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HomeMy WebLinkAbout#43_2018_0815_MC_FINALLaboratory Cert. : 43 Laboratory Name: Lexington Regional WWTP Laboratory Inspection Type: Municipal Maintenance Inspector Name(s): Michael Cumbus, Beth Swanson, Anna Ostendorff, Jason Smith, Thomas Halvosa, Todd Crawford Inspection Date: August 15-16, 2018 Date Forwarded for Initial Review: September 11, 2018 Initial Review by: Anna Ostendorff Date Initial Review Completed: September 14, 2018 Cover Letter to use: ❑ Insp. Initial ❑ Insp. Reg ❑Insp. No Finding ❑Insp. CP ❑Corrected ®Insp. Reg. Delay Unit Supervisor/Chemist III: Beth Swanson Date Received: October 6, 2018 Date Forwarded to Admin.: October 25, 2018 Date Mailed: October 26, 2018 Special Mailing Instructions: Michael emails a copy to Sherri Knight at WSRO rJ i l f� 7 1 kl,I Cll,1, EI_'S, R E G NNN ,i rcr�r` inlNDA 0,JI.i FPPE: Nr; Rf 11 r A; (D L I A, (n rl'r s 1?I • 10 EaWronnentat i uWdkY October 26, 2018 43 Ms. Eglantina Minerali Lexington Regional WWTP Laboratory 28 West Center Street Lexington, NC 27292 Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) Maintenance Inspection Dear Ms. Minerali: Enclosed is a report for the inspection performed on August 15 and 16, 2018 by Michael Cumbus. 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 21-1 .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, ---?J Beth Swanson Technical Assistance & Compliance Specialist Division of Water Resources Attachment cc: Michael Cumbus, Dana Satterwhite, Todd Crawford North Carolina Department of Environmental Quality I Division of Water Resources 1623 Mail Service Center I Raleigh, North Carolina 27699-1623 Phone 919.733,3908/Fax 919.733.6241 •' •' ff ' P�� LABORATORY NAME: Lexington Regional WWTP NPDES PERMIT : NC0055786 ADDRESS: 500 Glendale Rd Lexington, NC 27292 CERTIFICATE #: 43 DATE OF INSPECTION: August 15-16, 2018 TYPE OF INSPECTION: Municipal Maintenance AUDITOR(S): Michael Cumbus, Beth Swanson, Anna Ostendorff, Jason Smith, Thomas Halvosa and Todd Crawford LOCAL PERSON(S) CONTACTED: Eglantina Minerali and Sarah West I. INTRODUCTION: 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. II. GENERAL COMMENTS: The facility is neat and well organized and has all the equipment necessary to perform the analyses. Laboratory personnel communicate well with sample collectors and coordinate sample analyses effectively to manage workload and holding times. Laboratory personnel changed since the last inspection. With Ms. Minerali taking over as supervisor, the laboratory has been proactive in its in-house data audits, reaching out to the Certification Branch concerning quality control issues and initiating corrections to their procedures prior to the inspection once receiving the parameter checklists. Examples include initiating the sterility check of the bacteria sample bottles in June 2018 and the analysis of a second source standard for Phosphorus analysis. The laboratory was forthcoming about quality control issues that it found and was very receptive to the feedback from the auditors. The laboratory seemed eager to adopt changes that would allow it to continue to produce quality data. All required Proficiency Testing (PT) Samples have been analyzed for the 2018 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 September 30, 2019. Page 2 #43 Lexington Regional WWTP 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., 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. Contract 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: General Laboratory A. Finding: The analytical balance weights have not been verified against ASTM standard weights in the past 5 years. Requirement: ASTM Class 1 and 2 weights must be verified at least every 5 years. ASTM Class 1 weights (20 g to 25 kg) and ASTM Class 2 weights (10 g to 1 mg) are equivalent to the NBS Class S weights specified in 15A NCAC 2H .0805 (a) (7) (K). Ref: NC WW/GW LC Policy. See attachment "Weight Verification (NC WW/GW LC Policy 05/23/2008)" for additional guidance. B. Finding: For chemicals/reagents/consumables that do not have an expiration date, the laboratory has not established a policy for assigning expiration dates. Requirement: Adherence to manufacturer expiration dates is required. Chemicals/ reagents/ consumables exceeding the expiration date can no longer be considered reliable. If the expiration is only listed as a month and year (with no specific day of the month), the last day of the month will be considered the actual date of expiration. Monitor materials for changes in appearance or consistency. Any changes may indicate potential contamination and the item should be discarded, even if the expiration date is not exceeded. If no expiration date is given the laboratory must have a policy for assigning an expiration date. Page 3 #43 Lexington Regional WWTP Laboratory If no date received or expiration date can be determined, the item should be discarded. Ref: NC WW/GW LC Policy. Comment: The policy for assigning expiration dates must be added to the laboratory's QA document. Quality Control C. Finding: The laboratory does not have an SOP for all parameters. 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: An SOP describes the method in such detail that an experienced analyst unfamiliar with the method can obtain acceptable results and meet documentation requirements. SOPs must be developed which describe in detail how a method is performed in that particular laboratory. Comment: The following methods were lacking an SOP at the time of the inspection: Temperature — Standard Methods, 2550 B-2010 (Aqueous) Dissolved Oxygen — Standard Methods, 4500 O C-2011 (Aqueous) Dissolved Oxygen — Standard Methods, 4500 O G-2011 (Aqueous) The laboratory must have an updated QC/SOP document for the parameters included on their Certified Parameters List (CPL) by December 14, 2018. This must be submitted for review upon completion. A written response is required. D. Finding: The laboratory is not evaluating reagent blank concentrations against the acceptance criterion for Ammonia Nitrogen. Requirement: 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. Ref: NC WW/GW LC Policy. 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 is documenting <0.1 mg/L on the benchsheet for blanks, rather than the actual reading from the instrument. The reporting limit is 0.1 mg/L, so this does not demonstrate adherence to the acceptance criterion. E. Finding: The laboratory is not analyzing an LFMD. 