#440- 06 - 2010 - FINAL

INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laborato Cert. M
Laboratory Name:
Inspection Type:
Inspector Name(s):
I nspection Date:
Date Report Completed:
Date Forwarded to Reviewer:
Reviewed by:
Date Review Completed:
Cover Letter to use:
Unit Supervisor:_
Date Received:
Date Forwarded to Alberta:
Date Mailed:
440
Statesville Analytical Labs
Commercial Maintenance
Chet Whiting Jason Smith, Gary Francies
June 23, 2010
July 15 2010
July 15 2010
Jason Smith
July 20 2010
Insp. Initial X Insp. Reg. _ Insp. No Finding _ Insp. CP
Gary Francies
7/21 /2010
7/2712010 t 11

Beverly Eaves Perdue
Governor
440
Ms. Dena Meyers
Statesville Analytical Labs
P.O. Box 228
Statesville, NC 28687
NCDENR
North Carolina Department of Environment and Natural Resources
Division of Water Quality
Coleen H. Sulilns
Director
July 28, 2010
SUBJECT: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Ms. Meyers:
Dee Freeman
Secretary
Enclosed is a report for the inspection performed on June 23, 2010 by Chet Whiting, Jason Smith, and myself.
Where finding(s) are cited in this report, a response is required. Within thirty days of receipt, please supply this
office with a written item for item description of how these finding(s) were corrected. If the finding(s) cited in the
enclosed report are not corrected, enforcement actions may 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. If you wish to obtain an electronic copy of this report by email, or if you have
questions or need additional information please contact me at 828-296-4677.
Sincerely,
Gary F 2cies
Unit Supervisor
Laboratory Section
CC: Chet Whiting
Central files
DENR DWQ Laboratory Section NC Wastewater/Groundwater Laboratory Certification Branch
1623 Mail Service Center, Raleigh, North Carolina 27699-1623
Location: 4405 Reedy Creek Road, Raleigh, North Carolina 27607-6445
Phone: [phone] FAX: [phone]
Intemet www,dwglab.org
One
NofthCarofina
Naturally
An Equal Opportun!W kAffirmafmAdlon Employer Customer Service:1-877-E2W48 www.newaterqualKy.org

LABORATORY NAME: Statesville Analytical Labs
ADDRESS: P.O. Box 228
Statesville, NC 28687
CERTIFICATE #: 440
DATE OF INSPECTION: June 23, 2010
TYPE OF INSPECTION: Commercial Maintenance
AUDITOR(S): Chet Whiting, Jason Smith, Gary Francies
LOCAL PERSON(S) CONTACTED: Dena Myers
INTRODUCTION:
This laboratory was inspected to verify its compliance with the requirements of 15A NCAC 2H .0800 for the analysis
i
of environmental samples.
II. GENERAL_ COMMENTS:
Benchsheets are well designed, easy to follow and concise. Records ,are well organized and easy to retrieve..
Findings A, B, C, and I are new policies that have been implemented by our program since the last inspection
III. FINDINGS RE UIREMENTS COMMENTS AND RECOMMENDATIONS:
General Laboratory
Quality Control
A. Finding: A calibration verification standard (CVS) and blank are not consistently analyzed at the end of
the sample run.
Requirement: The calibration blank and mid -range standard must be analyzed initially (i.e., prior to
sample analysis), after every tenth sample and at the end of each sample group to check for carry over
and calibration drift. If either fall outside established quality control acceptance criteria, corrective action
must be taken (e.g., repeating sample determinations since the last acceptable calibration verification,
repeating the initial calibration, etc.). Ref: North Carolina Wastewater/Groundwater Laboratory
Certification Policy based upon Standard Methods, 201h Edition, 1020 B. (10) (c), 3020 B. (2) (b), and 4020
B. (2).
- Comment: Various combinations of post analytical checks were observed: Analysis of a standard (not the
CVS), analysis of a CVS with no blank, analysis of a blank with no CVS, no analysis of a blank or CVS.
B. Finding: The laboratory needs to increase the documentation of purchased materials and reagents used
or made in the laboratory as well as procedures for standard and reagent preparation.
Requirement: All chemicals, reagents, standards and consumables used by the laboratory must have the
following information documented: Date received, Date Opened tin use). Vendor, Lot Number, and
Expiration Date (where specified). A system (e.g., traceable identifiers) must be in place that links
standard/reagent preparation information to analytical batches in which the solutions are used.
Documentation of solution preparation must include the analyst's initials, date of preparation, the volume
or weight of standard(s) used, the solvent and final volume of the solution. This information as well as the
vendor, manufacturer, lot number, and expiration date must be retained for primary standards, chemicals,
reagents, and materials used for a period of five years. Consumable materials such as pH buffers, lots of

