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Home My WebLink About#208 - 2012 Insp - final INSPECTION REPORT ROUTING SHEET To be attached to all inspection reports in-house only. Laboratory Cert. #: 208 Laboratory Name: Elementis Chromium LP Inspection Type: Industrial Maintenance Inspector Name(s): Todd Crawford and Jeff Adams Inspection Date: February 22, 2012 Date Report Completed: March 5, 2012 Date Forwarded to Reviewer: March 5, 2102 Reviewed by: Jason Smith Date Review Completed: March 16, 2012 Cover Letter to use: Insp. Initial X Insp. Reg. Insp. No Finding __ Insp. CP___ Corrected Unit Supervisor: Dana Satterwhite Date Received: March 21, 2012 Date Forwarded to Linda: April 10, 2012 Date Mailed: April 11, 2012 _____________________________________________________________________ On-Site Inspection Report LABORATORY NAME: Elementis Chromium LP NPDES PERMIT # NC0003875, NCS000003, WQ0001492 ADDRESS: 5408 Holly Shelter Rd Castle Hayne, NC 28429 CERTIFICATE #: 208 DATE OF INSPECTION: February 22, 2012 TYPE OF INSPECTION: Industrial Maintenance AUDITOR(S): Todd Crawford and Jeff Adams LOCAL PERSON(S) CONTACTED: Treva Croker and Dean Riggs 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. A system of traceability for prepared reagents and standards was in place; however, a system of traceability for purchased reagents and consumable supplies needs to be implemented. The facility maintains certification for Total Dissolved Residue but is not required to report data to the State. Data for this parameter was not reviewed. The requirements associated with Findings D, H and I are new policies that have been implemented by our program since the last inspection. III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS: Quality Control A. Finding: The facility has not developed Standard Operating Procedures (SOPs) for the field analyses of pH, Dissolved Oxygen, Temperature or Residual Chlorine. 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). Recommendation: It is recommended that SOPs include a review date history, to show maintenance, and a revision date history with a brief description of the change(s) made. B. Finding: The facility has not updated established SOPs since 2002. Page 2 #208 Elementis Chromium LP 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). Recommendation: It is recommended that SOPs include a review date history, to show maintenance, and a revision date history with a brief description of the change(s) made. C. Finding: Auto-pipettors are only calibrated once 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. Documentation D. 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. Total Residual Chlorine - Standard Methods, 18th Edition, 4500 Cl G E. Finding: The units of measure are not documented in the logbook. 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). F. A calibration verification standard (mid-range) is not analyzed prior to sample analysis. 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, Page 3 #208 Elementis Chromium LP 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: A calibration verification standard was being analyzed at the end of the sample run. pH - Standard Methods, 18th Edition, 4500 H+ B Comment: The Automatic Temperature Compensator (ATC) check is no longer required. The temperature sensor check, however, is required if the meter is used to measure a temperature that is reported to the State. G. Finding: Data values are reported on the Discharge Monitoring Report to 0.01 S.U. instead of 0.1 S.U., as required by the method. Requirement: A variance of ± 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, 18th Edition, 4500 H+ B. (6). Temperature - Standard Methods, 18th Edition, 2550 B H. Finding: The DO meter used to obtain reported temperature values is not labeled with its temperature correction factor. 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. 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 document any correction that applies (even if zero) on both the thermometer/ meter and on a separate sheet to be filed. All thermometers, or temperature sensing devices on field meters must meet NIST specifications for accuracy or must be calibrated against a NIST certified or NIST traceable thermometer annually (every 12 months) and proper corrections made and documented. A correction factor must be posted on the meter even if that correction factor is 0ºC. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy. Total Suspended Solids - Standard Methods, 18th Edition, 2540 D I. 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). J. Finding: The laboratory is not basing the reporting limit on the minimum weight gain required by the method. Page 4 #208 Elementis Chromium LP 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: North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods, 20th and 21st Editions, 2540 D. (3) (b). Comment: The facility was using a reporting limit of 5.0 mg/L based on a 1000 ml sample. If 1000 mL of sample is analyzed and < 2.5 mg of dried residue is obtained, the value reported would be < 2.5 mg/L. If 500 mL of sample is analyzed and < 2.5 mg of dried residue is obtained, the value reported would be < 5 mg/L. Metals – EPA Method 200.7 Metals – Standard Methods, 18th Edition, 3120 B Recommendation: It is recommended that since the facility is certified for both Standard Methods 3120B and EPA Method 200.7, which have different quality control requirements, that the method being followed be identified on the benchsheets. K. Finding: Proficiency Testing (PT) samples were not analyzed in the same manner as routine environmental samples. Requirement: The analysis of PT samples is designed to evaluate the entire process used to routinely report environmental analytical results; therefore, PT samples must be analyzed and the process documented in the same manner as environmental samples. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy. TCLP Metals – SW-846 Method 1311 Recommendation: It is recommended that the tumbler revolutions per minute (rpm) be verified each time it is used. IV. PAPER TRAIL INVESTIGATION: The paper trail consisted of comparing laboratory benchsheets and contract lab reports to Discharge Monitoring Reports (DMRs) submitted to the North Carolina Division of Water Quality. Data were reviewed for October, November and December, 2011. No transcription errors were detected. The facility appears to be doing a good job of accurately transcribing data. Comment: It was observed that average Total Residual Chlorine values were being reported on the DMRs. The Wilmington Regional Office was contacted regarding the protocol for reporting averages and they responded that when duplicate analyses are performed, the average should be reported as the daily value on the DMR with an identifier stating that the value is an average. The individual results used to calculate the average should be listed in the comment section. 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. Page 5 #208 Elementis Chromium LP Report prepared by: Todd Crawford Date: March 5, 2012 Report reviewed by: Jason Smith Date: March 16, 2012