NC0005762_Lab Inspection_20010813

Michael F. Easley, Governor
William G. Ross Jr., Secretary
North Carolina Department of Environment and Natural Resources
Gregory J. Thorpe, Ph.D.
Acting Director
Division of Water Quality
August 13, 2001
156
Mr. George W. Brown
WestPoint Stevens Wastewater Laboratory
P.O. Box 388
Airbase Road
Wagram, NC 28396
SUBJECT: Laboratory Certification Maintenance Inspection
Dear Mr. Brown:
Enclosed is a report for the inspection performed on August 7, 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. We are seriously
concerned about the f E®i EVt U `LY defici!ency(ies) found during the inspection. 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 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,
allied (4
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
RMENR
[phone]

On -Site Inspection Report
LABORATORY NAME: WestPoint Stevens Wastewater Laboratory
ADDRESS: P.O. Box 3888
Airbase Road
Wagram, NC 28396
CERTIFICATE NO: 156
DATE OF INSPECTION: August 7, 2001
TYPE OF INSPECTION: Maintenance
EVALUATOR: Frederick L. Bone
LOCAL PERSON(S) CONTACTED: George Brown, Roy Guinn, and Herman Benton
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 sufficient quality control for it's duplicate sample
analyses. 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 inorganic benchsheets so that the
analyst will be able to immediately confirm whether or not 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 verifying the automatic temperature compensation of the pH
meter on an annual basis.

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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).
3. DEFICIENCY: The standard that the laboratory is analyzing, as a mid -point check standard is not
at the mid -point of the calibration curve.
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 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).
4. DEFICIENCY: The laboratory does not qualify data that does not meet established quality control
criteria. 'CITED -PREVIOUSLY -fat- BOD'
Example:
Q.uaaifying17e`r§11s...geje_c_t ng_BO,D_Qata'
The lab is not qualifying the data when quality control requirements are not met. The following
information is provided to enable compliance.
It is the desire of the State of North Carolina that all data generated for any permitted location under
NPDES requirements is to be reported. " Every person subject to [15A NCAC 2B .0506] shall file
certified monitoring reports setting forth the results of tests and measurements conducted pursuant
to NPDES permit monitoring requirements." Reference: 15A NCAC 2B .0506 (a) (1). Additionally, "
the results of all tests of the characteristics of the effluent, including but not limited to NPDES Permit
Monitoring Requirements, shall be reported on monthly report forms." Reference: 15A NCAC 2B
.0506 (b) (3) (J).
The-NPDES Permit itselfstates_in _la r_ili: Sectio.n_.D;=Monitoring::aridhRecofds,, Number 7--^R_ecor_ding
Res'ults,P_ - -ffor`eachir feasurement-or sample takenpursuant_td the.=req,uirem nts .of=this�perrnitahe
permittee_sshall:record_the.fo.11owing_inf-ormatidh ,the results ofsucKanalyses."
This means all_.dafa are reported and none=afe:refectedT'If all quality control requirements are not
met, it is required that the data be flagged and the qualification appear on the back of the Discharge
Monitoring Report (DMR). Any rejection of data from the storets will be issued by the agency that
receives the data.

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The Quality Control requirements of the method are outlined below:
1. The DO depletion of the dilution water blank must not be more than 0.2 mg/I.
2. The seed controls must deplete at least 2.0 mg/I DO and have at least 1.0.mg/I DO remaining.
3. The samples must also deplete at least 2.0 mg/I DO and have at least 1.0 mg/I DO remaining.
4. No evidence of toxicity should be present. This can only be evident when at least three dilutions
are analyzed. This is characterized by an increasing BOD value as the sample concentration
decreases.
5. The glucose glutamic acid standard must be in the acceptable range of 198 mg/I +/- 30.5 mg/I.
6. The seed correction, calculated from the seed controls, must be between 0.6 and 1.0 mg/I.
Anytime any of the above quality control requirements are not met, the data must be flagged. The
qualifying statement should indicate that all QC requirements were not met. But the data must
always be reported.
REQUIREMENT: The laboratory must qualify all data that does not meet the quality control criteria
established by either laboratory controls or by criteria given in each individual method. Any variation
in data quality should be explained by qualifying the data.
OBSERVATION: During the audit, the commercial laboratory used by this facility was present to
acquire samples from the laboratory. The analyst went and obtained a grab sample for fecal
coliform. The bottle used for this sample was a narrow mouth dilution bottle. The auditor did not
accompany the analyst in sampling. The type of bottle used was sterile and contained preservative,
but with the narrow opening of the bottle it would be difficult to pour sample from the grab bottle into
the sample bottle without contamination. The sample bottle may not be submerged or held under a
flow because this would result in the loss of preservative. A narrow mouth bottle would not be
recommended for fecal coliform samples.
A. COMMENT: The laboratory does not keep an adequate log for the preparation of standards and
reagents.. The laboratory is currently keeping a log for standard preparation, but does not record all
of the necessary preparation information. Information was provided during the audit concerning the
required information that must be contained in a standard preparation logbook
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 standards logbook will also enable the laboratory to document exactly when, by
whom, and how each reagent was prepared.
B. COMMENT: The laboratory does not list the acceptance ranges of quality control samples on the
bench sheets.
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 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 4
C. COMMENT: The laboratory does not analyze second source QC standards daily for each certified
parameter.
REQUIREMENT: Analyze one known standard in additionto 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.
D. COMMENT: The laboratory does not demonstrate linearity of the analytical curves. The
laboratory is not calculating correlation coefficients for the standard curves.
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).
E. COMMENT: The laboratory is analyzing a blank daily for some parameters, but does not fully
document the analysis on the laboratory benchsheet.
REQUIREMENT: All blank information must be recorded on the laboratory benchsheet. All blank
information must be fully calculated in order to demonstrate that no contamination is present.
Blanks must be analyzed in order to determine bias in each sample batch. Ref: Standard Methods,
18 Edition - Method 2020 pg. 2-1.
F. COMMENT: Some of the daily logs and bench sheets 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 benchsheets and log books to make sure
that every entry is marked with the appropriate unit of measure. Every number recorded on a bench
sheet or logbook must have an appropriate unit assigned to it.
Total Suspended Solids:
G. COMMENT: The laboratory is not weighing a weight in the less than one gram range.
REQUIREMENT: An analytical balance capable of weighing 0.1 mg is required for certification. Ref:
15A NCAC 2H .0805 (a) (6) (d). The balance must be calibrated with class "S", "1" or "2" weights to
bracket the range of the instrument.
H. COMMENT: The laboratory does not record the time that the samples were placed into the oven
or removed from the oven on the benchsheet. The laboratory does record this information on a
second logbook.

