Developments in Applied Spectroscopy: 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

339 Pages·1969·9.28 MB·English

by  Frank L. Chan (auth.)

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