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HomeMy WebLinkAbout#143_2017_1207_JS_FINALTo be attached to all inspection reports in-house only. Laboratory Cert. #: 143 Laboratory Name: City of Newton Clark Creek WW Facility Inspection Type: Municipal Maintenance Inspector Name(s): Jason Smith and Todd Crawford Inspection Date: December 7, 2017 Date Forwarded for Initial Review: January 3, 2018 Initial Review by: Anna Ostendorff Date Initial Review Completed: January 5, 2018 Cover Letter to use: ❑ Insp. Initial ❑Insp. No Finding ❑Corrected ❑ Insp. Reg ❑Insp. CP ®Insp. Reg. Delay Unit Supervisor/Chemist III: Todd Crawford Date Received: January 9, 2018 Date Forwarded to Admin.: February 14, 2018 Date Mailed: February 15, 2018 Special Mailing Instructions: Email to wes.bell@ncdenr.gov (/Vats=r Resour ces f N V I R G N M F N 1 A L Q U A, L'Ty February 15, 2018 143 Mr. Eric Jones City of Newton Clark Creek WW Facility P.O. Box 550 Newton, NC 28658 ROY COOPER MICHEAL S. REGAN LINDA CULPEPPER Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) Maintenance Inspection Dear Mr. Jones: Enclosed is a report for the inspection performed on December 7, 2017 by Jason Smith. I apologize for the delay in getting this report to you. Where Finding(s) are cited in this report, a response is required. Within thirty days of receipt, please supply this office with a written item for item description of how these Finding(s) were corrected. Please describe the steps taken to prevent recurrence and include an implementation date for each corrective action. If the Finding(s) cited in the enclosed report are not corrected, enforcement actions may be recommended. For Certification maintenance, your laboratory must continue to carry out the requirements set forth in 15A NCAC 2H .0800. A copy of the laboratory's Certified Parameter List at the time of the audit is attached. This list will reflect any changes made during the audit. Copies of the checklists completed during the inspection may be requested from this office. Thank you for your cooperation during the inspection. If you wish to obtain an electronic copy of this report by email or if you have questions or need additional information, please contact me at (919) 733-3908 ext. 251. Sincerely, Todd Crawford Technical Assistance & Compliance Specialist NC WW/GW Laboratory Certification Branch Attachment cc: Dana Satterwhite, Jason Smith, Master File #143 Water Sciences Section NC Wastewater/Groundwater Laboratory Certification Branch 1623 Mail Service Center, Raleigh, North'Carohna 27699-1623 Location: 4405 Reedy Creek Road, Raleigh, North Carolina 27607 Phone: 919-733-39081 FAX: 919-733-6241 Internet: http://deg.nc,goviaboutldivisions/water-resources/water-resources-data/water-sciences-home-pagetlaboratory-certification branch On -Site Inspection Report LABORATORY NAME: NPDES PERMIT #: ADDRESS: CERTIFICATE #: DATE OF INSPECTION: TYPE OF INSPECTION: AUDITOR(S): LOCAL PERSON(S) CONTACTED INTRODUCTION: City of Newton Clark Creek WW Facility NC0036196 1407 McKay Farm Road Newton, NC 28658 143 December 7, 2017 Municipal Maintenance Jason Smith and Todd Crawford Eric Jones, Stacy Rowe, Scott Bryan, Carmella Tucker and Matt Herman This laboratory was inspected by representatives of the North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) program to verify its compliance with the requirements of 15A NCAC 2H .0800 for the analysis of compliance monitoring samples. II. GENERAL COMMENTS: The laboratory is clean, spacious and contains all equipment necessary to perform the analyses. The analysts were forthcoming and expressed interest in the inspection process. All required Proficiency Testing (PT) Samples have been analyzed and the laboratory has fulfilled its PT requirements for the 2017 PT Calendar Year. The laboratory submitted their Quality Assurance (QA) and/or Standard Operating Procedures (SOP) document(s) in advance of the inspection. These documents were reviewed and editorial and substantive revision requirements and recommendations were made by this program outside of this formal report process. Although subsequent revisions were not requested to be submitted, they must be completed by December 31, 2018. The laboratory is reminded that any time changes are made to laboratory procedures, the laboratory must update the QA/SOP document(s) and inform relevant staff. Any changes made in response to the pre -audit review or to Findings, Recommendations or Comments listed in this report must be incorporated to insure the method is being performed as stated, references to methods are accurate, and the QA and/or SOP document(s) is in agreement with each approved practice, test, analysis, measurement, monitoring procedure or regulatory requirement being used in the laboratory. In some instances, the laboratory may need to create an SOP to document how new functions or policies will be implemented. The laboratory is also reminded that SOPs are intended to describe procedures exactly as they are to be performed. Use of the word "should" is not appropriate when describing requirements (e.g., Quality Control (QC) frequency, acceptance criteria, etc.). Evaluate all SOPs for the proper use of the word "should". Page 2 #143 City of Newton Clark Creek WW Facility Laboratory Fortified Matrix (LFM) and Laboratory Fortified Matrix Duplicate (LFMD) are also known as Matrix Spike (MS) and Matrix Spike Duplicate (MSD) and may be used interchangeably in this report. Requirements that reference 15A NCAC 2H .0805 (a) (7) (A), stating "All analytical data pertinent to each certified analysis must be