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HomeMy WebLinkAbout#7_0728_finalTS_2015_ INSPECTION REPORT ROUTING SHEET To be attached to all inspection reports in-house only. Laboratory Cert. #: 7 Laboratory Name: Fayetteville Cross Creek WWTP Lab Inspection Type: Municipal Maintenance Inspector Name(s): Tonja Springer, Dana Satterwhite, Nick Jones Gary Francies, Beth Swanson, Todd Crawford Inspection Date: July 28, 2015 Date Report Completed: October 27, 2015 Date Forwarded to Reviewer: October 27, 2015 Reviewed by: Beth Swanson Date Review Completed: October 29, 2015 Cover Letter to use: Insp. Initial Insp. Reg. Insp. No Finding Insp. CP Corrected Insp. Reg. Delay Unit Supervisor/Chemist III: Dana Satterwhite Date Received: November 4, 2015 Date Forwarded to Linda: December 11, 2015 Date Mailed: December 14, 2015 _____________________________________________________________________ On-Site Inspection Report LABORATORY NAME: Fayetteville Cross Creek WWTP Lab NPDES PERMIT #: NC0023957, NC0050105 and NC0076783 ADDRESS: P.O. Drawer 1089 Fayetteville, NC 28302-1089 CERTIFICATE #: 7 DATE OF INSPECTION: July 28, 2015 TYPE OF INSPECTION: Municipal Maintenance AUDITOR(S): Tonja Springer, Dana Satterwhite, Gary Francies, Beth Swanson, Todd Crawford and Nick Jones LOCAL PERSON(S) CONTACTED: Kim Chavis, Rhonda Locklear, Eugenia Edwards and Dane Reid I. INTRODUCTION: 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 laboratory was clean and well organized. Data was readily available and analysts were knowledgeable and forthcoming. The facility has all the equipment necessary to perform the analyses. Analytical data pertinent to each certified analysis was filed in an orderly manner and was readily available for inspection upon request. The organizational culture of this laboratory is one that focuses on quality of data. Laboratory personnel were accessible to answer questions that arose during the inspection. Everyone we interacted with was interested and willing to adapt their processes to the required and recommended changes. The laboratory is reminded that any time changes are made to laboratory operations; the laboratory must update the Quality Assurance (QA)/Standard Operating Procedure (SOP) document(s). Any changes made in response to the 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 approved practice and regulatory requirements. In some instances, the laboratory may need to create a SOP to document how a new function or policy will be implemented. The laboratory must also take steps to insure that all personnel are aware of the changes made; that they have fully implemented those changes and steps have been taken (e.g., detailed SOPs and guidance documents, documented training and demonstration of proficiency with new procedures, etc.) to prevent recurrence of Findings. Laboratory Fortified Matrix (LFM) and Laboratory Fortified Matrix Duplicate (LFMD) are also known as Matrix Spike (MS) and Matrix Spike Duplicate (MSD) and may be used interchangeably in this report. Contracted analyses are performed by Meritech, Inc. (Certification #165). Page 2 #7 Fayetteville Cross Creek WWTP Lab III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS: Quality Control Recommendation: It is recommended that the laboratory implement a temperature grid check of all block digesters by alternating the well location of the thermometer each time samples are digested. This will document heating uniformity and consistency of all sample wells in the block. A. Finding: The laboratory is not using the manufacturer’s statement of accuracy for micropippetors. Requirement: Mechanical volumetric liquid-dispensing devices (e.g., fixed and adjustable auto- pipettors, bottle-top dispensers, etc.), used for critical measurements, must be calibrated at least twice per year, approximately six months apart and documented. Each liquid-dispensing device must meet the manufacturer’s statement of accuracy. Ref: NC WW/GW LC Policy. Comment: The laboratory is currently calibrating the micropipettes gravimetrically with acceptance criterion of plus or minus 10%. It appears that most readings are 98% or better. Recommendation: It is recommended to use the manufacturer’s acceptance criteria for accuracy, if provided. If the manufacturer does not give an acceptance criterion, it is recommended that the acceptance criterion be based on the laboratory’s calibrations. If most are within 2% or better, the acceptance criterion could be set at 5%. B. Finding: The thermometer for the new residue oven has not been verified against a National Institute of Standards and Technology (NIST) traceable thermometer. Requirement: All thermometers must meet NIST specifications for accuracy or be checked, at a minimum annually, against a NIST traceable thermometer and proper corrections made. Ref: 15A NCAC 2H .0805 (a) (7) (O). Comment: The new residue oven did not have a thermometer inside and the oven’s electronic temperature readout had not been verified against an NIST thermometer. Proficiency Testing C. Finding: The preparation of Total Residual Chlorine (TRC) Proficiency Testing (PT) samples is not documented. Requirement: PT samples received as ampules must be diluted according to the PT provider’s instructions. The preparation of PT samples must be documented in a traceable log or other traceable format. The diluted PT sample becomes a routine environmental sample and is added to a routine sample batch for analysis. Ref: The Proficiency Testing Requirements, February 20, 2012, Revision 1.2. Comment: Dating and initialing the instruction sheet for the preparation of the TRC PT would satisfy the documentation requirement. D. Finding: The laboratory does not have a documented plan for PT procedures. Requirement: Each laboratory shall develop and maintain a document outlining the analytical quality control practices used for the parameters included in their certification. Supporting records Page 3 #7 Fayetteville Cross Creek WWTP Lab shall be maintained as evidence that these practices are being effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7). Requirement: Laboratories must have a documented plan (this is usually detailed in the laboratory’s Quality Assurance Manual) of how they intend to cover the applicable program requirements for proficiency testing per their scope of accreditation. This plan shall cover any commercially available proficiency testing and any inter-laboratory organized studies, as applicable. The laboratory must also be able to explain when proficiency testing is not possible for certain parameters and provide a description of what the laboratory is doing in lieu of proficiency testing. This shall be detailed in the plan. The plan must also address the laboratory’s process for submission of proficiency testing results and related corrective action responses. Laboratory Standard Operating Procedures (SOPs) must address how low level samples will be analyzed, including concentration of the sample or adjustment of the normality of a titrant. These instructions shall be followed when the concentration of a PT sample falls below the range of their routine analytical method. Instructions shall also be included in the laboratory’s SOP for how high level samples will be analyzed, including preparation of multiple dilutions of the sample. These instructions will be followed when the concentration of a PT falls above the range of their routine analytical method. Ref: Proficiency Testing Requirements, February 20, 2012, Revision 1.2. Documentation