Loading...
HomeMy WebLinkAbout#646_2023_0126_TLH_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 March 27, 2023 646 Mr. Benjamin Overton Johnnie Mosley Water Reclamation Lab 2101 Becton Farm Road Kinston, NC 28502 Subject: North Carolina Wastewater/Groundwater Laboratory Certification Branch (NC WW/GW LCB) Maintenance Inspection Dear Mr. Overton: Enclosed is a report for the inspection performed on January 26, 2023 by Tom Halvosa and Beth Swanson. 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: Tom Halvosa, Todd Crawford, #646 On-Site Inspection Report LABORATORY NAME: Johnnie Mosley Water Reclamation Lab NPDES PERMIT #: NC0024236 WATER QUALITY PERMIT #: WQ0029289 ADDRESS: 2101 Becton Farm Road Kinston, NC 28502 CERTIFICATE #: 646 DATE OF INSPECTION: January 26, 2023 TYPE OF INSPECTION: Municipal Maintenance AUDITOR(S): Tom Halvosa and Beth Swanson LOCAL PERSON(S) CONTACTED: James Elmore and Swindell Flowers I. INTRODUCTION: This laboratory was inspected by representatives 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 facility has all the equipment necessary to perform the analyses. All required Proficiency Testing (PT) Samples for the 2023 PT Calendar Year have not yet been analyzed. The laboratory is reminded that results must be received by this office directly from the vendor by September 30, 2023. Any time changes are made to laboratory procedures, QA/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/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. Revisions to the SOPs, based on the Findings, Comments and Recommendations within this report must be submitted to this office by February 29, 2024. Page 2 # 646 Johnnie Mosley Water Reclamation Lab 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”. 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. Contracted analyses are performed by Environment 1, Inc. (Certification # 10). Approved Procedure documents for the analysis of the facility’s currently certified Field Parameters were provided at the time of the inspection. III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS: Documentation A. Finding: Error corrections are not always 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 shall 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 (a) (7) (E). Comment: There were several instances of incorrect error corrections such as write overs and no date of change or initials of the responsible individual B. Finding: The Ammonia, Conductivity, pH, Total Phosphorus and Temperature laboratory benchsheets are lacking required documentation: the method or Standard Operating Procedure reference. 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. Each item shall be recorded each time samples are analyzed. Ref: 15A NCAC 02H .0805 (a) (7) (F) (i). Comment: The Ammonia, Conductivity, pH and Temperature benchsheets lack the entire method reference and the Total Phosphorus benchsheet lacks the method revision year. C. Finding: The Ammonia, Conductivity, Dissolved Oxygen (DO), Total Phosphorus, pH and Temperature laboratory benchsheets are lacking required documentation: the instrument identification. Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data shall be traceable to the associated sample analyses and shall consist of: the instrument identification. Each item shall be recorded each time samples are analyzed. Ref: 15A NCAC 02H .0805 (a) (7) (F) (iii). D. Finding: The laboratory is not consistently documenting the time of sample collection for Conductivity samples. Page 3 # 646 Johnnie Mosley Water Reclamation Lab 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. Ref: 15A NCAC 02H .0805 (a) (7) (F) (vi). Comment: On December 21, 2022 the laboratory did not record the time of sample collection on the benchsheet. E. Finding: Only one time for sample collection and analysis is documented on the DO and Temperature benchsheets without noting samples are analyzed in situ. Cited previously on September 15, 2009. Requirement: The State Laboratory may develop Approved Procedures for Field Parameters based upon the methods in any of the sources referenced in Parts(a)(1)(A) through (F) of this Rule. Ref: 15A NCAC 02H .0805 (a) (1) (F). Requirement: The following must be documented in indelible ink whenever sample analysis is performed: Date and time of sample collection; Date and time of sample analysis. Alternatively, one time may be documented for collection and analysis