NC0027103_Lab Inspection_20011105

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0illiam G. Ross Jr., Secretary ZL.
9 North Carolina Department of Environment and Natural Resources
Gregory J. Thorpe, Ph.D. v
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Acting Director
Division of Water Quality
November 5, 2001
552
Ms. Karen T. Dial
Pembroke WWTP Laboratory
P. O. Box 866
Pembroke, NC 28372-
SUBJECT: Laboratory Certification Maintenance Inspection
Dear Ms. Dial:
NOV 9 2001
Enclosed is a report for the inspection performed on October 24, 2001 by Mr.
Frederick L. Bone. Where deficiencies are cited in this report, a response is required as
well as for all lettered comments and/or recommendations. Within thirty days of receipt,
please supply this office with a written item for item description of how these deficiencies,
comments and/or recommendations were corrected. 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,
041/8,J ivmr_
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 Raleigh, NC 27699-1623
FAX: [phone] Internet: www.esb.enr.state.nc.us/lab
NCDENR
[phone]

On -Site Inspection Report
LABORATORY NAME:
ADDRESS:
CERTIFICATE NO:
DATE OF INSPECTION:
TYPE OF INSPECTION:
EVALUATOR:
LOCAL PERSON(S) CONTACTED:
I. INTRODUCTION:
Pembroke VUVVfP
P.O. Box 866
Pembroke, NC 28372
552
October 24, 2001
Maintenance
Frederick L. Bone
Rhonda Locklear
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.
Ill. DEFICIENCIES, RECOMMENDATIONS, REQUIREMENTS, AND COMMENTS:
General:
1. DEFICIENCY: The laboratory is not verifying the automatic temperature compensation or
temperature sensor of the pH and Conductivity meter on an annual basis.
REQUIREMENT: All thermometers must meet National Institute of Standards and Technology
(NIST) specifications for accuracy or be checked against a NIST traceable thermometer and
proper corrections made. Ref: 15A NCAC 2H .0805 (a) (7) (o).
A. COMMENT: The laboratory does not list the acceptance ranges of quality control samples
on the laboratory benchsheets.
RECOMMENDATION: It is strongly recommended that the laboratory list the acceptance
ranges for each 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.

Page 2
B. COMMENT: Thelaboratory does not analyze a second source QC standard for all required
parameters.
REQUIREMENT: Analyze one known standard in addition to calibration standards each day
that samples are analyzed to document accuracy. This laboratory control standard must be
from a second source. For held curves for colorimetric methods, it must be analyzed after the
calibration verification standard is analyzed. It is recommended that this laboratory control
standard, like the calibration verification standard, 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.
C. COMMENT: The laboratory does not keep a log for the preparation of standards and
reagents.
REQUIREMENT: The laboratory must have a written record of all standards and reagents on
file for a period of at least five years. A standard reagent log will help the laboratory to meet
this requirement. A standards logbook will also enable the laboratory to document exactly
when, by whom, and how each reagent was prepared.
D. COMMENT: The laboratory is reporting data for some parameters as "0". (Residual
Chlorine and Ammonia)
REQUIREMENT: All data must be reported as less than the lowest standard concentration
demonstrated by the laboratory. 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. Ref: 15A NCAC 2H .0800 (a) (7) (I).
Specific Conductance
E. COMMENT: The laboratory indicated at the time of the audit that this parameter is being
considered to be removed from the labs certified parameter list.
REQUIREMENT: If the laboratory desires to remove this parameter from its certified
parameter list, the laboratory must provide this office with written notification of this intent.
Total Suspended Solids:
2. DEFICIENCY: The laboratory is not filtering enough sample to get between 1 and 200 mg of
residue on each filter..
Note: An increase in the amount of sample analyzed from 250mI to 500m1 should satisfy this
requirement.