Recommendation: It is recommended to add an asterisk (*) and statement on the NIST verification log to indicate which thermometers are used for drinking water. Recommendation: It is recommended to include calculation formulas on all benchsheets. Recommendation: It is recommended to include Quality Control (QC) acceptance criteria on all benchsheets. Recommendation: It is recommended to remove the date at the top of the NIST verification log and instead add a column to document the verification dates along with the associated thermometer serial numbers. Recommendation: It is recommended that the laboratory adopt a policy of how to document oven, incubator, and refrigerator temperature readings on the logs so that everyone is documenting the same thing. Temperature readings on the logs are not being documented in a consistent manner. Some analysts are documenting the readings in whole numbers and some are documenting to one decimal place. Recommendation: It is recommended the facility name be documented on laboratory benchsheets. Comment: There were several examples (e.g., observed on benchsheets for Ammonia and Fecal Coliform) where the analyst’s handwriting was difficult to read. This could pose issues with data defensibility and/or transcription errors. E. Finding: Samples are not identified as process control or drinking water samples on the benchsheet. 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). Page 4 #7 Fayetteville Cross Creek WWTP Lab Recommendation: It is recommended to add an asterisk (*) and statement on the benchsheets to indicate which samples are process control and drinking water samples. F. Finding: Sample preservation verification checks are not documented. Requirement: A record of date collected, time collected, sample collector, and use of proper preservatives must be maintained. Each sample must clearly indicate the State of North Carolina collection site on all record transcriptions. Ref: 15 NCAC 2H .0805 (a) (7) (M). Comment: For metal samples, acid must be added at least 24 hours before analysis to dissolve any metals that adsorb to the container walls. If samples are received without preservation, they must then be preserved and the time documented. G. Finding: The temperature correction factor is not always applied, when applicable. Requirement: All thermometers must meet National Institute of Standards and Technology (NIST) specifications for accuracy or be checked, at a minimum annually, against a NIST traceable thermometer and proper corrections made. Ref: 15A NCAC 2H .0805 (a) (7) (O). Comment: The autoclave temperature log has a space to document the temperature correction but it is not being documented. Comment: The older residue oven’s thermometer has been verified against the NIST thermometer. The correction is posted on the thermometer but no correction was applied to the documented temperature reading. Recommendation: It is recommended to put a statement on the temperature log to indicate that temperature corrections, if applicable, are being applied to the temperature readings. H. Finding: The laboratory needs to increase the documentation of purchased materials, consumable materials, and reagents, as well as documentation of standards and reagents prepared in the laboratory. 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: Following are examples of Traceability issues observed. This list may not be complete.  Traceability is not being documented for fecal consumable materials (i.e., media, bacteria filters), pH buffers and conductivity standards. Page 5 #7 Fayetteville Cross Creek WWTP Lab  Date put in use and date opened is not documented in the reagent log. This information is being documented only on the reagent bottle.  Traceability is not being extend to distillation/digestion logs and computer print outs.  Lot numbers for commercially prepared standards used to make laboratory prepared standards are not being documented in the Ammonia Nitrogen reagent preparation log (e.g., stock ammonium chloride solution for Ammonia Nitrogen analyses).  The Total Phosphorus worksheet and Total Phosphorus Curve worksheets do not have lot numbers documented for the ammonium molybdate solution, ascorbic acid solution, 5N sulfuric acid, and each of the chemicals used to make the combined color reagent. I. Finding: Some instances of writing over a number and not always initialing and dating as a means of error correction were observed. 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. Comment: Examples of improper error corrections were observed on benchsheets for Total Phosphorus dated 7/14/2015 and 7/15/2015. J. Finding: Units of measure are not always 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. 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 complete.  Units are not documented for the “1.0 check standard” (i.e., mg/L) on the Total Phosphorus worksheet.  Units are not documented for absorbance (i.e., nm) on the Total Phosphorus calibration curve.  Units are not documented for temperatures (i.e., C) on the PWC Thermometer Calibration Record log.  Units are not documented for the reported value for Fecal Coliform (i.e. CFU/100 mL).  Units are not documented on the Ammonia benchsheet for the QC standard (i.e., mg/L), reported value (i.e., mg/L), probe efficiency (i.e., %) and slope reading (i.e., mv). Page 6 #7 Fayetteville Cross Creek WWTP Lab  Units for temperatures (i.e., C) are not documented on the Temperature logs (i.e. TSS ovens, autoclave) Standard Operating Procedures: Recommendation: It is recommended that all SOPs include all applicable references (e.g., method, manufacturer’s manuals, 40 CFR, etc.). Recommendation: It is recommended that all SOPs include a revision and review history with relevant dates (e.g., effective, review and revision dates) and a brief description of any change(s) made. Recommendation: It is recommended that all SOPs include a definition of all QC terms and acronyms used. Recommendation: It is recommended to revise the Material Safety Data Sheets (MSDS) reference in SOPs to also include the term Safety Data Sheets (SDS), where applicable. Recommendation: It is recommended that the SOPs include catalog numbers for commercially prepared reagents. Recommendation: It is recommended to define what the “zero bottle” is in Section V. A. 5. of the CBOD SOP. Recommendation: It is recommended to remove Section I. B. 1. Grab Samples, in the CBOD SOP if grab samples are not being analyzed. Recommendation: It is recommended that the Temperature SOP define “sand bath” in the Procedures section sentence #1. Recommendation: It is recommended that the Temperature SOP define what is meant by “depending on the requirement” in #1 of the Procedures section. The SOP states, “Report results to the nearest 0.1 ºC or 1 ºC, depending on the requirement.” Recommendation: It is recommended to include in the Temperature SOP, the type of thermometer that is used to take the temperature readings. Recommendation: It is recommended to define “resistant glass” in Section 1C of the CBOD SOP. Recommendation: It is recommended to add the make/model of all the instruments and equipment in the SOPs. Recommendation: It is recommended that the following be added to the Theory Section in the Ammonia SOP at the end of the second sentence: NH3 (aq) diffuses through the membrane and changes the internal solution pH that is sensed by a pH electrode. A chloride ion-selective electrode (ISE) serves as a reference electrode and potentiometric measurements are made with a pH meter or specific ion meter. Recommendation: It is recommended to add the pounds per square inch (psi) equivalents for autoclave operations (i.e., 98-137 kPa is roughly equivalent to 14-20 psi.) to the Total Phosphorus SOP. 