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HomeMy WebLinkAbout#5633_2023_0914_MC_FINAL NC Department of Environmental Quality | Division of Water Resources | Laboratory Certification Branch 4405 Reedy Creek Road | 1623 Mail Service Center | Raleigh, North Carolina 27699-1623 919-733-3908 November 2, 2023 5633 Mr. Benjamin Marion City of King WTP P.O. Box 1132 King, NC 27021- Subject: North Carolina Wastewater/Groundwater Laboratory Certification Branch (NC WW/GW LCB) Maintenance Inspection Dear Mr. Marion: Enclosed is a report for the inspection performed on September 14, 2023 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, 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 02H .0800. A copy of the laboratory’s Certified Parameter List at the time of the audit is attached. This list will not 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 have questions or need additional information, please contact me at (919) 733- 3908 Ext. 259. Sincerely, Beth Swanson Technical Assistance & Compliance Specialist Division of Water Resources Attachment cc: Michael Cumbus, Todd Crawford, #5633 On-Site Inspection Report LABORATORY NAME: City of King WTP NPDES PERMIT #: NC0088897 ADDRESS: 6949 DonnahaIs Rd Tobaccoville, NC 27050 CERTIFICATE #: 5633 DATE OF INSPECTION: September 14, 2023 TYPE OF INSPECTION: Field Municipal Initial AUDITOR: Michael Cumbus LOCAL PERSONS CONTACTED: Benjamin Marion, Taylor Baskin and Mark Danley I. INTRODUCTION: This laboratory was inspected by a representative of the North Carolina Wastewater/Groundwater Laboratory Certification Branch (NC WW/GW LCB) to verify its compliance with the requirements of 15A NCAC 02H .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. Staff were forthcoming and responded well to suggestions from the auditor. The laboratory records all results and supporting documentation electronically. Staff were reminded that electronic records must be maintained for five years. All required Proficiency Testing (PT) Samples have been analyzed and the laboratory has fulfilled its PT requirements for the 2023 PT Calendar Year. Any time changes are made to laboratory procedures, Quality Assurance (QA) and/or Standard Operating Procedure (SOP) document(s) must be updated and relevant staff retrained. Staff must acknowledge that they have read and understand the changes as part of the documented training program. The same requirements apply when changes are made in response to Findings, Recommendations or Comments listed in this report, to ensure the methods are being performed as stated, references to methods are accurate, and the QA and SOP documents are 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. Revisions to the SOPs and a copy of the laboratory’s documented training program (see Finding A), based on the Findings, Comments and Recommendations within this report must be submitted to this office by January 30, 2024. Page 2 #5633 City of King WTP The laboratory is reminded that SOPs are required to be reviewed at least every two years and 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”. Contracted analyses are performed by Pace Analytical Services LLC – Eden NC (Certification #633) and Statesville Analytical Holdings LLC (Certification #440). Approved Procedure documents for the analysis of the facility’s currently certified Field Parameters were provided at the time of the inspection. III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS: Documentation Recommendation: It is recommended that the laboratory replace the term “operator” on the laboratory benchsheet with “sample collector” for clarity. A. Finding: The laboratory lacks a documented training program. Requirement: Each laboratory shall develop and implement a documented training program that includes the following: that staff have the education, training, experience, or demonstrated skills needed to generate quality control results within method-specified limits and that meet the requirements of these Rules; that staff have read the laboratory quality assurance manual or applicable Standard Operating Procedures; that staff have obtained acceptable results on Proficiency Testing Samples pursuant to Rule .0803(1) of this Section or other demonstrations of proficiency (e.g., side-by-side comparison with a trained analyst, acceptable results on a single-blind performance evaluation sample, an initial demonstration of capability study prescribed by the reference method). Ref: 15A NCAC 02H .0805 (g) (5). B. Finding: The laboratory does not document all traceability information for purchased materials, reagents and standards. Requirement: 15A NCAC 02H .0805 (a) (7) (K) and (g) (7) requires laboratories to have a documented system of traceability for the purchase, preparation, and use of all chemicals, reagents, standards, and consumables. That system must include documentation of the following information: 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 LCB Traceability Documentation Requirements for Chemicals, Reagents, Standards and Consumables Policy (03/27/2020). Comment: Dates opened were missing from the Reagent Log but were written on the individual containers as required. While this can provide a traceability link to analyses while the chemicals are still in use, that link is lost once the bottles are discarded. C. Finding: The laboratory benchsheet is lacking required documentation: the method or SOP reference; the laboratory identification; the instrument identification; the signature or initials of Page 3 #5633 City of King WTP the analyst; the date of sample analysis; the time of sample analysis; the proper units of measure and the facility name or permit number. Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data shall be traceable to the associated sample analyses and shall consist of: the method or Standard Operating Procedure; the laboratory identification; the instrument identification; the signature or initials of the analyst, the date and time of sample collection; the time of sample analyses (when required to document a required holding time or when time-critical steps are imposed by the method, a federal regulation, or this Rule); and the proper units of measure. Each item shall be recorded each time samples are analyzed. Analyses shall conform to methodologies found in Subparagraph (a)(1) of this Rule. Ref: 15A NCAC 02H .0805 (g) (2) (A) (B) (C) (E) (G) (H) and (L). Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref: 15A NCAC 02H .0805 (g) (4). Requirement: The following must be documented in indelible ink whenever sample analysis is performed: Facility name or permit number. Ref: NC WW/GW LCB Approved Procedure for the Analysis of pH. Comment: If the sample collector and the analyst are the same person, the laboratory may include a blanket statement to this effect on the benchsheet. Comment: Instrument identification and units of measure are lacking for pH analyses. All other items are lacking for both pH and TRC analyses. D. Finding: The laboratory benchsheet for Total Residual Chlorine (TRC) is lacking required documentation: Date of most recent TRC calibration curve verification and the facility name or permit number. Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref: 15A NCAC 02H .0805 (g) (4). Requirement: The following must be documented in indelible ink whenever sample analysis is performed: Date of most recent calibration curve generation or calibration curve verification and the facility name or permit number. Ref: NC WW/GW LCB Approved Procedure for the Analysis of Total Residual Chlorine (DPD Colorimetric by SM 4500 Cl G-2011). Proficiency Testing E. Finding: The laboratory is lacking a documented plan for PT procedures. Requirement: Each laboratory shall develop documentation outlining the analytical quality control practices used for the Parameter Methods included in its Certification, including Standard Operating Procedures for each certified Parameter Method. Quality assurance, quality control, and Standard Operating Procedure documentation shall indicate the effective date of the document and be reviewed every two years and updated if changes in procedures are made. Each laboratory shall have a formal process to track and document review dates and any revisions made in all quality assurance, quality control, and Standard Operating Procedure documents. Supporting Records shall be maintained as evidence that these practices are implemented. The quality assurance, quality control, and Standard Operating Procedure documents shall be available for inspection by the State Laboratory. Ref: 15A NCAC 02H .0805 (a) (7). Page 4 #5633 City of King WTP 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 plan must also address the laboratory’s process for submission of PT Sample results and related Corrective Action Reports (CARs). Ref: Proficiency Testing Requirements, January 1, 2023, Revision 6, Section 3.0. F. 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, however the instructions must be maintained. Ref: Proficiency Testing Requirements, January 1, 2023, Revision 6, Section 3.6. Comment: Dating and initialing the instruction sheet for the TRC PT Sample would satisfy the documentation requirement. Quality Assurance/ Quality Control G. Finding: The laboratory is not calibrating the mechanical volumetric liquid-dispensing devices used for critical measurements. Requirement: Mechanical volumetric liquid-dispensing devices (e.g., fixed and adjustable auto-pipettors and bottle-top dispensers) shall be calibrated at least once every twelve months. Ref: 15A NCAC 02H .0805 (g) (10). Comment: The laboratory uses mechanical pipettes that do not get calibrated for preparing the TRC PT Sample, which is considered a critical measurement. The laboratory also has Class A glass pipettes which may be used instead. H. Finding: SOPs have not been fully developed for the methods included on the laboratory’s Certified Parameters Listing (CPL). Requirement: Each laboratory shall have a documented analytical quality assurance and quality control program. Each laboratory