HomeMy WebLinkAboutNC0037508_Lab Certification Inspection_20081014October 14, 2008
134
Ms. Janna Scherer
Moore Co. Water Pollution
1094 Addor Road
Aberdeen, NC 28315-
Michael F. Easley, Governor.
WilliamG. Ross Jr., Secretary
North Carolina Department of Environment and Natural Resources
Coleen H. Sullins, Director
Division of Water Quality
RECEIVED
OCT 171008
OBVR-FAYETTEVILLE REGIONALOFFFICE
SUBJECT: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Laboratory Certification Maintenance Inspection
Dear Ms. Scherer :
Enclosed is a report for the inspection performed on September 16, 2008 by Ms. Tonja
Springer . 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 us at 919-733-3908.
Sincerely,
Dana Satterwhite
Certification Unit Supervisor
Laboratory Section
Enclosure
cc: Tonja Springer
Fayetteville Regional Office
- r Carolina
IVoatura!!y
North Carolina Division of Water Quality 1623 Mail Service Center Raleigh, NC 27699-1623 Phone (919) 733-3908 Customer Service
Internet: www.dwglab.org Location: 4405 Reedy Creek Rd Raleigh, NC 27607 Fax (919) 733-6241. 1-877-623-6748
An Equal Opportunity/Affirmative Action Employer— 50% Recycled/10% Post Consumer Paper
On -Site Inspection Report
LABORATORY NAME: Moore County Water Pollution
NPDES PERMIT #:. NC0037508
ADDRESS: 1094 Addor Road
Aberdeen, NC 28315
CERTIFICATE #: 134
DATE OF INSPECTION: September 16, 2008
TYPE OF INSPECTION: Commercial Maintenance
AUDITOR(S): Tonja Springer
LOCAL PERSON(S) CONTACTED: Janna Scherer
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:
Laboratory benchsheets and supporting documentation were accurate and complete and the traceability
procedures in place were effective and easy to follow. The laboratory is of adequate size and is well equipped.
Comment: The following findings: A, B, C, and E are new policies that have been implemented by our program
since the last inspection..
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
General Laboratory
A. Finding: Error corrections are not dated.
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 (NC WW/GW LC)
Policy, 11/30/2007.
BOD — Standard Methods, 18th Edition, 5210 B
Comment: Because of the recent Method Update Rule (MUR) to the Federal Register, there are now four approved
Standard Methods (18th, 19th, 20th, and 21st Editions) for BOD. As a result, North Carolina Wastewater/Groundwater
Laboratory Certification has added or changed some of its requirements for BOD analysis and quality control
evaluation to provide continuity between our program and the approved methods. The comments listed below are
in relation to the recent changes.
Comment: When BOD sample results must be qualified, the qualifying statement on, the laboratory report form or
the Discharge Monitoring Report (DMR) must state that all QC requirements were not met, and the description of
the QC failure involved when that is the case. (See. Attachment for Flagging QC Failures)
Page 2
#134 Moore County Water Pollution
Comment: For dilutions with >67% sample (i.e., >201 mL when the total volume is 300 mL) extra nutrients must
be added. The way to do this is to use pillows made for 300 mL bottle size. Add 1 pillow to each bottle containing
more than 201 mL sample. Ref: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW
LC) policy; based upon Standard Methods, 20th Edition — Method 5210 B. (4) (f). and Standard Methods, 21st Edition —
Method 5210 B. (5) (c) (2):
Total Suspended Solids - Standard Methods, 18th Edition, 2540 D
B. Finding: A minimum dried residue weight gain of 1 mg is used to determine the reporting limit.
Requirement: 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. Ref: North Carolina
Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) Policy, 09/11/08; based upon
Standard Methods, 20thand 21st Editions - Method 2540 D. (3) (b).
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.
�H — Standard Methods, 18th Edition, 4500 H+B
Comment: The temperature sensor on the pH meter has been calibrated against a NIST thermometer; however; the
serial number of the NIST thermometer that was used for the comparison was not documented. Document the serial
number and manufacturer of the NIST thermometer that was used in the comparison. Ref: North Carolina
Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) Policy.
C. Finding: The temperature at which pH is measured is not documented.
Requirement: Document the temperature at which the pH sample(s) are analyzed. Ref: Standard Methods
18th Edition — Method 4500H+ B. (1) (b).
