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HomeMy WebLinkAbout#192_1013_FINALINSPECTION REPORT ROUTING SHEET To be attached to all inspection reports in-house only. Laboratory Cert. #: 192 Laboratory Name: Charlotte Water- Environmental Laboratory Services Inspection Type: Commercial Maintenance Inspector Name(s): Beth Swanson, Gary Francies, Jason Smith, Dana Satterwhite, Nick Jones, Tonia Springer Todd Crawford 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 Linda: Date Mailed: 10/13/2015 and 11 /5/2015 1 /05/2016 1 /05/2015 Tonia Springer January 12, 2016 ❑ Insp. Initial ❑ Insp. No Finding ❑ Corrected Gary Francies 1/14/2015 2/15/2016 2/15/2016 ® Insp. Reg. ❑ Insp. CP ❑ Insp. Reg. Delay jf �Jr rNtl l Water Resources ENVIRONMENTAL QUALITY February 15, 2016 192 Ms. Rhonda Hutson Charlotte Water- Environmental Laboratory Services 4222 Westmont Drive Charlotte, NC 28217 PAT MCCRORY DONALD R. VAN DER VAART S 'I'i'[1111 S. JAY ZIMMERMAN Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) Maintenance Inspection Dear Ms. Hutson: Enclosed is a report for the inspection performed on October 13 and November 5, 2015 by Beth Swanson, Gary Francies, Dana Satterwhite, Todd Crawford, Jason Smith, Nick Jones, and Tonja Springer. I apologize for the delay in getting this report to you. Where Finding(s) are cited in this report, a response is required. Within thirty days of receipt, please supply this office with a written item for item description of how these Finding(s) were corrected. Please describe the steps taken to prevent recurrence and include an implementation date for each corrective action. If the Finding(s) cited in the enclosed report are not corrected, enforcement actions may be recommended. For certification maintenance, your laboratory must continue to carry out the requirements set forth in 15A NCAC 2H .0800. 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: ADDRESS: CERTIFICATE #: DATE OF INSPECTION: TYPE OF INSPECTION: AUDITOR(S): LOCAL PERSON(S) CONTACTED: I. INTRODUCTION: • 4Mt Charlotte Water- Environmental Laboratory Services 4222 Westmont Drive Charlotte, NC 28217 192 October 13, 2015 and November 5, 2015 Commercial Maintenance Beth Swanson, Gary Francies, Dana Satterwhite, Todd Crawford, Jason Smith, Nick Jones, and Tonja Springer Rhonda Hutson 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. GENERAL COMMENTS: The laboratory facility is impressive. It is spacious, well laid out, and has all the equipment necessary to perform the analyses. Laboratory personnel were knowledgeable and forthcoming and operate within a professional culture that focuses on quality data. The laboratory is to be commended on its efforts to stay current with changes in NC WW/GW LC program requirements. Contracted analyses are performed by Pace Analytical Services, Inc. - Huntersville (Certification #12) and Prism Laboratories, Inc. (Certification #402). The laboratory is reminded that all changes made in response to the Findings, Recommendations or Comments listed in this report must be incorporated in the Quality Assurance (QA)/Standard Operating Procedures (SOP) document(s). The laboratory must ensure the method is being performed as stated, references to methods are accurate, and the QA and/or SOP document(s) is/are in agreement with approved practice and regulatory requirements. In some instances, the laboratory may need to create a SOP to document how new functions or policies will be implemented. Proficiency Testing samples have been analyzed for all certified parameters for the 2015 calendar year and the graded results were 100% acceptable. 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. Page 2 #192 Charlotte Water- Environmental Laboratory Services III. FINDINGS,_ REQUIREMENTS, COMMENTS AND RECOMMENDATIONS: Documentation A. Finding: There are instances where error correction is not properly performed (i.e., the correction was not initialed and dated). 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. B. Finding: Some reagents and consumables are not traceable from analysis to manufacturer. 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: Consumables such as pH buffers, Total Suspended Residue filters and Fecal Coliform filters are not fully traceable. Some reagents used to adjust sample pH during analysis are also not traceable (e.g., H2SO4 and NaOH used in SM 4500 Cl- B-1997, Rev. 2011). The date opened or put into use is not recorded on the receiving log with the rest of the required information and lot numbers were not recorded on the benchsheet. Employing either of those options will provide acceptable traceability. C. Finding: Method references are incomplete or incorrect on benchsheets, supporting documentation and /or SOPs. 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: Laboratory Procedures. 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). Comment: Following are examples of where incomplete or incorrect method references can be found. This list may not be all inclusive. The Chlorophyll a validation record references EPA 445.0, without the revision number (i.e., Rev. 2.1). The Chlorophyll a benchsheet does not have a method reference listed. Page 3 #192 Charlotte Water- Environmental Laboratory Services • The Color, PC validation worksheet and visual comparison worksheet list the method reference as SM 2120B, 20th instead of the full method reference including approval year (i.e., Standard Methods, 2120 B-2001, Rev. 2011). • The Fluoride benchsheet does not contain the approval year (i.e., 1997, Rev. 2011). • The Nitrogen, Nitrate benchsheet references QuikChem Method 10-107-04-1-L, which is the Nitrate + Nitrite method. The correct reference is QuikChem Method 10-107-05-1-A. • The Oil and Grease benchsheet does not include the revision (i.e., Rev. B). • The Organic Carbon, Total benchsheets have the method reference listed as SM 5310 C- 11. It needs to reference the full method approval year of SM 5310 C-2000, Rev. 2011. • The Residue, Suspended benchsheet references SM 2540 D-11. It needs to reference the full method approval year of SM 2540 D-1997, Rev. 2011. • The Residue, Dissolved benchsheet references SM 2540 C-11. It needs to reference the full method approval year of SM 2540 C-1997, Rev. 2011. • The Residue, Total benchsheet and Quality Control (QC) worksheet reference SM 2540 B-11. It needs to reference the full method approval year of SM 2540 B-1997, Rev. 2011. • The Phosphorus, Total benchsheets for May and August, 2015 