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HomeMy WebLinkAbout#402_2016_0510_BS_FINALTo be attached to all inspection reports in-house only. Laboratory Cert. #: Laboratory Name: Inspection Type: Inspector Name(s): Inspection Date: Date Report Completed: Date Forwarded to Reviewer: Reviewed by: Date Review Completed: Cover Letter to use: Unit Supervisor/Chemist III: Date Received: Date Forwarded to Admin: Date Mailed: 402 Prism Laboratories, Inc. Commercial Maintenance Beth Swanson, Gary Francies, Anna Ostendorff, Dana Satterwhite, Todd Crawford, Tonia Springer, Nick Jones Jason Smith May 10-11, 2016 June 1, 2016 June 2. 2016 Jason Smith June 9, 2016 ❑ Insp. Initial ® Insp. Reg. ❑ Insp. No Finding ❑ Insp. CP ❑ Corrected ❑ Insp. Reg. Delay Gary Francies e 13. 2016 7/21 /2016 7/22/201 Special Mailing Instructions: Wes Bell - MRO Water Resources ENVIRONMENTAL allAU! Y July 21, 2016 402 Mr. Helmuth M.B. Janssen Prism Laboratories, Inc. P.O. Box 240543 Charlotte, NC 28224-0543 PAT MCCRORY DONALD R. VAN DER VAART S. JAY ZIMMERMAN Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) Maintenance Inspection Dear Mr. Janssen: Enclosed is a report for the inspection performed on May, 11, 2016 by Beth Swanson Gary Francies, Dana Satterwhite, Todd Crawford, Tonja Springer, Jason Smith, Nick Jones, and Anna Ostendorff 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. 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 (828) 296-4677. Sincerely, Gary Francies, Technical Assistance/Compliance Specialist Division of Water Resources Attachment cc: Beth Swanson Master file LABORATORY NAME: CERTIFICATE : DATE OF INSPECTION: F&79Ar6Tx1H3 114WIXIF AUDITOR(S): LOCAL PERSON(S) CONTACTED: I. INTRODUCTION: Prism Laboratories, Inc. 449 Springbrook Road Charlotte, NC 28217 402 May 10 and 11, 2016 Commercial Maintenance Beth Swanson, Gary Francies, Anna Ostendorff, Dana Satterwhite, Todd Crawford, Tonja Springer, Nick Jones and Jason Smith This laboratory was inspected by a representative 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 environmental samples. II. GENERAL COMMENTS: Overall, the laboratory's system of traceability is thorough, well thought out and easy to follow. Interaction with laboratory staff showed analysts who are knowledgeable and forthcoming and management that is quality control oriented. The laboratory has instituted many quality control practices throughout their systems that are beyond our program requirements. All required Proficiency Testing (PT) samples for the 2016 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, 2016. 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 May 10, 2017. 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 Page 2 #402 Prism Laboratories, Inc. (e.g. Quality Control (QC) frequency, acceptance criteria, etc.). Evaluate all SOPS for the proper use of the word "should". 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 Gulf Coast Analytical Laboratories (Certification #618). III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS: Documentation Recommendation: It is recommended that an indication such as "out of service" be included on the thermometer calibration records when that thermometer is no longer being used. The calibration records could be misconstrued, indicating that calibrations were not being performed at the required frequency. Recommendation: It is recommended that a diagram be made of the metals digestion block so that it is possible to tell which digestion well is used for the daily temperature check. A. 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: NC WW/GW LC Policy. Recommendation: It is recommended that when any documentation correction that affects the final reported sample result is made, the lab also note the reason the change was made. For example, changing an original sample absorbance or weight observation due to further stabilization of the spectrophotometer or balance, the lid to the spectrophotometer was left open in error during sample measurement, etc. Also be aware that improper error corrections that result in QC evaluations going from outside the acceptance range to within the acceptance range, could give the perception of falsification. Some instances of this were noted on the Hexavalent Chromium data from 2/12/2016. B. Finding: All traceability information is not documented or is documented incorrectly. 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 Page 3 #402 Prism Laboratories, Inc. 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: INC WW/GW LC Policy. Comment: While the laboratory has a good system of traceability, there were instances noted where the proper traceability information was not transferred to the applicable benchsheet or the volumes/concentrations of stock standards were either not documented or were incorrect. Much of this information can be found in the laboratory's information management system (LIMS), but when spaces for this information are left blank or the information is incorrect, it appears there is a lack of traceability. The following examples were noted during data review, but this list is not all inclusive. Please review all benchsheets and supporting records for adherence to the Requirement. If a specific method reference is not listed, the Finding is referring to all methods on the laboratory's Certified Parameter Listing at the time of the inspection: ® Hexavalent Chromium (Standard Methods (SM) 3500-Cr B-2009) benchsheet — The Continuing Calibration Verification (CCV) ID is not documented. ® Hexavalent Chromium (SW-846 7196 A (Non -Aqueous)) digestion log — Traceability information for the insoluble spike (PbCr04) is not documented. ® Oil & Grease (EPA 1664 Rev. B) — The Laboratory Control Sample (LCS) true value was not documented on any of the three data sets reviewed. ® Oil & Grease (EPA 1664 Rev. B) — The Matrix Spike (MS) true value was not documented on 9/8/2015 or 3/9/2016. ® Nitrogen, Ammonia (SM 4500 NH3 C-1997) — The stock concentration was incorrectly documented as 100 mg/L for the MS/Matrix Spike Duplicate (MSD) and LCS instead of 1000 mg/L on the 3/6/2015 titration log. ® Nitrogen, Ammonia (SM 4500 NH3 C-1997) — The stock concentration was incorrectly documented as 100 mg/L for the LCS instead of 1000 mg/L on the 8/13/2015 and 11 /6/2015 titration logs. ® Total Kjeldahl Nitrogen (TKN) (EPA 351.2, Rev, 2.0, 1993) — The MS/MSD stock solution was not identified on the 8/31/2015 digestion log. ® Anions IC — The Nitrite CCV is consistently not documented in the Source Standard column of the "IC Standards and Reagents Documentation Sheet". ® MBAS — The stock concentration for the LCS was incorrectly documented as 10 mg/L instead of 100 mg/L on the two benchsheets reviewed. C. Finding: Method references are incomplete or incorrect on some benchsheets and/or supporting documentation. This is considered pertinent information. 