NC0020427_Lab Certification Inspection_20010803

Michael F. Easley, Governor Do.
William G. Ross Jr., Secretary 11
North Carolina Department of Environment and Natural Resources JJL -
Gregory J. Thorpe, Ph.D. !D>Q-=
Acting Director_ Kk
Division of Water Quality
August 3, 2001
178
Mr. Larry D. Cobler
City of Rockingham WWTP
311 East Franklin Street
Rockingham, NC 28379
SUBJECT: Laboratory Certification Maintenance Inspection
Dear Mr. Cobler:
A �
AUG 6 2001
D Q
Enclosed is a report for the inspection performed on July 19, 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
CITED PREVIOUSLY deficiency (s) found during the inspection. Another inspection will
be scheduled within 3 to 6 months. 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 have been included per
your request. 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
FFakefteille�Regional�O
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]

LABORATORY NAME:
ADDRESS:
CERTIFICATE NO:
DATE OF INSPECTION:
TYPE OF INSPECTION:
EVALUATOR:
On -Site Inspection Report
City of Rockingham VVVVTP
311 East Franklin Street
Covington Street Ext.
Rockingham, NC 28379
178
July 19, 2001
Maintenance
Frederick L. Bone
LOCAL PERSON(S) CONTACTED: Larry Cobler
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.
The laboratory supervisor is currently attempting to perform too many tasks for the VVWTP. He does not.
appear to have the time or resources to meet the .various demands of the laboratory quality control
program. It is recommended that additional personal and resources be allotted to him so that the
laboratory can meet its certification requirements.
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).

Page 2
2. DEFICIENCY: The laboratory is not verifying the automatic temperature compensation of the pH
.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).
3. DEFICIENCY: The laboratory not checking the analytical balance daily with one class S, "1" or "2"
standard weight.
REQUIREMENT: The analytical balance must be checked with one class S, "1" or "2" standard
weight each day used and at least three standard weights quarterly. The values obtained must be
recorded in a log and initialed by the analyst. Ref: 15A NCAC 2H .0805 (a) (7) (k).
4. DEFICIENCY: The laboratory does not check the analytical balance with at least three standard
weights quarterly.
REQUIREMENT: The analytical balance must be checked with one class S, "1" or "2" standard
weight each day_ used and at least three standard weights quarterly. The values obtained must be
recorded in a log and initialed by the analyst. Ref: 15A NCAC 2H .0805 (a) (7) (k).
Note: The only balance check that the laboratory is performing is to press the autocalibrate button on
the balance daily.
5. DEFICIENCY: The Laboratory is measuring and recording the temperature and pressure of the
autoclave daily. The thermometer used is not checked .against an autoclave maximum holding
thermometer weekly.
Note: The laboratory does not currently have a minimum/maximum holding thermometer.
REQUIREMENT: Check the operating temperature weekly with a minimum/maximum holding
thermometer. Ref: Standard Methods, 18th Edition - Method 9020 B. 2. i.
6. DEFICIENCY: The laboratory is not recording corrected temperature values for the laboratory
thermometers.
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 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 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.

Page 3
B. COMMENT: The laboratory does not qualify data that does not meet established quality control
criteria.
RECOMMENDATION: 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. For
example if the GGA is not within the control limits for a given day, the data should be reported and
the results qualified with a note that indicates the laboratory recognizes that the GGA is out of range,
but that in the technician's professional opinion that the data is valid. Any variation in data quality
should be explained by qualifying the data.
C. COMMENT: The thermometer in the drying oven is currently reading the internal airtemperatureand 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.
D. COMMENT: The thermometers in the laboratory refrigerator and BOD incubator are not in sealed
bottles of water. The bottles that contain the thermometers are open to the atmosphere allowing for
uncontrolled evaporation.
RECOMMENDATION: The laboratory must seal each thermometer in a bottle of water or other
applicable liquid matrix. This will control, the evaporation rate ofthe liquid and lessen the chance of
the thermometer bulb becoming exposed to the atmosphere. All temperature readings should be
taken in the same matrix as the samples.
E. COMMENT: The laboratory is reporting values of "0" (zero) for fecal coliform results on the DMR
Reporting forms.
REQUIREMENT: The reporting limit of the fecal coliform analysis is <1.0 colony / 100m1.
F.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 qualitycontrol 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.
Fecal Coliform:
G. 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

