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HomeMy WebLinkAbout#57 - 10 - 2011 - FINALTo be attached to all inspection reports in-house only. Laboratory Cert. #. 57 Laboratory Name: Environmental Inc. Inspection Type: Commercial Maintenance Inspector Name(s): Jason Smith Inspection Date: November 18, 2011 Date Report Completed: December 20, 2011 Date Forwarded to Reviewer: December 20, 2011 Reviewed by: Chet Whiting Date Review Completed: January 18, 2012 Cover Letter to use: _ Insp. Initial X Insp. Reg. _ Insp. No Finding _ Insp. CP _Corrected Unit Supervisor: Gary Francies Date Received: 1/20/2012 Date Forwarded to Linda: 1/27/2012 Date Mailed: I 4-NCDENR NAA Ir North Carolina Department of Environment and Natural Resources Division of Water Quality Beverly Eaves Perdue Governor 57 Mr. Anthony Tirona Environmental, Inc. P.O. Box 954 Cullowhee, NC 28723 Charles Wakild, P. E. Director January 27, 2012 Dee Freeman Secretary Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) Maintenance Inspection Dear Mr. Tirona: Enclosed is a report for the inspection performed on November 18, 2011 by Jason Smith. I apologize for the delay in getting this report to you. 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. Sincerely, G c?� Gary Francies Certification Unit Supervisor Laboratory Section Enclosure cc: master file DENR DWQ Laboratory Section NC Wastewater/Groundwater Laboratory Certification Branch 1623 Mail Service Center, Raleigh, North Carolina 27699-1623 Location: 4405 Reedy Creek Road. Raleigh, North Carolina 27607-6445 Phone: 919-733-3908 \ FAX: 919-733-6241 Internet: www.dwglab.org One N6fthCarohna Naturally An Equal opportunity \ Affirmative Action Employer LABORATORY NAME: F_10101 CERTIFICATE #: TYPE OF INSPECTION: AUDITOR(S): I. INTRODUCTION: I -6• Environmental, Inc. P.O. Box 954 Cullowhee, NC 28723 57 November 18, 2011 Commercial Maintenance Jason Smith Anthony Tirona and Steve Graham 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 facility is neat and well organized and has all the equipment necessary to perform the analyses. Laboratory personnel communicate well with sample collectors and coordinate sample analyses effectively to manage workload and holding times. Findings A, B, C, D, E, H, I, K, L, M, N, O, P, Q, R, and S are new policies that have been implemented by our program since the last inspection. A. Finding: The laboratory is not calibrating the mechanical volumetric liquid -dispensing devices. 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. Each liquid -dispensing device must meet the manufacturer's statement of accuracy. For variable volume devices used at more than one setting, check the accuracy at the maximum, middle and minimum values. Testing at more than three volumes is optional. When a device capable of variable settings is dedicated to dispense a single specific volume, calibration is required at that setting only. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy. Recommendation: It is recommended that the laboratory document the date that the Standard Operating Procedures (SOPs) are reviewed. Recommendation: Most benchsheets include a place for the analyst to circle yes or no for all quality control criteria being met. This section is rarely completed. It is recommended that the laboratory consistently complete this section of the benchsheets. Page 2 #57 Environmental, Inc. B. Finding: The laboratory needs to increase the documentation of purchased materials and reagents. 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: The laboratory has a good system of traceability in place; however, the date put in use needs to be documented when it is not the same as the date opened. For example, fecal coliform consumables are opened in order to perform comparison tests, but not put into use for sample analysis until a later date. C. Finding: The laboratory needs to increase the documentation of standards and reagents prepared in the laboratory. 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. D. 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 Policy. Settleable Solids — Standard Methods, 18tn Edition, 2540 F E. Finding: The laboratory is not documenting the agitation of the sample after 45 minutes. Requirement: Settle for 45 min, gently agitate sample near the sides of the cone with a rod or by spinning, settle for 15 min longer. Ref: Standard Methods, 18th Edition, 2540 F. (3) (a). Page 3 #57 Environmental, Inc. 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). Fecal Coliform — Standard Methods, 18th Edition, 9222 D Comment: The laboratory has not been checking the operating temperature weekly with a maximum holding thermometer in the autoclave. Standard Methods, 18th Edition, 9020 B. (2) (i) states: Autoclave: Check operating temperature weekly with a minimum/maximum thermometer. This procedure was implemented on November 17, 2011, prior to the inspection. No further response is necessary for this finding. F. Finding: The laboratory has not established acceptance criteria for duplicates and consumable comparison testing. 