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). Requirement: Analytical methods, sample preservation, sample containers and sample holding times shall conform to those requirements found in 40 CFR-136.3. Ref: 15A NCAC 2H .0805 (a) (1). Page 4 #402 Prism Laboratories, Inc. Comment: Data is reported on client reports with the correct methods/revisions. The following examples were noted during data review, but this list is not all inclusive. Please review all benchsheets and supporting records for adherence to the Requirement: e Most benchsheets and supporting records for Standard Methods methods did not include the approval year as stated in 40 CFR Part 136.3 Table IB (i.e., the Turbidity reference would be SM 2130B-2001 rather than SM 2130B). • The Mercury Analysis Review Checklist and Instrument printouts reference 7471 A rather than 7471 B. e The TKN digestion log references Nor9 B instead of No,9 C. D. Finding: The units of measure are not consistently documented on the benchsheets. 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. Ref: 15A NCAC 2H .0805 (a) (7) (H). Comment: The units of measure are not documented and/or incorrect in the following locations. If a specific method reference is not listed, the Finding is referring to all methods on the laboratory's Certified Parameter Listing at the time of the inspection: e MBAS benchsheet — Reporting Limit column. • Acidity benchsheet — pH. • Alkalinity benchsheet — pH and Total Volume column of the standard preparation section. e Coliform- Fecal (MF) benchsheet — Waterbath Temperatures e COD benchsheet — wavelength and Quality Control (QC) true value. • Color, PC benchsheet — Instrument Reading column, LCS calculation and LCS obtained value. e Oil & Grease (EPA 1664 Rev. B) — the units for the 2 mg weight column are listed as mg but analysts occasionally document in grams. • Oil & Grease (SW-846 9071 B) — the units for the spike concentration are mg/kg instead of mg/L. e Total, Dissolved and Suspended Residue benchsheets — QC True Value • Turbidity benchsheet — Initial Calibration Verification (ICV), True Value, pH, Meter Reading, Reporting Limit (RL) and duplicate results. • Settleable Residue benchsheet — Reported Result column. • Hexavalent Chromium benchsheet (SM 3500 Cr-B-2009) — cell path length, Absorbance column, Minimum Reporting Limit (MRL) column, and wavelength. E. Finding: Precision (e.g., Relative Percent Difference (RPD)) and/or accuracy (e.g., percent recovery) of quality control results are not consistently evaluated and/or documented to demonstrate the analytical process is in control and the established acceptance criteria are met. 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). Comment: The precision and accuracy of QC results must be documented and evaluated against the prescribed acceptance criteria to demonstrate that the analytical Page 5 #402 Prism Laboratories, Inc. process is in control. Any samples associated with QC not meeting the criteria must be reanalyzed if possible. If this is not possible, the data must be flagged on the laboratory reports as all quality control requirements not met and giving a brief description of the QC exceedance that occurred. The laboratory indicated that all QC calculations are entered into the LIMS system and evaluated at a later time, however there are some instances where the analyst needs to know immediately if the QC results are within acceptance criteria. Also, for instances where there is a space to enter QC results on the benchsheet and that space is left blank, it appears that the evaluation did not occur, even if it was later executed in LIMS. The following examples were noted during data review, but this list is not all inclusive. Please review all benchsheets and supporting records for adherence to the Requirement. If a specific method reference is not listed, the Finding is referring to all methods on the laboratory's Certified Parameter Listing at the time of the inspection: ® Suspended Residue benchsheet — The RPD for duplicates was not documented for two benchsheets reviewed. The third benchsheet did not include analysis of a duplicate. ® Dissolved Residue benchsheet — The RPD for duplicates was not documented for all three benchsheets reviewed and LCS recovery was not documented for two out of three benchsheets reviewed. ® Total Residue benchsheets — The RPD for duplicates was not documented on all three benchsheets reviewed. ® Oil & Grease (EPA 1664 Rev. B) — The standard concentration and the volume used to prepare the LCS were not documented on the 3/9/2016 benchsheet. ® Oil & Grease (EPA 1664 Rev. B) — The concentration of the standard used for the LCS and spike preparation were incorrectly documented as 40 mg/L instead of 4000 mg/L on the 1/4/2016 benchsheet. ® Oil & Grease (SW-846 7071 B) — The LCS for both Oil & Grease and Oil & Grease (SGT) are not always calculated. Occasionally, the SGT recovery is calculated. ® Oil & Grease (SW-846 7071 B) — The MS/MSD recoveries and RPD were not documented on the 1/27/2016 benchsheet, which has spaces to enter all values. One recovery and the RPD failed, and the sample was qualified on the client report since the results were entered into the LIMS system and calculated there. ® Oil & Grease (EPA 1664 Rev. B) — The LCS result and evaluation were not documented on any of the three data sets reviewed. ® Oil & Grease (EPA 1664 Rev. B) — The matrix spike evaluation was not documented on 9/8/2015 or 3/9/2016. ® Oil & Grease (EPA 1664 Rev. B) — The duplicate was not evaluated on any of the three data sets reviewed. ® Anions IC — The evaluation of all QC standard percent recoveries is not documented, however, it appears they are calculated at some point based on the "Analysis Review Checklist". ® Conductivity (SM 251013-1997) — The RPD for duplicates were not calculated and documented. General F. Finding: The State Laboratory is not notified when samples are received out of compliance and analyzed at the client's request. Page 6 #402 Prism Laboratories, Inc. Requirement: At any time a laboratory receives samples which do not meet sample collection, holding time, or preservation requirements, the laboratory must notify the sample collector or client and secure another sample if possible. If another sample cannot be secured the original sample may be analyzed but the results reported must be qualified with the nature of the infraction(s) and the laboratory must notify the State Laboratory about the infraction(s). The notification must include a statement indicating corrective actions taken to prevent the problem for future samples. Ref: 15A NCAC 2H .0805 (a) (7) (N). Proficiency Testing G. Finding: The preparation of Proficiency Testing (PT) samples is not documented. Requirement: PT samples received as ampules must be diluted according to the PT provider's instructions. The preparation of PT samples must be documented in a traceable log or other traceable format. The diluted PT sample becomes a routine environmental sample and is added to a routine sample batch for analysis. Ref: Proficiency Testing Requirements, February 20, 2012, Revision 1.2. Comment: Dating and initialing the instruction sheet for the preparation of applicable PTs would