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HomeMy WebLinkAbout#68 10-final INSPECTION REPORT ROUTING SHEET To be attached to all inspection reports in-house only. Laboratory Cert. #: 68 Laboratory Name: Unifi, Inc. – Reidsville Inspection Type: Industrial Maintenance Inspector Name(s): Jeffrey R. Adams Inspection Date: September 30, 2010 Date Report Completed: October 18, 2010 Date Forwarded to Reviewer: October 18, 2010 Reviewed by: Todd Crawford Date Review Completed: October 20, 2010________ Cover Letter to use: Insp. Initial X Insp. Reg. Insp. No Finding Insp. CP Unit Supervisor: Dana Satterwhite Date Received: October 20, 2010 Date Forwarded to Alberta: November 29, 2010 Date Mailed: November 29, 2010 _____________________________________________________________________ On-Site Inspection Report LABORATORY NAME: Unifi, Inc. - Reidsville NPDES PERMIT #: NCG170176 ADDRESS: P.O. Box 1437 Reidsville, NC 27323-1437 CERTIFICATE #: 68 DATE OF INSPECTION: September 30, 2010 TYPE OF INSPECTION: Industrial Maintenance AUDITOR(S): Jeffrey R. Adams LOCAL PERSON(S) CONTACTED: Lisa Haynes and Darlene Moore 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: Mr. Mike Thomas, with the North Carolina Division of Water Quality (NCDWQ) Winston-Salem Regional Office was in attendance to observe a portion of the audit. The laboratory was neat and equipment was well maintained. Records were well organized, however, some quality control procedures need to be implemented. The laboratory filed an Amendment to Certification Application with the inspector during the audit and COD HACH Method 8000 has been removed from the laboratory’s certificate attachment. The laboratory was given a packet containing North Carolina Laboratory Certification quality control requirements and policy changes during the inspection. Finding A is a new policy that has been implemented by our program since the last inspection. III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS: Documentation Recommendation: It is recommended that the laboratory review Standard Operating Procedures (SOPs) periodically. Since there are often changes in technology or options within a particular method that are not covered in published references the laboratory SOP is the prescriptive reference document that describes a laboratory’s analytical procedure in detail. This document is intended to be the reference for analysts performing the specified test procedure. Please review laboratory SOPs and update as necessary to ensure that: The method is being performed as stated, references to standard methods are correct, the SOP is in agreement with approved practice and regulatory requirements. Copies of the most current versions of SOPs must be readily available to the analyst(s). A. Finding: The laboratory needs to increase the documentation of purchased materials and reagents, as well as, documentation of standards and reagents prepared in the laboratory. Page 2 #68 Unifi, Inc. - Reidsville 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. Biochemical Oxygen Demand – Standard Methods, 18th Edition, 5210 B B. Finding: The laboratory is not checking for total residual chlorine prior to sample analysis. Requirement: If possible, avoid samples containing residual chlorine by sampling ahead of chlorination processes. If the sample has been chlorinated but no detectable chlorine residual is present, seed the dilution water. If residual chlorine is present, dechlorinate sample and seed the dilution water (¶ 4f). Ref: Standard Methods, 18th Edition, 5210 B. (4) (e) (2). See attached document titled, Neutralizing Total Residual Chlorine in BOD Samples, for additional information. C. Finding: Dilution water was not prepared according to method instructions. Requirement: Place desired volume of water in a suitable bottle and add 1ml each of phosphate buffer, MgSO4, CaCl2, and FeCl3 solutions/L of water. Ref: Standard Methods, 18th Edition, 5210 B. (4) (a). Comment: HACH nutrient pillows are added to the dilution water which contains all of the necessary nutrients required by the method, but an additional amount of phosphate buffer is also added. This exceeds the amount of phosphate buffer required in the method. pH – Standard Methods, 18th Edition, 4500 H+ B D. Finding: The annual NIST temperature sensor check is being performed but the process is not properly documented. Requirement: All thermometers must meet National Institute of Standards and Technology (NIST) specifications for accuracy or be checked, at a minimum annually, against a NIST traceable thermometer and proper corrections made. Ref: 15A NCAC 2H .0805 (a) (7) (O). 