NC0020656_Lab Inspection_20010801

- c.vva;,
Qr . , Michael F. Easley, Governor
C G Wiliiam G. Ross Jr., Secretary
�
j r Department of Environment and Natural Resources
- — Kerr T. Stevens
r Y Division of Water Quality
DL
814-
`
K.K --/
August 1,, 2001
133
Mr. Robert Ellis
Leith Creek VWVTP Lab.
P.O. Box 249
Covington Street Ext.
Laurinburg, NC 28353-0249
SUBJECT: Laboratory.Certification Maintenance inspection
Dear Mr. Ellis:
E e° .
AUG 2 ' 2001
D\ O:
Enclosed •isa report for the inspection performed on July 13, 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 arenot corrected, enforcement actions will be recommended: For
certification maintenance, your laboratory must continue to carry out the requirements set
forth in 15A NCAC for 21-I .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 -Reg lanai -Office-)
Sincerely,
kMor
James W. Meyer
Laboratory Section
A,
NCDENR
Laboratory Section
FAX: [phone]
Division of Water Quality 1623 Mail Service Canter Raleigh, NC 27699-1623 [phone]
Internet: www.esb.enr.state.nc.usilab

On -Site Inspection Report
LABORATORY NAME: Leith Creek WVVfP
ADDRESS:
P.O. Box 249
Covington Street Ext.
Lauinburg, NC 28353-0249
CERTIFICATE NO: 133
DATE OF INSPECTION: July 13, 2001
TYPE OF INSPECTION: Maintenance
EVALUATOR: Frederick L. Bone
LOCAL.PERSON(S) CONTACTED: Robert Ellis, Ricky Odem and Loren Dunn ...
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 bench. sheets 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.
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).

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3. DEFICIENCY: The analyst does not initial the temperature Togs on a daily basis.
REQUIREMENT: Alllaboratories 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, andeach-:item must:..
be recorded each time samples are analyzed. Ref: 15A NCAC 2H .0800 (a):(7) (h).
4. DEFICIENCY: The laboratory is using non -class "S" weights for daily -balance :::calibrations:;..The
laboratory is currently measuring class "P " weights.
REQUIREMENT: Theanalytical 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).
5. DEFICIENCY: The final value to be reported is not clearly labeled on the laboratory 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).
A. COMMENT: Some of the daily logsused 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.
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 bench sheet or logbook must
have an appropriate unit assigned to it.
B. COMMENT: The laboratory does not keep a log for the preparation ofstandards 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.
C. COMMENT: The laboratory is currently decertified for Turbidity and Conductivity.
REQUIREMENT: The laboratory must complete the following steps in order to become recertified.
1. The laboratory must return the LC-22 form included in the decertification package.
2. The period of decertification must be complete.
3. A written request for recertification of the parameter must be submitted.
4. Two acceptable Performance Evaluation results must be performed for the requested method.
5. Payment of the recertification invoice must be received.
D. COMMENT: The laboratory does not mark temperature corrections on each thermometer.
Note: The laboratoryhas recently purchased certifiable thermometers to replace thermometers previously
used in the laboratory.

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RECOMMENDATION: It is strongly recommended that the laboratory mark each thermometer with .the::.
appropriate temperature, adjustrrient. • This. will • ensure that. proper corrections are made each time! ,a,
temperature reading is recorded.
E. COMMENT: The laboratory does not have the balance serviced on an annual basis:
RECOMMENDATION:, It is strongly: recommendedthat- the laboratory have all analytical and top loading
balances serviced on an annual basis. This will ensure that the balances are properly calibrated and capable,.
of producing reliable and reproducible data.
F. COMMENT: The. laboratory -does not measure a range =of:weights that fully bracket .the range of.
samples analyzed.
REQUIREMENT: The laboratory must analyze class "S", "1" or "2" weights in a range that fully bracket the
weights of the samples analyzed by the laboratory.
G. 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 limitsfor 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.
H. COMMENT: The Laboratory is measuring and recording the temperature and pressure of the autoclave
daily. The thermometer used isnot checked against an autoclave maximum holding thermometer weekly.
REQUIREMENT: Check the . operating temperature weekly with a minimum/maximum holding
thermometer. Ref: Standard Methods, 18th Edition - Method 9020 B. 2. i.
Fecal Coiiform:
6. DEFICIENCY: The laboratory is not consistently setting dilutions that yield colonies in the 20 to 60 fecal
colony range. The laboratory is not setting a 100 ml full volume sample.
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.
7. DEFICIENCY: The laboratory is averaging fecal values that are not in the countablerange of 20 — 60
colonies per 100mI with values that are within acceptance range.
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.
1. COMMENT: The laboratory does not record the time of sample collection on the fecal coliform
benchsheet.