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). Page 4 #43 Lexington Regional WWTP Laboratory Requirement: Include a minimum of one LFM/LFMD for every 20 samples in an analytical batch, or include more LFM/LFMDs if appropriate. Ref: Standard Methods, 3020 B-2005, Rev. 2011. (2) (h). Comment: The laboratory has been analyzing a sample duplicate as part of its routine analysis for Total Phosphorus, Metals, Nitrate, Nitrite and Total Kjeldahl Nitrogen (TKN) but has not been analyzing an LFMD. Comment: Spiked or fortified samples must be treated the same way as the source sample. This includes, but is not limited to, acidification, digestion, filtration and dilution. F. Finding: The laboratory is not analyzing a Method Blank. Requirement: Method blank (MB): Include at least one MB daily or with each batch of 20 or fewer samples, whichever is more frequent. Ref: Standard Methods, 4020 B-2010. (2) (d) and Table 4020:1. Requirement: A reagent blank (method blank) consists of reagent water (see Section 1080) and all reagents (including preservatives) that are normally in contact with a sample during the entire analytical procedure. Ref: Standard Methods, 1020 B-2011. (5). Comment: The laboratory is not analyzing a MB for Ammonia and Total Phosphorus. G. Finding: Preservative is not being added to laboratory fortified blanks (LFB) for Ammonia samples. Requirement: Include at least one LFB daily or per each batch of 20 or fewer samples. Ref: Standard Methods, 4020 B-2010 (2) (e). Requirement: A laboratory -fortified blank [laboratory control standard (LCS)] is a reagent water sample (with associated preservatives) to which a known concentration of the analyte(s) of interest has been added. Process the LFB through all sample preparation and analysis steps. Ref: Standard Methods, 1020 B-2011. (6). Comment: The laboratory is running a standard with each Ammonia run; however, the standard is not a true LFB since it does not have the chemical preservation and (if necessary) dechlorinating agent added to it. H. Finding: A second source standard is not analyzed. Requirement: 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. This standard must be prepared from materials obtained from a source independent from the one used for preparing the calibration standards (often referred to as a second source standard or external reference standard). A second source standard may be: ® a quality control standard obtained from a vendor, ® a standard prepared from primary standards obtained from a second vendor, or ® a standard made from primary standards from the same vendor but from a different lot number (i.e., an independent lot) as those used to make the calibration standards. Page 5 #43 Lexington Regional WWTP Laboratory Laboratory control standards are evaluated to assess whether the lab is in control of the processes involved in the preparation and analysis of specific tests. Laboratory control standards must be similar in composition to the environmental samples. They must contain known concentrations of all analytes of interest and undergo the same preparatory and determinative procedures as the environmental samples. Second source standards must be evaluated using one of the following: vendor supplied criteria, method -defined acceptance criteria, in-house calculated acceptance limits that are statistically -derived from historical data based on three standard deviations from the mean in the detectable range or other statistically viable evaluation criterion. 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. Ref: NC WW/GW LC Policy. Comment: The laboratory was not analyzing a second source standard for Nitrate and Nitrite analyses. Documentation Recommendation: It is recommended that the laboratory document the acceptance criteria for TKN QC standard and spike recoveries and RPD of the LFM/LFMD on the benchsheet so that acceptability can be easily ascertained. I. Finding: The laboratory needs to increase the traceability documentation of purchased materials and reagents, as well as documentation of standards and reagents prepared in the laboratory. Requirement: All chemicals, reagents, standards and consumables used by the laboratory must have the following information documented: Date received, Date Opened (in use), Vendor, Lot Number, and Expiration Date (where specified). A system (e.g., traceable identifiers) must be in place that links standard/reagent preparation information to analytical batches in which the solutions are used. Documentation of solution preparation must include the analyst's initials, date of preparation, the volume or weight of standard(s) used, the solvent and final volume of the solution. This information as well as the vendor and/or manufacturer, lot number, and expiration date must be retained for primary standards, chemicals, reagents, and materials used for a period of five years. Consumable materials such as pH buffers, lots of pre -made standards and/or media, solids and bacteria filters, etc. are included in this requirement. Ref: 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: This finding applies to pH probes and fecal membrane filters as well as purchased and laboratory prepared standards/reagents. Comment: The laboratory benchsheet for Total Suspended Residue has a place for lot number of the filters, but it has not been utilized. The laboratory has begun recording all information except lot number in a logbook specifically for Total Suspended Residue filters. Therefore, a link cannot be made between the lot number and analysis. Comment: This finding also applies when portions of pH buffers are placed into separate containers for daily and/or weekly use. Page 6 #43 Lexington Regional WWTP Laboratory J. Finding: Some benchsheets and/or report summaries reference unapproved methods and/or do not fully reference the approved methods. Requirement: Laboratory procedures, analytical methods, sample preservation, sample containers and sample holding times shall conform to those requirements found in 40 CFR- 136.3. Ref: 15A NCAC 21-1.0805 (a) (1). Comment: The laboratory documentation must reference the method versions as found on the CPL. Comment: The metals digestion log incorrectly cited Standard Methods 18'" edition 3030F, and needs to be updated to Standard Methods, 3030 F-2004. Recommendation: It is recommended that the laboratory review the benchsheets for all parameters to ensure that the correct method reference is cited. K. Finding: Chemical containers are not consistently dated when received and when opened. Requirement: Chemicals must be dated when received and when opened. Ref: 15A NCAC 21-1.0805 (a) (7) (Q. L. Finding: The Total Phosphorus and Settleable Residue benchsheets are lacking pertinent data: volume of sample analyzed. 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 21-1.0805 (a) (7) (H). M. Finding: The laboratory benchsheet is lacking pertinent data: units of measure. Requirement: The following must be documented in indelible ink whenever sample analysis is performed: units of measure. Ref: NC WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen, NC WW/GW LC Approved Procedure for the Analysis of Specific Conductance (Conductivity). 