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HomeMy WebLinkAbout#159_2018_0321_AO_FINALTo be attached to all inspection reports in-house only. Laboratory Cert. #: 159 Laboratory Name: Tarboro WWTP Laboratory Inspection Type: Municipal Maintenance Inspector Name(s): Anna Ostendorff and Beth Swanson Inspection Date: March 21 & 22, 2018 Date Forwarded for Initial Review: April 19, 2018 Initial Review by: Jason Smith Date Initial Review Completed: April 23, 2018 Cover Letter to use: ❑ Insp. Initial ❑Insp. No Finding ❑Corrected (to use: rt click, properties, check) ® Insp. Reg ❑Insp. CP ❑Insp. Reg. Delay Unit Supervisor/Chemist III: Beth Swanson Date Received: April 30, 2018 Date Forwarded to Admin.: May 15, 2018 Date Mailed: May 16, 2016 Special Mailing Instructions: May 16, 2018 159 Mr. Michael Allen Tarboro WWTP Laboratory P.O. Box 220 Tarboro, NC 27886-0220 ROY COOPER MICHAE1.., S. REGAN LINDA CULPEPPER Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) Maintenance Inspection Dear Mr. Allen: Enclosed is a report for the inspection performed on March 21 and 22, 2018 by Anna Ostendorff. 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. Please describe the steps taken to prevent recurrence and include an implementation date for each corrective action. 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. A copy of the laboratory's Certified Parameter List at the time of the audit is attached. This list will reflect any changes made during the audit. 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 me at (919) 733-3908 ext. 259. Sincerely, 1 Beth Swanson Technical Assistance & Compliance Specialist Division of Water Resources Attachment cc: Anna Ostendorff, Dana Satterwhite Water Sciences Section NC Wastewater/Groundwater Laboratory Certification Branch 1623 Mall Service Center, Raleigh, North Carolina 27699-1623 Location: 4405 Reedy Creek Road, Raleigh, North Carolina 27607 Phom 919-733-39061 FAK 919-733-6241 Internet: U Q91V 0*o]21k6'i:2*A0[QkiF TYPE OF INSPECTION /111 r7 f1 t771+'iir LOCAL PERSON(S) CONTACTED: I. INTRODUCTION: Tarboro WWTP Laboratory NC0020605 WQ0002047 Hwy 64/ Service Rd 268 Tarboro, NC 27886 159 March 21 & 22, 2018 Municipal Maintenance Anna Ostendorff and Beth Swanson Michael Allen and Kevin Peaden This laboratory was inspected by representatives 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 compliance monitoring samples. IL GENERAL COMMENTS: The facility is neat and well organized and has all equipment necessary to perform the analyses. Records are well organized and easy to retrieve. The laboratory has Quality Assurance (QA)/Quality Control (QC) systems in place that exceed the minimum requirements. Additional voluntary monitoring beyond the frequency required in the NC0020605 permit is performed and all data is reported as required. Staff were forthcoming and seemed eager to adopt the necessary changes. All required Proficiency Testing (PT) Samples for the 2018 PT Calendar Year have not yet been analyzed. The laboratory is reminded that results must be received by this office directly from the vendor by September 30, 2018. The laboratory submitted their QA and/or Standard Operating Procedures (SOP) document(s) in advance of the inspection. These documents were reviewed and editorial and substantive revision requirements and recommendations were made by this program outside of this formal report process. Although subsequent revisions were not requested to be submitted, they must be completed by May 31, 2019. Page 2 #159 Tarboro yWVFP Laboratory The laboratory is reminded that any time changes are made to laboratory procedures, the laboratory must update the QA/SOP document(s) and inform relevant staff. Any changes made in response to the pre -audit review or to 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 each approved practice, test, analysis, measurement, monitoring procedure or regulatory requirement being used in the laboratory. In some instances, the laboratory may need to create an SOP to document how new functions or policies will be implemented. The laboratory is also reminded that SOPs are intended to describe procedures exactly as they are to be performed. Use of the word "should" is not appropriate when describing requirements (e.g., QC frequency, acceptance criteria, etc.). Evaluate all SOPs for the proper use of the word "should". Laboratory Fortified Matrix (LFM) and Laboratory Fortified Matrix Duplicate (LFMD) are also known as Matrix Spike (MS) and Matrix Spike Duplicate (MSD) and may be used interchangeably in this report. Requirements that reference 15A NCAC 2H .0805 (a) (7) (A), stating "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", are intended to be a requirement to document information pertinent to reconstructing final results and demonstrating method compliance. Use of this requirement is not intended to imply that existing records are not adequately maintained unless the Finding speaks directly to that. Contracted analyses are performed by Environment 1, Inc. (Certification # 10). Approved Procedure documents for the analysis of the facility's currently certified Field Parameters were provided at the time of the inspection. III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS: Documentation A. Finding: The units of measure are not consistently documented on the benchsheets. 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. Ref: 15A NCAC 2H .0805 (a) (7) (H). Comment: The BOD benchsheet "seed correction" column heading units were documented as mg instead of mg/L. The refrigerator and incubator temperature logs do not specify units of measure. B. Finding: The laboratory benchsheet for Field Parameters was lacking pertinent data: meter calibration time. 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). Page 3 #159 Tarboro WWTP Laboratory Requirement: The following must be documented in indelible ink whenever sample analysis is performed: meter calibration and meter calibration time(s). Ref: NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine, NC WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen and NC WW/GW LC Approved Procedure for the Analysis of pH. Comment: This applies to Total Residual Chlorine (TRC), Dissolved Oxygen (DO) and pH. C. Finding: The laboratory benchsheet was lacking pertinent data: instrument identification. 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). Requirement: The following must be documented in indelible ink whenever sample analysis is performed: Instrument identification (serial number preferred). Ref: NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine, NC WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen and NC WW/GW LC Approved Procedure for the Analysis of pH. Comment: This applies to TRC, DO and pH. D. Finding: The laboratory needs to increase the traceability 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). 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: NC WW/GW LC Policy. Requirement: Supporting records shall be maintained as evidence that these practices are being effectively carried out. All analytical records must be available for a period of five years. Ref: 15A NCAC 2H .0805 (a) (7) and (a) (7) (G). Comment: The laboratory maintains a reagent preparation log that documents the lot numbers, vendor and expiration date of all parent materials. Consumable materials that are not used in the preparation of reagents or solutions, such as pH buffers and TSS filters, are not documented. E. Finding: The laboratory was not documenting their use of heat -indicating tape. This is considered pertinent data. Requirement: Use heat -indicating tape to identify supplies and materials that have been sterilized. Ref: Standard Methods 9020 B-2005. (4) (h). 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). Page 4 #159 Tarboro WWTP Laboratory 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). General Laboratory F. Finding: The laboratory is analyzing compliance samples and reporting data for Fecal Coliform in sludge samples without certification by NC WW/GW LC. Requirement: Municipal and Industrial Laboratories are required to obtain certification for parameters which will be reported to the State to comply with State surface water monitoring, groundwater, and pretreatment Rules. Ref: 15A NCAC 2H .0804 (a). Comment: The laboratory was analyzing Fecal Coliform by membrane filtration (i.e., SM 9222 D-1997) in Class B sludge samples for land application. The laboratory was unaware separate certification is required for non -aqueous samples under the Code of Federal Regulations, Title 40, part 503. The laboratory must contract out future sludge analyses or obtain certification for the non -aqueous membrane filtration method (i.e., SM 9222 D-2006 (MF) 24hr 503). Quality Control G. Finding: Composite samples for Ammonia and COD are not being chemically preserved toapH<2. Requirement: Preservation: Cool, :56 °C, H2SO4 to pH <2. Ref: Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 82, No. 165, August 28, 2017; Table