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Home My WebLink About#188 2012-Final INSPECTION REPORT ROUTING SHEET To be attached to all inspection reports in-house only. Laboratory Cert. #: 188 Laboratory Name: City of Burlington WWTP Laboratory Inspection Type: Municipal Maintenance Inspector Name(s): Jeffrey R. Adams and Nick Jones Inspection Date: November 15, 2012 Date Report Completed: November 20, 2012 Date Forwarded to Reviewer: December 4, 2012 Reviewed by: Todd Crawford Date Review Completed: December 11, 2012 Cover Letter to use: Insp. Initial Insp. Reg. Insp. No Finding Insp. CP Corrected Unit Supervisor: Dana Satterwhite Date Received: December 11, 2012 Date Forwarded to Linda: December 17, 2012 Date Mailed: December 17, 2012 _____________________________________________________________________ On-Site Inspection Report LABORATORY NAME: City of Burlington WWTP Laboratory NPDES PERMIT # NC0023876; NC0023868; NC0083828 ADDRESS: P.O. Box 1358 Burlington, NC 27216-1358 CERTIFICATE #: 188 DATE OF INSPECTION: November 15, 2012 TYPE OF INSPECTION: Municipal Maintenance AUDITOR(S): Jeffrey R. Adams and Nick Jones LOCAL PERSON(S) CONTACTED: Glenn McGirt and Sharon Wagoner 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. The facility has all the equipment necessary to perform the analyses. The data was filed in an orderly manner and readily available for review. Some quality control procedures need to be implemented. The laboratory is reminded that any time changes are made to laboratory operations; the laboratory must update the Quality Assurance (QA)/Standard Operating Procedures (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 new functions or policy will be implemented. On May 18, 2012, EPA promulgated changes to the list of Clean Water Act (CWA) methods at 40 CFR Part 136.3. This action, referred to as the Methods Update Rule (MUR) approves new methods, or changes to existing methods, that affects over 100 EPA methods, Standard Methods, ASTM methods, and other test procedures in Part 136 of Title 40 of the Code of Federal Regulations (CFR). The rule also contains a number of clarifications relating to approved methods, sample preservation and holding times, and method modifications. The final rule may be found at: http://water.epa.gov/scitech/methods/cwa/updateindex.cfm. The North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) program will be asking certified laboratories to move toward implementation of the new rule with changes fully implemented by the end of 2012. Each laboratory will need to review the MUR and evaluate its effect on current laboratory practices. These changes must be made in the laboratory’s Standard Operating Procedures and in Quality Manuals, as well as any other place where the method is cited, e.g., reports, benchsheets, logs, etc. During this transition period, inspection reports will refer to the methods employed at the Page 2 #188 City of Burlington WWTP Laboratory laboratory at the time of the inspection, but will reference the requirements in the most recently approved version of the method. Any difficulties encountered with meeting the requirements of these references by the date due may be addressed in the written corrective action response. Contracted analyses are performed by Meritech, Inc. (Certification #165) and Eastern Analytical Laboratories, Inc. (Certification #257). The laboratory was given a packet containing North Carolina Laboratory Certification policies during the inspection. The requirements associated with Findings A and E are new policies that have been implemented by our program since the last inspection. III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS: Traceability A. Finding: The laboratory needs to increase the documentation of purchased materials and reagents. 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: North Carolina Wastewater/Groundwater Laboratory Certification Policy. Comment: The laboratory was documenting all of the traceability information required except date opened (or put in use) and expiration dates. Documentation B. Finding: Several instances of using Wite-out® over a number 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: North Carolina Wastewater/ Groundwater Laboratory Certification Policy. Quality Control C. Finding: An inconsistency was noted between the Standard Operating Procedure (SOP) and laboratory practice as follows: Page 3 #188 City of Burlington WWTP Laboratory The SOP does not describe in detail how the method is performed. 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: 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). Comment: SOPs do not describe analytical control procedures including: types of quality control samples analyzed, frequency of analysis of quality control samples, calculations and acceptance limits for accuracy and precision, how acceptance limits are derived for all quality control procedures performed and corrective action procedures when quality control samples exceed established acceptance limits. Cyanide – Standard Methods, 4500 CN E-1999 (Total) Total Kjeldahl Nitrogen – Standard Methods, 4500 Norg B – 1997 (4500 NH3 C – 1997) Nitrate + Nitrite – Standard Methods, 4500 NO3 E – 2000 Total Phosphorous – Standard Methods, 4500 P E – 1999 Total Phosphorous – Hach Method 8190 Metals - Standard Methods, 3111 B - 1999 Metals - Standard Methods, 3111 D – 1999 Metals – Standard Methods, 3111 E – 1999 Metals – Standard Methods, 3113 B - 2004 D. Finding: The laboratory is not analyzing matrix spikes. Requirement: Unless the referenced method states a greater frequency, spike 5% of samples on a monthly basis. Laboratories analyzing less than 20 samples per month must analyze at least one matrix spike each month samples are analyzed. Prepare the matrix spike from a reference source different from that used for calibration unless otherwise stated in the method. If matrix spike results are out of control, the results must be qualified or the laboratory must take corrective action to rectify the effect, use another method, or employ the method of standard additions. When the method of choice specifies matrix spike performance acceptance criteria for accuracy, and the laboratory chooses to develop statistically valid, laboratory-specific limits, the laboratory-generated limits cannot be less stringent than the criteria stated in the approved method. 