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 Page 7 #7 Fayetteville Cross Creek WWTP Lab to store “at 4°C”. 40 CFR Part 136.3 Table II allows ≤6°C for most inorganic parameters and <10°C for bacterial tests, without evidence of freezing. K. Finding: An inconsistency and/or omission was noted between the Standard Operating Procedure (SOP) and laboratory practice as follows (observations are listed for each):  General o The SOPs do not include page numbers (e.g., Ammonia, Fecal Coliform, Nitrate + Nitrite TNT, CBOD, TSS), revision date, lab name, interferences and their mitigation (e.g., Total Residual Chlorine). o The SOPs do not include that when samples are preserved that preservative is also to be added to the Laboratory Control Standard and Method Blanks. o The SOPs do not clearly document how to prepare the Matrix Spike (MS). This is required in order to show that it is being prepared and calculated properly. o All SOPs do not include acceptance criteria for all QC elements (e.g., Method Blanks, Laboratory Fortified Blanks, Matrix Spikes, etc.). o All SOPs do not describe corrective actions for instances where QC fail acceptance criteria. o The SOPs do not include QC calculation formulas (e.g., percent recovery, linear regression, Relative Percent Difference [RPD], dilutions). o The SOPs do not address reporting (e.g., significant figures, rounding, etc.) . o The SOPs do not include a section for sample calculations, dilutions, etc. o SOPs are intended to describe procedures exactly as they are to be performed. Evaluate all SOPS for the proper use of the word “should”.  Organic Carbon, Total – Standard Methods, 5310 B-2000 o The SOP references the 19th Edition of Standard Methods rather than Standard Methods Committee approval year. This Edition does not contain the approved method. o The SOP does not contain a requirement or procedure for analyzing Matrix Spikes.  COD – Standard Methods, 5220 D-1997 o The SOP states that there are three curve ranges analyzed; 0-150 ppm, 0-1500 ppm and 0-15000 ppm. The lab is only analyzing the 0-1500 ppm range. o The SOP does not state that the method blank and calibration verification standard must be preserved like the samples. o The SOP does not include the digestion temperature. o The SOP does not contain detailed instructions for the calibration curve preparation. The SOP does not include what corrective action to take whenever acceptance criteria is not met. o The SOP does not define acceptance criteria for blanks, standards, spikes and duplicates.  Coliform, Fecal – Standard Methods, 9222 D-1997 o The SOP does not include what corrective action to take whenever QC acceptance criteria is not met. o The SOP states that 20-30 mLs of dilution water are used to rinse the funnel. The method specifies that three 20-30 mL portions be used to rinse the funnel. o The SOP does not state that samples are verified to have no total residual chlorine or what to do if total residual chlorine is present. o The SOP does not state that at least two sample dilutions must be analyzed. o The SOP does not state how sample volumes are measured. Page 8 #7 Fayetteville Cross Creek WWTP Lab o The SOP does not state that prepared samples must be placed into the incubator within 30 minutes of filtration. o The SOP does not state how to calculate the density of colony forming units (CFU) (i.e., CFU/100 ml = coliform colonies counted x 100 ) ml sample filtered  CBOD – Standard Methods, 5210 B-2001 o The SOP says nitrification inhibitor is being added separately but the laboratory is actually using seed with inhibitor. o The SOP references the 18th Edition of Standard Methods rather than Standard Methods Committee approval year. This Edition does not contain the approved method. o The SOP states pH is checked after inhibitor is added. The method states to check the pH before the inhibitor is added. o The SOP states, in Section V B. Analytical Procedure, to add one HACH nutrient buffer pillow to any dilution of 250+ mLs of sample. The method states for dilutions with >67 % (>201 mL) add extra nutrients. o The SOP does not state that inhibitor must not be added until the bottle is at least 2/3 full. o The SOP does not state that if pH is adjusted, the sample must not be diluted by more than 0.5%. o The SOP does not state that a dechlorination check must be performed or describe the procedure. o The SOP states in Section 1. B. 1. that thermal preservation is not required if analysis begins within 2 hours of collection. Thermal preservation must be performed unless analysis begins within 15 minutes of collection. o The SOP does not state to set at least 3 dilutions for samples. o The SOP does not state to record the time dilutions are set and the time they are placed in the incubator to show the 30 minute requirement has been met. o The SOP does not state that initial dissolved oxygen (DO) of the dilution water must be between 7.5 and 9.0 mg/L and what corrective action to take if it isn’t within that range. o The SOP does not state that initial DO of all bottles other than the blank must be between 7 and 9 mg/L and what corrective action to take if it isn’t within that range. o The SOP does not include the seed control factor in the calculation. It is recommended that the simpler equivalent formula be documented in the SOP: BOD5, mg/L = ((Initial DO) – (Final DO) – (Seed Correction Factor)) x (Dilution Factor). Dilution factor = 300 / (volume of sample used). o The SOP does not include corrective action for Quality Control failures (i.e., blanks, GGA, duplicates, drift check). o The SOP does not state that the seed control dilutions that meet the requirement of 2 mg/L DO uptake and 1 mg/L DO remaining are averaged to determine the seed control factor. o The SOP does not state the acceptable range of the seed correction. It generally should be between 0.6 and 1.0 mg/L but the amount of the seed added should be adjusted from this range to that required to provide GGA check results of 164 + 30.7 mg/L. If the lab is getting Seed Control Factor (SCF) greater than 1.0 the laboratory must have data on file to show this is the only way to get acceptable results on GGA. The range would then be extended to 1.4 mg/L and this would be documented in the SOP, as well, if this is the case. o The SOP states that the duplicates should be within 15%. The method states that they must check within 30% of each other. Page 9 #7 Fayetteville Cross Creek WWTP Lab o The SOP does not state that dilution water must be added to the GGA bottle before the seed is added.  Phosphorus, Total – Standard Methods, 4500 P E-1999 o The SOP for Total Phosphorus and Ortho Phosphate is combined but the analytical and quality control requirements are not clearly identified for each parameter. The laboratory will need to revise the current SOP to clearly identify the analytical and quality control requirements f or each method or develop separate SOPs for Total Phosphorus and Ortho Phosphate. o The SOP did not include blank acceptance criterion. o The SOP states calibration curve standards do not need to be digested. The laboratory is digesting the standards for Total Phosphorus but not Ortho Phosphate. The SOP must clearly distinguish the different requirements for the two parameters. o The SOP does not reference the digestion method (i.e., Standard Methods 4500-B (5)-1999 Persulfate Digestion). o The SOP incorrectly states the molarity of the Ascorbic Acid as 0.01M instead of 0.1M. o The SOP does not include the minimum cell path length (i.e., 2.5 cm).  