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INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #: 628
Laboratory Name: Environmental Chemists, Inc. / Outer Banks Div.
Inspection Type: Commercial Maintenance
Inspector Name(s): Todd Crawford
Inspection Date: November 24, 2009
Date Report Completed: December 10, 2009
Date Forwarded to Reviewer: December 10, 2009
Reviewed by: Tony Hatcher
Date Review Completed: December 11, 2009
Cover Letter to use: Insp. Initial X Insp. Reg. Insp. No Finding Insp. CP
Unit Supervisor: Dana Satterwhite
Date Received: December 14, 2009
Date Forwarded to Alberta: December 14, 2009
Date Mailed:
_____________________________________________________________________
On-Site Inspection Report
LABORATORY NAME: Environmental Chemists Inc. / Outer Banks Div.
NPDES PERMIT #: N/A
ADDRESS: P.O. Box 2228
Manteo, NC 27954
CERTIFICATE #: 628
DATE OF INSPECTION: November 24, 2009
TYPE OF INSPECTION: Commercial Maintenance
AUDITOR(S): Todd Crawford, Tony Hatcher
LOCAL PERSON(S) CONTACTED: Katherine McAvoy, Denise Burroughs
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 lab was generally clean and well organized. All equipment appeared well maintained. Some
additional Quality Control measures are needed.
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
Quality Control
A. Finding: Standard Operating Procedures (SOPs) have not been developed and/or updated 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. Ref: 15A
NCAC 2H .0805 (a) (7).
Comment: The Analytical Quality Control document must include standard operating procedures.
Since there are often changes in technology or options within a particular method that are not
covered in published references, the laboratory SOP is the prescriptive reference document
that describes a laboratory’s analytical procedure in such detail that an experienced analyst
unfamiliar with the method can obtain acceptable results and meet documentation
requirements. This document is intended to be the reference for analysts performing the
specified test procedure. Standard operating procedures must be developed which describe in
detail how a method is performed in that particular laboratory and they must be reviewed
periodically for accuracy. They must be revised any time a change in analytical procedure is
made.
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Requirement: The laboratory must have updated Quality Control/Standard Operating
Procedures documents for the parameters included on the certificate attachment by July 1,
2010. Review SOPs and update as necessary to ensure that: The method is being performed
as stated, references to methods are accurate, the SOP is in agreement with approved practice
and regulatory requirements. This must be submitted for review by July 1, 2010. A written
response is required.
B. Finding: The National Institute of Standards and Technology (NIST) traceable thermometer
(Control Company # 51082499) used to check all laboratory thermometers and temperature
sensing devices was due to be calibrated on April 19, 2007.
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).
C. Finding: All of the thermometers and temperature sensing devices in the lab were checked on
February 5, 2009 using the Control Company thermometer # 51082499, which was expired at
the time.
Requirement: All thermometers, or temperature sensing devices on field meters must meet
NIST specifications for accuracy or must be calibrated against a NIST certified or NIST
traceable thermometer annually (every 12 months) and proper corrections made and
documented. A correction factor must be posted on the meter even if that correction factor is
0ºC. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy.
Requirement: Perform a Temperature Sensor Check for any and all temperature sensing
devices using a thermometer with a current calibration certificate. Submit results to this office
with your reply.
Residual Chlorine – HACH Method 10014 ULR
D. Finding: The flow through cell had growth on the inside walls. This could be due to a buildup of
colored reaction products or algae.
Requirement: Clean and maintain equipment as indicated by manufacturer’s instructions. Ref:
15 A NCAC 2H .0805 (a) (6) (H).
Comment: Equipment required to perform the analysis means properly maintained equipment.
The Hach Water Analysis Handbook Third Edition (pg. 389) states that the Pour-Thru Cell may
accumulate a buildup of colored reaction products, especially if the reacted solutions are
allowed to remain in the cell for long periods after measurement. Remove the buildup by rinsing
the cell with 5.25 N sulfuric acid followed by rinsing with deionized water.