filed in an orderly manner so as to be readily available for inspection upon request", are intended to be a requirement to document information pertinent to reconstructing final results and demonstrating method compliance. Use of this requirement is not intended to imply that existing records are not adequately maintained unless the Finding speaks directly to that. Contracted analyses are performed by Meritech (Certification # 165). Approved Procedure documents for the analysis of the facility's currently certified Field Parameters were provided at the time of the inspection. III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS: General Laboratory A. Finding: The analytical balance weights have not been verified against ASTM standard weights in the past 5 years. Requirement: ASTM Class 1 and 2 weights must be verified at least every 5 years. ASTM Class 1 weights (20 g to 25 kg) and ASTM Class 2 weights (10 g to 1 mg) are equivalent to the NBS Class S weights specified in 15A NCAC 2H .0805 (a) (7) (K). Ref: NC WW/GW LC Policy. See the attached Weight Verification policy for additional guidance. B. Finding: The National Institute of Standards and Technology (NIST) traceable thermometer used to check laboratory thermometers is not documented to be accurate to 0.1 °C. Requirement: Temperature measuring devices used in fecal coliform incubators, or NIST traceable temperature measuring devices used to calibrate fecal coliform incubator temperature measuring devices, must have a stated accuracy of at least ± 0.1 °C. Ref: NC WW/GW LC Policy. Comment: The policy referenced above was based on consultation with NIST and was implemented after the inspection took place. Comment: The NIST traceable thermometer had a stated accuracy of ± 0.4 °C and was 0.2 °C away from the manufacturer tested temperatures. The thermometer must be accurate to at least ± 0.1 °C due to the acceptable incubation temperature being 44.5 ± 0.2 °C. C. Finding: The laboratory is not checking all thermometers with a NIST certified or traceable thermometer annually. Requirement: All thermometers must meet NIST specifications for accuracy or be checked, at a minimum annually, against a NIST traceable thermometer and proper corrections made. Ref: 15 NCAC 2H .0805 (a) (7) (0). Page 3 #143 City of Newton Clark Creek WW Facility Requirement: All thermometers and temperature measuring devices must be checked every 12 months against a NIST certified or NIST traceable thermometer and the process documented. Ref: NC WW/GW LC Policy. Comment: The thermometer for the drying oven has not been checked since 2015 because the NIST traceable thermometer the laboratory purchased would not fit in the drying oven. All other thermometers and meters have been checked annually. Comment: If unable to find a thermometer that fits in the drying oven, the laboratory may put both thermometers in sand and heat it on a hot plate to the appropriate temperature if both are partial immersion thermometers. Proficiency Testing D. Finding: The laboratory does not have a documented plan for PT procedures. Requirement: Each laboratory shall develop and maintain a document outlining the analytical quality control practices used for the parameters included in their certification. Supporting records shall be maintained as evidence that these practices are being effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7). Requirement: Laboratories must have a documented plan (this is usually detailed in the laboratory's Quality Assurance Manual or may be a separate Standard Operating Procedure (SOP) of how they intend to cover the applicable program requirements for Proficiency Testing per their scope of accreditation. This plan shall cover any commercially available PT Samples and any inter -laboratory organized studies, as applicable. The laboratory must also be able to explain when PT Sample analysis is not possible for certain methods and provide a description of what the laboratory is doing in lieu of Proficiency Testing. This shall be detailed in the plan. The plan must also address the laboratory's process for submission of PT results and related Corrective Action Reports (CARs). Ref: Proficiency Testing Requirements, May 31, 2017, Revision 2.0. 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 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 falls below the range of their routine analytical method. Instructions shall also be included in the laboratory's SOP for how high-level samples will be analyzed, including preparation of multiple dilutions of the sample. These instructions will be followed when the concentration of a PT falls above the range of their routine analytical method. Ref: Proficiency Testing Requirements, May 31, 2017, Revision 2.0. E. Finding: The laboratory is not documenting the preparation of PT Samples, Requirement: PT Samples received as ampules are diluted according to the Accredited PT Sample Provider's instructions. It is important to remember to document the preparation of PT Samples in a traceable log or other traceable format. The diluted PT Sample then becomes a routine Compliance Sample and is added to a routine sample batch for analysis. No documentation is needed for whole volume PT Samples which require no preparation (e.g., pH), but it is recommended that the instructions be maintained. Ref: Proficiency Testing Requirements, May 31, 2017, Revision 2.0. Page 4 #143 City of Newton Clark Creek WW Facility Comment: Dating and initialing the instruction sheet for each prepared PT Sample would satisfy the documentation requirement. F. Finding: PT Samples