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HomeMy WebLinkAbout#161_2023_1005_JP_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 December 18, 2023 161 Mr. Newlyn McCullen Whiteville WWTP Lab P.O. Box 607 Whiteville, NC 28472 Subject: North Carolina Wastewater/Groundwater Laboratory Certification Branch (NC WW/GW LCB) Maintenance Inspection Dear Mr. McCullen: Enclosed is a report for the inspection performed on October 5, 2023, by Jill Puff. 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. 251. Sincerely, Anna Ostendorff Technical Assistance & Compliance Specialist Division of Water Resources Attachment cc: Todd Crawford, Jill Puff, Master File #161 On-Site Inspection Report LABORATORY NAME: Whiteville WWTP Lab NPDES PERMIT #: NC0021920 ADDRESS: 1000 Nolan Avenue Whiteville, NC 28472 CERTIFICATE #: 161 DATE OF INSPECTION: October 5, 2023 TYPE OF INSPECTION: Municipal Maintenance AUDITOR(S): Jill Puff LOCAL PERSON(S) CONTACTED: Newlyn McCullen, Nathan Guyton, and Brandon Rich 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. All required Proficiency Testing (PT) Samples have been analyzed for the 2023 PT Calendar Year and the graded results were 100% acceptable. The laboratory did not have Quality Assurance (QA) and/or Standard Operating Procedure (SOP) document(s) in place for all currently certified parameters. These documents must be submitted for review as specified in Finding A. Any time changes are made to laboratory procedures, QA and/or 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 no later than December 31, 2024. 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”. Page 2 #161 Whiteville WWTP Lab 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 Waypoint Analytical - Greenville (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: SOPs have not been developed for all of 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: This Finding applies to Temperature. The SOP for this parameter is required to be submitted with the report response. B. Finding: The laboratory does not document SOP revisions. Requirement: 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. Ref: 15A NCAC 02H .0805 (a) (7). C. Finding: The laboratory is lacking documentation of the 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 (a) (7) (P). Comment: The laboratory’s training program is outlined in the laboratory QA manual but no documentation of completed training was available for review. Page 3 #161 Whiteville WWTP Lab D. Finding: Error corrections are not properly performed. Cited previously on March 9, 2011. 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 multiple instances of overwritten entries. E. Finding: The laboratory benchsheet is 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: This Finding applies to Temperature and Dissolved Oxygen (DO) on the Stream Grab Samples benchsheet. F. Finding: The laboratory benchsheet sometimes does not reference the currently approved methods. Requirement: Analytical methods, sample preservation, sample containers, and sample holding times shall conform to the requirements found in: 40 CFR Part 136 and 40 CFR Part 503. Ref: 15A NCAC 02H .0805 (a) (1) (A). 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: Benchsheets for the parameters listed below do not reference the approved method as listed on the laboratory's Certified Parameters Listing (CPL): • Nitrogen, Ammonia – Standard Methods, 4500 NH3 D-2011 (Aqueous) • Bacteria, Fecal Coliform – Standard Methods, 9222 D-2015 (Aqueous) • BOD – Standard Methods, 5210 B-2016 (Aqueous) • Residue, Suspended – Standard Methods, 2540 D-2015 (Aqueous) G. Finding: The laboratory benchsheet is 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. Analyses shall conform to methodologies found in Subparagraph (a)(1) of this Rule. Ref: 15A NCAC 02H .0805 (a) (7) (iii). Comment: This Finding applies to all laboratory benchsheets. H. Finding: The laboratory benchsheets are lacking required documentation: meter calibration time. Cited previously on March 9, 2011. Page 4 #161 Whiteville WWTP Lab 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: Meter calibration and meter calibration time(s). Ref: NC WW/GW LCB Approved Procedure for the Analysis of Dissolved Oxygen (DO) and NC WW/GW LCB Approved Procedure for the Analysis of pH. Comment: This Finding applies to the DO and pH benchsheets. I. Finding: The units of measure are not consistently documented. Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data shall be traceable to the associated sample analyses and shall consist of: the proper units of measure. Each item shall be recorded each time samples are analyzed. Ref: 15A NCAC 02H .0805 (a) (7) (F) (xii). Comment: This Finding applies to the BOD, Fecal Coliform and Stream Grab Samples benchsheets. Comment: This Finding applies to the pH calibration log. Comment: This Finding applies to the Temperature verification log. J. Finding: The DO and BOD laboratory benchsheets are lacking required documentation: the salinity value 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: 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). 