satisfy the documentation requirement. H. Finding: The laboratory is not always analyzing PT samples in the same manner as routine compliance samples. Requirement: All PT samples are to be analyzed and the results reported in a manner consistent with the routine analysis and reporting requirements of compliance samples and any other samples analyzed according to the requirements of 15A NCAC 2H .0800. Ref: Proficiency Testing Requirements, February 20, 2012, Revision 1.2. Comment: The Nitrogen, Nitrite PT sample was analyzed with three additional QC standards which are not routinely analyzed with compliance samples. Other PT analyses observed did not include extra QC. Quality Control I. Finding: Data that does not meet all quality control requirements is not always qualified on the client report. Requirement: When quality control (QC) failures occur, the laboratory must attempt to determine the source of the problem and must apply corrective action. Part of the corrective action is notification to the end user. If data qualifiers are used to qualify samples not meeting QC requirements, the data may not be useable for the intended purposes. It is the responsibility of the laboratory to provide the client or end -user of the data with sufficient information to determine the usability of the qualified data. Ref: NC WW/GW LC Policy. Comment: Two instances were noted during data review where the relative percent difference (RPD) for the duplicates was not acceptable and it was flagged in LIMS but not carried through to the client report. These were for Settleable Residue sample # 6010269 and Dissolved Residue sample #601-103. Duplicates are not required for Settleable Residue, but if analyzed, the QC criterion must be evaluated and corrective action and/or qualifying the results must be performed when necessary. Page 7 #402 Prism Laboratories, Inc. Acidi —Standard Methods, 2310 B-1997, Rev. 2011 (Aqueous) J. Finding: The laboratory is correcting the sample result for the method blank. Requirement: The calculation does not include blank correction: Acidity, as mg CaCO3/L = [(A a)—(CxA)]x5D000 mL saniple Where: A = mL NaOH titrant used, B = normality of NaOH, C = mL H2SO4 used (2310B.4a), and D = normality of H2SO4 Ref: Standard Methods, 2310 B-1997. (5). K. Finding: The laboratory is not documenting all sample volumes. 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. Ref: 15A NCAC 2H .0805 (a) (7) (H). Comment: The benchsheet did not include the volume analyzed for the blank, LCS, or RL standard. The volume is needed to calculate the Acidity result for these samples. Bacteria — Coliform Fecal — Standard Methods, 9222 D-1997 (MF) (Aqueous) Bacteria — Coliform Fecal — Standard Methods, 9222 D-1997 (MF) 24hr 503 (Non -Aqueous) L. Finding: Consumable materials used for the Fecal and Total Coliform Membrane Filtration (MF) methods are not properly tested. Requirement: When a new lot of culture medium, pads, or membrane filters is to be used, a comparison of the current lot in use (reference lot) against the new lot (test lot), be made. As a minimum, make single analyses on five positive samples. Ref: NC WW/GW LC Policy. Comment: The laboratory is analyzing a culture positive with each new lot of filters and media. The old and new lots are not compared, and new lots of pads are not being tested at all. A copy of the Testing of Consumable Materials for Fecal Coliform MF Method policy is attached to the end of this report. M. Finding: Plate comparison counts are not performed and documented monthly. 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). Page 8 #402 Prism Laboratories, Inc. Comment: The analyst stated that positive plate count comparisons among analysts were occasionally performed, but not on a monthly basis and the process was not documented. N. Finding: Filtration start time is not documented to show that plates are placed into the incubator within 30 minutes. 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: 15A NCAC 2H .0805 (a) (7) (A). O. Finding: Culture positive plates are not countable. Requirement: A culture positive must be analyzed with each batch of prepared media and once per week for purchased ready -to -use media. A sample volume that yields a countable plate must be analyzed so that individual colonies may be verified to have proper morphology (i.e. color, shape, size, surface appearance). Ref: NC WW/GW LC Policy. P. Finding: The UV lamp bulbs are not cleaned monthly. Requirement: When used, disconnect lamps monthly and clean blubs with a soft cloth moistened with ethanol, 70% methanol/30% reagent -grade water, or use spectroscopic grade 2-propanol where baked on material may be collecting. Ref: Standard Methods, 9020 B-2005. (4) (1). Q. Finding: The laboratory is using a partial immersion thermometer in the fecal water bath improperly. Requirement: Thermometers with no indicated depth are the total immersion type. When a partial -immersion thermometer is used, the bottom of the thermometer up to the immersion line should be exposed to the temperature being measured, with the remainder of the thermometer exposed to ambient conditions. When a total immersion thermometer is used, the bulb and the entire portion of the stem containing liquid, except for the last 1 cm, are exposed to the temperature being measured. If the thermometer is not used in this manner, the thermometer immersion is incorrect. Ref: "Selecting Alternatives to Mercury - Filled Thermometers", http:l/tLy\iv v.e a.goy/mercury/alternatives.htrn. Comment: The thermometers in the #1 and #3 fecal water baths were not immersed to the proper depth. The water was a few inches above the immersion line on each thermometer. Bacteria — Coliform Total — Standard Methods, 9222 B-1997 (MF) (Aqueous) Recommendation: It is recommended that the shelf on which the incubator temperature is obtained be documented on the benchsheet. The laboratory currently has an incubator with three shelves and a thermometer on each one. Bacteria — Coliform Fecal — Standard Methods, 9221C E-2006 (MPN) 24hr 503 (Non - Aqueous) Bacteria — Coliform Fecal — Standard Methods, 9221C E-2006 (MPN) (Aqueous) R. Finding: The laboratory is not analyzing duplicates. Page 9 #402 Prism Laboratories, Inc. Requirement: Analyze five percent of all samples in duplicate to document precision. Laboratories analyzing less than 20 samples per month must analyze at least one duplicate each month samples are analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (C). Comment: A duplicate is only required on one dilution per sample for Fecal Coliform. Bacteria — Coliform Fecal — Standard Methods, 9221C E-2006 (MPN) 24hr 503 (Non - Aqueous) Bacteria — Coliform Fecal — Standard Methods, 9221 C E-2006 (MPN) (Aqueous) S. Finding: The A-1 media is not properly stored and is used beyond the method stated shelf life. Requirement: Store in the dark at room temperature for not longer than 7 days. Ref: Standard Methods, 9221 E-2006. (2) (a). Comment: The A-1 media is currently stored in the refrigerator for 2 weeks. BOD —Standard