Page 3
REQUIREMENT: When analyzing suspended residue, sufficient sample must be filtered to yield
at least 1.0 mg of residue. Ref: EPA-600/4-79-020 Methods Manual, March 1979 - Method
160.2. The size of a total suspended solid sample must be between 1 and 200 mg. Limit the
sample size to that yielding no more than 200 mg of residue. Ref: Standard Methods, 18th
Edition - Method 2540 D. Total Suspended Solids Dried at 103-105°C section (3) c p. 2-56.
3. DEFICIENCY: The laboratory does not properly rinse all filters prior to analysis.
REQUIREMENT: Apply vacuum and wash disk with three successive 20-mI portions of
reagent —grade water. Continue suction to remove all traces of water and discard washings.
Ref: Standard Methods 18th Edition 2540D. (3) (A) p. 2-56.
4. DEFICIENCY: The lab is not analyzing a quarterly check standard for total suspended
residues.
REQUIREMENT: Analyze one suspended residue standard quarterly. Ref: 15A NCAC 2H
.0805 (a) (7) (B).
F. COMMENT: No units of measure are associated with some of the data values listed on the
total suspended solids benchsheets.
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).
AMMONIA:
5. DEFICIENCY: The laboratory is not distilling any samples before analysis and has no
comparative data on file.
REQUIREMENT: To analyze samples without distillation, laboratories shall accumulate
comparative data by analyzing at least six samples distilled and undistilled, but at least two
samples from all waste types. Analyze one sample distilled and undistilled yearly from all
waste types.
Note: Additional samples must be analyzed comparatively if the above sample results do not
indicate approximately the same values for distilled and undistilled samples. Ref: Federal
Register, January 31, 1994; 40 CFR 136; Footnote 6.
G. COMMENT: The curve used for ammonia analysis is 0.1 — 10mg/L. The laboratory stated
difficulty with obtaining stability at the lower region of the analytical curve.

Page 4
RECOMMENDATION: In order to increase the accuracy and stability of the analytical
measurement, it is recommended that the laboratory analyze two separate ammonia curves.
The first curve from 0.1 - 1.0 mg/L and the second curve 1.0 — 10 mg/L. The laboratoryy may
also attempt to stabilize the curve readings by increasing the lower reporting limit from 0.1 to
0.5mg/I. A curve from 0.5 tol0mg/L may provide the stability sought by the laboratory.
H. COMMENT: The laboratory does not record the pH electrode calibration information on the
same benchsheet with the sample data. The calibration information is logged on a separate
pH calibration log.
RECOMMENDATION: It is strongly recommended that the laboratory record all calibration
information on the same benchsheet as the sample data. This allows for ease of data
verification as well as eliminating the possibility of data becoming separated from essential
calibration information.
RESIDUAL CHLORINE:
6. DEFICIENCY: The laboratory is not analyzing and recording a standard at the mid -range of
the calibration curve daily for this parameter.
COMMENT: 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.
Note: The laboratory is analyzing a second source check standard daily. 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.
REQUIREMENT: Verify the standard curve daily by analyzing one or more standards within
the linear range, as specified in the individual method. The curve must be updated as set forth
in the standard procedures, each time the slope changes by more than 10 percent at
midrange. Ref: Standard Methods 18th Edition 1020 B. Quality Control section 5 p. 1-5, and
Ref: 15A NCAC 2H .0805 (a) (7) (i).
7. 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).

Page 5
I. COMMENT: The laboratory is not calculating a correlation coefficient for the standard curve
for the residual chlorine analysis. The laboratory does not demonstrate statistically that the
analytical curve is linear.
REQUIREMENT: The laboratory must calculate a correlation coefficient for each analytical
curve in order to demonstrate linearity. Analytical Quality Control Program. 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 quality control document
shall be available for inspection by the State Laboratory. Ref: 15A NCAC 2H .0805 (a) (7).
BOD:
8. DEFICIENCY: The laboratory does not determine the amount of sodium sulfite necessary to
neutralize the residual chlorine as described in the approved method.
Note: 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.
J. COMMENT: The laboratory does not qualify data that does not meet established quality
control criteria on the laboratory benchsheet as well as the DMR reporting form. The
laboratory qualifies data only on the DMR report. This information is not recorded on the
laboratory benchsheets themselves.
REQUIREMENT: Anytime quality control requirements are not met, the data must be flagged.
The qualifying statement should indicate that all QC requirements were not met. However, the
data must always be reported.
K. COMMENT: The benchsheets used for BOD analyses refer to the 19'h Edition of Standard
Methods. This edition of Standard Methods is not approved for wastewater parameters. The
laboratory must cite the most recently approved methods (Standard Methods 18'h Edition) on
the laboratory benchsheets.
REQUIREMENT: The laboratory must properly label each benchsheet. The benchsheets must
accurately reflect the methodology used in the lab. Ref: 15A NCAC 2H .0805 (a) (7) (H).
Fecal Coliform:
L. COMMENT: The laboratory does not clearly label duplicate samples on the general
worksheets.

