SAMPLING, STANDARDS AND HOMOGENEITY A symposium presented at the Seventy-fifth Annual Meeting AMERICAN SOCIETY FOR TESTING AND MATERIALS Los Angeles, Calif., - 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 © BY 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 presented 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 Spectroscopy 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 To Sample the Moon—A W ENGLAND A Lunar Sample Conclusion 3 15 Role of Homogeneity in Powder Sampling—c L GRANT AND P A PELTON Sampling Theory Experimental Work Results 16 18 22 25 How to Sample a Mountain—J J CONNOR AND A T MTERS A Model of Geochemical Variation The Problem of Geochemical Error A Geochemical Example Conclusion 30 31 33 34 36 Collection and Handling of Physical Evidence for a Forensic Laboratory— P C BUSCEMI AND W D WASHINGTON Protecting the Scene of a Crime Documentation of the Location Collection of the Potential Evidence Preservation of the Evidence Labeling Requirements Chain-of-Custody Considerations Letter of Transmittal Collection of Reference Materials Conclusion 37 38 39 39 41 42 42 43 43 43 How and What to Sample in the Analytical Gap—J p WALTERS AND S A GOLDSTEIN Instrumentation for Stabilization Instrumentation for Viewing the Discharge What to View Fully Resolved Spectra Practical Application Problems in Manufacture of National Bureau of Standards Cast Metal Standard Reference Materials—w R KENNEDY The Ductile Irons The Blast Furnace Irons The Cast Steels and High Temperature Alloys The Combination Chemical Spectrographic SRMs Conclusion 45 46 51 56 62 67 72 72 81 84 85 87 CONTENTS Problems in Sampling Ferroalloys with Emphasis on Ferrosilicon—j c CLINE Manufacturing Procedures for Ferroalloys Metallurgical Structures of Ferrosilicon Sampling Procedure Selection of the Sample Conclusions 88 88 89 91 92 96 Sampling and On-Stream X-Ray Control of Portland Cement Raw Mix Slurry—CLYDE W MOOEE AND C DAVID MAARS Laboratory Investigation Plant Raw Mix Control Conclusions 97 99 102 108 Sampling and Analysis for an Oxygen Steel Shop—c B JENKINS AND G C SOTH Sampling of Preliminary Steel Samples Analysis of Preliminary Steel Samples Sampling for Final Heat Analysis Discussion Alternative Sampling and Analysis Methods Slag Samples Summary 110 110 112 114 116 119 121 121 Paper Fiber Filters for Sampling Trace Metals in Airborne Particulate Matter—T Y KOMETANI, J L BOVE, AND B NATHANSON Experimental Discussion Conclusion 123 124 126 131 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 ecology—air 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 considering 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 discussed The problem of sampling large masses such as a mountain, or large areas, for mineral identification is only diminished in the real problem of that of sampling the moon to help discover how it was formed Both subjects are adequately covered The pubhcation shows that the sampling problem is dynamic and present in all analytical methods It is inherent in all good analytical methods, that they are independent of the sample and it is incumbent on the "standard method producers" to make them so Homogeneity can be good or bad, depending on ones point of view, but we must first learn to measure it I Copyright® 1973 b y AS FM International www.astm.org INTRODUCTION Finally, we cannot have good analytical methods without good standard reference materials and we must find the best ways to manufacture these in sufficient quantities W R Kennedy American Cast Iron Pipe Co., Birmingham, Ala., symposium chairman J F Woodruff Armco Steel Corp., Middletown, Ohio, symposium co-chairman FIG 1—A preliminary lunar regional geology map D WUhelms and J McCauley, U.S Geological Survey, 1966 FIG 9—A color enhanced far UV-photo of the earth Note the two, little understood, equatorial airglow belts 18 SAMPLING, STANDARDS AND HOMOGBJEITY Ui O 115 O ~ - -H 0 ( !88 :8 oooo oooooi ooooooooooo a IV HPlOOBOOOOOOgOOOOCo o o o drHodddddddd II 8S88888! COQ ddddddddddd dodo §8 I-I d Q O '-' *-< O ;8888 ;S dddd d c o Đ is sô o O T3 S E O =4 '-S HNooooooooeSooooSo d^ddddddddd dddd N » H N * H i a o O NO© ddddddddd 'odd d SS8808888 : 8o8 I O P- ^ N » « ) N H Q P O I H Q Q Q Q oj v o N U I O O O O O O O S S M O C G O S S d d d d d d d d d odd d O 02PH02t»!»olz;o>S