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HomeMy WebLinkAbout#210_2016_00712_JS_FINALINSPECTION REPORT ROUTING SHEET To 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: -r 210 City of Gastonia — Crowders Creek Laboratory Commercial Maintenance Jason Smith Todd Crawford Gary Francies Nick Jones, Anna Ostendorff, Tonia Springer and Beth Swanson July 12 and 15 2016 September 9 2016 September 9 2016 Beth Swanson September 14 2016 ❑ Insp. Initial ❑ Insp. No Finding ❑ Corrected Todd Crawford September 15 2016 September, 26 2016 September 28 2016 ® Insp. Reg. ❑ Insp. CP ❑ Insp. Reg. Delay Special Mailing Instructions: Send copy to Wes Bell at the MRO Wester € esources ENVIRONMENI"AL QUALITY September 28, 2016 210 Ms. Annette McMurray City of Gastonia - Crowders Creek Laboratory City of Gastonia P.O. Box 1748 Gastonia, NC 28054-1748 PAT MCCRORY DONALD R. VAN DER VAART fr„ , S. JAY ZIMMERMAN Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) Maintenance Inspection Dear Ms. McMurray: Enclosed is a report for the inspection performed on July 15, 2016 by Jason Smith. 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 21-1.0800. 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 (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 #210 LABORATORY NAME: ADDRESS: NPDES PERMIT #: CERTIFICATE #: DATE OF INSPECTION: TYPE OF INSPECTION: AUDITOR(S): LOCAL PERSON(S) CONTACTED: INTRODUCTION: • • : ' • City of Gastonia — Crowders Creek Laboratory 5642 South York Highway Gastonia, NC 28052 NC0074268, NC0006033, NC0020184, NC0020052 and NC0068888 210 July 12 and 15, 2016 Commercial Maintenance Jason Smith, Todd Crawford, Gary Francies, Nick Jones, Anna Ostendorff, Tonja Springer and Beth Swanson Annette McMurray and David Shellenburger 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: The facility has all the equipment necessary to perform the analyses. Laboratory personnel communicate well with sample collectors and coordinate sample analyses effectively to manage workload and holding times. Staff were forthcoming and seemed eager to adopt necessary changes. All required Proficiency Testing (PT) samples have been analyzed and the laboratory has fulfilled its PT requirements for the 2016 PT calendar year. Contracted analyses are performed by Shealy Environmental Services, Inc. (Certification # 329). Current Approved Procedure documents for the analysis of the facility's currently certified Field parameter methods were provided at the time of the inspection. 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 within 1 year of this report. 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 Page 2 #210 City of Gastonia — Crowders Creek Laboratory 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". 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. III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS: Documentation A. Finding: Process control samples are not clearly identified. 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 laboratory understands which samples are process control based on the sample naming system. However, it is not apparent to outside observers. This caused confusion during the inspection because they were often mixed in with compliance samples and it appeared that some QC elements were not being performed at the required frequency. The laboratory acknowledged the issue and agreed that they would take steps to more clearly identify and segregate process control samples to reduce ambiguity. B. Finding: Units of measure are not consistently documented. 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: • Chain of Custody — pH • Eagle Road Field Analysis benchsheet — Total Residual Chlorine units were incorrectly labeled as mg/L instead of pg/L (the laboratory submitted a benchsheet with the correct units of measure on July 22, 2016) Page 3 #210 City of Gastonia — Crowders Creek Laboratory ® Nitrogen, Ammonia benchsheet — initial pH, final pH and temperature (the laboratory submitted a benchsheet including all units of measure on July 22, 2016) C. Finding: Several omissions and transcription errors in the laboratory's traceability system were noted during the inspection. 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 media, solids and bacteria filters, etc. are included in this requirement. Ref: NC WW/GW LC Policy. Comment: The following omissions were noted: ® Date that disposable sample bottles were put into use ® All traceability for monitoring well field analyses ® Date reagents are put in use for pretreatment field analyses Comment: The following transcription errors were noted: ® Lot number of MFC medium in media preparation log (the laboratory submitted a corrected media preparation log on July 22, 2016) ® Lot number of petri dishes in consumables testing log (the laboratory submitted a corrected consumables testing log on July 22, 2016) General Laboratory Comment: The laboratory is checking the balance with five weights daily. The laboratory may reduce this to one weight daily and three weights quarterly as allowed in North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (K). Proficiency Testing D. Finding: Proficiency Testing samples for field parameters are not analyzed by the personnel responsible for routine analyses. 