data reference Standard Methods 4500 P F-1997, which is the not the current method approval year (i.e., 1999).They also reference QuikChem Method, 10-115-01-1-E, which does not correspond to this method. • The Organic Carbon, Total (TOC) SOP references "SM 5310 C-2011 ", not the full Standard Methods approval year (i.e., SM 5310 C-2000, Rev. 2011). • The "Conductivity Measurements with Thermo Orion Meter" SOP and "Conductivity Analysis" SOP reference "SM 2510 B-11 ", not the full Standard Methods approval year (i.e., SM 2510 B- 1997, Rev. 2011). • The Residue, Settleable SOP references "SM 2540 F-11 ", not the full Standard Methods approval year (i.e., SM 2540 F- 1997, Rev. 2011). • The pH SOP references "SM 4500 H+ B -11 ", not the full Standard Methods approval year (i.e., SM 4500 H+ B-2000, Rev. 2011). • The Residue, Suspended SOP references "SM 2540 D -2011", not the full Standard Methods approval year (i.e., SM 2540 D-1997, Rev. 2011). • The Residue, Total SOP references "SM 2540 B -2011 ", not the full Standard Methods approval year (i.e., SM 2540 B-1997, Rev. 2011). • The Residue, Dissolved SOP references "SM 2540 C -2011", not the full Standard Methods approval year (i.e., SM 2540 C-1997, Rev. 2011) D. Finding: The units of measure are not documented on all 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. 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: Following are some examples of where units were lacking. This list may not be all inclusive. • Units are not documented on the "result" column of the "TSS2" Excel worksheet. • Units are not documented on any columns of the "percent TS/TVS" worksheet. • Units are not documented on any columns of the "TS3/TVS" worksheet. • Units are not documented for Final Result (i.e., mg/L), initial and final buret readings (i.e., mL) and pH (i.e., S.U.) on the Chloride (SM 4500 Cl- B-1997) benchsheet Page 4 #192 Charlotte Water- Environmental Laboratory Services Units are not documented for pH (i.e., S.U.) on the Color worksheet. Units are not documented for the results (i.e., mg/L ) on the HEM Excel worksheet Units are not documented for pH (i.e., S.U.) on the Hexane Extractable Material (HEM) worksheet. Quality Control Comment: For Standard Methods methods that require a Laboratory Fortified Blank (LFB), Standards Methods suggests varying the concentration of the standard between the middle and lower part of the calibration range, including the reporting limit. E. Finding: The laboratory does not have an acceptance criterion for the Conductivity cell constant. Requirement: Any quality control procedures required by a particular approved method shall be considered as required for certification for that analysis. Ref: 15 NCAC 2H .0805 (a) (7) (D). Requirement: It is satisfactory for most samples when the cell has a constant between 1 and 2 cm -1. Ref: Standard Methods, 2510 B- 1997, Rev. 2011. (3) (b). Comment: Each analysis day, the laboratory compares the new cell constant to the previous one, but there is no acceptance criterion for this comparison. F. Finding: All analytical results for effluent samples are not being reported. Requirement: The results of all tests on the characteristics of the effluent, including but not limited to NPDES permit monitoring requirements, shall be reported on the monthly report forms. Ref: 15A NCAC 2B .0506 (b) (3) (J). Comment: The laboratory does not average duplicate values for reporting, assuming that only the first value is an analytical result and the second is a quality control result. When an effluent sample is used as a duplicate, the results must be averaged or both reported. Note that pH values cannot be averaged, which is why duplicates are not recommended or required for Field Parameters. Proficiency Testing G. Finding: The preparation of Proficiency Testing (PT) samples is not always 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 the Total Residual Chlorine PT would satisfy the documentation requirement. The PT instructions for TOC were retained, but they were not initialed and dated to show the instructions were followed. Standard Operating Procedure Recommendation: It is recommended that all SOPs be reviewed at least every two years and the review date documented in the revision history if no changes are necessary. Page 5 #192 Charlotte Water- Environmental Laboratory Services Recommendation: The Dissolved Residue SOP states that the reporting limit is 25 mg/L but does not state that this is only for sample volumes of 100 mL. It is recommended that this be stated as well as how to adjust the reporting limit for other volumes. Recommendation: It is recommended that the make and model of the analytical instrument be added to the Cyanide SOP. Recommendation: It is recommended that all SOPs with a calibration curve include in the reporting/detection limit definition the statement that the concentration is equivalent to the low standard concentration. Recommendation: It is recommended that the NO2 + NO3 SOP more clearly describe how pH adjustments are made to samples. Recommendation: It is recommended that the Oil and Grease SOP define the nomenclature of the extraction methods used as indicated on the benchsheet (i.e., LLE and SPE). Recommendation: It is recommended that the Oil and Grease SOP include language about allowable method modification as found in the method. Recommendation: It is recommended that Section 7.10 of the Oil and Grease SOP detailing the preparation of the Hexadecane/Stearic Acid solution include a statement about what would happen if the solution is not allow to cool or is vigorously shaken. Recommendation: It is recommended that the Oil and Grease SOP include a definition of "split 2X" and "2X", which are found on the Excel worksheet and analysis worksheet, respectively. Recommendation: It is recommended that the Oil and Grease SOP include definitions of the LIMS headers (e.g., HEM_1, HEM_INIT, HEM_E, etc.). Recommendation: It is recommended that Section 15.2 of the Oil and Grease SOP include the appropriate comment that this listed on the benchsheet and in LIMS when MS recovery does not meet the requirement. Also, state who documents the comment (i.e., the analyst). Recommendation: It is recommended that the Purgeable, Organics SOP more clearly state when an MSD versus sample duplicate will be analyzed. Recommendation: It is recommended that the TOC SOP be reviewed for items which are required versus recommended and clearly state each. Recommendation: It is recommended