II. Requirement: For a composite sample collected with an automated sampler (e.g., using a 24-hour composite sampler; see 40 CFR 122.21 (g) (7) (i) or 40 CFR Part 403, Appendix E), refrigerate the sample at 56 °C during collection unless specified otherwise in this Table II or in the method(s). For a composite sample to be split into separate aliquots for preservation and/or analysis, maintain the sample at :56 °C, unless specified otherwise in this Table II or in the method(s), until collection, splitting, and preservation is completed. Add the preservative to the sample container prior to sample collection when the preservative will not compromise the integrity of a grab sample, a composite sample, or an aliquot split from a composite sample; otherwise, preserve the grab sample, composite sample, or aliquot split from a composite sample within 15 minutes of collection. Ref: Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 82, No. 165, August 28, 2017; Table ll, Footnote 2. Requirement: A record of date collected, time collected, sample collector, and use of proper preservatives must be maintained. Each sample must clearly indicate the State of North Carolina collection site on all record transcriptions. Ref: 15 NCAC 2H .0805 (a) (7) (M). Comment: Chemical preservation of the samples must be verified with a meter or test strips and documented. H. Finding: The laboratory is not monitoring and documenting pretreatment sample temperatures upon receipt in the laboratory. Page 5 #159 Tarboro yW TP Laboratory Requirement: A record of date collected, time collected, sample collector, and use of proper preservatives must be maintained. Each sample must clearly indicate the State of North Carolina collection site on all record transcriptions. Ref: 15 NCAC 2H .0805 (a) (7) (M). Requirement: Basic documentation requirements to verify that sample preservation and hold time requirements are met include: Preservation status; temperature and chemical preservative(s) used (i.e., name of preservative, pH<2, pH>9, etc., where pH is not adequately adjusted document the measured pH). Ref: NC WW/GW LC Policy. Comment: Pretreatment samples are placed on ice and transported in a cooler to the Tarboro WWTP Laboratory for analysis, but the sample temperatures are not checked or documented upon arrival at the laboratory. If transport times are not long enough for sample temperatures to reach <_6 °C, the laboratory may measure and document sample temperatures at collection and upon arrival at the laboratory to document a downward trend. 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: NC WW/GW LC Policy. J. Finding: Precision of sample duplicates for COD is not consistently evaluated to demonstrate the analytical process is in control and the established acceptance criterion is met. 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 precision and accuracy of QC results must be documented and evaluated against the prescribed acceptance criteria to demonstrate that the analytical process is in control. Any samples associated with QC not meeting the criteria must be reanalyzed if possible. If this is not possible, the data must be flagged on the laboratory reports and electronic Discharge Monitoring Reports (eDMR) as all quality control requirements not met and giving a brief description of the QC exceedance that occurred. K. Finding: Data that does not meet all QC requirements is not always qualified on the eDMR. Requirement: When QC failures occur, the laboratory must attempt to determine the source of the problem and must apply corrective action. If data qualifiers are used to qualify samples not meeting QC requirements, the data may not be useable for the intended purposes. A notation must be made on the electronic Discharge Monitoring Page 6 #159 Tarboro WWTP Laboratory Report (eDMR) form, when any required sample quality control does not meet specified criteria, and another sample cannot be obtained. Ref: NC WW/GW LC Policy. Comment: This was only observed for Suspended Residue sample duplicates, which had low Suspended Residue values and were evaluated against a 30% RPD. Recommendation: It is recommended that the laboratory implement tiered acceptance criteria for evaluating duplicates. For example, the acceptance criterion for low-level samples could be ± mg/L, while high-level samples could be %RPD. Proficiency Testing L. Finding: PT Samples have not been distributed among all analysts from year to year. Requirement: Laboratories shall also ensure that, from year to year, PT Samples are equally distributed among personnel trained and qualified for the relevant tests and instrumentation (when more than one instrument is used for routine Compliance Sample analyses), that represents the routine operation of the work group at the time the PT Sample analysis is conducted. Ref: Proficiency Testing Requirements, May 31, 2017, Revision 2.0. M. Finding: The laboratory does not have a documented plan for PT procedures. 