Page 6
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.
M. COMMENT: The laboratory is not consistently counting the membrane filters under a 10X
microscope.
REQUIREMENT: To determine colony counts on membrane filters, use a magnification of 10
to 15 diameters and a cool white fluorescent light source adjusted to give maximum sheen
discernment. Ref: Standard Methods, 18th Edition - Method 9222 B. (1) (k) p. 9-55.
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 and implementing the recommendations
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: November 1, 2001.

Town of Pembroke
POST OFFICE BOX 866
PEMBROKE, NORTH CAROLINA
28372
MILTON R. HUNT
MAYOR
McDUFFIE CUMMINGS
MANAGER
JoANNNEVILLLE
CLERK
December 12, 2001
N.C. Division of Water Quality
1623 Mail Service Center
Raleigh, NC 27699-1623
Attention: Fred Bone
SUBJECT: Response to Laboratory Certification Inspection
Dear Fred:
Enclosed is a report of how the deficiencies were corrected.
Sincerely,
?hada 4cea.,2
Rhonda H. Locklear
Laboratory Supervisor
Enclosure cc: Fayetteville Regional Office
COUNCILMEN:
LARRY BROOKS
LARRY McNEILL
GREGORY CUMMINGS
ALLEN G. DIAL

Town of Pe broke
POST OFFICE BO 866
PEMBROKE, NORTR CAROLINA
28372
MILTON R. HUNT
MAYOR
McDUFFIE CUMMINGS
MANAGER
JoANNNEVILLE
CLERIC
December 13, 2001
NC Division of Water Quality
1623 Mail Service Center
Raleigh, NC 27699-1623
Attention: Fred Bone
Dear Fred:
!DEC I 2001
V�V
i' CP
COUNCILMEN:
LARRY BROOKS
LARRY McNEILL
GREGORY CUMMINGS
ALLEN G.-DIAL
This letter is to notify the division that we wish to drop specifi conductance off our certified parameter list
since it is no longer on the permit.
Sincerely,
vrtot-oti. iccoule,0
Rhonda Locklear
Laboratory Supervisor.

Town of Pembroke
INastewater Laboratory
Town of Pembroke
P.O. Box 888
Pembroke NC, 28372
Phone: [phone]
Fax [phone]
Corrective Acton Response
Laboratory Name: Pembroke WWTP
Address: P.O. Box 866
Pembroke, NC 28372
Certificate No: 552
/DEC ;1 7 2001

I. GENERAL DEFICIENCIES, RECOMMENDATIONS, REQUIREMENTS, AND COMMENTS:
1. DEFICIENCY: The laboratory is not verifying the automatic temperature compensation or
temperature sensor of the pH and Conductivity meter on an annual basis.
CORRECTION: Conductivity is no longer a permit parameter and we wish to drop
conductivity certification. The pH temperature compensation has been checked against a
NIST traceable thermometer and proper corrections made.
A. COMMENT: The laboratory does not list the acceptance ranges of quality control
samples on the laboratory bench sheets.
Correction: We are currently creating all new bench sheets, to reflect
acceptance ranges stated in quality control manual.
B. COMMENT: The laboratory does not analyze a second source QC standard for all
required parameters.
Correction: The laboratory has ordered second source standards for each
parameter.
C. COMMENT: The laboratory does not keep a log for the preparation of standards and
reagents.
Correction: The laboratory created new log book for preparation of standards
and reagents.
D. COMMENT:. The laboratory is reporting data for some parameters as "0". (Residual
Chlorine and Ammonia)
Correction: The laboratory has been reporting <20ug/l and <1.0 mg/I, for these
parameters.
SPECIFIC CONDUCTANCE:
E. COMMENT: The Laboratory indicated at the time of audit that this parameter is being
considered to be removed from the labs certified parameter list.
Correction: Enclosed is a•written notification to drop specific conductance off
the certified parameter list.
2