that the TOC SOP state that the blank acceptance criterion is <_1/2 the reporting limit instead of <0.25 mg/L in case the reporting limit is changed. The current reporting limit is 0.5 mg/L, so it is technically correct. Recommendation: It is recommended that Section 9.8 of the TOC SOP state that the MS is randomly selected from a routine sample. Recommendation: It is recommended that the word "greater than" replace "of' in Section 4.5 of the TOC SOP. The sentence reads "Chloride concentration of 0.05%, oxidation of organic matter may be inhibited completely". Page 6 #192 Charlotte Water- Environmental Laboratory Services Recommendation: It is recommended that the TOC SOP include direction on what to do if samples are received with gross solids or insoluble matter (i.e., homogenize according to the method). The checklist indicated that no samples of this nature have been received at this time. Recommendation: It is recommended that the SOP include a note that if ascorbic acid is used for mitigating oxidizers at collection, the holding time is reduced to 24 hours. Also, sodium thiosulfate may be used in place of ascorbic acid to mitigate oxidizers without reducing hold time. This issue has not yet been encountered. Recommendation: Section 25.1 of the QAM states the rules for manual rounding but also states that this is different for results in an Excel spreadsheet. This would create an inconsistency and it is recommended that if a number is to be reported, that the Excel spreadsheet include all significant digits and the analyst manually round the final result using the same rules as specified in Section 25.1. Comment: The TOC SOP states that an MDL is required. This is not required by NC WW/GW LC since the method itself does not require an MDL. Comment: The sample preservation and storage temperature requirements may be changed in accordance with 40 CFR Part 136.3 Table II in all pertinent SOPs and in practice. The current practice is to store "at 40C". 40 CFR Part 136.3 Table II allows <_6°C for most inorganic parameters and <10°C for bacterial tests, without evidence of freezing. Comment: The Anion and Fluoride (Standard Methods 4500 F- C-1997, Rev. 2011) SOPs state that the blank must be < Y2 of the reporting limit. NC WW/GW LC Policy allows <_ 1/ the reporting limit. Comment: The Nitrogen, Ammonia SOP needs to include the make and model of the flow injection analysis instrument since the SOP is specific to this piece of equipment. Comment: Section 9.3.1 of the combined NO3 + NO2 and NO2 SOP appears to contain an error. "Analyst" should be "analytes". Comment: The COD SOP notes that the digested samples must be analyzed within 24 hours. A specific time limit is not mentioned in the method, but it is inferred that they are analyzed as soon as the vials have cooled. Comment: The Quality Assurance Manual (QAM) references DENR, which is now called DEQ (Department of Environmental Quality). H. Finding: An inconsistency and/or omission was noted between the Standard Operating Procedure (SOP) or Quality Assurance Manual (QAM) and laboratory practice as follows (observations are listed for each): General o SOPs are intended to describe procedures exactly as they are to be performed. All SOPs need to be reviewed and evaluated for use of the word "should". While some uses of the word "should" versus "must" are noted in this Finding, not all have been listed. o The SOPs state that a J value is associated with data which are reported between the reporting limit and MDL. The SOPs do not state for which data J values are allowed and that the data would be labeled as "estimated". o The SOPs do not list the demonstration of capability criteria or reference where it can be found. Page 7 #192 Charlotte Water- Environmental Laboratory Services o SOPs that include a description of the Linear Dynamic Range (LDR) state that the LDR is established when the highest calibration standard is less than 10% below the known concentration. It needs to also state that the calibration standard is less than 10% above the known concentration (i.e., ±10% of the known value). NC WW/GW LC Policy states that LDRs are not required. o Many SOPs (e.g., Nitrogen, Ammonia) stated that the blank must be ±50% instead of 550% the reporting limit. o SOPs need to reference the QAM where applicable for definitions and procedural descriptions. This would include references to such things as glassware washing procedures, pH meter calibration, sample preservation, ASTM Type 1 water, etc. Residue, Settleable — Standard Methods, 2540 F-1997, Rev. 2011 o Section 4.0 states that large floating particles should not be estimated. This needs to be clarified. Chlorine, Total Residual — Standard Methods, 4500 Cl G- 2000, Rev. 2011 o Section 9.4 of the Low Level SOP does not state that a reagent blank is required each day standards are prepared. o Section 9.2 of the Low Level SOP and 9.1 of the Hach Pocket SOP describe a Minimum Detection Limit (MDL) procedure, which is not being done. An MDL study is not required for this parameter. o Section 10.2 of the Hach Pocket SOP, in the section titled "Annual Standard Curare Verification for Factory Set Curve", does not describe analyzing the 5 prepared standards and reagent blank. o Sections 10.19.1 and 10.21.1 of the Hach Pocket SOP, state that the reporting limit standard recovery must be ± 20%. NC WW/GW LC Policy requires that any standards greater than 50 ug/L must have a recovery of ± 10% of the true value. Reviewed data shows that the daily reporting limit standard's observed concentration is generally 0.21 mg/L and the benchsheet shows a recovery criterion of ± 10% for all standards. o Section 10.20.1 of the Hach Pocket SOP states that 3 standards and a reagent blank are prepared, but the daily practice is to analyze 3 Gel ® standards. Conductivity — Standard Methods, 2510 B- 1997, Rev. 2011 o Section 2.1 of the "Conductivity Measurements with Thermo Orion Meter" SOP states that anything below the reporting limit is qualified. It does not state how the result is qualified or how the value is reported (e.g., < the lowest standard concentration). The "Conductivity Measurements with Thermo Orion Meter" SOP was not completed. The sections from 6.0 forward appear to belong to another parameter's SOP. o Section 9.3 of the "Conductivity Analysis" SOP states that the Laboratory Control Standard (LCS) is mid -level, however, the LCS standard is 100 umhos/cm, which is not mid -level Dissolved Oxygen — Standard