NC0037508_Lab Certification Inspection_20010829

bc: WA 7z-R Michael F. Easley, Governor
William G. Ross Jr., Secretary
QG North Carolina Department of Environment and Natural Resources
rGregory J. Thorpe, Ph.D.
—I Acting Director
K Division of Water Quality J
(C1C_
IDL'
August 29, 2001
134
Ms. Lillian Stephens
Moore Co. Water Pollution
P.O. Box 813
1060 Addor Road
Pinebluff, NC 28373
SUBJECT: Laboratory Certification Maintenance Inspection
Dear Ms. Stephens:
AUG 3 0 2001
Enclosed is a report for the inspection performed on August 23, 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.
Sincerely,
James W. Meyer
Laboratory Section
Enclosure
cc: Frederick L. Bone
Fayetteville Regional Office
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
1.4.471
NCDENR
[phone]

On -Site Inspection Report
LABORATORY NAME:
ADDRESS:
Moore Co. Water Pollution
P.O. Box 813
1060_Addor Road
Pinebluff, NC 28373
CERTIFICATE NO: 134
DATE OF INSPECTION: August 23, 2001
TYPE OF INSPECTION: Maintenance
EVALUATOR: Frederick L. Bone
LOCAL PERSON(S) CONTACTED: Lillian Stevens and Alvin Simpson
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:
1. DEFICIENCY: The laboratory is not performing and documenting sufficient quality control
for it's duplicate sample analysis. The laboratory must calculate either the relative percent
difference, or the absolute difference for each duplicate pair analyzed. This value is then used
to establish control charts or other appropriate acceptance criteria. This type of data is
necessary to demonstrate that the data is within acceptable control limits. The %RPD must be
listed on the inorganicbench sheets so that the analyst will be able to immediately confirm
whether ornot the data falls within acceptable limits:
REQUIREMENT: Any time quality control results indicate an analytical problem, the problem
must be resolved, and any samples involved must be rerun if the holding time has not expired.
Ref: 15A NCAC 2H .0805 (a) (7) (f).
2. DEFICIENCY: The laboratory is not analyzing a second source QC standard daily.

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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.
3. DEFICIENCY: The laboratory is using a temperaturerange of 1-5°C for sample and reagent
refrigerators.
REQUIREMENT: The acceptable temperature range of samples during storage and for stored
sample extracts, is 1.0 - 4.4°C. Ref: Federal Register, July 1, 1995; 40 CFR 136; Table II.
Required Containers, Preservation Techniques, and Holding Times. EPA letters of January and
February 1995.
4. DEFICIENCY: The laboratory is not counting the membrane filters under a 10X microscope.
REQUIREMENT: Count colonies with a low -power (10-15 magnification) binocular wide- field
dissection microscope or other optical device Ref: Standard Methods, 18th Edition - Method
9222 D. (2) (e) p. 9-61.
A. COMMENT: The Laboratory is measuring and recording the temperature and pressure of
the autoclave . daily. The recorded temperature of the autoclave is checked against an
autoclave maximum holding thermometer monthly. This check must be performed weekly.
REQUIREMENT: The Laboratory must use an autoclave maximum holding thermometer to
verify that the autoclave thermometer reading is accurate. This type of monitoring check
should be performed on a weekly basis. Standard Methods, 18th Edition - Method 9020, pg. 9-
4.
B. COMMENT: Some of the daily Togs used by the laboratory do not contain all of the
necessary labeling information. No units of measure areassociated with some of the data
values listed in the logbooks.
Note: The laboratory corrected some of the temperature log sheets during the audit.
REQUIREMENT: The laboratory must review all benchsheets and logbooks to ensure that
every entry is marked with the appropriate units of measure. Every number recorded on a
benchsheet or logbook must have an appropriate unit assigned to it.
C. 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 foreach quality control sample on the benchsheet. 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.
Residual Chlorine:
5. DEFICIENCY: The laboratory does not record the volume of each sample analyzed on the
laboratory benchsheet.
REQUIREMENT: 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. Ref: 15A
NCAC 2H .0800 (a) (7) (h).
6. DEFICIENCY: The laboratory is not using the proper calculation to determine residual
chlorine content of samples as stated in Standard Methods 18th Edition 4500E. The laboratory
is standardizing a purchased titrant monthly, but does not include the variance in normality of
the titrant in the equation to determine the final residual chlorine content of the samples.
Note: It is strongly recommended that the laboratory list the calculations used for each final
value determination on the laboratory benchsheet.
REQUIREMENT: The laboratory must determine values for residual chlorine according to the
method stated calculation that accounts for variances in the normality of the titrant. Ref:
Standard Methods 18th Edition 4500E.
D. COMMENT: The laboratory benchsheets do not accurately reflect the method used for the
analysis of residual chlorine in the laboratory. The benchsheets state that the laboratory is.
using Standard Methods 18th Edition 4500D and the laboratory is actually using Standard
Methods 18th Edition 4500E.
REQUIREMENT: The laboratory benchsheets must be modified to reflect the method that is
actually, performed in the laboratory.
COD and Residual Chlorine:
7. DEFICIENCY: The laboratory does not analyze and record blanks for these parameters
daily.
REQUIREMENT: Blanks must be analyzed in order to determine bias in eachsample batch.
Ref: Standard Methods, 18 Edition - Method 2020 pg. 2-1.