are not logged in using the sample tracking (sample receipt) system that is used for Compliance Samples. Requirement: Laboratories shall conduct the analyses in accordance with their routine testing, calibration and reporting procedures, unless otherwise specified in the instructions supplied by the Accredited PT Sample Provider. This means that they are to be logged in and analyzed using the same staff, sample tracking systems, standard operating procedures including the same equipment, reagents, calibration techniques, analytical methods, preparatory techniques (e.g., digestions, distillations and extractions) and the same quality control acceptance criteria. Ref: Proficiency Testing Requirements, May 31, 2017, Revision 2.0. Documentation Comment: A method reference was not documented on the benchsheets for Dissolved Oxygen (DO), pH, Temperature, Total Residual Chlorine (TRC) and Conductivity. Although not required at the time of the inspection, this is now required. Please review all benchsheets to ensure that this requirement is met. Recommendation: The laboratory documents the manufacturer and model of the meters in use on the benchsheet. It is recommended that the serial number also be documented in order to more specifically identify the meter in use. G. Finding: Error corrections are not always properly performed. Requirement: All documentation errors must 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. Write the correction adjacent to the error. The correction must be initialed by the responsible individual and the date of change documented. All data and log entries must be written in indelible ink. Pencil entries are not acceptable. Ref: INC WW/GW LC Policy. Comment: Some instances of overwriting and omitting the date of the correction were noted. H. Finding: The date opened (in use) of purchased reagents is not consistently documented. Requirement: All chemicals, reagents, standards and consumables used by the laboratory. must have the following information documented: Date received, Date Opened (in use), Vendor, Lot Number, and Expiration Date (where specified). A system (e.g., traceable identifiers) must be in place that links standard/reagent preparation information to analytical batches in which the solutions are used. Documentation of solution preparation must include the analyst's initials, date of preparation, the volume or weight of standard(s) used, the solvent and final volume of the solution. This information as well as the vendor and/or manufacturer, lot number, and expiration date must be retained for primary standards, chemicals, reagents, and materials used for a period of five years. Consumable materials such as pH buffers, lots of pre -made standards and/or Page 5 #143 City of Newton Clark Creek WW Facility media, solids and bacteria filters, etc. are included in this requirement. Ref: NC WW/GW LC Policy. Requirement: Supporting records shall be maintained as evidence that these practices are being effectively carried out. All analytical records must be available for a period of five years. Ref: 15A NCAC 2H .0805 (a) (7) and (a) (7) (G). Comment: The laboratory has an adequate reagent preparation log; however, one instance of a new lot being put into use without updating the log was noted. The laboratory began using a new lot of Dextrose on September 14, 2017 as indicated on the container, but the reagent preparation log indicated that the old lot was still in use at the time of the inspection. I. Finding: The laboratory benchsheets for DO, pH, TRC, Temperature and Conductivity were lacking pertinent data: facility name. Requirement: The following must be documented in indelible ink whenever sample analysis is performed: Sample site including facility name and location, ID, etc. Ref: NC WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen, NC WW/GW LC Approved Procedure for the Analysis of pH, NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine, NC WW/GW LC Approved Procedure for the Analysis of Temperature and NC WW/GW LC Approved Procedure for the Analysis of Specific Conductance (Conductivity). J. Finding: The DO meter calibration documentation does not include all applicable information. Requirement: Calibration documentation must include the following, where applicable to the instrument used and the type of calibration performed: elevation, temperature, barometric pressure (in mmHg), salinity. Ref: NC WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen, K. Finding: The time of analysis is not documented when pH is analyzed for Vector Attraction Reduction, Option 6: Addition of Alkali. This is considered pertinent data. Requirement: Sewage sludge is considered to have undergone adequate vector attraction reduction if sufficient alkali is added to: • Raise the pH to at least 12 • Maintain a pH of at least 12 without addition of more alkali for 2 hours • Maintain a pH of at least 11.5 without addition of more alkali for an additional 22 hours Ref: Control of Pathogens and Vector Attraction in Sewage Sludge, EPA/625/R-92/013, July 2003, Section 8.7. Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as to be readily available for inspection upon request. Ref: 15 NCAC 2H .0805 (a) (7) (A). L. Finding: The BOD documentation does not demonstrate that the initial DO is measured within 30 minutes of sample preparation. This is considered pertinent data. Requirement: After preparing dilution, measure initial DO within 30 min. Ref: Standard Methods, 5210 B-2001. (5) (g). Page 6 #143 City of Newton Clark Creek WW Facility Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as to be readily available for inspection upon request. Ref: 15 NCAC 2H .0805 (a) (7) (A). M. Finding: The laboratory benchsheet for the analysis of the quarterly Suspended Residue standard was lacking pertinent data: value from the measurement system (i.e., units of measure). Requirement: All laboratories must use printed laboratory bench worksheets that include a space to enter the signature or initials of the analyst, date of analyses, sample identification, volume of sample analyzed, value from the measurement system, factor and final value to be reported and each item must be recorded each time samples are analyzed. The date and time BOD and coliform samples are removed from the incubator must be included on the laboratory worksheet. Ref: 15A NCAC 2H .0805 (a) (7) (H). Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as to be readily available for inspection upon request. Ref: 15A NCAC 21-1.0805 (a) (7) (A). N. Finding: The time coliform samples are removed from the incubator is not consistently documented. Requirement: The date and time BOD and coliform samples are removed from the incubator must be included on the laboratory worksheet. Ref: 15A NCAC 2H .0805 (a) (7) (H) Comment: This was noted for samples removed from the incubator on June 19, 2017. O. Finding: The time sample filtration begins for Fecal Coliform is not recorded on the benchsheet to show that no more than 30 minutes has passed before filters are placed into the incubator. This is considered pertinent data. Requirement: Place all prepared cultures in the water bath within 30 min after filtration. Ref: Standard Methods, 9222 D-1997. (2) (d). Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as to be readily available for inspection upon request. Ref: 15 NCAC 2H .0805 (a) (7) (A). Bacteria — Coliform Fecal — Standard Methods, 9222 D-1997 (MF) (Aqueous) Recommendation: The acceptance criteria for duplicates is set at ± 3 for 0-5 colonies, ± 10 for 6- 19 colonies and ± 15 for 20 or more colonies. It is recommended that the acceptance criteria be made more stringent. For example, ± 5 for 0-20 colonies and ± 15% Relative Percent Difference (RPD) for 20 or more colonies could be established or the acceptance could be based on the standard deviation for the different count ranges of actual duplicate sample results over time. Recommendation: It is recommended that the laboratory refer to the "spike" as a "positive control sample" in order to avoid confusion with Matrix Spike analyses used for other parameters. P. Finding: The laboratory is not monitoring the quality of the reagent water used in fecal coliform analysis. Page 7 #143 City of Newton Clark Creek WVV Facility Requirement: At a minimum, reagent water used to prepare buffered dilution/rinse water or media must be analyzed at least every twelve months for the following parameters: Specific Conductance, Total Organic Carbon, Cadmium, Chromium, Copper, Nickel, Lead, and Zinc. Maximum Acceptable Limits are: Total Organic Carbon < 1.0 mg/L Specific Conductance < 2 pmhos/cm Heavy Metals, single element < 0.05 mg/L Heavy Metals, Total of cited elements < 0.10 mg/L If the facility is using vendor purchased dilution/rinse water this testing is not required as long as the Certificate of Analysis from the manufacturer meets these requirements and is kept on file. Ref: NC WW/GW LC Policy. Q. Finding: The Fecal Coliform incubator temperature is not being monitored and recorded twice daily. Requirement: When incubator is in use, monitor and record calibration -corrected temperature twice daily. Ref: Standard Methods, 9020 B- 2005 (4) (n). Comment: The incubator temperature is checked and recorded once per day. R. Finding: Heat -indicating tape is not used each sterilizing cycle. Requirement: Use heat -indicating tape to identify supplies and materials that have been sterilized. Ref: Standard Methods 9020 B-2005. (4) (h). Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A). Comment: This is considered pertinent data and documentation must be maintained. S. Finding: Plate comparison counts are not being performed. Requirement: For routine performance evaluation, repeat counts on one or more positive samples at least monthly, record results, and compare the counts with those of other analysts testing the same samples. Replicate counts for the same analyst should agree within 5% (within analyst repeatability of counting) and those between analysts should agree within 10% (between analysts reproducibility of counting). If they do not agree, initiate investigation and any necessary corrective action. Ref: Standard Methods, 9020 13- 2005. (9) (a). Comment: The primary analyst must recount one plate monthly and compare the two values and any auxiliary analysts will count the same plate twice comparing the two values and compare the values with the main analyst. If any comparisons do not agree with the established criteria, retraining may be necessary. All counts must be documented. Page 8 #143 City of Newton Clark Creek WW Facility BOD —Standard Methods, 5210 B-2001 (Aqueous) T. Finding: The laboratory does not prepare Sodium Sulfite daily. Requirement: Sodium sulfite solution: This solution is not stable; prepare daily. Ref: Standard Methods, 5210 B-2001. (3) (f). Comment: The laboratory prepares the Sodium Sulfite weekly. U. Finding: Samples used for duplicate analysis are not randomly selected. Requirement: When appropriate (Table 5020:1), randomly select routine samples to be analyzed twice. Ref: Standard Methods, 5020 B-2010. (2) (f). Comment: The laboratory always duplicates the influent sample based