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EPA 747-R-95-008September 1997METHODOLOGY FOR XRF PERFORMANCECHARACTERISTIC SHEETSTechnical BranchNational Program Chemicals DivisionOffice of Pollution Prevention and ToxicsOffice of Prevention, Pesticides, and Toxic SubstancesU.S. Environmental Protection Agency401 M Street, S.W.Washington, D.C. 20460
The material in this document has been subject to Agency technical and policy review andapproved for publication as an EPA report. Mention of trade names, products, or servicesdoes not convey, and should not be interpreted as conveying, official EPA approval,endorsement, or recommendation.This report is copied on recycled paper.
CONTRIBUTING ORGANIZATIONSThe methodology described in this report is part of a task funded by the U.S.Environmental Protection Agency and the U.S. Department of Housing and UrbanDevelopment. The task was managed by the U.S. Environmental Protection Agency. Thetask was conducted collaboratively by three organizations under contract to theEnvironmental Protection Agency: Battelle Memorial Institute, Midwest Research Institute,and QuanTech. Each organization's responsibilities are listed below.Battelle Memorial InstituteBattelle Memorial Institute (Battelle) was responsible for oversight of archive samplemaintenance and archive testing.Midwest Research InstituteMidwest Research Institute (MRI) was responsible for the operations manual,sample maintenance, collection of paint samples, laboratory analysis, and supervision oftesting.QuanTechQuanTech (formerly David C. Cox & Associates) was responsible for testing design,data management, development of statistical methods, and the writing of this report andthe XRF Performance Characteristic Sheets.U.S. Environmental Protection AgencyThe U.S. Environmental Protection Agency (EPA) co-funded the task, managed thetask, reviewed task documents, and managed the peer review of this report. The EPAProject Leader was John Schwemberger. The EPA Work Assignment Managers wereSam Brown, John Scalera and John Schwemberger. The EPA Project Officers were SamBrown, Jill Hacker, Phil Robinson, and Sineta Wooten.U.S. Department of Housing and DevelopmentThe Department of Housing and Urban Development (HUD) co-funded the task, andwas responsible for reviews of the XRF Performance Characteristic Sheets and forcontacts with the manufacturers of lead-based paint testing technologies. The key HUDstaff member was Bill Wisner.iii
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ACKNOWLEDGMENTSSpecial thanks are due to Mary McKnight of the National Institute of Standards andTechnology (NIST) for operating XRF instruments during archive testing and for her adviceand comments.v
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TABLE OF CONTENTSEXECUTIVE SUMMARY . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xix1.INTRODUCTION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11.1Background . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11.2Peer Review . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42.COMPLIANCE WITH QUALITY ASSURANCE PROJECT PLAN OBJECTIVES . . . . . . . . . . . . 73.ARCHIVE FACILITY TESTING AND REPORTING . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3.1Initial Testing of New Instruments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3.2Testing Practices . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3.3Analysis of Data and Release of the XRF Performance Characteristic Sheets . . . . . .3.4Future Improvements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .13131314154.SAMPLE DESCRIPTIONS AND SAMPLING PROTOCOL SUMMARY . . . . . . . . . . . . . . . . . .4.1Sample Descriptions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4.1.1 EPA/HUD Field Study Sample Descriptions . . . . . . . . . . . . . . . . . . . . . . . . . .4.1.2 Archive Sample Descriptions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4.2Component Makeup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4.3Distribution of Lead Levels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4.4Control Blocks and Quality Control Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4.5Order of Testing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4.5.1 Archive Sample Ordering . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4.6Testing Protocols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4.7EPA/HUD Field Study Data vs. Archive Facility Data . . . . . . . . . . . . . . . . . . . . . . . . . .4.8EPA/HUD Field Study Data vs. National Survey Data . . . . . . . . . . . . . . . . . . . . . . . . .1717171820202324242627315.PCS DEVELOPMENT AND STATISTICAL METHODOLOGY . . . . . . . . . . . . . . . . . . . . . . . . .5.1Bias and Precision Estimation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5.1.1 The XRF Measurement Model . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5.1.2 Data Used in Model Estimation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5.1.3 Estimation Using XRF Instrument Testing Data . . . . . . . . . . . . . . . . . . . . . . .5.1.4 Combining XRF Results from Different Testing Scenarios . . . . . . . . . . . . . . .5.1.5 Standard Error Estimates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5.1.6 Relation to Previous Work . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5.2Laboratory Measurement of Lead Levels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5.3Substrate Correction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5.3.1 Criteria for Recommending Substrate Correction . . . . . . . . . . . . . . . . . . . . . .5.3.2 Measurement Range Subject to Substrate Correction . . . . . . . . . . . . . . . . . .5.4Inconclusive Ranges and Thresholds . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5.4.1 Classification Using Inconclusive Ranges and Thresholds . . . . . . . . . . . . . . .5.4.2 Data Used in Inconclusive Range and Threshold Derivation . . . . . . . . . . . . .5.4.3 Model-Based Derivation of Inconclusive Ranges and Thresholds . . . . . . . . .5.4.4 Number of Decimal Places Reported . