Loading...
HomeMy WebLinkAbout#92_2016_0826_BS_FINALINSPECTION 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 Admin: Date Mailed: Special Mailing Instructions: 92 City of Thomasville — Hamby Creek WWTP Laboratory Municipal Maintenance Beth Swanson, Gary Francies, Anna Ostendorff August 25 and 26, 2016 September 19, 2016 September 20, 2016 Anna Ostendorff September 27, 2016 ❑ Insp. Initial ® Insp. Reg. ❑ Insp. No Finding ❑ Insp. CP ❑ Corrected ❑ Insp. Reg. Delay Gary Francies September 29, 2016 10/18/2016 10/21 /2016 ater Reso arces ENVIRONMENTAL Cdlir' UTY October 24, 2016 92 Ms. Misty Conder City of Thomasville - Hamby Creek WWTP Laboratory P.O. Box 368 Thomasville, NC 27361 PAT MCCRORY DONALD R. VAN DER VAART S. JAY ZIMMERMAN /..: Ut"T Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) Maintenance Inspection Dear Ms. Conder: Enclosed is a report for the inspection performed on August 25 and 26, 2016 by Beth Swanson, Anna Ostendorff, and myself. 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. 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 (828) 296-4677. Sincerely, Gary Francies, Technical Assistance/Compliance Specialist Division of Water Resources Attachment Cc: master file Beth Swanson LMM LABORATORY NAME: City of Thomasville — Hamby Creek WWTP Laboratory NPDES PERMIT #: NC0024112 and NC0088200 ADDRESS: 110 Optimist Park Rd Thomasville, NC 27360 CERTIFICATE #: 92 DATE OF INSPECTION: August 25 and 26, 2016 TYPE OF INSPECTION: Municipal Maintenance AUDITOR(S): Beth Swanson, Gary Francies and Anna Ostendorff LOCAL PERSON(S) CONTACTED: Misty Conder INTRODUCTION: 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: The laboratory is spacious and well laid -out. Personnel were forthcoming and receptive to required changes, comments and recommendations. Many items were implemented before the creation of this report. The alum lagoon at the facility was brought back online in May 2016 after extended disuse. Some Findings applied only to the alum samples so they have been temporary in nature. All required Proficiency Testing (PT) samples have been analyzed for the 2016 PT calendar year and the graded results were 100% acceptable. The laboratory submitted their Quality Assurance (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 August 25, 2017. 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. Page 2 #92 City of Thomasville — Hamby Creek WWTP Laboratory 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. Quality Control (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 Meritech, Inc. (Certification # 165). 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: General Laboratory Comment: The laboratory was using sulfuric acid which expired in June 2010. NC WW/GW LC Policy states: 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. Notification of acceptable corrective action (i.e., a statement that the expired sulfuric acid has been discarded and replaced with a bottle expiring November 19, 2018) was received by email on September 9, 2016. No further response is necessary for this Finding. Documentation Comment: The laboratory needed to increase documentation of purchased materials and reagents as well as documentation of standards and reagents prepared in the laboratory. INC WW/GW LC Policy states: 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. Notification of acceptable corrective action (i.e., copies of updated benchsheets, completed receipt logs and reagent preparation logs containing the missing traceability items with an implementation date on or before September 9, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Page 3 #92 City of Thomasville — Hamby Creek VW TP Laboratory Comment: Error corrections were not always properly performed. There were a few instances of write-overs and most corrections that were made had initials but no date. NC WW/GW LC Policy states: 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. Notification of acceptable corrective action (i.e., a statement that the correct procedure for error correction was reviewed and implemented with all staff and beginning in September 2016, a monthly review of data sheets with an eye to error correction will be performed) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The autoclave cycle time was not documented. This is considered pertinent information. North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (A) states: 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. Notification of acceptable corrective action (i.e., an updated autoclave log implemented by September 9, 2016 that includes the time required to sterilize items in each cycle and a QC evaluation checklist that shows the timer on the autoclave was checked on September 1, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The pH of preserved samples was not consistently documented. This is considered pertinent information. North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (A) states: 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. Notification of acceptable corrective action (i.e., a statement that staff has been retrained on the use of the total phosphorus benchsheet, which includes a column for pH of samples, and the practice was implemented on analyses during the week of September 12, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: Data