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Home My WebLink About#227 - 2012 Insp - Final INSPECTION REPORT ROUTING SHEET To be attached to all inspection reports in-house only. Laboratory Cert. #: 227 Laboratory Name: ELS, EMD, Camp LeJeune Marine Corps Base Inspection Type: Municipal Maintenance Inspector Name(s): Todd Crawford Inspection Date: September 6, 2012 Date Report Completed: September 28, 2012 Date Forwarded to Reviewer: September 28, 2012 Reviewed by: Jason Smith Date Review Completed: October 5, 2012 Cover Letter to use: Insp. Initial Insp. Reg. Insp. No Finding Insp. CP Corrected Unit Supervisor: Gary Francies Date Received: October 8, 2012 Date Forwarded to Linda: October 10, 2012 Date Mailed: October 11, 2012 _____________________________________________________________________ On-Site Inspection Report LABORATORY NAME: ELS, EMD, Camp LeJeune Marine Corps Base NPDES PERMIT #: NC0063029 WATER QUALITY PERMIT # : WQ0012346 ADDRESS: I&E/EMD/ECB 12 Post Lane Camp LeJeune, NC 28547 CERTIFICATE #: 227 DATE OF INSPECTION: September 6, 2012 TYPE OF INSPECTION: Municipal Maintenance AUDITOR(S): Todd Crawford LOCAL PERSON(S) CONTACTED: Patricia Raper and Alberta Yokamoto 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 system for traceability of standard and reagent preparation is effective, thorough and easy to follow. Proficiency Testing (PT) samples have been analyzed for all certified parameters for the 2012 proficiency testing calendar year. 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/update_index.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, Page 2 #227 ELS, EMD, Camp LeJeune Marine Corps Base 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 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 Environmental Chemists (Certification #94), Research & Analytical Laboratories (Certification #34), and Environment 1, Inc. (Certification #10). The requirements associated with Findings A, C and H are new policies that have been implemented by our program since the last inspection. III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS: Quality Control A. 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. Comment: Pipettes were last calibrated on 6/30/09. At that time, only one measurement was made at the tested volume. Temperature – Standard Methods, 2550 B - 2000 Comment: The unit of measure for temperature (ºC) was not documented on the Field Measurement/Dissolved Oxygen Worksheet. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (H) states: 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. 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. Demonstration of acceptable corrective action (i.e., an updated benchsheet which includes proper units of measure for Temperature) was received by email on 09/19/12. No further response is necessary for this finding. Ammonia Nitrogen – Standard Methods, 4500 NH3 D - 1997 Comment: Distillation of samples and/or annual distillation studies are no longer required for the electrode method. Comment: The units of measure for temperature (ºC) and pH (S.U.) were not documented on the Ammonia benchsheet. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (H) states: 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. Demonstration of acceptable corrective action (i.e., an updated benchsheet which includes proper units of measure for Temperature and pH) was received by email on 09/19/12. No further response is necessary for this finding. Page 3 #227 ELS, EMD, Camp LeJeune Marine Corps Base B. Finding: Calibration curve standards did not always bracket the concentration of the samples. Requirement: For analytical procedures requiring analysis of a series of standards, the concentrations of those 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. Ref: 15A NCAC 02H .0805 (a) (7) (I). Comment: Samples were being routinely diluted in order to make the volume of ISA added to the samples the same as that added to the standards. However in doing so, the concentration of the sample was then lower than the lowest calibration standard. Had the sample not been diluted, its concentration would have been within the calibration range. Samples should not be diluted for the sole reason of standardizing the volume of ISA solution added to samples and standards. If the volume of ISA solution added to a sample is different from that added to the calibration standards, then that is addressed by calculation. Comment: It would be acceptable to increase the amount of ISA reagent added to standards so that it matches that added to samples. This would negate the need to account for the ISA volume in the final calculations. Ammonia Nitrogen – Standard Methods, 4500 NH3 D - 1997 Total Phosphorus – HACH Method 8190 C. 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. