THE HISTORY AND PRESERVATION OF CHEMICAL INSTRUMENTATION CHEMISTS AND CHEMISTRY A seriesofbooks devoted to the examination ofthehistory and develop mentofchemistryfrom itsearly emergenceasaseparate discipline to the presentday. The series willdescribe thepersonalities, processes, theoreti caland technical advances which have shapedour current understanding ofchemicalscience. THE HISTORY AND PRESERVATION OF CHEMICAL INSTRUMENTATION Proceedings oftheACSDivision oftheHistoryofChemistry Symposium heldinChicago, Ill., September 9-10, 1985 Editedby JOHN T. STOCK Professor Emeritus, DepartmentofChemistry, UniversityofConnecticut and MARY VIRGINIA ORNA, O.S.U. ProfessorofChemistry, CollegeofNew Rochelle D. REIDEL PUBLISHING COMPANY AMEMBEROFTHEKLUWER ACADEMICPUBUSHERSGROUP DORDRECHT/BOSTON/ LANCASTER/TOKYO library of Congress Cataloging in Publication Data The history and preservation of chemical instrumentation. (Chemists and chemistry) Includes bibliographies and indexes. 1. Instrumental analysis-History-Congresses. I. Stock, John T. (John Thomas), 1911- . II. Orna, Mary Virginia. III. American Chemical Society. Division of the History of Chemistry. IV. Series. QD79.15H57 1986 543 86-10028 ISBN-13: 978-94-010-8585-4 e-ISBN-13: 978-94-009-4690-3 001: 10.1007/978-94-009-4690-3 Published by D. Reidel Publishing Company, P.O. Box 17,3300 AA Dordrecht, Holland. Sold and distributed in the U.S.A. and Canada by Kluwer Academic Publishers, 101 Philip Drive, Assinippi Park, Norwell, MA 02061, U.S.A. In aU other countries, sold and distributed by Kluwer Academic Publishers Group, P.O. Box 322, 3300 AH Dordrecht, Holland. All Rights Reserved © 1986 by D. Reidel Publishing Company, Dordrecht, Holland Reprint of the original edition 1986 No part of the material protected by this copyrigh t notice may be reproduced or utilized in any form or by any means, electronic or mechanical including photocopying, recording or by any information storage and retrieval system, without written permission from the copyright owner TABLE OF CONTENTS Introduction vii JOHN K. TAYLOR / The Impact of Instrumentation on Analytical Chemistry WILBUR KAYE / Rise and Fall of Specifications as Indicators of Instrument Performance 11 PAUL A. WILKS / The Origins of Commercial Infrared Spectrometers 27 MELVYN C. USSELMAN / The Reflective Goniometer and Its Impact on Chemical Theory 33 M. EUGENE RUDD / D.B. Brace's Measurement of Double Refraction Due to Ether Drift 41 DUANE H. JAECKS / Developments in 18th Century Optics and Early Instrumentation 51 WILLIAM J. ANGELOTTI / The History of Optical Emission Techniques for the Industrial User 67 C. EUGENE BENNETT / My Rememberance of Gas Chromatography 79 HAMISH SMALL / A Personal History of the Conception and Early Development of Ion Chromatography 97 GERALD L. HAWK / The Next Step in Laboratory Automation - Robotics 109 WILLIAM B. JENSEN / The Development of Blowpipe Analysis 123 WALTER J . BLAEDEL / The Practical Aspects of Collecting, Preserving, and Exhibiting Analytical Balances 151 WILLIAM J. READ / Renovation and Repair of Scientific Instruments 157 A. D. MORRISON-LOW / Kemp &Co., Laboratory Suppliers 163 DAVID J. BOULLIN / Mechanical Control of Gaslight: An Account of Clockwork Mechanisms Used for Operating Gaslights 187 vi TABLEOFCONTENTS WILLIAM J. READ / The Development of Scientific Instruments Relating to Negretti & Zambra, Instrument Makers, England, 1850-1985 211 JOHN BURNETT / The Use of New Materials in the Manufacture of Scientific Instruments, C.1880-C.1920 217 JOHN T. STOCK / Historic Instruments: Survival or Disappearance? 239 Name Index 249 Subject Index 255 INTRODUCTION The development of chemistry, like that of the other fields of science and technology, has depended greatly upon the availability of instruments. Accordingly, the study of the history of instrumentation is a major area in any survey of the progress in this science. Recognizing this fact, the Division of the History of Chemistry of the American Chemical Society organized and held a very successful symposium on the history of chemical instrumentation during the Washington, D.C. National Meeting in 1979. Re~arks, both formal and informal, made during this symposium stressed points that soon become obvious to anyone who looks at the ancestry of present-day instruments. In some cases, the total history is measured in years, rather than in centuries. Chemical instrumentation, by no means confined to the laboratory, is vital in industry. There is a natural tendency to discard an item of any kind when a newer version is acquired. Often, "to discard" means "to scrap". If the item scrapped is an instrument that is unique - sometimes the last of its kind - we have a permanent artefactual gap in the history of science. These points, together with the ever-growing importance and development of the tools of the chemist, led the Divisions of the History of Chemistry and of Analytical Chemistry to the joint organization of a more extensive symposium that formed part of the ACS National Meeting in Chicago in 1985. The inclusion of the