with the notation that samples are measured in situ or immediately at the sampling site (i.e., immediately following collection at a location as near to the collection point as possible). When this 'one time' option is used, state that the documented time is both collection and analysis time. Ref: NC WW/GW LCB Approved Procedure for the Analysis of Temperature. Requirement: Date and time of sample analysis must be documented to verify the 15-minute holding time is being met. Alternatively, one time may be documented for collection and analysis with the notation that samples are measured in situ or immediately at the sampling site. Ref: NC WW/GW LCB Approved Procedure for the Analysis of Dissolved Oxygen. F. Finding: The BOD laboratory benchsheet is lacking required documentation: meter calibration time. Requirement: Determination of Initial DO: Use the Azide modification of the iodometric method (Section 4500-O.C), membrane-electrode method (Section 4500-O.G), or optical- probe method (Section 4500-O.H) to determine initial DO on all sample dilutions, dilution water blanks, and, where appropriate, seed controls. Ref: Standard Methods, 5210 B-2016. (5) (g). Requirement: Calibrate probe in accordance with manufacturer's instructions to obtain the guaranteed precision and accuracy. Ref: Standard Methods, 4500 O H-2016. (4). 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 (a) (7) (E). Comment: The benchsheet labeled "Kinston Regional WRF BOD Benchsheet" is missing the DO meter calibration times (day one and day five). Comment: The method procedures are meant to be followed sequentially and therefore documentation needs to indicate the meter calibration was performed prior to sample analysis. G. Finding: The BOD, Fecal Coliform and Suspended Residue laboratory benchsheets are lacking required documentation: date of sample collection and units of measure. Page 4 # 646 Johnnie Mosley Water Reclamation Lab Requirement: The laboratory benchsheet is lacking required documentation: the date and time of sample collection and the proper units of measure. Each item shall be recorded each time that samples are analyzed. The date and time that samples are placed into and removed from ovens, water baths, incubators and other equipment shall be documented if a time limit is required by the method. Ref: 15A NCAC 02H .0805 (a) (7) (F) (vi) and (xii). Comment: On the Fecal Coliform benchsheet, the temperature in and out of the incubator is lacking units. On the Total Suspended Residue benchsheet, the units for temperature are missing in several places. Comment: The benchsheet labeled "Kinston Regional WRF BOD Benchsheet" is missing the sample collection date. H. Finding: The BOD and DO laboratory benchsheets are lacking required documentation: barometric pressure and salinity used for meter calibration. Requirement: The State Laboratory may develop Approved Procedures for Field Parameters based upon the methods in any of the sources referenced in Parts(a)(1)(A) through (F) of this Rule. Ref: 15A NCAC 02H .0805 (a) (1) (F). Requirement: The following must be documented in indelible ink whenever sample analysis is performed: Calibration variables (temperature, elevation or barometric pressure [in mmHg], and salinity). Ref: NC WW/GW LCB Approved Procedure for the Analysis of Dissolved Oxygen (DO). Requirement: Determination of Initial DO: Use the Azide modification of the iodometric method (Section 4500-O.C), membrane-electrode method (Section 4500-O.G), or optical- probe method (Section 4500-O.H) to determine initial DO on all sample dilutions, dilution water blanks, and, where appropriate, seed controls. Ref: Standard Methods, 5210 B-2016. (5) (g). Requirement: Calibrate probe in accordance with manufacturer's instructions to obtain the guaranteed precision and accuracy. Ref: Standard Methods, 4500 O H-2016. (4). 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 (a) (7) (E). Comment: After the inspection the laboratory was provided with instructions on how to display the barometric pressure on their Hach HQ30D meter. Comment: A note on both benchsheets indicating that the salinity of the samples are ≤ 9 ppt would be sufficient. I. Finding: The Total Phosphorus laboratory benchsheet is lacking required documentation: the volume of sample analyzed. Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data shall be traceable to the associated sample analyses and shall consist of: the volume of sample analyzed, where applicable. Each item shall be recorded each time that samples are analyzed. Ref: 15A NCAC 02H .0805 (a) (7) (F) (xi). Comment: The laboratory has a column labeled “Volume of Sample, mL” on their benchsheet but was not documenting the sample volume. Page 5 # 646 Johnnie Mosley Water Reclamation Lab J. Finding: The Percent Total Solids benchsheet for the VAR Option 4 Parameter Method is lacking required documentation: the signature or initials of the analyst and the time that samples are placed into and removed from the oven. Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data shall be traceable to the associated sample analyses and shall consist of: the signature or initials of the analyst. Each item shall be recorded each time that samples are analyzed. The date and time that samples are placed into and removed from ovens, water baths, incubators and other equipment shall be documented if a time limit is required by the method. Ref: 15A NCAC 02H .0805 (a) (7) (F) (v). Requirement: Evaporate to dryness on a water bath, on a hot plate or block, or in a drying oven, then dry the evaporated sample at 103–105°C for ≥1 h, cool to ambient temperature in a desiccator and weigh. Ref: Standard Methods, 2540 G-2014. (3.)(a.)(2)(a). Comment: The laboratory does not record the time the sample is placed in or taken out of the drying oven in order to demonstrate compliance with the minimum one-hour requirement. K. Finding: Chemical containers are not consistently dated when opened. Requirement: Chemical containers shall be dated when received and when opened. Ref: 15A NCAC 02H .0805 (a) (7) (K). Comment: The Ammonia ISA solution bottle lacked a date opened. L. 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 (a) (7) (E). Comment: The laboratory reported a DO result on their DMR for May 21, 2022, and there was no supporting documentation of this result. The laboratory is cautioned that this could appear to outside parties as data falsification. M. Finding: The laboratory does not have documented traceability of the Suspended Residue filters. 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. Page 6 # 646 Johnnie Mosley Water Reclamation Lab N. Finding: The laboratory is not documenting all quality control assessments for Total Phosphorus and Suspended Residue. Requirement: Certified Data shall be traceable to the associated sample analyses and shall consist of: all quality control assessments. Ref: 15A NCAC 02H .0805 (a) (7) (F) (xv). Comment: The accuracy of the LFB and MS/MSD recovery and the precision of the duplicates are calculated and documented on the Total Phosphorus benchsheet. However, there are no acceptance criteria listed for the Laboratory Fortified Blanks (LFB) and MS/MSD on the benchsheet to assess whether they meet the established QC requirements. Comment: The Total Suspended Residue benchsheet does not have the acceptance criterion for the method blank listed, nor a place to indicate that it meets the criterion. The benchsheet lacks documentation that shows the analyst is aware whether the constant weight requirement has been met. The analyst calculates and documents the duplicate RPD on the benchsheet, but there is no acceptance criterion listed on the benchsheet or any documentation acknowledging whether the values are within the acceptable range. Recommendation: It is recommended that the laboratory use a separate low-level acceptance criterion for the Total Suspended Residue effluent sample duplicates that may be based upon calculated recoveries or a ±mg/L criterion. O. Finding: The laboratory is lacking a sufficiently documented training program. Requirement: Each laboratory shall develop and implement a documented training program that includes documentation that: staff have the education, training, experience, or demonstrated skills needed to generate quality control results within method-specified limits and meet the requirements of these Rules; staff have read the laboratory quality assurance manual and applicable Standard Operating Procedures; and 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 method). Ref: 15A NCAC 02H .0805 (a) (7) (P). Comment: The existing training requirements in Section 4 of the laboratory’s Quality Assurance Plan are inadequate. The QA manual must document how the analyst will be required to demonstrate proficiency for each certified method. Also, in Section 4.1.2 and 4.2.1, the word “should” needs to be changed to “must”. Proficiency Testing P. 