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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 Page 2 #654 Cameron Testing Services, Inc. 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 Page 3 #654 Cameron Testing Services, Inc. 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). Page 4 #654 Cameron Testing Services, Inc. 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. Page 5 #654 Cameron Testing Services, Inc. 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 Page 6 #654 Cameron Testing Services, Inc. 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. Page 7 #654 Cameron Testing Services, Inc. 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