Methods, 5210 B-2001 (Aqueous) CBOD — Standard Methods, 5210 B-2001, Rev. 2011 (Aqueous) Recommendation: It is recommended that the spaces for the drift check and calibration check be labeled accordingly. The current system causes confusion, as the calibration check is labeled "drift ±0.1 mg/L" and the drift check is labeled "calibration blank". T. Finding: Seed controls with less than 2.0 mg/L Dissolved Oxygen (DO) depletion are used for seed correction calculation. Requirement: For the ratio method, divide the DO depletion by the volume of seed in milliliters for each seed control bottle having a 2.0 mg/L depletion and greater than 1.0 mg/L minimum residual DO and average the results. Ref: Standard Methods, 5210 B-2001. (6) (d) . Comment: This was noted on BOD data from 3/3/2016 and the analyst indicated that a minimum depletion is not considered when evaluating the individual seed controls. U. Finding: The laboratory is incorrectly reporting results for samples that do not meet the minimum depletion. Requirement: The reporting limit for BOD5/CBOD5 is 2 mg/L. Only bottles giving a minimum DO depletion of 2.0 mg/L and a residual DO of 1.0 mg/L after 5 days of incubation are considered to produce valid data. It is not acceptable to elevate the reporting limit and report as less than the value that would have been obtained if the dilution had depleted the required 2.0 mg/L. It is required that the data be flagged as a quality control failure if it does not deplete the 2.0 mg/L. The only exception to this is when a 100% sample does not deplete 2.0 mg/L. In this case, report the value as <2.0 mg/L without qualification. Ref: NC WW/GW LC Policy. Comment: The laboratory does not analyze 100% samples and when there are no dilutions that meet the minimum DO depletion, the reporting limit is elevated and it is reported as less than the elevated reporting limit without qualification. This is automatically performed in LIMS. The BOD/CBOD value must be calculated using the smallest dilution (i.e., most sample) and reported with a qualifier and not reported as a less than value. Page 10 #402 Prism Laboratories, Inc. V. Finding: The barometric pressure at the time of meter calibration is not documented. This is considered pertinent data. 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). W. Finding: Initial DO concentrations of all bottles other than the blank are not always brought to the required range of 7 and 9 mg/L. Requirement: The working range is equal to the difference between the maximum initial DO (7 to 9 mg/L) and minimum DO residual of 1 mg/L corrected for seed, and multiplied by the dilution factor. Ref: Standard Methods, 5210 B-2001. (8) (b). Requirement: Samples supersaturated with DO — Samples containing DO concentrations above saturation at 20 °C may be encountered in cold waters or in water where photosynthesis occurs. To prevent loss of oxygen during incubation of such samples, reduce DO to saturation by bringing sample to about 20 ± 3 °C in partially filled bottle while agitating by vigorous shaking or by aerating with clean, filtered compressed air. Ref: Standard Methods, 5210 B-2001. (4) (b) (4). Comment: The laboratory is using an initial DO maximum of 9.2 mg/L. The DO saturation table used as part of the DO meter calibration verification procedure lists the saturation of DO at 20 ° C as 9.08 mg/L. X. Finding: The benchsheet does not document that initial DO is read within 30 minutes of dilution preparation. Requirement: After preparing dilution, measure initial DO within 30 minutes. Ref: Standard Methods, 5210 B-2001. (5) (g). 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). Y. Finding: The position of the drift check during the analytical batch is not indicated on the benchsheet. Requirement: If the membrane electrode method is used, take care to eliminate drift in calibration between initial and final DO readings. Ref: Standard Methods, 5210 B-2001. (5) (g) 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 reanalyze the drift check bottle and document the concentration (day one final drift check). The laboratory should verify the DO Meter calibration throughout the sample set if needed. Repeat process on Day 5. If the meter drifts more than 0.20 mg/L, recalibrate meter and reanalyze all samples since the last drift check. Ref: NC WW/GW LC Policy. Comment: There is one spot for a drift check on each page of the BOD/CBOD benchsheet, but it is not clear at what point during analysis these drift checks are read. Page 11 #402 Prism Laboratories, Inc. Anions (Cl-, F-, SO4, NO2, NO3, NO3+NO2) — EPA 300.0, Rev. 2.1, 1993 (Aqueous & Non - Aqueous) Anions (Cl-, F-, SO4, NO2, NO3, NO3+NO2) — SW-846 9056 A (Aqueous & Non -Aqueous) Comment: An acceptance criterion for method/reagent blanks of <_ 1/2 RL may be used in place of the EPA 300.0 requirement of <MDL. Recommendation: It is recommended that the Analysis Review Checklist be edited to remove the phrase "percent recoveries and" in item #4, which only concerns RPD acceptance. Z. Finding: The initial and continuing calibration blank acceptance criterion exceeds 50% of the reporting limit. Requirement: For analyses requiring a calibration curve, the concentration of reagent, method and calibration blanks must not exceed 50% of the reporting limit or as otherwise specified by the reference method. Ref: NC WW/GW LC Policy. Comment: The laboratory's initial and continuing calibration blank acceptance criterion is <RL. The reviewed data often showed calibration blanks that were >'/2 RL for Nitrate, so the RL for this analyte may need to be elevated. Chlorine, Total Residual — Standard Methods, 4500 Cl G- 2000, Rev. 2011 (Aqueous) AA. Finding: A reagent blank is not analyzed each day standards are prepared. Requirement: Each day that prepared standards are analyzed, a reagent blank must be analyzed to determine if method analytes or other interferences are present in the laboratory environment, the reagents or the apparatus. A reagent blank is made from the same laboratory water source used to make quality control 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. Ref: NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine. Comment: The laboratory currently prepares and analyzes three standards daily. COD — Standard Methods, 5220 D-1997, Rev. 2011 (Aqueous) COD — Hach 8000 (Aqueous) Inorganic Phenols — EPA 420.1 Rev. 1978 (Aqueous) Inorganic Phenols — SW-846 9065 (Aqueous) MBAS — Standard Methods, 5540 C-2000, Rev. 2011 (Aqueous) Phosphate, Ortho — Standard Methods, 4500 P E-1999, Rev. 2011 (Aqueous) Phosphorus, Total — Standard Methods, 4500 P E-1999, Rev. 2011 (Aqueous) Phosphorus, Total — EPA 365.1, Rev. 2.0, 1993 (Aqueous) Chromium Hexavalent— Standard Methods, 3500 Cr-B-2009 (Aqueous) BB. Finding: A blank is not analyzed after every ten samples and/or at the end of the 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., Page 12 #402 Prism Laboratories, Inc. repeating sample determinations since the last acceptable calibration verification, repeating the initial calibration, etc.). Ref: NC WW/GW Policy. Comment: Most of the data reviewed had fewer than 10 samples, so only the blank at the end of the group would apply. COD —Standard Methods, 5220 D-1997, Rev. 2011 (Aqueous) CC. Finding: The CCV acceptance criterion is ±10% recovery. Requirement: Prepare calibration curve for each new lot of tubes or ampules or when standards prepared in ¶a above differ by >_5% from calibration curve. Ref: Standard Methods, 5220 D-1997. (4) (c). Comment: The three benchsheets reviewed included CCV values that did not differ by more than >_5% from the calibration curve. Cyanide — Standard Methods, 4500 CN- E-1999, Rev. 2011 (Total) (Aqueous) DD. Finding: The laboratory is not always documenting the sample volume and/or final distillation volume. 