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. Requirement: Laboratories shall also ensure that PT samples are equally distributed among personnel trained and qualified for the relevant tests, which represent the routine operation of the work group at the time the PT study is conducted. Ref: Proficiency Testing Requirements, February 20, 2012, Revision 1.2. Page 4 #210 City of Gastonia — Crowders Creek Laboratory Bacteria — Coliform Fecal — SM 9222 D-1997 (MF) (Aqueous) Bacteria — Coliform Fecal — SM 9222 D-1997 (MF) 24hr 503 (Non -Aqueous) Recommendation: It is recommended that the colonies per 100 mL be calculated on the benchsheet for all dilutions, even if they will not be used to calculate the final result. This allows the analyst to monitor results for abnormal counts. Recommendation: It is recommended that a column be added to the benchsheet for the reported results. Recommendation: It is recommended that an identifier be added to the benchsheet to indicate which method of calculation of results is used. Recommendation: The laboratory only duplicates effluent samples, which often have no colonies. It is recommended that duplicate analyses be randomized to include all sample types in order to get more meaningful precision data. Recommendation: The laboratory currently determines the acceptance of new consumable materials by calculating the RPD between each dilution and then averaging the RPD values. It is recommended that the acceptance be determined by averaging the colony counts of the old and new materials and determining the RPD of these two values. Recommendation: If the previous recommendation is not implemented, it is recommended that the Consumable Testing form be clarified to indicate that the acceptance criterion is based on the average RPD of the samples. Based upon the current form, it appears some individual RPD results are unacceptable (i.e., >20%); however, the acceptance is based on the average of all RPD values rather than each individual RPD value. Recommendation: The duplicate acceptance criterion for plates with fewer than twenty colonies is ± 5 CFU and the acceptance criterion for plates with twenty or more colonies is 20% RPD. It is recommended that the benchsheet indicate which duplicate acceptance criterion is used to determine acceptability. Comment: The time filtration begins was not documented. Standard Methods, 9222 D-1997. (2) (d) states: Place all prepared cultures in the water bath within 30 min after filtration. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (A) states: 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. This is considered pertinent data in order to demonstrate that the samples were incubated within thirty minutes of filtration. Notification of acceptable corrective action (i.e., the benchsheet was updated to include analysis start time and it is now being recorded) was received by email on July 22, 2016. No further response is necessary for this Finding. Comment: The pH of prepared media was being checked prior to sterilization rather than after sterilization. Standard Methods, 9020 B-2005. (5) 0) (1) states: Check and record pH of a portion of each medium after sterilization. Notification of acceptable corrective action (i.e., the SOP and laboratory procedure were updated July 21, 2016 to check the pH of the media after sterilization) was received by email on July 22, 2016. No further response is necessary for this Finding. Comment: Media was not being stirred during preparation. Standard Methods, 9020 B-2005. (5) Q) (1) states: Stir media, particularly agars, while heating. Notification of acceptable corrective action (i.e., the SOP and laboratory procedure were updated July 21, 2016 to include stirring the media when it is heated) was received by email on July 22, 2016. No further response is necessary for this Finding. Page 5 #210 City of Gastonia — Crowders Creek Laboratory Comment: The pH of the stock phosphate buffer solution (K2HPO4) was not being checked to determine if it needed to be adjusted. Standard Methods, 9050 C-2006. (1) (a) (1) states: adjust to pH 7.2 ± 0.5 with 1N sodium hydroxide. Notification of acceptable corrective action (i.e., the SOP and laboratory procedure were updated on July 21, 2016 to include checking the pH prior to sterilization and adjusting it if needed) was received by email on July 22, 2016. No further response is necessary for this Finding. Comment: The phosphate buffer and magnesium chloride buffer solutions were not being sterilized after preparation. Standard Methods, 9050 C-2006. (1) (a) (1) states: Stock phosphate buffer solution — Sterilize by filtration or autoclave. Standard Methods, 9050 C-2006. (1) (a) (2) states: Magnesium chloride stock solution — Sterilize and store stock solution under refrigerated conditions. Notification of acceptable corrective action (i.e., the SOP and laboratory procedure were updated on July 21, 2016 to include autoclaving the phosphate and magnesium chloride buffer solutions) was received by email on July 22, 2016. No further response is necessary for this Finding. Comment: The phosphate buffer and magnesium chloride buffer solutions were not being refrigerated. Standard Methods, 9050 C-2006. (1) (a) (1) states: Stock phosphate buffer solution — Store stock solution under refrigerated conditions and discard if turbidity develops. Standard Methods, 9050 C-2006. (1) (a) (2) states: Magnesium chloride stock solution — Sterilize and store stock solution under refrigerated conditions, discarding if solution becomes turbid. Acceptable corrective action (i.e. the stock solutions were refrigerated and laboratory staff indicated that this requirement would be maintained) was performed by the laboratory and approved by the auditor during the inspection. No further response is necessary for this Finding. Comment: A culture positive was not being analyzed with each batch of prepared media. NC WW/GW LC Policy states: 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 (e.g., color, shape, size, surface appearance). Notification of acceptable corrective action (i.e., positive cultures will be analyzed with each batch of medium effective July 22, 2016) was received