Methods, 4500 O G-2001, Rev. 2011; ASTM D 888-09 C (LDO) o The SOP only describes the LDO procedure. The SOP needs to include the electrode method or create a separate SOP for Standard Methods O G- 2001, Rev. 2011. o Section 10.5.26 and 14.1 state that the water saturated air check should confirm with the chart value but does not describe acceptance criteria. NC WW/GW LC Approved Procedure requires that it agree within ± 0.5 mg/L. o Section 10.5 does not state how often the calibration is performed. The NC WW/GW LC Approved Procedure document requires calibration each day compliance samples are analyzed. Page 8 #192 Charlotte Water- Environmental Laboratory Services pH — Standard Methods, 4500 H+ B-2000, Rev. 2011 o The SOP contains incorrect values in multiple places for the accuracy of standards. The accuracy is stated as 0.10 S.U. in the SOP and 0.1 S.0 on the calibration benchsheet. Residue, Suspended — Standard Methods, 2540 D-1997, Rev. 2011 o The SOP requires a method blank, which is not analyzed in practice. Method blanks are not required by the method. o The SOP states that laboratory prepared filters are dried only once but does not state that a dry filter blank is analyzed or give its acceptance criterion. Residue, Total — Standard Methods, 2540 B-1997, Rev. 2011 o Section 3.1 of the SOP incorrectly states that the samples are dried in a 96°C oven rather than 103-105°C. o Sections 9.2.2 and 14.2 of the SOP state that the method blank "should not exceed ±0.0005g of original weight". A method blank is not required, but if an acceptance criterion is listed, it needs to be stated as "must". o The directions in Section 11.3.8 incorrectly reference Sections 11.3.2-11.3.5. o Section 14.3 of the SOP states the Relative Percent Difference (RPD) of the duplicate should be 510%. The rest of the SOP states it must be. o Section 15.4 of the SOP states a different RPD limit from Section 14.3. • Residue, Dissolved — Standard Methods, 2540 C-1997, Rev. 2011 o Sections 11.5.8 and 12.4 of the SOP contradict each other over the proper number if significant figures for reporting. • Residue, Total Volatile— Standard Methods, 2540 G-1997 o There is no SOP for this method. Cyanide — Lachat 10-204-00-1-X, Rev. 2.2, 2005 (Total) o The SOP does not state how the instrument software constructs the curve (i.e., absorbance vs concentration). o The SOP does not define "minimum level" in regards to the blank acceptance criterion in Section 9.5.2. If it is synonymous with reporting limit, the acceptance criterion is incorrect. NC WW/GW LC Policy states that blank acceptance must be 5 '/2 the reporting limit. o The SOP does not specify which standards are used in the wastewater versus drinking water curves (i.e., no 25 ug/L standard is used in the drinking water curve). Anions — EPA 300.0, Rev. 2.1, 1993 o The standard preparation table in Section 7.4 contains two errors (i.e., the IC2 mixed standard requires 500 pL of chloride stock and the IC3 mixed standard requires 1000 pl- of chloride stock). o The SOP does not state that the retention time is monitored and must not vary by more than ±10% from the calibration value. o Section 8.2 of the SOP does not state that polyethylene collection containers are required if Fluoride is requested. o Section 14.8 of the SOP states that the duplicate RPD must be < 20%. An RPD acceptance criterion of :520% is used in practice. • Color, PC — Standard Methods, 2120 B-2001, Rev. 2011 o The SOP does not reflect the current calibration curve concentrations (i.e., 5, 10, 15, 20, 25, 30, 35, 40, 45, 50, 60, 70 c.u.). Page 9 #192 Charlotte Water- Environmental Laboratory Services o The SOP does not reflect the current LCS concentration (i.e., 35 c.u.). o The SOP does not include the filter assembly in the equipment list. o The SOP contains references to an MDL, which is not relevant to this parameter. • Fluoride —Standard Methods, 4500 F- C-1997, Rev. 2011 o Section 14.8 of the SOP incorrectly states that the criterion for duplicate RPD is ±10% instead of :510%. Chloride — Standard Methods, 4500 Cl- B-1997, Rev. 2011 o The SOP incorrectly states that the RPD for duplicates must be ±10% while the criterion used is <_10%. o The SOP does not state which blank (i.e., first one) is used to calculate results. Nitrogen, Ammonia — Standard Methods, 4500 NH3 H-1997, Rev. 2011 o The SOP does not describe in detail the filtration of samples when particulates, color, or turbidity are present. o The interference section in both the analysis and distillation SOPs do not contain the detail required for all applicable interferences and their mitigation (e.g., cyanate, urea, color, TRC, etc.) o The distillation SOP does not state the frequency of the LCS standard in Section 9.3. o The distillation SOP incorrectly states that the 0.04N H2SO4 is prepared in the laboratory. It is purchased commercially prepared. o The distillation SOP has an error in Sections 7.10 and 7.11. It incorrectly states that the sodium tetraborate is 0.25M instead of 0.025M. o The SOP does not clearly distinguish between distillation method blanks and analytical method blanks. o The SOP does not state which standards are primary and which are secondary source standards. o The SOP does not state that in cases where samples must be filtered, that the method blank and LFB must also be filtered. NOTE: The laboratory has not yet needed to filter samples. o Section 14.6 of the SOP needs the phrase "at least one daily" added when referring to the frequency of the matrix spike and matrix spike duplicate (MS/MSD). • Alkalinity —Standard Methods, 2320 B-1997, Rev. 2011 o The SOP states that an Initial Demonstration of Capability (IDOC) should be performed by each analyst before the method is used by that analyst. An IDOC is required by each new analyst per Standard Methods 2020 B- 2010. (1) (a). • Oil and Grease — EPA 1664 Rev. B o The SOP does not describe the pH verification procedure (i.e., checking the sample lid). Organic Carbon, Total — Standard Methods, 5310 C-2000, Rev. 2011 o The SOP does not include preparation instructions for the MS/MSD. o The SOP does not dictate that the LFM/LFMD concentration be rotated in the low to middle range to verify performance at various levels as stated in Standard Methods, 5020 B-2000. (2) (g). No Compliance samples had been analyzed at the time of inspection. Page 10 #192 Charlotte Water- Environmental Laboratory Services Nitrogen, Total Kjeldahl — EPA 351.2, Rev. 2.0, 1993 o The SOP does not state that the approved method has been modified. 