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Home My WebLink About#128 - 2012 Insp - Final INSPECTION REPORT ROUTING SHEET To be attached to all inspection reports in-house only. Laboratory Cert. #: 128 Laboratory Name: Jacksonville Wilson Bay Laboratory Inspection Type: Municipal Maintenance Inspector Name(s): Todd Crawford Inspection Date: March 6, 2012 Date Report Completed: March 20, 2012 Date Forwarded to Reviewer: March 22, 2102 Reviewed by: Jeff Adams Date Review Completed: March 22, 2012 Cover Letter to use: Insp. Initial X Insp. Reg. Insp. No Finding __ Insp. CP___ Corrected Unit Supervisor: Dana Satterwhite Date Received: March 22, 2012 Date Forwarded to Linda: April 25, 2012 Date Mailed: April 25, 2012 _____________________________________________________________________ On-Site Inspection Report LABORATORY NAME: Jacksonville Wilson Bay WWTP Laboratory NPDES PERMIT # NC0088455, WQ0006735 ADDRESS: PO Box 128 Jacksonville, NC 28541 CERTIFICATE #: 128 DATE OF INSPECTION: March 6, 2012 TYPE OF INSPECTION: Municipal Maintenance AUDITOR(S): Todd Crawford LOCAL PERSON(S) CONTACTED: Jill Puff I. INTRODUCTION: This laboratory was inspected 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. Benchsheets were easy to understand and records were well organized. A system of traceability for consumables, prepared reagents and standards was in place, however, there was not a clear link to individual analyses. 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. The requirements associated with Findings C, D, F, H, L, M and O are new policies that have been implemented by our program since the last inspection. Ms. Jill Puff is also the supervisor of the laboratory at the Jacksonville Nano-Filtration Water Treatment Plant. Analyses performed by staff at that facility are pH, Dissolved Oxygen (DO) and Conductivity. Data and equipment at that facility were not included in this inspection. III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS: Quality Control A. Finding: The National Institute of Standards and Technology (NIST) traceable thermometer used to check all laboratory thermometers has not been calibrated in the past 12 months. Page 2 #128 Jacksonville Wilson Bay WWTP Laboratory Requirement: Once the NIST thermometer has been certified, repeat the calibration verification for all thermometers in the lab. Include all supporting documentation with your response to this report. Requirement: All thermometers must meet NIST specifications for accuracy or checked, at a minimum annually, against a NIST traceable thermometer and proper corrections made. Ref: 15A NCAC 2H .0805 (a) (7) (O). Requirement: All thermometers and temperature measuring devices must be checked every 12 months against a NIST certified or NIST traceable thermometer and the process documented. To check a thermometer or the temperature sensor of a meter, read the temperature of the thermometer/meter against a NIST certified or NIST traceable thermometer and record the two temperatures. The calibration must be performed at a temperature that corresponds to the temperature used by the incubator, refrigerator, freezer, etc. In the case of temperature measuring devices used to perform variable temperature readings the calibration must be performed at a temperature range that approximates the range of the samples. The thermometer/meter readings must be less than or equal to 1ºC from the NIST certified or NIST traceable thermometer reading. The documentation must include the serial number of the NIST certified thermometer or NIST traceable thermometer that was used in the comparison. Also make any corrections to the data and document any correction that applies (even if zero) on both the thermometer/meter and on a separate sheet to be filed. • NIST traceable thermometers used for temperature measurement must be recalibrated in accordance with the manufacturer’s recalibration date. If no recalibration date is given, the NIST traceable thermometer must be recalibrated annually. • NIST certified thermometers must be recalibrated, at a minimum, every five years. A new certificate must be issued and maintained for inspection upon request. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy. B. Finding: Consumable materials used for the Fecal Coliform MF method are not tested prior to use to ensure that they are reliable. Requirement: When a new lot of culture medium, pads, or membrane filters is to be used, a comparison of the current lot in use (reference lot) against the new lot (test lot), be made. As a minimum, make single analyses on five positive samples. Ref: Standard Methods, 18th Edition, 9020 B. (3) (d). Include all supporting documentation with your response to this report. Comment: Guidance for conducting the comparison was provided during the inspection. Since there is no baseline for determining the acceptability of materials currently in use, acceptable consumables from another lab must be used for the initial testing of materials currently in use. Another option would be to use a contract laboratory with acceptable consumables to perform this testing. Documentation C. Finding: The laboratory needs to increase the documentation that links purchased materials, reagents and standards to individual analyses. 