by email on July 22, 2016. No further response is necessary for this Finding. Comment: The laboratory voluntarily has third shift personnel record the temperature of the Fecal incubator at night. This recording was regularly outside of the acceptable range of 44.5 ± 0.2 °C. It was determined that third shift personnel were reading the temperature off of the incubator, which is off by 0.5 °C, rather than the thermometer in the incubator. The temperature readings would have been acceptable if obtained from the correct thermometer. Standard Methods, 9222 D-1997. (2) (d) states: Place prepared dishes in waterproof plastic bags or seal, invert, and submerge petri dishes in water bath, and incubate for 24 ± 2 h at 44.5 ± 0.2 'C. Notification of acceptable corrective action (i.e., third shift personnel were provided additional training and will no longer record this temperature effective July 22, 2016, only verify that the incubator is functioning properly) was received by email on July 22, 2016. No further response is necessary for this Finding. Comment: The laboratory measures sample volume with graduations on the funnel, but has not verified the accuracy of the graduations. Standard Methods, 9020 B-2005. (4) (k) states: When volumetric graduation marks are used to measure sample volumes, check accuracy of graduation marks initially using a Class A graduated cylinder or volumetric pipet. Record results. Notification of acceptable corrective action (i.e., the funnels were checked on July 20, 2016 and marked appropriately if inaccurate) was received by email on July 22, 2016. No further response is necessary for this Finding. Page 6 #210 City of Gastonia — Crowders Creek Laboratory Comment: Plate count comparisons were not being performed. Standard Methods, 9020 B-2005. (9) (a) states: Analyst colony counting variability. 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. Notification of acceptable corrective action (i.e., plate count verifications are being performed beginning July 21, 2016 and a form was created to document the results) was received by email on July 22, 2016. No further response is necessary for this Finding. Comment: The sterility of the bottles was not being verified and the Certificate of Analysis documenting sterility of each lot was not being maintained. The laboratory uses purchased sterilized sample containers. NC WW/GW Policy states: Minimally test for sterility one sample bottle per batch sterilized in the laboratory, or at a set percentage such as 1 to 4%. This is performed by adding sterile dilution/rinse water to the bottle after sterilization and then subsequently analyzing it as a sample. Document results. If sample bottles or bags are purchased pre -sterilized, verification of sterilization is not required if the laboratory maintains copies of the Certificate of Analysis from the vendor. Acceptable corrective action (i.e. Certificate of Analysis documents were obtained from the manufacturer and the laboratory will maintain them for each lot of sample boftles) was performed by the laboratory and approved by the auditor during the inspection. No further response is necessary for this Finding. E. Finding: The Phosphate Buffer and Magnesium Chloride solutions in use were beyond the laboratory established expiration date. Requirement: Adherence to manufacturer expiration dates is required. Chemicals/reagents/ consumables exceeding the expiration date can no longer be considered reliable. If the expiration is only listed as a month and year (with no specific day of the month), the last day of the month will be considered the actual date of expiration. Monitor materials for changes in appearance or consistency. Any changes may indicate potential contamination and the item should be discarded, even if the expiration date is not exceeded. If no expiration date is given, the laboratory must have a policy for assigning an expiration date. If no date received or expiration date can be determined, the item should be discarded. Ref: NC WW/GW LC Policy. Comment: The method does not specify the shelf life of the solutions, but states that the solutions must be discarded if they become turbid. The laboratory assigned expiration dates were March and April 2016, respectively. The solutions were not turbid at the time of the inspection so the laboratory may want to consider establishing expiration dates that will allow them to be used for longer periods of time. F. Finding: The incubator water level was below the immersion line of the partial immersion thermometer. 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: "User -Friendly Guidance on the Replacement of Mercury Thermometers", bg2� //vjww eta gov�sites/ rod€�ction/filesl2015- 10/documents/nistuserfriendly uide. df. Page 7 #210 City of Gastonia — Crowders Creek Laboratory Comment: The water was at the proper level on July 12, 2016; however, by July 15, 2016 it had dropped well below the immersion line. The analyst stated that the incubator is refilled on Mondays. It appears that the incubator needs to be refilled occasionally during the week to maintain the appropriate water level. Recommendation: In order to refill the incubator without affecting the temperature, it is recommended that the water be preheated to the appropriate temperature before filling. G. Finding: The laboratory does not document the use of heat indicating tape on the autoclave log. Requirement: Use heat -indicating tape to identify supplies and materials that have been sterilized. Ref: Standard Methods 9020 B-2005. (4) (h). 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: NCAC 15A NCAC 2H .0805 (a) (7). H. Finding: The laboratory is not maintaining copies of Certificates of Analysis of the purchased dilution water. Requirement: 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. 