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: 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 21-1.0805 (a) (7) (H). Comment: The laboratory benchsheets for DO lack units of measure. The laboratory benchsheet for Conductivity incorrectly labels the units of measure for "average results" as "pohms/cm" instead of "pmhos/cm". The "Laboratory Worksheet For Plant Analyses" is missing units for initial weight, final weight and net weight for Total Suspended Residue and Total Residue samples. Page 7 #43 Lexington Regional WWTP Laboratory N. Finding: The laboratory benchsheets for Conductivity, Dissolved Oxygen and Temperature are lacking pertinent data: method reference. Requirement: The following must be documented in indelible ink whenever sample analysis is performed: method reference. Ref: NC WW/GW LC Approved Procedure for the Analysis of Specific Conductance (Conductivity), NC WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen, NC UWV/GW LC Approved Procedure for the Analysis of Temperature 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). ®. Finding: The laboratory benchsheet is 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 Temperature, NC WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen, NC WW/GW LC Approved Procedure for the Analysis of pH. Comment: Documentation of the instrument ID is inconsistent across all benchsheets and operator logs. P. Finding: Process control samples are not documented as such. 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. 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 Field parameter notebook calls the aeration basin DO "effluent" and operator logs do not specify location. Comment: The laboratory is recording pH values in operator logs for process control without identifying the values as such. Q. Finding: The laboratory benchsheet is lacking pertinent data: meter calibration time (daily check standard) and date of most recent curve verification. 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: meter calibration time (daily check standard), date of most recent curve verification. Ref: NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine. Page 8 #43 Lexington Regional WWTP Laboratory R. Finding: The volume of 10N NaOH added to standards and samples is not documented. This is considered pertinent data. Requirement: Add a sufficient volume of 10N NaOH solution (1 mL usually is sufficient) to raise pH above 11. If the presence of silver or mercury is possible, use NaOH/EDTA solution in place of NaOH solution. If it is necessary to add more than 1 mL of either NaOH or NaOH/EDTA solution, note volume used, because it is required for subsequent calculations. Ref: Standard Methods, 4500 NH3 D-2011. (4) (b). 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 2H .0805 (a) (7) (A). S. Finding: The date and time that. samples for metals analysis are digested is not consistently documented. Requirement: All laboratories must use printed laboratory bench worksheets that include a space to enter the signature or initials of the analyst, date and time 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: Sample digestion is considered part of the analysis. T. Finding: The laboratory is not documenting the pH of the phosphate buffer solution used in BOD analyses to be 7.2 S.U. after preparation. This is considered pertinent data. 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: Phosphate buffer solution: Adjust pH to 7.2 with 30% NaOH and dilute to 1 L. Ref: Standard Methods, 5210 B-2011. (3) (a). U. Finding: The laboratory benchsheet for Total Phosphorus is lacking pertinent data: volume of sample digested and post -digestion sample volume. 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) 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: Documentation of the initial and final volumes will help the laboratory to verify the appropriate use of, or lack of, a dilution factor. V. Finding: The laboratory is not clearly documenting sample identification for all pH values. Page 9 #43 Lexington Regional WWTP Laboratory 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. The date and time BOD and coliform samples are removed from the incubator must be included on the laboratory worksheet. Ref: 15A NCAC 21-1.0805 (a) (7) (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 21-1.0805 (a) (7). Comment: The laboratory calibration log does not clearly identify buffers used for calibration versus those used to check calibration. The laboratory must clearly identify which buffers/ values are used to calibrate, and which buffers/values are used to verify calibration. Comment: pH values used to determine the necessity of pH adjustment on BOD samples are documented on the Laboratory Worksheet for Plant Analysis, but not identified as such. They appear to be a pH value for compliance data reporting. Proficiency Testing W. 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 Standard Operating Procedure (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. X. Finding: The laboratory is not documenting the preparation of PT Samples. 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. Page 10 #43 Lexington Regional WWTP Laboratory Y. Finding: Additional QC beyond what is routine for Compliance Samples is being analyzed with PT Samples. Requirement: Laboratories are required to analyze an appropriate PT Sample by each parameter method on the laboratory's Certified Parameters Listing (CPL). The same PT Sample may be analyzed by one or more methods. Laboratories shall conduct the analyses in accordance with their routine testing, calibration and reporting procedures, unless otherwise specified in the instructions supplied by the Accredited PT Sample Provider. This means that they are to be logged in and analyzed using the same staff, sample tracking systems, standard operating procedures including the same equipment, reagents, calibration techniques, analytical methods, preparatory techniques (e.g., digestions, distillations and extractions) and the same quality control acceptance criteria. PT Samples shall not be analyzed with additional quality control. They are not to be replicated beyond what is routine for Compliance Sample analysis. Although, it may be routine to spike Compliance Samples, it is neither required, nor recommended, for PT Samples. PT Sample results from multiple analyses (when this is the routine procedure) must be calculated in the same manner as routine Compliance Samples. Ref: Proficiency Testing Requirements, May 31, 2017, Revision 2.0. Comment: The laboratory's common practice is to analyze a purchased reference standard along with the PT Sample as additional QC. Since this is not performed with all Compliance Samples, it is considered additional QC. However, additional QC is recommended as part of the troubleshooting and corrective action process, prior to analyzing remedial PT Samples. Z. Finding: PT Samples for Field Parameters have not been distributed among all operators 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. Conductivity — Standard Methods, 2510 B-2011 (Aqueous) Recommendation: It was noted during the inspection that some conductivity standards exhibited algae growth in the container. It is recommended that the standards be checked periodically for growth and discarded when algae or turbidity is evident. Recommendation: It is recommended that the laboratory