Loading...
HomeMy WebLinkAbout#5116_2021_1109_JP_FINAL January 25, 2022 5116 Mr. Samuel Toke Hospira Inc. 4285 N. Wesleyan Blvd. Rocky Mount, NC 27804 Subject: North Carolina Wastewater/Groundwater Laboratory Certification Branch (NC WW/GW LCB) Maintenance Inspection Dear Mr. Toke: Enclosed is a report for the inspection performed on November 9, 2021 by Jill Puff. I apologize for the delay in getting this report to you. Where Finding(s) are cited in this report, a response is required. Within thirty days, please supply this office with a written item for item description of how these Finding(s) were corrected. Please describe the steps taken to prevent recurrence and include an implementation date for each corrective action. If the Finding(s) cited in the enclosed report are not corrected, enforcement actions may be recommended. For Certification maintenance, your laboratory must continue to carry out the requirements set forth in 15A NCAC 02H .0800. A copy of the laboratory’s Certified Parameter List at the time of the audit is attached. This list will reflect any changes made during the audit. Copies of the checklists completed during the inspection may be requested from this office. Thank you for your cooperation during the inspection. If you have questions or need additional information, please contact me at (919) 733- 3908 ext. 251. Sincerely, Anna Ostendorff Technical Assistance & Compliance Specialist Division of Water Resources Attachment cc: Todd Crawford, Jill Puff, Master File 5116 On-Site Inspection Report LABORATORY NAME: Hospira Inc. NPDES PERMIT #: NC0001589 ADDRESS: 4285 N. Wesleyan Blvd. Rocky Mount, NC 27804 CERTIFICATE #: 5116 DATE OF INSPECTION: November 9, 2021 TYPE OF INSPECTION: Field Industrial Maintenance AUDITOR(S): Jill Puff and Anna Ostendorff LOCAL PERSON(S) CONTACTED: Samuel Toke, Mike Lewis and Jason Price I. INTRODUCTION: This laboratory was inspected by representatives of the North Carolina Wastewater/Groundwater Laboratory Certification Branch (NC WW/GW LCB) to verify its compliance with the requirements of 15A NCAC 02H .0800 for the analysis of compliance monitoring samples. II. GENERAL COMMENTS: The facility is neat and well organized and has all the equipment necessary to perform the analyses. Staff were forthcoming and responded well to suggestions from the auditors. All required Proficiency Testing (PT) Samples have been analyzed for the 2021 PT Calendar Year and the graded results were 100% acceptable. The laboratory submitted their Quality Assurance (QA) and/or Standard Operating Procedure (SOP) document(s) in advance of the inspection. These documents were reviewed, and editorial and substantive revision requirements and recommendations were made by this program outside of this formal report process. Although subsequent revisions were not requested to be submitted, they must be comple ted by July 31, 2022. The laboratory is reminded that any time changes are made to laboratory procedures, the laboratory must update the QA/SOP document(s) and inform relevant staff. Any changes made in response to the pre - audit review or to Findings, Recommendations or Comments listed in this report must be incorporated to ensure the method is being performed as stated, references to methods are accurate, and the QA and/or SOP document(s) is in agreement with each approved practice, test, analysis, measurement, monitoring procedure or regulatory requirement being used in the laboratory. In some instances, the laboratory may need to create an SOP to document how new functions or policies will be implemented. The laboratory is also reminded that SOPs are required to be reviewed at least every two years and are intended to describe procedures exactly as they are to be performed. Use of the word “should” is not Page 2 #5116 Hospira Inc. appropriate when describing requirements (e.g., Quality Control (QC) frequency, acceptance criteria, etc.). Evaluate all SOPs for the proper use of the word “should”. Contracted analyses are performed by Pace Analytical Services, LLC – Asheville NC (Certification # 40), Pace Analytical Services, LLC – Eden NC (Certification #633) and Meritech, Inc. (Certification #165). Approved Procedure documents for the analysis of the facility’s currently certified Field Parameters were provided at the time of the inspection. III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS: Comment: The laboratory does not currently analyze compliance samples for Conductivity. Proficiency Testing data was made available for review during the audit. The instrument is not being calibrated according to the manufacturer’s calibration procedure prior to analysis of samples each day. The laboratory is not analyzing a second-source calibration verification check standard. The Automatic Temperature Compensator (ATC) was not verified prior to initial use and every 12 months thereafter. The NC WW/GW LCB Approved Procedure for the Analysis of Specific Conductance (Conductivity) states: Instruments are to be calibrated according to the manufacturer’s calibration procedure prior to analysis of samples each day compliance monitoring is performed. For most meters, this is a