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HomeMy WebLinkAbout#5586_2023_0719_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 August 30, 2023 5586 Mr. Lee Garner Reed Gold Mine 9621 Reed Mine Road Midland, NC 28107- Subject: North Carolina Wastewater/Groundwater Laboratory Certification Branch (NC WW/GW LCB) Maintenance Inspection Dear Mr. Garner: Enclosed is a report for the inspection performed on July 19, 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, #5586 On-Site Inspection Report LABORATORY NAME: Reed Gold Mine WATER QUALITY PERMIT #: WQ0006946 ADDRESS: 9621 Reed Mine Road Midland, NC 28107 CERTIFICATE #: 5586 DATE OF INSPECTION: July 19, 2023 TYPE OF INSPECTION: Field Maintenance AUDITOR(S): Michael Cumbus LOCAL PERSON(S) CONTACTED: Lee Garner 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. The analyst was forthcoming and responded well to suggestions from the auditor. The facility where data is transcribed to the reporting form is poorly illuminated, which may contribute to transcription errors. All required Proficiency Testing (PT) Samples have been analyzed for the 2023 PT Calendar Year and the graded results were 100% acceptable. 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, based on the Findings, Comments and Recommendations within this report must be submitted to this office by November 30, 2023. Page 2 #5586 Reed Gold Mine 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 K & W Laboratories (Certification #559). Approved Procedure documents for the analysis of the facility’s currently certified Field Parameters were provided at the time of the inspection. III.FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS: Documentation A.Finding: Error corrections are not properly performed. Requirement: All documentation errors shall be corrected by drawing a single line through the error so that the original entry remains legible. Entries shall not be obliterated by erasures or markings. Wite-Out®, correction tape, or similar products designed to obliterate documentation are not to be used; instead the correction shall be written adjacent to the error. The correction shall be initialed by the responsible individual and the date of change documented. Ref: 15A NCAC 02H .0805 (g) (1). B.Finding: The laboratory has not fully developed and implemented 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). Comment: The laboratory SOPs do not specify what is required to meet each training requirement for compliance sample analysis. The following items must be addressed to ensure that current and future employees are able to produce reliable data: •The TRC SOP Section 15.1 says “Include education, training, experience and/or demonstrated skills required for the position” but does not specify what would meet this requirement (e.g., wastewater operator certification, prior laboratory experience, etc.). •The TRC SOP Section 15.3 and the pH SOP Section 15.2 list the options for Demonstration of Proficiency (DOP). The primary option is a PT result graded Acceptable, but also includes alternative options such as an Initial Demonstration of Capability or side by side analysis with an established analyst. The SOP must clearly state which options are in practice, as well as state the acceptance criteria for the alternative DOPs. Page 3 #5586 Reed Gold Mine C.Finding: All original records are not being maintained for five years. Requirement: All analytical records, including original observations and information necessary to facilitate historical reconstruction of the calculated results, shall be maintained for five years. Ref: 15A NCAC 02H .0805 (g) (1). Comment: The testing data is initially written on a piece of paper, transported back to the laboratory, and transferred to an electronic copy of the benchsheet which is then printed. This original paperwork is then discarded. D.Finding: The laboratory is not documenting 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. Comment: Dates received and opened were written on the DPD powder pillow bulk container and pH buffer bottles, 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. E.Finding: The laboratory benchsheet for pH and Total Residual Chlorine (TRC) is lacking required documentation: the date of sample collection. Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data shall be traceable to the associated sample analyses and shall consist of: the date and time of sample collection. 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) (F). Comment: A blanket statement that the dates of collection and analysis are the same would satisfy the requirement. F. Finding: The laboratory benchsheet does not correctly document the acceptance criterion of the TRC Daily Check Standard. Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref: 15A NCAC 02H .0805 (g) (4). Requirement: The value obtained for the Daily Check Standard must read within ±10% of the true value of the Daily Check Standard for standards ≥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). Page 4 #5586 Reed Gold Mine Comment: The TRC Daily Check Standard has an assigned True Value of 0.20 mg/L. The benchsheet lists two acceptance ranges; ±10% of the true value and 0.20 to 0.20 mg/L. However, the correct range is 0.18 to 0.22 mg/L. No data were examined where the Daily Check Standard did not meet the required acceptance criterion. Proficiency Testing Recommendation: The laboratory performs the analysis of PT samples at K & W Laboratories after the annual verifications are performed. K & W provides glassware, pipettes and reagent water. It is recommended that the laboratory add this information to each SOP’s PT section. G.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 each prepared PT Sample would satisfy the documentation requirement. Quality Assurance/Quality Control H.Finding: The laboratory is not evaluating the recovery of the pH Check Standard Buffer to demonstrate the analytical process is in control and the established acceptance criterion is met. Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data shall be traceable to the associated sample analyses and shall consist of: the quality control assessments. Ref: 15A NCAC 02H .0805 (g) (2) (O). Comment: The benchsheet has a footnote that states that the check standard buffer must read within ± 0.1 S.U. of the buffer’s true value, but it lacks an acknowledgement that this requirement has been met. Chlorine, Total Residual – Standard Methods, 4500 Cl G-2011 (Aqueous) I.Finding for Immediate Response: The laboratory failed to perform corrective action when the verification of the TRC meter was outside the recovery acceptance criteria. Requirement: If quality control results fall outside established limits or indicate an analytical problem, the laboratory shall identify the Root Cause of the failure. The problem shall be resolved through corrective action, the corrective action process documented, and any samples involved shall be reanalyzed, if possible. If the sample cannot be reanalyzed, or if the quality control results continue to fall outside established limits or indicate an analytical problem, the results shall be qualified as such. Ref: 15A NCAC 02H .0805 (g) (8). 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 Page 5 #5586 Reed Gold Mine LCB Approved Procedure for the Analysis of Total Residual Chlorine (DPD Colorimetric by SM 4500 Cl G-2011). 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 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: The Hach Pocket Colorimeter II currently in use was sent for the annual factory curve verification on May 25, 2023. The report issued by the contract laboratory notes that the 2.0 mg/L standard had a recovery of 87%, which does not meet the acceptance criterion of ± 10%. A Notice of Finding for Immediate Response (NOFIR) was issued on July 25, 2023. In an email dated July 26, 2023, the laboratory agreed to immediately take the instrument out of service, and put their backup instrument, which has a passing calibration curve verification, into use until the issue is resolved. The laboratory submitted a revised benchsheet on August 21, 2023 with the instrument ID updated to the meter currently in use. No further response is necessary for this Finding. J. Finding: The laboratory is not documenting the results of the Method Blank when using laboratory-prepared standards. 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: Value obtained for the Method Blank, if applicable (verification of ≤ ½ concentration of the lowest calibration curve, or calibration curve verification, standard). Ref: NC WW/GW LCB Approved Procedure for the Analysis of Total Residual Chlorine (DPD Colorimetric by SM 4500 Cl G-2011). Comment: Proficiency Testing samples are included in this requirement. pH – Standard Methods, 4500 H+B-2011 (Aqueous) K.Finding: Values were reported that exceed the method specified accuracy of 0.1 units. Requirement: By careful use of a laboratory pH meter with good electrodes, a precision of ±0.02 unit and an accuracy of ±0.05 unit can be achieved. However, ± 0.1 pH unit represents the limit of accuracy under normal conditions, especially for measurement of water and poorly buffered solutions. For this reason, report pH values to the nearest 0.1 pH unit. Ref: Standard Methods, 4500 H+ B-2011. (6). Comment: Per PT Vendor instructions, the PT Sample results should be reported to two decimal places, which is an exception to the requirement for Compliance Samples. Recommendation: The laboratory currently reports pH sample results to two decimal places. It is recommended that the laboratory continue to measure and document sample results on the benchsheet to two decimal places, and to round to the nearest 0.1 S.U. when reporting results on the Non-Discharge Monitoring Report (NDMR). Reporting L. Finding: The laboratory is producing Uncertified Data without reporting it as such. Page 6 #5586 Reed Gold Mine Requirement: “Uncertified Data" means any analytical result, including the Supporting Records, obtained using a method or procedure that is not acceptable to the State Laboratory pursuant to these Rules; analytical results produced by a laboratory for an analysis not within the scope of the rules of this Section; or analytical results produced by a laboratory without proper Certification. Ref: 15A NCAC 02H .0803 (35). Requirement: All Uncertified Data shall be documented as such on the benchsheet and on the final report. Ref: 15A NCAC 02H .0805 (e) (3). Comment: At the time of the inspection, the laboratory was analyzing Temperature and reporting the results on the NDMR without qualifying the data as Uncertified. Upon review of the permit, it was noted that Temperature is not a required parameter. In an email dated July 24, 2023, staff agreed to immediately cease analyzing and reporting Temperature for the permitted site. No Further Response is necessary for this Finding. M.Finding: Values less than the established reporting limit for TRC are being reported on the NDMR. Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref: 15A NCAC 02H .0805 (g) (4). 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 less than the permitted Daily Maximum 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 LCB Approved Procedure for the Analysis of Total Residual Chlorine (DPD Colorimetric by SM 4500 Cl G- 2011). Comment: The lowest standard concentration used to verify the factory pre-set curve is 0.1 mg/L. Therefore, any value less than this concentration must be reported as < 0.1 mg/L. IV.PAPER TRAIL INVESTIGATION: The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks, etc.) and contract laboratory reports to NDMRs submitted to the North Carolina Division of Water Resources. Data were reviewed for Reed Gold Mine (Water Quality permit # WQ0006946) for January, February, March, April and May 2023. The following errors were noted: Date Parameter Location Value on Benchsheet Value on NDMR 5/2/2023 pH Effluent 6.35 S.U. 6.53 S.U. 4/25/2023 TRC Effluent 0.05 mg/L 0.26 mg/L 3/7/2023 pH Effluent 6.66 S.U. 6.56 S.U. 3/7/2023 TRC Effluent 0.34 mg/L 0.54 mg/L 2/28/2023 pH Effluent 6.7 S.U. 6.71 S.U. 2/14/2023 pH Effluent 7.06 S.U. 7 S.U. 1/11/2023 pH Effluent 6.74 S.U. 6.71 S.U. Page 7 #5586 Reed Gold Mine To avoid questions of legality, it is recommended that you contact the appropriate Regional Office for guidance as to whether amended NDMRs 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 Recommendation(s) 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: July 28, 2023 Report reviewed by: Tom Halvosa Date: August 4, 2023 Certificate Number:5586 Effective Date:1/1/2023 Expiration Date:12/31/2023 Lab Name:Reed Gold Mine Address:9621 Reed Mine Road Midland, NC 28107- 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.