pH – Standard Methods, 4500 H+ B-2000 o The SOP does not state that the 6.0 s.u. check buffer is only used for drinking water. o The SOP references the 18th Edition of Standard Methods rather than Standard Methods Committee approval year. This Edition does not contain the approved method.  Temperature – Standard Methods, 2550 B-2000 o The SOP references the 18th Edition of Standard Methods rather than Standard Methods Committee approval year. This Edition does not contain the approved method. o The SOP states that temperature should be read within 15 minutes. Temperature samples must be read immediately. o The SOP states in Section I.C. that the verification thermometer/meter readings must be less than or equal to 1C. It needs to state that the difference must be less than or equal to 1C.  Chlorine, Total Residual – Standard Methods, 4500 Cl G-2000 o The SOP references the 18th Edition of Standard Methods rather than Standard Methods Committee approval year. This Edition does not contain the approved method. o The SOP states in Section I B. “These samples should be neutralized to pH 6 to 7 with 1N sulfuric acid or 1N sodium hydroxide.” The method does not allow for pH adjustment of samples. o The SOP does not state to analyze a reagent blank when analyzing a prepared standard. The acceptance criterion of < ½ the reporting limit will need to be added as well. o The SOP does not state to zero the instrument. o The SOP does not include directions to assign a true value to the gel standard. o The SOP does not include the acceptance criteria for the annual curve verification. (i.e., correlation coefficient > 0.995, recovery of +25% for standards <50 µg/L and +10% for standards ≥50 µg/L). Page 10 #7 Fayetteville Cross Creek WWTP Lab o The SOP does not include in Section V. D. Quality Control, the acceptance criterion of the gel standard (i.e., + 10% of the assigned true value).  Residue, Suspended – Standard Methods, 2540 D-1997 o The SOP lists the minimum weight gain requirement as at least 0.001 grams of dried residue. The method specifies 0.0025 grams. o The SOP does not state to rinse the sample down with three 10 mL portions of reagent-grade water. o The SOP does not give an acceptance criterion for the duplicates.  Nitrogen, Ammonia – Standard Methods, 4500 NH3 D-1997 o The SOP does not state that 1 mL of 10N NaOH must be added to 100 mLs of blanks to raise pH above 11 in Section V. C Calibration of Meter. o The SOP does not include sample preservation and hold time. o The SOP does not clearly identify which standards are calibration standards in Section V. A. Standard Preparation. o The SOP states place 100 mLs or 200 mLs of each standard solution in a 150 mL beaker or a 250 beaker. The SOP must document the actual volume used or clearly describe what dictates which volume to use. o The SOP does not state that calibration standards must be analyzed in order of lowest to highest concentration. o The SOP does not state the frequency, acceptance criterion, corrective actions and preparation for any of the QC (e.g., Method Blank (MB), Laboratory Fortified Blank (LFB), Laboratory Fortified Matrix/Laboratory Fortified Matrix Duplicate (LFM/LFMD)). o The SOP does not describe the preparation of the Ammonia-Free Water as stated in Standard Methods 4500 NH3 D-1997 (3) (a). o The SOP does not describe the pH meter calibration. If this is in another SOP it must be referenced in this SOP. o The SOP does not include support equipment (e.g., pH meter). o The SOP does not include the concentration of the NH4Cl stock solution.  Specific Conductance – Standard Methods, 2510 B-1997 o The SOP does not include QC acceptance criteria and corrective actions for QC failures. o The SOP does not state to calibrate the instrument prior to analyzing samples. o The SOP does not state the proper units (i.e., µmhos/cm).  Metals – Standard Methods, 3111 B-1999  Metals – Standard Methods, 3111 D-1999  Metals – Standard Methods, 3113 B-2004 o The SOP does not state that the working standards are made by the instrument for Calcium, Magnesium, and Sodium. o The SOP states “The calibration curve must include a low point equal to the detection limit of the metal being analyzed.” The requirement is to analyze a standard at a concentration equal to or less than the laboratory’s lowest reporting concentration. o The SOP does not state to analyze a calibration blank and calibration verification standard (mid-range) at the end of the analytical batch. o The SOP states, “the blank must read less than the detection limit of the metal being analyzed”, instead of the requirement of ≤ ½ the reporting limit. Page 11 #7 Fayetteville Cross Creek WWTP Lab  Metals – Standard Methods, 3113 B-2004 o The SOP does not state what the final volume is in Section D. It only states to bring the digested aliquot to volume. 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 will be revised to address the items in this Finding within one year. Bacteria – Coliform, Fecal – Standard Methods, 9222 D-1997 Recommendation: The laboratory is currently utilizing an air incubator. Due to its design, it is very difficult to properly monitor and maintain the method required temperature. It is recommended a water bath be utilized because of the greater temperature stability provided by the water over the air environment. We recommend that the laboratory begin the process to budget for the replacement of the currently used air incubator with a water bath. Recommendation: It is recommended that new and old lots be clearly documented on the consumable testing log. L. Finding: The laboratory was not conducting comparison testing on new lots of consumables (i.e., media before being put in use. Requirement: When a new lot of culture medium, pads, or membrane filters is to be used, a comparison of the current lot in use (reference lot) against the new lot (test lot) is to be made. As a minimum, make single analyses on five positive samples. Ref: NC WW/GW LC Policy. Requirement: If the test and reference materials check within what you have determined is acceptable for duplicates of samples, the test material would be considered acceptable to use. Ref: NC WW/GW LC Policy. Comment: Comparison testing was not being performed on the media because by the time the new media is obtained the old media has been all used. Recommendation: There is no acceptance criteria for testing consumable material. The acceptance criterion outlined in SM 9020 B. 5. (f) (k) (2) may be used or, per the NC WW/GW Policy, it is acceptable to use your current acceptance criteria for fecal duplicates. M. Finding: The laboratory is not documenting time of sample filtration to demonstrate that the time from sample filtration until incubation was < 30 minutes. Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A). Requirement: Place all prepared cultures in the water bath within 30 min after filtration. Ref: Standard Methods, 9222 D-1997. (2) (d). CBOD – Standard Methods, 5210 B-2001 Recommendation: Seed is not being aerated, only stirred during the transfer to the bottles. It is recommended that seeding material should be both “stirred” and “aerated” during preparation. The Page 12 #7 Fayetteville Cross Creek WWTP Lab extra oxygen from aeration appears to result in a more viable seeding material. This is accomplished by bubbling air through the mixture while stirring. (A common aquarium air pump and aeration stone may be used.) Ref: NC WW/GW LC Policy. N. Finding: The lab is measuring sample volumes <20 mLs without using wide tip pipets. Requirement: Sample volumes less than 20 mLs must be measured using a wide-tip pipet. Ref: NC WW/GW LC Policy. O. Finding: Sample volumes <3 mLs are being measured without preliminary dilutions. Requirement: For dilutions greater than 1:100 make a primary dilution before making final dilution. This would be any measurements of less than 3 mLs sample volume if diluting directly into BOD bottles. Ref: NC WW/GW LC Policy. P. Finding: The GGA true value was incorrect on the benchsheet. Requirement: Based upon guidance from EPA Region IV, a laboratory may choose one of the following acceptance criteria for the CBOD GGA: 198 ± 30.5 mg/L (167.5 – 228.5 mg/L) or 164 ± 30.7 mg/L (133.3 – 194.7 mg/L). The laboratory must choose which acceptance criterion they will follow and not switch between them. The lab must take corrective actions whenever the limits are exceeded (i.e., qualifying the data) and the procedures must be documented in laboratory standard operating procedures. It is required to analyze three duplicate GGAs and the resulting average of the three bottles must meet the acceptance criteria. Ref: NC WW/GW LC Policy. Comment: The acceptance range being used and documented on the benchsheet was correct at 133.3 – 194.7 mg/L, but the true value was documented as 170 mg/L instead of 164 mg/L. Q. Finding: Multiple dilution water blanks are being analyzed but not averaged. Requirement: Multiple dilution water blanks in the same batch using the same dilution water are to be treated as replicates and averaged. The average of the dilution water blanks in a batch must not be >0.20 mg/L. Ref: “BOD Multiple Dilution Water Blanks”, Standard Methods Joint Editorial Board memorandum dated August 1, 2014. R. Finding: The dilution water blank acceptance criterion that is being used is incorrect. Requirement: The DO uptake in 5 d must not be more than 0.20 mg/L and preferably not more than 0.10 mg/L, before making seed corrections. Ref: Standard Methods, 5210 B-2001. (6) (c). Comment: An acceptance criterion of 0.2 mg/L is being used. Nitrogen, Ammonia – Standard Methods, 4500 NH3 D-1997 Recommendation: It is recommended that the lab label the 0.5 ppm and 5 ppm standards as check standards on the laboratory benchsheet to distinguish them from the calibration curve standards. S. Finding: Laboratory Fortified Matrix (LFM) recoveries are not always calculated properly. Page 13 #7 Fayetteville Cross Creek WWTP Lab Requirement: LFM recovery: CS – (C X f) X 100 = %Recovery LFM or LFMD S where: Cs= LFM concentration determined experimentally, f = spike dilution correction, C = concentration of sample before spiking, and S = concentration of spike. NOTE: f should be greater than 0.95. More than 5% dilution due to spiking changes the matrix significantly. Ideally keep f to above 0.99 (equivalent to 1% dilution of sample due to spike addition), in which case f can be ignored and the equation simplified to eliminate f. Ref: Standard Methods, 4020 B-2009, Rev. 2011. (3) (a). Comment: The note above from Standard Methods states that the volume of spike should be ≤5% of the total, but as a reminder, NC WW/GW LC policy allows up to 10% as long as spike volumes above 1% are corrected through calculation. Comment: LFM recovery evaluations are based on the observed concentration, rather than the calculated final result with applied dilution factors. T. Finding: The benchsheet layout makes it difficult to determine if quality assurance frequency requirements are being met. Requirement: Each laboratory shall develop and maintain a document outlining the analytical quality control practices used for the parameters included in their certification. Supporting records shall be maintained as evidence that these practices are being effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7). Comment: QC samples are not listed with the samples in the order they are analyzed. This makes it impossible to determine whether the continuing calibration verification standard and calibration blank are analyzed initially, after every ten samples and at the end of each sample group. U. Finding: The volume of 10N NaOH added to the samples, blanks, and calibration standards was not documented on the benchsheet. Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A). Comment: A statement may be added to the benchsheet that “unless otherwise noted, 1 mL of NaOH is added to all samples and standards” to fulfill this requirement. V. Finding: The difference in volume of 10N NaOH used in the samples versus the calibration standards was not compensated for in the sample results calculation. Page 14 #7 Fayetteville Cross Creek WWTP Lab Requirement: When the volume of 10N NaOH used for the samples is different than that used for the calibration standards this must be compensated for in the calculation. Ref: NC WW/GW LC Policy. Requirement: The following formula must be used in the calculation: mg NH3 – N/L = A x B x (100 + D) (100 + C) A= Dilution Factor B= Concentration of NH3-N/L, mg/L, from calibration curve C= Volume of 10N NaOH added to the calibration standards, mL D= Volume of 10N NaOH added to sample, Ml Ref: Standard Methods, 4500 NH3 D-1997. (5). Comment: A different volume of 10N NaOH is rarely required for samples. W. Finding: Samples are not preserved and are not analyzed within 15 minutes of collection. Requirement: Except where noted in this Table II and the method for the parameter, preserve each grab sample within 15 minutes of collection. For a composite sample collected with an automated sample (e.g., using a 24-hour composite sample; see 40 CFR 122.21 (g)(7)(i) or 40 CFR Part 403, Appendix E), refrigerate the sample at ≤6°C during collection unless specified otherwise in this Table II or in the method(s). For a composite sample to be split into separate aliquots for preservation and/or analysis, maintain the sample at ≤6°C, unless specified otherwise in this Table II or in the method(s), until collection, splitting, and preservation is completed. Add the preservative to the sample container prior to sample collection when the preservative will not compromise the integrity of a grab sample, a composite sample, or aliquot split from a composite sample within 15 minutes of collection. Ref: Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012; Table II, Footnote 2. X. Finding: The percent recovery of the Laboratory Fortified Matrix Duplicate (LFMD) is not calculated nor documented on the benchsheet. 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 .085 (a) (7). Comment: The 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. Comment: The Laboratory Fortified Matrix (LFM) percent recovery and the Relative Percent Difference (RPD) between the LFM and LFMD are documented on the benchsheet. Y. Finding: Samples are not appropriately pretreated for residual chlorine. Page 15 #7 Fayetteville Cross Creek WWTP Lab Requirement: Residual Chlorine reacts with ammonia; remove by sample pretreatment. If a sample is likely to contain residual chlorine, immediately upon collection, treat with dechlorinating agent as in 4500-NH3.B.3d. Ref: Standard Methods, 4500 NH3 A.