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. Page 7 # 646 Johnnie Mosley Water Reclamation Lab Q. Finding: The laboratory does not have 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). 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. Requirement: SOPs must address situations where the instructions from the Accredited PT Provider for the preparation, analysis or result calculations would constitute a deviation from the laboratory’s routine procedure. Examples of this may include how low-level PT Samples will be analyzed, including concentration of the sample or adjustment of the normality of a titrant. These instructions shall be followed when the concentration of a PT Sample is below the range of their routine analytical method. Instructions shall also be included in the laboratory’s SOP for how high-level PT Samples will be analyzed, including preparation of multiple dilutions of the sample. These instructions will be followed when the concentration of a PT Sample is above the range of their routine analytical method. Ref: Proficiency Testing Requirements, January 1, 2023, Revision 6, Section 3.0. Quality Assurance/Quality Control R. Finding: Precision of QC results are not consistently evaluated and/or documented to demonstrate the analytical process is in control and the established acceptance criteria are met. Requirement: Unless specified by the method or this Rule, each laboratory shall establish performance acceptance criteria for all quality control analyses. Each laboratory shall calculate and document the precision and accuracy of all quality control analyses with each sample set. When the method of choice specifies performance acceptance criteria for precision and accuracy, and the laboratory chooses to develop laboratory-specific limits, the laboratory-specific limits shall not be less stringent than the criteria stated in the approved method. Ref: 15A NCAC 02H .0805 (a) (7) (A). Comment: When analyzing Fecal Coliform, the analyst writes down the low and high value of the 95% confidence limit from the IDEXX MPN generator, for the sample and duplicate, but does not understand how to evaluate whether they meet the acceptance criterion from that point. The process was explained to the analyst on the day of the inspection. When looking at the sample and duplicate ranges, they are acceptable as long as those 2 ranges overlap. Page 8 # 646 Johnnie Mosley Water Reclamation Lab Comment: The BOD SOP states that the acceptance criterion for duplicates is 25% Relative Percent Difference (RPD), however, the duplicate RPD is not calculated nor is there an acceptance criterion listed on the benchsheet. Recommendation: For BOD analysis, the laboratory only duplicates the effluent sample which rarely has a value above the reporting limit. It is recommended that the influent be used as a duplicate since the values will be high enough to adequately assess precision and generate useful evaluations of the duplication process. Conductivity – Standard Methods, 2510 B-2011 (Aqueous) S. Finding: The Automatic Temperature Compensator (ATC) check is not being performed. Requirement: The State Laboratory may develop Approved Procedures for Field Parameters based upon the methods in any of the sources referenced in Parts(a)(1)(A) through (F) of this Rule. Ref: 15A NCAC 02H .0805 (a) (1) (F). Requirement: The 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 (see #3 below). The manner in which the ATC is verified may depend upon the meter’s capabilities and the manufacturer’s instructions. The following is one option. 1. Pour an adequate amount of conductivity standard or sample into a beaker or other container and analyze at 25°C. Document the temperature and conductivity value. 2. Lower the temperature of the standard or sample (e.g., by placing the container in a refrigerator or ice chest) to less than the lowest anticipated sample temperature and analyze. Document the temperature and conductivity value. 