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# 440 Statesville Analytical Labs
pre -made standards and/or media, solids and bacteria filters, etc. are included in this requirement. Ref:
North Carolina Wastewater/Groundwater Laboratory Certification Policy.
Total Suspended Solids - Standard Methods, 18t" Edition, Method 2540 D.
Comment: A minimum dried residue weight gain of 1 mg was used to determine the reporting limit. North Carolina
Wastewater/Groundwater Laboratory Certification based upon Standard Methods, 20t" and 215t Editions, 2540 D.
(3) (b), states: Choose sample volume to yield between 2.5 and 200 mg dried residue. If volume filtered fails to
meet minimum yield, increase sample volume up to 1 L. If complete filtration takes more than 10 minutes increase
filter diameter or decrease sample volume. An updated bench sheet submitted June 30, 2010 addressed this issue.
No further response is necessary for this finding.
Comment: Since the publication of the Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 72,
No. 47, March 12, 2007, there is no longer an approved method that allows for a 1 mg weight gain. Currently, the
minimum weight gain allowed is 2.5 mg. In instances where the weight gain is less than the required 2.5 mg, the
value must be reported as less than the appropriate value based upon the volume used. For example, if 500 mL of
sample is analyzed and < 2.5 mg of dried residue is obtained, the value reported would be < 5 mg/L. The minimum
reporting value is now established at 2.5 mg/L based upon a sample volume used of 1000 mL.
Total Solids - Standard Methods, 18t" Edition, Method 2540 B
Total Dissolved Solids - Standard Methods,18t" Edition, Method 2540 C
Comment: The laboratory was not properly reporting the data based on the method required weight gain of 2.5
mg dried residue. North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon Standard
Methods, 20th and 215t Editions, 2540 C. (3) (d) and 2540 B. (3) (b), states: Choose sample volume to yield
between 2.5 and 200 mg dried residue. To obtain the required residue yield, successive aliquots of samples may
be added to the same dish after evaporation or adjust reporting level based upon the weight gain and sample
volume used. The minimum reporting value is established at 2.5 mg/L based upon a sample volume used of 1000
mL. An updated bench sheet submitted June 30, 2010 addressed this issue. No further response is necessary for
this finding.
Comment: For example, if 100 mL sample is analyzed, and less than 2.5 mg of dried residue is obtained, the
value reported would be < 25 mg/L.
Settleable Solids - Standard Methods, 18t" Edition, Method 2540 F
Comment: The analysis start and end times as well as the time the sample is agitated at forty-five minutes were not
documented. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) states: 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. An updated bench sheet submitted June 30, 2010 addressed this issue. No further response is
necessary for this finding.
Alkalinity -Standard Methods, 18t" Edition, Method 2320 B
Comment: The laboratory was not following the procedure nor applying the formula to determine low level
alkalinities. Standard Methods, 18t" Edition, 2320 B. (4) (d) states: For alkalinities less than 20 mg/L titrate 100 to
200 mL according to the procedure of (4) (c) above, using a 10 mL microburet and 0.02 N standard acid solution.
Stop the titration at a pH in the range of 4.3 to 4.7 and record volume and exact pH. Carefully add additional titrant
to reduce the pH exactly 0.30 pH unit and again record volume. Additionally, the formula for low level alkalinities in
Standard Methods, 18t" Edition 2320 B. (5) (b) must be used. An updated bench sheet submitted June 30, 2010
addressed this issue. No further response is necessary for this finding.
Biochemical Oxygen Demand — Standard Methods,18t" Edition, 5210 B
C. Finding: Extra nutrient, mineral, and buffer solutions are not added to the Biochemical Oxygen Demand
(BOD) bottles containing more than 67% (> 201 mL) sample.