pour an aliquot of standards into a beaker or other vessel prior to taking measurements, rather than taking measurements directly from the storage container, in order to minimize contamination of the standards. AA. Finding: The Automatic Temperature Compensator (ATC) has not been verified initially and every 12 months. Requirement: The Automatic Temperature Compensator (ATC) must be verified prior to initial use and annually (i.e., 12 months) thereafter at two temperatures by analyzing a standard or sample at 25°C (i.e., the temperature to which conductivity values are reported) and a temperature(s) that brackets the temperature ranges of the environmental samples routinely analyzed. This may require the analysis of a third temperature reading that is > 25°C. As the temperature increases or decreases, the value of the conductivity Page 11 #43 Lexington Regional WWTP Laboratory standard or sample must be within ±10% of the true value of the standard or ±10% of the value of the sample at 25°C. If not, corrective action must be taken. Ref: NC WW/GW LC Approved Procedure for the Analysis of Specific Conductance (Conductivity). BB. Finding: The calibration verification standards are prepared incorrectly. Requirement: Potassium Chloride (KCI) Conductivity standards may be purchased in the ranges desired, or they may be prepared according to Table 2510:1 of Standard Methods 2510 A-2011. Ref: NC WW/GW LC Approved Procedure for the Analysis of Specific Conductance (Conductivity). Comment: The preparation of the standards in Table 2510:1 indicates that the relationship between mass of KCI used and standard concentration is not linear. CC. Finding: Accuracy (e.g. percent recovery) of QC results are not evaluated to demonstrate the analytical process is in control and the established acceptance criteria are met. Requirement: The value obtained for the post -analysis calibration verification check - standard must read within 10% of the standard's true value. If the obtained value is outside of the ±10% range, corrective action 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 reanalyzed, the data must be qualified. Ref: NC WW/GW LC Approved Procedure for the analysis of Specific Conductance (Conductivity). 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: Many instances were noted where the 88.2 pmhos/cm standard was not within the 10% acceptance criteria. Corrective action must be taken any time there are QC exceedances. Temperature — Standard Methods, 2550 B-2010 (Aqueous) DD. Finding: The laboratory is not performing the annual temperature -measuring device check procedure properly. Requirement: To check a compliance temperature -measuring device, compare readings at two temperatures that bracket the range of compliance samples routinely analyzed against a National Institute of Standards and Technology (NIST) traceable temperature - measuring device and record all four readings. The readings from both devices must agree within 0.5 °C. Ref: NC WW/GW LC Approved Procedure for the Analysis of Temperature. Comment: The laboratory is checking the temperature -measuring device at a single temperature. EE. Finding: The temperature sensor on the Hach H2606 meter (s/n: 010012068) used to obtain reported temperature values was not checked against an NIST traceable temperature -measuring device initially. Requirement: All compliance temperature -measuring devices without a valid NIST certificate must be checked initially and every 12 months against an NIST traceable Page 12 #43 Lexington Regional WVVTP Laboratory temperature -measuring device and the process documented. Documentation must include the serial number of the device being checked. The serial number, stated accuracy and expiration date of the NIST traceable temperature -measuring device used in the comparison must also be documented. Verification data must be kept on file and be available for inspection for 5 years. (NOTE: Vendors or other Certified laboratories may provide assistance in meeting this requirement. When a vendor or other Certified laboratory provides this assistance, they must provide a copy of their NIST Certificate or the serial number, accuracy and calibration expiration date.) Ref: NC WW/GW LC Approved Procedure for the Analysis of Temperature. FF. Finding: The laboratory is not standardizing the sodium thiosulfate titrant initially. Requirement: Standard sodium thiosulfate titrant: Dissolve 6.205 g NA2S2O3 • 51­12O in distilled water. Add 1.5 mL 6N NaOH or 0.4 g solid NaOH and dilute to 1000 mL. Standardize with bi-iodate solution. Ref: Standard Methods, 4500 O C-2011. (2) (e). Chlorine. Total Residual — Standard Methods, 4500 Cl G-2011 (Aqueous) Recommendation: The laboratory is currently verifying the factory -set calibration curve with standard concentrations (i.e. 20, 200, 500, 1000 and 2000 pg/L) that do not place enough emphasis on the range between permit and compliance limits. It is recommended that the laboratory change the concentrations to 20, 40, 50, 200 and 400 pg/L. GG. Finding: The annual Factory -set Calibration curve verification did not pass the individual standard recovery criteria. Requirement: The calibration standard values obtained must not vary by more than 10% from the known value for standard concentrations greater than or equal to 50 pg/L and must not vary by more than 25% from the known value for standard concentrations less than 50 pg/L. Ref: NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine. Please submit a passing calibration curve verification with the report reply. Requirement: If the factory -set readings vary by more than the stated acceptance criteria, the stored calibration program must not be used for compliance monitoring until troubleshooting is carried out to determine and correct the source of error. Ref: NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine. Comment: The 200 pg/L standard had a recovery of 65%, while the 20 pg/L standard had a recovery of 50%. HH. 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: A Reagent Blank is made from the same laboratory water source used to make liquid standards. The concentration of Reagent Blanks must not exceed 50% of the reporting limit (i.e., the lowest calibration or calibration verification standard concentration) or corrective action must be taken. Page 13 #43 Lexington Regional WWTP Laboratory Finding: Values less than the established reporting limit are being reported on the Discharge Monitoring Report (DMR). Requirement: For analytical procedures requiring analysis of a series of standards, the concentrations of those standards must bracket the concentration of the samples analyzed. One of the standards must have a concentration equal to the laboratory's lower reporting concentration for the parameter involved. Ref: 15A NCAC 02H .0805 (a) (7) (1). Requirement: For all calibration options, the range of standard concentrations must bracket the permitted discharge limit concentration, the range of sample concentrations to be analyzed and anticipated PT