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Total Suspended Solids and COD:
8. DEFICIENCY: The laboratory does not record the time and date that the samples were
placed into the oven or on the reactor and time and date that the samples were removed from
the oven or the reactor on the laboratory benchsheet.
REQUIREMENT: The laboratory must record the time and date that the samples were placed
into the oven or on the reactor and time and date that the samples were removed from the
oven or reactor on the laboratory benchsheet. The methods require that samples be dried for
at least one hour or placed on the COD reactor for at least 2 hours. The laboratory must
document that this minimum dryingand reaction time is performed. Ref: Standard Methods,
18th Edition - Method 2540 D. Total Suspended Solids Dried at 103-105° C section (3) c p2-
56. And Standard Methods 18th Edition 5520C Section (4) p. 5-9.
Total Solids:
9. DEFICIENCY: The laboratory is not analyzing any duplicate samples for the total solids
analysis.
Note: The laboratory is currently only using this method for quality control purposes and
meeting requirements for method 503.1. All certified data must meet the requirements of both
the methods and 15A NCAC 2H .0805. All process control samples that do not meet these
criteria must be labeled as non -certified or does not meet certification requirements:
REQUIREMENT: Excluding oil and grease, 10% of all samples must be analyzed in duplicate.
Ref: 15A NCAC 2H .0805 (a) (7) (C).
Ammonia:
E. COMMENT: The laboratory does not analyze a second source calibration standard on a
daily basis. The laboratory is analyzing a second source calibration standard on a quarterly
basis.
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, itmust 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.
F. COMMENT: The laboratory is not making corrections to the data in an approved manner.

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REQUIREMENT: If a mistake is made in data recording, the mistake must be removed by
making a single line through the incorrect entry, recording the correct entry beside mistake,
and initialing and dating the error. Ref: SW 846 Sept. 1994 Test Methods for Evaluating
Wastes, Chapter One pg. 13
Ammonia and Fecal Coliform:
10. DEFICIENCY: The lab is not checking Ammonia and Fecal Coliform samples for residual
chlorine.
REQUIREMENT: A record of date collected, time collected, sample collector and use of proper
preservatives must be maintained. The residual chlorine check must be performed to verify
that the residual chlorine level is below 0.2 mg/L. Commercially available starch iodide paper
can be used to perform this determination. Ref: 15A NCAC 2H .0805 (a) (7) (M).
Fecal Coliform:
G. COMMENT: The laboratory does not record all of the analytical information associated with
initial and final blanks.
REQUIREMENT: All blanks must be analyzed and recorded in the same manner as other
samples.
Conductivity:
H. COMMENT: The labeling system for duplicates is unclear on the benchsheets for
conductivity.
RECOMMENDATION: For duplicate samples the sample name should be followed by the
term "Dup." or "Duplicate" to indicate sample duplication. This will clearly delineate duplicate
samples from regular samples.
BOD:
11. DEFICIENCY: The laboratory does not determine the amount of sodium sulfite necessary
to neutralize the residual chlorine as described in the approved method.
Note: The laboratory uses 30 drops of sodium sulfite to neutralize all BOD samples each
analysis day. Excess sodium sulfite will cause a increase in the reduction potential of each
sample. For this reason, the method requires that only the exact amount sodium sulfite that is
necessary be used to neutralize each sample.
REQUIREMENT: The. laboratory must perform the titrametric test for the removal of residual
chlorine, and the amount of sodium sulfite necessary to neutralize that chlorine as described in
Standard Methods,l8th Edition p 5-4.

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I. COMMENT: The laboratory does not rinse the DO electrode between sample sets.
REQUIREMENT: Failure to rinse the DO electrode between each sample set introduces
contamination from previous sample sets. The laboratory must rinse the DO electrode
between each sample set.
J. COMMENT: The laboratory lists all quality control samples on one page of the data
package and the following sheets in the package contain the data values. The data sets and
the quality controls are not linked together.
REQUIREMENT: The Jaboratory must clearly .identify each quality control set with the data
values associated with them.
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, May, and
June 2001' indicated no problems in proper data reporting.
V. CONCLUSIONS:
Correcting the above deficiencies and comments will help the laboratory to produce quality data
and meet certification requirements.
Please respond to all Deficiencies and lettered Comments cited in this report.
Report prepared by: Frederick L. Bone
Date: August 28, 2001