-1997, Rev. 2011. (2). Comment: The laboratory is adding sodium sulfite to all effluent samples as a dechlorinating agent. The method specifies sodium thiosulfate. Z. Finding: The adjusted pH is not verified and documented on the benchsheet. Requirement: Add a sufficient volume of 10N NaOH solution (1 mL usually is sufficient) to raise the pH above 11. If the presence of silver or mercury is possible, use NaOH/EDTA solution in place of NaOH solution. If it is necessary to add more than 1 mL of either NaOH or NaOH/EDTA solution, note volume used, because it is required for subsequent calculations. Ref: Standard Methods, 4500 NH3 D (4) (b). Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A). AA. Finding: The laboratory does not have a Method Blank acceptance criterion. Requirement: For analyses requiring a calibration curve, the concentration of reagent, method and calibration blanks must not exceed 50% of the reporting limit or as otherwise specified by the reference method. Ref: NC WW/GW LC Policy. Phosphorus, Total – Standard Methods, 4500 P E-1999 Nitrogen, Ammonia – Standard Methods, 4500 NH3 D-1997 BB. Finding: The samples chosen for the Laboratory Fortified Matrices (LFMs) are not being randomly selected. Requirement: To prepare a LFM, add a known concentration of analytes (ideally from a second source) to a randomly selected routine sample without increasing its volume by more than 5%. Ref: Standard Methods, 4020 B-2009, Rev. 2011. (2) (g). Comment: Only the Rockfish (RF) Influent sample is being spiked. Recommendation: It is recommended that the lab take steps to insure that all sample matrices analyzed by the laboratory be spiked over time to demonstrate that no matrix attributes bias to the test. Recommendation: It is recommended that the laboratory take steps to insure that all sample matrices analyzed by the laboratory be spiked over time to demonstrate that no matrix attributes bias to the test. The laboratory’s normal procedure has been to spike whichever sample is last. CC. Finding: The volume of sample analyzed is not 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: 15 NCAC 2H .0805 (a) (7) (H). Page 16 #7 Fayetteville Cross Creek WWTP Lab Comment: The dilution factor is documented but the volume analyzed must be documented as well. Phosphorus, Total – Standard Methods, 4500 P E-1999 Recommendation: It is recommended that the following instruction be added to the Combined Color Reagent preparation on the Total Phosphorus curve worksheet “Mix well after addition of each reagent.” DD. Finding: A calibration blank is not analyzed at the end of the sample group. Requirement: Verify calibration by periodically analyzing a calibration standard and calibration blank during a run – typically, after each batch of ten samples and at the end of the run. Ref: Standard Methods, 4020 B- 2009, Rev. 2011. (2) (b). 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. EE. Finding: Laboratory-generated stored calibration curves are not traceable to data generated on subsequent days. Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A). Comment: The documentation must provide for historical reconstruction of the reported results. Documentation must unequivocally link the calculated sample results to the linear regression used to generate those results. This is easily accomplished by documenting the date the curve was generated on subsequent benchsheets. Recommendation: It is recommended that the benchsheet be revised to contain a space for the calibration curve date to provide unequivocal traceability to the curve used with each set of data. FF. Finding: The analyst is not signing/initialing or dating electronically generated laboratory records to verify the data produced. 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: 15A NCAC 2H .0805 (a) (7) (A). Requirement: Electronic records must be complete and in a form that does not allow alteration without detection. The lab must insure that the complete records, including related support data, can be maintained in a secure and accessible form on the pre-existing system or migrated to a new system without modification, as needed, throughout the required retention period (5 years per 15A NCAC .0800). The system must use secure, computer-generated, time-stamped audit trails to automatically record the date and time of operator entries and actions that create, modify, or delete electronic records. Audit trails must also be maintained throughout the required record-retention period and must be readily available for review. Audit trails must track Page 17 #7 Fayetteville Cross Creek WWTP Lab the old and new records when a change is made and these changes must not obscure previously recorded information. Ref: NC WW/GW LC Policy. Comment: The Total Phosphorus and Total Phosphorus Curve worksheets are generated electronically and do not have the analyst’s initials or dates. For electronic records generated from a system that is not secure, hand initialing and dating the data printouts will meet the requirement. GG. Finding: The spike solution volume constitutes >1% of the total sample volume when preparing matrix spikes and the laboratory is not using the proper correction factor when calculating the final result. 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 spike solution to total matrix spike volume ratio the lab is using is 2%. HH. Finding: The lab is documenting an incorrect chemical formula for the ammonium molybdate solution used on the Total Phosphorus worksheet. Requirement: Ammonium Molybdate Solution: Dissolve 20 g (NH4)6Mo7O24  4H2O in 500 mL distilled water. Store in a glass-stoppered bottle. Ref: Standard Methods, 4500 P E (3) (c). Comment: The lab was documenting the use of (NH3)6Mo7O24  6H2O but was correctly using the quadrahydrate formulation in practice. II. Finding: The laboratory is not analyzing a Laboratory Fortified Matrix Duplicate (LFMD). Requirement: Include at least one LFM/LFMD daily or with each batch of 20 or fewer samples. Ref: Standard Methods, 4020 B-2009, Rev. 2011, Table 4020: I and (2) (g). Comment: The laboratory is analyzing sample duplicates and LFMs. Analysis of the LFMD (or MSD) is acceptable to satisfy the sample duplicate requirement listed in North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (C). Residue, Suspended – Standard Methods, 2540 D-1997 Comment: The laboratory analyzes a 1000 mL blank. This is not a method requirement. Comment: If pre-weighed filters are used, dry filter blanks are not required. JJ. Finding: Samples chosen to be duplicated are not being randomly selected. Requirement: When appropriate (Table 2020: II), randomly select routine samples to be analyzed twice. Independently prepare and analyze duplicate samples. Ref: SM 2020 B-2010. (2) (f). KK. Finding: The laboratory is not basing the reporting limit on the minimum weight gain required by the method. Page 18 #7 Fayetteville Cross Creek WWTP Lab Requirement: The minimum weight gain allowed by any approved method is 2.5 mg. Choose sample volume to yield between 2.5 and 200 mg dried residue. This establishes a minimum reporting value of 2.5 mg/L when 1000 mL of sample is analyzed. If complete filtration takes more than 10 minutes increase filter diameter or decrease sample volume. In instances where the weight gain is less than the required 2.5 mg, the value must be reported as less than the appropriate value based upon the volume used. Ref: NC WW/GW LC Policy. Comment: Final results are not correctly calculated when the minimum residue weight is not obtained. For instance, 10 mL of the Influent on 2/23/2015 had a residue weight of 0.0015 grams. The results were listed as 