ASTM_DS55S5S6S8-1975.pdf

FINAL REPORTS on Interlaboratory Cooperative Study of ftQ 55-S5 the Precision and Accuracy of the*J*J ww Measurement of Lead in the Atmosphere Using the Colorimetric Dithizone Procedure Interlaboratory Cooperative Study of IQ 55-S6 thePrecisin of Sampling Stacks for w particulates and Collected Residue DS 55-S8 Interlaboratory Cooperative Study of the Precision and Accuracy of the Determination of Oxides of Nitrogen in Gaseous Combustion Products(Phenol Disulfonic Acid Procedure)Using ASTM Method D 1608-60 ASTM DATA SERIES PUBLICATIONS List price$18.00 05-055099-17 ft AMERICAN SOCIETY FOR TESTING AND MATERIALS 1916 Race Street,Philadelphia,Pa.19103 BY AMERICAN SOCIETY FOR TESTING AND MATERIALS 1975 Library of Congress Catalog Card Numbers:DS 55-S5 74-76287 DS 55-S6 74-76288 DS 55-S8 74-76291 NOTE The Society is not responsible,as a body,for the statements and opinions advanced in this publication.Battelle is not engaged in research for advertising,sales promotion,or publicity purposes,and this report may not be reproduced in full or in part for such purposes.Printed in Baltimore,Md.June 1975 CONTENTS Interlaboratory Cooperative Study of the Precision and Accuracy of the Measurement of Lead in the Atmosphere Using the Colorimetric Dithizone ProcedureDS 55-S5 see white section Interlaboratory Cooperative Study of the Precision of Sampling Stacks for Particulates and Collected ResidueDS 55-S6 see gray section Interlaboratory Cooperative Study of the Precision and Accuracy of the Determination of Oxides of Nitrogen in Gaseous Combustion Products(Phenol Disulfonic Acid Procedure)Using ASTM Method D 1608-60DS55-S8 see white section following gray section Related ASTM Publications Inter laboratory Cooperative Study of the Precision and Ac-curacy of the Measurement of Nitrogen Dioxide Content in the Atmosphere Using ASTM Method D 1607,DS 55(1974),$5.00,05-055000-17 Inter lab oratory Cooperative Study of the Precision and Ac-curacy of the Measurement of Sulfur Dioxide Content in the Atmosphere Using ASTM Method D 2914,DS 55-S1(1974),$5.00,05-055010-17 Inter laboratory Cooperative Study of the Precision and Ac-curacy of the Measurement of Total Sulfation in the At-mosphere Using ASTM Method D 2010,DS 55-S2(1974),$5.00,05-055020-17 Inter laboratory Cooperative Study of the Precision of the Measurement of Particulate Matter in the Atmosphere(Optical Density of Filtered Deposit)Using ASTM Method D 1704,DS 55-S3(1974),$5.00,05-055030-17 Inter laboratory Cooperative Study of the Precision and Ac-curacy of the Measurement of Dustfall Using ASTM Method D 1739,DS 55-S4(1974),$5.00,05-055040-17 Inter laboratory Cooperative Study of the Precision of the De-termination of the Average Velocity in a Duct(Pitot Tube Method Using ASTM Method D 3154-72;DS 55-S7(1974),$5.00,05-055070-17 Inter laboratory Cooperative Study of the Precision and Ac-curacy of the Determination of the Relative Density of Black Smoke(Ringelmann Method)Using ASTM Method D 3211-73 T,DS 55-S10(1974),$5.00,05-055100-17 INTERLABORATORY COOPERATIVE STUDY OF THE PRECISION AND ACCURACY OF THE MEASUREMENT OF LEAD IN THE ATMOSPHERE USING THE COLORIMETRIC DITHIZONE PROCEDURE J.F.Foster,G.H.Beatty,and J.E.Howes,Jr.Battelle Memorial Institute ASTM DATA SERIES PUBLICATION DS 55-S5 TABLE OF CONTENTS Page INTRODUCTION 1 SUMMARY OF RESULTS 2 Particulate Lead 2 Precision.2 Accuracy *.2 Vaporous Lead 3 Precision 3 Accuracy 3 EXPERIMENTAL PROGRAM 3 Test Method Description.3 Sampling Apparatus 4 Sample Generating System 4 Test Pattern 9 Spiking Procedure 15 Particulate Lead 15 Vaporous Lead 15 Participitating Laboratories 16 STATISTICAL ANALYSIS OF LEAD MEASUREMENTS 16 Statistical Measures 16 Measure of Precision 16 Measure of Accuracy 19 Analysis of Particulate Lead Data 19 Experimental Results 19 Between-Laboratory and Within-Lahoxatojjy Precision Estimates,.23 Accuracy 30 Analysis of Vaporous Lead Data 33 Experimental Results 33 Precision Estimates.33 Accuracy 35 DISCUSSION AND CONCLUSIONS Particulate Lead 39 Vaporous Lead 40 RECOMMENDATIONS 42 TABLE OF CONTENTS(Continued)Page ACKNOWLEDGEMENTS 43 REFERENCES 45 APPENDIX A TENTATIVE METHOD OF TEST FOR LEAD IN THE ATMOSPHERE 49 APPENDIX B STATISTICAL ANALYSIS PROCEDURES .69 APPENDIX C PRACTICAL APPLICATIONS OF THE STATISTICAL MEASURES GENERATED FROM THE COOPERATIVE STUDY OF THE LEAD METHOD(D 3112)77 n LIST OF TABLES Page TABLE 1.TEST PATTERN FOR PARTICULATE LEAD DETERMINATIONS AT SITE I.12 TABLE 2.TEST PATTERN FOR PARTICULATE LEAD DETERMINATIONS AT SITE II.13 TABLE 3.TEST PATTERN FOR PARTICULATE LEAD DETERMINATIONS AT SITE III.14 TABLE 4.DATA FROM PARTICULATE LEAD ANALYSIS AT LOS ANGELES(SITE I).20 TABLE 5.DATA FROM PARTICULATE LEAD ANALYSIS AT BLOOMINGTON(SITE II).21 TABLE 6.DATA FROM PARTICULATE LEAD ANALYSIS AT MANHATTAN(SITE III).22 TABLE 7.SUMMARY OF PARTICULATE LEAD DATA REJECTED FROM STATISTICAL ANALYSIS.24 TABLE 8.ANALYSIS OF VARIANCE,BY SITE,FOR ALL UNSPIKED SAMPLES OF PARTICULATE LEAD 28 TABLE 9.ANALYSIS OF VARIANCE