on recommendations made by NC WW/GW LC staff in previous inspections performed prior to this being required. COD — Hach 8000 (Aqueous) Recommendation: It is recommended that the column on the benchsheet labeled "Date" be clarified to "Collection Date". Recommendation: It is recommended that the laboratory analyze a method blank, which includes preservatives used in samples, with each sample group. V. Finding: The laboratory is not analyzing an LFM. Requirement: Unless the referenced method states a greater frequency, spike 5% of samples on a monthly basis. Laboratories analyzing less than 20 samples per month must analyze at least one matrix spike (MS) each month samples are analyzed. If MS results are out of control, the results must be qualified or the laboratory must take corrective action to rectify the effect, use another method, or employ the method of standard additions. When the method of choice specifies MS performance acceptance criteria for accuracy, and the laboratory chooses to develop statistically valid, laboratory -specific limits, the laboratory -generated limits cannot be less stringent than the criteria stated in the approved method. Ref: NC WW/GW LC Policy. Comment: See the NC WW/GW LC Matrix Spiking Policy and Technical Assistance document at the end of this report. Recommendation: It is recommended that the laboratory analyze a LFMD instead of a sample duplicate to ensure measurable concentrations for assessing precision. W. Finding: The calibration verification standard is not mid -range. Requirement: The calibration blank and calibration verification standard (mid -range) must be analyzed initially (i.e., prior to sample analysis), after every tenth sample and at the end of each sample group to check for carry over and calibration drift. If either fall outside established quality control acceptance criteria, corrective action must be taken (e.g., repeating sample determinations since the last acceptable calibration verification, repeating the initial calibration, etc.). Ref: NC WW/GW LC Policy. Page 9 #143 City of Newton Clark Creek WW Facility Conductivity — Standard Methods, 2510 B-1997 (Aqueous) X. Finding: The calibration verification standards are prepared by diluting the 1412 pS standard. Requirement: Potassium Chloride (KCI) Conductivity standards may be purchased in the ranges desired, or they may be prepared according to Table 2510:1 of Standard Methods 2510 A-1997. Ref: NC WW/GW LC Approved Procedure for the Analysis of Specific Conductance (Conductivity). Comment: The preparation of the standards in Table 2510:1 indicates that the relationship between mass of KCI used and standard concentration is not linear; therefore, standards may not be diluted, but must be prepared individually. Y. Finding: The Automatic Temperature Compensator (ATC) check has not been verified every 12 months. 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 LC Approved Procedure for the Analysis of Specific Conductance (Conductivity). Nitrogen, Ammonia — Standard Methods, 4500 NH3 D-1997 (Aqueous) Comment: The laboratory reanalyzes the calibration standards after calibration. This is not required. Z. Finding: Samples are not warmed to room temperature prior to analysis. Requirement: Maintain the same stirring rate and a temperature of about 25 °C throughout calibration and testing procedures. Ref: Standard Methods, 4500 NH3 D-1997. (4) (b). Page 10 #143 City of Newton Clark Creek VWV Facility AA. Finding: The larger volume of 10N NaOH used in the samples versus the calibration standards was not compensated for in the calculation. Requirement: The following formula must be used in the calculation: mg NH3 —N/L=AxBX 100+D (100 + C) A = Dilution Factor B = Concentration of NH3-N/L, mg/L, from calibration curve C = Volume of 10N NaOH added to the calibration standards, mL D = Volume of 10N NaOH added to sample, mL Ref: Standard Methods, 4500 NH3 D-1997. (5). 13I3. Finding: A calibration blank is not analyzed after every ten samples. Requirement: The calibration blank and calibration verification standard (mid -range) must be analyzed initially (i.e., prior to sample analysis), after every tenth sample and at the end of each sample group to check for carry over and calibration drift. If either fall outside established quality control acceptance criteria, corrective action must be taken (e.g., repeating sample determinations since the last acceptable calibration verification, repeating the initial calibration, etc.). Ref: NC WW/GW LC Policy. CC. Finding: A calibration verification standard (mid -range) is not analyzed after every tenth sample and at the end of each sample group. Requirement: The calibration blank and calibration verification standard (mid -range) must be analyzed initially (i.e., prior to sample analysis), after every tenth sample and at the end of each sample group to check for carry over and calibration drift. If either fall outside established quality control acceptance criteria, corrective action must be taken (e.g., repeating sample determinations since the last acceptable calibration verification, repeating the initial calibration, etc.). Ref: NC WW/GW LC Policy. DD. Finding: The laboratory is not analyzing a Method Blank. Requirement: Method blank (MB): Include at least one MB daily or with each batch of 20 or fewer samples, whichever is more frequent. Ref: Standard Methods, 4020 B-2011. (2) (d). Requirement: A reagent blank (method blank) consists of reagent water (see section 1080) and all reagents (including preservatives) that normally are in contact with a sample during the entire