shall have a copy of each approved test, analysis, measurement, or monitoring procedure being used in the laboratory. Each laboratory shall develop documentation outlining the analytical quality control practices used for the Parameter Methods included in its Certification, including Standard Operating Procedures for each certified Parameter Method. Quality assurance, quality control, and Standard Operating Procedure documentation shall indicate the effective date of the document and be reviewed every two years and updated if changes in procedures are made. Each laboratory shall have a formal process to track and document review dates and any revisions made in all quality assurance, quality control, and Standard Operating Procedure documents. Supporting Records shall be maintained as evidence that these practices are implemented. The quality assurance, quality control, and Standard Operating Procedure documents shall be available for inspection by the State Laboratory. Ref: 15A NCAC 02H .0805 (a) (7). Comment: Since there are often changes in technology or options within a particular method that are not covered in published references the laboratory SOP is the prescriptive reference Page 5 #5633 City of King WTP document that describes a laboratory’s analytical procedure in detail. This document is intended to be the reference for analysts performing the specified test procedure. Please review the SOPs and update as necessary to ensure that the method is being performed as stated, references to standard methods are correct, and that the SOP is in agreement with approved practice and regulatory requirements. pH – Standard Methods, 4500 H+ B-2011 (Aqueous) I. Finding for Immediate Response: The pH meter is not calibrated prior to analysis of samples each day compliance monitoring is performed. Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref: 15A NCAC 02H .0805 (g) (4). Requirement: Instruments are to be calibrated according to the manufacturer’s calibration procedure prior to analysis of samples each day compliance monitoring is performed. Calibration must include at least two buffers. The meter calibration must be verified with a third standard buffer solution (i.e., check buffer) prior to sample analysis. The calibration and check standard buffers must bracket the range of the samples being analyzed. Ref: NC WW/GW LCB Approved Procedure for the Analysis of pH. Comment: During the inspection, staff noted that the pH meter was calibrated weekly, and subsequently verified with a check standard buffer daily prior to sample analysis. The laboratory agreed to immediately initiate daily calibration of the instrument. Documentation of the implementation of the daily calibration and verification with a check standard buffer was submitted on September 27, 2023. No further response is necessary for this Finding. Chlorine, Total Residual – Standard Methods, 4500 Cl G-2011 (Aqueous) J. Finding for Immediate Response: The laboratory is not verifying the instrument’s Factory- set Calibration Curve initially and every 12 months thereafter. Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref: 15A NCAC 02H .0805 (g) (4). Requirement: Annual Factory-set Calibration Curve Verification: This type of calibration curve verification must be performed initially, at least every 12 months and any time the instrument optics are serviced. Zero the instrument with a Calibration Blank and then analyze a Method Blank and a series of five standards (do not use gel or sealed liquid standards for this purpose). 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 μg/L and must not vary by more than ±25% from the known value for standard concentrations less than 50 μg/L. Ref: NC WW/GW LCB Approved Procedure for the Analysis of Total Residual Chlorine (DPD Colorimetric by SM 4500 Cl G-2011). Comment: During the inspection, it was discovered that the laboratory was having the instrument serviced by FCX Services annually but was not verifying the factory pre-set calibration curve with the required 5 standards. The laboratory was informed that verification of the curve, with standards bracketing the permitted discharge limit concentration, the range of sample concentrations to be analyzed and anticipated PT Sample concentrations, was required. A Notice of Finding for Immediate Response was issued on September 14, 2023, with a deadline of October 14, 2023 for the laboratory to have the pre-set calibration curve verified by a contract laboratory. The laboratory submitted documentation of a passing Page 6 #5633 City of King WTP calibration curve verification on October 2, 2023. No further response is necessary for this Finding. K. Finding for Immediate Response: The laboratory is not assigning the gel-type TRC standard concentration a true value initially and every twelve months thereafter. Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref: 15A NCAC 02H .0805 (g) (4). Requirement: Purchased “gel-type” or sealed liquid standards may be used only for daily calibration curve verifications. These standards must have a true value assigned initially and every 12 months thereafter. Ref: NC WW/GW LCB Approved Procedure for the Analysis of Total Residual Chlorine (DPD Colorimetric by SM 4500 Cl G-2011). Comment: During the inspection, it was discovered that the laboratory was using the true value (0.21 mg/L) and acceptance criterion (± 0.09 mg/L) assigned to the gel-type standard by the manufacturer. The laboratory was informed of the requirement and the process for assigning a True Value to the standard. A Notice of Finding for Immediate Response was issued on September 14, 2023, with a deadline of October 14, 2023 for a True Value to be assigned to the gel-type standard by a contract laboratory, while verifying the calibration curve. The laboratory submitted documentation of the new True Value for the gel-type standard on October 2, 2023. No further response is necessary for this Finding. L. Finding: The laboratory is not analyzing a Method Blank when analyzing PT Samples. Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref: 15A NCAC 02H .0805 (g) (4). Requirement: The Method Blank is deionized or distilled water from the same source used to prepare the calibration verification standards or the PT Sample, and is analyzed like a sample (i.e., with DPD/buffer added). The concentration of the Method Blank must not exceed 50% of the reporting limit (i.e., the lowest calibration verification standard concentration) or corrective action must be taken. Method Blanks would be required when using laboratory- prepared standards [including Proficiency Testing (PT) Samples] and anytime sample dilutions are performed. Ref: NC WW/GW LCB Approved Procedure for the Analysis of Total Residual Chlorine (DPD Colorimetric by SM 4500 Cl G-2011). Comment: Current laboratory procedure is to prepare the PT Sample and zero the instrument with a portion of the PT Sample that does not contain DPD/buffer reagents. This is permissible if compliance samples are analyzed in the same manner (i.e., zeroed with a portion of the sample prior to adding DPD/buffer). However, the laboratory must first zero the instrument with the gel-type Blank, then read and record the results of the gel-type Standard and the Method Blank. Reporting Comment: During the inspection, it was discovered that the laboratory was not verifying the factory pre-set calibration curve (see Finding J). An acceptable calibration curve verification was performed on October 2, 2023 by Statesville Analytical Holdings, LLC. The lowest standard concentration analyzed was 15 μg/L, which establishes the lower reporting limit as 15 μg/L. Compliance Sample results less than that must be reported as <15 μg/L on the Discharge Monitoring Report (DMR). Page 7 #5633 City of King WTP M. Finding: The laboratory is not correctly transcribing analytical results from the contract laboratory to the DMR. Requirement: Daily analyses must be performed using EPA-approved methods that are capable of producing results less than or equal to the corresponding permit limits, where such methods exist. In the case of ‘non-detect’ values, permittees (or their laboratories) are expected to report daily values to the Practical Quantitation Level (PQL) for each parameter (or “<[PQL] for values less than the PQL). Ref: Precision in Discharge Monitoring Reports, Section 3.1. Comment: Values below the detection limit, listed as “ND” on the contract laboratory report, were consistently reported as “0” instead of the listed detection limit preceded by the less than (<) symbol. N. 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 monthly report forms. Ref: 15A NCAC 02B .0506 (b) (3) (J). Comment: The laboratory is analyzing Turbidity on the effluent (called “decant” on the laboratory benchsheet) as process control. The laboratory must either choose a different sampling point prior to the effluent or apply for certification for Turbidity. Until that determination is made, all Turbidity results on the effluent must be reported as “uncertified data”. IV. CONCLUSIONS: Correcting the above-cited Findings and implementing the Recommendation 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: September 28, 2023 Report reviewed by: Tonja Springer Date: October 4, 2023 Certificate Number:5633 Effective Date:1/1/2023 Expiration Date:12/31/2023 Lab Name:City of King WTP Address:6949 Donnaha Rd Tobaccoville, NC 27050- North Carolina Wastewater/Groundwater Laboratory Certification Certified Parameters Listing Date of Last Amendment: The above named laboratory, having duly met the requirements of 15A NCAC 2H.0800, is hereby certified for the measurement of the parameters listed below. CERTIFIED PARAMETERS INORGANIC CHLORINE, TOTAL RESIDUAL SM 4500 Cl G-2011 (Aqueous) pH SM 4500 H+B-2011 (Aqueous) This certification requires maintance of an acceptable quality assurance program, use of approved methodology, and satisfactory performance on evaluation samples. Laboratories are subject to civil penalties and/or decertification for infractions as set forth in 15A NCAC 2H.0807.