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). Comment: The sample volume and final distillation volumes were documented as a check mark on the 9/1/2015 distillation sheet. EE. Finding: The laboratory is not back calculating the calibration standards. Requirement: Back calculate the concentration of each calibration point. The back - calculated and true concentrations should agree within ± 10%. Ref: Standard Methods, 4020 B-2009. (2) (a). Cyanide — Standard Methods, 4500 CN- E-1999, Rev. 2011 (Total) (Aqueous) Cyanide — SW-846 9014 (Total) (Colorimetric) (Aqueous & Non -Aqueous) Comment: Samples analyzed by SW-846 9014 are distilled according to SW-846 9010C, which is a Method Defined Parameter. SW-846 9010C must be followed exactly as written, or the resulting data cannot be used to ensure regulatory compliance. FF. Finding: Ethylenediamine solution is being added to all samples. Requirement: There is no mention of this compound in either SW-846 9010C or SW-846 9014 Ref: EPA SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 9010 C. Rev. 3, November 2004 and EPA SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 9014. Rev. 1, July 2014. Page 13 #402 Prism Laboratories, Inc. Requirement: If formaldehyde, acetaldehyde, or other water-soluble aldehydes are known or suspected to be present, treat the sample with 2 mL 3.5 % ethylenediamine (Section 6.10) per 100 mL of sample to avoid the formation of cyanohydrins. It has been found that this quantity of ethylenediamine addition is suitable to overcome the interference caused by up to 50 mg/L CH2O present. Samples can be screened for the presence of formaldehyde and other watersoluble aldehydes using test strips for formaldehyde or aldehydes. Ref: Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012; Table II, #23 Footnote 6 and ASTM Method D7365-09a, Section 8.3.8. Recommendation: It is recommended that Ethylenediamine solution only be added to samples that have tested positive for aldehydes. Cyanide — SW-846 9014 (Total) (Colorimetric) (Aqueous & Non -Aqueous) Comment: Samples analyzed by SW-846 9014 are distilled according to SW-846 9010C, which is a Method Defined Parameter. SW-846 9010C must be followed exactly as written, or the resulting data cannot be used to ensure regulatory compliance. GG. Finding: A 0.25 N sodium hydroxide solution is being used in the gas scrubber. Requirement: Pipet 50 mL of 1.25 N sodium hydroxide into the gas scrubber. Ref: EPA SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 9010 C. Rev. 3, November 2004, Section 7.2.1. MBAS — Standard Methods, 5540 C-2000, Rev. 2011 (Aqueous) HH. Finding: The linear alkylbenzene sulfonate (LAS) molecular weight is not documented on the calibration curve. Requirement: From the calibration curve (5540C.4a) read micrograms of apparent LAS (mol wt ___) corresponding to the measured absorbance. Ref: Standard Methods, 5540 C-2000. (5). Nitrogen, Ammonia — Standard Methods, 4500 NH3 C-1997, Rev. 2011 (Aqueous) II. Finding: Sample pH adjustment to 9.5 s.u. is not checked with a pH meter. Requirement: Add 25 mL borate buffer solution and adjust to pH 9.5 with 6N NaOH using a pH meter. JJ. Finding: Borate buffer is not being used to steam out the distillation apparatus. Requirement: Equipment preparation: Add 500 mL water and 20 mL borate buffer, adjust pH to 9.5 with 6N NaOH solution, and add to a distillation flask. Add a few glass beads or boiling chips and use this mixture to steam out the distillation apparatus until distillate shows no traces of ammonia. Ref: Standard Methods, 4500 NH3 B- 1997, Rev. 2011. (4) (a). Nitrogen, Nitrite — Standard Methods, NOz" B-2000, Rev. 2011 (Aqueous) KK. Finding: The blank acceptance criterion is not properly evaluated. Page 14 #402 Prism Laboratories, Inc. Requirement: For analyses requiring a calibration curve, the concentration of reagent, method and calibration blanks must not exceed 50% of the reporting limit or as otherwise specified by the reference method. Ref: NC WW/GW LC Policy. 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). Comment: The precision and accuracy of QC results must be documented and evaluated against the prescribed acceptance criteria to demonstrate that the analytical process is in control. Any samples associated with QC not meeting the criteria must be reanalyzed if possible. If this is not possible, the data must be flagged on the laboratory reports and Discharge Monitoring Reports (DMR) as all quality control requirements not met and giving a brief description of the QC exceedance that occurred. Comment: Blank values were being documented on benchsheets as < 0.01 mg/L, which is the reporting level. This does not allow for proper evaluation against the required acceptance criterion. Nitrogen, Total Kieldahl — Standard Methods, Nog C-1997 (Standard Methods 4500 NH3 C- 1997, Rev. 2011) (Aqueous) Comment: No results are reported by this method, only EPA 351.2, Rev. 2.0, 1993. Nitrogen, Total Kieldahl — EPA 351.2, Rev. 2.0, 1993 LL. Finding: The incorrect volume of mercury -free digestion solution is being added to the samples. Requirement: Note 1: An alternate mercury -free digestion solution can be prepared by dissolving 134 g K2SO4 and 7.3 g CUSO4 in 800 mL reagent water and then adding 134 mL conc. H2SO4 and diluting to 1 L. Use 10 mL solution per 25 mL of sample. Comment: The laboratory is adding 5 mL of mercury -free digestion solution per 25 mL of sample, which is the volume used for digestion solutions that contain mercury. MM. Finding: Each calibration standard is not being digested independently. Requirement: Prepare a series of at least three standards, covering the desired range, and a blank by diluting suitable volumes of standard solution (Section 7.11) with reagent water. Ref: EPA 351.2, Rev. 2.0, 1993, Section 10.1. Requirement: Process standards and blanks as described in Section 11.0, Procedure. Ref: EPA 351.2, Rev. 2.0, 1993, Section 10.2. Comment: The laboratory is digesting a 10 mg/L intermediate standard and then making dilutions of that to prepare the curve. Oil & Grease — EPA 1664 Rev. B (Aqueous) NN. Finding: The acceptance criterion for the 2 mg weight is not within the method specified limit and the balance is not always recalibrated if outside the laboratory's acceptance limit. Page 