DEVELOPMENTS IN APPLIED SPECTROSCOPY Volume 5 A Publication 0/ the Chicago Section 0/ the Society lor Applied Spectroscopy DEVELOPMENTS IN APPLIED SPECTROSCOPY Volume 5 edited by 1. R. Pearson E. 1. Grove Research Center Illinois Institute 0/ Technology American Can Company Research Laboratories Barrington, Illinois Chicago, Illinois Proceedings of the Sixteenth Annual Mid-America Spectroscopy Symposium Held in Chicago, Illinois June 14-17, 1965 PLENUM PRESS NEW YORK 1966 Library of Congress Catalog Card No. 61-17720 ISBN 978-1-4684-8696-4 ISBN 978-1-4684-8694-0 (eBook) DOl 10.1007/978-1-4684-8694-0 Plenum Press A Division of Plenum Publishing Corporation 227 West 17 Street, New York, N. Y.10011 © 1966 Chicago Section of the Society for Applied Spectroscopy Softcover reprint o/the hardcover 1st edition 1966 All rights reserved No part of this publication may be reproduced in any form without written permission from the publisher Preface This volume presents a collection of papers given at the 16th Mid -America Symposium on Spectroscopy held in Chicago, June 14-17, 1965. The Mid-America Symposium is sponsored annually by the Chicago Section of the Society for Applied Spectroscopy in cooperation with the St. Louis, Niagara Frontier, Cleveland, Detroit, lndianapolis, and Milwaukee Sections of the Society and the Chicago Gas Chromatography Discussion Group. Although we refer to this meeting as the Mid-America Symposium, it continues to attract attendance, interest, and inquiry from many parts of the world. Sessions on lnfrared, Raman, Ultraviolet, Visible, Emis sion, Flame, Atomic Absorption, Nuclear Particle, Gamma Ray, Nuclear Magnetic Resonance, X-Ray Spectroscopy, Spec troscopy, Spectrophosphorimetry, and Gas Chromatography provided interesting papers involving both applied and theo retical principles. This volume continues a series of the Proceedings initiated in 1961 and is composed of a collection of 37 papers presented at this meeting. It is the opinion of the Symposium Committee that although not a complete account of the proceedings, publication of this collection as a reference is warranted. As editors of this volume, we wish to express our gratitude to the authors who gave their time and effort in submitting their manuscripts so that this volume could be published. The Symposium Committee, L. S. Gray, W. Baer, Vivian Biske, W. Los eki , M. S. Wang, F. Leahy, J. L. Ogilvie, B. D. Field, T. E. Reichard, H. Szymanski, H. O'Neill, N. Armstrong, L. C. Afremow, R. L. Terry, A. M. Palmer, L. Malter, Borghild Pearson, W. Rivkin, S. P. McGlynn, are to be recommended for their untiring efforts to make this meeting a success. The efforts of our secretaries, Anne Peterson of American Can, and Catherine Mischek of lIT Research Labs must also be acknowledged. v vi PREFACE Thanks must also be given to the exhibitors for lending their support to the symposium. We are also grateful to the American Can Co. and lIT Research Labs for permission to use their time and facilities to organize this Symposium and edit these Proceedings. L. R. Pearson E. L. Grove Contents X-Ray Spectroscopy Use of X-Ray Emission Spectroscopy in the Chemical Analyses of Lake Sediments, Determining 41 Elements Ursula M. Cowgill. . . . . . . . . . . . . . . . . . . . . . 3 X-Ray Fluorescence Emission Anaylsis of Slurries C. R. Hudgens and G. Pish. . . . . . . . . . . . . . . . . 25 An X-Ray Fluorescent Method for the Determination of Copper in Silver-Copper Alloys A. Carnevale and A. J. Lincoln. . . • . . . . . . . . • . 31 X-Ray Fluorescent Determination of Major Constituents in Multi-Element Matrices by the Use of Coherent to Incoherent Scattering Ratios Charles J. Carman. . . . • . • . . . . . . . . . . . . . . . 45 An Apparatus for the Analysis of Liquid Samples by the X-Ray Fluorescence Method with a Vacuum Spectrograph Frank L. Chan. . . . . . . . . . . . . . . . . . . . . . . . . 59 Interpretation of Changes in Shape of K Emission Bands of Light Elements with Chemical Combina tion J. E. Holliday. . . . . . . . . . . . . . . . . . . . . . . . . 77 The Electron Microprobe and Light-Element Analysis A. V. Manzione and D. E. Fornwalt. . . . . . . . . .. 