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# 440 Statesville Analytical Labs
Requirement: When a bottle contains more than 67% of the sample after dilution, nutrients may be
limited in the diluted sample and, subsequently, reduce biological activity. In such samples, add the
nutrient, mineral, and buffer solutions (3a through e) directly to individual BOD bottles at a rate of 1 mUL
(0.33 mL/300-mL bottle) or use commercially -prepared solutions designed to dose the appropriate bottle
size. Ref: North Carolina Wastewater/Groundwater LaboratoryCertification Policy based upon Standard
Methods, 20t" Edition, 5210 B. (4) (f) and Standard Methods, 215t Edition, 5210 B. (5) (c) (2).
Comment: Dilution water prepared as normal with nutrient, mineral, and buffer solutions would still be
used in the BOD bottles. For the bottles containing more than 67% sample, extra nutrient, mineral, and
buffer solutions would be added in addition to the dilution water.
Recommendation: Rather than pipetting 0.33 mL of each reagent into the BOD bottle, it is recommended
that commercially prepared nutrient buffer pillows for 300 mL bottles be used.
Total Phosphorus — Standard Methods, 181" Edition, 4500 P E
D. Finding: Start and end times for Total Phosphorus digestion are not documented.
Requirement: 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. Ref: 15A NCAC 2H .0805 (a)
(7).
Hexane Extractable Material — EPA Method 1664 Revision A
Comment: The extraction solvent in use does not meet method required purity criteria. EPA Method 1664 A, Section
7.3, states: n-hexane - 85% minimum purity, 99.0% min. saturated C6 isomers, residue less than 1 mg/L. A
communication from the laboratory on June 30, 2010 states that the next solvent order will meet the purity
requirements stated above. No further response is necessary for this finding.
Metals — Standard Methods, 18t" Edition, 3111 B
Metals — Standard Methods, 18t" Edition, 3113 B
E. Finding: The laboratory control standard (second source) is not digested.
Requirement: Laboratory control standards are evaluated to assess whether the lab is in control of the
processes involved in the preparation and analysis of specific tests. Laboratory control standards must be
similar in composition to the environmental samples. They must contain known concentrations of all
analytes of interest and undergo the same preparatory and determinative procedures as the
environmental samples. Ref: North Carolina Wastewater/ Groundwater Laboratory Certification Policy
based upon 15A NCAC 2H .0805 (a) (7) (B), (a) (7) (F), and Standard Methods, 20t Edition, 1020 B. (2)
and (5).
Ammonia Nitro en — Standard Methods, 18" Edition, 4500 NH3 E
Alkalini — Standard Methods, 18" Edition, 2320 B
F. Finding: Titrants are standardized when prepared, then approximately every six months.
Requirement: All certified titrants which are purchased may be'used initially without standardization. They
must be standardized after one month; and they must be standardized monthly, thereafter, for as long as
they are used. Ref: "Standardization of Titrants", North Carolina Wastewater/Groundwater Laboratory
Certification memorandum dated August 6, 1999.
Fluoride — Standard Methods, 181" Edition, 4500 F C
G. Finding: The calibration verification standard (same source as calibration standards) is not in the mid range
of the analytical curve.