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: North Carolina Wastewater/Groundwater Laboratory Certification Policy. E. Finding: The laboratory is not analyzing a calibration verification standard and blank after calibration, every 10 samples and at the end of the run. 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 Page 4 #188 City of Burlington WWTP Laboratory 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: North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods, 20th Edition, 1020 B. (10) (c), 3020 B. (2) (b), and 4020 B. (2). Comment: The laboratory is analyzing second source standards every 5 samples, but is not analyzing same source calibration verification standards and blanks. Ammonia – Standard Methods, 4500 NH3 D-1997 F. Finding: The laboratory is using a matrix spike solution volume >1% of sample volume and is not adjusting the sample or spike concentration by calculation nor documenting the matrix spike volume used on the benchsheet. 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: North Carolina Wastewater/Groundwater Laboratory Certification Policy. Requirement: Each laboratory shall develop and maintain a document outlining the analytical quality control practices used for the parameters included in their certification. Supporting records shall be maintained as evidence that these practices are being effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7). G. Finding: The laboratory was calculating the %Relative Standard Deviation (%RSD) incorrectly. 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: This anomaly was observed on 8/03/12. Comment: Percent RSD can be calculated as follows: %RSD = s x 100 x where: s = standard deviation with n - 1 degrees of freedom (n = total number of observed values) = mean of observed values. Settleable Residue – Standard Methods, 2540 F – 1997 H. Finding: The laboratory is not documenting the 45 minute sample stir time. Requirement: Fill an Imhoff cone to the 1L mark with a well mixed sample. Settle for 45 minutes, gently agitate sample near the sides of the cone with a rod or by spinning, settle 15 min longer, and record volume of settleable solids in the cone as milliliters per liter. Ref: Standard Methods, 2540 F-1997. (3) (a). Page 5 #188 City of Burlington WWTP Laboratory 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). Total Residual Chlorine – Standard Methods, 4500 Cl G – 2000 I. Finding: The laboratory is not verifying the instrument’s stored calibration curve every 12 months. Requirement: For analytical procedures requiring analysis of a series of standards, the concentrations of these standards must bracket the concentration of the samples analyzed. One of the standards must have a concentration equal to the laboratory's lower reporting concentration for the parameter involved. For colorimetric analyses, a series of five standards for a curve prepared annually or three standards for curves established each day or standards as set forth in the analytical procedure must be analyzed to establish a standard curve. Ref : 15A NCAC 2H .0805 (a) (7) (I). A copy of the new annual 5-point Total Residual Chlorine curve verification and documentation must be submitted with the response to this report. Requirement: When linear regression is used, use the minimum correlation coefficient specified in the method. If the minimum correlation coefficient is not specified, then a minimum value of 0.995 (or a coefficient of determination, r2, of 0.99) is required. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods, 1020 B. (10) (b). Recommendation: The laboratory’s National Pollutant Discharge Elimination System (NPDES) Permit limit is 28 µg/L for Total Residual Chlorine. It is recommended that the laboratory verify the internal calibration using the concentrations: 20, 30, 50, 200 and 400 µg/L. This will verify the analytical range used to measure Proficiency Testing (PT) samples as well as environmental samples. Recommendation: It is recommended that the values obtained not vary by more than 10% of the known value for standard concentrations greater than or equal to 50 g/L and not vary by more than 25% of the known value for standard concentrations less than 50 g/L. Comment: This laboratory has 3 Hach DR-2800 instruments being used for compliance monitoring. Each instrument must be verified annually with a 5 point verification curve. Comment: It is acceptable to use Gel® standards (Note: Gel® standards are approved only when used in a field setting). These Gel® standards must be verified annually with the 5 point verification curve. The value obtained will be the “True Value” for the year and until a new 5 point curve is verified. This value may be posted on the gel standard container, the meter or wherever it is readily available to the analyst. If Gel standards are to be used, please submit documentation on the verification with the 5 point annual curve along with the response to this report. Comment: Laboratories currently certified by the North Carolina Wastewater/Groundwater Laboratory Certification program as Commercial, Municipal, Industrial, or Other may use sealed standards (liquid or “Gel-type”) for daily standard curve verification in a field setting. For this application, a field setting is defined as a location off the primary facility grounds and/or at such a distance that sample collection and analysis could not be achieved at the primary facility within the parameter holding time (i.e., 15 minutes). Page 6 #188 City of Burlington WWTP Laboratory IV. PAPER TRAIL INVESTIGATION: No paper trail was performed. 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. Report prepared by: Jeffrey R. Adams Date: November 20, 2012 Report reviewed by: Todd Crawford Date: December 4, 2012