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). Requirement: Laboratories must have a documented plan (this is usually detailed in the laboratory's Quality Assurance Manual or may be a separate SOP) of how they intend to cover the applicable program requirements for Proficiency Testing per their scope of accreditation. This plan shall cover any commercially available PT Samples and any inter - laboratory organized studies, as applicable. The laboratory must also be able to explain when PT Sample analysis is not possible for certain methods and provide a description of what the laboratory is doing in lieu of Proficiency Testing. This shall be detailed in the plan. The plan must also address the laboratory's process for submission of PT results and related Corrective Action Reports (CARs). Ref: Proficiency Testing Requirements, May 31, 2017, Revision 2.0. Requirement: SOPs must address situations where the instructions from the Accredited PT Provider for the preparation, analysis or result calculations would constitute a deviation from the laboratory's routine procedure. Examples of this may include how low-level samples will be analyzed, including concentration of the sample or adjustment of the normality of a titrant. These instructions shall be followed when the concentration of a PT sample falls below the range of their routine analytical method. Instructions shall also be included in the laboratory's SOP for how high-level samples will be analyzed, including preparation of multiple dilutions of the sample. These instructions will be followed when the concentration of a PT falls above the range of their routine analytical method. Ref: Proficiency Testing Requirements, May 31, 2017, Revision 2.0. N. Finding: The laboratory is not documenting the preparation of PT Samples. Page 7 #159 Tarboro WWTP Laboratory Requirement: PT Samples received as ampules are diluted according to the Accredited PT Sample Provider's instructions. It is important to remember to document the preparation of PT Samples in a traceable log or other traceable format. The diluted PT Sample then becomes a routine Compliance Sample and is added to a routine sample batch for analysis. No documentation is needed for whole volume PT Samples which require no preparation (e.g., pH), but it is recommended that the instructions be maintained. Ref: Proficiency Testing Requirements, May 31, 2017, Revision 2.0. Comment: Dating and initialing the instruction sheet for each prepared PT Sample would satisfy the documentation requirement. Bacteria — Coliform, Fecal — Standards Methods, 9222 D-1997 (MF) (Aqueous) Comment: The laboratory was in the process of gaining certification for the IDEXX Colilert-18® method for the analysis of Fecal Coliform at the time of the inspection. The SM 9222 D-1997 (MF) method was audited but the laboratory is no longer certified for the method. This change was effective March 29, 2018. ®. Finding: The time sample filtration begins was not recorded on the benchsheet to show that no more than 30 minutes had passed before filters were placed into the incubator. This is considered pertinent data. Requirement: Place all prepared cultures in the water bath within 30 min after filtration. Ref: Standard Methods, 9222 D-2006. (2) (d). 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: 15 NCAC 21-1.0805 (a) (7) (A). P. Finding: Compliance sample results were not always calculated and reported correctly. Requirement: Countable Membranes with 20-60 Blue Colonies: Calculate the fecal coliform results from membrane filters within the ideal counting range of 20-60 blue colonies using the general formula: Number of colonies counted x 100 = Fecal coliform colonies per 100 ml volume of sample filtered in ml If more than one filter (including a 100-mL sample volume) has a count in the acceptable range, calculate the values in counts/100 mL for each filter in the countable range and average. Ref: NC WW/GW LC Policy Requirement: Countable Membranes with less than 20 Blue Colonies: If all counts are below the lower