Integration of DOE’s QSAS and DoD’s QSM Laboratory Requirements

1. Integration of DOE’s QSAS and DoD’s QSM Laboratory Requirements Joe Pardue, DOECAP Technical Operations Coordinator Nile Luedtke, DOECAP Operations Team Leader DOECAP Operations Team ASP Workshop 2011 Pleasanton, California

2. Development To-Date • Initial Concept Discussions - Nov. & Dec. 2010 • Review of Gray-Boxes Meeting - Feb. 7-9, 2011 (held at NAVSEA offices, Charleston, SC) • DOE and DoD Management Buy-In - Mar. 30, 2011 (held during DoD Workshop, Arlington, VA) • Integration Working Meeting - Jun. 2-3, 2011 (held at ACE offices, Omaha, NE) • Integration Working Meeting (2) - Aug. 17, 2011 (held during NEMC Meeting, Bellevue, WA)

3. Continuing Development • Integration Working Meeting (3) - Oct-Nov. 2011 (to be held at DOE Offices, Oak Ridge, TN) • Draft Document Available for Review - Dec. 2011 • Revisions to Draft Document - Mar. 2012 • Final Document for DOE/DoD Signature - May 2012 • Development of DOECAP Audit Checklists • Auditing to Integrated Document in FY2013

4. Integrated Document • There will not be any “gray boxes” • This will not be a “stand-alone” document • It will need to be utilized in conjunction with the established 2009 TNI Standard • The format will match the 2009 TNI Standard but will not repeat ISO 17025 or TNI requirements • Laboratories will be held to ISO 17025 and TNI 2009 requirements, plus the additional clarifications and requirements of the integrated DOE/DoD document

5. Integrated Document • DOE and DoD “gray boxes” were either: • Eliminated • Retained as written • Retained but revised per DOE or DoD needs • Combined to reflect consistent DOE/DoD thoughts • Split to clearly identify individual requirements and issues • Identified as DOE Requirement/DoD Recommendation or visa/versa • Some TNI verbiage and requirements that were dropped during the transition from the 2003 TNI Standard to the 2009 TNI Standard will be retained in the DOE/DoD document

6. Laboratory Document Control • Quality Manual shall be reviewed annually and updated as necessary • Technical SOPs shall be reviewed for accuracy and adequacy annually and whenever method procedures change, and updated as appropriate • Reviews shall be documented and documentation shall be made available for assessment • Copies of historical SOPs shall be archived for historical reference • These documents include instructions to laboratory personnel (e.g., posters, notices, operator aids, etc.)

7. Subcontracting • Laboratories must ensure that subcontracted laboratories meet the requirements of the DOE/DoD. • Subcontracted laboratories performing analytical services in support of DoD must be accredited in accordance with the DoD ELAP. • Subcontracted laboratories performing analytical services for the DOE must be approved by the applicable DOE procurement representative. • Subcontracted laboratories must receive project-specific approval from the DOE or DoD client before any samples are analyzed.

8. Control of Records • Date and Time Requirement • Both date and time of preparation and analysis are considered essential information, regardless of the length of the holding time • Both shall be included in the laboratory records • If the time of sample collection is not provided, the laboratory must assume the most conservative time of day (i.e., earliest)

9. Data Integrity Training • A list of specifically prohibited practices must be provided to laboratory personnel during initial and annual integrity training • Fabrication, falsification, or misrepresentation of data • Improper clock setting or improper date/time recording • Unwarranted manipulation of samples, software, or analytical conditions • Misrepresenting or misreporting QC samples • Improper calibrations • Concealing a known analytical or sample problem • Failing to report the occurrence of a prohibited practice or known improper or unethical act

10. Environmental Conditions • Samples suspected of containing high concentrations of target analytes shall be isolated from other samples • Potentially high radiation samples must be segregated from other samples • Volatile organics samples must be segregated from other samples and extracts • Samples suspected of containing high concentrations of volatile organics shall be further isolated • A storage blank must be stored with all volatile organic samples, regardless of suspected concentration levels • Laboratories shall have documented procedures and criteria for evaluating storage blanks

11. Manual Integrations • When manual integrations are performed, raw data records shall include a complete audit trail for those manipulations • This requirement applies to all analytical runs including calibration standards and QC samples • The person performing the manual integration must sign and date each chromatogram and document the rationale for performing manual integration (electronic signature is acceptable) • Records for manual integrations may be maintained electronically as long as all requirements, including signature requirements, are met and the results can be historically reconstructed.

12. Support Equipment Table

13. Sample Disposal • Disposal of the physical sample shall occur only with the concurrence of the sample management office who submitted the sample • All conditions of disposal and all correspondence between all parties concerning the final disposition of the physical sample shall be recorded and retained • Records shall indicate the date of disposal, the nature of disposal (such as sample depleted, sample disposed in hazardous waste facility, or sample returned to client), and the name of the individual who performed the task.

14. Data Reporting • Identify the name of the laboratory contact person • Identify the total number of report pages • Each page is identified with the unique report identification • Identify all QC failures • Identify soil/sediment data as dry weight or as received • Identify reporting units • Identify date of issue • Provide information on non-standard conditions • Provide use and definition of data qualifiers • Provide a statement of compliance/noncompliance with requirements and/or specifications

15. Standard Data Qualifiers • (DoD ONLY Requirement) In the absence of project-specific requirements, the minimum standard data qualifiers are: • U – Analyte was not detected and is reported as less than the LOD or as defined by the client. The LOD has been adjusted for any dilution or concentration of the sample • J – The reported result is an estimated value (e.g., matrix interference was observed or the analyte was detected at a concentration outside the quantitation range) • B – Blank contamination. The recorded result is associated with a contaminated blank. • N – Non-target analyte. The analyte is a tentatively indentified compound using mass spectrometry. • Q – One or more quality control criteria failed (e.g., LCS recovery, surrogate spike recovery, or CCV recovery).