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# 440 Statesville Analytical Labs
Requirement: For colorimetric analyses, a series of five standards for a curve prepared annually or three
standards for curves established each day or standards as set forth in the analytical procedure must be
analyzed to establish a standard curve. The curve must be updated as set forth in the standard
procedures, each time the slope changes by more than 10 percent at mid -range, each time a new stock
standard is prepared, or at least every twelve months. Ref:15A NCAC 2H .0805 (a) (7) (1).
H. Finding: Samples are not being distilled prior to analysis and no distillation study is on file.
Requirement: The titration method requires all samples to be distilled. For all other methods, manual
distillation is not required if comparability data on representative effluent samples are on file to show that
this preliminary distillation step is not necessary; however, manual distillation will be required to resolve
any controversies. Ref: North Carolina Wastewater/ Groundwater Laboratory Certification Policy based
upon Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 72, No. 47, March 12, 2007;
Table IB Footnote 6.
Recommendation: It is recommended that the distilled and undistilled sample portions be analyzed by the same
lab, using the same instrument, technology and methodology to minimize uncertainty introduced by the analysis,
yielding a truer representation of the effect of matrix and the distillation process on sample results.
Cyanide: — Laehat Method, 10-204-001 -X
Comment: The calibration verification standard (same source as calibration standards) was not in the mid range of
the analytical curve. The North Carolina Administrative Code, NCAC 2H .0805 (a) (7) (1) states: For colorimetric
analyses, a series of five standards for a cure prepared annually or three standards for curves established each
day or standards as set forth in the analytical procedure must be analyzed to establish a standard cure. The
cure must be updated as set forth in the standard procedures, each time the slope changes by more than 10
percent at mid -range, each time a new stock standard is prepared, or at least every twelve months. Analytical data
submitted June 30, 2010 addressed this issue. No further response is necessary for this finding
Total Phosphorus — Standard Methods, 18th Edition, 4500 P E
MBAS — Standard Methods, 18th Edition, 5540 C
Inorganic Phenols — EPA Method 420.1
Finding: The laboratory is not analyzing matrix spikes (MS).
Requirement: Unless the referenced method states a greater frequency, spike 5% of samples on a
monthly basis. Laboratories analyzing less than 20 samples per month must analyze at least one matrix
spike each month samples are analyzed. Prepare the matrix spike from a reference source different from
that used for calibration unless otherwise stated in the method. If matrix spike results are out of control,
the results must be qualified or the laboratory must take corrective action to rectify the effect, use another
method, or employ the method of standard additions. When the method of choice specifies matrix spike
performance acceptance criteria for accuracy, and the laboratory chooses to develop statistically valid,
laboratory -specific limits, the laboratory -generated limits cannot be less stringent than the criteria stated in
the approved method. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy.
Recommendation: It is recommended that the spike solution constitutes 51 % of the total MS volume
Recommendation: If the duplicate sample value is near or below the reporting limit, it is recommended that
a Matrix Spike Duplicate (MSD) be analyzed. The MSD fulfills the, duplicate required by 15A NCAC 2H .0805
(a) (7) (C). This would result in better statistical results to monitor method and analyst precision.
Fecal Coliform (MF) — Standard Methods, 18th Edition, 9222 D
J. Finding: Comparison testing is not conducted on the media before a new lot is put into use.
Requirement: It is required that when a new lot of culture medium, pads, or membrane filters is to be
used, a comparison of the current lot in use, (reference lot) against the new lot (test lot), be made. As a
minimum, make single analyses on five positive samples. Ref: Standard Methods, 18t' Edition, 9020 B. (3)
(d).

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# 440 Statesville Analytical Labs
Comment: All other consumable materials were tested.
1V. PAPER TRAIL INVESTIGATION:
No paper trail performed.
V. CONCLUSIONS:
Correcting the above -cited findings and implementing the recommendations will help this lab to produce quality
data and meet certification requirements. The inspector would like to thank the staff for its assistance during the
inspection and data review process. Please respond to all findings.
Report prepared by: Chet Whiting
'Report reviewed by: Jason Smith
Date: July 15, 2010
Date: July20, 2010