15 #402 Prism Laboratories, Inc. Requirement: Calibration shall be within ± 10% (i.e. ± 0.2 mg) at 2 mg, ± 0.5% (i.e., ± 5 mg) at 1000 mg, and if applicable, at the appropriate user -specified tolerance for Class 1 weights greater than 1000 mg. If values are not within these limits, recalibrate the balance. Ref: EPA Method 1664 Rev. B, Section 10.2. Comment: The laboratory uses an acceptance criterion of ± 0.5 mg for the 2 mg weight. On 9/8/2015, the weight check was recorded as 0.0026 (which is in grams instead of the column heading of mg), which would have failed the laboratory's elevated acceptance criterion. The balance was not recalibrated at this time. Oil & Grease — SW-846 9071 B (Non -Aqueous) Recommendation: It is recommended that the blank on the benchsheet be identified as the method blank. Paint Filter Liquids — SW-846 9095B Recommendation: It is recommended that the LCS and Blank, which are pre-printed onto the benchsheet, be removed since they are not analyzed. Residue, Settleable — Standard Methods, 2540 F-1997 (Aqueous) 00. Finding: The 45-minute sample stir time is not documented. Requirement: The following must be documented in indelible ink whenever sample analysis is performed: 45-minute stir time (use of a check box is acceptable). Ref: NC WW/GW LC Approved Procedure for the Analysis of Settleable Solids. Residue, Dissolved 180 C — Standard Methods, 2540 C-1997, Rev. 2011 (Aqueous) Residue, Suspended —Standard Methods, 2540 D-1997, Rev. 2011 (Aqueous) Residue, Total — Standard Methods, 2540 B-1997, Rev. 2011 (Aqueous) PP. Finding: The oven temperature and the amount of time in the oven are not documented for the second drying cycle. This is considered pertinent information. Requirement: Dry evaporated sample for at least 1 h in an oven at 180 ± 2°C, cool in a desiccator to balance temperature, and weigh. Repeat drying cycle of drying, cooling, desiccating, and weighing until a constant weight is obtained or until weight change is less than 4% of previous weight or 0.5 mg, whichever is less. Ref: Standard Methods, 2540 C- 1997. (3) (d). Requirement: Dry for at least 1 h at 103 to 105°C in an oven, cool in a desiccator to balance temperature, and weigh. Repeat drying cycle of drying, cooling, desiccating, and weighing until a constant weight is obtained or until weight change is less than 4% of previous weight or 0.5 mg, whichever is less. Ref: Standard Methods, 2540 D-1997. (3) (c). Requirement: Dry evaporated sample for at least 1 h in an oven at 103 to 105°C, cool in a desiccator to balance temperature, and weigh. Repeat drying cycle of drying, cooling, desiccating, and weighing until a constant weight is obtained or until weight change is less than 4% of previous weight or 0.5 mg, whichever is less. Ref: Standard Methods, 2540 B- 1997. (3) (b). Page 16 #402 Prism Laboratories, Inc. 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: In lieu of drying to a constant weight daily, the laboratory may choose to perform a drying study at least every 12 months. The drying study policy is attached to the end of this report. Residue, Dissolved 180 C — Standard Methods, 2540 C-1997, Rev. 2011 (Aqueous) Residue, Suspended —Standard Methods, 2540 D-1997, Rev. 2011 (Aqueous) QQ. Finding: The sample is occasionally allowed to filter for more than 10 minutes. Requirement: If more than 10 min are required to complete filtration, increase filter size or decrease sample volume. Ref: Standard Methods, 2540 C-1997. (3) (c). Requirement: If complete filtration takes more than 10 min, increase filter diameter or decrease sample volume. Ref: Standard Methods, 2540 D-1997. (3) (b). Comment: The analyst stated that samples were allowed to filter for approximately 15 minutes before re -analyzing a smaller volume. Residue, Total — Standard Methods, 2540 B-1997, Rev. 2011 (Aqueous) RR. Finding: Samples are being evaporated in an oven above 100°C. Requirement: When evaporating in a drying oven, lower temperature to approximately 20C below boiling to prevent splattering. Ref: Standard Methods, 2540 B-1997. (3) (b). Comment: The Total Residue and Total Dissolved Solids (TDS) samples are being evaporated in the 103 to 1050C oven. At the inspection, the laboratory was told that both Total Residue and Dissolved Residue required the samples to be evaporated below 100°C, however, it is only specified in the Total Residue method. Despite this, the same issue with boiling and splatter is likely to occur with TDS samples. Residue, Suspended —Standard Methods, 2540 D-1997, Rev. 2011 (Aqueous) SS. Finding: Duplicates are not analyzed at the required frequency. Requirement: Analyze at least 10% of all samples in duplicate. Ref: Standard Methods, 2540 D-1997. (3) (c). Comment: On 9/3/2015, one duplicate was analyzed with 20 samples. On 1/5/2016, one duplicate was analyzed with 14 samples. On 3/7/16, no duplicates were analyzed with 12 samples. Residue, Dissolved 180 C — Standard Methods, 2540 C-1997, Rev. 2011 (Aqueous) TT. Finding: The filters are not being washed before use. Requirement: Preparation of glass -fiber filter disk: If pre -prepared glass fiber filter disks are used, eliminate this step. Insert disk with wrinkled side up into filtration apparatus. Apply vacuum and wash disk with three successive 20-mL volumes of reagent -grade water. Page 17 #402 Prism Laboratories, Inc. Continue suction to remove all traces of water. Discard washings. Ref: Standard Methods, 2540 C-1997. (3) (a). Sulfide — Standard Methods, 4500 S2- F-2000, Rev. 2011 (Aqueous) Comment: The laboratory currently verifies the sample pH at receipt is above 12 Standard Units (s.u.). 40 CFR Part 136.3 Table II states that it only needs to be preserved to pH >9 s.u., if the laboratory wishes to change their requirement. Recommendation: It is recommended that the pH column on the benchsheet be removed if it is not consistently and correctly used. Since the sample pH is checked upon receipt and recorded with the Chain of Custody (COC) on the Sample Receiving Summary, the extra documentation is unnecessary. The benchsheet from 9/9/2015 documented the sample pH as <12 s.u., which would not sufficiently demonstrate that the pH is >9 s.u. On the 3/22/2016 benchsheet, the pH was not documented at all. Temperature — Standard Methods, 2550 B-2000 (Aqueous) UU. Finding: The laboratory benchsheet was lacking pertinent data: sample analysis time. Requirement: The following must be documented in indelible ink whenever sample analysis is performed: Date and time of sample analysis. Ref: NC WW/GW LC Approved Procedure for the Analysis of Temperature. Turbidi — Standard Methods, 2130 B-2001, Rev. 2011 (Aqueous) Turbidi — EPA 180.1, Rev. 2.0, 1993 (Aqueous) Comment: It is not necessary for the laboratory to check the pH of Turbidity samples. Recommendation: It is recommended that the analysts be educated on properly filling out the Turbidity benchsheet in regards to the use of the "meter reading", "dilution", "calculated value" and "reported value" columns. Data reviewed showed that some analysts record the