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Home My WebLink About#426 11-final INSPECTION REPORT ROUTING SHEET To be attached to all inspection reports in-house only. Laboratory Cert. #: #426 Laboratory Name: Raleigh, E.M. Johnson Water Plant Inspection Type: Municipal Maintenance Inspector Name(s): Jeffrey R. Adams Inspection Date: August 2, 2011 Date Report Completed: August 22, 2011 Date Forwarded to Reviewer: August 22, 2011 Reviewed by: David Livingston Date Review Completed: August 23, 2011 Cover Letter to use: Insp. Initial X Insp. Reg. Insp. No Finding Insp. CP ___ Corrected Unit Supervisor: Dana Satterwhite Date Received: August 24, 2011 Date Forwarded to Linda Chavis August 25, 2011 Date Mailed: August 25, 2011 _____________________________________________________________________ On-Site Inspection Report LABORATORY NAME: Raleigh, E.M. Johnson WTP Laboratory NPDES PERMIT #: NC0082376 ADDRESS: P.O. Box 590 Raleigh, NC 27602 CERTIFICATE #: 426 DATE OF INSPECTION: August 2, 2011 TYPE OF INSPECTION: Municipal Maintenance AUDITOR(S): Jeffrey R. Adams LOCAL PERSON(S) CONTACTED: Vanessa Barnes 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, however, some quality control procedures need to be implemented. The water plant has not discharged any effluent since 2005 and is currently reclaiming all of its effluent and is analyzing only lake waters, reclaimed water and Proficiency Testing (PT) samples. As a reminder, the 2011 proficiency testing results must be submitted by your vendor and received in the certification laboratory no later than October 31, 2011. The laboratory was given a packet containing North Carolina Laboratory Certification quality control requirements and policies during the inspection. The requirements associated with Findings, A, B, D, and F are new policies that have been implemented by our program since the last inspection. III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS: General Laboratory A. Finding: The laboratory needs to increase the documentation of materials and reagents used or made 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 Page 2 #426 Raleigh, E.M. Johnson WTP Laboratory 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 microbiology section is maintaining thorough and effective traceability logs on all of its reagents, media and consumables. It is recommended that this method of traceability be implemented throughout the laboratory. B. Finding: Auto-pipettors are not calibrated twice per year. Requirement: Mechanical volumetric liquid-dispensing devices (e.g., fixed and adjustable auto- pipettors, bottle-top dispensers, etc.) 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: North Carolina Wastewater/Groundwater Laboratory Certification Policy. (Refer to the example Calibration of Mechanical Volumetric Liquid-Dispensing Devices Procedure instructions left with the laboratory during the inspection.) Ammonia Nitrogen – EPA Method 350.1 C. Finding: Samples are not being distilled prior to analysis and no distillation study is on file. 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. 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. Recommendation: It is recommended that the distilled and undistilled sample portions be analyzed by the same lab, using the same instrument, technology and methodology to minimize uncertainty introduced by the analysis, yielding a truer representation of the effect of matrix and the distillation process on sample results. Ammonia Nitrogen – EPA Method 350.1 Ion Chromatography – EPA Method 300.0 for Cl -, F -, NO2 + NO3, and SO4 Total Organic Carbon – Standard Methods, 18th Edition, 5310 C Metals – EPA Method 200.8 Purgeable Organics – EPA Method 624 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 (MS) each month samples are analyzed. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy. When spiking with multi-component standards, if the method does not specify the spiking components, the laboratory control spike and matrix spike must contain all analytes that are reported. (Refer to the Matrix Spiking Technical Assistance Document for matrix spike options and instructions left with the laboratory during the inspection.) Page 3 #426 Raleigh, E.M. Johnson WTP Laboratory Fecal Coliform – Standard Methods, 18th Edition, 9222 B (MF) E. Finding: Samples are not being checked for presence of chlorine. Finding Requirement: Dechlorinating agents used at the time of sampling must be documented to have been effective upon receipt in the laboratory. A variety of field testing kits are considered to be adequate for most chlorine checks and a maximum detection limit of 0.5 mg/L is allowed. Ref: “Required Documentation for Sampling Preservation and Hold Time”, North Carolina Wastewater/Groundwater Laboratory Certification memorandum dated June 20, 2007. Metals – EPA Method 200.8 (ICP/MS) Recommendation: Perform an annual Linear Dynamic Range Study (LDR). The upper limit of the linear calibration range should be established for each analyte by determining the signal responses from a minimum of three different concentration standards, one of which is close to the upper limit of the linear range. Care should be taken to avoid potential damage to the detector during this process. The linear calibration range which may be used for the analysis of samples should be judged by the analyst from the resulting data. The upper LDR limit should be an observed signal no more than 10% below the level extrapolated from lower standards. Determined sample analyte concentrations that are greater than 90% of the determined upper LDR limit must be diluted and reanalyzed. The LDRs should be verified whenever, in the judgment of the analyst, a change in analytical performance caused by either a change in instrument hardware or operating conditions would dictate they be re-determined. Ref: EPA Method 200.8, Section 9.2.2. Total Residue – Standard Methods, 18th Edition, 2540 B Total Dissolved Residue – Standard Methods, 18th Edition, 2540 C Total Suspended Residue – Standard Methods, 20th Edition, 2540 D F. Finding: A minimum dried residue weight gain of 1 mg is used to determine the reporting limit. 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: North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods, 20th and 21st Editions, 2540 C. (3) (d) and 2540 B. (3) (b) and 2540 D (3) (b). Comment: For example, if 100 mL sample is analyzed, and less than 2.5 mg of dried residue is obtained, the value reported would be <25 mg/L. Or if 500 mL of sample is analyzed and < 2.5 mg of dried residue is obtained, the value reported would be < 5 mg/L. IV. PAPER TRAIL INVESTIGATION: No paper trail was performed. Page 4 #426 Raleigh, E.M. Johnson WTP Laboratory 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: August 22, 2011 Report reviewed by: David Livingston Date: August 23, 2011