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5.4.5 Criteria for Inconclusive Range and Threshold Derivation . . . . . . . . . . . . . . .5.4.6 Use of 0.5 mg/cm2 and 2.0 mg/cm2 as Pivotal Values . . . . . . . . . . . . . . . . . . .5.4.7 Properties of Inconclusive Ranges and Thresholds . . . . . . . . . . . . . . . . . . . .5.4.8 Calculation of Inconclusive Ranges and Thresholds . . . . . . . . . . . . . . . . . . . .5.4.9 Classification Performance of Inconclusive Ranges and Thresholds . . . . . . .5.5XRF Calibration Check Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5.6XRF Re-evaluation Test Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . 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5.76.05.6.1 Re-Testing in Multifamily Housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5.6.2 Re-Testing in Single-Family Housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5.6.3 Examples of Re-Test Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5.6.4 Error in Re-Test Formula . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .XRF Results That Do Not Consist of Fixed Reading Time Measurements . . . . . . . . .6265666768REFERENCES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69APPENDIX A:A.1A.2A.3XRF INSTRUMENT OPERATING PROTOCOLS . . . . . . . . . . . . . . . . . . . . . . . . . . . .Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .Brief Description of Testing Areas . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .Summary of Testing Protocols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-1A-1A-1A-1APPENDIX B: METHODOLOGICAL ISSUES IN THE ANALYSIS OF XRF MEASUREMENTSWITH VARIABLE READING TIMES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B.1Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B.2Variable Reading Time Measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B.3A Model for Variable Reading Time Measurements . . . . . . . . . . . . . . . . . . . . . . . . . .B.3.1 Precision Mode Readings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B.3.2 Unlimited Mode Readings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B.4Nonparametric Inconclusive Ranges for Unlimited Mode Readings . . . . . . . . . . . . .B.5Substrate Correction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-1B-1B-2B-2B-3B-4B-5B-6APPENDIX C: XRF PERFORMANCE CHARACTERISTIC SHEETS ERRATA.C.1Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .C.2Errors Appearing in the “Instructions for Evaluating XRF Testing” Section . . . . . . . .C.3Errors Appearing in the MAP-3 PCS and Corrections . . . . . . . . . . . . . . . . . . . . . . . .C.4Errors Appearing in the LeadStar and MAP 4 PCSs and Corrections . . . . . . . . . . . .C.5Errors Appearing in the LPA-1 PCS and Corrections . . . . . . . . . . . . . . . . . . . . . . . . .C.6Errors Appearing in the Microlead I PCS and Corrections . . . . . . . . . . . . . . . . . . . . .C.7Errors Appearing in Titles of PCSs and Corrections . . . . . . . . . . . . . . . . . . . . . . . . . .C-1C-1C-1C-1C-2C-2C-2C-2APPENDIX D: XRF PERFORMANCE CHARACTERISTIC SHEETS AND RELATED RESULTS . . D-1D.1Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-1D.2XRF Performance Characteristic Sheet for the Advanced Detectors LeadStar andRelated Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-2D.3XRF Performance Characteristic Sheet for the Radiation Monitoring Device LPA-1and Related Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-17D.4XRF Performance Characteristic Sheet for the Scitec MAP-3 and Related Results. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-45D.5XRF Performance Characteristic Sheet for the Scitec MAP 4 and Related Results. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-59D.6XRF Performance Characteristic Sheet for the Warrington Microlead I Revision 4and Related Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-76D.7XRF Performance Characteristic Sheet for the TN Technologies Pb Analyzer andRelated Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-86D.8XRF Performance Characteristic Sheet for the Princeton Gamma-Tech XK-3 andRelated Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-95D.9XRF Performance Characteristic Sheet for the Niton XL-309 Spectrum Analyzerand Related Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-105APPENDIX E: XRF PERFORMANCE CHARACTERISTIC SHEET: AN EXAMPLE . . . . . . . . . . . . E-1viii
E.1E.2Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-1Example . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-1ix
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LIST OF TABLESTable 4-1.Table 4-2.Table 4-3.Table 4-4.Table 4-5.Table 4-6.Table 4-7.Table 4-8.Table 4-9.Table 4-10.Table 4-11.Table 4-12.Table 4-13.Table 4-14.Table 5-1.Table 5-2.Table A-1.Table A-2.Table D-1.Table D-2.Table D-3.Table D-4.Table D-5.Table D-6.Number of Test Locations Per Substrate by Dwelling in the EPA/HUD Field Study. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18The Originating City and Construction Date (if known) of Archive SamplesCategorized by Dwelling and Substrate Type . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21The Number and Overall Percent of Samples in the EPA/HUD Field Study for EachType of Component . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22The Number and Overall Percent of Samples in the EPA/HUD Archive Facility forEach Type of Component . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23Summary Statisti
Readings (Metal Substrates Corrected and Uncorrected), Classified Using Inconclusive Ranges Reported in the XRF Performance Characteristic Sheet For Instruments With Software Versions Earlier Than Version 4.1 .D-16 Table D-9. Threshold Results For Radiation Monitoring Device LPA-1 30-Second Standard Mode Readings For Results Where Substrate Correction Is Not Performed, But Substrate .