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REQUIREMENT: The laboratory must record the ,time -of sample collection and time of sample analysis on
the laboratory: benchsheet for fecal coliform. This allows the analyst to verify that the 6-hour holding time
is achieved.
Total Suspended Solids:
-8. 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'fi?ter.enough sample to achieve >1.0 mg residue on Ref: EPA
600/4 - 79 -020, Revised Method.1983 Method 160.2 pg. 2-1.
9. 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 tirne is
adequate.
J. 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 onmultiple weighingsof 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. Reoeat.cvcle of drvina, cooling, desiccation, and weiohine
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 B Total Solids at 103-105° C section (3) b
p2-56. This process will establish the required dry time for samples
K. 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:
10. DEFICIENCY: The laboratory does not document the pH of the buffered dilution water to be 7.2.
REQUIREMENT: The pH of the buffered dilution water should be 7.2 without further adjustment. Ref:
Standard Methods, 18 Edition - Method 5210 B (3) (a). pg. 5-3.
11. 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 the range of 198 ± 30.5
mg/L can be averaged toobtain. passing GGA results. Data that does not meet the method criteria must

Page 5
not be averaged with: acceptable .data to obtain an acceptable result. Ref: Standard Methods, 18 Edition
Method 5210 B pg. 5-3.
12. DEFICIENCY: The laboratory is reporting values that are less than the lower reporting limit of the
method for BOD.
REQUIREMENT: For BOD the lower reporting limit of the method is 2.0 rng/L based on the requirement
that Samples -use at least ,2.0:mg/L of DO uptake --after 5 days. Dilutions that -result in a'; residual D0. of:at,
-=least 1 rng/L and- a.DO-uptake of,at.Ieast 2.mg/L after5,days. incubation produce.the most reliable results.
Make severat`dilutions -of a'prepared sample to.obtain-DO- uptake in this range: •Ref::Standard .Methods,.
18th Edition. 5210B. (4)(F) p. 5-4.
13. 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 iaboratory.:must analyze, 1,00% 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,5days 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.
14. DEFICIENCY: The laboratory does not document the pH of each sample.
REQUIREMENT: Samples must be neutralized to a pH of 6.5 - 7.5. Ref: Standard Methods, 18 Edition -
Method 5210 B (4) (e) (1). pg. 5-4 .
L. 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.
M. COMMENT: The labeling system for duplicates is unclear on the laboratory benchsheets.
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.
N. 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 Reductiontests for all seeded samples. This
is required by the method,inorder 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.

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O. COMMENT: The laboratory does not qualifydata that does rot meet established quality control. criteria..::.
Qualifying Versus Rejecting BOD 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 II, Section... D, Monitoring and Records, . Number 7.`-
Recording Results, " for .each measurement or sample taken pursuant to the requirements of this
permit, the permittee shall record the: following information...the results of such analyses."
This means all: data arereported and 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 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 DU 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.
Turbiditv:
P. COMMENT: The laboratory does not include the calibration information for Turbidity on the laboratory
benchsheet.
REQUIREMENT: All calibration information must be listed on each laboratory bench sheet.

Page 7
15. DEFICIENCY:. The laboratory benchsheet:.Iisted incorrect acceptance criteria.. for, pH.:.The..laboratory
benchsheet uses a`70.7 acceptance criteria for the pH 7 buffer. The correct acceptance criterion is 0.1pH
units. t...
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 "unitsfrom the expected value. Ref: Standard methods 18th Edition 4500-H, L.(4):(a) p4-68.
Residual Chlorine:
16. DEFICIENCY: The laboratory does not meet the 15-min. holding time for residual chlorine analysis.
The laboratory was not performing analysis for up to lhour after sample collection. The laboratory ,does
not qualify this: data.
REQUIREMENT: The maximum holding time for residual chlorine samples is 15 min. Ref: 40CFR Ch.1(7-
1-95) p. 644 table II.
17. 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.
Q. COMMENT: The laboratory does not have 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 8.3.
R. COMMENT: The laboratory is not calculating a correlation coefficient for the standard curve. The
laboratory must provide statistical proof of the linearity of the standard curve..
REQUIREMENT: 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. Thequality control document shall be available for inspection by the State Laboratory. Ref:
15A NCAC 2H .0805 (a) (7).
Ammonia:
18. DEFICIENCY: The laboratory is not analyzing a blank daily for this analysis.

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:REQUIREMENT: Analyze reagent blanks whenever new reagentsare used and as _:often as_. required in.: _
soewifc` methods; -Analyze a minimum of 5% of ihe.sample load as reagent blanks; this, monitors purity of
reagents and the' overall procedural biank. 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.l8th Edition 10208 Quality Control (4) p 1
Note: The'decertificetion of this parameter has been rescinded and the laboratory is.currently .certified :to:
perform Ammonia sample analysis.
Conductivity:
'19. Deficiency: The laboratory is not verifying the automatic temperature. compensation of the conductivity
meter on an annual basis.
REQUIREMENT: All thermometers must meet Nationai 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).
20. DEFICIENCY: The calibration information on the benchsheets -does not accurately reflect the
standards that are analyzed by the laboratory. The laboratory lists one set of -.values on the benchsheet
and actually analyzes a second set of values for calibration.
REQUIREMENT: All -information on the benchsheet must reflect what is actually donein the laboratory..
S. COMMENT: "The laboratory does not verify the automatic cell constant adjustment for the conductivity
meter on an annual basis.
REQUIREMENT: The laboratory must verify the automatic cell constant on an annual basis. The
procedure for doing the'cell constant can be found in Standard Methods, 18th Edition 2510B.4a. p2-45.
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.
CONCLUSIONS:
Correcting the above Deficiencies and Comments will help the laboratory 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: July 27, 2001