3. If samples greater than 25°C are to be analyzed, perform the following additional step: Raise the temperature above 25°C to greater than the highest anticipated sample temperature (e.g., by placing the container in a hot water bath) and analyze. Document the temperature and conductivity value. As the temperature increases or decreases, the value of the conductivity 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 LCB Approved Procedure for the Analysis of Specific Conductance (Conductivity). Dissolved Oxygen – Standard Methods, 4500 O G-2016 (Aqueous) T. Finding: When analyses are performed at multiple sample sites, the laboratory is not calibrating prior to sample analysis at each sample site or performing a Post-Analysis Calibration Verification. Requirement: The State Laboratory may develop Approved Procedures for Field Parameters based upon the methods in any of the sources referenced in Parts(a)(1)(A) through (F) of this Rule. Ref: 15A NCAC 02H .0805 (a) (1) (F). Requirement: When performing analyses at multiple sample sites, the meter must be calibrated at each sample site prior to analysis or a post-analysis calibration verification must be performed at the end of the run, regardless of meter type. The calculated theoretical DO value must verify the meter reading within ±0.5 mg/L. If the meter verification does not read Page 9 # 646 Johnnie Mosley Water Reclamation Lab within ±0.5 mg/L of the theoretical DO, corrective action must be taken. If the meter is not calibrated at each sample site, it is recommended that a mid-day calibration be performed when samples are extended over an extended period of time. Ref: NC WW/GW LCB Approved Procedure for the Analysis of Dissolved Oxygen (DO). Comment: The laboratory calibrates the meter in the lab then measures the DO at multiple process control locations before analyzing the effluent sample. Recommendation: It is recommended that the laboratory analyze the effluent sample immediately after calibration in the lab then measure the process control locations. If samples are analyzed in this order, recalibration or a post-analysis verification would not be required. U. Finding: The laboratory is not certified for the DO method currently in use. Requirement: Commercial Laboratories shall obtain Certification for Field Parameter Methods used to generate data that will be reported by the client to the State in accordance with the rules of this Section. Municipal and Industrial laboratories shall obtain Certification for Field Parameter Methods used to generate data that will be reported to the State in accordance with the rules of this Section. Ref: 15A NCAC 02H .0804 (a). Comment: On the day of the inspection the laboratory was certified for DO by Standard Methods, 4500 O G-2016 (Aqueous), however, they were using a Luminescent Dissolved Oxygen (LDO) meter and should have been certified for Standard Methods, 4500 O H-2016 (Aqueous). After the inspection, the laboratory submitted an Amendment Form requesting a Parameter Method Substitution to the LDO method. This was finalized on February 3, 2023. pH – Standard Methods, 4500 H+ B-2011 (Aqueous) V. Finding: The acceptance criterion for the check standard buffer is not being assessed. Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data shall be traceable to the associated sample analyses and shall consist of: all quality control assessments. Ref: 15A NCAC 02H .0805 (a) (7) (F) (xv). Comment: The laboratory analyzes a check buffer after calibration which they call “Buffer 7 (measure mode)”, however, the results are not being assessed against the acceptance criterion of ± 0.1 S.U. There were no instances observed where the acceptance criterion was not met. W. 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 DMR. Page 10 # 646 Johnnie Mosley Water Reclamation Lab Temperature – Standard Methods, 2550 B-2010 (Aqueous) X. Finding: The compliance temperature-measuring device is not checked at two temperatures that bracket the range of observed sample temperatures. Requirement: The State Laboratory may develop Approved Procedures for Field Parameters based upon the methods in any of the sources referenced in Parts(a)(1)(A) through (F) of this Rule. Ref: 15A NCAC 02H .0805 (a) (1) (F). Requirement: To check a compliance temperature-measuring device, compare readings at two temperatures that bracket the range of compliance samples routinely analyzed against a Reference Temperature-Measuring Device and record all four readings. The readings from both devices must agree within 0.5ºC. If they do not, the device may not be used for temperature compliance monitoring. Ref: NC WW/GW LCB Approved Procedure for the Analysis of Temperature. Bacteria - Coliform Fecal – IDEXX Colilert ® 18 (MPN) (Aqueous) Y. Finding: The comparator