150.0 mg/L but the correct result is <250 mg/L. Similar errors were observed in the months of February-June, 2015. Incorrect results were also reported on the Discharge Monitoring Reports (DMR). Comment: Current sample volumes used may not be adequate to document compliance with permit limits. LL. Finding: The true value and acceptance criterion of the QC standard analyzed on 2/23/2015 were not documented. The volume filtered and the percent recovery were also 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. Supporting records shall be maintained as evidence that these practices are being effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7). Requirement: All laboratories must use printed bench worksheets that include a space to enter the signature or initials of the analyst, date of analyses, sample identification, volume of samples analyzed, value of the measurement system, factor and final value to be reported and each item must be recorded each time samples are analyzed. Ref: 15 NCAC 2H .0805 (a) (7) (H). Comment: 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. Residue, Total – Standard Methods, 2540 B-1997 Comment: The laboratory does not report Total Residue for compliance. At the time of the inspection, it was requested that this parameter be dropped from their Certification. This request was completed effective 8/26/2015 and an updated Certified Parameters Listing was sent to the laboratory. Residue, Dissolved – Standard Methods, 2540 C-1997 Comment: The size of the dishes accommodate adequate sample volume to demonstrate compliance. Comment: The laboratory is analyzing a reagent blank, which is not required. MM. Finding: The laboratory is not basing the reporting limit on the minimum weight gain required by the method. Requirement: Choose sample volume to yield between 2.5 and 200 mg dried residue. If more than 10 min are required to complete filtration, increase filter size or decrease sample volume. Ref: Standard Methods, 2540 C-1997 (3) (c). Page 19 #7 Fayetteville Cross Creek WWTP Lab Requirement: Choose sample volume to yield between 2.5 and 200 mg dried residue. To obtain the required residue yield, successive aliquots of samples may be added to the same dish after evaporation or adjust reporting level based upon the weight gain and sample volume used. The minimum reporting value is established at 2.5 mg/L based upon a sample volume used of 1000 mL. Ref: NC WW/GW LC Policy. Comment: For example, 25 mL of Monitoring Well #1 on 2/6/2015 had a residue weight of 1.9 mg. The results were listed as 76 mg/L but the correct result is <100 mg/L. The same calculation error was observed for Monitoring Wells 3, 6, 7 and 8 in February and wells 1-3 and 6-8 in March. The incorrect results were reported on the Groundwater Monitoring form (GW -59). Comment: Current sample volumes used may not be adequate to document compliance. NN. Finding: The samples are not weighed to constant weight, nor is an annual multiple weighing study to verify the adequacy of the drying time, performed. Requirement: Constant weights must be documented. The approved methods require the following: “Repeat the cycle of drying, cooling, desiccating, and weighing until a constant weig ht is obtained or until the weight change is less than 4% of the previous weight or 0.5 mg, whichever is less.” In lieu of this, an annual study documenting the time required to dry representative samples to a constant weight may be performed. Verify minimum daily drying time is greater than or equal to the time used for the initial verification study drying cycle. Drying cycles must be a minimum 1 hour for verification. Ref: NC WW/GW LC Policy. Comment: North Carolina allows for an annual drying study in lieu of the requirement above to repeat the drying cycle for every sample. A random full set of samples should be used for the drying study. The repeated drying time in the oven should be at least 1 hour long. The time used for the annual drying study is the minimum time that samples are to be dried until a new drying study is performed. Organic Carbon, Total (TOC) – Standard Methods, 5310 B-2000 Comment: An annual method detection limit (MDL) study is not required. OO. Finding: Efficiency of inorganic carbon removal for each sample matrix is not being verified. Requirement: Check efficiency of inorganic carbon removal for each sample matrix by splitting a sample into two portions and adding to one portion an inorganic carbon level similar to that of the sample. The TOC values should agree: if they do not, adjust sample container, sample volume, pH, purge gas flow rate, and purge time to obtain complete removal of inorganic carbon. Ref: Standard Methods, 5310 B-2000. (4) (b). PP. Finding: A reagent blank and a second source QC standard are not being consistently analyzed after every 10 samples. Requirement: After every tenth analysis, analyze a blank and a laboratory control sample prepared from a source of material other than the calibration standards, at a level similar to the analytical samples. Preferably prepare the laboratory control sample in a matrix similar to that of the samples. Ref: Standard Methods, 5310 B-2000. (6). QQ. Finding: A calibration blank and/or calibration verification standard (mid-range) are not analyzed after every tenth sample and at the end of the sample group. Page 20 #7 Fayetteville Cross Creek WWTP Lab 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: A calibration blank and mid-range standard are not analyzed after samples that are added at the end of run to be reanalyzed. Comment: Data observed typically had 13 samples between standards. Comment: Making the calibration verification standard from a source of material other than the calibration standards will serve to satisfy the requirements associated with this Finding and with Finding PP. Metals – Standard Methods, 3113 B-2004 Recommendation: It is recommended that the standards are digested with the samples. Metals – Standard Methods, 3111 D-1999 Metals – Standard Methods, 3111 B-1999 Recommendation: For direct aspiration flame atomic absorption determinations (FLAA) a combination acid (nitric and hydrochloric acids) digestion is preferred prior to analysis. Ref: 40 CFR Part 136 Table IB, footnote 4. Depending upon the matrices encountered, the hydrochloric acid in this combination acid digestion procedure may be required to solubilize silver. It is recommended that the lab evaluate spike recoveries for silver to determine if the current procedure provides adequate digestion. RR. Finding: The laboratory is not analyzing a Laboratory Fortified Matrix (LFM) duplicate. Requirement: Use LFM (also known as matrix spike) and LFM duplicate to evaluate the accuracy and precision, respectively, of the method as influenced by a specific matrix. Include a minimum of one LFM/LFMD for every 20 samples in an analytical batch, or include more LFM/LFMDs if appropriate. Ref: SM3020 B-2005. (2) (h). SS. Finding: The calibration standards are not digested when required. Requirement: If digestion is used, carry standards through the same digestion procedure used for samples. Ref: Standard Methods, 3111 A-1999, Rev. 2011. (5). TT. Finding: The sample to acid ratio being utilized is incorrect. Requirement: Transfer a measured volume (100 mL recommended) of well-mixed, acid- preserved sample appropriate for the expected metals concentrations to a flask or beaker (see 3030D for sample volume). In a hood, add 5 mL conc. HNO3. Ref: Standard Methods 3030 E. (1). Comment: The