40 CFR Part 136.6 (b) states that the method user's SOP must clearly document the modifications made to the reference method. The modifications include but may not be limited to: ® Section 7.7 of the SOP says to use 0.5 g of sodium nitroprusside for preparing 500 mL of Salicylate Nitroprusside. For 500 mL, the method requires 0.15 g. ® Section 7.8 of the SOP, describing the preparation of buffer solution, merges Sections 7.7 and 7.8 of the method, but the ratios used are incorrect. ® Section 11.6 of the SOP does not specify that the second heating must be maintained at 3800C for at least 30 minutes as stated in 11.5 of the method. ® Section 11.7.4 of the SOP states that the manifold heater is set at 60°C, but the method diagram shows that it needs to be set at 37°C. However, the SOP does state that the diagram is built to meet Lachat Method 10- 107-06-2-H. COD — Hach 8000 o Analysts are not following the calculation stated in Section 12.13 of the SOP for MS/MSD recoveries. The calculation being used is [spk/((sample*0.75)+50)]100. The resulting recoveries are approximately 1 % different from those produced using the calculation stated in the SOP. Chlorophyll a — EPA 445.0, Rev. 1.2 (Fluorometric) o The SOP states that the filtration vacuum pressure should not exceed 6 in. Hg, instead of listing a requirement. Nitrogen, NO3 + NO2 and Nitrogen, NO2 — EPA 363.2, Rev. 2.0, 1993 o The SOP is a combined SOP for both NO3 + NO2 and NO2, but some procedures in the SOP would not apply to both and it is not specified to which parameter they apply. Specifically, Section 7.13.1 states that the ammonium chloride buffer is adjusted to 8.5 pH with 15N sodium hydroxide solution, which is acceptable for NO2 but not NO3+NO2. o The SOP does not state that the method blank is treated like a sample, including addition of all reagents added to samples. o The SOP does not state that the approved method has been modified. 40 CFR Part 136.6 (b) states that the method user's SOP must clearly document the modifications made to the reference method. It appears the SOP is written to follow Lachat QuikChem Method 10-107-04-1-L.The modifications include but may not be limited to: ® The SOP states that in the preparation of the color reagent, 1g of N-1- naphthylethylenediamine dihydrochloride is added, but the method states to add 2g. Base Neutral/Acid, Organics — EPA 625 and SW846 8270 D o The SOP does not define how many samples are in a batch. Many QC elements have a frequency of "per batch", so it is not clearly evident that the QC frequency is acceptable. Purgeable, Organics — EPA 624 and SW846 8260 B o The SOP does not state that when the unfortified sample result is in the top 40% or the calibration range, that the sample is diluted before adding spike solution for MS analysis. Page 11 #192 Charlotte Water- Environmental Laboratory Services o The SOP does not define how many samples are in a batch. Many QC elements have a frequency of "per batch", so it is not clearly evident that the QC frequency is acceptable. o The SOP does not always clearly state that the surrogate is added to both samples and standards. o The SOP does not contain the acceptance criterion for the method reporting limit standard (i.e., ± 50% recovery). Metals — EPA 200.7, Rev. 4.4, 1994 o Section 9.5 of the SOP states that a blank should be analyzed at the end of analysis. This is required by the method. o The SOP QC table lists the blank acceptance criterion as 2.2 times the analyte MDL or <1/ reporting limit. Only <1/z the reporting limit is used in practice. Metals — EPA 200.8, Rev. 5.4, 1994 o The SOP QC table lists the blank acceptance criterion as 2.2 times the analyte MDL or <1/2 reporting limit. Only <% the reporting limit is used in practice. o The SOP QC table lists the frequency of the QCS as "quarterly to verify calibration or to meet QC needs". It is analyzed daily so the SOP needs to be update to reflect current practice. Mercury — EPA 245.1, Rev. 3.0, 1994 o The laboratory utilizes two distinct instruments called FIMS and CETAC for Mercury analysis and each instrument has its own SOP. Both SOPs state in Section 9.7 that the ICB/CCB should always be <MDL, and do not include a required acceptance limit. o The QC table of both SOPs is missing the acceptance criterion for the ICB. o Both SOPs state the LRB acceptance criterion as <2.2 times the MDL or 10% of the reporting limit. In practice, <Y2 the reporting limit is used. Section 9.3.1 of the method states: 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. o The CETAC SOP states that the reporting limit standard acceptance criterion is ±10%. An acceptance criterion of ±20% is used in practice and is stated throughout the rest of the SOP. Chromium Hexavalent —Standard Methods, 3500-Cr-B-2009 o Section 9.9 of the SOP states that the laboratory should spike, in duplicate, 5% of samples. Standard Methods, 3020 B-2005. (2) (h) requires a minimum of one LFM/LFMD for every 20 samples. o The SOP does not specify that the NC WW/GW LC Policy blank acceptance criterion of <_1/z the reporting limit is used in place of subtracting blanks. • Vector Attraction Reduction- Option 1, Option 2, Option 3 o There are no SOPs for these methods. The applicable options could be included in one of the residue SOPs. • QAM o Section 20.9 does not include the use of heat indicating tape in each use of the autoclave for microbiological parameters. Page 12 #192 Charlotte Water- Environmental Laboratory Services o Section 23.4 does not state that when external customers submit a compliance sample with collection, preservation, or hold time issues and choose to have it analyzed after notification of the infraction, the laboratory must notify NC WW/GW LC of the infraction in addition to qualifying the sample. 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). Please respond in writing stating that the SOPs and QAM will be revised to address the items in this Finding by February 15, 2017. Bacteria- Coliform Fecal — Standard Methods, 9222 D-1997 Comment: The laboratory was using the incorrect amount of MgC12 • 61­112O when preparing the Magnesium Chloride Stock Solution. It was being prepared with 81.2 g MgC12 • 61­112O per liter. Standard Methods, 9050 C-2006. (1) (a) (2) states: Add magnesium chloride (38 g/L MgC12 or 81.19 MgC12 • 61-12O) to 1 L reagent -grade water. Acceptable corrective action (i.e., a new batch of magnesium chloride stock solution was prepared with 81.1 g MgC12 • 61­112O listed as the recipe in the preparation log) was performed and observed by the inspector to be adequate on the second day of the inspection, November 5, 2015. No further response is necessary for this Finding. I. Finding: A monthly recount of a positive plate by a single analyst is not being conducted. 