that did not meet all quality control requirements was not qualified on the electronic Discharge Monitoring Report (eDMR). When the lab originally began submitting data on the eDMR, the sample qualifiers were not being included with the reported results. This was a function of not understanding the new system. Qualifiers were included on the hard copies before the eDMR process began, and since the submission of the July 2016 eDMR, any necessary qualifiers are added to the comments section there. Notification of acceptable corrective action (i.e., a copy of the July 2016 eDMR comments section page showing qualifiers for BOD and TSS data) was received by email on September 9, 2016. No further response is necessary for this Finding. Proficiency Testing A. Finding: The laboratory does not have a documented plan for analysis of Proficiency Testing (PT) samples. 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) of how they intend to cover the applicable program Page 4 #92 City of Thomasville — Hamby Creek WWTP Laboratory requirements for proficiency testing per their scope of accreditation. This plan shall cover any commercially available proficiency testing and any inter -laboratory organized studies, as applicable. The laboratory must also be able to explain when proficiency testing is not possible for certain parameters 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 proficiency testing results and related corrective action responses. Ref: Proficiency Testing Requirements, February 20, 2012, Revision 1.2. Requirement: Laboratory Standard Operating Procedures (SOPs) must address 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, February 20, 2012, Revision 1.2. B. Finding: The preparation of PT samples is not documented. Requirement: PT samples received as ampules must be diluted according to the PT provider's instructions. The preparation of PT samples must be documented in a traceable log or other traceable format. The diluted PT sample becomes a routine environmental sample and is added to a routine sample batch for analysis. Ref: Proficiency Testing Requirements, February 20, 2012, Revision 1.2. Comment: Dating and initialing the instruction sheet for the preparation of the PT samples not received as whole volumes would satisfy the documentation requirement. C. Finding: The laboratory is not analyzing PT samples in the same manner as compliance samples. Requirement: All PT samples are to be analyzed and the results reported in a manner consistent with the routine analysis and reporting requirements of compliance samples and any other samples analyzed according to the requirements of 15A NCAC 2H .0800. Ref: Proficiency Testing Requirements, February 20, 2012, Revision 1.2. Comment: The laboratory's common practice was to analyze a known standard along with the PT sample as additional quality control. Since this is not performed with all compliance samples, it is considered additional quality control. However, known samples are recommended when analyzing remedial PT samples as part of the troubleshooting and corrective action process. PT samples were also analyzed on multiple days as a trial and to determine dilutions. Compliance samples are not analyzed in this manner, especially those with short holding times. Bacteria - Coliform Fecal — Standard Methods, 9222D-1997 (MF) (Aqueous) Comment: The laboratory was using 45.3°C as the target temperature for the warm air incubator. Standard Methods, 9222 D-1997. (2) (d). states: Place prepared dishes in waterproof plastic bags and seal, invert, and submerge petri dishes in water bath; incubate for 24 ± 2 h at 44.5 ± 0.2 °C. Alternatively, use an appropriate, accurate solid heat sink or equivalent incubator. Acceptable corrective action (i.e., the incubator thermostat was turned down to reach a temperature of 44.5 ± Page 5 #92 City of Thomasville — Hamby Creek WWTP Laboratory 0.2 °C) was performed by the laboratory on August 25, 2016 and approved by the auditor on August 26, 2016. No further response is necessary for this Finding. Comment: Sample duplicates were not being analyzed. A countable positive control was being analyzed in duplicate daily,_ since the laboratory usually only analyzes effluent samples with rarely more than 10 colonies per plate. North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (C) states: Analyze five percent of all samples in duplicate to document precision. Laboratories analyzing less than 20 samples per month must analyze at least one duplicate each month samples are analyzed. Notification of acceptable corrective action (i.e., a statement that analyzing duplicates of the effluent sample will be implemented by September 9, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory was not sterilizing the phosphate buffer and magnesium chloride stock solutions. Standard Methods, 9050 C-2006. (1) (a) (1) states: Stock phosphate buffer solution: Dissolve 34.0 g potassium dihydrogen phosphate (KH2PO4) in 500 mL reagent -grade water, adjust to pH 7.2 ± 0.5 with 1 N sodium hydroxide (NaOH), and dilute to 1 L with reagent -grade water. Sterilize by filtration or autoclave. Store stock solution under refrigerated conditions and discard if turbidity develops. Standard Methods, 9050 C-2006. (1) (a) (2) states: Magnesium chloride stock solution: Add magnesium chloride (38 g/L MgC12 