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 is kept on file. 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: NCAC 15A NCAC 2H .0805 (a) (7). BOD —Standard Methods, 5210 B-2001 (Aqueous) I. Finding: The laboratory is not seeding all samples over six hours old. Requirement: Some samples (for example, some untreated industrial wastes, disinfected wastes, high -temperature wastes, wastes having pH values less than 6 or greater than 8, or wastes stored more than 6 h after collection) do not contain a sufficient microbial population. Seed such samples by adding a population of suitable microorganisms. Ref: Standard Methods 5210 B-2001. (4) (d). Comment: The laboratory is currently seeding samples that are held overnight, but not other samples greater than 6 hours old which are analyzed on the same day as collection. COD — Hach 8000 (Aqueous) Comment: The laboratory is analyzing a second source standard. This is not required since the laboratory uses a verified factory curve and all standards prepared by the laboratory are considered second source to the original factory calibration. Page 8 #210 City of Gastonia — Crowders Creek Laboratory Comment: The benchsheet includes a statement that an annual five -point curve verification is performed. However, this is not performed because the laboratory now performs a daily three-point verification. This statement needs to be removed or updated to indicate current practice. Comment: The COD reaction vials were not being inverted while still warm. The Hach Water Analysis Handbook, Method 8000, Reactor Digestion Procedure, Step 11 states: Invert each vial several times while it is still warm. Notification of acceptable corrective action (i.e., the vials are now inverted while still warm after digestion) was received by email on July 22, 2016. No further response is necessary for this Finding. Comment: The MS recovery formula was not properly adjusted for dilution caused by the spike solution volume being >1% of the total sample volume. NC WW/GW LC Policy states: If the spike solution volume constitutes >1% of the total sample volume, the sample concentration or spike concentration must be adjusted by calculation. Notification of acceptable corrective action (i.e., the MS percent recovery formula was modified to adjust for the dilution of the sample caused by the spike solution on July 22, 2016) was received by email on July 22, 2016. No further response is necessary for this Finding. Comment: The laboratory's calibration verification standard was not mid -range. The laboratory was analyzing a 250 mg/L standard; however, this was not mid -range since the curve goes up to 1000 mg/L. NC WW/GW LC Policy states: The calibration blank and calibration verification standard mid -ran e) 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. Notification of acceptable corrective action (i.e., the concentration of the calibration verification standard concentration was changed on July 22, 2016 to 500 mg/L which is mid -range) was received by email on July 22, 2016. No further response is necessary for this Finding. Comment: Samples with concentrations greater than the largest calibration verification point were reported without dilution. The vials state that they are for concentrations up to 1500 mg/L; however, the curve is only verified up to 1000 mg/L. Samples >1500 mg/L were diluted properly as required. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (1) states: For analytical procedures requiring analysis of a series of standards, the concentrations of these standards must bracket the concentration of the samples analyzed. Notification of acceptable corrective action (i.e., the SOP has been clarified regarding this requirement and samples are now properly diluted as required) was received by email on July 22, 2016. No further response is necessary for this Finding. J. Finding: A blank and mid -range standard are 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. Comment: The laboratory replied to this Finding on July 22, 2016 indicating that this requirement is being met when non-compliance samples are taken into account and that the SOP already requires this. However, Sections 9.2 and 9.3 of the revised SOP submitted July 22, 2016 still do not indicate that a blank and mid -range standard are analyzed after every ten samples. The SOP still states that they are analyzed initially and at the end of the sample set. Page 9 #210 City of Gastonia — Crowders Creek Laboratory e ature of the Comment: Since drift may occur excluded from beingrdless of countedfor thins this requirement when non-compliance n they a e samples are not e analyzed together with compliance samples. Comment: Some of the data submitted after the inspection for other parameters (e.g., NOx) had all of the non-compliance samples analyzed after all compliance samples. When samples are analyzed in this manner, the frequency of calibration blank and calibration verification standard analysis will only apply to the compliance samples. Color. ADMI — Standard Methods, 2120 E-1993 (ADMI) (Aqueous) Comment: The true value and acceptance criterion of the second source standard was not documented on the benchsheet. The true value of quality control samples and percent recovery obtained must be documented on the benchsheet and evaluated against established acceptance criteria to demonstrate that the analyst was aware of any out -of -control situation. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) states: 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. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (F) states: Any time quality control results indicate an analytical problem, the problem must be resolved and any samples involved must be rerun if the holding time has not expired. Notification of acceptable corrective action (i.e., the benchsheet was modified on July 22, 2016 to include the true value and acceptance criterion of the second source standard) was received by email on July 22, 2016. No further response is necessary for this Finding. Comment: The sample volume wasn't documented on the benchsheet. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (H) states: 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. Notification of acceptable corrective action (i.e., the benchsheet was modified and put into use on July 22, 2016 to include the sample volume) was received by email on July 22, 2016. No further response is necessary for this Finding. Mercu — EPA 245.1, Rev. 3.0, 1994 (Aqueous) Comment: The laboratory is analyzing the second source standard at the end of the analytical batch. This is not required. Recommendation: The laboratory currently only lists the initial Instrument Performance Check called a Clthat oCalibration l otherlPC (orCCS) result bdocumnted on tth s summary Standard or CCS by Ise laboratory) on t he QC summary sheet. t. It is recommended sheet as well. Recommendation: It is recommended that the blank results be added to the QC summary sheet. Recommendation: It is recommended that QC acceptance criteria be added to the QC summary sheet. K. Finding: Sample pH values are verified to be <2 S.U. at least 16 hours prior to digestion, but this is not documented. Requirement: Each laboratory shall develop and maintain a document outlining the analytical quality control practices used for the parameters included in their certification. Page 10 #210 City of Gastonia — Crowders Creek Laboratory Supporting records shall be maintained as evidence that these practices are being effectively carried out. 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: NCAC 15A NCAC 21-1.0805 (a) (7) and NCAC 15A NCAC 21-1.0805 (a) (7) (A). L. Finding: The calibration blank is being digested. Requirement: The calibration blank must contain all reagents in the same concentrations and in the same volume as used in preparing the calibration solutions. The laboratory reagent blank (LRB) is prepared in the manner as the calibration blank except the LRB must be carried through the entire sample preparation scheme. Ref: EPA Method 245.1, Rev. 3.0 (1994), Sections 7.11.1 and 7.11.2. M. Finding: The calibration standards are being digested. Requirement: Prepare calibration standards by transferring 0.5, 1.0, 2.0, 5.0, and 10 mL aliquots of the 0.1 pg/mL CAL (Section 7.6) to a series of sample containers (Section 6.5.2). Dilute the standard aliquots to 100 mL with reagent water (Section 7.2) and process as described in Sections 11.1.2, 11.1.3 (without heating), and 11.1.5. These solutions contain 0.05-1.0 pg of Hg. (Other appropriate calibration standards, volumes, and ranges may also be used.) Ref: EPA Method 245.1, Rev. 3.0 (1994), Section 11.2.2. N. Finding: The second source standard is being digested. Requirement: The QCS must be obtained from an outside source different from the standard stock solution, but prepared in the same manner as the calibration solutions. Ref: EPA Method 245.1, Rev. 3.0 (1994), Section 7.13. Comment: The second source standard is called a QCS in the method and Outside Check Sample (OCS) by the laboratory. O. Finding: The Instrument Performance Check (IPC) is being digested. Requirement: Instrument performance check (IPC) solution - For all determinations the laboratory must analyze the IPC solution (Section 7.12) and a calibration blank immediately following each calibration, after every 10th sample (or more frequently, if required) and at the end of the sample run. Analysis of the IPC solution immediately following calibration must verify that the instrument is within ±5% of calibration. Subsequent analyses of the IPC solution must be within ±10 % of calibration. If the calibration cannot be Ref: EPA Method 245.1, Rev. 3.0 (1994), Section 9.3.4. Comment: The laboratory calls the IPC a CCS. Comment: Since the purpose of the IPC (or CCS) is to verify instrument performance and monitor for drift, it does not get digested since the calibration standards are not digested. P. Finding: The laboratory is not using the correct amount of Sodium Chloride — Hydroxylamine Sulfate solution. Requirement: When the samples are at room temperature, to each container, add 6 mL of NaCI-(NH2OH)2H2SO4 solution (Section 7.9) to reduce the excess permanganate. Ref: EPA Method 245.1, Rev. 3.0 (1994), Section 11.1.5. Page 11 #210 City of Gastonia — Crowders Creek Laboratory Requirement: Sodium chloride-hydroxylammonium chloride solution - Dissolve 12 g of NaCl and 12 g of hydroxylamine hydrochloride (NH2OH-HCI) in 100 mL reagent water. (Hydroxylamine sulfate (NH2OH)2-H2SO4 may be used in place of hydroxylamine hydrochloride.) Ref: EPA Method 245.1, Rev. 3.0 (1994), Section 7.9. Comment: The laboratory uses reduced sample volumes of 20% of the method requirement. The laboratory is currently adding 0.6 mL of Sodium Chloride - Hydroxylamine Sulfate solution, but needs to be using 1.2 mL. Mercu - EPA 1631 E (Aqueous) Recommendation: The highest standard concentration in the calibration curve is 100 ng/L and the true value of the QCS is 96 ng/L. It is recommended that the QCS concentration be closer to the mid -range of the calibration curve. The analyst indicated that they would begin diluting the QCS standard to bring it closer to the mid -point of the curve at the time of the inspection. Metals - EPA Method 200.8, Rev. 5.4, 1994 (Aqueous) Comment: The percent recovery of the LFM was documented on the benchsheet; however, the result of the LFM was not documented to show how the percent recovery was obtained. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) states: 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. Notification of acceptable corrective action (i.e., obtained value of the LFM is now being documented) was received by email on July 22, 2016. No further response is necessary for this Finding. Nitrogen, Nitrate - (NO3 + NO2 SM 4500 NO3 F-2000) - (NO2 SM 4500 NO3 F-2000) (Aqueous) Nitrogen, Nitrite - Standard Methods, 4500 NO3- F-2000 (Aqueous) Comment: Data reviewed for July and September 2015 did not include LFMD analyses. Standard Methods, 4020 B-2009. (2) (g) states: When appropriate for the analyte (Table 4020:1), include at least one LFM/LFMD daily or with each batch of 20 or fewer samples. Table 4020:1 indicates that this is required for this parameter. Notification of acceptable corrective action (i.e., an LFMD has been analyzed daily with each batch of 20 or fewer samples beginning November, 2015) was received by email on July 22, 2016. No further response is necessary for this Finding. Nitrogen, Total Kieldahl - Standard Methods, 4500 NoRc C-1997 (SM 4500 NH3 G-1997) (Aqueous) Comment: LFM recoveries were not being properly calculated. The laboratory was calculating the accuracy of the LFM and LFMD using the average of the two values. Improper calculation resulted in LFM results being deemed acceptable when they would have been unacceptable if calculated properly. This was noted on August 5, 2015 and December 17, 2015. Standard Methods, 1020 B- 2011. (7) and (8) state: Evaluate the results obtained for LFMs for accuracy or percent recovery. Evaluate LFM duplicate results for precision and accuracy. Notification of acceptable corrective action (i.e., a statement that beginning July 19, 2016, LFM recoveries are now being calculated individually instead of averaged to calculate) was received by email on July 22, 2016. No further response is necessary for this Finding. Comment: Duplicate results for samples analyzed on August 5, 2015 were unacceptable and the results were not qualified. NC WW/GW LC Policy states: 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 Page 12 #210 City of Gastonia — Crowders Creek Laboratory 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. Notification of acceptable corrective action (i.e., the analyst responsible for the data is no longer employed by the facility as of September 2015, but the laboratory acknowledged that the results should have been qualified and stated their intent to continue monitoring QC results and qualifying data when required) was received by email on July 22, 2016. No further response is necessary for this Finding. Comment: Data qualifiers for the previous two comments have been submitted to NC Division of Water Resources (DWR). Comment: Some instances of more than ten samples being analyzed between blanks and calibration standards were noted. NC WW/GW LC Policy states: 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. Notification of acceptable corrective action (i.e., the analyst responsible for the samples is no longer employed by the facility as of September 2015 and the current analyst has been meeting this requirement) was received by email on July 22, 2016. No further response is necessary for this Finding. Nitrogen, Nitrate — (NO3 + NO2 SM 4500 NOs" F-2000) - (NO2 SM 4500 NOa' F-2000) (Aqueous) Nitrogen, Nitrite — Standard Methods, 4500 NO3 F-2000 (Aqueous) Nitrogen, Total Kieldahl — Standard Methods, 4500 NORG C-1997 (SM 4500 NH3 G-1997) (Aqueous) Comment: Acceptance criteria had not been established for standards that are back calculated. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) states: 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. Notification of acceptable corrective action (i.e., acceptance criteria of ±20% for the reporting limit standard and ±10% for all other standards that are back calculated was established and implemented July 22, 2016) was received by email on July 22, 2016. No further response is necessary for this Finding. Phosphorus, Total — Standard Methods, 4500 P E-1999 (Aqueous) Comment: The percent recovery of the second source standard was not calculated and documented on the benchsheet. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) states: 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. Notification of acceptable corrective action (i.e., the percent recovery of the second source standard is now being calculated and documented on the benchsheet) was received by email on July 22, 2016. No further response is necessary for this Finding. Comment: The laboratory was analyzing a sample duplicate instead of an MSD. Standard Methods, 4020 B-2009. (2) (g) states: When appropriate for the analyte (Table 4020:1), include at least one LFM/LFMD daily or with each batch of 20 or fewer samples. Table 4020:1 indicates that this is required for this parameter. Notification of acceptable corrective action (i.e., an LFMD is being analyzed daily with each batch of 20 or fewer samples) was received by email on July 22, 2016. No further response is necessary for this Finding. Page 13 #210 City of Gastonia — Crowders Creek Laboratory Phosphate, Ortho - Standard Methods, 4500 P E-1999 (Aqueous) Phosphorus, Total - Standard Methods, 4500 P E-1999 (Aqueous) Comment: Standards were not back calculated after calibration. Standard Methods, 4020 B-2009. (2) (a) states: Back calculate the concentration of each calibration point. The back -calculated and true concentrations should agree within ± 10%. Notification of acceptable corrective action (i.e., standards are now being back calculated