one-standard calibration; Analyze and document a second-source calibration verification check standard prior to compliance sample analysis. It is recommended that this standard value approximate (may be higher or lower than the calibration standard, as applicable) the expected range of sample values measured. The value obtained for the calibration verification check-standard must read within 10% of the true value of the calibration verification check standard. If the obtained value is outside of the ±10% range, corrective action must be taken and; The Automatic Temperature Compensator (ATC) must be verified prior to initial use and annually (i.e., 12 months) thereafter at two temperatures by analyzing a standard or sample at 25°C (i.e., the temperature to which conductivity values are reported) and a temperature(s) that brackets the temperature ranges of the environmental samples routinely analyzed. This may require the analysis of a third temperature reading that is > 25°C. As the temperature increases or decreases, the value of the conductivity standard or sample must be within ±10% of the true value of the standard or ±10% of the value of the sample at 25°C. If not, corrective action must be taken. The laboratory voluntarily relinquished certification for Conductivity effective November 19, 2021. No further response is necessary for this Corrected Finding. General Laboratory A. Finding: The laboratory is lacking a documented training program. Requirement: Each laboratory shall develop and implement a documented training program that includes the following: that staff have the education, training, experience, or demonstrated skills needed to generate quality control results within method-specified limits and that meet the requirements of these Rules; that staff have read the laboratory quality assurance manual or applicable Standard Operating Procedures; that staff have obtained acceptable results on Proficiency Testing Samples pursuant to Rule .0803(1) of this Section or other demonstrations of proficiency (e.g., side-by-side comparison with a trained analyst, acceptable results on a single-blind performance evaluation sample, an initial demonstration of capability study prescribed by the reference method). Ref: 15A NCAC 02H .0805 (g) (5). Documentation B. Finding: The laboratory benchsheet is lacking required documentation: the method or SOP reference; the laboratory identification; the instrument identification, the proper units of measure. Page 3 #5116 Hospira Inc. Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data shall be traceable to the associated sample analyses and shall consist of: the method or SOP; the laboratory identification; the instrument identification; the proper units of measure. Each item shall be recorded each time samples are analyzed. Analyses shall conform to methodologies found in Subparagraph (a)(1) of this Rule. Ref: 15A NCAC 02H .0805 (g) (2) (A), (B), (C) and (L). Comment: This Finding applies to Total Residual Chlorine (TRC), pH and Temperature. No compliance sample data was available for review for DO or Conductivity. Any benchsheets for future compliance sample data must adhere to the same Requirements. Comment: The units of measure are not documented on the parameter benchsheet for pH analyses. C. Finding: The laboratory is not documenting traceability information for purchased materials, reagents and standards. Requirement: The laboratory shall have a documented system of traceability for all chemicals, reagents, standards, and consumables. Ref: 15A NCAC 02H .0805 (g) (7). Requirement: 15A NCAC 02H .0805 (a)(7)(K) and (g)(7) requires laboratories to have a documented system of traceability for the purchase, preparation, and use of all chemicals, reagents, standards, and consumables. That system must include documentation of the following information: Date received, Date Opened (in use), Vendor, Lot Number, and Expiration Date (where specified). 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: NC WW/GW LCB Policy. Comment: The system of traceability must make it clear what lot numbers of reagents were used for each analysis. D. Finding: Chemical containers are not consistently dated when received and when opened. Requirement: Chemical containers shall be dated when received and when opened. Ref: 15A NCAC 02H .0805 (g) (7). Comment: The laboratory does not document dates received and opened on the pH buffer bottles. E. Finding: The laboratory is not documenting the results of the Method Blank when using laboratory-prepared standards. Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref: 15A NCAC 02H .0805 (g) (4). Requirement: The following must be documented in indelible ink whenever sample analysis is performed: Value obtained for the Method Blank, if applicable (verification of ≤ ½ concentration of the lowest calibration curve, or calibration curve verification, standard). Ref: NC WW/GW LCB Approved Procedure for the Analysis of Total Residual Chlorine (DPD Colorimetric by SM 4500 Cl G-2011). Page 4 #5116 Hospira Inc. Proficiency Testing F. Finding: The laboratory does not have a documented plan for PT procedures. Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. A copy of each analytical method or Approved Procedure and Standard Operating Procedure shall be available to each analyst and available for review upon request by the State Laboratory. Standard Operating Procedure documentation shall state the effective date of the document and shall be reviewed every two years and updated if changes in procedures are made. Each laboratory shall have a formal process to track and document review dates and any revisions made in all Standard Operating Procedure documents. Supporting Records shall be maintained as evidence that these practices are implemented. Ref: 15A NCAC 02H .0805 (g) (4). Requirement: Laboratories must have a documented plan [this is usually detailed in the laboratory’s Quality Assurance Manual or may be a separate Standard Operating Procedure (SOP)] of how they intend to cover the applicable program requirements for Proficiency Testing per their scope of accreditation. This plan shall cover any commercially available PT Samples and any inter-laboratory organized studies, as applicable. The laboratory must also be able to explain when PT Sample analysis is not possible for certain methods and provide a description of what the laboratory is doing in lieu of Proficiency Testing. This shall be detailed in the plan. The plan must also address the laboratory’s process for submission of PT Sample results and related Corrective Action Reports (CARs). Ref: Proficiency Testing Requirements, February 19, 2020, Revision 5, Section 3.0. G. Finding: PT Samples are not being analyzed in the same manner as routine Compliance Samples. Requirement: Laboratories are required to analyze an appropriate PT Sample by each parameter method on the laboratory’s CPL. The same PT Sample may be analyzed by one or more methods. Laboratories shall conduct the analyses in accordance with their routine testing, calibration and reporting procedures, unless otherwise specified in the instructions supplied by the Accredited PT Sample Provider. This means that they are to be logged in and analyzed using the same staff, sample tracking systems, standard operating procedures including the same equipment, reagents, calibration techniques, analytical methods, preparatory techniques (e.g., digestions, distillations and extractions) and the same quality control acceptance criteria. PT Samples shall not be analyzed with additional quality control. They are not to be replicated beyond what is routine for Compliance Sample analysis. Although, it may be routine to spike Compliance Samples, it is neither required, nor recommended, for PT Samples. PT sample results from multiple analyses (when this is the routine procedure) must be calculated in the same manner as routine Compliance Samples. Ref: Proficiency Testing Requirements, February 19, 2020, Revision 5, Section 3.6. Comment: The laboratory is analyzing the PT Sample multiple times for TRC, pH and Specific Conductance and averaging the results. Sample duplicates are not required for Field Parameters, nor is the laboratory analyzing Compliance Samples in duplicate. H. Finding: The laboratory is not documenting PT Sample analyses in the same manner as routine Compliance Samples. Requirement: All PT Sample analyses must be recorded in the daily analysis records as for any Compliance Sample. This serves as the permanent laboratory record. Ref: Proficiency Testing Requirements, February 19, 2020, Revision 5, Section 3.6. Page 5 #5116 Hospira Inc. Requirement: The laboratory shall retain all records necessary to facilitate historical reconstruction of the analysis and reporting of analytical results for PT Samples. This means the laboratory must have available and retain for five years [pursuant to 15A NCAC 02H .0805 (a) (7) (E) and (g) (1)] all of the raw data, including benchsheets, instrument printouts and calibration data, for all PT Sample analyses and the associated QC analyses conducted by all parameter methods. Ref: Proficiency Testing Requirements, February 19, 2020, Revision 5, Section 4.0. Comment: Results from PT Sample analyses are documented on the PT vendor instruction sheets. The data does not include analysis date or time, analyst, or any traceable link to the calibration data. This Finding applies to pH, TRC and Specific Conductance. Quality Control I. Finding: The compliance temperature-measuring device is not checked at two temperatures that bracket the range of observed sample temperatures. Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref: 15A NCAC 02H .0805 (g) (4). Requirement: To check a compliance temperature-measuring device, compare readings at two temperatures that bracket the range of compliance samples routinely analyzed against a National Institute of Standards and Technology (NIST) traceable temperature-measuring device and record all four readings. The readings from both devices must agree within 0.5 ºC. Ref: NC WW/GW LCB Approved Procedure for the Analysis of Temperature. Comment: The pH meter used for compliance Temperature monitoring is only verified at a single temperature. J. Finding: The compliance temperature-measuring device is not being verified against a National Institute of Standards and Technology (NIST) traceable thermometer. Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref: 15A NCAC 02H .0805 (g) (4). Requirement: All compliance temperature-measuring devices without a valid NIST certificate must be checked initially and every 12 months against an NIST traceable temperature- measuring device and the process documented. Documentation must include the serial number of the device being checked. The serial number, stated accuracy and expiration date of the NIST traceable temperature-measuring device used in the comparison must also be documented. Verification data must be kept on file and be available for inspection for 5 years. (NOTE: Vendors or other Certified laboratories may provide assistance in meeting this requirement. When a vendor or other Certified laboratory provides this assistance, they must provide a copy of their NIST Certificate or the serial number, accuracy and calibration expiration date.) Ref: NC WW/GW LCB Approved Procedure for the Analysis of Temperature. Requirement: A Reference Temperature-Measuring Device is an NIST traceable temperature-measuring device used only to verify the calibration of other temperature- measuring devices. It must have a stated accuracy of ± 0.5 °C, be able to distinguish temperature changes of 0.1 °C and equilibrate rapidly. Ref: NC WW/GW LCB Approved Procedure for the Analysis of Temperature. Page 6 #5116 Hospira Inc. Comment: The Omega #98090409 thermometer used to verify the pH meter temperature sensor is not a Reference Temperature-Measuring device. Please submit a copy of a passing temperature verification, along with a copy of the NIST Traceable certificate for the Reference device used to verify the meter, with the report response. pH – Standard Methods, 4500 H+ B-2011 (Aqueous) K. Finding: Values were reported that exceed the method specified accuracy of 0.1 pH 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-2011. (6). Comment: pH was reported to 2 decimal places on the Discharge Monitoring Report (DMR) for Permit #NC0001589 on July 29, August 18, and September 29, 2021. Comment: Per PT Vendor instructions, the PT Sample results should be reported to two decimal places. L. Finding: Instances were observed where the pH calibration check standard did not read within ± 0.1 S.U. of the true value and no corrective action was taken. Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref: 15A NCAC 02H .0805 (g) (4). Requirement: All check standard buffers must read within ±0.1 S.U. to be acceptable. If the meter verification does not read within ±0.1 S.U., corrective actions must be taken before any samples are analyzed. Ref: NC WW/GW LCB Approved Procedure for the Analysis of pH. Comment: If the check buffer does not read within ± 0.1 S.U., the laboratory should first try pouring a new aliquot of the check buffer and reading it again. If it still does not read within ± 0.1 S.U., the meter must be recalibrated. If, after recalibration, the check buffer does not read within ± 0.1 S.U., the meter and/or probe operation may be suspect and may require servicing. If the laboratory does not have a back-up meter/electrode, or another meter/electrode cannot be procured, the laboratory is required to report the measured pH results with a qualifier that indicates the value is estimated. Comment: Check buffer measurements of the 7.0 S.U. pH buffer were repeated after analysis of the compliance sample. Laboratory staff misinterpreted how to evaluate the check buffer. The laboratory staff were evaluating the check buffer measurement against the automatic display immediately following calibration, rather than against the true value of the buffer solution. Total Residual Chlorine – Standard Methods, 4500 Cl G-2011 (Aqueous) Comment: The laboratory is currently verifying a three-point curve daily and a five-point curve annually. The laboratory may discontinue either the three-point daily verification or the five-point annual verification. However, if the laboratory elects to retain only the five-point annual verification, Page 7 #5116 Hospira Inc. the date last performed must be documented on the benchsheet. Staff were informed that the option exists to perform a five-point verification of the programmed curve annually and analyze the gel-type standard daily in the lab in lieu of the daily three-point curve verification. Dissolved Oxygen – Hach 10360-2011, Rev. 1.2 (Aqueous) Comment: The laboratory did not have compliance data available for review. M. Finding: The holding time for DO analysis is routinely exceeded. Requirement: Analyze within 15 minutes. Ref: Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 86, No. 95, May 19, 2021; Table II. Comment: The laboratory is certified for the parameter and possesses the equipment to analyze DO in-house. Pace Analytical Services, LLC – Asheville NC was analyzing DO outside of holding time and qualifying the results on the contract laboratory report. Comment: As the permitted facility that is conducting sample collection, it is the responsibility of Hospira, Inc. to ensure that contracted samples are delivered to the contract laboratory in time for the holding time to be met. This