or 81.1 g MgC12 - 6H2O) to 1 L reagent grade water. Sterilize and store stock solution under refrigerated conditions, discarding if solutions becomes turbid. Notification of acceptable corrective action (i.e., a statement that the individual reagents will be sterilized prior to adding to the dilution water starting at the first opportunity after September 9, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The stock phosphate buffer was not documented to be pH 7.2 ± 0.5. This is considered pertinent information. North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (A) states: 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. Notification of acceptable corrective action (i.e., an updated reagent preparation log with space to enter the pH of the phosphate buffer implemented at the next opportunity after September 9, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The pH of the M-FC media was not being checked and documented. Standard Methods, 9020 B-2005. (5) Q) (1) states: Check and record pH of a portion of each medium after sterilization. This is the actual pH required for adequate growth. Adjustment of pH will seldom be necessary when commercially available media are used. If needed, make minor adjustments to the pH specified in the formulation with filter -sterilized 1 N NaOH or 1 N HCI solutions. If the pH difference is larger than 0.5 units, discard the batch and check preparation instructions and pH of reagent water to resolve the problem. If medium is known as requiring pH adjustment, adjust pH appropriately prior to sterilization and record final pH. Standard Methods, 9222 D-1997. (1) (a) states: Final pH should be 7.4 ± 0.2. Notification of acceptable corrective action (i.e., an updated reagent preparation log with space to enter the pH and a statement that the media pH is being checked with a pH meter as of September 9, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory was not documenting their use of heat indicating tape. This is considered pertinent information. North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (A) states: 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. North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) states: 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 Page 6 #92 City of Thomasville — Hamby Creek vW TP Laboratory carried out. Notification of acceptable corrective action (i.e., an updated autoclave log with a column to note the autoclave tape was confirmed, implemented by September 9, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory was not monitoring the quality of the reagent water used in fecal coliform analysis. NC WW/GW LC Policy states: Reagent water used to prepare buffered dilution/rinse water or media must be analyzed at least every twelve months for the following parameters: Specific Conductance, Total Organic Carbon, Cadmium, Chromium, Copper, Nickel, Lead, and Zinc. Maximum Acceptable Limits are: Specific Conductance = < 2 pmhos/cm; TOC = < 1.0 mg/L; Heavy Metals, single element = < 0.05 mg/L; Heavy Metals Total of cited elements = < 0.10 mg/L. Notification of acceptable corrective action (i.e., documentation showing results of the required parameters were within the maximum acceptable limits and a Periodic QC Evaluation Checklist that includes an entry for DI reagent water check indicating it is annual and the date it was performed) was received by email on October 18, 2016. No further response is necessary for this Finding. Comment: The time samples are placed into the incubator was not being documented. This is considered pertinent information to show they are incubated within 30 minutes of filtration. Time of filtration was already being documented on the benchsheet. North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (A) states: 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. Notification of acceptable corrective action (i.e., an updated benchsheet with space to enter time placed into incubator implemented by September 9, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. D. Finding: Time samples are removed from the incubator is not documented. Requirement: The date and time BOD and coliform samples are removed from the incubator must be included on the laboratory worksheet. Ref: 15A NCAC 2H .0805 (a) (7) (H)• Comment: The benchsheet documents the time colonies are counted. E. Finding: Plate comparison counts are not being conducted. 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). Comment: When more than one analyst counts plates for reporting, a single positive plate will be counted twice by the primary analyst and any secondary analysts will count the same plate once and compare the result with the primary result. F. Finding: Consumable testing is not performed. Requirement: When a new lot of culture medium, pads, or membrane filters is to be used, a comparison of the current lot in use (reference lot) against the new lot (test lot), be Page 7 #92 City of Thomasville — Hamby Creek WVVfP Laboratory made. As a minimum, make single analyses on five positive samples. Ref: NC WW/GW LC Policy. Comment: The analyst commented that some form of consumable testing has been performed but there is no documentation. G. Finding: The sterility of laboratory sterilized bottles is 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. Ref: NC WW/GW LC Policy. BOD —Standard Methods, 5210 B-2001 (Aqueous) Comment: The analyst stated that the sample pH range and adjustment criterion used is the old requirement of adjusting samples to 6.5 — 7.5 S.U., instead of 7.0 — 7.2 S.U. There were no instances in the data reviewed where sample pH adjustment was needed. It would only be encountered rarely with industry samples. Comment: One result was found that did not include calculation of all dilutions that met the 2.0 mg/L minimum DO depletion and at least 1.0 mg/L residual DO criterion. This appears to be an isolated error during manual calculation as no other incident was found in the data reviewed. The sample was the January 26, 2016 influent which was reported as 80.75 mg/L but should have been calculated and reported as 84 mg/L. Recommendation: In order to avoid questions of legality, it is recommended that you contact the appropriate Regional Office for guidance as to whether an amended eDMR will be required. A copy of this report will be made available to the Regional Office. Recommendation: It is recommended that the Certificate of Analysis for the nutrient buffer pillows be retained to document the pH of phosphate buffer is 7.2 S.U. Comment: The BOD benchsheet did not include all units of measure. Units were missing from the Initial DO, 5-day DO, Oxygen Used and Corrected DO columns. North Carolina Administrative Code, 15A NCAC 21H .0805 (a) (7) (A) states: 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. Notification of acceptable corrective action (i.e., an updated benchsheet including all missing units of measure implemented by September 9, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The results of all acceptable seed controls were not being averaged. The laboratory was using an old criterion of >50% depletion. Standard Methods, 5210 B-2001. (6) (d) states: For the ratio method, divide the DO depletion by the volume of seed in milliliters for each seed control bottle having a 2.0 mq/L depletion and greater than 1.0 mg/L minimum residual DO and average the results. Notification of acceptable corrective action (i.e., a statement that the practice of averaging all seed control dilutions that meet the 2 and 1 rule was implemented by September 9, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Page 8 #92 City of Thomasville — Hamby Creek WWTP Laboratory Comment: The laboratory was not analyzing three glucose-glutamic acid (GGA) standard solutions. Two GGA standards were analyzed per day. Standard Methods, 5210 B-2001. (6) (b) states: Add sufficient amounts of standard glucose-glutamic acid solution (¶ 3h) to give 3.0 mg glucose/L and 3.0 mg glutamic acid/L in each of three test bottles (20 mL GGA solution/L seeded dilution water or 6.0 mU300-mL bottle). Notification of acceptable corrective action (i.e., an updated benchsheet preprinted with 3 GGA standards implemented by September 9, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory was not always -averaging the GGA standard solutions. When one GGA standard was outside of the acceptance range, it was not used to calculate an average result. Standard Methods, 5210 B-2001. (6) (b) states: Add sufficient amounts of standard glucose-glutamic acid solution (¶ 3h) to give 3.0 mg glucose/L and 3.0 mg glutamic acid/L in each of three test bottles (20 mL GGA solution/L seeded dilution water or 6.0 mU300-mL bottle). The resulting average BOD for the three bottles after correction for dilution and seeding, must fall into the range of 198 ± 30.5 mg/L. Notification of acceptable corrective action (i.e., a statement that the practice of averaging all GGA standards was implemented by September 9, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory was not applying corrective action to results outside of the laboratory set Relative Percent Difference (RPD) acceptance criterion for duplicates. The criterion was set very low, approximately 5 to 6% RPD. No data showed results outside of 30% RPD, which is the method required limit. NC WW/GW LC Policy states: When quality control (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 Discharge Monitoring Report (DMR) form, in the comment section or on a separate sheet attached to the DMR form, when any required sample quality control does not meet specified criteria, and another sample cannot be obtained. Notification of acceptable corrective action (i.e., a statement that as of September 9, 2016 the laboratory implemented a 30% RPD for all duplicate samples and will qualify all QC failures on the eDMR) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory was not seeding samples analyzed more than 6 hours after collection. Standard Methods 5210 B-2001. (4) (d)" states: Some samples (for example, some untreated industrial wastes, disinfected wastes, high -temperature wastes, wastes having pH values less than 6 or greater than 8, or wastes stored more than 6 h after collection) do not contain a sufficient microbial population. Seed such samples by adding a population of suitable microorganisms. Notification of acceptable corrective action (i.e., a statement that as of September 9, 2016, all samples are seeded) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory was not analyzing three dilutions for all samples. Only two dilutions were analyzed for each influent sample. Standard