Sample concentrations. One of the standards must have a concentration equal to or less than the permitted discharge limit. The lower reporting limit concentration is equal to the lowest standard concentration. Sample concentrations that are less than the lower reporting limit must be reported as a less -than value. Ref: NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine. RHH — Standard Methods, 4500 H+R-2011 (Aqueous) JJ. Finding: Instances were observed where the pH calibration check standard did not read within ± 0.1 S.U. of the true value and the meter was not recalibrated. Requirement: If the meter response shows a difference greater than 0.1 pH unit from expected value, look for trouble with the electrodes or potentiometer (see 4500-H+ B.5A and b). Ref: Standard Methods, 4500 H+ B-2011. (4) (a). Requirement: All check standard buffers must read within ±0.1 S.U. to be acceptable. If the meter verification does not read within ±0.1 S.U., corrective actions must be taken before any samples are analyzed. Ref: NC WW/GW LC Approved Procedure for the Analysis of pH. Comment: If the check buffer does not read within ±0.1 S.U., the lab should first try pouring a new aliquot of the check buffer and reading it again. If it still does not read within ± 0.1 S.U., the meter must be recalibrated. If, after recalibration, the check buffer does not read within ± 0.1 S.U., the meter and/or probe operation may be suspect and may require servicing. If the laboratory does not have a back-up meter/electrode, or another meter/electrode cannot be procured, it is recommended that the lab report the measured pH results with a qualifier that indicates the value is estimated. Comment: Possible corrective actions include: check the meter calibration procedure, refer to the trouble shooting section in the instrument manual, and check the buffers. Even though the buffers were within their expiration dates, the method and vendors point out that the expiration date is for unopened buffers. Once buffers are opened the methods and manufacturers state that buffers degrade and should be replaced in four weeks. Nitrogen, Ammonia — Standard Methods, 4500 NH3 D-2011 (Aqueous) Recommendation: It is recommended that each individual sample and standard is documented to have a pH > 11 S.U. rather than a single Yes/No option on the benchsheet. KK. Finding: Samples containing residual chlorine are not neutralized immediately upon collection. Page 14 #43 Lexington Regional WWTP Laboratory 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). ILL. Finding: The laboratory is not chemically preserving the samples to a pH <2 S.U. within 15 minutes of collection. Requirement: 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: 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 II, Footnote 2. MM. Finding: The laboratory did not verify quantitation at the minimum reporting level initially, nor is it verified quarterly. Requirement: 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 (preferably daily) by analyzing a QC Sample (subjected to all sample preparation steps) spiked at 1 to 2 times the MRL. Laboratories must define acceptance criteria for the operational range — including the MRL — in their QA documentation. Ref: Standard Methods, 4020 B-2011. (1) (c). Bacteria, Coliform Fecal — Standard Methods, 9222 D-1997 (Aqueous) Comment: The water level in the water bath was not above the plates on August 15, 2018. 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. Anchor dishes below water surface to maintain critical temperature requirements. Acceptable corrective action (i.e., the water level was corrected and a mark indicating the acceptable water level was added to the water bath interior) was performed by the laboratory and approved by the auditor during the inspection. No further response is necessary for this corrected Finding. Comment: The laboratory was not using the required magnification to count fecal coliform colonies. Standard Methods, 9222 D-1997. (2) (e) states: Count colonies with a low -power (10 to 15 magnifications) binocular wide -field dissecting microscope or other optical device. Acceptable corrective action (i.e., the analyst began using a 10X microscope to count colonies) was performed by the laboratory and approved by the auditor during the inspection. No further response is necessary for this corrected Finding. Page 15 #43 Lexington Regional WWTP Laboratory Comment: It was noted that the laboratory was obtaining the pH of the agar when it was still warm enough to not have solidified. This was considered acceptable. Comment: It was observed during the inspection that the fecal water bath thermometer was resting of the bottom of the incubator. This is not ideal, as the heating elements for water baths are often housed at the bottom. The laboratory placed a stopper on the thermometer during the inspection to keep it from resting on the bottom. Recommendation: It is recommended that the laboratory document counts of zero as "0" rather than "<1". The laboratory would still report a count of 0 colonies as "<1" on the DMR. NN. Finding: Sample results are 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 Ref: NC WW/GW LC Policy Comment: On May 24, 2018 the 100 ml, 10 mL, and 1 mL plates had counts of 3, 2, and 0 colonies respectively. The laboratory reported 8 col/100 mL, but the calculated value should have been 5 col/100 mL. Bacteria. Coliform Fecal — Standard Methods, 9222 D-1997 (Aqueous) Bacteria, Coliform Fecal — Standard Methods 9221 C E-2006 (MPN) 24hr 503 (Non -Aqueous) 00. Finding: The laboratory is not verifying the temperature of the autoclave with a maximum registering thermometer (MRT). Requirement: For routine use, verify the autoclave temperature weekly by using a maximum registering thermometer (MRT) to confirm that 121 °C has been reached. Ref: Standard Methods, 9020 B-2005. (4) (h). Requirement: Each laboratory requesting certification must contain or be equipped with the glassware, chemicals, supplies and equipment required to perform all analytical procedures included in their certification. Ref: 15A NCAC 02H .0805 (a) (6) (H). PP. Finding: The laboratory is not documenting the actual time period at sterilization temperature and the total run time. Requirement: Record items sterilized and sterilization temperature, along with total run- time (exposure to heat) actual time period at sterilization temperature, set and actual pressure readings, and initials of responsible person for each run cycle. Ref: Standard Methods, 9020 B-2005. (4) (h). Nitrogen, Total Kieldahl — Standard Methods, 4500 Narg B-2011 (Standard Methods, 4500 NH3 C-2011) (Aqueous) Page 16 #43 Lexington Regional WWTP Laboratory Recommendation: It is recommended that the laboratory switch from Mercuric Sulfate to Cupric Sulfate as the catalyst for safety and disposal reasons. QQ. Finding: The laboratory is not standardizing the sulfuric acid titrant monthly. Requirement: All of the reagents listed for the determination of Nitrogen (Ammonia), Section 4500-NH3 