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy. Total Phosphorus – HACH Method 8190 D. Finding: The meter is not being zeroed with the sample prior to adding the contents of one PhosVer 3 Phosphate Reagent Powder Pillow to the vial. Page 4 #227 ELS, EMD, Camp LeJeune Marine Corps Base Requirement: Zero the meter with the sample prior to adding the contents of one PhosVer 3 Phosphate Reagent Powder Pillow to the vial. Ref: HACH Method 8190, step 14. E. Finding: Samples are not preserved to pH < 2 S.U. within 15 minutes of collection. Requirement: Preserve with H2SO4 to pH < 2. Ref: Ref: Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012; Table II. 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. If a composite measurement is required but a composite sample would compromise sample integrity, individual grab samples must be collected at prescribed time intervals (e.g., 4 samples over the course of a day, at 6-hour intervals). Grab samples must be analyzed separately and the concentrations averaged. Alternatively, grab samples may be collected in the field and composited in the laboratory if the compositing procedure produces results equivalent to results produced by arithmetic averaging of results of analysis of individual grab samples. Ref: Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012; Table II, Footnote 2. Residue Suspended – Standard Methods, 2540 D - 1997 Comment: The laboratory is not basing the reporting limit on the minimum weight gain required by the method. North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods, 20th and 21st Editions, 2540 D. (3) (b) states: 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. For example, if 500 mL of sample is analyzed and < 2.5 mg of dried residue is obtained, the value reported would be < 5 mg/L. Demonstration of acceptable corrective action (i.e., an updated benchsheet showing that the reportable limit is 2.5 mg/L) was received by email on 09/19/12. No further response is necessary for this finding. F. Finding: A quarterly check standard is not being analyzed. Requirement: Excluding Oil and Grease, all residue parameters, leachate extractions, residual chlorine, and coliform, analyze one known standard in addition to calibration standards each day samples are analyzed to document accuracy. Analyze one suspended residue, one dissolved residue, one residual chlorine and one oil and grease standard quarterly. For residual chlorine, all calibration standards required by the approved procedure in use and by EPA must be analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (B). Residue Suspended – Standard Methods, 2540 D - 1997 Residue Total – Standard Methods, 2540 B - 1997 G. 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. Page 5 #227 ELS, EMD, Camp LeJeune Marine Corps Base Requirement: Constant weights must be documented. The approved methods require the following: “Repeat the cycle of drying, cooling, desiccating, and weighing until a constant weight 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: North Carolina Wastewater/Groundwater Laboratory Certification Policy based on Standard Methods, 20th Edition, 2540 D. (3) (c), 2540 B. (3) (b), and 2540 C. (3) (d). 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. Residue Total – Standard Methods, 2540 B - 1997 H. Finding: The laboratory is not choosing sample volume to yield between 2.5 and 200 mg dried residue. 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). Comment: The laboratory was typically getting dried residue weights in the range of 700 – 800 mg. pH – Standard Methods, 4500 H+ B - 2000 I. 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). BOD – Standard Methods, 19th Edition, 5210 B J. Finding: Extra nutrient, mineral, and buffer solutions are not added to the Biochemical Oxygen Demand (BOD) bottles containing more than 67% (i.e., > 201 mL) sample. Requirement: When a bottle contains more than 67% of the sample after dilution, nutrients may be limited in the diluted sample and, subsequently, reduce biological activity. In such samples, add the nutrient, mineral, and buffer solutions (3a through e) directly to individual BOD bottles at a rate of 1 mL/L (0.33 mL/300-mL bottle) or use commercially-prepared solutions designed to dose the appropriate bottle size. Ref: Standard Methods, 5210 B-2001, (5) (c) (2). Page 6 #227 ELS, EMD, Camp LeJeune Marine Corps Base Comment: Dilution water prepared as normal with nutrient, mineral, and buffer solutions would still be used in the BOD bottles. For the bottles containing more than 67% sample, extra nutrient, mineral, and buffer solutions would be added in addition to the dilution water. Recommendation: Rather than pipetting 0.33 mL of each reagent into the BOD bottle, it is recommended that commercially prepared nutrient buffer pillows for 300 mL bottles be used. IV. PAPER TRAIL INVESTIGATION: No paper trail performed. Dean Hunkele with the Wilmington Regional Office of the North Carolina Division of Water Quality performed a paper trail investigation on July 21, 2012. V. CONCLUSIONS: Correcting the above-cited findings 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: September 28, 2012 Report reviewed by: Jason Smith Date: October 5, 2012