ASTM International Proficiency Test Programs and Interlaboratory Studies Program Presenters: Steve Hepburn, PTP Director Phillip Godorov, ILS Director 1 ASTM Proficiency Testing Programs What is a Proficiency Testing Program? Designed as a statistical quality control tool enabling participating laboratories to assess their performance in conducting ASTM or other test methods Uniform samples are analyzed by participating labs using specified methods and results are reported for statistical treatment 2 September 2012 ASTM Proficiency Testing Programs ASTM : Provides management and administrative support to the program Program registration, contract negotiations for sample prep and distribution, data collection and generation of statistical summary reports Coordinates the preparation and distribution of test samples Sample are prepared by outside contractors Provides reporting instructions, worksheets and electronic data report forms for submitting data 3 September 2012 ASTM Proficiency Testing Programs • ASTM statistical summary reports include: Listing of all lab data Charts and graphs • Lab data is coded to maintain lab confidentiality. • Final summary reports are provided electronically to participants and appropriate Committee contacts. • ASTM Custom Company Reports – provided to companies with multiple lab performance data upon request. 4 September 2012 ASTM #2Diesel Fuel Sample ID: DF21102 Acid Number – D664 Lab data coded to maintain lab confidentiality 5 September 2012 ASTM Proficiency Testing Programs 6 September 2012 ASTM Proficiency Testing Programs Box and Whiskers graph to compare methods 7 September 2012 ASTM Proficiency Testing Programs Globally recognized programs: Over 4,300 laboratories participating Over 57% participation outside continental U. S. 8 September 2012 ASTM Proficiency Testing Programs Click here 9 ASTM Proficiency Testing Programs 10 ASTM Proficiency Testing Programs Metals Testing: (E28 and E01) Mechanical Properties Testing of Metals Plain Carbon and Low-Alloy Steel (Chemical Analysis) Stainless Steel (Chemical Analysis) Aluminum (Chemical Analysis) Determination of Gold in Bullion Plastics Testing: (D20) Polyethylene Plastics Testing Multiple Plastics - Mechanical Properties Testing Polypropylene - Mechanical Properties Testing Flammability of Plastics Testing Thermal Analyses of Plastics Elemental Analyses of Plastics 11 September 2012 ASTM Proficiency Testing Programs Aromatic Hydrocarbons Testing (D16) Engine Coolants Testing (D15) Electrical Insulating Liquids: (D27) Insulating Fluid Quality Dissolved Gas Analyses-In-Service Insulating Fluid Textiles :(D13) 12 Light, Medium, Heavy Fabric Testing Yarns and Threads September 2012 ASTM Proficiency Testing Programs Petroleum Products and Lubricants (D02) Turbine Oil Lubricating Grease Crude Oil In-Service Diesel Oil InService Hydraulic Fluids / Oils Base Oils Wax General Gas Oils Ultra Low Sulfur Diesel Fuel Ethanol Biodiesel(B100) Fuel Petroleum Coke 13 Engine Oil Lubricants #2 Diesel Fuel Aviation Turbine (Jet A) Fuel Motor Gasoline #6 Fuel Oil Automatic Transmission Fluid Gear Oil Reformulated Gasoline Hydraulic Fluids & Oils Lube Additives Industrial Gear Oil Naphtha September 2012 ASTM Proficiency Testing Programs ASTM's Cement and Concrete Reference Laboratory (CCRL) Works with • ASTM Committee C01 - Cement • ASTM Committee C09 - Concrete and Aggregates Located in Frederick, MD • Operates the following proficiency sample programs: • Portland cement • Hydraulic cement concrete • Masonry mortar • Blended cement • Pozzolans • Masonry cement • Concrete masonry units Visit the CCRL web site on ASTM web page for more information. 14 Use of Programs by Participants Lab QA Tool Data for monitoring lab strengths and weaknesses Residual sample material useful as internal QA sample Tool to evaluate other test methods for lab use Participation helps satisfy lab accreditation requirements Can demonstrate testing capability to customers Results and associated statistics helps ASTM validate test method performance under real world conditions 15 September 2012 Use of Programs by ASTM Committees Obtain valuable feedback on methods Resource for increased membership Database of laboratories for test method validation 16 September 2012 Establishing New Programs Concept approved by Executive Subcommittee Program pre-proposal Market research - survey Final program proposal Promote & Launch Bulk sample requirements Sample preparation and distribution ASTM staff will provide guidance and assistance. 17 September 2012 ASTM Proficiency Testing Programs The programs are open to all companies and industry test professionals worldwide. 18 September 2012 ASTM Proficiency Testing Programs For more information please contact: ASTM - PTP Steve Hepburn shepburn@astm.org Phone: (610) 832-9688 “Until a measurement is in a state of statistical control, it can not be believed in any logical sense that it's measuring anything at all." Dr. Churchill Eisenhart 19 September 2012 ASTM International Interlaboratory Study Program (ILS) Presenter: Phillip Godorov, ILS Director 20 September 2012 The Interlaboratory Study (ILS) Program Who we are and what we do … We were originated following approval by the Board of Directors to create a unit that would help to strengthen the perceived quality of ASTM Test Methods by: facilitating the production of data to develop Precision & Bias statements and Research Reports; providing administrative support to the committees; offering financial support to the committees; helping to ensure the confidentiality of participating labs. 21 September 2012 Administrative Support Review of Experimental Design Assistance identifying volunteer laboratories Identification of sample vendors Coordination of sample distribution Data collection Statistical processing Generation of reports 22 September 2012 Strengths of the ASTM Interlaboratory Study Program Input is encouraged from active Committee volunteers, as well as non-members, broadening the range and diversity of the study participants, allowing the study to most accurately demonstrate expected “real-world” precision Scientific neutrality of ASTM in reviewing test data Providing value-added Quality Assurance Programs to participating laboratories 23 September 2012 Potential Benefits of Participation Statistical program to monitor strengths and weaknesses of lab testing when compared to peers Assess testing performance and adherence to written procedures by lab technicians Recognition in the final Research