C.3 are required. Ref: Standard Methods, 4500 No,9 B-2011. (3). Requirement: Restandardize once a month or when improper storage occurs. Ref: Standard Methods, 2020 B-2011. (2) (b). Nitrogen, Nitrate — Standard Methods, 4500 NO3" ®-2011 (Aqueous) Comment: The laboratory was previously performing analyses using the method of known addition, although the instrument is capable of reading concentration directly. No explanation of why this was being performed could be found. The laboratory has recently been contracting this analysis to a commercial laboratory. The laboratory will be looking into direct calibration and reading of sample concentration. If the laboratory switches to the method of directly reading sample concentration, they will need to verify quantitation at the reporting limit upon first use and on a quarterly basis thereafter. RR. Finding: The volume of spike solution exceeds 5% of the total MS volume. Requirement: The volume of spike solution used in MS preparation must in all cases be 5 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 constitutes >1 % of the total sample volume, the sample concentration must be adjusted by calculation. Ref: NC WW/GW LC Policy. Nitrogen, Nitrite — Standard Methods, 4500 NO2- B-2011 (Aqueous) SS. Finding: The laboratory did not verify quantitation at the reporting level initially, nor is it verified quarterly. Requirement: 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 (preferably daily) by analyzing a QC Sample (subjected to all sample preparation steps) spiked at 1 to 2 times the MRL. Laboratories must define acceptance criteria for the operational range — including the MRL — in their QA documentation. Ref: Standard Methods, 4020 B-2011. (1) (c). TT. Finding: The laboratory is not evaluating the recoveries of the back -calculated standards. 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: The back -calculated and true concentrations should agree within ± 10%, unless different criteria are specified in an individual method. At the lower limit of the operational range, acceptance criteria are usually wider. Such criteria must be defined in the laboratory's QA plan. Ref: Standard Methods, 4020 B-2011. (2) (a). Page 17 #43 Lexington Regional WWTP Laboratory UIJ. Finding: A calibration blank and calibration verification standard are not analyzed initially and at the end of the sample group. 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. Comment: The laboratory was occasionally filtering industrial samples that are turbid, but not filtering compliance samples. The laboratory was told to follow the method for addressing turbidity as described in Standard Methods, 4500 P E-2011. (4) (b). W. Finding: The laboratory is not analyzing samples at the correct wavelength. Requirement: After at least 10 min but no more than 30 min, measure absorbance of each sample at 880 nm, using reagent blank as the reference solution. Ref: SM 4500 P E-2011 (4) (a). Comment: The laboratory is analyzing samples at a wavelength of 650 nm. WW. Finding: The laboratory is zeroing the spectrophotometer improperly. Requirement: Use a distilled water blank with the combined reagent to make photometric readings for the calibration curve. Ref: Standard Methods, 4500 P E-2011. (4) (c). Comment: The laboratory is zeroing the instrument with the digested blank, which does not give a true indication of whether reagents and the preparatory steps contribute to measurement uncertainty. Bacteria, Coliform Fecal — Standard Methods 9221C E-2006 (MPN) 24hr 503 (Non -Aqueous) Comment: The laboratory is currently analyzing reconstituted dry -weight residue for pH. This is not required. XX. Finding: The laboratory is not analyzing 30 grams of sample for analysis. Requirement: In a sterile dish, weigh out 30.0 grams of well mixed sample. Ref: Control of Pathogens and Vector Attraction in Sewage Sludge, EPA/625/R-92/013, (July 2003) Appendix F. (1.1), solid samples (1). Comment: The laboratory is analyzing 10 g of sample. Decreasing the sample amount could bias the results since bacteria may not be evenly distributed throughout the compost pile being sampled. YY. Finding: The laboratory is not collecting 7 grab samples for analysis. Requirement: To demonstrate that a given domestic sludge sample meets Class B Pathogen requirements under alternative 1, the density of fecal coliform from at least seven samples of treated sewage sludge must be determined and the geometric mean of the fecal coliform density must not exceed 2 million Colony Forming Units (CFU) or Most Page 18 #43 Lexington Regional WWTP Laboratory Probable Number (MPN) per gram of total solids (dry weight basis). Ref: Control of Pathogens and Vector Attraction in Sewage Sludge, EPA/625/R-92/013, (July 2003) Appendix F. (1) (1.1). Finding: The pH of the A-1 media is not adjusted and documented to be 6.9 ± 0.1 S.U. Requirement: Check and record the pH of a portion of each medium after sterilization. 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. Ref: Standard Methods 9020 B-2005 (5) 0) (1). Requirement: Adjust to pH 6.9 ± 0.1 S.U. Ref: Standard Methods 9221 E-2006 (2) (a) Comment: The pH of the media was consistently around 8.0 S.U. AAA. Finding: The laboratory is not documenting the time required for the autoclave to reach sterilization temperature. 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: Use autoclaves of sufficient size to prevent internal crowding; constructed to provide uniform temperatures within the chamber (up to and including the sterilizing temperature of 121 °C); and capable of reaching the desired temperature within 15 minutes. Ref: Standard Methods 9030 B-2006 (3) BBB. Finding: The laboratory is not monitoring the quality of the reagent water. Requirement: At a minimum, reagent water used to make dilutions, prepare buffered dilution/rinse water or prepare 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: Total Organic Carbon < 1.0 mg/L Specific Conductance < 2 pmhos/cm Heavy Metals, single element < 0.05 mg/L Heavy Metals, Total of specified elements < 0.10 mg/L If the facility is using vendor purchased reagent water or dilution/rinse water, this testing is not required as long as the Certificate of Analysis from the manufacturer meets these requirements and is kept on file. Ref: NC WW/GW LC Policy. CCC. Finding: The drying cycle is not repeated for an additional 1 hour on the second day. Requirement: Place in an oven at 103 to 105°C overnight. Cool to balance temperature in a desiccator and weigh. Repeat drying (1 h), cooling, weighing, and desiccating steps until weight change is less than 4% or 50 mg, whichever is less. Ref: Standard Methods, 2540 G-2011 (3) (a) (2) (b). Page 19 #43 Lexington Regional WWTP Laboratory Comment: The laboratory is drying samples overnight but is not repeating the 1 hour drying cycle to verify that the samples are at constant weight. DDD. Finding: The "largest volume" value used in the MPN calculation is not properly determined. Requirement: Compute the MPN/g according to the