DEVELOPMENTS IN APPLIED SPECTROSCOPY Volume 7A DEVELOPMENTS IN APPLIED SPECTROSCOPY Selected papers from the Annual Mid-America Spectroscopy Symposia 1962: Volume 1 - Twelfth Annual Symposium, 1961 Edited by W. D. Ashby 1963: Volume 2 - Thirteenth Annual Symposium, 1962 Edited by 1. Ziomek and J. R. Ferraro 1964: Volume 3 - Fourteenth Annual Symposium, 1963 Edited by J. E. Forrette and E. Lanterman 1965: Volume 4 - Fifteenth Annual ,symposium, 1964 Edited by E. N. Davis 1966: Volume 5 - Sixteenth Annual Symposium, 1965 Edited by L. R. Pearson and E. L. Grove 1968: Volume 6 - Eighteenth Annual Symposium, 1967 Edited by W. K. Baer, A. J. Perkins, and E. L. Grove 1969: Volume 7A } Nineteenth Annual Symposium, with the Volume 7B Seventh National Meeting of the SAS, 1968 Edited by E. L. Grove and A. J. Perkins A Publication of the Chicago Section of the Society for Applied Spectroscopy DEVELOPMENTS IN APPLIED SPECTROSCOPY Volume7A edited by E. L. Grove Alfred J. Perkins Illinois Institute of Technology University of Illinois Research Laboratories College of Pharmacy Chicago, Illinois Chicago, Illinois Selected papers from the Seventh National Meeting of the Society .for Applied Spectroscopy (Nineteenth Annual Mid·America Spectroscopy Symposium) Held in Chicago, Illinois, May 13·17, 1968 g:> PLENUM PRESS· NEW YORK-LONDON· 1969 ISBN 978-1-4684-8702-2 ISBN 978-1-4684-8700-8 (eBook) DOl 10.1007/978-1-4684-8700-8 Library of Congress Catalog Card No. 61-17720 Plenum Press, New York A Division of Plenum Publishing Corporation 227 West 17 Street, New York, N. Y. 10011 United Kingdom edition published by Plenum Press, London A Division of Plenum Publishing Company, Ltd. Donington House, 30 Norfolk Street, London W.C. 2, England © 1969 Chicago Section of the Society for Applied Spectroscopy Softcover reprint oft he hardcover 1st edition 1969 A II rights reserved No part of this publication may be reproduced in any form without written permission /rom the publisher Preface Volume 7 of Developments in Applied Spectroscopy is a collection of forty-two papers selected from those that were presented at the 7th National Meeting of the Society of Applied Spectroscopy, held (in place of the 19th Mid-America Symposium on Spectroscopy) in Chicago, May 13-17, 1968. These papers, selected by the editors and reviewed by persons knowledgeable in the field, are those of the symposium type and not those pertaining to specific research topics that one would expect to be submitted to a journal. It is the opinion of the committee that this type of publication has an important place in the literature. The relatively large number of papers would result in quite a sizable volume if bound in one set of covers. For this reason, and to present the material in areas of more specific mterest, Volume 7 was divided into two parts, Part A, Physical-Inorganic, and Part B, Physical-Organic Developments. The 7th National Meeting was sponsored by the Chicago Section as host in cooperation with the St. Louis, New England, Penn York, Niagara-Frontier, Cincinnati, Ohio Valley, New York, Baltimore-Washington, North Texas, Rocky Mountain, and Southeastern Sections of the Society for Applied Spectroscopy and the Chicago Gas Chromatography Group. The editors wish to express their appreciation to the authors and to those who helped with the reviewing. The latter include Dr. Elma Lanterman, Mr. John E. Forrette, Dr. Carl Moore, Dr. B. Jaselskis, Mr. H. G. Zelinski, Mr. D. J. Rokop, Mr. N. R. Stalica, Dr. Charles Reagan, Dr. Morris A. Wahlgren, and Dr. David Edgington. Thanks should also be extended to the exhibitors for their part in the Symposium and the exhibitor seminars. E. L. Grove A. J. Perkins v Contents X-RAY SPECTROSCOPY Dispersive and Nondispersive X-Ray Fluorescence Methods for the Measurement of the Thicknesses of Films of Cadmium Sulfide and Other II - VI Compounds ........ 3 Frank L. Chan Applications of X-Ray Topography in the Characterization of Semi- conductor Surface Layers . . . . . . . .. 