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General Analytical Chemistry of Berylliunn CHEMICAL ANALYSIS OF METALS A symposium sponsored by ASTM Committee E-3 on Chemical Analysis of Metals Philadelphia, PA, 19 June 1985 ASTM SPECIAL TECHNICAL PUBLICATION 944 Francis T. Coyle, Cabot Corporation, editor ASTM Publication Code Number (PCN) 04-944000-01 1916 Race Street, Philadelphia, PA 19103 # Copyright by ASTM Int'l (all rights reserved); Sun Dec 27 14:13:49 EST 2015 Downloaded/printed by University of Washington (University of Washington) pursuant to License Agreement. No further reproductions authorized. Libtaiy of Congress Catalo^ng-in-Publication Data Chemical analysis of metals. (ASTM special technical publication; 944) "ASTM publication code number (PCN) 04-944000-01." Includes bibliographies and index. 1. Metals—Analysis—Congresses. 2. Alloys- Analysis—Congresses. I. Coyle, Francis T. II. American Society for Testing and Materials. Committee E-3 on Chemical Analysis of Metals. III. Series. QD132.C44 1987 620.1'6 86-32130 ISBN 0-8031-0942-3 Copyright © by AMERICAN SOCIETY FOR TESTING AND MATERIALS 1987 Library of Congress Catalog Card Number: 86-32130 NOTE The Society is not responsible, as a body, for the statements and opinions advanced in this publication. Printed in Baltimore, MD Feb. 1987 Copyright by ASTM Int'l (all rights reserved); Sun Dec 27 14:13:49 EST 2015 Downloaded/printed by University of Washington (University of Washington) pursuant to License Agreement. No further reproductions authorized. Foreword The symposium, Chemical Analysis of Metals, was presented at Philadel­ phia, PA, 19 June 1985. The symposium was sponsored by ASTM Committee E-3 on Chemical Analysis of Metals. Francis T. Coyle, Cabot Corporation, served as chairman of the symposium and is editor of the resulting publica­ tion. Copyright by ASTM Int'l (all rights reserved); Sun Dec 27 14:13:49 EST 2015 Downloaded/printed by University of Washington (University of Washington) pursuant to License Agreement. No further reproductions authorized. Related ASTM Publications Impediments to Analysis, STP 708 (1980), 04-708000-24 Flameless Atomic Absorption Analysis: An Update, STP 618 (1977), 04-618000-39 Metals and Alloys in the Unified Numbering System, Fourth Edition, DS 56c (1986), 05-056003-01 Copyright by ASTM Int'l (all rights reserved); Sun Dec 27 14:13:49 EST 2015 Downloaded/printed by University of Washington (University of Washington) pursuant to License Agreement. No further reproductions authorized. A Note of Appreciation to Reviewers The quality of the papers that appear in this pubHcation reflects not only the obvious efforts of the authors but also the unheralded, though essential, work of the reviewers. On behalf of ASTM we acknowledge with appreciation their dedication to high professional standards and their sacrifice of time and effort. ASTM Committee on Publications Copyright by ASTM Int'l (all rights reserved); Sun Dec 27 14:13:49 EST 2015 Downloaded/printed by University of Washington (University of Washington) pursuant to License Agreement. No further reproductions authorized. ASTM Editorial Staff Susan L. Gebremedhin Janet R. Schroeder Kathleen A. Greene William T. Benzing Copyright by ASTM Int'l (all rights reserved); Sun Dec 27 14:13:49 EST 2015 Downloaded/printed by University of Washington (University of Washington) pursuant to License Agreement. No further reproductions authorized. Contents Overview Rapid Dissolatioii of Steel Industry Materials for Clieinical Analysis—OM p. BHARGAVA 5 The Application of Ion Exchange to the Determination of Impurities in Aluminum and Aluminom Alloys—H. TEROME SEIM 17 Applications of Automatic Titration Instruments In the Specialty Metals Industry—THOMAS R. DULSKI 31 Novel Sample Pzeparation Techniques for Chemical Analysis- Microwave and Pressure Dissolution- GERALD T. DEMENNA AND WILLIAM J. EDISON 45 The Use of Modem Atomic Spectroscopy in Industrial Analysis— ARNOLD SAVOLAINEN, HANK GRIFFIN, AND GEORGE OLEAR 60 General Analytical Chemistry of Beiyllium—RAYMOND K. HERTZ 74 Microprocessor-Based Determlnator Design and the Impact of Future Trends in the Area of Computer-Controlled Automation of Analytical Chemistry Methods—RUDOLPH B. FRICIONI 89 Analytical Laboratory Information Management System (ALIMS)— FORD A. BLAIR, JON M. ARRITT, AND LARRY J. LUNDY 97 Quality Assurance in Metals Analysis Using the Inductively Coupled Plasma—ROBERT L. WATTERS, JR. 108 Interdependence of Chemical and Instrumental Methods of Analysis—SILVE KALLMANN 128 Index 135 Copyright by ASTM Int'l (all rights reserved); Sun Dec 27 14:13:49 EST 2015 Downloaded/printed by University of Washington (University of Washington) pursuant to License Agreement. No further reproductions authorized. STP940-EB/Feb. 1987 Overview For years ASTM Committee E-3 on Chemical Analysis