following equation: Ref: Control of Pathogens and Vector Attraction in Sewage Sludge, EPA/625/R-92/013, (July 2003) Appendix F. (1.1), liquid samples (6). Comment: The "largest volume" in the calculation above is the volume of the original solution (30 g in 270 ml) that is in 1 mL of the mixture that is incubated. The laboratory combines 10 mL of the original solution with 10 mL of media. This new 20 mL solution has 10 mL of the original solution. Therefore, you have 0.50 ml of original sample in 1 ml of the new solution that gets incubated. In this case, the "largest volume" value that is used in the calculation is 0.50 mL. The laboratory was using a volume of 10 mL in the calculation. BOD — Standard Methods, 5210 B-2011 (Aqueous) Recommendation: It is recommended that the laboratory analyze a seeded blank to check the calculated seed correction factor (SCF). Recommendation: It is recommended that the sample pH values be documented on the BOD worksheet, rather than the Laboratory Worksheet for Plant Analysis. EEE. Finding: Extra nutrient, mineral, and buffer solutions are not added to the Biochemical Oxygen Demand (BOD) bottles containing more than 67% (i.e., > 201 mL) sample. Requirement: When a bottle contains more than 67% of the sample after dilution, nutrients may be limited in the diluted sample and subsequently reduce biological activity. In such samples, add the nutrient, mineral, and buffer solutions (3a through e) directly to diluted sample at a rate of 1 mUL (0.30 mU300-mL bottle) or use commercially -prepared solutions designed to dose the appropriate bottle size. Ref: Standard Methods, 5210 B- 2011. (5) (c) (2). FFF. Finding: The laboratory is not evaluating the drift check of the Dissolved Oxygen (DO) meter to demonstrate the analytical process is in control and the established criteria are met. Requirement: If the membrane electrode method is used, take care to eliminate drift in calibration between initial and final DO readings. Ref: Standard Methods, 5210 B-2011. (5) (g)• Requirement: Immediately after calibration, measure the DO of a BOD bottle of dilution water. Stopper the bottle. Document the concentration on the benchsheet (day one initial drift check). At the end of the sample set reanalyze the drift check bottle and document the concentration (day one final drift check). The laboratory should verify the DO Meter calibration throughout the sample set if needed. Repeat process on Day 5. If the meter Page 20 #43 Lexington Regional WWTP Laboratory drifts more than 0.20 mg/L, recalibrate meter and reanalyze all samples since the last drift check. Ref: NC WW/GW LC Policy. Comment: The laboratory was checking the drift at the beginning and end of the run with the probe and documenting the results, but not evaluating the results of the drift check. Examination of past benchsheets showed that the final drift check value was always within ± 0.2 mg/L of the initial drift check. Residue, Total — Standard Methods, 2540 B-2011 (Aqueous) Residue, Suspended — Standard Methods, 2540 D-2011 (Aqueous) Recommendation: It is recommended that the laboratory use a tiered acceptance criterion for duplicates that better evaluates the results at each sample location. In this case, 20% relative percent difference (RPD) would be appropriate for the smaller values of routine effluent samples, while 10% RPD would be better suited for the larger values characteristic of influent samples. Recommendation: It is recommended that the laboratory relabel "mLs" to "sample volume (mL)" and "mg/L" to "results (mg/L)" on the laboratory benchsheet. GGG. Finding: The samples are not weighed to constant weight, nor is an annual drying study to verify the adequacy of the drying time, performed. Requirement: 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. Ref: NC WW/GW LC Policy. Residue, Total — Standard Methods, 2540 B-2011 (Aqueous) Recommendation: It is recommended that the laboratory purchase and use a 50 mL wide bore pipet to measure 50 mL of sample, rather than using a 25 mL wide bore pipet multiple times. HHH. Finding: The laboratory does not report results of all tests on the characteristics of the effluent. Requirement: 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. Ref: 15A NCAC 2B .0506 (b) (3) (J). Comment: The laboratory is analyzing influent and effluent samples for Total Residue, but this parameter is not on the permit and is not being reported on the DMR. Residue, Suspended — Standard Methods, 2540 D-2011 (Aqueous) Comment: The laboratory was not analyzing a volume of sample to yield a minimum of 2.5 mg dried residue. Standard Methods, 2540 D-2011 (3) (b) states: Choose sample volume to yield between 2.5 and 200 mg dried residue. Acceptable corrective action (i.e., the laboratory began analyzing larger volumes in order to achieve the necessary minimum residue weight after receiving the parameter checklist prior to the inspection) was performed by the laboratory and approved by the auditor during the inspection. No further response is necessary for this corrected Finding. Page 21 #43 Lexington Regional WWTP Laboratory III. Finding: The laboratory is not weighing filters to constant weight or analyzing a dry filter blank daily. Requirement: If pre -prepared filters are not used, the method requires that filters must be weighed to a constant weight after washing. Repeat cycle of drying, cooling, desiccating, and weighing until a constant weight is obtained or until weight change is less than 4% of the previous weighing or 0.5 mg, whichever is less. In lieu of this process, it is acceptable to analyze a single daily dry filter blank to fulfill the method requirement of drying all filters to a constant weight prior to analysis. Ref: NC WW/GW LC Policy. JJJ. 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. To obtain the required residue yield, successive aliquots of samples may be added to the same dish after evaporation or adjust reporting level based upon the weight gain and sample volume used. The minimum reporting value is established at 2.5 mg/L based upon a sample volume used of 1000 mL. Ref: NC WW/GW LC Policy. Comment: For example, for an effluent sample collected January 5, 2018, 500 mL of sample was filtered, and a value of 2.47 mg/L was reported on the DMR, instead of <5 mg/L. Metals — Standard Methods, 3120 B-2011 (Aqueous) Comment: The laboratory's acceptance criterion for the LFB is 85-115%, which is required by Standard Methods, 3020 B-2011 (3) (b). However, Standard Methods 3120 B-2011 (4) (f) says that "results should agree to within 5% of the certified values". While QC criteria written in the method supersede that found in 3020, 85-115% recovery may be used in this case because the method states that it "should" be within 5%, which is considered a, recommendation. KKK. Finding: The laboratory is not analyzing a Calibration Blank immediately after calibration and after each sample. Requirement: Begin each sample run with an analysis of the calibration blank, then analyze the method blank. Analyze