NO2 + NO3 Nitrogen - Standard Methods, 18th Edition, 4500 NO2 B & NO3 E
Ammonia Nitrogen - Standard Methods, 18th Edition, 4500 NH3 F
E. Finding: The QC standard and spike true values, as well as, their percent recoveries are not
documented on the benchsheet.
Requirement: A blank and mid-range standard must be analyzed after every tenth sample and
at the end of each sample group to check for calibration drift. If either fall outside established
quality control acceptance criteria, corrective action must be taken (e.g., repeating sample
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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) and 3020 B 2 (b).
Requirement: Unless the referenced method states a greater frequency, include one Matrix
Spike (MS) with each sample set (batch – 20 or fewer samples) or on a 5% basis. Prepare
the MS from a reference source different from that used for calibration unless otherwise
stated in the method. Laboratories analyzing less than 20 samples per month must analyze at
least one MS each month samples are analyzed. If MS 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. Refer to the method of choice
for specific acceptance criteria for the MS until the laboratory develops or adopts statistically
valid, laboratory-specific performance criteria for accuracy. Ref: North Carolina
Wastewater/Groundwater Laboratory Certification Policy.
Requirement: Supporting records shall be maintained as evidence that these practices are
being effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).
Ammonia Nitrogen - Standard Methods, 18th Edition, 4500 NH3 F
F. Finding: The distillation study was due to be repeated in October 2009.
Requirement: Commercial Laboratories shall analyze initially at least six samples distilled and
undistilled, but at least two samples from all waste types. Analyze one sample distilled and
undistilled yearly from all wastes types. 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 1B Footnote 6.
Recommendation: Samples with a concentration < 1.0 mg/L should be spiked to yield a value
in the 1 – 5 mg/L range. Comparisons performed in this concentration range should check
within 20% RPD. Additional samples must be analyzed comparatively if the results do not
indicate approximately the same values for distilled and undistilled samples. It is recommended
that both the distilled and undistilled portions of the sample be analyzed by the same laboratory
using the same methodology.
Comment: This laboratory is not equipped to perform distillations. It is recommended that
samples from this lab be sent to the parent lab in Wilmington, NC for the distillation study. It is
recommended that same lab analyze both the distilled and undistilled samples.
BOD - Standard Methods, 18th Edition, 5210 B
Recommendation: The BOD benchsheet has been photocopied so many times that the column
headings are practically unreadable. Please reprint the benchsheet from the original or create a new
benchsheet. Make sure the new benchsheet provides space to document the addition of extra nutrients
for sample dilutions that contain more than 201 mL of sample.
G. Finding: The time that samples were taken out of the incubator on 08/05/09 was 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
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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: In-house guidelines state that duplicates must agree within 10%, however,
calculations to determine if they do are not being done.
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).
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).
I. Finding: Extra nutrient, mineral, and buffer solutions are not added to the sample bottles
containing more than 67% sample.
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 mL/L (0.33 mL/300-mL bottle) or use commercially-prepared
solutions designed to dose the appropriate bottle size. Ref: North Carolina
Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods, 20th
Edition, 5210 B. (4) (f) and Standard Methods, 21st Edition, 5210 B. (5) (c) (2).
Recommendation: It is recommended that a powder pillow for a 300-mL sample bottle be
used. Dilution water would be prepared as it currently is and for the bottles containing more
than 67% sample, one powder pillow would be added in addition to the dilution water containing
the nutrient solutions.
Documentation
J. Finding: Error corrections are being made with a single line but there no dates or initials.
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.
IV. PAPER TRAIL INVESTIGATION:
Raw data is sent the Wilmington office for final report generation. No paper trail performed.
V. CONCLUSIONS:
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Correcting the above-cited findings and implementing the recommendations will help this lab to
produce quality data and meet certification requirements. The inspectors 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: December 10, 2009
Report reviewed by: Tony Hatcher Date: December 11, 2009