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 B-2005. (9) (a). Comment: The laboratory was conducting a monthly comparison count between analysts but not a recount by the same analyst. Bacteria- E. coli — Colilert-180 (MPN) Bacteria- Enterococci — Enterolert® IDEXX Comment: The laboratory was not analyzing true duplicates. A 100mL volume and whatever volume was left over (usually 20 mL) were being analyzed and called a duplicate instead of analyzing two dilutions of the same volume. 15A NCAC 02H .0805 (a) (7) (C) states: Except for Oil and Grease (EPA Method 413.1), settleable solids or where otherwise specified in an analytical method, 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. Acceptable corrective action (i.e., the SOP was updated to include analysis of two 50 mL dilutions and the new procedure was implemented) was performed by the laboratory and observed by the inspector to be adequate on the second day of the inspection, November 5, 2015. No further response is necessary for this Finding. BOD — Standard Methods, 5210 B-2001, Rev. 2011 BOD — Standard Methods, 5210 B-2001 (ASTM D 888-09 C) (LIDO) J. Finding: The laboratory is not analyzing the Glucose Glutamic Acid (GGA) standard at a 2% dilution. Page 13 #192 Charlotte Water- Environmental Laboratory Services Requirement: Together with each batch of samples, check seed effectiveness and analytical technique by using procedures in 5210B.5 to make BOD measurements on an equal weight mixture of glucose and glutamic acid as follows: Add sufficient amounts of standard glucose- glutamic acid solution (5210B.3h) to -give 3.0 mq glucose/L and 3.0 mq glutamic acid/L in each of three test bottles (20 mL GGA solution/L seeded dilution water, or 6.0 mL/300-mL bottle). Commercial solutions may contain other glucose-glutamic acid concentrations; adjust doses accordingly. Ref: Standard Methods, 5210 B- 2001. (6) (b). Requirement: Glucose-glutamic acid solution: Dry reagent -grade glucose and reagent -grade glutamic acid at 103°C for 1 h. Add 150 mg glucose and 150 mg glutamic acid to distilled water and dilute to 1 L. Prepare fresh immediately before use unless solution is maintained in a sterile condition. Store all glucose-glutamic acid mixtures at 40C or lower. Commercial preparations may be used but concentrations may vary. Ref: Standard Methods, 5210 B- 2001. (3) (h). Comment: The laboratory was using a commercial preparation (i.e., Hach) and adding 3 mL because the product they were using was twice as concentrated. However, this preparation does not result in 2% GGA standard per bottle. EPA Region IV has stated that commercial product with a different concentration of GGA is OK to use, but the concentration must be adjusted prior to setting up. That is, it must be diluted by half with lab water, not BOD dilution water, before adding to the BOD sample bottles. Chloride —Standard Methods, 4500 Cl- B-1997, Rev. 2011 Recommendation: It is recommended that a negative sign be added to CI (i.e., CI-) on all benchsheets and the SOP to distinguish it from chlorine. K. Finding: The laboratory is using greater than 10% spike to sample ratio to prepare MS. Requirement: The volume of spike solution used in MS preparation must in all cases be 5 10% of the total MS volume. It is preferable that the spike solution constitutes <_ 1 % of the total MS volume so that the MS can be considered a whole volume sample with no adjustment (i.e., volume correction) by calculation necessary. If the spike solution volume constitutes >1 % of the total sample volume, the sample concentration or spike concentration must be adjusted by calculation. Ref: NC WW/GW LC Policy Comment: There was only PT data to review and the laboratory has only recently begun analyzing a MS for this parameter. The MS is being prepared by spiking 50 mL of 50 mg/L standard into 50 mL of sample. The result was correctly being adjusted by calculation, however the 50% ratio does not meet the above requirement. Anions (CI-, F-, SOa, NO2, NOs, NO3+NO2) — EPA 300.0, Rev. 2.1, 1993 L. Finding: The LRB and LFB are not filtered when filtered samples are analyzed. Requirement: Laboratory Reagent Blank (LRB) -- An aliquot of reagent water or other blank matrices that are treated exactly as a sample including exposure to all glassware, equipment, solvents, reagents, and surrogates that are used with other samples. The LRB is used to determine if method analytes or other interferences are present in the laboratory environment, the reagents, or the apparatus. Ref: EPA 300.0, Rev. 2.1, 1993. Section 3.8. Requirement: Laboratory Fortified Blank (LFB) -- An aliquot of reagent water or other blank matrices to which known quantities of the method analytes are added in the laboratory. The LFB is analyzed exactly like a sample, and its purpose is to determine whether the methodology is in Page 14 #192 Charlotte Water- Environmental Laboratory Services control, and whether the laboratory is capable of making accurate and precise measurements. Ref: EPA 300.0, Rev. 2.1, 1993. Section 3.6. Chlorophyll a — EPA 445.0, Rev. 1.2 (Fluorometric) Recommendation: It is recommended that the filtration vacuum pressure be documented on the filtration bench record and the centrifuge speed and time be documented on the benchsheet. Recommendation: It is recommended that the column on the analytical benchsheet titled "Extraction Factor (Dilution of Concentration) Multiplier" be updated to better reflect the calculation process. The factors recorded in the column are concentration factors, and they are used to divide the raw concentration, not multiply. Chromium Hexavalent — Standard Methods, 3500-Cr-B-2009 Comment: The laboratory is using the method provided by the Lachat instrument manufacturer, which does not include the same reagents and color development steps as the method on the laboratory's Certified Parameters Listing. There is no documentation in the SOP that the modifications to the approved method meet the criteria laid out in 40 CFR Part 136.6 (b) (1) which requires that the underlying chemistry and determinative technique in a modified method are essentially the same as an approved Part 136 method.... Please submit documentation showing these modifications are allowed by 40 CFR Part 136.6 for NPDES reporting purposes. COD — Hach 8000 Comment: Duplicates (i.e., MSD) are being analyzed at a 10% frequency. The method and NC WW/GW LC Rules only require a 5% frequency. Comment: The laboratory is having each analyst create their own user curve annually. The factory -set curve can be verified annually and used by all analysts. Recommendation: It is recommended that method blanks be preserved in the same manner as compliance samples. Color, PC — Standard Methods, 2120 B-2001, Rev. 2011 M. Finding: The benchsheet states the incorrect RPD acceptance criterion for duplicates. 