of Metals has held symposia relating to the analysis of metals and alloys, which produced special technical publications. Committee E-3 is concerned with the standardization of referee methods relating to chemical analysis of metals and alloys for com­ pliance with compositional specifications. The symposium "Chemical Analy­ sis of Metals" was held in concurrence with the celebration of the 50th anni­ versary of Committee E-3 and the 25th anniversary of Committee E-16 on the Sampling and Analysis of Metal-Bearing Ores and Related Materials. In con­ structing the program, suggestions were sought from knowledgeable people engaged in the use and development of standards. ASTM Committee E-3 has subcommittees, two that deal with the analysis of ferrous and nonferrous materials, thus this symposium provides informa­ tion relative to the analysis of these materials. For the last 50 years, a great deal of time and effort has been spent developing referee methods for use by producers and users of metals and alloys as well as by commercial, govern­ mental, and educational laboratories. The subject material was organized with a view to expounding upon the state of the art, development and applica­ tion to future needs. E-3 standard methods are based upon chemical dissolu­ tion of the samples followed by detection and measurement of the elements of interest. Pertinent papers on these subjects were selected and reviewed for this volume. The paper entitled "Rapid Dissolution of Steel Industry Materials for Chemical Analysis" provides information of value to chemists involved in the analysis of these materials. This covers selection of proper acids and fusion media in order that the selected method of analyses can give acceptable results. After proper dissolution, measurements can be made by atomic ab­ sorption spectroscopy, photometry, redoximetric, or complexometric titra­ tions. Examples are given which include data on accuracy and precision. "Novel Sample Preparation Techniques for Chemical Analyses—Micro­ wave and Pressure Dissolution" further addresses the importance of sample dissolution with respect to performing high volume analyses with speed, relia­ bility, and safety. Classical old techniques and new techniques are discussed, and examples achieved through their use are presented. "The Application of Ion Exchange to the Determination of Impurities in Aluminum and Aluminum Alloys" is a vivid example of work that has led to a new standard, which is incorporated in the revision of aluminum analytical Copyright by ASTM Int'l (all rights reserved); Sun Dec 27 14:13:49 EST 2015 Downloaded/printedCopyright 198 7 AS FM Internationaby l www.astm.org University of Washington (University of Washington) pursuant to License Agreement. No further reproductions authorized. CHEMICAL ANALYSIS OF METALS methods. Separation of aluminum has considerably lowered the detection limits for residual metallic impurities. Classical volumetric analysis is widely used in the laboratory. The presenta­ tion on the "Applications of Automatic Titration Instruments in the Specialty Metals Industry" offers valuable hints on how the use of automatic titrators has led to improved precision and performance. The details involving analy­ ses of specialty metals for major levels of various elements such as chromium, vanadium, boron, and cobalt are presented. The ongoing transition of elemental analyses is demonstrated by the au­ thors in their paper entitled "The Use of Modern Atomic Spectroscopy in an Industrial Laboratory." One laboratory's experience with the DC plasma Echelle Grating Spectrometer is followed through various stages of usage un­ til it is now the mainstay of their analytical methodology. An interesting excursion through the analytical chemistry of beryllium is portrayed under the title of "General Analytical Chemistry of Beryllium." The reader may follow the evolution of methods from the classical of the past to modern day instrumental techniques. Volumetric, spectrophotometric, gravimetric, and fluorometric methods have largely been replaced by atomic absorption, plasma emission methods. The chemistry of beryllium and its similarity to that of other elements is demonstrated. The evolution of analyti­ cal techniques and the descriptions of the methods are of value to all chem­ ists, since this evolution is taking place with respect to elemental analyses of all metals and alloys. The needs of modern industry have led to automation in almost every as­ pect of manufacturing. This volume addresses the utilization of laboratory automation in the paper entitled "Microprocessor-Based Determinator De­ sign and the Impact of Future Trends in the Area of Computer-Controlled Automation of Analytical Chemistry Methods." Some examples are dis­ cussed at length. Analytical
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