Ammonia - Standard Methods, 18th Edition, 4500 — NH3 F
D. Finding: The laboratory is not distilling samples and an annual distillation comparison study has not been
performed.
Requirement: Municipal and Industrial laboratories shall analyze initially four samples distilled and
undistilled from each discharge and, thereafter, analyze two samples a year from each effluent. Additional
samples must be analyzed comparatively if the above samples results do not indicate approximately the
same values for distilled .and undistilled samples. Ref: Code of Federal Regulations, Title 40, Part 136;
Federal Register Vol. 72, No. 47, March 12, 2007; Table 1 B, Footnote 6.
Recommendation: Samples may need to be spiked when performing the comparison if the ammonia
concentration in the sample is low (i.e., < 1 mg/L). It is recommended that the samples be spiked to a
concentration of at least 1 to 5 mg/L.
E. Finding: A calibration verification standard (CVS) and blank are not analyzed at the end of the sample
run.
Requirement: The calibration blank and mid -range standard must be analyzed 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:
Page 3
#134 Moore County Water Pollution
North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) Policy, 01/28/08;
based upon Standard Methods 20th Edition — Methods 1020 B. (10) (c), 3020 B. (2) (b), and 4020 B. (2).
Fecal — Standard Methods, 18th Edition, 9222 D
Recommendation: The acceptance limits for precision have not been updated in several years. It is recommended
the acceptance limits be evaluated at a minimum annually.
F. Finding: The laboratory is not performing the consumables testing on the laboratory supplies being used in
the Fecal Coliform analyses.
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, 18th Edition — Method
9020 B. (3) (d). (See Attachment).
Total Residual Chlorine — Standard Methods, 18th Edition, 4500 CI G
Recommendation: The meter that is used for the field analysis is verified in the morning but the sample analysis
is not performed until later in the afternoon. It is recommended that the meter verification be performed just prior
to the analysis.
Comment: When a factory -set calibration is used, a second source standard is no longer required each analysis
day. A single daily check standard and blank satisfy dailyquality control requirements. Ref: North Carolina
Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) Policy, 09/10/2008.
IV. PAPER TRAIL INVESTIGATION:
The paper trail consisted of comparing field testing records and contract lab reports to Discharge Monitoring Reports
(DMRs) submitted to the North Carolina Division of Water Quality. Data were reviewed for NPDES permit
NC0037508 for January, April and August 2008. No transcription errors were detected. The facility appears to be
doing a good job of accurately transcribing data.
V. CONCLUSIONS:
Correcting the above -cited findings and implementing the recommendation 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: Tonja Springer Date: October 8, 2008
Report reviewed by: Tony Hatcher Date: October 10, 2008
Flagging BOD Quality Control Failures
It is the intent 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 this section 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).
This means all data are reported and none are rejected by the laboratory or permittee. If all quality control
requirements are not met, it is required that the data are flagged and the qualifications appear on the back of the
Discharge Monitoring Report (DMR). Any rejection of data will be issued by the agency which receives the data.
NC WW/GW LC policy for flagging quality control failures is based upon the Quality Control requirements of the
method as outlined in Standard Methods, 21st Edition — Method 5210 B. (7) (b) which states: "Identify results in the
test reports when any of the following quality control parameters are not met:"
Anytime any ofthe following quality control failures occur the data must be flagged.
1. No sample dilutions deplete at least 2.0 mg/L DO and have a residual of at.
least 1.0 mg/L DO (unless 100% sample is analyzed).
2. The dilution water blank is greater than 0.20 mg/L.
3. The Glucose - Glutamic Acid (GGA) check falls outside the acceptance limits
(i.e., 198 mg/L ± 30.5 mg/L or 167.5 - 228.5 mg/L). When multiple GGA
standards are analyzed, the average of those results must be within the
acceptable limits.
4. Duplicates vary more than 30% between low and high values.
5. No seed control dilutions deplete at least 2.0 mg/L DO and have a
residual of at least 1.0 mg/L DO.
The qualifying statement on the laboratory report form and/or the Discharge Monitoring Report (DMR) must state:
1. All QC requirements were not met, and
2. What the QC failure involved. For example, "blank was >0.20 mg/L", "GGA was
less than 167.5 mg/L", "duplicates exceeded 30% difference due to low BOD
concentration", etc.