Finding emphasizes the importance of a documented training program. Reporting N. Finding: Data qualifiers from the contract laboratory reports are not being transferred to the DMR. Requirement: Each certified Field Laboratory shall be in accordance with Paragraph (e) of this Rule. Ref: 15A NCAC 02H .0805 (g) (17). Requirement: Reported data associated with quality control failures, improper sample collection, holding time exceedances, or improper preservation shall be qualified as such. Ref: 15A NCAC 02H .0805 (e) (5). Comment: The effluent collected August 18, 2021 and analyzed by Pace Analytical Services, LLC – Asheville NC was lacking the following qualifications on the DMR: Zinc – BC – Analyte was detected in the blank above ½ the reporting limit, Turbidity – H3 - Analyte was analyzed outside of holding time, Dissolved Oxygen data for Effluent, Upstream and Downstream for July, August, and September 2021 – H3 – Analyte was analyzed outside of holding time. It is recommended that you contact the Raleigh Regional Office for guidance as to whether amended DMRs will be required. A copy of this report will be made available to the Regional Office. O. Finding: Data that does not meet all QC requirements is not qualified on the DMR. Requirement: If quality control limits fall outside established limits or indicate an analytical problem, the laboratory shall identify the Root Cause of the failure. The problem shall be resolved through corrective action, the corrective action process documented, and any samples involved shall be reanalyzed, if possible. If the sample cannot be reanalyzed, or if the quality control results continue to fall outside established limits or indicate an analytical problem, the results shall be qualified as such. Ref: 15A NCAC 02H .0805 (g) (8). Comment: This Finding applies to pH. Page 8 #5116 Hospira Inc. P. Finding: The laboratory does not report all characteristics of the pollutants analyzed from permitted locations. Requirement: If the Permittee monitors any pollutant more frequently than required by this permit using test procedures approved under 40 CFR Part 136 and at a sampling location specified in this permit or other appropriate instrument governing the discharge, the results of such monitoring shall be included in the calculation and reporting of the data submitted on the DMR. Ref: Standard Conditions for NPDES Permits, Rev. 11/09/2011, Section (E) (5) (b). Comment: On July 21, 2021, effluent was analyzed for TRC, pH and Temperature but not reported on the DMR. IV. PAPER TRAIL INVESTIGATION: The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks, etc.) and contract laboratory reports to DMRs submitted to the North Carolina Division of Water Resources. Data were reviewed for Hospira Inc. (NPDES permit # NC0001589) for July, August and September 2021. The following errors were noted: Date Parameter Location Value on Benchsheet *Contract Laboratory Data Value on DMR 7/21/2021 pH Effluent 6.88 S.U. No value 7/21/2021 Total Residual Chlorine Effluent 11 µg/L No value 7/21/2021 Temperature Effluent 24.5 °C No value 7/29/2021 pH Upstream No value 6.34 S.U. 7/29/2021 Arsenic Effluent *<10 µg/L 0 7/29/2021 Copper Effluent *<5 µg/L 0 7/29/2021 Zinc Effluent *<10 µg/L 0 7/29/2021 Ammonia Nitrogen Effluent *<0.1 mg/L 0 8/18/2021 Arsenic Effluent *<10 µg/L 0 8/18/2021 Copper Effluent *<5 µg/L 0 8/18/2021 Zinc Effluent *<10 µg/L 0 8/18/2021 Ammonia Nitrogen Effluent *<0.1 mg/L 0 To avoid questions of legality, it is recommended that you contact the appropriate Regional Office for guidance as to whether an amended DMR(s) will be required. A copy of this report will be made available to the Regional Office. V. CONCLUSIONS: Correcting the above-cited Findings and implementing the Recommendation(s) will help this laboratory to produce quality data and meet Certification requirements. The inspector would like to thank the staff for their assistance during the inspection and data review process. Please respond to all Findings and include supporting documentation, implementation dates and steps taken to prevent recurrence for each corrective action. Report prepared by: Jill Puff Date: November 22, 2021 Report reviewed by: Jason Smith Date: November 24, 2021 Certificate Number:5116 Effective Date:1/1/2021 Expiration Date:12/31/2021 Lab Name:Hospira Inc. Address:4285 N. Wesleyan Blvd. Rocky Mount, NC 27804- North Carolina Wastewater/Groundwater Laboratory Certification Certified Parameters Listing Date of Last Amendment: The above named laboratory, having duly met the requirements of 15A NCAC 2H.0800, is hereby certified for the measurement of the parameters listed below. CERTIFIED PARAMETERS INORGANIC CHLORINE, TOTAL RESIDUAL SM 4500 Cl G-2011 (Aqueous) CONDUCTIVITY SM 2510 B-2011 (Aqueous) DISSOLVED OXYGEN Hach 10360-2011, Rev. 1.2 (Aqueous) pH SM 4500 H+B-2011 (Aqueous) TEMPERATURE SM 2550 B-2010 (Aqueous) This certification requires maintance of an acceptable quality assurance program, use of approved methodology, and satisfactory performance on evaluation samples. Laboratories are subject to civil penalties and/or decertification for infractions as set forth in 15A NCAC 2H.0807.