ASTM_DS55S2-1974.pdf

FINAL REPORT on INTERLABORATORY COOPERATIVE STUDY OF THE PRECISION AND ACCURACY OF THE MEASUREMENT OF TOTAL SULFATION IN THE ATMOSPHERE USING ASTM METHOD D 2010 J.F.Foster,G.H.Beatty and J.E.Howes,Jr.Battelle Memorial Institute ASTM DATA SERIES PUBLICATION DS 55-S2 List price$5.00 05-055020-17 AMERICAN SOCIETY FOR TESTING AND MATERIALS 1916 Race Street,Philadelphia,Pa.19103 BY AMERICAN SOCIETY FOR TESTING AND MATERIALS 1974 Library of Congress Catalog Card Number:74-76284 NOTE The Society is not responsible,as a body,for the statements and opinions advanced in this publication.IBattelle is not engaged in research for advertising,sales f promotion,or publicity purposes,and this report may I not be reproduced in full or in part for such purposes.I Printed in West Point,Pa.April 1974 TABLE OF CONTENTS Page INTRODUCTION 1 SUMMARY 2 EXPERIMENTAL PROGRAM 3 Characteristics of ASTM Method D 2010 3 Test Procedure .3 Test Pattern 4 Spiking Procedures 4 Test Sites 4 Site No.1,Los Angeles,California 4 Site No.2,Bloomington,Indiana 7 Site No.3,Manhattan,New York City 7 Participating Laboratories 7 STATISTICAL ANALYSIS OF SULFATION MEASUREMENTS 10 Statistical Measures 10 Reproducibility 10 Repeatability 11 Accuracy 11 Experimental Results 11 Analysis of Reproducibility 15 Analysis of Repeatability 19 Analysis of Accuracy 22 Analysis of Between-Rack and Within-Rack Variability 27 DISCUSSION AND CONCLUSIONS 27 RECOMMENDATIONS 28 ACKNOWLEDGEMENTS 29 REFERENCES 31 APPENDIX STANDARD METHOD FOR EVALUATION OF TOTAL SULFATION IN ATMOSPHERE BY LEAD PEROXIDE CANDLE 35 STANDARD METHODS OF TEST FOR SULFATE ION IN WATER AND WASTE WATER 39 LIST OF TABLES Page Table 1.Statistical Design of Sulfation Experiments 5 Table 2.Data From Sulfation Experiments at Los Angeles 12 Table 3.Data From Sulfation Experiments at Bloomington 13 Table 4.Data From Sulfation Experiments at Manhattan 14 Table 5.Summary of Between-Laboratory Variability(Reproducibility)of Sulfation Rate Measurements 16 Table 6.Summary of Within-Laboratory Variability(Repeatability)of Sulfation Rate Measurements 20 Table 7.Summary of Sulfate Spike Recovery Data 23 LIST OF FIGURES Page Figure 1.Diagram of Placement of the Sulfation Stations(D 2010).6 Figure 2.Arrays of Dustfall Collectors(D 1739)and Total Sulfation Detectors(D 2010)on Rooftop Racks at Los Angeles 8 Figure 3.Ground Level Site at Columbus,Ohio,of the Dustfall(D 1739)and Total Sulfation(D 2010)Test Started at Bloomington,Indiana 9 Figure 4.Least-Squares Curve Showing the Relationship Between Reproducibility and Sulfation Rate 18 Figure 5.Least-Squares Curve Showing the Relationship Between Repeatability and Sulfation Rate 21 Figure 6.Relationship of Estimated Spiking Rate to Actual Spiking Rate at Los Angeles 24 Figure 7.Relationship of Estimated Spiking Rate to Actual Spiking Rate at Bloomington 25 Figure 8.Relationship of Estimated Spiking Rate to Actual Spiking Rate at Manhattan .26 XI INTERLABORATORY COOPERATIVE STUDY OF THE PRECISION AND ACCURACY OF THE MEASUREMENT OF TOTAL SULFATION IN THE ATMOSPHERE USING ASTM METHOD D 2010 by J.F.Foster,G.H.Beatty,and J.E.Howes,Jr.INTRODUCTION This report presents the results obtained from an experimental study of the variability inherent in measurements of total sulfation,using ASTM Method D 2010v .The evaluation of Method D 2010 was per-formed as part of the first phase of Project Threshold,a comprehensive program to validate ASTM methods for measuring various atmospheric contam-inants.In addition,methods for measuring the content of nitrogen dioxide(D 1607),sulfur dioxide(D 2914),lead(D 3112),dustfall(D 1739),and particulate matter(D 1704)in the atmosphere have also been evaluated during Phase 1.Project Threshold is a multiphase program sponsored by American Society for Testing and Materials to provide tested methods for measuring contaminants in both ambient air and in source emissions.Tests of the methods are performed by groups of competent laboratories who are brought together at field locations for concurrent analysis of actual ambient and source atmospheres.Coordination of the Threshold program has been performed by Battelles Columbus Laboratories.The following section provides a brief summary of the results of the study of Method D 2010.Subsequent sections include detailed descriptions of the test method,test procedure,test sites,and the statistical analysis of the experimental data.*References at end of report.DS55S2-EB/Apr.1974Copyright 1974 by ASTM International www.astm.org SUMMARY OF RESULTS A statistical analysis of 79 total sulfation determinations performed in accordance with ASTM Method D 2010 produced the following results:The standard deviation,s,for variations among single sulfation rate measurements by different laboratories(reproducibility)is related to the mean sulfation rate,m,as follows:s,=0.0136)m 2 where,s,and,m,are given in mg/cm-day.This relationship is based on measurements at three sulfation rates over the range of 0.00178 to 0.01371 mg/c