Methods, 5210 B-2001. (5) (c) states: Using the dilution water prepared as in ¶ 5a, make at least three dilutions of prepared sample estimated to produce a residual DO of at least 1.0 mg/L and a DO uptake of at least 2.0 mg/L after 5-d incubation. Five dilutions are recommended if experience with a particular sample does not produce at least three bottles having acceptable minimum DO depletions and residual limits (¶ 6a). Notification of acceptable corrective action (i.e., a statement that as of September 9, 2016, all samples are analyzed with at least three dilutions) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory was not consistently meeting the 48 hour holding time for samples collected on Mondays. The laboratory's common practice is to collect around 10 AM on Mondays Page 9 #92 City of Thomasville — Hamby Creek WWTP Laboratory and start the analysis around the same time on Wednesday. There were several days noted where the holding time was slightly (i.e., <30 minutes) exceeded. Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012; Table II states: Biochemical oxygen demand. Maximum holding time. 48 hours. Notification of acceptable corrective action (i.e., a statement that as of September 9, 2016 it has been reiterated to staff to be conscious of the Monday sample collection times and implemented the practice of always beginning the analyses on Wednesdays before 48 hours has passed) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory was not using wide -tipped pipettes for sample volumes <20 mL NC WW/GW LC Policy states: Sample volumes less than 20 mis must be measured using a wide -tip pipet. Notification of acceptable corrective action (i.e., a statement that as of September 9, 2016 the laboratory is using 25 mL wide -tipped serological pipets until the 10 mL wide -tipped pipets that were ordered arrive) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: When multiple dilution water blanks were analyzed, the values were not averaged and results qualified if >0.20 mg/L. Two blanks were analyzed each day, but when one was not acceptable, it was not considered in the final evaluation. The "BOD Multiple Dilution Water Blanks", Standard Methods Joint Editorial Board memorandum dated August 1, 2014 states: 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 >0.20 mg/L. Notification of acceptable corrective action (i.e., a statement that as of September 9, 2016, only one dilution water blank will be analyzed each day and any unacceptable blank value will be flagged on the eDMR) was received by email on September 9, 2016. No further response is necessary for this Finding. Nitrogen, Ammonia — Standard Methods, 4500 NH3 D-1997 (Aqueous) Comment: The benchsheet previously in use contained a few errors. It stated that the acceptance criterion for blanks was 0.9-1.1 mg/L. This was a typographical error since this is not the required acceptance criterion nor what the analyst uses since the reporting limit is 0.1 mg/L. The Continuing Calibration Verification (CCV) sample volume analyzed had also not been updated to the current volume. An updated benchsheet implemented August 31, 2016 includes the proper acceptance criterion of <0.05 mg/L and the current CCV volume analyzed. Comment: Samples were not being checked for Total Residual Chlorine and neutralized if necessary. This only applies to the quarterly alum lagoon sample, since the WWTP utilizes Ultra Violet disinfection. Standard Methods, 4500 NH3 A-1997. (2) states: 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. Notification of acceptable corrective action (i.e., a statement that the new standard procedure implemented on October 18, 2016 is to add 0.5 mL of 10% sodium thiosulfate to alum samples before preservation and verify with DPD powder or strips, the results of which will be documented on the COC) was received by email on September 9, 2016 and October 18, 2016. No further response is necessary for this Finding. Comment: Samples are being frozen and not chemically preserved. This was an acceptable method of preservation prior to the 2012 40 CFR Method Update Rule per guidance from previous Laboratory Certification auditors and Standard Methods. The NC WW/GW LC program does not currently have procedures and guidelines in place for laboratories to conduct studies to demonstrate the impact of freezing on sample integrity, and as such do not allow freezing of samples. The Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, Page 10 #92 City of Thomasville — Hamby Creek WWTP Laboratory May 18, 2012; Table II states: Preservation: Cool, :56 °C'$, H2SO4 to PH <2. Footnote 18 states: Aqueous samples must be preserved at <6 °C, and should not be frozen unless data demonstrating that sample freezing does not adversely impact sample integrity is maintained on filed and accepted as valid by the regulatory authority. Notification of acceptable corrective action (i.e., a statement and completed benchsheet saying that all samples since September 8, 2016 have and will be preserved with H2SO4 to pH <2 at collection and not frozen) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The second source standard was not analyzed prior to sample analysis. The second source was used as a mid -analysis meter check.NC WW/GW LC Policy states: When a standard curve is manually prepared (as opposed to a