TOTAL SUSPENDED SOILDS:
2. DEFICIENCY: The laboratory is not filtering enough sample to get between 1 and 200 mg of
residue on each filter.
Correction: The laboratory has increased sample to 500m1.
3. DEFICIENCY: The laboratory does not properly rinse all filters prior to analysis.
Correction: The laboratory washed disk with three successive 20-mi portions of reagent
water.
4. DEFICIENCY: The laboratory is not analyzing residue standard quarterly.
Correction: The laboratory ordered standards later in the year and will be sure to order
quarterly check standards.
F. COMMENT: No units of measure are associated with some of the data values listed on
the total suspended solids bench sheets.
Correction: Bench sheets are been revised to contain appropriate data.
AMMONIA:
5. DEFICIENCY: The laboratory is not distilling any samples before analysis and has no
comparative data on file.
pH:
Correction: The laboratory is having distilled ammonia samples analyzed for
comparative data.
G. COMMENT: the curve used for ammonia analysis is 0.1 — 10mg/I. The laboratory
stated difficulty with obtaining stability at the lower region of the analytical curve.
Correction: The laboratory has increased the 0.ling/l to 1.0mg/I.
H. COMMENT; The laboratory does not record the pH electrode calibration information on
the same bench sheet with the sample data. The calibration information is logged on a
separate pH calibration log.
Correction: The laboratory is attempting to place pH calibration and sample
data on one bench sheet.
RESIDUAL CHLORINE:
6. DEFICIENCY: The laboratory is not analyzing and recording a standard at the mid -range of
the calibration curve daily for this parameter.

CORRECTION: The laboratory is analyzing a mid -range standard.
7. 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.
Correction: The back-up has analytical curve on file.
I. COMMENT: The laboratory is not calculating a correlation coefficient for the standard curve for the
residual chlorine analysis. The laboratory does not demonstrate statistically that the analytical curve is
linear.
Correction: The laboratory is consulting with other laboratories and placing this information on file that
proves the linear curve.
BOD:
8. DEFICIENCY: The laboratory does not determine the amount of sodium sulfite necessary to neutralize
the residual chlorine as described in the approved method.
Correction: The laboratory is performing the titrametric test for the removal of residual chlorine, and the
amount of sodium sulfite necessary to neutralize that chlorine.
J. COMMENT: The laboratory does not qualify data that does not meet established quality control criteria on
the laboratory bench sheet as well as the DMR reporting form. The laboratory qualifies data only on the DMR
report The information is not recorded on the laboratory bench sheets themselves.
Correction: The laboratory is currently flagging out of range controls on the BOD bench sheet We are
currently revising the BOD bench sheet to provide a response for the qualifier. The DMR reporting form has
an additional BOD qualifier when necessary.
K. COMMENT: The bench sheets used for BOD analyses refer to the 19th Edition of Standard Methods.
This edition is not approved for wastewater parameters. The laboratory must cite the most recently approved
methods (Standard Methods 18 Edition) on the laboratory.
Correction: This was a typographical error and has been corrected.
FECAL COLIFORM:
1,. COMMENT: The laboratory does not clearly label duplicate samples on the general worksheets.
Correction: The laboratory is currently performing duplicate samples with the sample and sample
volumes dearly marked. The laboratory will have to revise bench sheet in order to provide a separate
column labeled duplicate.
M. COMMENT: The laboratory is not consistently counting the membranes under a 10x microscope.
Correction: The laboratory is consistently counting membranes under an 10x microscope.
4