analytical procedure. The reagent blank is used to determine whether, and how much, reagents and the preparative analytical steps contribute to measurement uncertainty. Ref: Standard Methods, 1020 B-2011. (5). Recommendation: It is recommended that the acceptance criterion (s'/z the reporting limit) be added to the benchsheet. EE. Finding: A laboratory -fortified blank (LFB) is not analyzed. Requirement: Include at least one LFB daily or per each batch of 20 or fewer samples. Ref: Standard Methods, 4020 B-2011. (2) (e). Page 11 #143 City of Newton Clark Creek WW Facility Requirement: A laboratory -fortified blank [laboratory control standard (LCS)] is a reagent water sample (with associated preservatives) to which a known concentration of the analyte(s) of interest has been added. An LFB is used to evaluate laboratory performance and analyte recovery in a blank matrix. Ref: Standard Methods, 1020 B-2011. (6). FF. Finding: The laboratory is not analyzing an LFM/LFMD. Requirement: When appropriate for the analyte (Table 4020:1), include at least one LFM/LFMD daily or with each batch of 20 or fewer samples. To prepare an LFM, add a known concentration of analytes (ideally from a second source) to a randomly selected routine sample without increasing its volume by more than 5%. Ref: Standard Methods, 4020 B-2011, Table 4020:1 and (2) (g). Residue, Suspended — Standard Methods, 2540 D-1997 (Aqueous) Comment: The laboratory analyzes a blank using reagent water. This is not required. Residue, Total — Standard Methods, 2540 B-1997 (Aqueous) Comment: The laboratory does not analyze compliance samples using this method, but maintains certification voluntarily. Chlorine, Total Residual — Standard Methods, 4500 Cl G-2000 (Aqueous) GG. Finding: The laboratory is not verifying the instrument's factory -set curve every 12 months. Requirement: Zero the instrument with chlorine -free water and then analyze a reagent blank (i.e., reagent water plus buffer and DPD) and a series of five standards. The curve verification must bracket the range of the samples to be analyzed. This type of curve verification must be performed at least every 12 months. The values obtained must not vary by more than 10% of the known value for standard concentrations greater than or equal to 50 pg/L and must not vary by more than 25% of the known value for standard concentrations less than 50 pg/L. The reagent blank concentration must not exceed half the concentration of the lowest standard. The overall correlation coefficient of the curve must be >_0.995. Ref: NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine. Please submit a curve verification with the report reply. Comment: The last curve verification available during the inspection was performed on January 8, 2016. The laboratory supervisor thought that a previous analyst performed the curve verification in 2017 prior to his retirement, but could not find documentation of this. Recommendation: The previous curves have been prepared by plotting the absorbance and true values and evaluated based upon the correlation coefficient. It is recommended that the laboratory follow the verification procedure in the Approved Procedure (Option 1), which evaluates the curve based on the true and observed values in pg/L. Recommendation: It is recommended that the laboratory verify the curve at the following concentrations: 25, a concentration between 25 and 50, 50, 200 and 400 pg/L in order to ensure PT and Compliance Sample values are bracketed by calibration standards. Page 12 #143 City of Newton Clark Creek WW Facility HH. Finding: The laboratory is not analyzing a reagent blank. Requirement: A reagent blank (sometimes also referred to as a method blank) is only required when laboratory water is used to make quality control and/or calibration standards. If you are using a sealed standard (e.g., gel) for your daily check standard, a reagent blank would only be analyzed when preparing the annual 5-point calibration curve or 5 annual calibration curve verification standards. Ref: NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine. Comment: A reagent blank is made from the same laboratory water source used to make QC and/or calibration standards with DPD. The concentration of reagent blanks must not exceed 50% of the reporting limit (i.e., the lowest calibration or calibration verification standard concentration), unless otherwise specified by the reference method, or corrective action must be taken. Comment: Analysis of a reagent blank is only required when standards are prepared (e.g., when performing the calibration curve verification and when PT Samples are analyzed). Comment: A reagent blank is made from the same laboratory water source used to make QC and/or calibration standards with DPD. The concentration of reagent blanks must not exceed 50% of the reporting limit (i.e., the lowest calibration or calibration verification standard concentration), unless otherwise specified by the reference method, or corrective action must be taken. Dissolved Oxygen — Standard Methods, 4500 O G-2001 (Aqueous) Dissolved Oxygen — Hach 10360-2011, Rev. 1.2 (LDO) (Aqueous) pH — Standard Methods, 4500 H+ B-2001 (Aqueous) II. Finding: The laboratory is not performing a post -analysis calibration verification when analyses are performed away from the certified laboratory's primary location. Requirement: When performing analyses away from the certified laboratory's primary location, a post -analysis calibration verification must be analyzed at the end of the run. It is recommended that a mid -day calibration verification be