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). Requirement: When samples have measurable levels of the constituent being determined, analyses of duplicate samples is effective for assessing precision. See table 1020 1: for acceptable limits for duplicate analysis. Ref: Standard Methods, 18th Edition, 1020 B (6). Comment: Other sound acceptable procedures for establishing duplicate acceptance criteria may be used. • - - r . 1 - • r •' • 1 • • - • •II-Em . • I M - • • a 11 • 1 k Requirement: Excluding Oil and Grease, all residue parameters, leachate extractions, residual chlorine, and coliform, analyze one known standard in addition to calibration standards each day samples are analyzed to document accuracy. Analyze one suspended residue, one dissolved residue, one residual chlorine and one oil and grease standard quarterly. For residual chlorine, all calibration standards required by the approved procedure in use and by EPA must be analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (B). Comment: Only one standard (the Proficiency Testing sample) was analyzed in the last year. IF .. • - : •1 r H. Finding: Filters are not weighed to constant weight prior to sample analysis, nor is a dry filter blank analyzed with each set of samples. 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 Page 4 #57 Environmental, Inc. 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). I. Finding: The laboratory is not basing the reporting limit on the minimum weight gain required by the method. 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. StandardAmmonia Nitrogen — .. J. Finding: Samples are not being distilled prior to analysis and no distillation study is on file. Requirement: The titration method requires all samples to be distilled. For all other methods, manual distillation is not required if comparability data on representative effluent samples are on file to show that this preliminary distillation step is not necessary; however, manual distillation will be required to resolve any controversies. In the case of low concentration effluents, the samples must be spiked to allow for a meaningful statistical comparison. It is recommended that samples with a concentration < 1.0 mg/L 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. The following frequencies are required: 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 (NC WW/GW LC) Policy, 01/15/2009; based upon Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 72, No. 47, March 12, 2007: Table 1 B Footnote 6. Requirement: Since it has been more than a year since the last distillation study was performed, the laboratory is required to perform a distillation study on six samples. Please submit the distillation studies by June 1, 2012. K. Finding: The volume of 10N NaOH added is not documented. Requirement: Record volume of 10N NaOH added in excess of 1 mL. The volume of 10N NaOH used is a part of the calculation to determine the concentration of NH3-N. Ref: Standard Methods, 18th Edition, 4500 NH3 F. (4) (e) and (5). Page 5 #57 Environmental, 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)• Comment: The laboratory is currently adding 2 mL of color indicating Ammonia pH Adjusting ISA, per manufacturer's instructions, to all samples standards and blanks. Therefore, the calculation of the final result has been correct for samples. This documentation requirement can be fulfilled by adding the following statement to the benchsheet: "Unless otherwise noted, 2 mL of Ammonia pH Adjusting ISA added to all samples, standards, and blanks". L. Finding: After the addition of the 10 N NaOH, the pH is verified to be greater than 11 with Ammonia pH Adjusting ISA; however, the elevated pH is not documented. Requirement: Supporting records shall be maintained as evidence that these practices are being effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7). M. Finding: The laboratory is not analyzing matrix spikes. 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 spike 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. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy. Recommendation: If the duplicate sample value is near or below the reporting limit, it is recommended that a Matrix Spike Duplicate (MSD) be analyzed. The MSD fulfills the duplicate required by 15A NCAC 2H .0805 (a) (7) (C). This would result in better statistical results to monitor method and analyst precision. N. Finding: A calibration verification standard (mid -range) is not analyzed. Requirement: The calibration blank and calibration verification standard (mid -range) must be analyzed initially (i.e., prior to sample analysis), after everyy 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, 20`h 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. The laboratory was analyzing a mid -range second source standard at the frequency required for the calibration verification standard. The second source standard does not have to be at mid -range and is only required to be analyzed once each day samples are analyzed. O. Finding: A calibration blank is not analyzed after every tenth sample. Requirement: See Finding M. Page 6 #57 Environmental, Inc. Biochemical Oxygen Demand — Standard Methods, 18th Edition, 5210 B P. Finding: The final Dissolved Oxygen (DO) is not always analyzed after 5 days ± 6 hours. Requirement: After 5 d ± 6 h of incubation, determine DO in all sample dilutions, and in all blanks and checks. North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods, 21 st Edition, 5210 B. (5) (h) and (i). Comment: Samples are always read out after five days, but occasionally the ± 6 hour portion of the requirement is not met. Q. Finding: The laboratory is not documenting that the blank meets the required acceptance criterion. Requirement: With each batch of samples incubate one or more bottles of dilution water that contains nutrient, mineral, and buffer solutions but no seed or nitrification inhibitor. This dilution water blank serves as a check on quality of unseeded dilution water and cleanliness of incubation bottles. The DO uptake in 5 d must not be more than 0.20 mg/L and preferably not more than 0.10 mg/L, before making seed corrections. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods, 21st Edition, 5210 B. (6) (c). Requirement: Identify results in the test reports when any of the following quality control parameters are not met: The dilution water blank is greater than 0.20 mg/L. Ref: North Carolina Wastewater/Groundwater Laboratory Certification policy based upon Standard Methods, 21st Edition, 5210 B. (7) (b). Comment: In order to show that the blank is :50.20 mg/L the results must be read to two decimal places. R. Finding: The laboratory is not averaging the Glucose — Glutamic Acid (GGA) standard results in order to determine if the required quality control criterion is met. Requirement: Identify results in the test reports when any of the following quality control parameters are not met: The GGA check falls outside the acceptance limits [i.e., 198 g/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]. When multiple GGA standards are analyzed, the average of those results must be within the acceptable limits. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods, 21st Edition, 5210 B. (7) (b). S. Finding: Extra nutrient, mineral, and buffer solutions are not added to the Biochemical Oxygen Demand (BOD) bottles containing more than 67% (i.e., > 201 ml-) 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 mU300-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). Comment: Dilution water prepared as normal with nutrient, mineral, and buffer solutions would still be used in the BOD bottles. For the bottles containing more than 67% sample, extra nutrient, mineral, and buffer solutions would be added in addition to the dilution water. Page 7 #57 Environmental, Inc. Recommendation: Rather than pipetting 0.33 mL of each reagent into the BOD bottle, it is recommended that commercially prepared nutrient buffer pillows for 300 mL bottles be used. T. Finding: The laboratory only considers the DO depletion of the sample, rather than sample and seed correction, to determine if it meets the minimum depletion of 2.0 mg/L. Requirement: Only bottles, including seed controls, giving a minimum DO depletion of 2.0 mg/L and a residual DO of at least 1.0 mg/L after 5 d of incubation are considered to produce valid data. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods, 21st Edition, 5210 B. (6) (a). U. Finding: The laboratory elevates the reporting limit when samples do not meet the 2.0 mg/L DO depletion requirement. Requirement: North Carolina Wastewater/Groundwater Laboratory Certification Policy prohibits raising the (PQL) reporting limit because the "use 2 rule" was not met. Instead the value obtained is reported and flagged. This policy is designed to prevent labs from artificially raising the PQL by setting "too low" dilutions and not demonstrating permit compliance. Ref: BOD Sample Calculations and Reporting document. The paper trail consisted of comparing laboratory benchsheets to client reports. Data were reviewed for Sapphire Valley WWTP (NPDES permit #NC0022985) for October, 2011. No transcription errors were detected. The facility appears to be doing a good job of accurately transcribing data. VANNNROUTOTs� 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: Jason Smith Report reviewed by: Chet Whiting Date: December 20, 2011 Date: January 18, 2012