in use is expired. Requirement: Chemical containers shall be dated when received and when opened. Reagent containers shall be dated, identified and initialed when prepared. Chemicals and reagents exceeding the expiration date shall not be used. The laboratory shall have a documented system of traceability for the purchase, preparation and use of all chemicals, reagents, standards and consumables. Ref: 15A NCAC 02H .0805 (a) (7) (K). Comment: The expiration date of the comparator was November 2022. BOD – Standard Methods, 5210 B-2016 (Aqueous) Comment: The laboratory qualifies data when the calculated seed correction factor is outside the range of 0.6 - 1.0 mg/L. This is not a requirement of the method and can be discontinued. Comment: The analyst compares the mg/L reading obtained after calibration to the DO solubility table to determine if the values are within ±0.2 mg/L of each other, which is not required. Z. Finding: The analyst does not properly evaluate the drift check. 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 (i.e., a group of samples analyzed without interruption) reanalyze the drift check bottle and document the concentration (day one final drift check). If the meter drifts more than 0.2 mg/L, recalibrate the meter and reanalyze all samples since the last acceptable drift check. If additional samples are analyzed later the same day, begin the set with a drift check and compare to the initial drift check value. If the drift check fails, recalibrate prior to starting the additional sample set and begin new drift checks for that set. Repeat process on Day 5. Ref: NC WW/GW LCB BOD5/CBOD5 - DO Meter Drift Check Policy. Comment: The analyst compares ongoing drift check values to the previous drift check value, not to the drift check value obtained immediately after calibration. During the data review process, it was discovered that the final drift check value for samples set up on Page 11 # 646 Johnnie Mosley Water Reclamation Lab November 23, 2022 had drifted >0.2 mg/L from the initial check. The meter was not recalibrated, nor were sample bottles reanalyzed. AA. Finding: The initial DO of the water used for BOD analysis is not always at least 7.5 mg/L. Requirement: Check to ensure that the DO concentration is at least 7.5 mg/L before using water for BOD tests. If not, add DO by shaking bottle or aerating it with organic-free filtered air. Alternatively, store the water in cotton-plugged bottles long enough for the DO concentration to approach saturation. Ref: Standard Methods, 5210 B-2016. (5) (a). BB. Finding: Calculated results of sample dilutions are not being evaluated to ensure < 30% difference between high and low values. Requirement: Identify results in the test reports when any of the following QC conditions occur: test replicates show >30% difference between highest and lowest values. Ref: Standard Methods, 5210 B-2016. (7) (b). Comment: Evaluating the difference between high and low dilutions can illuminate a problem with toxic substances or analytical problems. Toxicity should only be claimed after thorough investigation. CC. Finding: Documentation does not demonstrate that the initial DO for BOD analysis is measured within 30 minutes of sample preparation. This is considered pertinent data. Requirement: All analytical records, including original observations and information necessary to facilitate historical reconstruction of the calculated results, shall be maintained for five years. All analytical data and records pertinent to each certified analysis shall be available for inspection upon request. Ref: 15A NCAC 02H .0805 (a) (7) (E). Requirement: After preparing dilution, measure initial DO within 30 min. Ref: Standard Methods, 5210 B-2016. (5) (g). Total Phosphorus – Standard Methods, 4500 P E-2011 (Aqueous) Comment: The benchsheet has a column for “Absorbance Reading”. However, the values listed there are actually the concentration of total phosphate in mg/L. Nitrogen, Ammonia – Standard Methods, 4500 NH3 D-2011 (Aqueous) Total Phosphorus – Standard Methods, 4500 P E-2011 (Aqueous) DD. Finding: The laboratory is not back calculating the concentration of the calibration standards analyzed during the annual calibration curve and comparing them against acceptance criteria. Requirement: Compare each calibration point to the curve and recalculate its concentration. If any recalculated values are not within the method’s acceptance