limit (20) of the ideal counting range: (a) Select the count most nearly acceptable and compute the count using the general formula. Report the count as an Estimated Count per 100 mL: or (b) Total the counts on all filters and report as number per 100 mL. For example, if 50, 25, and 10 mL portions were examined and counts were 15, 6, and 0 coliform Page 8 #159 Tarboro VW TP Laboratory colonies respectively, calculate results as follows and report the count as 25 colonies per 100 mL. (15 + 6 + 0) counts x 100 = 25 colonies per 100 mL 50+25+10mL Ref: NC WW/GW LC Policy Comment: When a sample batch produced plate counts with both 20 — 60 colonies and less than 20 colonies, the laboratory was calculating and reporting results using option (b). This method of calculating and reporting results is only applicable when all plates produce less than 20 blue colonies. Comment: When all plates produce less than 20 blue colonies, most laboratories elect to calculate and report results using option (b) as opposed to option (a). Q. Finding: Sample bottle sterility was not verified. Requirement: Minimally test for sterility one sample bottle per batch sterilized in the laboratory, or at a set percentage such as 1 to 4%. This is performed by adding sterile dilution/rinse water to the bottle after sterilization and then subsequently analyzing it as a sample. Document results. If sample bottles or bags are purchased pre -sterilized, verification of sterilization is not required if the laboratory maintains copies of the Certificate of Analysis from the vendor. Ref: NC WW/GW LC Policy. Comment: This requirement also applies to sample bottles that are reused for analysis with the IDEXX Colilert-18® method. If pre -sterilized disposable bottles are used, retaining the vendor's Certificate of Analysis will satisfy this requirement. R. Finding: Plate comparison counts were not being performed. Requirement: For routine performance evaluation, repeat counts on one or more positive samples at least monthly, record results, and compare the counts with those of other analysts testing the same samples. Replicate counts for the same analyst should agree within 5% (within analyst repeatability of counting) and those between analysts should agree within 10% (between analysts reproducibility of counting). If they do not agree, initiate investigation and any necessary corrective action. Ref: Standard Methods, 9020 B- 2005. (9) (a). BOD —Standard Methods, 5210 B-2011 (Hach 10360-2011, Rev. 1.2) (LDO) S. Finding: Seed controls with less than 2.0 mg/L DO depletion are sometimes used for the seed correction calculation. Requirement: For the ratio method, divide the DO depletion by the volume of seed in milliliters for each seed control bottle having a 2.0 mg/L depletion and greater than 1.0 mg/L minimum residual DO and average the results. Ref: Standard Methods, 5210 B- 2011. (6) (d). T. 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. Page 9 #159 Tarboro WWTP Laboratory 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 diluted sample at a rate of 1 mUL (0.30 mL/300-mL bottle) or use commercially -prepared solutions designed to dose the appropriate bottle size. Ref: Standard Methods, 5210 B- 2011. (5) (c) (2). U. Finding: Samples with less than 2.0 mg/L DO depletion are sometimes used for calculating the final BOD results. 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, because at least 2.0 mg oxygen uptake/L is required to give a meaningful measure of oxygen uptake and at least 1.0 mg/L must remain throughout the test to ensure that insufficient DO does not affect the rate of oxidation of waste constituents. Ref: Standard Methods, 5210 B-2011. (6) (a). Requirement: Average the test results for all qualified bottles within each dilution series. Ref: Standard Methods, 5210 B-2011. (7) (b). Recommendation: It is recommended a system of peer review be implemented to ensure calculations are properly performed and the data is reported correctly. Chlorine, Total Residual — Standard Methods, 4500 Cl G-2011 (Aqueous) Recommendation: It is recommended the laboratory verify the factory -set calibration curve annually using a 400 tag/L standard as the highest standard concentration. Currently, the highest standard concentration verified is 200 tag/L. PT Sample concentrations can exceed 300 tag/L, though all observed historical PT Samples analyzed by the laboratory were bracketed. Increasing the highest standard concentration to 400 tag/L will ensure future PT Sample concentrations are