words "and preservation" in the title stresses the importance of thinking and inquiring before scrapping. Only by the co-operation of all scientists and technologists can we hope to minimize or, hopefully, avoid losses like those of the past. The eighteen papers in the symposium deal with instruments ranging from the very simple to the highly complex, with histories long, medium, or short. Some of the authors have not only first-hand knowledge of the history of a particular type of instrument, but have also contributed to the making of this history. These facts, together with the many favorable comments received during and after the symposium, strengthened our resolve that the accounts presented should be placed on permanent record in a single collection. The Editors intend this book to be a tribute to instrument makers, whether vii viii INTRODUCTION of today or of times past. The progess of science has, does, and will depend upon their skill and ingenuity. John T. Stock Mary Virginia Orna, O.S.U. (Editors) John K. Taylor THE IMPACT OF INSTRUMENTATION ON ANALYTICAL CHEMISTRY 1. INTRODUCTION In 1985, it is hard for anyone to remember, and most analytical chemists have never known, an instrumentationless world. When one enters a modern analytical laboratory, one is surrounded by equipment so that the analyst may be dwarfed by the instruments at his or her command. Contrast this with the laboratory of the 1930's; the analyst was surrounded by chemical reagents and the most conspicuous installation was a fume hood. Several drawers contained the tools of the profession beakers, filters, burets and pipets. Every analyst had virtually the same kind of equipment. Such as they were, almost all needs could be provided by a laboratory supply house. Capital outlay was low and interchangeability was high. While some analysts had specialized experience in certain materials areas, the techniques employed were remarkably similar in most of the measured areas. However, to say that analysts were independent of instruments would be wrong. The balance has always been the key instrument of quantitative analysis, and was a limiting aspect in important cases. Chemical analysis, just as any kind of measurement, is a comparison process, in which unknowns are compared with knowns. Substances of interest in a matrix were separated, converted to a measurable form, purified and weighed. In fact, G. E. F. Lundell once described analytical chemistry as a manufacturing process in which chemicals are quantitatively produced in small quantities of high purity (1). The standard for comparison was one of the most fundamental measurement standards, the kilogram or its submultiple. The balances of as late as fifty years ago were ill suited for the routine measurement of small masses and were manually operated. In fact, best performance was J.T.StockandM.V.Orna(eds.},TheHistoryandPreservationof ChemicalInstrumentation,1-10. © /986 byD.ReidelPublishingCompany. 2 JOHNK.TAYLOR obtained by multiple swings, and protection from environmental fluctuations. An analyst's set of calibrated weights and a sensitive, well-functioning balance could be one of his or her most prized possessions. Volumetric titration was a well-used tool because it could speed up analysis. The buret was the instrument used, again in a manual mode of operation. Endpoint detections were largely visual, based on indicators of various kinds. An analyst's greatest asset was a detailed, comprehensive knowledge of chemistry since the chemical steps of separations, digestions, isolation and purification often limited the kinds of measurements that could be made. 2. EARLY INSTRUMENTATION Early advances in instrumentation consisted largely of adjuncts to conventional methodology. Improvements in balances, expecially the single pan balance, increased the speed of weighings while greatly facilitating gravimetry. For example, the early microbalances, essentially super-sensitive double-pan balances, were slow, temperamental and critically influenced by environmental conditions. They had to be protected from air currents, and even the presence of the operator affected their performance. Modern balances are much less sensitive to such factors and those based on electronic and load cells or piezo-electric principles are even less so. Better understanding of electrochemical principles led to new methods for endpoint detection and later to electrical sensors, anticipators, controllers, and very sensitive measurement systems. The manual buret has been largely replaced by mechanical volumetric displacement devices that can be coupled with electric sensors to provide volumetric analytical systems. Improvement of pH measurement is a good example of how instrumentation has affected an analytical measurement related to many analytical methods. The advent of the glass electrode revolutionized this measurement and the research to produce durable electrodes and circuit designs to provide digital readouts has enabled pH m~asurements to be made at least
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