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: 15 NCAC 2H .0805 (a) (7). Comment: The first page of the Color, Visual Comparison Worksheet/Validation Sheet states that the acceptance criterion for duplicates is ±10%, but it needs to be 510%. N. Finding: The sample pH at the time of analysis is not always documented. Requirement: The color value of water is extremely pH -dependent and invariably increases as the pH of the water is raised. When reporting a color value, specify the PH at which color is determined. Ref: Standard Methods, 2120 B- 2001, Rev. 2011. (1) (d). Page 15 #192 Charlotte Water- Environmental Laboratory Services Comment: The laboratory occasionally uses the pH at the time of sample collection when reporting the color value. Since the color value is determined in the lab, measure the pH in the lab at the time of analysis. pH is temperature dependent, so the value will change from the field to the bench. Cyanide — Lachat 10-204-00-1-X, Rev. 2.2, 2005 (Total) Recommendation: It is recommended that the laboratory obtain a copy of Standard Practice for Sampling, Preservation and Mitigating interferences in Water Samples for Analysis of Cyanide, ASTM D7365-09a. Comment: QuikChem Method 10-204-00-1-X recommends establishing limits for the back calculation of calibration standard results. Fluoride — Standard Methods, 4500 F' C-1997, Rev. 2011 Comment: It is recommended that a negative sign be added to F (i.e., F-) on all benchsheets and the SOP to distinguish it as an anion. Comment: The benchsheet contains a place to circle which instrument was used for analysis (i.e., Mettler/Accumet) but this is not consistently being done. Comment: Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012; Table IB requires samples to be distilled. However, footnote 6 states, manual distillation is not required if comparability data on representative effluent samples are on file to show that this preliminary distillation step is not necessary; however, manual distillation will be required to resolve any controversies NC WW/GW Policy recommends that the distilled and undistilled sample portions be analyzed by the same lab, using the same instrument, technology and methodology to minimize uncertainty introduced by the analysis, yielding a truer representation of the effect of matrix and the distillation process on sample results. No compliance samples had been analyzed by the laboratory prior to the inspection. If compliance samples are analyzed, the laboratory is reminded that distillation would be required until sufficient comparison data is obtained showing that the distillation in not needed. Nitrogen, Ammonia —Standard Methods, 4500 NH3 H-1997, Rev. 2011 O. Finding: The laboratory is not evaluating the back calculation of calibration standards against an established acceptance criterion. 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). 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: 15 NCAC 2H .0805 (a) (7). Comment: Residuals are calculated for each calibration point after the curve is constructed, however, no set acceptance criteria are being used to evaluate. The method says they should agree within ±10%, however, a wider acceptance range may be needed for the lowest concentration standard. Be aware that the acceptance criteria need to be set at values where it won't weaken confidence in the data. Page 16 #192 Charlotte Water- Environmental Laboratory Services P. 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). Comment: The laboratory has a distillation comparison study on file and therefore does not routinely distill samples. Nitrogen, Total Kieldahl — EPA 351.2, Rev. 2.0, 1993 Q. Finding: A sample volume adjustment is not being made in the recovery calculation of the MS/MSD. Requirement: The volume of spike solution used in matrix spike preparation must in all cases be <_ 10% of the total matrix spike volume. It is preferable that the spike solution constitutes <_ 1 % of the total matrix spike volume so that the matrix spike can be considered a whole volume sample with no adjustment by calculation necessary. If the spike solution volume constitutes >1% of the total sample volume, the sample concentration or spike concentration must be adjusted by calculation. Ref: NC WW/GW LC Policy. Comment: The laboratory is adding 1 mL of spiking solution to 25 mL of sample, which constitutes a 4% dilution. The unspiked sample concentration needs to be multiplied by 0.96 prior to subtracting it from the spiked sample concentration to adjust for this dilution in the calculation of the percent recovery. The SOP includes the proper calculation. Recommendation: It is recommended that the spike solution constitutes :51 % of the total MS volume. Oil and Grease — EPA 1664 Rev. B Recommendation: It is recommended that the weight checks of the method required weights (i.e., 2 mg and 100 mg) be documented on the benchsheet. The checks are only recorded on the balance logs, so it has to be traced through the times on the balance log and the benchsheet. Residue, Suspended —Standard Methods, 2540 D-1997, Rev. 2011 Residue, Total — Standard Methods, 2540 B-1997, Rev. 2011 Residue. Dissolved — Standard Methods, 2540 C-1997, Rev. 2011 R. Finding: The laboratory does not have a duplicate RPD acceptance criterion for all sample concentrations. 