bracketed. V. Finding: The laboratory is not analyzing a Reagent Blank. Requirement: If preparing standards, analyzing a PT Sample or analyzing diluted samples, a Reagent Blank is required. Ref: NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine. Comment: The laboratory prepares an aqueous standard to verify instrument calibration each day of analysis. A reagent blank must be analyzed each day to document there is no interference from the reagent water used to prepare the standard. This must also be done with the annual 5-standard factory -set calibration curve verification. COD — Standard Methods, 5220 D-2011 (Aqueous) Comment: Because the laboratory uses a spectrophotometer with a factory -set calibration curve, all standards used in the preparation of QC elements are from a source independent of what was used to generate the calibration curve and are therefore considered second source. The laboratory analyzes an additional second source standard, which is not necessary and may be eliminated. Page 10 #159 Tarboro VWVfP Laboratory Comment: The preservative that is added to compliance samples must also be added to the digested blank and Laboratory Fortified Blank (LFB) once the laboratory begins to chemically preserve samples. W. Finding: The laboratory was not using an undigested blank as the reference solution for evaluating the digested blank for samples analyzed at 600 nm. Requirement: At 600 nm, use an undigested blank as reference solution. Analyze a digested blank to confirm good analytical reagents and to determine the blank COD; subtract blank COD from sample COD. Alternately, use digested blank as the reference solution once it is established that the blank has a low COD. Ref: Standard Methods, 5220 D-2011. (4) (b). Comment: The laboratory uses a digested blank as the reference solution, but has not evaluated the digested blank against the undigested blank to establish the digested blank has a low COD. X. Finding: The laboratory was not using reagent water as the reference solution for samples analyzed at 420 nm. Requirement: At 420 nm, use reagent water as a reference solution. Measure all samples, blanks, and standards against this solution. The absorption measurement of an undigested blank containing dichromate, with reagent water replacing sample, will give initial dichromate absorption. Any digested sample, blank, or standard that has a COD value will give lower absorbance because of the decrease in dichromate ion. Ref: Standard Methods, 5220 D-2011. (4) (b). Comment: The laboratory currently uses a digested blank as the reference solution for analyzing samples. The initial dichromate absorption must be determined by zeroing the meter with reagent water and analyzing the undigested blank. The digested blank is then analyzed and that value is subtracted from sample and standard measurements to obtain the final result. Y. Finding: The laboratory has not established an acceptance criterion for the calibration curve verification. 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 laboratory must set an acceptance criterion for the % recovery of the calibration standards when the calibration curve is verified. The acceptance criterion may not exceed 15%. Z. Finding: A reporting limit verification standard is not analyzed initially and at least quarterly for the low range curve. Requirement: Verify quantitation at the Minimum Reporting Level (MRL) initially and at least quarterly (preferably daily) by analyzing a QC sample (subjected to all sample - preparation steps) spiked at a level 1 to 2 times the MRL. A successful verification meets the method's or laboratory's accuracy requirements at the MRL. Laboratories must define Page 11 #159 Tarboro WWTP Laboratory acceptance criteria for the operational range, including the MRL, in their QA documentation. Ref: Standards Methods, 5020 B-2010. (1) (c). Comment: A reporting limit verification standard is analyzed for the high range curve each day compliance samples are analyzed. AA. Finding: A calibration blank and calibration verification standard (mid -range) are not analyzed at the end of the sample group. Requirement: Verify calibration by periodically analyzing a calibration standard and calibration blank during a run — typically, after each batch of ten samples and at the end of the run. Ref: SM 5020 B-2010. (2) (b). Requirement: The calibration blank and calibration verification standard (mid -range) must be analyzed initially (i.e., prior to sample analysis), 