after calibration with acceptance criteria of ± 20% for the reporting limit standard and ± 10% for all other standards) was received by email on July 22, 2016. No further response is necessary for this Finding. Residue, Suspended -Standard Methods, 2540 D-1997 (Aqueous) Comment: The thermometer used in the Suspended Residue oven has a correction of +5 °C. NC WW/GW LC Policy states: The thermometer/meter readings must be less than or equal to 1 °C from the NIST certified or NIST traceable thermometer reading. Notification of acceptable corrective action (i.e., two new thermometers were ordered and a thermometer with a correction of -1 °C was put into use on July 20, 2016) was received by email on July 22, 2016. No further response is necessary for this Finding. Residue, Total - Standard Methods, 2540 B-1997 (Aqueous) Comment: The laboratory maintains certification for this parameter voluntarily since compliance samples are not being analyzed. Recommendation: It is recommended that samples be evaporated at 103-105 °C to prevent splattering. This is required if the laboratory analyzes any compliance samples. Vector Attraction Reduction - Option 1: Reduction in Volatile Solids Q. Finding: The benchsheet indicates that the acceptable reduction in volatile solids is 37% Requirement: Under this option, reduction of vector attraction is achieved if the mass of the volatile solids in the sewage sludge is reduced by at least 38% during sludge treatment. Ref: Control of Pathogens and Vector Attraction in Sewage Sludge, EPA/625/R-92/013, July 2003, Section 6.2. Comment: At the time of the inspection, the SOP also listed the acceptance criteria as 37%. The laboratory submitted a corrected SOP on July 22, 2016 but has not submitted a corrected benchsheet. Field Analyses - Temperature - Standard Methods, 2550 B-2000 (Aqueous) Recommendation: The SWR Precision in Discharge Monitoring Reports document recommends that Temperature results be rounded to whole numbers for reporting purposes-. This document was emailed to the laboratory on September 22, 2016. Field Analyses - General Comment: The correlation coefficient had not been calculated for the most recent Total Residual Chlorine curve verification for Crowders Creek, Long Creek, Eagle Road, and the pretreatment program. The NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine (TRC) document states: The overall correlation coefficient of the curve must be >-0.995. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) states: Supporting records shall be maintained as evidence that these practices are being effectively carried out. Notification of Page 14 #210 City of Gastonia — Crowders Creek Laboratory acceptable corrective action (i.e., a statement that completion of the calculations was still pending at the time of the inspection and submission of the completed form including the correlation coefficient for each facility) was received by email on July 22, 2016. No further response is necessary for this Finding. Recommendation: The laboratory currently verifies the TRC meter calibration curve at the following concentrations: 20, 50, 100, 200 and 400 pg/L. It is recommended that the laboratory verify the TRC meter calibration curves using the following concentrations: 20, 40, 50, 200 and 400 pg/L. This is recommended because most sample concentrations are <50 lag/L, the Division of Water Resources effluent compliance limit. R. Finding: Original records of all analyses are not being maintained for all facilities. 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: Some field personnel record data on a note and discard the note after transferring to a benchsheet. Field Analyses — Crowders Creek and Long Creek Recommendation: The benchsheet includes the following statement regarding sample collection and analysis: "Performed on location, together, by the operator and completed within 10 minutes." The analyst clarified that the reference to 10 minutes was to indicate the approximate time it takes for the meters to stabilize. It is recommended that this statement be updated to: "samples are analyzed immediately upon collection." Analysis time is considered the beginning of analysis and it is understood that it may take a short time for the meter to stabilize. Field Analyses — McAdenville Comment: The sample collection and analysis time was not clearly documented for Temperature. The NC WW/GW LC Approved Procedure for the Analysis of Temperature document states: The following must be documented in indelible ink whenever sample analysis is performed: Date and time of sample collection; Date and time of sample analysis. Notification of acceptable corrective action (i.e., the benchsheet was updated and put into use on July 22, 2016 with the following statement: The collection and analysis time is the same for pH and Temperature) was received by email on July 22, 2016. No further response is necessary for this Finding. Field Analyses — Pretreatment Recommendation: For pH, the values obtained for the check buffers are recorded in the "Comments" column. It is recommended that the benchsheet be updated to clearly label calibration buffers and check buffers. S. Finding: The sample collection and analysis time is not clearly documented for pH, DO and Temperature. Requirement: The following must be documented in indelible ink whenever sample analysis is performed: Date and time of sample collection; Date and time of sample analysis to verify the 15-minute holding time is met. Alternatively, one time may be documented for collection and analysis with the notation that samples are measured in situ or immediately at the sample site: Ref: NC WW/GW LC Approved Procedure for the Page 15 #210 City of Gastonia — Crowders