criteria—up to twice the MRL ± 50%; between 3 and 5 times the MRL ± 20%; or greater than 5 times the MRL ± 10%— unless otherwise specified in individual methods, identify the source of any outlier(s) and correct before sample quantitation. Ref: Standard Methods, 4020 B-2014. (1) (b). Comment: For the laboratory’s current curve; the acceptance criteria would be ± 50% for the 0.25 and 0.50 mg/L calibration standards, ± 20% for the 1.0 mg/L calibration standard and ± 10% for the 1.5 and 2.0 mg/L calibration standards. Page 12 # 646 Johnnie Mosley Water Reclamation Lab Comment: The MRL is defined as the Method Reporting Limit and usually corresponds to the lowest calibration standard value. EE. Finding: The laboratory is not analyzing the results of a standard at the same concentration as the laboratory's lowest reporting concentration every day samples are analyzed. Requirement: With each analytical batch, analyze a reagent-water sample spiked at the MRL and ensure that it meets MRL acceptance criteria (generally ±50%). If not, re-analyze the entire batch or flag results for all samples in the batch. If the MRL is biased high, non-detect (ND) samples can be reported with flags if the method or regulation allows. Ref: Standard Methods, 4020 B-2014. (9). Residue, Total Suspended – Standard Methods, 2540 D-2015 (Aqueous) FF. Finding: Filters are not prepared prior to sample analysis. Requirement: Insert filter with wrinkled side up in filtration apparatus. Apply vacuum and wash disk with three successive portions of ≥20 mL reagent-grade water. Continue suction to remove all traces of water. Remove filter from filtration apparatus and transfer to an inert weighing dish. If a Gooch crucible is used, remove crucible and filter combination. Dry in a 103-105°C oven for ≥ 1 h. Cool in desiccator to ambient temperature and weigh. Store filters (on inert dishes or pans) in desiccator or 103-105°C oven until needed. Adequate filter preparation is demonstrated by negligible weight loss or gain for method blanks. Ref: Standard Methods, 2540 D-2015. (3) (a). GG. Finding: The laboratory is not evaluating the LFB recovery. Requirement: Plot the percent recoveries on a control chart for laboratory evaluation. Ref: Standard Methods, 2540 A-2015. (5). Requirement: Calculate percent recovery, plot control charts, and determine control limits (Section 1020B.13) for these measurements to demonstrate ongoing capability. Ref: Standard Methods, 2020 B-2017. (2) (e). Requirement: Unless specified by the method or this Rule, each laboratory shall establish performance acceptance criteria for all quality control analyses. Each laboratory shall calculate and document the precision and accuracy of all quality control analyses with each sample set. When the method of choice specifies performance acceptance criteria for precision and accuracy, and the laboratory chooses to develop laboratory-specific limits, the laboratory-specific limits shall not be less stringent than the criteria stated in the approved method. Ref: 15A NCAC 02H .0805 (a) (7) (A). Comment: A chart with LFB recoveries is prepared at the end of each month, however, the LFB recovery is not evaluated against the control limits determined from that chart during the subsequent month. HH. Finding: The laboratory is not analyzing 5% of samples in duplicate each day analyses are performed. Requirement: Analyze ≥5% of all samples in duplicate or at least one duplicate sample with each batch of ≤20 samples. Ref: Standard Methods, 2540 A-2015. (5). Page 13 # 646 Johnnie Mosley Water Reclamation Lab Comment: The laboratory analyzes the influent and effluent in duplicate on the same day, one day per week. However, suspended residue analysis is performed multiple times per week. II. Finding: The laboratory has not set acceptance criteria for daily and monthly balance weight checks. Requirement: Unless specified by the method or this Rule, each laboratory shall establish performance acceptance criteria for all quality control analyses. Ref: 15A NCAC 02H .0805 (a) (7) (A). Comment: It is recommended that the laboratory use the acceptance criteria in the NC WW/GW LCB Verification of Analytical Balance Weights Policy. Vector Attraction Reduction – Option 4: Specific Oxygen Uptake Rate Recommendation: It is recommended that the sample bottle not be more than half full upon collection to provide oxygen for respiration of the microorganisms in the