HomeMy WebLinkAbout#161-final_ammended
INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #: 161
Laboratory Name: Whiteville WWTP Lab
Inspection Type: Municipal Maintenance
Inspector Name(s): Todd Crawford
Inspection Date: February 1, 2011
Date Report Completed: February 21, 2011
Date Forwarded to Reviewer: February 21, 2011
Reviewed by: Jason Smith
Date Review Completed: February 25, 2011
Cover Letter to use: ___ Insp. Initial X Insp. Reg. Insp. No Finding Insp. CP
Unit Supervisor: Dana Satterwhite
Date Received: February 25, 2010
Date Forwarded to Alberta: March 9, 2011
Date Mailed: March 9, 2011
_____________________________________________________________________
On-Site Inspection Report
LABORATORY NAME: Whiteville WWTP Lab
ADDRESS: P.O. Box 607
Whiteville, NC 28472
CERTIFICATE #: 161
DATE OF INSPECTION: February 1, 2011
TYPE OF INSPECTION: Municipal Maintenance
AUDITOR(S): Todd Crawford
LOCAL PERSON(S) CONTACTED: Newlyn McCullen
I. INTRODUCTION:
This laboratory was inspected to verify its compliance with the requirements of 15A NCAC 2H .0800 for the analys is
of environmental samples.
II. GENERAL COMMENTS:
The laboratory was well equipped, neatly organized and clean. The staff was extremely helpful and professional.
The Standard Operating Procedures (SOPs) were well written, although not all were up to date with current Quality
Control requirements.
Findings D, I, N, Q, R, and S are new policies that have been implemented by our program since the last inspection.
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
Documentation
A. Finding: The use of Wite-Out®, as well as several instances of writing over a number as a means of error
correction, and corrections without dates and initials 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-Out®,
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.
B. Finding: The grab sample collection time (for all parameters) does not indicate that it is from the effluent.
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).
C. Finding: The Dissolved Oxygen field meter calibration time is not being documented. Th is is considered
pertinent information.
Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so
as to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A).
Page 2
#161 Whiteville WWTP Lab
General Quality Control
D. Finding: The preparation of standards and reagents is not documented in such a way as to provide a
traceable history from analysis to manufacturer.
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.
Comment: Forms for documenting traceability of purchased and prepared standards and reagents were
provided to the laboratory at the time of the inspection.
E. Finding: The NIST traceable thermometer (ERTCO #1337) was due for calibration on April 23, 2003.
After the calibration due date, the thermometer is no longer considered traceable to NIST specifications.
Requirement: All thermometers must meet National Institute of Standards and Technology (NIST)
specifications for accuracy or checked, at a minimum annually, against a NIST traceable thermometer and
proper corrections made. Ref: 15A NCAC 2H .0805 (a) (7) (O).
Comment: You may have trouble getting your NIST thermometer re-certified. As part of an initiative to
reduce the use of mercury in products, EPA is working with stakeholders to reduce the use of mercury-
containing non-fever thermometers in industrial and commercial settings. The National Institute of
Standards and Technology (NIST), which is working with EPA on this effort, announced on February 2,
2011 that it will no longer calibrate mercury-in-glass thermometers for traceability purposes beginning on
March 1, 2011. Other vendors may follow this lead. Additional information on the phase-out of mercury-
filled thermometers and selecting alternatives to mercury-filled thermometers can be found on the
following EPA website: http://www.epa.gov/hg/thermometer.htm .
F. Finding: All thermometers and temperature sensing devices were checked against the expired NIST
traceable thermometer (ERTCO #1337).
Requirement: All thermometers must meet NIST specifications for accuracy or checked, at a minimum
annually, against a NIST traceable thermometer and proper corrections made. Ref: 15A NCAC 2H .0805
(a) (7) (O).
G. Finding: SOPs have not been updated with current quality control requirements for all of the parameters
included on the laboratory’s certificate attachment.
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). Submit the
updated SOPs for review by August 1, 2011. A written response is required.
H. Finding: The Class 1 balance weights have not been certified within the past 5 years.
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.
Page 3
#161 Whiteville WWTP Lab
I. Finding: The mechanical pipettes have not been properly calibrated.
Requirement: Mechanical volumetric liquid-dispensing devices (e.g., fixed and adjustable auto-pipettors,
bottle-top dispensers, etc.) must be calibrated at least twice per year, approximately six months apart and
documented. Each liquid-dispensing device must meet the manufacturer’s statement of accuracy. Ref:
North Carolina Wastewater/Groundwater Laboratory Certification Policy.
Comment: Aliquots dispensed from the pipette should be weighed in order to determine the volume
dispensed. Guidance information was provided at the time of the inspection.
Temperature – Standard Methods, 18th Edition, 2550 B
J. Finding: The temperature readings are not being performed immediately.
Requirement: The hold time in the Federal Register is listed as “Analyze”. Ref: Code of Federal
Regulations, Title 40, Part 136; Federal Register Vol. 72, No. 57, March 26, 2007; Table II.
