_STP_540-1988.pdf

SAMPLING,STANDARDS AND HOMOGENEITY A symposium presented at the Seventy-fifth Annual Meeting AMERICAN SOCIETY FOR TESTING AND MATERIALS Los Angeles,Calif.,25-30 June 1972 ASTM SPECIAL TECHNICAL PUBLICATION 540 W.R.Kennedy,symposium chairman J.F.Woodruff,co-chairman 04-540000-34#AMERICAN SOCIETY FOR TESTING AND AAATERIALS 1916 Race Street,Philadelphia,Pa.19103 B Y AMERICAN SOCIETY FOR TESTING AND MATERIALS 1973 Library of Congress Catalog Card Number:73-80190 ISBN 0-8031-0561-4 NOTE The Society is not responsible,as a body,for the statements and opinions advanced in this publication.Printed in Baltimore,Md.September 1973 Second Printing,Mars,Pa.March 1986 Third Printing,Mars,Pa.October 1988 Foreword The Symposium on Sampling,Standards and Homogeneity was pre-sented at the Seventy-fifth Annual Meeting of the American Society for Testing and Materials held in Los Angeles,Calif.,25-30 June 1972.The symposium was sponsored by ASTM Committee E-2 on Emission Spec-troscopy.W.R.Kennedy,American Cast Iron Pipe Co.,presided as the symposium chairman,and J.F.Woodruff,Armco Steel Corp.,served as co-chairman.Related ASTM Publication Manual on Quality Control of Materials,STP 15 C(1951),04-015030-34 Contents Introduction 1 To Sample the MoonA.W.ENGLAND 3 A Lunar Sample 3 Conclusion 15 Role of Homogeneity in Powder Samplingc.L.GRANT AND P.A.PELTON 16 Sampling Theory 18 Experimental Work 22 Results 25 How to Sample a MountainJ.J.CONNOR AND A.T.MTERS 30 A Model of Geochemical Variation 31 The Problem of Geochemical Error 33 A Geochemical Example 34 Conclusion 36 Collection and Handling of Physical Evidence for a Forensic Laboratory P.C.BUSCEMI AND W.D.WASHINGTON 37 Protecting the Scene of a Crime 38 Documentation of the Location 39 Collection of the Potential Evidence 39 Preservation of the Evidence 41 Labeling Requirements 42 Chain-of-Custody Considerations 42 Letter of Transmittal 43 Collection of Reference Materials 43 Conclusion 43 How and What to Sample in the Analytical GapJ.p.WALTERS AND S.A.GOLDSTEIN 45 Instrumentation for Stabilization 46 Instrumentation for Viewing the Discharge 51 What to View 56 Fully Resolved Spectra 62 Practical Application 67 Problems in Manufacture of National Bureau of Standards Cast Metal Standard Reference Materialsw.R.KENNEDY 72 The Ductile Irons 72 The Blast Furnace Irons 81 The Cast Steels and High Temperature Alloys 84 The Combination Chemical Spectrographic SRMs 85 Conclusion 87 CONTENTS Problems in Sampling Ferroalloys with Emphasis on Ferrosiliconj.c.CLINE 88 Manufacturing Procedures for Ferroalloys 88 Metallurgical Structures of Ferrosilicon 89 Sampling Procedure 91 Selection of the Sample 92 Conclusions 96 Sampling and On-Stream X-Ray Control of Portland Cement Raw Mix SlurryCLYDE W.MOOEE AND C.DAVID MAARS 97 Laboratory Investigation 99 Plant Raw Mix Control 102 Conclusions 108 Sampling and Analysis for an Oxygen Steel Shopc.B.JENKINS AND G.C.SOTH 110 Sampling of Preliminary Steel Samples 110 Analysis of Preliminary Steel Samples 112 Sampling for Final Heat Analysis 114 Discussion 116 Alternative Sampling and Analysis Methods 119 Slag Samples 121 Summary 121 Paper Fiber Filters for Sampling Trace Metals in Airborne Particulate MatterT.Y.KOMETANI,J.L.BOVE,AND B.NATHANSON 123 Experimental 124 Discussion 126 Conclusion 131 STP540-EB/Sep.1973 Introduction While the analyst is always confronted with a sample problem,he encounters a definite homogeneity problem less often and he seldom has to deal with the standards making problems.While many have been aware that the three entities,sampling,standards and homogeneity,are all closely bound,it has been only recently recognized through E2 Subcommittee 04 discussions how necessary it is that we define these three aspects of the sample.All of the papers presented at the symposium could not be included in this Special Technical Pubhcation for various reasons,but problems in the manufacture of some standards are covered.Sampling of various products,such as ferrosilicon and cement are covered as well as the two foremost subjects of ecologyair and water:probably the two most difficult fields today.The difficulty in these latter two fields probably arises in a definition of homogeneity.While air and water may be polluted,they are only polluted locally.Where the sample is taken,and when,are very important things to know.The statistics of homogeneity is needed to help define the direction in finding a needed handle to measure jts goodness or poorness.The paper given in this publication certainly points in the right direction.In emission spectroscopy,one cannot discuss the sample without con-sidering the means of volitilization or excitation or both to produce the spectra.Such a fundamental picture of excitation appears here.One hopes that further efforts in this direction will help us understand the sample problem.An outstanding problem of criminal investigation is not the sample,per se,but what was the sample prior to the catastrophe,and this is d