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: Follow manufacturer's calibration procedure exactly to obtain guaranteed precision and accuracy. Ref: Standard Methods, 4500 O G-2016. (3) (a). 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: Per NC WW/GW LC Branch policy, facilities may use the Salinity default value of zero when calibrating the DO meter unless it is known or suspected that the Salinity value of the samples being analyzed is > 9 ppt. In those situations, actual Salinity values must be used. Regardless of which value is used, it must be documented. Ref: NC WW/GW LCB Approved Procedure for the Analysis of Dissolved Oxygen (DO). Page 5 #161 Whiteville WWTP Lab K. Finding: The laboratory benchsheet is lacking required documentation: Date of most recent Total Residual Chlorine (TRC) calibration curve 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: The following must be documented in indelible ink whenever sample analysis is performed: Date of most recent calibration curve generation or calibration curve verification. Ref: NC WW/GW LCB Approved Procedure for the Analysis of Total Residual Chlorine (DPD Colorimetric by Hach 10014 ULR). L. Finding: The laboratory does not document all QC assessments. 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. Each item shall be recorded each time that samples are analyzed. Ref: 15A NCAC 02H .0805 (a) (7) (F) (xv). Comment: The true value of QC standards and percent recovery obtained must be documented on the benchsheet and evaluated against established acceptance criteria to demonstrate that the analyst was aware of any out-of-control situation. The corrective actions taken must be documented. Any samples not meeting the acceptance criteria must be reanalyzed, if possible. If this is not possible, the data must be flagged on the laboratory reports as all QC requirements were not met. Comment: This Finding applies to the laboratory benchsheets for pH, TRC and Fecal Coliform Colony Verification. M. Finding: The laboratory is not documenting all variables used in calibrating the mechanical volumetric liquid-dispensing devices used for critical measurements. Requirement: The following shall be documented with each calibration of a mechanical liquid-dispensing device: date performed, analyst performing the test, unique identifier (e.g., serial number, etc.), manufacturer’s specification of accuracy, balance test-weight reading, volumes tested, volume weights observed, reagent water used is at ambient temperature and all calculations used to assess accuracy Ref: NC WW/GW LCB Mechanical Volumetric Liquid-Dispensing Devices Calibration Policy (07/06/2021). Comment: The calibration log for the auto-pipettors does not include the manufacturer’s specification of accuracy, the volumes tested, the units of measure for the volume weights observed, the temperature of the reagent water used, and calculations used to assess accuracy. N. Finding: The laboratory is not documenting the temperature each time samples are placed into and removed from the drying oven. Requirement: The date, time and temperature must be documented each time samples are placed into and removed from a drying oven. Ref: NC WW/GW LCB Residue Oven Temperature Documentation Policy (07/30/2021). O. Finding: The autoclave temperature, pressure and cycle time are not being documented. Requirement: During each use of an autoclave, the temperature, pressure, cycle time, and items autoclaved shall be checked, recorded, dated, and initialed. Ref: 15A NCAC 02H .0805 (a) (7) (I). Page 6 #161 Whiteville WWTP Lab Requirement: After each run cycle, record the items sterilized, sterilization temperature, total run time (heat exposure), programmed/preset sterilization period, actual pressure readings, and analyst initials. Ref: Standard Methods 9020 B-2015. (4) (h). Proficiency Testing P. Finding: PT Samples are not distributed among all analysts 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, January 1, 2023, Revision 6, Section 3.6. Quality Assurance/Quality Control Q. Finding: The laboratory did not have a copy of each approved analytical procedure available. Requirement: Each laboratory shall have a copy of each approved test, analysis, measurement, or monitoring procedure being used in the laboratory. Ref. 15A NCAC 02H .0805 (a) (7). Comment: The 21st Edition of Standard Methods was the most recent one available. Not all of the laboratory’s certified parameter methods are referenced in this edition. R. Finding: Thermometers in the BOD incubator and the water bath are not