factory -set calibration), it is required to analyze one known standard in addition to calibration standards each day samples are analyzed to document accuracy. If the results fall outside of acceptance limits, the analysis is out of control. The analysis must be terminated and the problem corrected prior to sample analysis. Notification of acceptable corrective action (i.e., an updated benchsheet showing an analytical run on August 31, 2016, with the second source standard analyzed prior to samples) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory was not analyzing an LFM/LFMD. Standard Methods, 4020 B-2009, Rev. 2011, Table 4020:1 and (2) (g) state: 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%. Notification of acceptable corrective action (i.e., an benchsheet showing an analytical run on August 31, 2016, with analysis of LFM/LFMD and statement that it is implemented for the future) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory was not analyzing a blank at the end of the sample group. NC WW/GW LC Policy states: 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. Notification of acceptable corrective action (i.e., a benchsheet with an analytical run on August 31, 2016, with analysis of a blank at the end of the sample group and statement that it is implemented for the future) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory was not using an acceptance criterion of 550% of the reporting limit for blanks. The analyst would complete other tasks while the blank reading was allowed to stabilize. If the analyst returned from the task and the value was at least below the reporting limit, she assumed it had finished stabilizing and recorded the value. NC WW/GW LC Policy states: For analyses requiring a calibration curve, the concentration of reagent, method and calibration blanks must not exceed 50% of the reporting limit or as otherwise specified by the reference method. Notification of acceptable corrective action (i.e., a statement that the blank result will not be recorded until it reaches <_'/2 the reporting limit and an updated benchsheet including the correct acceptance criterion implemented August 31, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory was not documenting that the sample pH was adjusted to >11 S.U. This is considered pertinent information. North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (A) states: 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. Notification of acceptable corrective action (i.e., an updated benchsheet with a column to document that the sample or Page 11 #92 City of Thomasville — Hamby Creek WVVTP Laboratory standard turned blue, indicating pH >11 S.U., implemented by September 9, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Phosphorus, Total — Standard Methods, 4500 P E-1999 (Aqueous) Comment: The laboratory was not back calculating calibration standards. Standard Methods, 4020 B-2009, Rev. 2011. (2) (a) states: Back calculate the concentration of each calibration point. The back -calculated and true concentrations should agree within ± 10%. Notification of acceptable corrective action (i.e., documentation showing that back calculation of the calibration standards was implemented the week of September 19, 2016 with acceptance criteria of ±20% recovery and a statement that this was updated on October 18, 2016 to be implemented on the next analysis to a recovery of ±10% for all standards except the lowest concentration, which remains at ±20% ) was received by email on September 20 and 21 and October 18, 2016. No further response is necessary for this Finding. Comment: The laboratory was not analyzing a reporting limit standard quarterly. Standard Methods 4020 B-2009, Rev. 2011. (1) (c) states: The minimum reporting level (MRL) is set to a concentration at or above the lowest standard used in the analysis. Verify quantitation at the MRL initially and at least quarterly (preferable 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 acceptance criteria for the operational range- including the MRL-in their QA documentation. Notification of acceptable corrective action (i.e., a statement that a reporting limit standard will be analyzed at least quarterly beginning on September 20, 2016 with an acceptance criterion of ±20% recovery) was received by email on September 20 and 28, 2016. No further response is necessary for this Finding. Comment: The laboratory was not analyzing a blank at the end of the sample group. NC WW/GW LC Policy states: 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. Notification of acceptable corrective action (i.e., an updated benchsheet with a blank preprinted at the end of the sample group and statement that the practice would be implemented the week of September 12, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory was not analyzing an LFM/LFMD. Standard Methods 4020 B-2009, Rev. 2011, Table 4020:1 and (2) (g) state: 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%. Notification of acceptable corrective action (i.e., a statement that the analysis of an LFM/LFMD would be implemented the week of September 12, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory was not using an acceptance criterion of <_50% of the reporting limit for blanks. NC WW/GW LC Policy states: For analyses requiring a calibration curve, the concentration