1	IMPLEMENTATION OF THE PERFORMANCE TESTING PROGRAM UNDER NELAC – The SPEX CertiPrep Solution Dr. Ralph H. Obenauf Vanaja Sivakumar SPEX CertiPrep 203 Norcross Ave, Metuchen, NJ 08840
2	History of PE/PT Programs Under CWA, SDWA EPA Supplied PT’s 1994: USEPA Ends PT Program 1995: NELAC Forms PT Committee to Fill Void 1996: EPA Announced PT Privatization 1998: NIST/NVLAP As PTOB/PTPA 1999: NVLAP Approves First Set Of PT Providers
3	GOALS OF THE PROGRAM Continue Monitoring Compliance of Labs Under CW ACT, SDW ACT, etc. Assure Data Quality Required by Environmental and Regulatory Programs Keep USEPA Data Base Updated Improve Performance of Labs Over Time
4	THE NEW NELAC PROGRAM USEPA, NELAC, Individual States Have Authority to Set Standards Organize PT Program by PT FOT Start with WP and WS Programs Mirroring Historical Studies Expand Analytes and Matrices Over Time Set Concentration Ranges, Develop Regression Equations
5	IMPLEMENTATION OF NELAC PROGRAM BY SPEX CERTIPREP Manufactured and distributed CRMs for Over 45 Years USEPA CRADA Partner for QC Samples Beginning in 1991 Supplied QC Samples (Mirror PT Samples) for 10 Years
6	IMPLEMENTATION OF NELAC PROGRAM BY SPEX CERTIPREP Well Defined, ISO 9001 Quality System Accredited by UL Since 1994 Leader in Traceability and Certification Technically Qualified, Skilled Personnel World-Wide Distribution System
7	APPROVAL PROCESS: Components of Accreditation: (NELAC Criteria) 1. Qualifications 2. Quality System 3. On-Site Assessments By PTOB 4. Proficiency Testing Samples 5. On-Going Quality Assurance/Quality Control
8	QUALITY SYSTEMS FOR PT PROVIDERS ISO Standard 17025 (Test and Cal. Labs) ISO 9001 ISO Guide 34 (Production of Raw Materials) ISO Guide 43 (Proficiency Testing) NELAC Documents NIST Handbook 150-19 (Req. for PT’s) NIST Handbook 150 (Req. For Cal. Labs)
9	ASSESSMENT CRITERIA ISO GUIDE 17025/9001 Quality Policy and Objectives Management Commitment and Responsibilities Quality System Contract Review Design Control Document Control Purchasing Subcontracting Product Identification and Traceability
10	ASSESSEMENT CRITERIA ISO 17025/9001 Process Control Inspection and Testing Calibration Control of Nonconforming Products Corrective and Preventive Action
11	ASSESSMENT CRITERIA ISO 17025/9001 Handling Storage & Shipping Quality Records Internal Quality Audits Training Statistical Techniques
12	ASSESSEMENT CRITERIA NIST Handbook 150-19 Accuracy of Value Assignment Homogeneity Stability Traceability to SRM’s Equal Challenge USEPA Criteria Sample Design (Analytes/Concentrations) Use of Regression Equations & Evaluation
13	ASSESSMENT CRITERIA NELAC CHAPTER 2 (PT) APPENDIX A – Provider Qualifications APPENDIX B – Sample Specs, WS/WP APPENDIX C – Scoring Criteria, WS/WP APPENDIX D – PTOB/PTPA APPENDIX E – Microbiology APPENDIX F – WET (Effluent Tox) APPENDIX G – Radiochemistry APPENDIX H - Air
14	NELAC IMPLEMENTATION PT Testing, Direst and Indirect ON-SITE Assessment by NVLAP Quality Assurance Activities
15	DESIGN OF PT STUDES Drinking Water (WS Studies) Historical Extended NELAC Analytes from NELAC Field of Testing Waste Water ( WP Studies) Historical Extended NELAC Analytes DMRQA Federal Studies
16	SAMPLE DESIGN Follow EPA (NERL Ci0045) Criteria Provide Labs Equal Challenge Use Random Numbers to Select Concentrations within Range Follow Historical Design Guidelines Basis for Separation of Analytes Stability Regression Equations from Historical Data Rules for Number of Analytes Required to be Presented
17	MANUFACTURE Obtain Raw Materials Analyze for Impurities Analyte Content Batch Plan Weigh Components Dissolve and Dilute Seal in Pre-cleaned Ampoules Autoclave as Required
18	BATCH PLAN SHEET
19	ASSIGNED VALUE Must Meet Specifications: NIST 150-19 NELAC Chspter 2 and Appendices State Specific Documents Verify Assigned Value: Agreement with Gravimetric Value Associated Uncertainty Traceable to NIST SRM Homogeneity
20	ASSIGNED VALUE NIST CRITERIA FOR ACCEPTANCCE Published in NIST Handbook 150-19 Criteria #1: Provider’s QC Analytical Mean Shall be Within the Prepared (Target) Value +/- 1/3 the Acceptance Limits as calculated for the Labs Under Test Discard Batch if Outside Limits