sewage sludge and ensure initial DO > 2mg/L. Standard Methods 2710 B-2011 3.d.3) states "Low DO (≤ 2 mg/L at the start of the test) may limit oxygen uptake by the biological suspension and will be indicated by a decreasing rate of oxygen consumption as the test progresses. Reject such data as being unrepresentative of suspension oxygen consumption rate and repeat test beginning with higher initial DO levels." JJ. Finding: The laboratory is not repeating the sample drying cycle until the weight change is less than 50 mg when determining total solids. Requirement: Total solids concentration is determined by Standard Method 2540 G. Ref: Control of Pathogens and Vector Attraction in Sewage Sludge, EPA/625/R-92/013, July 2003, Appendix D (2). Requirement: Repeat cycle (drying, cooling, desiccating, and weighing) until weight change <50 mg. Ref: Standard Methods, 2540 G-2015. (3) (a) (2) (b). KK. Finding: The laboratory does not analyze a duplicate sample for Percent Total Solids. Requirement: Analyze ≥5% of all samples in duplicate or at least one duplicate sample with each batch of ≤20 samples. The laboratory may plot duplicate determinations on a control chart for evaluation. Typically, the relative percent difference (RPD) of duplicates should not exceed 10%, but RPDs may vary considerably due to sample matrix and concentration. Ref: Standard Methods, 2540 A-2015 (5). Reporting LL. Finding: The laboratory does not report results of all tests on the characteristics of the effluent when duplicate sample analyses are performed. 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 analyzes duplicates for Conductivity, Fecal Coliform, pH and Suspended Residue but does not report the duplicate results or, if applicable, the average results on their DMR. Page 14 # 646 Johnnie Mosley Water Reclamation Lab Comment: The laboratory was advised that duplicates are not required for Field Parameters. IV. PAPER TRAIL INVESTIGATION: The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks, etc.) and contract laboratory reports to DMRs submitted to the North Carolina Division of Water Resources. Data were reviewed for Johnnie Mosley Water Reclamation Lab (NPDES permit # NC0024236) for January, May and November 2022. The following errors were noted: Date Parameter Location Value on Benchsheet Value on DMR 5/10/2022 Suspended Residue Influent 76 mg/L 41 mg/L* 5/21/2022 Dissolved Oxygen Effluent No Value 8.56 mg/L * This was the value obtained for the PT sample To avoid questions of legality, it is recommended that you contact the appropriate Regional Office for guidance as to whether an amended DMR(s) will be required. A copy of this report will be made available to the Regional Office. V. CONCLUSIONS: We are concerned with the Finding that was cited previously and not corrected. Laboratory Decertification Ref: 15A NCAC 02H .0807 (a) (1), (13) and (14): A laboratory may be decertified for any or all parameters for up to one year for any or all of the following infractions: (1) Failing to maintain the facilities, or records, personnel, equipment, or quality control program as set forth in these Rules; or (13) Failing to respond to requests for information by the date due; or (14) Failing to comply with any other terms, conditions, or requirements of this Section or of Laboratory certification. (20) Failing to correct findings in an inspection report. 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 its 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: Tom Halvosa Date: February 7, 2023 Report reviewed by: Jason Smith Date: February 10, 2023 Certificate Number:646 Effective Date:1/1/2023 Expiration Date:12/31/2023 Lab Name:Johnnie Mosley Water Reclamation Lab Address:2101 Becton Farm Road Kinston, NC 28502 North Carolina Wastewater/Groundwater Laboratory Certification Certified Parameters Listing Date of Last Amendment:10/28/2021 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 BACTERIA - COLIFORM FECAL IDEXX Colilert ®18 (MPN) (Aqueous) BOD SM 5210 B-2016 (Aqueous) CONDUCTIVITY SM 2510 B-2011 (Aqueous) DISSOLVED OXYGEN SM 4500 O G-2016 (Aqueous) NITROGEN, AMMONIA SM 4500 NH3 D-2011 (Aqueous) pH SM 4500 H+B-2011 (Aqueous) PHOSPHORUS, TOTAL SM 4500 P E-2011 (Aqueous) RESIDUE, SUSPENDED SM 2540 D-2015 (Aqueous) TEMPERATURE SM 2550 B-2010 (Aqueous) VECTOR ATTRACTION REDUCTION: OPTION 4 Specific Oxygen Uptake Rate 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.