Page 4
Total Suspended Solids:
7. DEFICIENCY: The laboratory is not analyzing a sample of sufficient size to yield 1.0 mg of residue
on each filter.
REQUIREMENT: The lab must filter enough sample to achieve >1.0 mg residue on the filter. Ref:
EPA 600/4 - 79 -020, Revised Method 1983 Method 160.2 pg. 2-1.
8. DEFICIENCY: The laboratory does not record the time that the samples were placed into the oven
or removed from the oven on the bench sheet.
REQUIREMENT: The time in and out of the drying oven must be documented to verify drying time is
adequate.
9. DEFICIENCY: The laboratory did not conduct a drying time verification study for 2001.
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 0.5 mg, whichever is less. Ref: Standard Methods 18th Edition 2540 D Total Suspended
Solids at 103-105° C section (3) c p2-56. This process will establish the required drying time for
samples
10. DEFICIENCY: The lab is not analyzing a quarterly standard for total suspended residues.
REQUIREMENT: Analyze one suspended residue standard quarterly. Ref: 15A NCAC 2H .0805 (a)
(7) (B)•
H. 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:
11. DEFICIENCY: The laboratory does not document the air calibration of the DO meter at the
beginning, end, and throughout each analytical run.
COMMENT: The laboratory must document all relevant calibration information. If the information is not
recorded, the laboratory has no means with which to demonstrate that the calibration was actually
performed.
REQUIREMENT: Calibration: Follow manufacturer's calibration procedure exactly to obtain
guaranteed precision and accuracy. Generally, calibrate membrane electrodes by reading against
water saturated air or a sample of known DO concentration. Preferably, calibrate with samples of
water under test. Check one or two points frequently to confirm original calibration. If calibration

Page 5
changes, the new calibration should be parallel to the original, provided that the same membrane
material is used. Ref: Standard Methods, 18th Edition 4500-0 (2) and (3) p. 4-104.
12. DEFICIENCY: The initial DO: for BOD of some samples is above 9.0 mg/L. CITED PREVIOUSLY
REQUIREMENT: Samples that are supersaturated with DO must be brought to 20°C and vigorously
shaken or aerated with clean compressed air to bring the sample to an initial DO below 9.0 mg/L. The
initial accepted DO range is 7 - 9 mg/L Standard Methods, 18th Edition 5210B (6)b p.5-6.
13. DEFICIENCY: The BOD blank values were not in the method accepted range. Some blanks were
as high as 3.7mg/L. The .laboratory must take immediate corrective action based on the problems
associated with its blanks. CITED PREVIOUSLY
REQUIREMENT: Blanks must be analyzed and calculated each analysis day. The DO uptake in 5d
at 20 °C should not be more than 0.2 mg/L and preferably not more than 0.1 mg/L. Standard
Methods, 18th Edition 5210B (4) (b) p.5-3.
14. DEFICIENCY: The laboratory GGA standards are frequently outside of the accepted range of 198
± 30.5 mg/L. CITED PREVIOUSLY
REQUIREMENT: Use a mixture of 150-mg glucose/L and 150 mg glutamic acid/L as a standard
check. Determine the 5-d 20 °C BOD of a 2% dilution of the glucose glutamic acid standard check
solution. The average 5- d BOD would be 198 mg/L with a standard deviation of 30.5 mg/L. Ref:
Standard Methods, 18 Edition - Method 5210 pg. 5-3 to 5-5.
15. DEFICIENCY: The laboratory is not seeding the GGA standard.
REQUIREMENT: The laboratory must treat the GGA standard as any other type of sample. For this
reason, the laboratory must use the same amount of seed in the GGA standard as it does in all other
seeded samples. Ref: Standard Methods, 18 .Edition - Method 5210 pg. 5-3 to 5-4.
16. DEFICIENCY: The seed corrections are often outside of the 0.6 - 1.0 mg/I range.
Note: The laboratory is using an in—house influent as the seeding material. The laboratory is
furthermore obtaining this seed source daily as needed. This seed source is very unstable. The seed
correction factors seldom meet the required limits of 0.6 — 1.0 -mg/L. It is recommended that the
laboratory either use a commercially available seeding material or freeze influent seeding material in
lots. This will help the laboratory to obtain more stable seed controls and seed correction factors.
REQUIREMENT: The DO uptake of seeded dilution water must be between-0.6 and 1.0 mg/I. Ref:
Standard Methods, 18 Edition -.Method 5210 pg. 5-4.`
17. DEFICIENCY: The laboratory is averaging values that do not meet the acceptance criteria of the
method with values that do meet method criteria to report results.
REQUIREMENT: For seed corrections, only values, that meet the 0.6-1.0 mg/L may be used to
compute the averaged seed correction factor. Only data that meets the 2 mg/L used 1 mg/L
remaining criteria can be averaged to obtain a final BOD result. Only GGA standards that fall within

