#226 -08 - 2010 - FINAL

INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #:
226
Laboratory Name:
Spruce Pine WWTP Lab
Inspection Type:
Municipal Maintenance
Inspector Name(s):
Jason Smith
Inspection Date:
August 17, 2010
Date Report Com leted`
September 29 2010
Date Forwarded to Reviewer:
September 29 2010
Reviewed bv:
Jeff Adams
Date Review Completed:
October 1 2010
Cover Letter to use:
Insp. Initial X Insp. Reg. Insp, No Finding Insp. CP
Unit Supervisor:
Gary Francies
Date Received:
10/1/10
Date Forwarded to Alberta:
% �'o & WF7
Date Mailed:

Beverly Eaves Perdue
Governor
226
Mr. Darrell Graham
Spruce Pine WWTP Lab
P.O. Box 189
Spruce Pine, NC 28777
i .
NCDENR
�rarrorrrr
North Carolina Department of Environment and Natural Resources
Division of Water Quality
Coleen H. Sullins
Director
October 6, 2010
SUBJECT: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Mr. Graham:
Dee Freeman
Secretary
Enclosed is a report for the inspection performed on August 17, 2010 by Jason Smith. 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,
C
Gary Francies
Unit Supervisor
Laboratory Section
CC: Jason Smith
Central files
DRNR D+NQ 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]
Internet: www.dwglab.org
An Equal Opportunity\Affirmative Action Employer Customer Service:1-877-623-6748 www.ncwaterquality.arg
NorthCarolina

LABORATORY NAME:
NPDES PERMIT #:
:ITRr;
CERTIFICATE #:
DATE OF INSPECTION:
TYPE OF INSPECTION:
AUDITOR(S):
LOCAL PERSON(S) CONTACTED:
I. INTRODUCTION:
Spruce Pine WWTP Lab
NCO021432
P.O. Box 189
Spruce Pine, NC 28777
226
August 17, 2010
Municipal Maintenance
Jason Smith
Darrell Graham, Phillip Burleson, and Bob Haller
This laboratory was inspected to verify its compliance with the requirements of 15A NCAC 2H .0800 for
the analysis of environmental samples.
11. GENERAL COMMENTS:
The laboratory was clean and well organized. The facility has all the equipment necessary to perform the
analyses. Findings C, D, E, F, G, J, K, N and O are new policies that have been implemented by our
program since the last inspection.
III. FINDINGS REQUIREMENTS COMMENTS AND RECOMMENDATIONS:
General Laboratory
Comment: The laboratory was not clearly labeling process control data to differentiate between
regulatory and non -regulatory data.
Recommendation: Clearly document all process control data as such on the benchsheet.
A. Finding: The laboratory's Standard Operating Procedures (SOP's) have not been updated since
2002.
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. The quality
control document shall be available for inspection by the State Laboratory, Ref: 15A NCAC 2H
.0805 (a) (7).
Comment: Please submit updated SOPs for all certified parameters by April 6, 2011.
Recommendation: It is recommended that SOP's be reviewed annually and that the date of
review or revision be documented.