performed when samples are analyzed over an extended period of time. The calculated DO value must verify the meter reading within ±0.5 mg/L. If the meter verification does not read within ±0.5 mg/L of the theoretical DO, corrective action must be taken. Ref: NC WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen. Requirement: When performing analyses away from the certified laboratory's primary location, a post -analysis calibration verification using the check standard buffer must be analyzed at the end of the run. It is recommended that a mid -day check standard buffer be analyzed when samples are analyzed over an extended period of time. The post -analysis check standard buffer(s) must read within ±0.1 S.0 or corrective actions must be taken. Ref: NC WW/GW LC Approved Procedure for the Analysis of pH. Comment: Alternatively, the meters may be recalibrated at each sample site prior to analysis. Page 13 #143 City of Newton Clark Creek WW Facility IV. PAPER TRAIL INVESTIGATION: The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks, etc.) and contract lab reports to eDMRs submitted to the North Carolina Division of Water Resources. Data were reviewed for the City of Newton Clark Creek WW Facility (NPDES permit # NC0036196) for January, March, May and June 2017. The following error was noted: Date Parameter Location Value on Value on DMR Benchsheet 3/27/2017 BOD Effluent 6.6 mg/L <2 mg/L To avoid questions of legality, it is recommended that you contact the appropriate Regional Office for guidance as to whether an amended eDMR will be required. A copy of this report will be made available to the Regional Office. V. CONCLUSIONS: Correcting the above -cited Findings and implementing the Recommendations will help this laboratory to produce quality data and meet Certification requirements. The inspector would like to thank the staff for their assistance during the inspection and data review process. Please respond to all Findings and include supporting documentation, implementation dates and steps taken to prevent recurrence for each corrective action. Report prepared by: Jason Smith Date: January 3, 2018 Report reviewed by: Anna Ostendorff Date: January 5, 2018 Weight Verification (NC WW/GW LC Policy 05/23/2008) ASTM Class 1 and 2 weights must be verified at least every 5 years. ASTM Class 1 weights (20 g to 25 kg) and ASTM Class 2 weights (10 g to 1 mg) are equivalent to the NBS Class S weights specified in 15A NCAC 2H .0805 (a) (7) (K). Verification may be accomplished by: Sending laboratory weights back to the manufacturer for recertification - reference weights shall be calibrated by a body that can provide traceability to ASTM specifications, or 2. Checking laboratory weights against certified reference weights (i.e., weights that have been recertified as above) and found to be within ASTM Class 1 or Class 2 tolerances (see table below) - often the balance service technician may provide this service. Note: Although some manufacturers will assign a one-year calibration due date, 5 years is considered an acceptable calibration interval due to the limited use of the reference weight set. Documentation of weight verifications or recertification must be maintained for 5 years. If the condition of a weight(s) is in question at any time due to damage (e.g., corrosion, nicks, scratching, etc.), the laboratory must have that weight(s) re -verified as described above. Maximum tolerances (Ref. ASTM E 617-97, 2003) Denomination Maximum tolerance for ASTM Class 1 and 2 weights, (± mg) 500 g 1.2 300 g 0.75 200 g 0.50 100 g 0.25 50 g 0.12 30 g 0.074 20 g 0.074 10 g 0.074 5 g 0.054 3 g 0.054 2 g 0.054 1 g 0.054 500 mg 0.025 300 mg 0.025 200 mg 0.025 100 mg 0.025 50 mg 0.014 30 mg 0.014 20 mg 0.014 10 mg 0.014 5 mg 0.014 3 mg 0.014 2 mg 0.014 1 mg 0.014 North Carolina Wastewater/Groundwater Laboratory Certification Matrix Spiking Policy and Technical Assistance (05/1112012) Policy Statement Unless the referenced method states a greater frequency, spike 5% of samples on a monthly basis. Laboratories analyzing less than 20 samples per month must analyze at least one matrix spike (MS) each month samples are analyzed. If MS results are out of control, the results must be qualified or the laboratory must take corrective action to rectify the effect, use another method, or employ the method of standard additions. When the method of choice specifies MS performance acceptance criteria for accuracy, and the laboratory chooses to develop statistically valid, laboratory -specific limits, the laboratory -generated limits cannot be less stringent than the criteria stated in the approved method. When spiking with multi -component standards, if the method does not specify the spiking components, the Laboratory Control Spike (LCS) and MS must contain all analytes that are reported. If the unspiked sample result is in the top 40% of the calibration range, the sample should be diluted and the MS prepared using the diluted sample. The recovery of the MS samples must be bracketed by the calibration range. The volume of spike solution used in MS preparation must in all cases be <_ 10% of the total MS volume. It is preferable that the spike solution constitutes s 1 % of the total MS volume so that the MS can be considered a whole volume sample with no adjustment (i.e., volume correction) by calculation necessary. If the spike solution volume constitutes >1% of the total sample volume, the sample concentration or spike concentration must be adjusted by calculation. Technical Assistance Spike Preparation The spike concentration may be set at either 