consistently verified against a Reference Temperature-Measuring Device at least every three months. Requirement: Digital temperature-measuring devices and temperature-measuring devices used in incubators shall be verified at the temperature of use every three months against a Reference Temperature-Measuring Device and their accuracy shall be corrected. Ref: 15A NCAC 02H .0805 (a) (7) (N) (iii). Comment: The thermometers were verified on February 15, April 5, and September 21 of this year. S. Finding: Laboratory temperature-measuring devices are not labeled with their respective correction factors. Requirement: Document any correction that applies (e.g., add 0.2 °C, subtract 0.3 °C, or if no correction needed; 0.0 °C) on both the temperature-measuring device and in a format that can be retained for a minimum of five years. Routine temperature measurements must be documented with any applicable correction factor applied. Ref: NC WW/GW LCB Temperature Measuring-Devices used for Laboratory Operations Policy (08/30/2021). T. Finding: The laboratory is not consistently calibrating the mechanical volumetric liquid- dispensing devices used for critical measurements at least once every six months. Requirement: Mechanical volumetric liquid-dispensing devices (e.g., fixed and adjustable auto-pipettors and bottle-top dispensers) used for critical volume measurements shall be calibrated once every six months. Ref: 15A NCAC 02H .0805 (a) (7) (O). Comment: The most recent calibration of the auto-pipettors was February 15, 2023. Page 7 #161 Whiteville WWTP Lab U. Finding: The desiccant in the desiccator is exhausted. Requirement: Each laboratory requesting Certification shall be maintained so as to ensure the security and integrity of samples. Samples shall be analyzed in such a manner that contamination or error will not be introduced. Ref: 15A NCAC 02H .0805 (a) (6). Requirement: Interferences: See 2540A.2 and B.1b. Ref: Standard Methods, 2540 D- 2015. (1) (b). Requirement: Pay close attention to all samples during post-drying desiccation. Open desiccator as few times as possible to minimize the entry of moist air. If samples are stronger desiccants than the desiccants used in the desiccator, they may take on water. In general, weigh samples as soon as possible after removal from desiccator to minimize water absorption from the atmosphere. Ref: Standard Methods, 2540 A-2015. (2). V. Finding: The laboratory has not established acceptance criteria for the weights used during daily balance calibration. 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). W. Finding: The laboratory has not established a policy for assigning expiration dates for chemical/reagents/consumables that do not have an expiration date. Requirement: When commercially prepared chemicals, reagents, standards and consumables have expiration dates 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. If no expiration date is given by the manufacturer, the laboratory must use their policy for assigning one. If the laboratory is unable to determine an expiration date for a chemical, reagent or standard a one-year time period from the date of receipt shall be the expiration date unless degradation is observed prior to this date. If neither a date received nor an expiration date can be determined, the item must not be used. If the method does not specify an expiration date, chemicals, reagents and standards prepared in the laboratory for use with that method must be assigned an expiration date according to the laboratory’s policy for doing so. Monitor materials for changes in appearance or consistency. Any changes may indicate potential contamination or degradation, and therefore, the item must not be used, even if the manufacturer’s or laboratory’s expiration date has not been exceeded. Laboratory-assigned expiration dates may be re-evaluated based on performance and recovery data and new expiration dates assigned at that time. Manufacturer-assigned expiration dates may not be extended. Ref: NC WW/GW LCB Chemical, Reagent, Standard and Consumables Expiration Date Policy (04/21/2022). Comment: This Finding applies to: • Concentrated Sulfuric Acid • Hach Buffered Dilution Water Pillows used for Fecal Coliform testing X. Finding: Data that does not meet all QC requirements is not qualified on the Discharge Monitoring Report (DMR). Requirement: Reported data associated with quality control failures, improper sample collection, holding time exceedances, or improper preservation shall be qualified as such. Page 8 #161 Whiteville WWTP Lab Ref: 15A NCAC 02H .0805 (e) (5). Comment: The relative percent difference (RPD) for the Fecal Coliform duplicate on June 1, 2023 was greater than 30%. This is outside the QC acceptance limits but it was not qualified on the DMR as required. Chlorine, Total Residual – Hach 10014 (ULR) (Aqueous) Y. Finding: Samples are being filtered without documentation. 