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#226 Spruce Pine WWTP Lab
B. Finding: Several instances of the use of correction fluid were observed.
Requirement: All documentation errors must be corrected by drawing a single line through the
error so that the original entry remains legible. Entries shall not be obliterated by erasures or
markings. Wite-OutO, correction tape or similar products designed to obliterate documentation
are not to be used. Write the correction adjacent to the error. The correction must be initialed
by the responsible individual and the date of change documented. All data and log entries must
be written in indelible ink. Pencil entries are not acceptable. Ref: North Carolina Wastewater/
Groundwater Laboratory Certification Policy.
C. Finding: The reagent receipt log did not include the date opened and expiration date.
Requirement: All chemicals, reagents, standards and consumables used by the laboratory must
have the following information documented: Date received, Date Opened (in 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 and/or 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 pre -made standards and/or
media, solids and bacteria filters, etc. are included in this requirement. Ref: North Carolina
Wastewater/Groundwater Laboratory Certification Policy.
D. Finding: The analytical balance weights have not been verified against ASTM standard
weights.
Requirement: ASTM Class 1 and 2 weights must be verified at least every 5 years. ASTM
Class 1 weights (20 g to 25 kg) and ASTM Class 2 weights (10 g to 1 mg) are equivalent to the
NBS Class S weights specified in 15A NCAC 2H .0805 (a) (7) (K). Ref: North Carolina
Wastewater/Groundwater Laboratory Certification Policy. See attachment for additional
guidance.
pH — Standard Methods, 18'h Edition, 4500 H+ B
Dissolved Oxygen — Standard Methods, 18'h Edition, 4500 O G
E. Finding: The temperature sensor for the pH meter has not been checked against a NIST certified
or NIST traceable thermometer.
Requirement: All thermometers and temperature measuring devices must be checked every12
months against a NIST certified or NIST traceable thermometer and the process documented. To
check a thermometer or the temperature sensor of a meter, read the temperature of the
thermometer/meter against a NIST certified or NIST traceable thermometer and record the two
temperatures. The calibration must be performed at a temperature that corresponds to the
temperature used by the incubator, refrigerator, freezer, etc. In the case of temperature
measuring devices used to perform variable temperature readings the calibration must be
performed at a temperature range that approximates the range of the samples. The
thermometer/meter readings must be less than or equal to 10C from the NIST certified or NIST
traceable thermometer reading. The documentation must include the serial number of the NIST
certified thermometer or NIST traceable thermometer that was used in the comparison. Also
document any correction that applies (even if zero) on both the thermometer/meter and on a
separate sheet to be filed. (NOTE: Other certified laboratories may provide assistance in

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#226 Spruce Pine WWTP Lab
meeting this requirement.) Ref: North Carolina Wastewater/Groundwater Laboratory Certification
Policy.
F. Finding: —The temperature correction was not posted on the Dissolved Oxygen (DO) and pH
meters.
Requirement: See required above for Finding E.
Temperature — Standard Methods, 18'h Edition, 2550 B
Dissolved Oxygen — Standard Methods, 18'h Edition, 4500 O G
Recommendation: It is recommended that the benchsheet clearly indicate that samples are analyzed in
stream.
pH — Standard Methods, 18'h Edition., 4500 H+ B
G. Finding: Proper units of measure (Standard Units or S.U.) were not documented.
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. The date and time BOD and
coliform samples are removed from the incubator must be included on the laboratory worksheet.
Ref: 15A NCAC 2H .0805 (a) (7) (H).
H. Finding: The calibration does not always bracket the sample pH.
Requirement: Choose buffers that bracket the sample. Ref: Standard Methods, 18" Edition, 4500
H+ B. (1) (a).
Comment: The laboratory calibrates the meter with 4 and 7 S.U. buffers and then checks a 6
S.U. buffer. Checking a 10 S.U. buffer, rather than the 6, would fulfill this requirement.
Total Residual Chlorine —Standard Methods, 18'h Edition, 4500 Cl G
I. Finding: The concentration of the Performance Testing (PT) sample was outside of the
concentration range of the standards used to verify the internal program annually.
Requirement: For analytical procedures requiring analysis of a series of standards, the
concentrations of these standards must bracket the concentration of the samples anal. 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) (1).
Comment: The laboratory verified the meter using the following concentrations: 20, 25, 50, 75,
and 100 lag/L. The PT sample concentration was 164 lag/L.
Recommendation: It is recommended that the laboratory verify the curve using the following
concentrations: 20, 40, 50, 100, and 400 lag/L. The CVS would be 200. pg/L.
J. Finding: A calibration blank and CVS (mid -range) are not analyzed at the end of the sample
group.