5 to 50 times the Method Detection Limit (as determined by the Method Detection Limit or MDL study) for the analyte, or at 1 to 10 times the ambient level (average concentration) of the analyte in samples. There are several options for preparing spikes, for example: Option 1 (Recommended - easiest) - If the spike solution volume is equal to 1 % or less of the total sample volume, direct subtraction of the unspiked sample is allowed. When the volume of the standard solution spiked into a sample or a sample extract is less than 1 % of the total volume then the final concentration need not be adjusted (e.g., 10 pL of spike solution added to a 1 mL final extract results in only a negligible 1 % change in the final extract volume). Option 2 - Adjust spike solution to a known volume with sample. In this case the sample concentration must be adjusted. When the volume of spike solution exceeds 1 % of the total MS volume the sample concentration must be adjusted prior to determining spike recovery. The general equation for spike recovery is as follows: % R = amt. of target in spiked sample — amt. of target in unspiked sample (conc. or mass) (conc. or mass) x 100 amt. of target spiked into the sample (conc. or mass) To apply this to the sample preparation schemes described above, refer to the following examples. Spike Preparation Examples Option 1 - If the spike solution volume is equal to 1 % or less of the total sample volume, direct subtraction of the unspiked sample is allowed. Option 1 Example: 0.5 mis of a 1000 mg/L standard spike added to 100 mis of sample has a theoretical value of 5 mg/L. (A) The spiked sample recovery is 5.1 mg/L (B) If the unspiked sample result is 0.5 mg/L (C) Theoretical value is 5.0 mg/L The Percent Recovery = spiked sample recovery (A) — unspiked sample result (B) divided by theoretical value (C) X 100 or 5.1 — 0.5 X 100 = 92% recovery 5.0 A — B X 100 = Percent recovery C Option 2 - Adjust spike solution to a known volume with sample. In this case the sample concentration must be adjusted. Option 2 Example 1: 10 mis of spike (concentration 50 mg/L) brought to 100 mis with sample the theoretical MS value is 5 mg/L. (A) The spiked sample recovery is 5.1 (B) If the unspiked sample result is 0.5 mg/L (C) % sample is 0.90 (sample volume used (90) divided by final volume (100)) (D) Theoretical value is 5.0 mg/L The Percent Recovery = spiked sample recovery (A) — (unspiked sample result (B) x % sample (C)) divided by theoretical value (D) X 100 or 5.1 — (0.5 x 0.9) X 100 = 93% recovery A— (B x C) X 100 = Percent recovery 5.0 D Option 2 Example 2: Larger spike volume 25 mis of spike (concentration 50 mg/L) brought to 250 mis with sample the theoretical MS value is 5 mg/L. (A) The spiked sample recovery is 5.6 (B) If the unspiked sample result is 0.5 mg/L (C) % sample is 0.90 (sample volume used (225) divided by final volume (250)) (D) Theoretical value is 5.0 mg/L The Percent Recovery = spiked sample recovery (A) — (unspiked sample result (B) x % sample (C)) divided by theoretical value (D) X 100 or 5.6 — (0.5 x 0.9) X 100 = 103% recovery A— (B x C) X 100 = Percent recovery 5.0 D Corrective Action/Qualifications for MS Spike accuracy is usually based on a range of percent recovery (e.g., 80-120%). Refer to the method of choice for specific acceptance criteria for the matrix spikes until the laboratory develops or adopts statistically valid, laboratory -specific performance criteria for accuracy. If a MS fails, and the LCS is acceptable, qualify the data for the MS sample. Repeated failures for a specific matrix may require use of an alternate method or method of standard addition. Base the sample batch acceptance on the results of the LCS analyses (and other quality control results) rather than the MS alone, because the matrix of the spiked sample may interfere with the method performance. If a MS and the associated LCS fail, re -prepare and reanalyze affected samples. Post Digestion Spikes (PDS) Post Digestion Spikes (PDS) are used for some analyses (e.g., metals) to assess the ability of a method to successfully recover target analytes from an actual sample matrix after the digestion process has been performed. The PDS results are used with MS results to evaluate matrix interferences. The MS and PDS should be prepared from the same environmental sample. A PDS is not to be analyzed in place of a MS. Post Digestion Spikes must be reported as post -digested and must not be misrepresented as pre-digested spikes. (Exception: TCLP and SPLP samples are always spiked post digestion.) Corrective Action/Qualifications for Post Digestion Spikes In general, if the MS recovery for an analyte does not fall within the quality control acceptance range but the PDS recovery is acceptable, then a matrix affect (associated with the preparatory process) should be suspected and the unspiked sample results must be qualified on the basis of the matrix spike recovery. However, when historical data for the effect does not exist, the laboratory would normally be expected to perform a second digestion and reanalysis of the MS to confirm the result. The result would be confirmed if the MS recoveries and PDS recoveries for both sets of analyses were similar in magnitude and bias. When both the MS recovery and PDS recovery for a particular analyte falls outside of quality control acceptance range in the same manner (i.e., the PDS and MS failures are of similar magnitude and the direction of bias is the same), confirmatory analyses are unnecessary but the data must be qualified. 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