original meter reading in the "reported value" column, which gives the impression that the incorrect value is being reported to the client. In reality, this is the value that is entered into LIMS and it is then calculated in the system with the dilution factor and reported correctly to the client. W. Finding: The laboratory is diluting samples over 40 NTU. Requirement: In order to insure consistency among laboratories, NC WW/GW LC policy is to avoid dilutions whenever possible. Samples need only be diluted if their concentration falls outside the allowable calibration range of the meter. Ref: NC WW/GW LC Policy. Metals — EPA 200.7, Rev. 4.4, 1994 (Aqueous) Metals — SW-846 6010 D (Aqueous) Comment: The lab is utilizing Standard Methods, 3030 C for treatment of groundwater compliance samples. This method is no longer required by any North Carolina permitting authority. Recommendation: It is recommended that sample dilution and reanalysis be performed through the dilution test as described in EPA 200.7, Rev. 4.4, 1994, Section 9.5.2, for samples with Matrix Spike (MS) and Matrix Spike Duplicate (MSD) concentrations above the calibration range. Metals — EPA 200.8, Rev. 5.4, 1994 (Aqueous) Metals — SW-846 6020 B (Aqueous) Mercury — SW-846 7471 B (Non -Aqueous) Page 18 #402 Prism Laboratories, Inc. 1,2 - Dibromoethane (EDB) — SW-846 8011 (Aqueous) WW. Finding: The blank acceptance criterion exceeds 50% of the reporting limit or as otherwise specified by the reference method. Requirement: For analyses requiring a calibration curve, the concentration of reagent, method and calibration blanks must not exceed 50% of the reporting limit or as otherwise specified by the reference method. Ref: NC WW/GW LC Policy. Requirement: When LRB values constitute 10% or more of the analyte level determined for a sample or is 2.2 times the analyte MDL whichever is greater, fresh aliquots of the samples must be prepared and analyzed again for the affected analytes after the source of contamination has been corrected and acceptable LRB values have been obtained. Ref: EPA 200.8, Rev. 5.4, 1994, Section 9.3.1. Comment: For EPA 200.8 and SW-846 6020 B, the laboratory's current blank acceptance criterion is "<10% of the analyte level or <RL". Our policy states that the laboratory must either use the method criterion (i.e., <10% of the analyte level or <2.2 times MDL) or our criterion (i.e., <1/2 RL). The laboratory does not have the option to use <RL as a blank acceptance criterion by either our policy or the method. For SW-846 7471 B and SW-846 8011, the laboratory's blank criterion is < RL. Chromium, Hexavalent — SW-846 7196 A (Non -Aqueous) Recommendation: It is recommended that the analyst not attempt to weigh the sample to exactly 2.50 g. There is an allowance of ± 0.10 g and the actual amount weighed must be documented. XX. Finding: The laboratory is not analyzing post digestion spikes. Requirement: A post -digestion Cr(VI) matrix spike must be analyzed per batch as discussed in Chapter One. The post -digestion matrix spike concentration should be equivalent to 40 mg/kg or twice the sample concentration observed in the unspiked aliquot of the test sample, whichever is greater. Ref: EPA SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; 31 Edition, Method 3060 A. Rev. 1, December 1996, Section 8.6. Comment: A sample that has been spiked pre -digestion is still required. Chromium, Hexavalent — Standard Methods, 3500 Cr-B-2009 (Aqueous) Recommendation: The column "pH Adjust" is used to check that the pH has been adjusted to 2 ± 0.5 s.u. It is recommended that the column header be updated to indicate this adjustment. Pesticides, Organochlorine — SW-846 8081 B (Aqueous and Non -Aqueous) Polychlorinated Biphenyls — SW-846 8082 A (Aqueous and Non -Aqueous) YY. Finding: The laboratory is not analyzing matrix spikes or sample duplicates. 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 each month samples are analyzed. Ref: NC WW/GW LC Policy. Page 19 #402 Prism Laboratories, Inc. Requirement: Analyze five percent of all samples in duplicate to document precision. Laboratories analyzing less than 20 samples per month must analyze at least one duplicate each month samples are analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (C). Comment: The laboratory is analyzing Laboratory Control Sample/Laboratory Control Sample Duplicate (LCS/LCSD) in place of the matrix spike and matrix spike duplicate or sample duplicate. Recommendation: It is recommended that the laboratory supply extra sample bottles along with instructions to samplers that would ensure enough volume is available to perform MS and MSD or sample duplicate analyses with each batch. Polychlorinated Biphenyls — EPA 608 (Aqueous) Pesticides, Organochlorine — EPA 608 (Aqueous) ZZ. Finding: The laboratory is not analyzing matrix spikes at the required frequency. Requirement: The laboratory must, on an ongoing basis, spike and analyze a minimum of 10% of all samples to monitor and evaluate laboratory data quality. Ref: EPA Method 608, Section 8.1.4. Comment: Matrix spikes are being analyzed at a 5% frequency. Purgeable, Organics — EPA 624 (Aqueous) Purgeable, Organics — SW-846 8260 B (Aqueous) Purgeable, Organics — Standard Methods, 6200 B-1997 (Aqueous) Base Neutral/Acid, Organics — EPA 625 (Aqueous) Base Neutral/Acid, Organics — SW-846 8270 D (Aqueous) AAA. Finding: The laboratory is not always including both the original and manually integrated chromatograms, in a similar scale, in the data package when manual integrations are performed. Requirement: When manual integration is employed, the laboratory must clearly identify manually integrated compounds, document the reason the manual integration was performed, the date performed and who completed the work. A flag or qualifier code may suffice for simple manual integrations. In addition, a hardcopy printout of the data displaying the manual integration shall be included in the raw data package (i.e., both the original and manually integrated chromatograms, of similar scale, must be present in the data package). All information necessary for the historical reconstruction of data must be maintained by the lab. Additionally, the laboratory must employ a systematic data validation procedure to check manual integrations to assure integrations are technically sound and representative of the response. Ref: NC WW/GW LC Policy. Comment: Data reviewed shows that hard copies of manually integrated chromatograms are only printed for calibration curves and analyte hits in samples. Individual analytes in the calibration curve are not being printed. There was also an instance where the printed chromatogram was not at the appropriate scale to compare the manual integration with the original. 