Report Upon publication of the results of an ILS, all participating labs are eligible to receive a free 12 month listing in ASTM’s Lab Directory 24 September 2012 Benefits to the Committees Obtain valuable feedback on methods, leading to the correction of errors and omissions, as well as highlighting the need for technical updates Resource for increased membership Database of laboratories for test method validation Database of suppliers for common study materials 25 September 2012 Establishing New Programs Concept registered as a Work Item Program registered online as an ILS Initial conference call, with the a technical contact from the committee, to establish the basic study parameters Experimental design (with input from the committee’s statistical support person, if available) Identification of study materials, suppliers, a distributor, and volunteer laboratories 26 September 2012 Administering Programs Conference Calls or Virtual Meetings with the participants to discuss specific study instructions Coordination of acquisition and distribution of study material Physical Electronic Collection of data Analysis of data Compilation of Precision Statement and Draft Research Report (from registered information) 27 September 2012 Precision To calculate precision, we need usable data from at least six laboratories. The closer that we can get to 30 participants, the better. The precision statement in an ASTM test method is not meant to qualify it as good or bad. The published precision is there to help a user of the standard understand what can be expected based on the real world results of others. 28 September 2012 The Statistics (in a nutshell) ~ ASTM E691 All of the test results from one laboratory on one material constitute a cell. The cell average is calculated for each laboratory. The standard deviation of the test results in each cell is calculated. Then we calculate the average of all the cell averages for any one material – this shows up in the P&B as the “average.” For each laboratory we calculate the cell deviation by subtracting the cell average from the average of all the cell averages. Finally, we calculate the Standard Deviation of the Cell Averages. 29 September 2012 Repeatability (r) ranges With 95% confidence, the same operator, in the same laboratory, using the same equipment, under the same conditions, should obtain results when testing the same material that agree within this range. Example: repeatability range = 2.4 ppm Result 1: 79.1 ppm Result 2: 81.6 ppm Results differ by 2.5 ppm, therefore: Suspect Internal laboratory investigation may be advisable 30 September 2012 Reproducibility (R) ranges With 95% confidence, two operators, in different laboratories, using different equipment, under conditions meeting those specified in the standard, should obtain results when testing the same material that agree within this range. Example: reproducibility range = 3.2 ppb Result from lab 1: 50.8 ppb Result from lab 2: 47.9 ppb Results differ by 2.9 ppb, therefore: As Expected 31 September 2012 Bias To calculate bias, we need to include a reference “standard” among the sample specimens distributed to the participating laboratories. Bias may be determined as the average discrepancy between the “known” value and the reported values. 32 September 2012 Precision and Bias 33 September 2012 Remember … You can correct for bias. You cannot correct for imprecision. An ILS can be used to demonstrate improvement as standards are modified. Compare results from Method 1 with those from Method 2 The presence of a Precision Statement can make a standard stronger, but it doesn’t make it more repeatable. 34 September 2012 Research Reports The ASTM Form and Style Manual (Section A29.1) states, "Where numerical data have been generated to establish the precision and bias of a test method, a research report is required.” ASTM Research Report Template The draft research report should be made available to committee members while the associated precision statement is on ballot. Research report numbers are assigned after the ballot is approved. 35 September 2011 Parts of a Research Report List of participating laboratories Description of samples with their suppliers A copy of the laboratory instructions Description of equipment / apparatus used All of the raw data (lab names hidden) A statistical summary A copy of the precision and bias statement 36 September 2012 Research Report Assistance ILS can assist with the following research report tasks: Answer any research report inquiries Create research reports from ILS studies Reformat older research reports to fit the ASTM research report Template Assign research report numbers 37 September 2012 Research Report Numbers A research report number will be assigned by ASTM when all of the following have been completed: the research report is submitted to ILS; it has been reviewed for completeness; the ballot item to include the corresponding precision and bias statement is approved for publication. 38 September 2012 ILS informational Web pages http://www.astm.org/ILS/ 39 September 2012 40 September 2012 41 September 2012 42 September 2012 43 September 2012 If you are updating an ILS that you’ve already started When you are starting a brand new ILS 44 September 2012 First Page of the Registration 45 September 2012 Technical Contact 46 September 2012 Analyses 47 September 2012 Replicates 48 September 2012 Materials 49 September 2012 Suppliers 50 September 2012 Suppliers Continued… 51 September 2012 Distributor 52 September 2012 Laboratories 53 September 2012 Statistical Support 54 September 2012 ILS Registration Summary 55 September 2012 ILS Stats Number of active ILS programs Number of committees participating Number of programs registered in 2011 Number of programs registered so far in 2012 Total number of programs completed Number of programs completed in 2011 Number of programs completed so far in 2012 % of programs for new test methods Average amount of time taken to complete an ILS (months) Range of time taken to complete an ILS (months) 56 312 79 104 65 291 67 26 35 18 52 September 2012 Questions 57 ASTM International Interlaboratory Study Program (ILS) Phillip Godorov Director, Interlaboratory Study Program ASTM International 100 Barr Harbor Drive West Conshohocken, PA 19428-2959 Phone: 610-832-9715 Fax: 610-834-7011 E-mail: pgodorov@astm.org 58 September 2012 Thank you for your participation! Proficiency / Interlaboratory Crosscheck Testing Programs Interlaboratory Study Program (ILS) 59 September 2012