107 The Low-Temperature K X-Ray Absorption Spectra of Fe, FeZ03' and Fe304 C. J. Polk and W. F. Nelson. . . . . . . . . . . . . . .. 119 Infrared-Raman and Ultraviolet-Visible Spectroscopy Infrared Absorption Spectroscopy of Cellulose and Cel lulose Derivatives Robert T. O'Connor. . . . • . . . . . . . . . . . . . . .. 129 vii viii CONTENTS A Survey of Methods for Sample Preparation in Absorp tion Spectroscopy E. J. Truschke •.••.•.....•.......... '. 157 New Direct Spectrophotometric Determination of Alumi num in Steel, Spelter, and Iron Ores Uno T. Hill. • • • . • • . . . • • • . . . . . . • . . . . • .. 167 The Measurement of Infrared Emission Spectra Using Multiple -Scan Interferometry M. J. D. Low and 1. Coleman. . . . . . . • . . . . . .. 177 The Detection of Pesticides by Means of Infrared Emis- sion Spectroscopy I. ,Coleman and M. J. D. Low. . . . . . . . . . . . . .. 193 Infrared Emission Spectroscopy of Solids Using Disper- sion Instruments M. J. D. Low and H. Inoue. . . . . . . . . . . . . . . 203 Thermally Induced Aggregation of Color Centers in Sodium Fluoride Karl Konrad and Theodore J. Neubert. . . . . . . 217 Low-Frequency Motions of Water Molecules in Hydrated Salts of Transition Metals J. J. Rush, J. R. Ferraro, and A. Walker. . . . . .. 227 The Application of Spectral Data from Isotopically Subs tituted Molecules to the Determination of Anharmonic Potential Energy Constants Robert R. Hart. • . . . • . . . • . . . . . • . . . . . . .. 229 Spectrophosphorimetry Atomic Fluorescence J. W. Robinson .............. . 255 Vibrational Structuring in Optical Activity Oscar E. Weigang, Jr •.......... 259 NMR Spectroscopy Analysis of Steric Conditions by NMR. The Environment Around Phosphorus in Some of Its Esters Victor Mark. . . . . . . . . . . . . . . . . . . . . . . . .. 285 CONTENTS ix NMR Study of Polymers of Ethyl, Isopropyl Isobutyl, and t-Butyl Vinyl Ethers Kermit C. Ramey, Nathan D. Field, and Alfred E. Borchert . . . . . . . . . . . . . . . . . . . . . .. 295 Emission-Flame-Atomic Absorption Spectroscopy Spectrochemical Analysis of Abrasive Materials T. S. Long . . . • . . . . . • . • . . . . . . . . . . . . . .. 307 Developments in Flame Emission and Flame Absorption Photometry John A. Dean. . • • . • . . . • • . . . . . . • . . . • . . .. 317 The Spectrochemical Determination of Lead in Blood by the Residue AC Arc Method Jack C. Wells and Robert E. Seidner. . • • . • . . .. 333 Spectrographic Analysis of Biological Materials Isabel H. Tipton and Peggy Lou Stewart. • • . . . .. 343 Determination of Bismuth and Tellurium in Body Tissues of Animals by Atomic Absorption Spectro photometry Richard E. Kinser. . . . . . . . . . . . . . . . . . . . .. 359 Some Considerations on Burners for Flame Spectroscopy R. Mavrodineanu . . . . . . . . . . . . . . . . . . . . . .. 371 Ratio Determination of Antimony Trisulfide and Potas- sium Chlorate by Atomic Absorption Spec trophotometry D. J. Roth. . . . . . . . . . . . . . . . . . . . . . . . . . .. 403 Gas Chromatography Qualitative and Quantitative Analysis of Mixtures of Polynuclear Compounds by Gas Chroma tography Using a Fraction Collector William Lijinsky and Jean Ward. . . . . . . . . . . .. 411 The Analysis of Polymers by Oxidative Degradation R. G. Scholz, J. Bednarczyk, and T. Yamauchi. .. 423 Dual Carrier Gas Chromatography: Analysis of Samples Containing Hydrogen F. L. Boys. • • . . . . • • . . . . • . • • • . . • . . . . •• 429 x CONTENTS Nuclear Particle and Gamma Ray Spectroscopy Determination of Body Composition by Gamma Spectro metry Alexander P. Remenchik, M.D., RameshK. Hukkoo, M.S., and Charles E. Miller, Ph. D. . . . .. 437 Neutron Activation Analysis of Serum M. C. Haven and G. T. Haven. . • . • . . . • . . . . .. 459 Manganese and Copper Determinations in Body Fluids E. L. Kanabrocki, L. F. Case, T. Fields, L. Graham, Y. T. Oester, and E. Kaplan. . .. 471 Applications of Nuclear Spectrometry in Crime Detection M. A. Wahlgren. . . . . . . . . . . . . . . . . . . . . . .. 475 Activation Analysis in Process Control Applications Troy C. Martin, J. T. Prud'homme, and 1. L. Morgan. . . . . . . . . . . . . . . . . . . . . . .. 485 Current Developments in Activation Analysis Vincent P. Guinn. . . . . . . . . . . . . . . . . . . . . .. 495 X-Ray Spectroscopy