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: NC WW/GW LC Policy. BB. Finding: The laboratory is not analyzing an LFM. Requirement: When appropriate for the analyte (Table 5020:1), include at least one LFM/LFMD daily or with each batch of 20 or fewer samples. To prepare an LFM, add a known concentration of analytes (ideally from a second source) to a randomly selected routine sample without increasing its volume by more than 5%. Ref: SM 5020 B-2010, Table 5020:1 and (2) (g). Comment: For spike solution volumes that constitute >1 % of the total sample volume, the percent recovery calculation must be volume adjusted. Recommendation: Preparing the LFM in the vial without diluting the sample by more than 5% is difficult since only 2 mL of additional volume can be added to the digestion vials. It is recommended that the LFM be prepared in a volumetric flask using a larger sample volume and 2 mL of the prepared LFM be transferred to the vial. CC. Finding: The laboratory is not analyzing a sample duplicate for the high -range samples. Requirement: When appropriate for the analyte (Table 5020:1), include at least one LFM/LFMD daily or with each batch of 20 or fewer samples. To prepare an LFM, add a known concentration of analytes (ideally from a second source) to a randomly selected routine sample without increasing its volume by more than 5%. Ref: SM 5020 B-2010, Table 5020:1 and (2) (g). Comment: The laboratory may analyze either an LFMD or a sample duplicate to fulfil this requirement. Comment: Only one compliance sample is analyzed using the high -range test kit. The laboratory analyzes a sample duplicate with each batch for low -range samples. Nitrogen, Ammonia — Standard Methods, 4500 NH3 D-2011 (Aqueous) Page 12 #159 Tarboro WVVfP Laboratory Comment: The preservative that is added to compliance samples must also be added to the Method Blank (MB) and Laboratory Fortified Blank (LFB) once the laboratory begins to chemically preserve samples. DD. Finding: The laboratory does not document the slope of the meter calibration in units of mV. 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). Requirement: If the electrode is functioning properly a tenfold change of NH3-N concentration produces a potential change of about 59 mV. Ref: SM 4500 NH3 D-2011. (4) (c). Comment: The laboratory documents the slope of the meter calibration in percent efficiency. EE. Finding: The laboratory is not randomly selecting samples to fortify and duplicate. Requirement: When appropriate for the analyte (Table 4020:1), include at least one LFM/LFMD daily or with each batch of 20 or fewer samples. To prepare an LFM, add a known concentration of analytes (ideally from a second source) to a randomly selected routine sample without increasing its volume by more than 5%. Ref: SM 4020 B-2011, Table 4020:1 and (2) (g). Comment: The laboratory routinely fortifies and duplicates the Effluent sample only. FF. Finding: The laboratory is not adjusting the sample concentration in the percent recovery calculation when the spike volume is >1 % of the total sample volume. Requirement: The volume of spike solution used in MS preparation must in all cases be <_ 5% of the total MS volume. It is preferable that the spike solution constitutes <_ 1% of the total MS volume so that the MS can be considered a whole volume sample with no adjustment (i.e., volume correction) by calculation necessary. If the spike solution volume constitutes >1 % of the total sample volume, the sample concentration must be adjusted by calculation. Ref: NC WW/GW LC Policy. Comment: The spike solution volume constitutes 2.5% of the total volume for the LFM/LFMD. The laboratory must either use the volume adjusted calculation or reduce the volume of spiking solution added to _< 1 % of the total sample volume. pH — Standard Methods, 4500 H+ B-2011 (Aqueous) GG. Finding: The laboratory is not analyzing a post -analysis check standard buffer when analyses are performed at multiple locations. Requirement: When performing analyses at multiple sample sites, a post -analysis calibration verification using the check standard buffer must be analyzed at the end of the run. The post -analysis check standard buffer(s) must read within ±0.1 S.U. or corrective actions must be taken. If recalibration is necessary, all samples analyzed since the last acceptable calibration verification must be reanalyzed, if possible. If samples cannot be Page 13 #159 Tarboro WWTP Laboratory reanalyzed, the data must be qualified. Ref: NC WW/GW LC Approved Procedure