HomeMy WebLinkAbout#654_11_2014_FINALA'4
North Carolina Department of Environment and Natural Resources
Pat McCrory
Governor
November 21, 2014
654
Mr. Chris Cameron
Cameron Testing Services, Inc.
219 S. Steele Street
Sanford, NC 27330
John E, Skvarla, III
Secretary
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Mr. Cameron:
Enclosed is a report for the inspection performed on October 21, 2014 by Gary Francies, Dana
Satterwhite, Nick Jones, and Beth Swanson. 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 (828)
296-4677.
Attachment
cc: master file
Nick Jones
Sincerely,
Gary Francies, Technical Assistance/Compliance Specialist
Division of Water Resources
Water Sciences 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
Phone: 919-733-39081 FAX: 919-733-6241
Internet: www.dwglab.org
An Equal Opportunity 1 Affirmative Action Employer
INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #:
Laboratory Name:
Inspection Type:
Inspector Name(s):
Inspection Date:
Date Report Completed:
Date Forwarded to Reviewer:
Reviewed by:
Date Review Completed:
Cover Letter to use:
Unit Supervisor/Chemist III:
Date Received:
Date Forwarded to Linda:
Date Mailed:
Cameron Testing Services, Inc.
Abbreviated
Nick Jones. Dana Satterwhite. Gary Francies. Beth Swanson
October 21, 2014
November 5, 2014
November 5. 2014
Dana Satterwhite
November 21, 2014
❑ Insp. Initial
❑ Insp. No Finding
❑ Corrected
Gary Francies
® Insp. Reg.
❑ Insp. CP
❑ Insp. Reg. Delay
11 /5/2014
11/21/2014
\\ I,LI\A U
On -Site Inspection Report
LABORATORY NAME:
ADDRESS:
CERTIFICATE #:
DATE OF INSPECTION:
TYPE OF INSPECTION:
AUDITOR(S):
LOCAL PERSON(S) CONTACTED:
INTRODUCTION:
Cameron Testing Services, Inc.
219 S. Steele Street
Sanford, NC 27330
654
October 21, 2014
Commercial Abbreviated
Nick Jones, Dana Satterwhite, Gary Francies, Beth Swanson
Chris Cameron, Anna Miller
This laboratory was inspected by a representative of the North Carolina Wastewater/Groundwater
Laboratory Certification (NC WW/GW LC) program to verify its compliance with the requirements of 15A
NCAC 2H .0800 for the analysis of environmental samples.
II. GENERAL COMMENTS:
This was an abbreviated inspection performed at the request of the laboratory. The scope of the
inspection was limited to BOD/CBOD by SM 5210 B-2001. The request for the inspection was prompted
by concerns over inconsistencies in the Glucose Glutamic Acid (GGA) standard recovery, which often
showed a high bias, and blank values sometimes in the 0.3-0.5 mg/L range.
Laboratory personnel indicated that the water system filters were changed in early September and they
switched from using a Hach DO probe to a YSI probe. The laboratory also discovered that the membrane
had a tiny, barely detectable hole. This was replaced prior to the inspection. The length of time the
membrane was in this condition and the potential impact the changes in probe and water system filter had
on the final results of the GGA and blanks is unknown.
The laboratory is reminded that any time changes are made to laboratory operations; the laboratory
must update the Quality Assurance (QA)/Standard Operating Procedures (SOP) document(s). Any
changes made in response to the Findings, Recommendations or Comments listed in this report must
be incorporated to insure the method is being performed as stated, references to methods are
accurate, and the QA and/or SOP document(s) is in agreement with approved practice and regulatory
requirements. In some instances, the laboratory may need to create a SOP to document how new
functions or policy will be implemented.
III. FINDINGS REQUIREMENTS COMMENTS AND RECOMMENDATIONS:
BOD/CBOD —Standard Methods, 6210 B-2001
Comment: The lab is currently ageing/conditioning the dilution water at below room temperature. This
may be causing the water to be saturated with oxygen. The lab is also aerating the water for a few hours
before use. Even though the aeration occurs at room temperature, the water is still cold during the
aeration until the temperature equilibrates. This possibly causes the water to be super saturated with
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oxygen. At the very least it makes it more difficult for the Dissolved Oxygen (DO) concentration to
equilibrate to what it would be at room temperature. This technique of ageing/conditioning the water
could be contributing to the higher blank concentrations.
Recommendation: It is recommended that the water be aged/conditioned at 20°C.
Recommendation: It is recommended that the lab consider discontinuing the active mechanical aeration
of the dilution water and allow the water to acquire sufficient oxygen through passive contact with the
ambient air. If aeration is required, then manual aeration (e.g., through plunging or shaking) is
recommended. If the lab continues mechanical aeration of the dilution water and seed material, then it is
recommended that the tubing be replaced with latex rubber, polypropylene, or polyethylene tubing.
