ASTM_DS55S9-1976.pdf

FINAL REPORT on INTERLABORATORY COOPERATIVE STUDY OF THE PRECISION AND ACCURACY OF THE DETERMINATION OF SULFUR OXIDES IN GASEOUS COMBUSTION PRODUCTS(Barium Chloranilate Method)USING ASTM METHOD D 3226-73T J.E.Howes,Jr.,R.N.Pesut,and J.F.Foster Battelle Memorial Institute ASTM DATA SERIES PUBLICATION DS 55-S9 List price$12.00 05-055090-17#AMERICAN SOCIETY FOR TESTING AND MATERIALS 1916 Race Street,Philadelphia,Pa.19103 BY AMERICAN SOCIETY FOR TESTING AND MATERIALS 1976 Library of Congress Catalog Card Number:76-40798 NOTE The Society is not responsible,as a body,for the statements and opinions advanced in this publication.f 7 I Battelle is not engaged in research for advertising,sales I I promotion,or publicity purposes,and this report may I I not be reproduced in full or in part for such purposes.1 Printed in Lutherville-Timonium,Md.,December 1976 TABLE OF CONTENTS Page INTRODUCTION 1 SUMMARY OF RESULTS 2 EXPERIMENTAL PROGRAM 3 ASTM Test Method D 3226-73T 5 Apparatus 5 Pilot Plant Tests 11 Test Site Description 11 Spiking Procedure 17 Sampling Procedure.20 Test Pattern 22 Field Tests 25 Test Site Descriptions 25 Site 1 25 Site II 27 Site III 27 Sampling Procedure 27 Test Patterns 28 Analysis of Standard Sulfate Solutions 28 Participating Laboratories 28 STATISTICAL ANALYSIS OF SULFUR OXIDE TESTS 31 Statistical Measures 31 Measure of Precision 31 Measure of Accuracy 34 Experimental Results 34 Pilot Plant Tests 34 Field Tests 43 Analysis of Between-Laboratory and Within-Laboratory Components of Variance of Pilot Plant Data 53 Statistical Analysis of Field Test Data.63 Analysis of Accuracy 70 Analysis of Standard Nitrate Solutions 73*I TABLE OF CONTENTS Page DISCUSSION AND CONCLUSIONS.77 Between-Laboratory Component of Variance(Reproducibility).77 Within-Laboratory Component of Variance(Repeatability).79 Between-Laboratory Standard Error 79 Accuracy 79 RECOMMENDATIONS 82 REFERENCES 83 APPENDIX DETERMINATION OF SULFUR OXIDES IN FLUE GASES(BARIUM CHLORANILATE METHOD)11 LIST OF TABLES Page TABLE 1.RANGE OF MULTIFUEL FURNACE OPERATING CONDITIONS FOR SO TESTS X.13 TABLE 2.TARGET PATTERN OF SO SPIKE CONCENTRATIONS FOR PILOT PLANT TESTS AT BATTELLE.23 TABLE 3.SO SAMPLES TAKEN DURING PILOT PLANT TESTS 24 x TABLE 4.SUMMARY OF TEST SITE CHARACTERISTICS 26 TABLE 5.SAMPLING PATTERN FOR SO TESTS AT FIELD SITE II 29 x TABLE 6.SAMPLING PATTERN FOR SO TESTS AT FIELD SITE III 29 x TABLE 7.RESULTS OF PILOT PLANT SO DETERMINATIONS FOR BLOCKS IN WHICH LABORATORIES