It is recommended that the laboratory supervisor include a statement indicating whether the data is considered
"valid", "questionable", or "invalid". This is a subjective decision based upon the severity of the QC failure and its
impact on the value reported.
Data must always be reported. Accompanying documentation may be attached to justify any data believed to be
invalid.
NC DENR/DWQ LABORATORY CERTIFICATION
Testing of Consumable Materials for Fecal Coliform MF Method
Standard Methods requires that before a new lot of consumable materials are used for the Fecal Coliform MF
method, those materials be tested to ensure they are reliable. North Carolina policy requires the testing of the
following consumable materials before they can be used for sample analyses: membrane filters and/or pads (often
packaged together) and media. Test only one consumable at a time.
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, 18th Edition - Method 9020 B.3d. (page 9-7).
The following is provided as guidance in performing the required testing. Let's say you got a new batch of
membrane filters in. We will call the currently used filters lot #1 and the new filters lot #2.
1. Select a culture positive sample.
What you want is something that will yield 20-60 colonies when a reasonable sample volume is filtered. This may
be a stream sample or a sample taken somewhere within the waste treatment plant. If the concentration is high
enough that greater than 60 colonies are obtained when 1 mL is filtered then the solution is too strong and must
be diluted. Any time a sample is diluted be sure it is done with the BUFFERED dilution water used for rinsing the
funnels.
2. Test the culture positive to determine the appropriate volume to use.
When collecting the culture positive sample do not think about it as a sample. You do not have to be concerned
with a sterile sample bottle or 6 hour hold time. Collect enough sample so that you have plenty to work with,
probably more than your normal fecal bottle holds. Set a series of dilutions using the currently used materials, in
this example filter lot #1. Do not use the materials you want to prove are OK at this point. All you are trying to do is
to determine the volume of sample that will yield 20-60 colonies. Put the rest of the sample in the refrigerator. For
example:
Volume used Colonies obtained on lot #1 filters
50 ml TNTC
25 ml 138
10 ml 50
5 ml 22
1 ml 4
Based on this preliminary testing it appears that a 10 ml volume would probably be appropriate to use and will yield
the desired 20-60 colonies. Remember when you do the actual consumable test, the culture positive sample will
be 24 hours old and the results you obtain may be lower than the initial results yielded, but not so significantly
lower as to change your dilution choice. It is better to have your initial results on the high side of the 20-60 range
for this reason. In this example the 5 ml volume would probably be too low and would likely yield less than 20
colonies the next day.
3. Perform the consumable test
Once you determine the appropriate volume, in this case 10 mis, take the remaining culture positive sample from
the refrigerator, bring to room temperature and set five 10 ml plates with the currently used filters, lot #1, and five
10 ml plates with the new filters, lot #2.
4. Determine acceptability of new material
For example:
Lot #1-current filters Colonies obtained on lot #1 filters
10 ml 48
10m1 45
10 ml 50
10 mI
10 ml
44
43
Average: 46
Lot #2-new filters Colonies obtained on lot #2 filters
10m1 40
10m1 45
10mi 38
10ml 46
10ml 37
Average: 41
When determining the acceptability of the new material, compare the average of the five replicates for lot #1 to the
average of the five replicates for lot #2; that is 46 vs. 41 colonies. The recommended acceptance criteria would be
your current acceptance criteria used for your Fecal Coliform duplicates. If the test and reference materials check
within what you have determined is acceptable for duplicates of samples, the test material would be considered
acceptable to use. This may be a calculated acceptance criteria based on 3 times the standard deviation of the
mean or a set value like 20% RPD. No matter how you determine your duplicate acceptance criteria make sure
you use colony counts not final calculated values in doing this. Other factors to consider when determining if a
new material is suitable include:
Are the colonies obtained typical, that is normal looking blue colonies?
Are the colonies evenly distributed across the membrane surface?
Are there an unusual number of non typical colonies present?
Is there a pattern to the colony recoveries? For example are all the plates for the test materials significantly lower
in counts than the reference lot?
It is recommended that new consumables be tested as soon as possible after receipt to avoid problems" if the
materials are not acceptable. Once you determine that the new material is acceptable to use; you may begin to do
so. Document the date the new lot # is put into use.
Revised 2/06