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: Statement that samples were filtered. Ref: NC WW/GW LCB Approved Procedure for the Analysis of Total Residual Chlorine (DPD Colorimetric by Hach 10014 (ULR). Bacteria, Fecal Coliform – Standard Methods, 9222 D-2015 (MF) (Aqueous) Z. 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 µmhos/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 LCB Bacteriological Reagent Water Testing Policy (02/15/2018). AA. Finding: The Fecal Coliform incubator bath temperature is not being monitored and recorded twice daily. Requirement: When incubator is in use (i.e., samples are being incubated), monitor and record corrected temperature twice daily separated by 4 h. Ref: Standard Methods, 9020 B-2015. (4) (n). Comment: The laboratory records the temperature once each day of use. BB. Finding: The laboratory is not using an approved technique to sterilize the filtration apparatus. Requirement: Filtration units: See 9222B.1f. Ref: Standard Methods, 9222 D-2015. (1) (f). Requirement: Wrap the assembly (as a whole or separate parts) in heavy wrapping paper or aluminum foil, or place in commercial autoclave bags; sterilize via autoclaving; and store until use. Ref: Standard Methods 9222 B-2015. (1) (f). Page 9 #161 Whiteville WWTP Lab Comment: The laboratory is utilizing an ultraviolet (UV) apparatus for sterilization. Germicidal shortwave UV lights are commonly used to sanitize, not sterilize, such items as membrane filtration units between filtrations. CC. Finding: The UV lamp bulbs are not tested quarterly. Requirement: Test lamps quarterly with an appropriate (short-wave) UV light meter, and replace bulbs when output drops to <70% of initial output. Alternatively, expose spread plates containing 200 to 300 CFU/mL of a selected bacterial suspension for 2 min. Incubate plates at 35°C for 48 h and then count colonies. Replace bulb if colony count is not reduced 99%. It also is advisable to ask the manufacturer for the bulb’s expected life span and then track hourly usage. Ref: Standard Methods, 9020 B-2015. (4) (l) (1). DD. Finding: The UV lamp bulbs are not cleaned monthly. Requirement: When in use, disconnect lamps monthly and clean bulbs with a soft cloth moistened with ethanol (70% ethanol/30% reagent-grade water) or with spectroscopic grade 2-propanol in areas where baked-on material is collecting. Ref: Standard Methods, 9020 B-2015. (4) (l). BOD – Standard Methods, 5210 B-2016 (Aqueous) EE. Finding: The laboratory is not analyzing at least two dilution water blanks. Requirement: With each batch of dilution water, incubate two or more bottles of dilution water containing nutrient, mineral, and buffer solutions but no seed or nitrification inhibitor. Dilution water checks must be analyzed with each batch of samples; the dilution-water blank serves as a check on the quality of unseeded dilution water and cleanliness of incubation bottles. Determine initial and final DO for each bottle (5210B.5e and i), and average results. Ref: Standard Methods, 5210 B-2016. (6) (c). FF. Finding: Extra nutrient, mineral, and buffer solutions are not added to the incubation bottles containing more than 67% (i.e., > 201 mL) sample. Requirement: When a bottle contains >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 (5210B.3a-d) directly to diluted sample at a rate of 1 mL/L (0.30 mL/300-mL bottle), or use commercially-prepared solutions designed to dose the appropriate bottle size. Ref: Standard Methods, 5210 B-2016. (5) (c) (2). Conductivity – Standard Methods, 2510 B-2011 (Aqueous) GG. Finding: The Automatic Temperature Compensator (ATC) was not verified prior to initial use and every 12 months thereafter. 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 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 standard Page 10 #161 Whiteville WWTP Lab 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). Nitrogen, Ammonia – Standard Methods, 4500 NH3 D-2011 (Aqueous) HH. Finding: The laboratory is adding 10N NaOH before immersing the electrode. Requirement: Do not add NaOH solution before immersing electrode, because ammonia may be lost from a basic solution. Ref: Standard Methods 4500 NH3 D-2011 (4) (b). Residue, Suspended – Standard Methods, 2540 D-2015 (Aqueous) Comment: The laboratory evaluates sample duplicates against a 30% acceptance criterion. This criterion was not implemented based on control charts or other performance-based metrics and may be ineffectively broad. Typically, the relative percent difference (RPD) of duplicates should not exceed 10%, but RPDs may vary considerably due to sample matrix and concentration. The laboratory may plot duplicate determinations on a control chart for evaluation. If the laboratory is using %RPD as the acceptance criterion, check low concentration