samples, alternating them with analyses of calibration blank. Subtract result of an adjacent calibration blank from each sample result to make a baseline drift correction. Ref: Standard Methods, 3120 B-2011 (4) (d) and (5) (a). Comment: The laboratory was analyzing a calibration blank at the end of the sample set. LLL. Finding: The laboratory is not analyzing a method blank prior to sample analysis. Requirement: Begin each sample run with an analysis of the calibration blank, then analyze the method blank. Ref: Standard Methods, 3120 B-2011. (4) (d). Comment: The laboratory was analyzing a method blank at the end of the sample set. MMM. Finding: The laboratory is not analyzing an Instrument Check Standard (ICS) prior to sample analysis and after every ten samples. Requirement: Before analyzing samples, analyze instrument check standard. Concentration values obtained should not deviate from the actual values by more than ± Page 22 #43 Lexington Regional WWTP Laboratory 5% (or the established control limits, whichever is lower). Ref: Standard Methods, 3120 B- 2011 (4) (c). Requirement: Analyze instrument check standard once per ten samples to determine if significant instrument drift has occurred. If agreement is not within ± 5% of the expected values (or within control limits, whichever is lower), terminate analysis of samples, correct problem, and recalibrate instrument. Ref: Standard Methods, 3120 B-2011 (4) (e). Comment: The laboratory was analyzing the ICS at the end of the sample set, which is also required. Comment: The ICS is equivalent to the Calibration Verification Standard (CVS). It is an undigested standard from the same source as the calibration curve. NNN. Finding: The laboratory's acceptance criterion for the ICS does not meet the method requirements. Requirement: Before analyzing samples, analyze instrument check standard. Concentration values obtained should not deviate from the actual values by more than ± 5% (or the established control limits, whichever is lower). Ref: Standard Methods, 3120 B- 2011. (4) (c). Requirement: Analyze ICS once per 10 samples to determine if significant instrument drift has occurred. If agreement is not within ± 5% of the expected values (or the established control limits, whichever is lower), terminate analysis of samples, correct problem and recalibrate instrument. Ref: Standard Methods, 3120 B-2011. (4) (e). Comment: The laboratory's acceptance criterion of the ICS is 90-110%. 000. Finding: The laboratory is not performing a Reporting Limit Verification (RLV) by analyzing a reporting limit check solution before sample analysis. Requirement: Reporting limit verification (RLV): Verify with each calibration that the instrument is capable of accurately quantifying at the reporting limit. Prepare reporting limit check solution (RLCS) at the reporting limit concentration, or lower, and analyze it after calibration but before any samples are analyzed. Ref: Standard Methods, 3020 B-2005. (2) (e). Comment: The laboratory performs the RLV at the end of the sample set. PPP. Finding: The calibration standards are not being prepared properly. Requirement: Combine appropriate volumes of the stock solutions in 100-mL volumetric flasks. Add 2 mL 1+1 HNO3 and 10 mL 1+1 HCL and dilute to 100 mL with water. Ref: Standard Methods, 3120 B-2011. (3) (e). Comment: The laboratory was adding 2 mL of concentrated HNOsto standard solutions. QQQ. 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 Page 23 #43 Lexington Regional WWTP Laboratory 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 laboratory is using 5% spike solution per total volume to prepare the LFM/LFMD. RRR. Finding: The laboratory is not reanalyzing one or more samples near the end of the analytical run. Requirement: Reanalyze one or more samples analyzed just before termination of the analytical run. Results should agree to within ± 5%, otherwise all samples analyzed after the last acceptable instrument check standard analysis must be reanalyzed. Ref: Standard Methods, 3120 B-2011. (4) (e). Comment: The laboratory performed a duplicate analysis on the first sample in the sample set, but this is a true duplicate, not simply a reanalysis as required above. The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks, etc.) and contract lab reports to Discharge Monitoring Reports (DMRs) submitted to the North Carolina Division of Water Resources. Data were reviewed for Lexington Regional WWTP Laboratory NPDES permit # NC0055786 for October 2017, January 2018 and May 2018. The following errors were noted: Value on Benchsheet Date Parameter Location Value on DMR *Contract Lab Data 5/1/2018 Cyanide Effluent < 5 pg/L* 5 pg/L To avoid questions of legality, it is recommended that you contact the appropriate Regional Office for guidance as to whether an amended DMR will be required. A copy of this report will be made available to the Regional Office. 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. Report prepared by: Michael Cumbus Date: August 29, 2018 Report reviewed by: Anna Ostendorff Date: September 14, 2018 Weight Verification (NC WW/GW LC Policy 05/23/2008) ASTM Class 1 and 2 weights must be verified at leastevery5 years. ASTMClass1 weights (20 g to 25 - kg) and ASTM Class 2 weights (10 g to 1 mg) are equivalent to the NBS Class S weights specified in 15A NCAC 2H .0805 (a) (7) (K). Verification may be accomplished by: 1. Sending laboratory weights back to the manufacturer for recertification - reference weights shall be calibrated by a body that can provide traceability to ASTM specifications, or 2. Checking laboratory weights against certified reference weights (i.e., weights that have been recertified as above) and found to be within ASTM Class 1 or Class 2 tolerances (see table below) - often the balance service technician may provide this service. Note: Although some manufacturers will assign a one-year calibration due date, 5 years is considered an acceptable calibration interval due to the limited use of the reference weight set. Documentation of weight verifications or recertification must be maintained for 5 years. If the condition of a weight(s) is in question at any time due to damage (e.g., corrosion, nicks, scratching, etc.), the laboratory must have that weight(s) re -verified as described above. Maximum tolerances (Ref. ASTM E 617-97, 2003) Denomination Maximum tolerance for ASTM Class 1 and 2 weights, (± mg) 500 g 1.2 300 g 0.75 200 g 0.50 100 g 0.25 50 g 0.12 30 g 0.074 20 g 0.074 log 0.074 5 g 0.054 3 g 0.054 2 g 0.054 1 g 0.054 500 mg 0.025 300 mg 0.025 200 mg 0.025 100 mg 0.025 50 mg 0.014 30 mg 0.014 20 mg 0.014 10 mg 0.014 5 mg 0.014 3 mg 0.014 2 mg 0.014 1 mg 0.014 Vl Z f/1 N N N N (; N ',; N N N CN CN NO m O N1 NO co CL m m m m m m m m z m m m m m N U N D N g N N CL' N N N N N© uj N ;;----(( N 5 N N N M W M M U M 0 M� M M M ,`� M (j M gym-. M W uiaur uivuu)ivu�i8u)i�uiL�W uWi ui u`iSS2LLcn�vi viFq zw N 7 V1 3 7 O �J O .-1 �3 /may � 21, � N a pPyy 0. w r W G n W N N p N N T CL U) W © F- m m v L of Q N Ll C5 N t�i N z CL