Page 6
the range of 198 ± 30.5 mg/L can be averaged to obtain passing GGA results. Data that does not
meet the method criteria must not be averaged with acceptable data to obtain an acceptable result.
Ref: Standard Methods, 18 Edition - Method 5210 B pg. 5-3.
18. DEFICIENCY: Dilutions are set at levels that do not allow for appropriate usage of DO, and the
lab is not analyzing 100 % samples.
REQUIREMENT: The laboratory must analyze 100% samples to report results that do not achieve
the 2 mg/L used 1 mg/L remaining criteria. Dilutions that result in a residual DO of at least 1 mg/L
and a DO uptake of at least 2 mg/L after 5 days incubation produce the most reliable results. Make
several dilutions of a prepared sample to obtain DO uptake in this range. Ref: Standard Methods,
18th Edition. 5210B. (4)(F) p. 5-4.
I. 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.
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.
J. COMMENT: The laboratory does not qualify data that does not meet established quality control
criteria.
Qualifying Versus Rejecting...B10a Data
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 itself states in Part,ll;-Section D,-Monitoring-and-Records; Number-7 Recording
Results, - ``-for each measure`ment=or sample taken-pursuantAo the_.requirements..:6 this permit,-tl e
perrrfittee:shall-recordtf e-following -mformation...the results=of:such-analyses."
This-r:nans_alh_-data are-reported-antl _none_are_rejected. 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

Page 7
Monitoring Report (DMR). Any rejection of data from the storets will be issued by the agency that
receives the data.
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.
K. COMMENT: The laboratory is currently using a 400 ml sample and transferring 300m1 of that
sample into a BOD bottle.
RECOMMENDATION: It is strongly recommended that the laboratory pour 300 ml of sample directly
into the BOD bottle without the 400m1 intermediate step. The will help the laboratory reduce
contamination that is currently present in the laboratory.
L. COMMENT: The laboratory is not getting good agreement between the seed correction factor and
the seed blank.
RECOMMENDATION: The seed blank and the seed correction factor should agree within ±0.2mg/L.
The data reviewed showed differences of as much as .75-1.0 mg/L. This indicates possible problems
exist in the seeding of the samples. The laboratory needs to determine the source of the discrepancy
and correct the problem.
p
M. COMMENT: The laboratory is not calculating the pH meter consistent with the requirements of the
method. The laboratory calibrates the meter on a pH 4 and 7 buffer and checks the calibration with a
pH 10 buffer.
REQUIREMENT: The laboratory must calibrate the pH meter with at least two buffers and read a
third buffer below pH 10, approximately 3 pH units different from the second buffer and the reading
should be within 0.1 pH units from the expected value. Ref: Standard methods 18th Edition 4500-H
B.(4) (a) p4-68.
N. COMMENT: The laboratory does not clearly label the final value to be reported on the benchsheet •
for pH.

Page 8
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).
Residual Chlorine:
19. 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 18thEdition 1020B Quality Control (4) p 1-5.
N. COMMENT: The laboratory does not analyze a second source QC standard daily for this parameter.
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.
20` DEFICI,Eket-Y: The laboratory has a lower reporting limit of 200 ug/L. The laboratory permitted
reporting limit is 28 ug/L. The laboratory is reporting -values- in-ug/L_ on fhe;:DMR -reporting- f®-m.
Laboratory resuIts-,a re, reported, on. the=benchsheet as ug/L but-the-actual_Measurern_ents are in�rn=g/L.
The proper conversion is not being made between ug/L and mg/L. (i.e. <0.2 mg/L from benchsheet is
reported as <0.2 ug/L on the DMR). The laboratory data and the DMR data do not currently reflect
accurately measured values. Commented°on-previouslyin`0-ctober-9;11=998-report.
REQUIREMENT: The laboratory must analyze standards at or below the permitted limit. The
laboratory must develop an analytical curve with a low reporting limit at or below the permitted limit.
The laboratory must report data in the proper units on the both the benchsheets and the DMR
reporting forms.
Note: The laboratory must submit amended DMR reports with values corrected for ug/L for this
parameter.
21. DEFICIENCY: The standard that the laboratory is currently analyzing, as a mid -point check
standard is not at the mid -point of the calibration curve. The actual mid -point of the analytical curve
for residual chlorine in this laboratory is 1.0 mg/L.
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.

Page 9
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).
O. COMMENT: The laboratory is not calculating a correlation coefficient for the standard curve for
the residual chlorine analysis. The laboratory is graphically plotting the analytical curve, but 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 bythe
State Laboratory. Ref: 15A NCAC 2H .0805 (a) (7).
Ammonia:
P. COMMENT: The laboratory is not running 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.
Q. COMMENT: The laboratory is analyzing a blank daily, but does. not document the analysis on the
laboratory benchsheet.
REQUIREMENT: All blank information must be recorded on the laboratory benchsheet. Blanks must
be analyzed in order to determine bias in each sample batch. Ref: Standard Methods, 18 Edition -
Method 2020 pg. 2-1.
R. 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, 0.5, and
10mg/L.
RECOMMENDATION: It is 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

Page 10
more closely bracketed by standards. The laboratory may consider analyzing standards at 0.1, 0.5,
1.0 mg/L.
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:
We are concerned with the deficiencies that were cited previously and not corrected. Failure to correct
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:
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
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
certification requirements.
Please respond to all numbered Deficiencies and lettered Comments cited in this report.
Report prepared by: Frederick L. Bone Date: August 2, 2001