of reagent, method and calibration blanks must not exceed 50% of the reporting limit or as otherwise specified by the reference method. Notification of acceptable corrective action (i.e., a statement that the blank acceptance criterion of <_50% of the reporting limit would be implemented the week of September 12, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Page 12 #92 City of Thomasville — Hamby Creek WV TP Laboratory Residue, Suspended — Standard Methods, 2540 D-1997 (Aqueous) Recommendation: It is recommended that the "TSS report" column be renamed or only record the values that will be used for reporting. Currently, values are entered into the column that are below the reporting limit and so it appears that is how they were reported. Comment: The samples were not weighed to constant weight, nor was an annual multiple weighing study to verify the adequacy of the drying time, performed. NC WW/GW LC Policy states: Constant weights must be documented. The approved methods require the following: "Repeat the cycle of drying, cooling, desiccating, and weighing until a constant weight is obtained or until the weight change is less than 4% of the previous weight or 0.5 mg, whichever is less." In lieu of this, an annual study documenting the time required to dry representative samples to a constant weight may be performed. Verify minimum daily drying time is greater than or equal to the time used for the initial verification study drying cycle. Drying cycles must be a minimum 1 hour for verification. Notification of acceptable corrective action (i.e., submittal of an acceptable drying study performed on September 1, 2016 and statement that it will be repeated at least every 12 months) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory was not elevating the minimum reporting limit when samples with volumes <1000 mL did not meet the required weight gain. One instance was found on the June 23, 2016 influent sample where 20 mL of sample was used but the filter did not gain the required 2.5 mg. The result was reported as 115 mg/L rather than <125 mg/L. Standard Methods 2540 D- 1997. (3) (b) states: Choose sample volume to yield between 2.5 and 200 mg dried residue. If volume filtered fails to meet minimum yield, increase sample volume up to 1 L. NC WW/GW LC Policy states: 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. Notification of acceptable corrective action (i.e., a statement that the reporting limit will be raised when samples less than 1000 mL do not gain 2.5 mg and that the sample from June 23, 2016 will be corrected on the eDMR within 30 days as of September 9, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory was not randomly duplicating samples. Only the influent samples were being duplicated due to the low concentrations on the effluent samples. Standard Methods, 2020 B-2010. (2) (f) states: When appropriate (Table 2020:11), randomly select routine samples to be analyzed twice. Independently prepare and analyze duplicate samples. Notification of acceptable corrective action (i.e., a statement that the effluent sample will also be routinely analyzed in duplicate, with a tiered acceptance criterion due to the low concentrations, beginning on September 6, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. H. Finding: The drying oven thermometer has not been verified within the last 12 months and the temperature during use is not documented. This is considered pertinent information. Requirement: All thermometers and temperature measuring devices must be checked every 12 months (or sooner if the thermometer has been exposed to temperature extremes or other stresses) against a NIST certified or NIST traceable thermometer and the process documented. Ref: NC WW/GW LC Policy. Page 13 #92 City of Thomasville — Hamby Creek VWVfP 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). Comment: The drying oven has a sensor with digital readout on the outside of the oven that has not been verified and a verified thermometer that was placed inside the oven. When the verified thermometer stopped working several months previously, the analyst started monitoring the digital readout to determine if the oven was at the correct temperature. That temperature was not documented. I. Finding: The laboratory is not basing the reporting limit on the minimum weight gain required by the method. Requirement: Choose sample volume to yield between 2.5 and 200 mg dried residue. If volume filtered fails to meet minimum yield, increase sample volume up to 1 L. Ref: Standard Methods, 2540 D-1997 (3) (b). 