Comment: Converting to glass dilution water storage containers would lessen the likelihood of microbial
growth. If plastic is continued to be used be sure to have an adequate cleaning protocol and frequency
policy in place. Those procedures must be outlined in the SOP to ensure no contamination impact on the
blank.
Recommendation: Currently Glucose Glutamic Acid (GGA) is dispensed directly from the stock solution
bottle directly from the refrigerator. It is recommended that an aliquot be poured out into a beaker;
allowed to equilibrate to room temperature; then dispensed from the beaker. Any remaining solution in the
beaker would then be discarded.
Recommendation: It is recommended that the practice of rinsing the aeration tubes with deionized water
after the addition of nutrients to the dilution water be discontinued. Although a very small amount, this
does introduce excess water that does not contain the required nutrients and buffer.
Recommendation: To help determine the cause of the elevated blanks, it is recommended that blanks
modifying each of the following variables be analyzed: ageing water (cold vs. 20°C) and aeration (manual
vs. mechanical vs. none).
Recommendation: To avoid cross contamination of bottles, it is recommended the probe be rinsed
between readings. The only time it is acceptable to analyze multiple bottles without rinsing is when those
bottles are dilutions of the same sample; and then only if they are analyzed in order of increasing
concentration.
Comment: The lab is flagging data when the seed correction factor is outside of 0.6 — 1.0 mg/L. This is
no longer required. Please see the attached NC WW/GW LC Policy for Flagging BOD Quality Control
Failures for current flagging requirements.
Recommendation: There were multiple copies of the SOP observed in the lab. They were not all of the
same revision. A revision history page in the SOP is recommended. Also, controlling the distribution of
copies is recommended.
A. Finding: Chemicals/Reagents are used beyond the expiration date.
Requirement: Adherence to manufacturer expiration dates is required. Chemicals/reagents/
consumables exceeding the expiration date can no longer be considered reliable. If the expiration
is only listed as a month and year (with no specific day of the month), the last day of the month
will be considered the actual date of expiration. Monitor materials for changes in appearance or
consistency. Any changes may indicate potential contamination and the item should be
discarded, even if the expiration date is not exceeded. If no expiration .date is given, the laboratory
must have a policy for assigning an expiration date. If no date received or expiration date can be
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determined, the item should be discarded. Ref: North Carolina Wastewater/Groundwater
Laboratory Certification Policy.
Comment: Ferric Chloride expired February 1998. Dextrose expired September 2004.
B. Finding: For chemicals/reagents/consumables that do not have an expiration date, the
laboratory has not established a policy for assigning expiration dates.
Requirement: Adherence to manufacturer expiration dates is required. Chemicals/reagents/
consumables exceeding the expiration date can no longer be considered reliable. If the expiration
is only listed as a month and year (with no specific day of the month), the last day of the month
will be considered the actual date of expiration. Monitor materials for changes in appearance or
consistency. Any changes may indicate potential contamination and the item should be
discarded, even if the expiration date is not exceeded. If no expiration date is given, the laboratory
must have a policy for assigning an expiration date. If no date received or expiration date can be
determined, the item should be discarded. Ref: North Carolina Wastewater/Groundwater
Laboratory Certification Policy.
Comment: L-Glutamic Acid was received on 9/12/01. Calcium Chloride was received in 2003.
Magnesium Sulfate was opened on 7/14/06. None had expiration dates on the bottles.
C. Finding: When adding reagents to the dilution water, the volumes are not measured with the
required accuracy..
Requirement: Add 1 mL each of phosphate buffer, MgSO4i CaC12, and FeC13 solution/L to
prepared source water. Ref: Standard Methods, 5210 B-2001. (4) (c).
Comment: Currently the reagents are measured using a 10 ml graduated cylinder with 1 ml
increments.
D. Finding: The GGA reagents are not being dried at 103°C for at least one hour prior to storage
in a desiccator or prior to use.
Requirement: Dry reagent -grade glucose and reagent -grade glutamic acid at 103°C for 1 h.
Ref: Standard Methods, 5210 B-2001. (3) (h).
E. Finding: The lab is not averaging multiple Dilution Water Blanks of the same batch.
Requirement: After JEB [Joint Editorial Board] discussion with the Part Coordinator and Joint
Task Group chair for Section 5210, it has been determined that multiple Dilution Water Blanks
in the same batch using the same dilution water are to be treated as replicates and averaged.
Ref: Standard Methods for the Examination of Water and Wastewater Joint Editorial Board
Memorandum dated August 1, 2014. See attachmented..
F. Finding: The lab is starting a new carboy or mixing carboys of dilution water in the middle of a
sample batch without analyzing additional quality control. This constitutes a new batch. A new
blank and GGAs are needed with each batch.
Requirement: Source water may be stored before use as long as the prepared dilution water
(5210B.5a) meets quality control criteria in the dilution water blank (5210B.6c). Ref: Standard
Methods, 5210 B-2001. (4) (c).
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Comment: Individual storage containers must be checked for both the quality of the water and
cleanliness of the storage container through analysis of dilution water blanks.