Coliform, Fecal – Standard Methods, 18th Edition, 9222 D (MF)
K. Finding: Samples are allowed to sit on the bench at room temperature for up to 2 hours after collection
and before beginning analysis.
Requirement: Unless analysis is begun within 15 minutes of collection, preserve to < 10ºC. Ref: Code of
Federal Regulations, Title 40, Part 136.3; Federal Register Vol. 72, No 57, March 26, 2007; Table II,
Footnote 2.
Comment: Although the temperature may not reach < 10ºC before analysis begins, the temperature of
the sample must begin a downward trend within 15 minutes of collection.
Comment: Sample analysis should begin immediately, preferably within 2 hours of collection. The
maximum transport time to the laboratory is 6 hours, and samples should be processed within 2 hours of
receipt at the laboratory. Ref: Code of Federal Regulations, Title 40, Part 136.3; Federal Register Vol. 72,
No 57, March 26, 2007; Table II, Footnote 22.
L. Finding: Samples are not consistently checked for chlorine prior to analysis.
Requirement: Dechlorinating agents used at the time of sampling must be documented to have been
effective upon the receipt into the laboratory. A variety of field testing kits are considered to be adequate
for most residual chlorine checks and a maximum detection limit of 0.5 mg/L is allowed. Ref:
Memorandum: Required Documentation for Sample Preservation and Hold Time, Pat Donnelly, June 20,
2007.
Comment: The Total Residual Chlorine analysis has been used as the total residual chlorine check;
however, this practice is acceptable only if the Total Residual Chlorine analysis is performed at the same
time as the collection of the Fecal Coliform sample.
Biochemical Oxygen Demand – Standard Methods, 18th Edition, 5210 B
M. Finding: The initial pH and final pH of pH adjusted samples are not being documented.
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. The quality control document shall be available for inspection by the State Laboratory. Ref:
15A NCAC 2H .0805 (a) (7).
Ammonia Nitrogen – Standard Methods, 18th Edition, 4500 NH3 F
N. Finding: The laboratory is not analyzing matrix spikes.
Page 4
#161 Whiteville WWTP Lab
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 s pike 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.
If the unspiked sample result is in the top 40% of the calibration range, the sample should be diluted and
the matrix spike prepared using the diluted sample. The recovery of the matrix spike samples must be
bracketed by the calibration range.
The volume of spike solution used in matrix spike preparation must in all cases be ≤ 10% of the total
matrix spike volume. It is preferable that the spike solution constitutes ≤ 1% of the total matrix spike
volume so that the matrix spike can be considered a whole volume sample with no adjustment by
calculation necessary. If the spike solution volume constitutes >1% of the total sample volume, the sample
concentration or spike concentration must be adjusted by calculation.
Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy.
O. Finding: The raising of the pH above 11 Standard Units (S.U.) prior to analysis is not being confirmed and
documented.
Requirement: Add sufficient volume of 10N NaOH solution (1 mL usually is sufficient) to raise pH above
11. Ref: Standard Methods, 18th Edition, 4500 NH3 F (4) (b).
P. Finding: A calibration blank and calibration verification standard (mid-range) are not analyzed at the end
of the sample group.
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).
Comment: The calibration verification standard is prepared from the calibration stock standard solution.
Residue, Suspended – Standard Methods, 18th Edition, 2540 D
Q. 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 21st 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.
R. Finding: Filters are not weighed to constant weight prior to sample analysis, nor is a dry filter blank analyzed
with each set of samples.
Page 5
#161 Whiteville WWTP Lab
Requirement: If pre-prepared filters are not used, the method requires that filters must be weighed to a
constant weight after washing. Repeat cycle of drying, cooling, desiccating, and weighing until a constant
weight is obtained or until weight change is less than 4% of the previous weighing or 0.5 mg, whichever is
less. In lieu of this process, it is acceptable to analyze a single daily dry filter blank to fulfill the method
requirement of drying all filters to a constant weight prior to analysis. Ref: North Carolina
Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods 20th Edition 2540
D. (3) (a).
S. Finding: The drying time study was done with a blank filter instead of actual samples.
Requirement: Constant weights must be documented. The approved methods require the following:
“Repeat the cycle of drying, cooling, desiccating, and weighing until a constant weight is obtained or until
the weight change is less than 4% of the previous weight or 0.5 mg, whichever is less.” In lieu of this, an
annual study documenting the time required to dry representative samples to a constant weight may be
performed. Verify minimum daily drying time is greater than or equal to the time used for the initial
verification study drying cycle. Drying cycles must be a minimum 1 hour for ve rification. Ref: North
Carolina Wastewater/Groundwater Laboratory Certification Policy based on Standard Methods, 20th
Edition, 2540 D. (3) (c), 2540 B. (3) (b), and 2540 C. (3) (d).
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: Todd Crawford Date: February 21, 2011
Report reviewed by: Jason Smith Date: February 25, 2011