OBTAINED DUPLICATE SO-SPIKED SAMPLES(FIRST WEEK).35 TABLE 8.RESULTS OF PILOT PLANT SO DETERMINATIONS FOR BLOCKS IN WHICH LABORATORIES OBTAINED DUPLICATE SPIKED SAMPLES(SECOND WEEK)36 TABLE 9.RESULTS OF PILOT PLANT SO DETERMINATIONS FOR BLOCKS IN WHICH LABORATORIES OBTAINED DUPLICATE UNSPIKED SAMPLES(FIRST WEEK)37 TABLE 10.RESULTS OF PILOT PLANT SO DETERMINATIONS FOR BLOCKS IN WHICH LABORATORIES OBTAINED DUPLICATE UNSPIKED SAMPLES(SECOND WEEK)38 TABLE 11.RESULTS OF PILOT PLANT SO DETERMINATIONS FOR BLOCKS IN WHICH LABORATORIES OBTAINED CONCURRENT SO_-SPIKED AND UNSPIKED SAMPLES(FIRST WEEK)7 39 TABLE 12.RESULTS OF PILOT PLANT SO DETERMINATIONS FOR BLOCKS IN WHICH LABORATORIES OBTAINED CONCURRENT SPIKED AND UNSPIKED SAMPLES(SECOND WEEK)41 TABLE 13.RESULTS OF SULFUR OXIDE MEASUREMENTS AT FIELD TEST SITE I.44 TABLE 14.RESULTS OF SULFUR OXIDE MEASUREMENTS AT FIELD TEST SITE II 46 TABLE 15.RESULTS OF SULFUR OXIDE MEASUREMENTS AT FIELD TEST SITE III 49 TABLE 16.ANALYSIS OF VARIANCE TABLE 55 TABLE 17.BETWEEN-LABORATORY AND WITHIN-LABORATORY PRECISION FOR DETERMINATION OF DUPLICATE SPIKED SO.SAMPLES 57 iii LIST OF TABLES Page TABLE 18.BETWEEN-LABORATORY AND WITHIN-LABORATORY PRECISION FOR DETERMINATION OF DUPLICATE UNSPIKED SO SAMPLES 58 TABLE 19.BETWEEN-LABORATORY AND WITHIN-LABORATORY PRECISION FOR DETERMINATION OF DUPLICATE UNSPIKED S03 SAMPLES 59 TABLE 20.STATISTICAL ANALYSIS OF SO MEASUREMENTS PERFORMED AT FIELD TEST SITES X 66 TABLE 21.SUMMARY OF ACCURACY OF SO.DETERMINATIONS AS A FUNCTION OF SPIKE CONCENTRATION.7 72 TABLE 22.SUMMARY OF ACCURACY OF SO DETERMINATIONS BY LABORATORY.74 TABLE 23.RESULTS OF ANALYSIS OF STANDARD SULFATE SOLUTIONS FOLLOWING PILOT PLANT TESTS 75 TABLE 24.RESULTS OF ANALYSIS OF STANDARD SULFATE SOLUTIONS FOLLOWING FIELD TESTS 76 TABLE 25.BETWEEN-AND WITHIN-LABORATORY VARIATION IN THE RESULTS OBTAINED FROM ANALYSIS OF STANDARD SULFATE SOLUTIONS.78 IV LIST OF FIGURES Page FIGURE 1.CONDENSER COIL FOR COLLECTING SO/ELSO,6 3 2 4 FIGURE 2.DIMENSIONED DRAWING OF SO CONDENSATION COIL USED FOR TESTS OF D 3226-73T.7 FIGURE 3.MOUNTED COLLECTION SYSTEM WITH SO CONDENSER AND SO ABSORBERS.8 FIGURE 4.HEATED WATER SUPPLY SYSTEM FOR S03 CONDENSATION COILS.9 FIGURE 5.TYPICAL SO SAMPLING TRAIN 10 x FIGURE 6.SCHEMATIC DIAGRAM OF THE BATTELLE MULTIFUEL FURNACE ARRANGED FOR FIRING WITH FUEL OIL 12 FIGURE 7.MULTIFUEL FURNACE SETUP FOR GENERATING FLUE GASES FROM COMBUSTION OF NATURAL GAS OR FUEL OIL 14 FIGURE 8.OVERHEAD VIEW OF SAMPLING SYSTEM 15 FIGURE 9.DIMENSIONED SKET