1、i i .,7 A Manual for the TH OMAS R.DULS KI i/i i ll I!i i K i i !.,i?LIII i.i-,i ,i al,i 7 LIbel!i :/i.i i ,i ill i!i i i:?!ii:!i i i!L IIIG4!i!i.i.i:L._:7 r.,.,7 f A Manual for the Chemical Analysis of Metals Thomas R.Dulski ASTM Manual Series:MNL 25 ASTM Pblication Code Number(PCN)28-025096-50 100
2、 Barr Harbor Drive,West Conshohocken,PA 19428-2959 Library of Congress Cataloging-in-Publication Data Dulski,Thomas R.,1942-A manual for the chemical analysis of metals/Thomas R.Dulski.p.cm.-(ASTM manual series;MNL 25)Includes bibliographical references(p.-)and Index.ISBN 0-8031-2066-4 1.Metals-Anal
3、ysis-Handbooks,manuals,etc.I.Title.II.Series.QD132.D85 1996 669.92-dc20 96-1836 CIP Copyright 1996 AMERICAN SOCIETY FOR TESTING AND MATERIALS.All rights re-served.This material may not be reproduced or copied,in whole or in part,in any printed,mechanical,electronic,film,or other distribution and sto
4、rage media,without the written consent of the publisher.Photocopy Rights Authorization to photocopy items for internal,personal,or educational classroom use,or the internal,personal,or educational classroom use of specific clients,is granted by the American Society for Testing and Materials(ASTM)pro
5、vided that the appro-priate fee is paid to the Copyright Clearance Center,222 Rosewood Drive,Danvers,MA 01923,Tel:508-750-8400 online:http:/ manual does not purport to address(all of)the safety problems associated with its use.It is the responsibility of the user of this manual to establish appropri
6、ate safety and health practices and determine the applicability of regulatory limitations prior to use.Printed in Ann Arbor,MI March 1996 Dedication THIS BOOK IS DEDICATED to my father,Frank Dulski,who was both a gentleman and a gentle man.Acknowledgments THERE ARE three levels of indebtedness that
7、I would like to acknowledge.First,there are those individuals,living and deceased,who for over 32 years have taught me from their deep knowledge of classical and instrumental analysis:Charles J.Byrnes,Silve Kallmann,Ralph M.Raybeck,James O.Strauss,Alfons Suk,and George Vassilaros.These cherished fri
8、ends have contributed to this book in countless unrecognized ways.Next,there are those who have given their time and their effol ts in the review of the manuscript:their names and affiliations are listed below.The suggestions and correc-tions of these individuals have been an invaluable aid in the p
9、reparation of the final text.Finally,there are my friends,coworkers,and associates,including the members of ASTM Committee E-1,and my family-my wife,Grace,my daughter,Brittany,and my mother,Stephanie who have in their respective ways supported and sustained me in this work.Thank you,all.Terry F.Beck
10、with Zinc Corporation of America Monaca,PA Charles M.Beck NIST Gaithersburg,MD Charles J.Byrnes Crucible Materials Corp.-Research Center Pittsburgh,PA Robert N.Smith,retired American Cast Iron Pipe Co.Birmingham,AL D.A.Flinchbaugh Bethlehem Steel Corp.Bethlehem,PA Charles K.Deak C.K.Deak Technical S
11、ervices,Inc.Warren,MI Jeffrey C.Morrow Colonial Metals Co.-Lab Columbia,PA Foreword THIS PUBLICATION,A Manual for the Chemical Analysis of Metals,was approved by ASTM Committee E-1 on Analytical Chemistry for Metals,Ores,and Related Materials.This is Manual 25 in ASTMs manual series.Cover photo from
12、 the collection of Isabel and Alfred Bader.Disclaimer MUCH OF THE METHODOLOGY described in this book is potentially hazardous.The author,his affiliation,Carpenter Technology Corporation,and the publisher,ASTM,assume no liability whatsoever for any material,financial,or personal loss or injury incurr
13、ed from the implementation of the equipment,chemicals,or procedures described herein.Contents Introduction PART I:MATERIALS Chapter lLaboratory Design Chapter 2Equipment Chapter 3Reagents PART II:SAMPLES Chapter 4-Sampling Chapter 5Sample Preparation Chapter 6-Dissolution in Acids Chapter 7mMiscella
14、neous Dissolutions PART III:SEPARATIONS Chapter 8Separation by Precipitation Chapter 9Separation by Miscellaneous Techniques Chapter 10-The Separation of the Elements ix 3 15 29 51 61 70 82 95 110 125 PART IV:MEASUREMENT Chapter 1 l-Gravimetry Chapter 12-Titrimetry Chapter 13mAbsorption Spectrophoto
15、metry Chapter 14Emission Spectroscopy Chapter 15-Other Measurement Techniques PART V:QUALITY Chapter 16-Reference Materials,Calibration,and Validation Chapter 17mStatistics and Specifications Chapter 18-Good Laboratory Practices 141 147 158 169 177 189 196 203 ooo viii CONTENTS Chapter 19-Good Admin
16、istrative Practices Chapter 20-Personnel Afterword Glossary Bibliography Appendix I:A Brief Chronology Appendix II:The Chemical Behavior of Analytes Appendix IIA:The Alkali Metals Appendix IIB:The Rare Earths Index 213 219 223 224 226 231 234 242 243 245 Introduction WHILE THE ANCIENTS WERE intuitively aware of the particulate nature of matter and had developed a keen understanding of proportions and mathematics,it was not until the eighteenth century,when the mists of alchemy began to clear,tha