G. Finding: The lab is choosing the quantity of seed suspension added to ensure that the DO
uptake attributable to the seed will be between 0.6 and 1.0 mg/L rather than the amount
required to provide GGA check results of 198 ± 30.5 mg/L.
Requirement: The DO uptake attributable to the seed generally should be between 0.6 and 1.0
mg/L, but the amount of seed added should be adjusted from this range to that required to
provide GGA check results of 198 ± 30.5 mg/L. Ref: Standard Methods, 5210 B-2001. (5) (d).
H. Finding: Sample volumes <20 mis are not being measured using a wide -tip pipet.
Requirement: When measuring BOD/CBOD sample volumes: Sample volumes less than 20
mis must be measured using a wide -tip pipet. Ref: North Carolina Wastewater/Groundwater
Laboratory Certification Policy.
I. Finding: The pHs of samples are not adjusted to 7.0 to 7.2 S.0 when they are not originally
between 6.0 and 8.0.
Requirement: Check pH; if it is not between 6.0 and 8.0, adjust sample temperature to 20 ±
3°C, then adjust pH to 7.0 to 7.2 using a solution of sulfuric acid (H2SO4) or sodium hydroxide
(NaOH) of such strength that the quantity of reagent does not dilute the sample by more than
0.5%. Ref: Standard Methods, 5210 B-2001. (4) (b) (1).
J. Finding: Standard Operating Procedures (SOPs) have not been developed and/or updated for
Carbonaceous Biochemical Oxygen Demand (CBOD).
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: Adding a section to the BOD SOP covering CBOD will be sufficient. Be sure to
include specifics (e.g. inhibitor must not be added to blank, and the lower acceptance range for
GGA)
K. Finding: The SOP does not address duplicate acceptance criteria.
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 current lab practice is 20% Relative Percent Difference (RPD). The method
allows for 30% RPD.
L. Finding: The RPD for duplicates is not being documented on the benchsheet. This is considered
pertinent information.
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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)•
M. Finding: The benchsheet needs clarification to document that the sample is free of total
residual chlorine and if not, how many drops of sodium sulfite/100mL are added to neutralize it.
This 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)•
Recommendation: It is recommended that a column be added to the benchsheet with a
header reading "drops/100mU or "drops/total mU'
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: Nick Jones Date: November 4, 2014
Report reviewed by: Dana Satterwhite Date: November 4, 2014
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NC WW/GW LC Policy for Flagging BOD Quality Control Failures (NC WW/GW LC policy
08/26/2014)
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) or in the comment section for an eDMR. 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 SM 5210 B (7) (b)-2001 which states: "Identify results in the
test reports when any of the following quality control parameters are not met:"
Anytime any of the 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. Multiple dilution water blanks in the
same batch using the same dilution water are to be treated as replicates and averaged. The
average of the dilution water blanks in a batch must not be more than 0.20 mg/L.
3. The average of the three Glucose - Glutamic Acid (GGA) check standards falls
outside the acceptance limits [i.e., 198 mg/L ± 30.5 mg/L (167.5 — 228.5 mg/L) or
164 ± 30.7 mg/L (133.3 — 194.7 mg/L) for CBOD].
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.
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STANDARD D METHODS
rt►K •ri a i;
EXAMINATION OF WATER AND W,4S'1'EWA'l'ER
JOINT EDITORIAL BOARD
MEMORANDUM
• .- W. ... �11! C�-.
To: StandardMethadsUsers From: Andrew Eaton
Biochemical Ox Vm Demand (BOD) Joint Editorial Board
Re: ROD Afultiple Dilution Water Blanks Date: August 1, 2014
This mono is in response to questions about how to determine acceptance criteria when multiple
Dilution Alater Blads are performed in the S"faciedardl4 efhods 5210B 2011 method.
The method states in section 5210B.6.c: "With each batch of samples incubate one or more
bottles of dilution water that contains nutrient, mineral and buffer solatious but no seed, or
nitrification inhibitor. This dilution water bl", se Nw as a check on gr:Islity ofamLeeeded dihAoa
water and cleanliness of incubation bottles. Determine initUd and final DO as in 5210B,5g and i..
The DO uptake in 5 d, must mot be more than 0.20 mg/L and pareferably not mare than 0.10 mom..,
before making seed corrections. If the dilution crater blank exceeds 0.20 mg1i., discard all data
for tests using this dilution water or clearly identify such samples in data record,_"
The mod does not specifically address how to handle multiple dilution water blanks.
After JEB diwassion worth the Part Coordinator and Joint Task Group chair for Section 5210, it
has been determined that multiple Dilution grater Blanks in the same batch using the same
dilution waster are to be treated as replicates and averaged. The average of the dilution water
blanks in a batch must not be more than 0.20 mg/L We will include this information in the next
published version of the method.
cc: Rabin Parnell (Part Coordinator — Part 5000)
"04k,X14