for the Analysis of pH. Residue, Suspended — Standard Methods, 2540 D-2011 (Aqueous) Recommendation: It is recommended that the laboratory use a 0.1 g weight to check the balance each day of use since it is more representative of sample weights. Currently, the balance is checked with a 50-g weight each day of use. HH. Finding: Sample filters are not being washed after sample transfer. Requirement: Wash filter with three successive 10-mL volumes of reagent -grade water, allowing complete drainage between washings, and continue suction for about 3 min after filtration is complete. Samples with high dissolved solids may require additional washings. Ref: Standard Methods, 2540 D-2011. (3) (c). II. Finding: Samples chosen for duplicate analyses are not randomly selected. Requirement: When appropriate (Table 2020:1), randomly select routine samples to be analyzed twice. Ref: Standard Methods, 2020 B-2010. (2) (f). Comment: The laboratory routinely duplicates the Effluent samples. Bacteria — Coliform, Fecal — Standards Methods, 9222 D-1997 (Aqueous) Nitrogen, Ammonia — Standard Methods, 4500 NH3 D-2011 (Aqueous) JJ. Finding: Samples are not consistently checked for the presence of residual chlorine. Requirement: Except where noted in this Table II and the method for the parameter, preserve each grab sample within 15 minutes of collection. For a composite sample collected with an automated sample (e.g., using a 24-hour composite sample; see 40 CFR 122.21 (g)(7)(i) or 40 CFR Part 403, Appendix E), refrigerate the sample at <_6°C during collection unless specified otherwise in this Table II or in the method(s). For a composite sample to be split into separate aliquots for preservation and/or analysis, maintain the sample at <_6°C, unless specified otherwise in this Table II or in the method(s), until collection, splitting, and preservation is completed. Add the preservative to the sample container prior to sample collection when the preservative will not compromise the integrity of a grab sample, a composite sample, or aliquot split from a composite sample within 15 minutes of collection. If a composite measurement is required but a composite sample would compromise sample integrity, individual grab samples must be collected at prescribed time intervals (e.g., 4 samples over the course of a day, at 6-hour intervals). Ref: Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 88, No. 165, August 28, 2017; Table 11, Footnote 2. Requirement: Preservation: Coliform, total Na2S2O3. Ref: Code of Federal Regulations, No. 165, August 28, 2017; Table II. fecal, and E. coli: Cool, <10 °C, 0.008% Title 40, Part 136; Federal Register Vol. 82, Requirement: Residual Chlorine reacts with ammonia; remove by sample pretreatment. If a sample is likely to contain residual chlorine, immediately upon collection, treat with dechlorinating agent as in 4500-NH3.B.3d. Ref: Standard Methods, 4500 NH3 A-2011. (2). Page 14 #159 Tarboro WWTP Laboratory Requirement: Dechlorinating agents used at the time of sampling must be documented to have been effective upon receipt in the laboratory. A variety of field testing kits are considered to be adequate for most chlorine interference checks and a maximum detection limit of 0.5 mg/L is allowed. Ref: NC WW/GW LC Policy. Comment: The laboratory checks for TRC upon grab sample collection on Monday, Wednesday and Friday, but not Tuesday, Thursday, Saturday or Sunday. Recommendation: It is recommended the laboratory check for the presence or absence of TRC using test strips, and document the results on the benchsheet or Chain of Custody. The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks, etc.) and contract lab reports to electronic Discharge Monitoring Reports (eDMRs) submitted to the North Carolina Division of Water Resources. Data were reviewed for Tarboro WWTP Laboratory (NPDES permit # NC0020605) for January, May and August 2017. No transcription errors were observed. The facility appears to be doing a good job of accurately transcribing data. V. CONCLUSIONS: Correcting the above -cited Findings and implementing the Recommendations will help this laboratory to produce quality data and meet Certification requirements. The inspector would like to thank the staff for their assistance during the inspection and data review process. Please respond to all Findings and include supporting documentation, implementation dates and steps taken to prevent recurrence for each corrective action. 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