1,2 - Dibromoethane (EDB) — EPA 504.1 (Aqueous) 1,2 - Dibromoethane (EDB) — SW-846 8011 (Aqueous) Page 20 #402 Prism Laboratories, Inc. Comment: Due to instrument age and the sensitivity at low levels of analysis, a large number of manual integrations are being performed. Ways in which the analyst should seek to minimize manual integrations include properly maintaining the instrument, updating retention times, and optimizing peak integration parameters (e.g., area reject, peak width, threshold, etc.). While the manual integration data reviewed were consistent and well documented, the number of manual integrations required could leave the data open to scientific and legal scrutiny. Recommendation: The laboratory noted that clients rarely submit trip blanks for this method. It is recommended that project management educate clients on the importance of trip blanks due to the sensitivity of the method. BBB. Finding: The laboratory is not following the manual integration SOP. 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). Comment: The manual integration SOP states that the supervisor must initial and date the printout of the manual integration. In practice, the analyst does this and the supervisor signs the Analysis Review Checklist after reviewing the manual integrations. IV. PAPER TRAIL INVESTIGATION: The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks, etc.) and client reports. Data were reviewed for the following project/sample numbers: 5090184 (SW-846 8270), 6020247 (SM 3500 Cr-B-2009), 6030038 and 5090042 (SW-846 7071 B), 601-103 (SM 2540 C-1997) and 6020458 (SM 5220 D-1997, Hach 8000). No transcription errors were detected. The facility appears to be doing a good job of accurately transcribing data. 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 and implementation dates for each corrective action. Report prepared by: Beth Swanson Date: June 2, 2016 Report reviewed by: Jason Smith Date: June 9, 2016 TSS, TDS and TS Constant Weight/Drying Time Verification Policy (NC WW/GW LC Policy 03/09/2009) Constant weights must be documented. The approved methods require the following: "Repeat the cycle of drying, cooling, desiccating, and weighing until a constant weight is obtained or until the weight change is less than 4% of the previous weight or 0.5 mg, whichever is less." In lieu of this, an annual study documenting the time required to dry representative samples to a constant weight may be performed. Verify minimum daily drying time is greater than or equal to the time used for the initial verification study drying cycle. Drying cycles must be a minimum 1 hour for verification. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy based on Standard Methods, 20' Edition, 2540 D. (3) (c), 2540 B. (3) (b), and 2540 C. (3) (d). Testing of Consumable Materials for Fecal Coliform MF Method (NC WW/GW LC Policy 08/07/2015) Standard Methods requires that before a new lot of consumable materials are used for the Fecal Coliform MF method, those materials be tested to ensure they are reliable. North Carolina policy requires the testing of the following consumable materials before they can be used for sample analyses: membrane filters and/or pads (often packaged together) and media. It is recommended that only one consumable be tested at a time. The following is provided as guidance in performing the required testing. Let's say you got a new batch of membrane filters in. We will call the currently used filters lot #1 and the new filters lot #2. 1. Select a culture positive sample. What you want is something that will yield 20-60 colonies when a reasonable sample volume is filtered. This may be a stream sample or a sample taken somewhere within the waste treatment plant. If the concentration is high enough that greater than 60 colonies are obtained when 1 mL is filtered then the solution is too strong and must be diluted. Any time a sample is diluted be sure it is done with the BUFFERED dilution water used for rinsing the funnels. 2. Test the culture positive to determine the appropriate volume to use. When collecting the culture positive sample do not think about it as a sample. You do not have to be concerned with a sterile sample bottle or 6 hour hold time. Collect enough sample so that you have plenty to work with, probably more than your normal fecal bottle holds. Set a series of dilutions using the currently used materials, in this example filter lot #1. Do not use the materials you want to prove are OK at this point. All you are trying to do is to determine the volume of sample that will yield 20-60 colonies. Put the rest of the sample in the refrigerator. For example: Volume used Colonies obtained on lot #1 filters 50 ml TNTC 25 ml 138 10 ml 50 5 ml 22 1 ml 4 Based on this preliminary testing it appears that a 10 ml volume would probably be appropriate to use and will yield the desired 20-60 colonies. Remember when you do the actual consumable test, the culture positive sample will be 24 hours old and the results you obtain may be lower than the initial results yielded, but not so significantly lower as to change your dilution choice. It is better to have your initial results on the high side of the 20-60 range for this reason. In this example the 5 ml volume would probably be too low and would likely yield less than 20 colonies the next day. 3. Perform the consumable test Once you determine the appropriate volume, in this case 10 mis, take the remaining culture positive sample from the refrigerator, bring to room temperature and set five 10 ml plates with the currently used filters, lot #1, and five 10 ml plates with the new filters, lot #2. 4. Determine acceptability of new material For example: Lot #1-current filters Colonies obtained on lot #1 filters 10 ml 48 10ml 45 10 ml 50 10 ml 44 10 ml 43 Average: 46 Lot #2-new filters Colonies obtained on lot #2 filters 10 ml 40 10ml 45 10 ml 38 10 ml 46 10 ml 37 Average: 41 When determining the acceptability of the new material, compare the average of the five replicates for lot #1 to the average of the five replicates for lot #2; that is 46 vs. 41 colonies. The recommended acceptance criteria would be your current acceptance criteria used for your Fecal Coliform duplicates. If the test and reference materials check within what you have determined is acceptable for duplicates of samples, the test material would be considered acceptable to use. This may be a calculated acceptance criteria based on 3 times the standard deviation of the mean or a set value like 20% RPD. No matter how you determine your duplicate acceptance criteria make sure you use colony counts not final calculated values in doing this. Other factors to consider when determining if a new material is suitable include: Are the colonies obtained typical, that is normal looking blue colonies? Are the colonies evenly distributed across the membrane surface? Are there an unusual number of non typical colonies present? Is there a pattern to the colony recoveries? For example are all the plates for the test materials significantly lower in counts than the reference lot? It is recommended that new consumables be tested as soon as possible after receipt to avoid problems if the materials are not acceptable. Once you determine that the new material is acceptable to use; you may begin to do so. Document the date the new lot # is put into use.