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REQUIREMENT: The time in and out of the drying oven must be documented to verify drying time is
adequate. It is strongly recommended that this information be recorded on the laboratory
benchsheet. This will help to ensure that all information pertainingto this analysis is readily
assessable to the analyst.
I. COMMENT: The laboratory must reanalyze the drying time verification study for 2001. The
laboratory did not perform multiple weighings on samples that were taken through the complete
sample drying process. The study conducted by the laboratory was on multiple weighings of
samples in the desiccator, not samples that were redried in the drying oven.
REQUIREMENT: Dry evaporated sample for at least 1 hour in an oven at 103 the 105°C, cool in
desiccator to balance temperature, and weigh. Repeat cycle of drying, cooling, desiccation, and
weighing until a constant weight is obtained, or until weight change is less than 4% of previous
weight or 0.51 mg, whichever is less. Ref: Standard Methods 18th Edition 2540 B Total Solids at
103-105° C section (3) b p2-56. This process will establish the required dry time for samples
J. COMMENT: The laboratory is not analyzing water blanks for the Total Suspended Solids analysis.
The laboratory must filter a volume of DI water (equal to the maximum sample volume used) as a
method blank each analysis day.
REQUIREMENT: Blanks must be analyzed in order to determine bias in each sample batch. Ref:
Standard Methods 18th Edition - Method 1020B pg. 1-5.
BOD:
K. COMMENT: The laboratory is not currently performing an Oxidation and Reduction test for all
seeded samples. The laboratory must perform a titrametric analysis to determine the chlorine
content and neutralization for that chlorine for all BOD samples.
Note: If the laboratory can demonstrate that the chlorine level is less than 20-ug/L per day
neutralization is unnecessary. The laboratory must record this information on the laboratory
benchsheet for this parameter daily.
REQUIREMENT: The laboratory must perform Oxidation and Reduction tests for all seeded
samples. This is required by the method, in order to determine the amount of sodium sulfite or
Potassium Bi-iodate that is needed to neutralize the samples. The laboratory must perform the
titrametric test for the removal of residual chlorine, as described in Standard Methods, 18th Edition p
5-4.
pH and Residual Chlorine:
5. DEFICIENCY: The laboratory is not recording the time sampled and the time analyzed for pH and
Residual Chlorine samples on the General Worksheets.
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 .0805 (a) (7) (h).

Page 6
Note: This information is important to document that the holding times were met for these analyses.
Residual Chlorine: '
6. DEFICIENCY: The laboratory is not analyzing any duplicate samples for residual chlorine.
REQUIREMENT: Excluding oil and grease, 10% of all samples must be analyzed in duplicate. Ref:
15A NCAC 2H .0805 (a) (7) (C).
7. 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.
L. COMMENT: The residual chlorine samples analyzed in the laboratory are below the reporting limit
of the residual chlorine curve. The curve used by the laboratory is 3µg/L to 100 µg/L. The laboratory
analyzes a daily check standard at 10 µg/L. This check standard recovery vary by as much as 40%.
Note: As stated in the General Section of this report, the midpoint must be at one half the
concentration (i.e. 50µg/L for this curve). The stability at the mid -point must be ± 10%. The
laboratory also must have stability in the lower region of the analytical curve. The standards in the
lower region of the curve must be recovered in the 99% confidence interval (approximately ±25%).
RECOMMENDATION: Based on the data at the 10µg/L level, the lower end of this curve appears to
be unstable. The permitted chlorine level. of this facility is 28 µg/L. It is recommended that the
laboratory shorten the analytical curve and raise the low reporting limit standard to at least 15 pig/L.
This will increase the sensitivity of the curve and allow for better recovery of the check standards.
Conductivity:
8. DEFICIENCY: Some of the samples analyzed for conductivity are not properly bracketed by
calibration standards.
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. Ref: 15A NCAC 2H .0805 (a) (7) (I).
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.

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V. CONCLUSIONS:
We are concerned with the deficiencies that were cited previously and not corrected. Failure to
correct the deficiencies and comments cited in this report will lead to enforcement action.
Ref: 15A NCAC 2H .0807 (a) (1) and (14)
Laboratory Decertification:
A laboratory may be decertified for any or all parameters for up to one year for any or all of the
following infractions:
(1) Failing to maintain the facilities, or records, or personnel, or equipment, or quality control
program as set forth in the application, and these Rules; or
(14) Failing to comply with any other terms, conditions, or requirements of this Section or of a
Laboratory certification.
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 9, 2001