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. Ref: NC WW/GW LC Policy. Comment: The laboratory is not using a minimum reporting limit of 2.5 mg/L for 1 L. Instead, any result less than 5 mg/L is reported as <5 mg/L. Chlorine, Total Residual — Standard Methods, 4500 Cl G-2000 (Aqueous) Recommendation: The laboratory currently constructs a curve daily with the following standard concentrations: 15 lag/L, 100 pg/L, 500 pg/L, 1000 pg/L and 2000 lag/L. Since their permit limit is 17 tag/L and samples are not generally encountered above 50 lag/L, it is recommended that a standard concentration near the lower reporting limit and at the compliance limit (i.e., 50 lag/L) be analyzed in place of the 1000 lag/L and 2000 lag/L standards. The 500 lag/L would remain to include the concentration range of the annual PT sample. Comment: The laboratory was using free chlorine DPD powder packs. North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (6) (H) states: Glassware, chemicals, supplies, and equipment required to perform all analytical procedures included in their certification. Acceptable corrective action (i.e., the free chlorine DPD package was discarded and a total chlorine DPD package was opened) was performed by the laboratory and approved by the auditor during the inspection. No further response is necessary for this Finding. Comment: The potassium permanganate in use was expired. The expiration date was August 2007. NC WW/GW LC Policy states: 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. Notification of acceptable corrective action (i.e., a statement that the new standard had been ordered prior to the inspection and was received and put into use on August 26, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory did not have a reagent blank acceptance criterion. The NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine document states: The Page 14 #92 City of Thomasville — Hamby Creek WWTP Laboratory concentration of reagent blanks must not exceed 50% of the reporting limit (i.e., the lowest calibration or calibration verification standard concentration), unless otherwise specified by the reference method, or corrective action must be taken. Notification of acceptable corrective action (i.e., a statement that the acceptance criterion of 5 50% of the reporting limit was implemented August 26, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Conductivity — Standard Methods, 2510 B-1997 (Aqueous) Comment: The benchsheet did not clearly state what standards were used for calibration and the calibration check. The NC WW/GW LC Approved Procedure for the Analysis of Specific Conductance (Conductivity) document states: The following must be documented in indelible ink whenever sample analysis is performed: True value of the standard used for calibration. True value of the calibration check standard. Notification of acceptable corrective action (i.e., an updated benchsheet with preprinted notations of the true value of the calibration and check standards implemented by September 9, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. pH — Standard Methods, 4500 H+ B-2000 (Aqueous) Comment: The benchsheets did not clearly state what buffers were used for calibration and the calibration check. The NC WW/GW LC Approved Procedure for the Analysis of pH document states: The following must be documented in indelible ink whenever sample analysis is performed: True value of buffers used for calibration. True value for the check standard buffer. Notification of acceptable corrective action (i.e., updated benchsheets with preprinted notations of the true value of the calibration and check buffers implemented by September 9, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The laboratory was not reporting all effluent data generated. Duplicates of the pH were being analyzed and the highest value was reported unless the lowest resulted in non- compliance. North Carolina Administrative Code, 15A NCAC 2B .0506 (b) (3) (J) states: The results of all tests on the characteristics of the effluent, including but not limited to NPDES permit monitoring requirements, shall be reported on the monthly report forms. Notification of acceptable corrective action (i.e., a statement that the practice of analyzing pH in duplicate was terminated by September 9, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Comment: The alum lagoon benchsheet did not clearly document analysis time. The NC WW/GW LC Approved Procedure for the Analysis of pH document states: The following must be documented in indelible ink whenever sample analysis is performed: Date and time of sample analysis to verify the 15-minute holding time is met. Alternatively, one time may be documented for collection and analysis with the notation that samples are measured in situ or at the sample site. Notification of acceptable corrective action (i.e., a benchsheet with the notation that analysis is the same time as collection for pH and Temperature implemented by September 9, 2016) was received by email on September 9, 2016. No further response is necessary for this Finding. Temperature — Standard Methods, 2550 B-2000 (Aqueous) Recommendation: It is recommended that Temperature data be reported to whole numbers on the eDMR based on the NPDES Compliance Guidance document, "Significant Figures and Their Use on Discharge Monitoring Reports (DMRs)" found here: http:/ ncdenr.s3.amazonaws.coi,ns3ts- Page 15 #92 City of Thomasville — Hamby Creek WVVfP Laboratory iiq �A ate_r%2O uali Surface%2�3`Jt/titer%2OProtection/NPDES/MISC/Guidance 20— %20SF&R%20f rf2OI:3MRs- 201E08 5-DWR-SWP NPDES .Of IV. PAPER TRAIL INVESTIGATION: A paper trail was not performed due to an inspection on July 6, 2016, conducted by April Norton from the North Carolina Division of Water Resources Winston-Salem Regional Office, which included a paper trail investigation. 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 and implementation dates for each corrective action. Report prepared by: Beth Swanson Date: September 19, 2016 Report reviewed by: Anna Ostendorff Date: September 27, 2016