16. Integration of DOE Concept • Hazardous and Radioactive Materials Management and Health and Safety Practices • Radioactive Materials Management • Radiological Controls • TSCA Materials Control and Protection • Laboratory Safety and Health • Waste Management and Disposal

17. Target Analytes • Laboratories shall analyze those target analytes identified by the client on a project-specific basis • Laboratories shall analyze for analytes that are within their scope of accreditation • Laboratories need to work with and communicate to projects the analytes that are and are not on their scope of accreditation • Laboratories must obtain accreditation for analytes not on their scope or subcontract the analysis to a laboratory that has the accreditation

18. Limit of Detection (LOD) • Determination and Verification • Laboratories shall establish a detection limit (DL) using a scientifically valid and documented procedure • DLs are established for each suite of analyte-matrix-method, including surrogates • All sample processing steps of the analytical method shall be included in the determination of the DL • The DL shall be used to determine the LOD for each analyte and matrix, including all preparatory and cleanup methods routinely used

19. Limit of Quantitation (LOQ) • Establishment and Verification • The LOQ must be set within the calibration range (including the low calibration point) prior to sample analysis • The LOQ must be verified quarterly • Procedure for establishing the LOQ must empirically demonstrate precision and bias at the LOQ • The LOQ associated precision and bias must meet the client requirements and must be reported • If a method is modified the LOQ and its precision and bias must be demonstrated and reported

20. Calibration Verification • Initial Calibration Verification • Successfully completed prior to analyzing samples • Standard from second source (second lot is acceptable when only one manufacturer exists) • Concentration at or near the midpoint of the calibration range • Continuing Calibration Verification • Concentration between the low calibration standard and the midpoint calibration standard • Standard from same source as the initial calibration curve • Evaluation baseline is the initial calibration curve, except for retention times in organic chromatographic methods us ICV

21. Laboratory Control Sample • All target analytes must be spiked in the LCS (except for aroclor analysis) • Concentration of analytes shall be at project-specific concentrations of concern (if not specified, they shall be at or below the midpoint of the calibration curve) • Laboratory shall establish in-house control limits • Control limits must meet criteria specified by the project or as stated in the associated method • Control limits are statistically derived

22. Laboratory Control Sample (cont.) • Control limits shall be updated on an annual basis or as stated in the method (also after changes to the analytical process) • Do not exclude failed LCS data unless there is a scientifically valid reason • Control limits may not be greater than +3X the standard deviation of the mean • Marginal exceedances are only permitted for organic analytes • The same analyte exceeding the LCS control limit in two out of three consecutive LCS analyses is non-random behavior

23. Inclusion of DoD F-Tables • Table F-2: Organic Analysis by Gas Chromatography and HPLC (Methods 8011, 8015, 8021, 8070, 8081, 8082, 8330, etc.) • Table F-3: Nitroaromatics, Nitramines, and Nitrate Esters Analysis by HPLC (Method 8330B) • Table F-4: Organic Analysis by Gas Chromatography/Mass Spectrometry (Methods 8260 and 8270) • Table F-5: Dioxin/Furan Analysis by High-Resolution Gas Chromatography/Low-Resolution Mass Spectrometry (Method 8280) • Table F-6: Dioxin/Furan Analysis by High-Resolution Gas Chromatography/High-Resolution Mass Spectrometry (Method 8290)

24. Inclusion of DoD F-Tables (cont.) • Table F-7: Inorganic Analysis by Inductively Coupled Plasma (ICP) Atomic Emission Spectrometry and Atomic Absorption Spectrophotometry (AA) (Methods 6010 and 7000 series) • Table F-8: Trace Metals Analysis by Inductively Coupled Plasma/Mass Spectrometry (ICP/MS) (Method 6020) • Table F-9: Inorganic Analysis by Colorimetric Hexavalent Chromium (Method 7196) • Table F-10: Cyanide Analysis (Methods 9010, 9012, and 9014) • Table F-11: Common Anions Analysis (Method 9056) • Table F-12: Perchlorate Analysis (Methods 6850 and 6860)

25. Example of F-Table Content • Each F-Table Indentifies: • QC Checks • Minimum Frequencies • Acceptance Criteria • Corrective Actions • Flagging Criteria • General Comments

26. Example of F-Table Content (cont.) • Table F-2. Organic Analysis by GC and HPLC – QC Checks • Demonstration of Analytical Capability • LOD Determination and Verification • LOQ Establishment and Verification • Retention Time Width and Position for each Analyte and Surrogate • Breakdown Check • Minimum Five-Point Calibration (ICAL) for each Analyte • Second Source Calibration Verification (ICV)

27. Example of F-Table Content (cont.) • Table F-2. Organic Analysis by GC and HPLC – QC Checks • Continuing Calibration Verification (CCV) • Method Blank • Laboratory Control Sample (LCS) • Matrix Spike (MS and Matrix Spike Duplicate (MSD) • Surrogate Spikes • Positive Result Confirmation (second column/second detector)

28. QSM QSAS