31 P. Wang and F. X. Pink High-Energy Electron-Diffraction and X-Ray Emission Analysis of Surfaces and Their Reaction Products 61 P. B. Sewell, D. F. Mitchell, and M. Cohen Surface Analysis with the Electron Probe 80 Gudrun A. Hutchins Experience with a Computer-Coupled X-Ray Spectrometer 97 F. Bernstein Use of Total Reflection at the Critical Angle for Dispersion of Ultrasoft X-Rays. . . . . . . . . . . . . . . . . . . . . . 108 Heribert K. Herglotz The Shift in Wavelength with Voltage of Certain X-Ray Lines 121 A. F. Burr and R. J. Liefeld EMISSION, FLAME, AND ATOMIC ABSORPTION SPECTROSCOPY Spectroscopy Study of Hot Gases 133 Firouz Shahrokhi Analysis of Plant-Ash Solutions by Spark-Emission Spectroscopy 152 J. Benton Jones, Jr., and Myron H. Warner vii viii CONTENTS Routine Industrial Analysis of Stainless Steels 161 Robert L. Chapple and Charles A. Spellman Some Difficult Working Areas in Atomic-Absorption Flame Photometry. 169 Juan Ramfrez-Mufioz A New Look at Calcium Flame Interferences . . . . . . . . . . 189 R. E. Popham and W. G. Schrenk Some Experimental Considerations in Atomic Absorption 201 F. I. Grunder and E. A. Boettner An Experimental Device for Atomic-Absorption Spectroscopy 215 J. D. Johnson, G. K. Yamasaki, and J. C. Burger Indirect Atomic-Absorption Spectrometric Methods of Analysis 222 David F. Boltz Atomic-Absorption Spectrophotometry in Mineral and Trace-Element Studies in Man ............... . 227 Dace Osis, Kathryn Royston, Joseph Samachson, and Herta Spencer MASS SPECTROMETRY Investigation of Solids by Means of an Ion-Bombardment Mass Spec- trometer . . . . . . . . . . . . . . . . . . . . . . . . . .. 239 H. W. Werner Application of Mass Spectrometry to Forensic Toxicology. I. Acidic and Neutral Drugs . . . . . . . . . . . . . . . .. 267 Paritosh K. De and Charles J. Umberger Identification and Determination of Oxidation Inhibitors in Synthetic Lube Oils by Ultraviolet and Mass Spectrometry 274 John F. Kinder and James Neel Spectroscopy in Space - An Introduction and Overview 286 R. E. Ruckman A Computer-Controlled System for Automatically Scanning and Inter- preting Photographic Spectra ........ 294 C. A. Bailey, R. D. Carver, R. A. Thomas, and R. J. Dupzyk NUCLEAR PARTICLE SPECTROSCOPY Nuclear Applications of Liquid Scintillation Systems 303 Donald L. Horrocks CONTENTS ix INSTRUMENTAL PARAMETERS A Comparison of the Function of the Slit in Light-Absorption Studies Using Tungsten and Laser Sources ...... 329 Martin J. Houle, Marvin O. Fretwell, and William J. Romig Index . . . . . . . . . . . . . . . . . . . . . 339 X-Ray Spectroscopy Dispersive and Nondispersive X-Ray Fluorescence Methods for the Measurement of the Thicknesses of Films of Cadmium Sulfide and Other II-VI Compounds Frank L. Chan Chemistry Research Laboratory Aerospace Research Laboratories Wright-Patterson Air Force Base, Ohio Cadmium sulfide and other II-VI compounds have been deposited on various substrates by the vacuum technique using a setup consisting of a mechanical pump and a diffusion pump. Attempts are being made to employ a high-speed turbo-molecular pump to produce the necessary vacuum. Such pumps have been claimed to produce higher vacuum than those of earlier types. The use of x·ray fluorescence seems to be the best method for the determination of thicknesses of films of these compounds. By using this method the determination can be carried out both rapidly and nondestructively, so that the samples can be used for further experimentation or preserved for future reference. Both the vacuum and air· path spectrometers were employed with the dispersive (conventional) x-ray fluorescence method, depending on the x·ray spectra used and the film thickness to be determined. The vacuum spectrometer described earlier has been modified to improve the intensity of the secondary x·ray. The modified setup with 10w·Z kit has been changed to accommod.ate four analyzing crystals in the vacuum chamber. The radioisotopes dysprosium-l 59, iodine-12S, and others were used with the non dispersive x-ray fluorescence method. Recent instruments based on the dispersive and non dispersive systems are described here. Some of these instruments have been used to measure the thicknesses of films of II-VI compounds. 3