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. The quality control document shall be available for inspection by the State Laboratory. Ref: 15A NCAC 2H .0805 (a) (7). Recommendation: It is recommended that the date the sensor check is performed, analyst initials and any correction (even if zero) be posted on the meter, as well as, retained in hard copy format. Total Suspended Residue – Standard Methods, 18th Edition, 2540 D Page 3 #68 Unifi, Inc. - Reidsville E. 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. If volume filtered fails to meet minimum yield, increase sample volume up to 1 L. If complete filtration takes more than 10 minutes increase filter diameter or decrease sample volume. Ref: NC WW/GW LC Policy based upon Standard Methods, 20th and 21st Editions, 2540 D. (3) (b). Comment: Since the publication of the March 12, 2007 Code of Federal Regulations; 40 CFR Part 136; Vol. 72, No. 47, there is no longer an approved method that allows for a 1 mg weight gain. Currently the minimum weight gain allowed is 2.5 mg. 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. The minimum reporting value is now established at 2.5 mg/L based upon a sample volume used of 1000 mL. F. Finding: The temperature of the drying oven used in the analysis was not within the acceptable range. Requirement: Dry for at least 1 hour at 103 to 105°C in an oven, cool in a desiccator to balance temperature, and weigh. Ref: Standard Methods, 18th Edition, 2540 D. (3) (c). Comment: The inspector noticed the drying oven temperature to be 100.5°C, yet all earlier log book recordings showed the temperature to be ≥103°C. The temperature was again observed after 30 minutes and still remained 100.5°C, indicating the oven temperature needed adjusting to the required temperature. Oven temperatures must be allowed to equilibrate to the proper temperature range before the measured drying time begins. At that point, the actual observed temperature must be recorded in log books to demonstrate method requirements have been met. Recording a “≥” number is not acceptable. IV. PAPER TRAIL INVESTIGATION: The paper trail consisted of comparing laboratory benchsheets and contract lab reports to Periodic Self- Monitoring Reports (PSMRs) submitted to the Town of Reidsville, NC. Data were reviewed for Unifi, Inc., Reidsville, NC (Stormwater discharge permit #NCG170176) for the following months: March, May, and July, 2010. No transcription errors were detected. It appears the laboratory is doing a good job of accurately transcribing data. 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: October 18, 2010 Report reviewed by: Todd Crawford Date: October 20, 2010 Neutralizing Total Residual Chlorine in BOD Samples It is acceptable to screen samples with DPD powder for the presence of Total Residual Chlorine (use pillows appropriate for the volume of sample tested). Generally total residual chlorine test strips are not adequate; however, these may be used for samples where interference with DPD precludes their use. If DPD yields no pink color, chlorine is absent. Document and proceed to set sample. If pink color is observed, chlorine is present. In those cases, the titration procedure outlined below must be used to determine the proper amount of Sodium Sulfite needed to neutralize chlorine in the sample. Chemicals: 1. Sodium Sulfite solution - Dissolve 0.1575 g Na2SO3 in 100 mL distilled water. Prepare fresh daily. 2. 2% H2SO4 - Add 2 mL concentrated H2SO4 to 100 mL distilled water. 3. Potassium Iodide (KI) solution - Add 10 g KI to 100 mL distilled water. Initially this solution will be clear, but in a few days it will turn greenish yellow. That’s ok. 4. Starch - Commercially available or see Standard Methods, 20th Edition - Method 4500-O C. (2) (d). Procedure: To 100 mL of sample, add approximately 1 mL of 2% H2SO4, 1 mL KI solution, and 1 mL starch. If the solution remains clear, no chlorine is present. Document this on the bench sheet and proceed to set up the sample for BOD analysis. If the solution turns blue, chlorine is present. Add the Sodium Sulfite solution, drop by drop, while stirring the sample, until the sample is clear again. Count the drops of Sodium Sulfite solution needed to neutralize the 100 mL sample. Add the relative volume of Sodium Sulfite solution to the volume of sample needed. For example, if it took 6 drops to neutralize the 100 mL sample volume and you need 300 mL of sample to set the dilutions you want, add 18 drops of Sodium Sulfite solution to 300 mL of sample. Document this on the bench sheet. Wait about 15 minutes and recheck the sample to verify the chlorine has been neutralized. Proceed to set up the sample. Note: If the blue color returns after a few seconds, do not add more Sodium Sulfite solution. Recheck with DPD to verify that returning blue color is not caused by chlorine still in sample. If no chlorine is still present, add amount of Sodium Sulfite solution equivalent to when blue color first disappears. Adding an excessive amount of Sodium Sulfite solution creates an oxygen demand and will result in a false high BOD value.