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#226 Spruce Pine WWTP Lab
Requirement: The calibration blank and calibration verification standard (mid -range) 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, 20th Edition, 1020 B. (10) (c), 3020 B. (2) (b), and 4020 B. (2).
Total Suspended Solids - Standard Methods, 181h Edition, 2540 D
K. Finding: A minimum dried residue weight gain of 1 mg is used to determine the reporting limit.
Requirement: The minimum weight gain allowed by any approved method is 2.5 mg. Choose
sample volume to yield between 2.5 and 200 mg dried residue. This establishes a minimum
reporting value of 2.5 mg/L when 1000 mL of sample is analyzed. If complete filtration takes
more than 10 minutes increase filter diameter or decrease sample volume. 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. Ref: North Carolina Wastewater/Groundwater
Laboratory Certification Policy based upon Standard Methods, 20th and 21" Editions, 2540 D.
(3) (b).
Comment: 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.
Biochemical Oxygen Demand - Standard methods, 18th Edition, 5210 B
Comment: Although no samples have been analyzed in over a year with > 67% of sample, please be
aware of the following policy: 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 mL/L (0.33 mL/300-mL bottle) or use commercially -prepared solutions designed to dose
the appropriate bottle size.
Recommendation: The 216t Edition of Standard Methods requires that the dilution water blank DO
uptake in 5 days must not be more than 0.20 mg/L and preferably not more than 0.10 mg/L It is
recommended that the laboratory read the DO measurements to two decimal points in order to clearly
document this method criterion..
Fecal Coliform - Standard Methods, le Edition, 9222 D
L. Finding: Samples are not properly preserved between collection and analysis. They are allowed
to sit out at room temperature for one to two hours.
Requirement: Except where noted in this Table II and the method for the parameter, preserve
each grab sample within 15 minutes of collection. Ref: Code of Federal Regulations, Title 40,
Parts 136 and 503; Federal Register Vol. 72, No. 57, March 26, 2007; Table 11, Footnote 2.
M. Finding: Although not needed, a preservative to neutralize chlorine is being used. Additionally, it
is an improper preservative (Sodium Sulfite).
Requirement: Add a reducing agent only if an oxidant (e.g,, chlorine) is present. Reducing agents
shown to be effective are sodium thiosulfate, ascorbic acid, sodium arsenite, or sodium

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4226 Spruce Pine WWTP Lab
borohydride. Ref: Code of Federal Regulations, Title 40, Parts 136 and 503; Federal Register
Vol. 72, No. 57, March 26, 2007; Table 11, Footnote 5.
Cornmen#;—T-he-analysis-of—Total-Residual-Chlorine-at the -time -of -the -fecal -sample -collection
indicates if neutralization is required. If no residual chlorine is present, do not add any
dechlorination chemical.
Ammonia Nitrogen -- Standard Methods, 18t" Edition, 4500 NH3 F
N. Finding: While a CVS is analyzed at the end of the sample run, a CVS is not analyzed at the
beginning of the sample set.
Requirement: The calibration blank and calibration verification standard (mid -range) 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, 20"' Edition, 1020 B. (10) (c), 3020 B. (2) (b), and 4020 B. (2),
O. Finding: The laboratory is not analyzing matrix spikes.
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.
IV. 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: Jason Smith Date: September 29, 2010
Report reviewed by: Jeffrey R. Adams Date: October 1, 2010

Weight Verification (NC WW/GW LC Policy 05123/2008)
ASTM Class 1 and 2 weights must be verified at least every 5 years. ASTM Class 1 weights (20 g to 25
kg) and ASTM-Class 2 weights (10 g to 1 mg) are equivalent to the NBS Class S weights specified --in
15A NCAC 2H .0805 (a) (7) (K). Verification may be accomplished by:
........ .tj -,'Y - _✓ ' w '.— .,—­..— — ..., —w '. .
be calibrated by a body that can provide traceability to ASTM specifications, or
2. Checking laboratory weights against certified reference weights (i.e., weights that have been
recertified as above) and found to be within ASTM Class 1 or Class 2 tolerances (see table
below) - often the balance service technician may provide this service.
Note: Although some manufacturers will assign a one-year calibration due date, 5 years is considered
an acceptable calibration interval due to the limited use of the reference weight set.
Documentation of weight verifications or recertification must be maintained for 5 years. If the condition
of a weight(s) is in question at any time due to damage (e.g., corrosion, nicks, scratching, etc.), the
laboratory must have that weight(s) re -verified as described above.
Maximum tolerances (Ref. ASTM E 617-97, 2003)
Denomination
Maximum tolerance for
ASTM Class 1 and 2
weights, i m
5009
1.2
300 g
0.75
200 g
0.50
100 g
0.25
50 g
0.12
30 g
0.074
209
0.074
10 g
0.074
59
0.054
3 g
0.054
2 g
0.054
1 g
0.054
500 mg
0.025
300 mg
0.025
200 mg
0.025
100 mg
0.025
50 mg
0,014
30 mg
0.014
20 m
0.014
10 mg
0.014
5 mg
0.014
3 mg
0.014
2 mg
0.014
1 mg
0.014