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: 15 NCAC 2H .0805 (a) (7). Requirement: 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. Ref: 15A NCAC 2H .0805 (a) (7) (F). Page 17 #192 Charlotte Water- Environmental Laboratory Services Comment: The laboratory only applies the ±10% RPD acceptance criterion to samples with results 5 times or greater than the reporting limit. There is currently no criterion for samples lower than that range. Other laboratories often choose two -tiered acceptance criteria with a ± mg/L range for low-level samples. Residue, Dissolved — Standard Methods, 2540 C-1997, Rev. 2011 Comment: The laboratory is analyzing a blank daily. Blanks are not required for this method. Comment: The laboratory is analyzing a daily QC check standard. North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (B) only requires the check standard quarterly. Comment: As a reminder, the drying study is used to confirm the minimum amount of time which samples must be dried to be considered at constant weight. For example, the drying study that was reviewed during the inspection had an initial drying time of 1 hour 36 minutes. This means that any samples that are only dried one time have to be dried for at least 1 hour 36 minutes to be considered at constant weight. Not all analysts were aware of this requirement, however, the data reviewed showed drying times that exceeded this minimum. Residue, Suspended — Standard Methods, 2540 D-1997, Rev. 2011 Comment: The laboratory is analyzing a daily QC check standard. North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (B) only requires the check standard quarterly. Metals — EPA 200.7, Rev. 4.4, 1994 Comment: The laboratory is analyzing both MSD and sample duplicates. The MSD is acceptable to satisfy the sample duplicate requirement listed in North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (C). S. Finding: The initial Instrument Performance Check (IPC) solution acceptance criterion does not meet the method specified limit. Requirement: 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. Ref: EPA 200.7, Rev. 4.4, 1994. Section 9.3.4. Comment: The laboratory calls the IPC solution the Continuing Calibration Verification (CCV). The laboratory is using an acceptance criterion of ±10% recovery for all CCVs throughout the analytical run. Chlorine, Total Residual — Standard Methods, 4500 Cl G- 2000, Rev. 2011 Recommendation: It is recommended that the reagent blank value be added to the annual calibration curve verification log instead of going back to the daily calibration log for that date. Recommendation: It is recommended that a stock standard that has a specific known value instead of a concentration range and average, be utilized for making verification and check standards. Comment: A reporting limit standard is not required to be analyzed daily. Comment: An MDL study is not required for this method. Page 18 #192 Charlotte Water- Environmental Laboratory Services Comment: The laboratory was citing Standard Methods, 4500 Cl G-2000 and filtering samples. Standard Methods, 4500 CI G-2000. (1) (b) states: Compensate for color and turbidity by using sample to zero photometer. Acceptable corrective action (i.e., Hach 10014 ULR (which requires sample filtering) was added to the Certified Parameters Listing per the laboratory's request) was completed on January 8, 2016. No further response is necessary for this Finding. Conductivity —Standard Methods, 2510 B-1997, Rev. 2011 Comment: An IDOC and method blanks are not required. Recommendation: It is recommended that the acceptance criterion for the percent recovery of standard concentrations (i.e., ±10% of the standard true value) be added to the Automatic Temperature Compensation (ATC) check log. Comment: The ATC check was being performed improperly. The laboratory was verifying with a standard at room temperature (i.e., approximately 21 °C) instead of 25°C. The NC WW/GW LC Approved Procedure for the Analysis of Specific Conductance (Conductivity) states: The Automatic Temperature Compensator (ATC) must be verified annually (i.e., 12 months) at two temperatures by analyzing a standard or sample at 250C (the temperature that conductivity values are compensated to) and a temperature(s) that brackets the temperature ranges of the environmental samples routinely analyzed. Acceptable corrective action (i.e., ATC checks were completed on all seven conductivity meters with a standard at 25 ± 0.5°C) was performed by the laboratory and observed by the inspector to be adequate on the second day of the inspection, November 5, 2015. No further response is necessary for this Finding. Purgeable, Organics — EPA 624 and SW846 8260 B Comment: Instrument 5973 is having problems with data transfer into Agilent Custom Report, so the lab has not been able to maintain all performance records for QC data in one location. This is not an issue with the other instrument used for analysis and the issue is supposed to be resolved with implementation of the new LIMS system. T. Finding: The laboratory does not collect a preserved sample for benzene, ethylbenzene, or toluene or analyze the unpreserved samples within seven days. Requirement: Cool, <_ 6°C, 0.008% Na2S2O3, HCI to pH 21. Footnote 9: If the sample is not adjusted to pH 2, then the sample must be analyzed within seven days of sampling. Ref: Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012; Table II. Comment: Section 9.3 of EPA Method 624 states: Experimental evidence indicates that some aromatic compounds, notably benzene, toluene, and ethyl benzene are susceptible to rapid biological degradation under certain environmental conditions. Refrigeration alone may not be adequate to preserve these compounds in wastewaters for more than seven days. For this reason, a separate sample should be collected, acidified, and analyzed when these aromatics are to be determined. Collect about 500 mL of sample in a clean container. Adjust the pH of the sample to about 2 by adding 1+1 HCI while stirring vigorously. Check pH with narrow range (1.4- 2.8) pH paper. Page 19 #192 Charlotte Water- Environmental Laboratory Services IV. PAPER TRAIL INVESTIGATION: The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks, etc.) and Discharge Monitoring Reports (DMRs) for TSS for McAlpine Effluent (A-EFF) and McAlpine Influent (A- INF) collected 3/2/2015. Oil and Grease data were reviewed for project number AF30038B. No transcription errors were detected. V. CONCLUSIONS: Correcting the above -cited Findings and implementing the Recommendations will help this lab to produce quality data and meet Certification requirements. The inspector would like to thank the staff for its assistance during the inspection and data review process. Please respond to all Findings and include an implementation date for each corrective action. Report prepared by: Beth Swanson Date: January 5, 2016 Report reviewed by: Tonja Springer Date: January 12, 2016