Creek Laboratory Analysis of Dissolved Oxygen and NC WW/GW LC Approved Procedure for the Analysis of pH. Requirement: The following must be documented in indelible ink whenever sample analysis is performed: Date and time of sample collection; Date and time of sample analysis - Alternatively, since EPA requires samples to be analyzed immediately, one time may be documented for collection and analysis with the notation that samples are measured in situ or immediately at the sampling site (i.e., immediately following collection at a location as near to the collection point as possible). When this `one time' option is used, state that the documented time is both collection and analysis time. Ref: NC WW/GW LC Approved Procedure for the Analysis of Temperature. T. Finding: The benchsheet was lacking pertinent data: Instrument identification for DO and Temperature. Requirement: The following must be documented in indelible ink whenever sample analysis is performed: Instrument Identification, Ref: NC WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen and NC WW/GW LC Approved Procedure for the Analysis of Temperature. Comment: The DO meter is identified by model. However, the same model is also used at other locations. The meter must be assigned a unique identifier to be able to determine which meter is used in each location. U. Finding: The calibration elevation is not documented for DO. 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, slope, or % efficiency. Ref: NC WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen. Field Analyses — Monitoring Wells V. Finding: The benchsheet was lacking pertinent data: Instrument identification for pH, DO, Conductivity, and Temperature. Requirement: The following must be documented in indelible ink whenever sample analysis is performed: Instrument Identification. 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 Specific Conductance (Conductivity) and NC WW/GW LC Approved Procedure for the Analysis of Temperature. W. Finding: The sample analysis time is not clearly documented for pH, DO, Conductivity, and Temperature. Requirement: The following must be documented in indelible ink whenever sample analysis is performed: Date and time of sample analysis to verify the 15-minute holding time is met. Ref: NC WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen and NC WW/GW LC Approved Procedure for the Analysis of pH. 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. Page 16 #210 City of Gastonia — Crowders Creek Laboratory Requirement: The following must be documented in indelible ink whenever sample analysis is performed: Date and time of sample analysis to verify the 28 day holding time is met. Ref: NC WW/GW LC Approved Procedure for the Analysis of Specific Conductance (Conductivity). Comment: Alternatively, one time may be documented for collection and analysis with the notation that samples are measured in situ or immediately at the sample site. X. Finding: The calibration of the pH and Conductivity meters is not documented on the benchsheet. Requirement: The following must be documented in indelible ink whenever sample analysis is performed: Meter calibration and meter calibration time(s). Ref: NC WW/GW LC Approved Procedure for the Analysis of pH and NC WW/GW LC Approved Procedure for the Analysis of Specific Conductance (Conductivity). Requirement: The following must be documented in indelible ink whenever sample analysis is performed: True values of buffers used for calibration; True value for the check standard buffer; Value obtained for the check standard buffer (verification of ± 0.1 S.U.); True value and value obtained for the post analysis calibration verification(s), where applicable. Ref: NC WW/GW LC Approved Procedure for the Analysis of pH Requirement: The following must be documented in indelible ink whenever sample analysis is performed: True value of the standard used for calibration; True value of the calibration verification check standard; Value obtained and time analyzed for the check standard (verification of ± 10% recovery); True value and value obtained for the post analysis calibration verification(s), where applicable. Ref: NC WW/GW LC Approved Procedure for the Analysis of Specific Conductance (Conductivity). Comment: Documentation of calibration may be on another form, but it must be documented in a manner to link it to the meter being calibrated. Y. Finding: The Automatic Temperature Compensator (ATC) of the Conductivity meter has not been verified. Requirement: The ATC must be verified annually (i.e., every twelve months) and the process documented. The ATC must be verified by analyzing a standard at 25 °C (the temperature that conductivity values are compensated to) and a temperature(s) that brackets the temperature ranges of the samples to be analyzed. This may require the analysis of a third temperature reading that is > 25 'C. Ref: NC WW/GW LC Approved Procedure for the Analysis of Specific Conductance (Conductivity). Comment: Laboratory personnel indicated that this was performed as required; however, documentation of the verification could not be located at the time of the inspection. IV. PAPER TRAIL INVESTIGATION: The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks, etc.) and contract lab reports to Discharge Monitoring Reports (DMRs) submitted to the North Carolina Division of Water Resources. Data were reviewed for Crowders Creek WWTP (NPDES permit # NC0074268) for July, 2015 and Long Creek WWTP (NPDES permit # NC0020184) for Page 17 #210 City of Gastonia — Crowders Creek Laboratory December, 2015. 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: Jason Smith Date: September 9, 2016 Report reviewed by: Beth Swanson Date: September 14, 2016