21	ASSIGNED VALUE (NIST CRITERIA Cont.) Example Assigned Value For Be = 80 ppb Verification Analysis Value of Nine Random Ampoules from Beginning, Middle and End of Run: 79.1, 79.3, 79.8, 79.4, 79.6, 79.3, 79.5, 79.4, 79.6 AVERAGE = 79.4 PPB; SD = 0.207 SD (From EPA Reg. Equ.) = 3.96 Accept. Limit = 3x3.96 = 11.88 Provider Accept Range = 80 +/-3.96 = 76.0 – 84.0 Mean Recovery = 78.66 Lab Acceptance Range = 78.66 +/-11.87
22	ASSIGNED VALUE (NIST CRITERIA Cont.) Criteria #2 Method Repeatability (Expressed as a SD) Shall be Less than 1/6 of Lab Acceptance Limits of the Lab Under Test Discard Batch if Outside Limits
23	Assigned Value (NIST CRITERIA Cont.) Example USEPA Regression Equ. SD = 3.96 Verification Anal. SD < 1/6 of Acceptance Limit = 3*3.96/6 = 1.98 For Be Example: Method Repeatability (SD) = 0.212 0.212 < 1.98
24	ASSIGNED VALUE NELAC CRITERIA Criteria #1 Relative SD of Verification Analysis (Measured SD) Shall Be Less Than 50% of the Relative SD (from EPA Regression Equations) Predicted by the Assigned Value
25	ASSIGNED VALUE (NELAC CRITERIA CONT.) Criteria #2 Mean of the Verification Analysis Shall be Within the True Value +/- 1.5SD as Calculated from the EPA Regression Equations
26	EVALUATION Mean Recovery Estimated Mean Recovery X = aT + b Where: a & b Are Constants T = Assigned Value Estimated SD: S = cT + d Where: c & d Are Constants
27	ACCEPTANCE LIMITS Water Pollution (WP) Studies Acceptance Limits (For Labs): Estimated Mean Recovery +/- 3SD Warning Limits (Check For Error): Estimated Mean Recovery >+/- 2SD
28	ACCEPTANCE LIMITS Drinking Water Studies (WS) Acceptance Limits:: Estimated Mean Recovery +/- 2 Standard Deviations
29	FILES TO EPA/NIST At Start of Study Send File in ASCII INI, WPCHEM, 200392-0, P0100, 0036, 6-20DEM-PT, 27, Milligrams/L, 15.0, 37.3, 18.7, 33.6 INI, Study Type, Provider #, Target Value, Units, Acceptance Limits, Warning Limits Uncertainty Associated With Assigned Value
30	UNCERTAINTY Associated With Preparation Purity Of Raw Material Weighing Make Up To Volume
31	UNCERTAINTY EXAMPLE CALCULATION Uncertainty For Minerals Minerals Contain: CALCIUM CHLORIDE MAGNESIUM CHLORIDE SODIUM FLUORIDE POTASSIUM SULFATE SODIUM BICARBONATE
32	UNCERTAINTY (MINERALS CALC. CONT.) Steps Involved: Weighing CaCl, MgCl, NaF, KSO4, NaHCO3 Dilution to Volume Taking Test Aliquot Uncertainty Factor For Mg: U_mg(combined) = [S{U_i/(V_i)}²]^1/2
33	FINAL FILES TO EPA/NIST After Close of Study Final (Provider) Assigned Values Assigned Values for Some Analytes (EG TRESCL, FRESCL, Conductance, TDS) Are Study Averages Study Summary (# Labs, # Pass/Fail) Study Data Files (Raw Data From All Labs)
34	REPORTS Sent To: Participants Agencies As Requested By The Laboratories
35	STUDY TIMETABLE Day 1: Start of Study Day 45: Close of Study (All Data Must be Submitted) Day 49-55: Acceptance Limits Released (Optional) Day 66: Last Day For Provider to Submit Reports To: NIST/EPA STATE AGENCIES PARTICIPANTS
36	HELPFUL HINTS Verify Your Analytical Method Produces DL’s Lower than the Lowest Concentration (Range) on the Instruction Sheet. Observe Clean Lab Procedures and Techniques Use Appropriate QC Samples Read the Instructions EVERY TIME You Analyze PT Samples
37	HELPFUL HINTS Carry Blanks Through All Procedures Report Your Lab ID As: Your State Abbreviation Followed by Your Five Digit Numerical Code: eg: NJ00123 Report Method Descriptions Using the Standardized Format: Identification of the Origin of the Method, eg. EPA, ASTM, SM, etc. Followed by the Method Number EX: SM 4500-NH3B
38	New Method NELAC Codes Listed on NELAC Web Site Standardized Method Code Format Eight digits long Digits 1,2: Source code: EPA 10, SM 20… Digits 3,4,5,6,7: Heart of Code Digit 8: Units Check Sum
39	HELPFUL HINTS Never Use “>” Be Careful Reporting “Not Detected” Use < sign in front of DL Do not use Alpha’s (ND,BDL) These Score As Not Evaluated Be careful when using < Implies Reported Value of Zero Report Results to Three Significant Figures
40	HELPFUL HINTS Make Up/Use Only Fresh Ref. Materials Use Only Approved Methods Confirm That Your Reported Values Lie Within the Range on the Instruction Sheet Conduct an Independent Review of All Data