laboratory is using 45 mLs of sample and 5 mLs of HNO3 with a final volume of 50 mLs. The acid should be 2.5 mLs. Page 21 #7 Fayetteville Cross Creek WWTP Lab Field Parameters Comment: Duplicates are not required for field parameters. UU. Finding: The laboratory’s pH, Conductivity, Temperature and Total Residual Chlorine, benchsheets were lacking pertinent data: Instrument identification and Facility name. Requirement: The following must be documented in indelible ink whenever sample analysis is performed: Instrument Identification; Sample site including facility name and location, etc. Ref: NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine, 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. Please submit 2 weeks of updated completed benchsheets that include sample results with the response to this report. VV. Finding: The meter calibration time is not being documented on the pH and Conductivity benchsheets. Requirement: The following must be documented in indelible ink whenever sample analysis is performed: Meter calibration time. Ref: NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine and NC WW/GW LC Approved Procedure for Analysis of Specific Conductance (Conductivity). Please submit 2 weeks of updated completed benchsheets that include sample results with the response to this report. WW. Finding: The Groundwater (Well) monitoring benchsheet for Temperature, Conductivity, pH, and Total Residual Chlorine does not include analyst initials. Requirement: Field benchsheets must provide a space for the signature or initials, and proper units of measure for all analyses. Ref: 15A NCAC 02H .0805 (g) (1). pH – Standard Methods, Standard Methods, 4500 H+B-2000 Recommendation: The pH buffer 6.0 S.U. is only used for drinking water samples. It is recommended to indicate that this is only used for drinking water samples on the benchsheet. XX. Finding: A check buffer is not analyzed after meter calibration. Requirement: The meter must be calibrated with at least two buffers. In addition to the calibration buffers, the meter calibration must be verified with a third standard buffer solution. The calibration and check standard buffers must bracket the range of the samples being analyzed. Ref: NC WW/GW LC Approved Procedure for the Analysis of pH. YY. Finding: Values were reported that exceed the method specified accuracy of 0.1 units. Requirement: By careful use of a laboratory pH meter with good electrodes, a precision of ±0.02 unit and an accuracy of ±0.05 unit can be achieved. However, ± 0.1 pH unit represents the limit of accuracy under normal conditions, especially for measurement of water and poorly buffered solutions. For this reason, report pH values to the nearest 0.1 pH unit. Ref: Standard Methods, 4500 H+ B-2000. (6). Comment: Sample results are reported to two decimal places. Page 22 #7 Fayetteville Cross Creek WWTP Lab Temperature – Standard Methods, 2550 B-2000 Recommendation: It is recommended to include a statement on the benchsheet that samples are analyzed “in-situ”, therefore only one time is documented. ZZ. Finding: The temperature sensor on the pH, Conductivity and Temperature meter used to obtain reported temperature values had not been checked against a National Institute of Standards and Technology (NIST) traceable thermometer within the past 12 months. Requirement: Thermometers and temperature measuring devices, used to measure temperature for compliance monitoring, must be checked every 12 months against a NIST traceable thermometer. The thermometer/meter readings must be less than or equal to 1ºC from the NIST traceable thermometer reading. The documentation must include the serial number of the NIST traceable thermometer that was used in the comparison. Document any correction that applies on both the thermometer/meter and on a separate sheet to be filed. Ref: NC WW/GW LC Approved Procedure for the Analysis of Temperature. Specific Conductance (Conductivity) – Standard Methods, 2510 B-1997 AAA. Finding: A calibration verification check standard is not being analyzed each analysis day. Requirement: Analyze and document a calibration verification check standard prior to environmental sample analysis. It is recommended that this standard value bracket (may be higher or lower than the calibration standard, as applicable) the expected range of sample values measured. The value obtained for the calibration verification check standard must read within 10% of the true value of the calibration verification check standard. If the obtained value is outside of the 10% range, corrective action must be taken. Ref: NC WW/GW LC Approved Procedure for Analysis of Specific Conductance (Conductivity). BBB. Finding: The units on the benchsheet are incorrect. Requirement: Report temperature-compensated conductivities as “µmhos/cm @ 25.0C.” Ref: Standard Methods, 2510 B-1997. (5). Comment: Units of ms/cm were documented on the benchsheet. CCC. Finding: The Automatic Temperature Compensator (ATC) 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: Anticipated temperatures can be obtained from a review of the Discharge Monitoring Reports (DMRs) from the peak summer and winter months. Historical data should provide a reasonably accurate estimation of ranges that will bracket the expected sample temperatures. Comment: At the time of the inspection, a copy of the Approved Procedure for the Analysis of Specific Conductance (Conductivity) was provided that includes directions on how to verify the ATC. Page 23 #7 Fayetteville Cross Creek WWTP Lab Chlorine, Total Residual – Standard Methods, 4500 Cl G-2000 DDD. Finding: The check standard’s assigned, meter specific, true value of 204 µg/L was not being used when evaluating the standard’s percent recovery. Requirement: The assigned values will be used for the next twelve months, or until a new curve verification is performed. The gel/liquid standard verification must be performed for each instrument on which they are to be used. If multiple instruments and/or standard sets are used, each must have assigned values specific for the instrument and standard set. Documentation must link the gel standard identification to the meter with which the assigned value was determined. Ref: NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine. Comment: The assigned value on the gel standard box was being used. There were no check standards that were outside the acceptance criteria for the data reviewed. IV. PAPER TRAIL INVESTIGATION: The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks, etc.) and Discharge Monitoring Reports (DMRs) submitted to the North Carolina Division of Water Resources. Data were reviewed for Rockfish Creek (NPDES #NC0050105), and Cross Creek (NPDES #NC0023957) for January and February, 2015. The following errors were noted: For the months of February – June, 2015 Dissolved Residue results were reported incorrectly (see Finding MM). Suspended Residue results were reported incorrectly for the months of February and March, 2015 (see Finding -KK). In order to avoid questions of legality, it is recommended that you contact the appropriate Regional Office for guidance as to whether an amended Discharge Monitoring Report will be required. A copy of this report will be made available to the Regional Office. V. CONCLUSIONS: Correcting the above-cited Findings and implementing the recommendations will help this 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: Tonja Springer Date: October 27, 2015 Report reviewed by: Beth Swanson Date: October 29, 2015