samples for compliance. A separate low-level acceptance criterion may be appropriate based upon calculated recoveries or a ± mg/L criterion. Recommendation: It is recommended that the laboratory document on the Suspended Residue benchsheet that the analytical balance level indicator bubble is inside the circle of accepted range during each use. II. Finding: The drying cycle is not repeated until a weight change of <0.5 mg is achieved. Requirement: Repeat the cycle (drying, cooling, desiccating, and weighing) until the weight change is <0.5 mg. Ref: Standard Methods, 2540 D-2015. (3) (c). Comment: The laboratory was drying and weighing routine compliance samples only once but was conducting an annual drying study. Approval by NC WW/GW LCB for laboratories to conduct an annual drying study in lieu of obtaining constant weight was repealed with the 2021 Methods Update Rule published in 40 CFR 136. JJ. Finding: The laboratory is not analyzing a Method Blank. Requirement: Analyze one method (MB) per batch of 20 samples for each method except settleable solids (2540F). Blank analysis includes all container- and filter-preparation steps and procedures except sample addition. Ref: Standard Methods, 2540 A-2015. (5). Requirement: Using the same containers and glassware normally in contact with samples, put 30 mL of DI water through the sample filter and proceed through the entire analytical process. Acceptance criterion is ≤0.5 mg weight gain. Ref: NC WW/GW LCB Method Blank Analysis Requirement for Suspended, Dissolved and Total Residue Policy (07/19/2021). Comment: The laboratory was analyzing a dry filter blank. Analyzing a dry filter blank was previously permitted in lieu of drying all prepared filters to constant weight before use. This requirement is not in the updated method and the dry blank does not take the place of a method blank. KK. Finding: A Laboratory-Fortified Blank (LFB) is not being analyzed with each batch. Requirement: Include one laboratory-fortified blank (LFB) per batch of 20 samples for all tests except settleable solids (2540F) and total, fixed, and volatile solids in solid and Page 11 #161 Whiteville WWTP Lab semisolid samples (2540G). Plot the percent recoveries on a control chart for laboratory evaluation. Laboratories may purchase known standards or prepare in-house working controls for use. Ref: Standard Methods, 2540 A-2015. (5). LL. Finding: The laboratory is not always analyzing a volume of sample to yield a minimum of 2.5 mg dried residue. Requirement: Choose sample volume to yield between 2.5 and 200 mg dried residue. If volume filtered fails to meet minimum yield, increase sample volume up to 1 L. If filtration takes >10 min to complete, increase filter size or decrease sample volume. Ref: Standard Methods, 2540 D-2015 (3) (b). Comment: The laboratory’s practice is to filter 50 mL of the influent sample. On June 7, 2023, this yielded less than 2.5 mg dried residue. Temperature – Standard Methods, 2550 B-2010 (Aqueous) MM. Finding: The compliance temperature-measuring devices are 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. Comment: The compliance temperature-measuring devices were checked at 5.4° C and 21.5° C on September 20, 2023. On June 27, 2023, the effluent temperature reported on the DMR was 24.8° C. Reporting NN. 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: The laboratory reported the Ammonia Nitrogen results as less than the in-house reporting limit of 1 mg/L (i.e.; < 1 mg/L) rather than the values reported by the contract laboratory, which were below 1 mg/L. The contract laboratory has a reporting limit of 0.01 mg/L. Page 12 #161 Whiteville WWTP Lab IV. CONCLUSIONS: We are concerned with the Findings that were cited previously and not corrected. Laboratory Decertification Ref: 15A NCAC 02H .0807 (a) (1), (13), (14) and (20): 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; or (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 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: Jill Puff Date: October 17, 2023 Report reviewed by: Tom Halvosa Date: October 24, 2023 Certificate Number:161 Effective Date:1/1/2023 Expiration Date:12/31/2023 Lab Name:Whiteville WWTP Lab Address:1000 Nolan Avenue Whiteville, NC 28472 North Carolina Wastewater/Groundwater Laboratory Certification Certified Parameters Listing Date of Last Amendment:7/19/2021 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 SM 9222 D-2015 (MF) (Aqueous) BOD SM 5210 B-2016 (Aqueous) CHLORINE, TOTAL RESIDUAL Hach 10014 ULR (Aqueous) CONDUCTIVITY SM 2510 B-2011 (Aqueous) DISSOLVED OXYGEN Hach 10360-2011, Rev. 1.2 (Aqueous) SM 4500 O G-2016 (Aqueous) NITROGEN, AMMONIA SM 4500 NH3 D-2011 (Aqueous) pH SM 4500 H+B-2011 (Aqueous) RESIDUE, SUSPENDED SM 2540 D-2015 (Aqueous) TEMPERATURE SM 2550 B-2010 (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.