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 Page 3 #128 Jacksonville Wilson Bay WWTP Laboratory 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. D. Finding: Data that does not meet all quality control requirements is not qualified on the Discharge Monitoring Report (DMR). Requirement: When quality control (QC) failures occur, the laboratory must attempt to determine the source of the problem and must apply corrective action. If data qualifiers are used to qualify samples not meeting QC requirements, the data may not be useable for the intended purposes. A notation must be made on the Discharge Monitoring Report (DMR) form, in the comment section or on a separate sheet attached to the DMR form, when any required sample quality control does not meet specified criteria, and another sample cannot be obtained. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods, 20th Edition, 1020 B. (14). Dissolved Oxygen - Standard Methods, 19th Edition, 4500 O G E. Finding: The unit of measure is not documented on the calibration 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). Total Suspended Solids - Standard Methods, 19th Edition, 2540 D F. Finding: Filters are not weighed to constant weight prior to sample analysis, nor is a dry filter blank analyzed with each set of samples Requirement: If pre-prepared filters are not used, the method requires that filters must be weighed to a constant weight after washing. Repeat cycle of drying, cooling, desiccating, and weighing until a constant weight is obtained or until weight change is less than 4% of the previous weighing or 0.5 mg, whichever is less. In lieu of this process, it is acceptable to analyze a single daily dry filter blank to fulfill the method requirement of drying all filters to a constant weight prior to analysis. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods 20th Edition 2540 D. (3) (a). Comment: The lab was analyzing a wet filter blank. Biochemical Oxygen Demand - Standard Methods, 19th Edition, 5210 B G. Finding: Samples that require a pH adjustment are not being seeded. Requirement: Some samples do not contain a sufficient microbial population (for example, some untreated industrial wastes, disinfected wastes, high-temperature wastes or wastes with extreme Page 4 #128 Jacksonville Wilson Bay WWTP Laboratory pH values). For such wastes, seed the dilution water by adding a population of microorganisms. Ref: Standard Methods, 19th Edition, 5210 B. (4) (d). Total Residual Chlorine - Standard Methods, 19th Edition, 4500 Cl G H. Finding: A calibration verification standard (mid-range) is not analyzed prior to sample analyses and at the end of the sample group. Requirement: The calibration blank and calibration verification standard (mid-range) must be analyzed initially (i.e., prior to sample analysis), after every tenth sample and at the end of each sample group to check for carry over and calibration drift. If either fall outside established quality control acceptance criteria, corrective action must be taken (e.g., 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). I. Finding: Duplicate analyses are not analyzed. Requirement: Analyze five percent of all samples in duplicate to document precision. Laboratories analyzing less than 20 samples per month must analyze at least one duplicate each month samples are analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (C). Ammonia Nitrogen - Standard Methods, 18th Edition, 4500 NH3 F Comment: The laboratory was not analyzing matrix spikes prior to receiving the checklist for the inspection. North Carolina Wastewater/Groundwater Laboratory Certification Policy states: 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. Demonstration of acceptable corrective action (i.e., documentation of spikes performed after receiving the checklist and prior to the inspection) was observed during the inspection. No further response is necessary for this finding. Comment: Prior to receiving the inspection checklist, the laboratory was not verifying that sample pHs were being elevated above a pH of 11 Standard Units (S.U.) before reading results. Standard Methods, 18th Edition, 4500 NH3 F. (4) (b) states to add sufficient volume of 10 N NaOH solution to raise pH above 11. Demonstration of acceptable corrective action (i.e., documentation of pH on the benchsheets) was observed during the inspection. No further response is necessary for this finding. J. Finding: The distillation apparatus is not being properly steamed out. Requirement: Add 500 mL water and 20 mL borate buffer to a distillation flask and adjust pH to 9.5 with 6N NaOH solution. 