzed in duplicate. Ref: 15A
NCAC 2H .0805 (a) (7) (C).
3. DEFICIENCY: Each analyst that performs analysis of Residual Chlorine samples must produce a
standard curve on an annual basis. Currently the back-up operator that analyzes samples in the absence
of the laboratory chemist does not have an analytical curve on file.
REQUIREMENT: Each analyst performing the analytical procedure must produce a standard curve. Ref:
15A NCAC 2H .0800 (a) (7) (I).
J. COMMENT: The laboratory does not list the acceptance ranges of quality control samples on the
benchsheets.

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RECOMMENDATION: It is strongly recommended that the laboratory list the acceptance ranges for each
quality control sample on the bench sheet. This will enable the analyst to be able to compare the
analytical result to the acceptable range in a timely fashion. If the sample is out of the acceptable range, it
can then be reanalyzed immediately and within all holding times.
Ammonia:
K. COMMENT: The ammonia samples analyzed in the laboratory are normally in the lower region of the
analytical curve for ammonia. Currently the laboratory analyzes standards at 0.1, 1.0, and 100mg/L.
RECOMMENDATION: It is strongly recommended that that the laboratory shorten the analytical curve for
ammonia. This will increase the sensitivity of the ammonia curve. It will also allow samples to be more
closely bracketed by standards. The laboratory may consider analyzing two separate analytical curves for
ammonia. Curve 1: standards at 0.1, 0.5and 1.0 mg/L. Curve 2: Standards at 1.0, 10 and 20mg/L.
Note: When the analytical curves are adjusted, the mid -point check standards must be adjusted as well.
As was discussed at the time of the audit the mid -range is to be defined as one half the concentration of
the high standard. The mid -range check standard must be prepared from the same stock standards as the
analytical curve. A second source laboratory control standard (LCS) must be analyzed in addition to the
mid -range check standard daily. A second source .LCS sample does not constitute daily mid -range
verification.
TKN and NO2+NO3
Note: The laboratory is currently using a commercial facility to analyze these parameters. No data for
these analytes has been generated since December 2000.
IV. PAPER TRAIL INVESTIGATION:
This consisted of comparing data reported on DMR's submitted to this Division with the values obtained on
laboratory bench worksheets. Data reviewed for the months of January, March, and May 2001 indicated no
problems in proper data reporting.
V. CONCLUSIONS:
Correcting the above deficiencies and comments should help them to produce quality data and meet
certification requirements.
Please respond to all numbered Deficiencies and lettered Comments cited in this report.
Report prepared by: Frederick L. Bone Date: August 20, 2001