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, 18th Edition, 4500 NH3 B. (4) (a). Comment: The distillation apparatus was being steamed out with DI water only. K. Finding: The laboratory is not analyzing a sufficient number of samples in the distillation study. Requirement: The titration method requires all samples to be distilled. For all other methods, 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. In the case of low concentration effluents, the samples Page 5 #128 Jacksonville Wilson Bay WWTP Laboratory must be spiked to allow for a meaningful statistical comparison. It is recommended that samples with a concentration < 1.0 mg/L be spiked to yield a value in the 1 – 5 mg/L range. Comparisons performed in this concentration range should check within 20% RPD. Additional samples must be analyzed comparatively if the results do not indicate approximately the same values for distilled and undistilled samples. It is recommended that both the distilled and undistilled portions of the sample be analyzed by the same laboratory using the same methodology. The following frequencies are required: Municipal and Industrial Laboratories shall analyze initially four samples distilled and undistilled from each discharge and; thereafter, analyze two samples a year from each effluent. Submit analytical results for four samples, distilled and undistilled, from each discharge within 60 days of receipt of this report. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 72, No. 47, March 12, 2007; Table IB Footnote 6. L. Finding: A calibration blank is not analyzed at the end of the sample group. Requirement: The calibration blank and calibration verification standard (mid-range) must be analyzed initially (i.e., prior to sample analysis), after every tenth sample and at the end of each sample group to check for carry over and calibration drift. If either fall outside established quality control acceptance criteria, corrective action must be taken (e.g., 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). Nitrite Nitrogen - Standard Methods, 18th Edition, 4500 NO2 B M. 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. If the unspiked sample result is in the top 40% of the calibration range, the sample should be diluted and the matrix spike prepared using the diluted sample. The recovery of the matrix spike samples must be bracketed by the calibration range. 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. Page 6 #128 Jacksonville Wilson Bay WWTP Laboratory Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy. Recommendation: It is recommended that the spike solution constitutes ≤1% of the total MS volume. Recommendation: If the duplicate sample value is near or below the reporting limit, it is recommended that a Matrix Spike Duplicate (MSD) be analyzed. The MSD fulfills the duplicate required by 15A NCAC 2H .0805 (a) (7) (C). This would result in better statistical results to monitor method and analyst precision. N. Finding: Sample pH is not being adjusted to between 5 and 9 S.U. as needed. Requirement: If sample pH is not between 5 and 9, adjust to that range with 1N HCl or NH4OH as required. Ref: Standard Methods, 18th Edition, 4500 NO2 B. (4) (b). Comment: All routine sample data that was observed were within the proper pH range. Only monitoring well samples, which are analyzed quarterly, were in need of pH adjustment. Conductivity - Standard Methods, 19th Edition, 2510 B O. Finding: The Automatic Temperature Compensator (ATC) has not been verified. Requirement: The ATC must be verified annually (i.e., every twelve months) by analyzing a conductivity standard at 25°C (the temperature that conductivity values are compensated to) and a temperature(s) that bracket the temperature ranges of the samples to be analyzed. This may require the analysis of a third temperature reading that is > 25°C. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy. P. Finding: No acceptance criteria have been established for the calibration check standards. 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: Acceptance criteria must be established in order to determine whether or not there are quality control exceedances. Acceptance criteria for the check standards may be determined using control charts or may be set using default limits such as a ± 10% recovery. IV. PAPER TRAIL INVESTIGATION: No paper trail 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: Todd Crawford Date: March 20, 2012 Report reviewed by: Jeff Adams Date: March 22, 2012