Table Of ContentDEVELOPMENTS
IN
APPLIED
SPECTROSCOPY
Volume 4
A Publication of the Chicago Section of the Society for Applied Spectroscopy
DEVELOPMENTS
IN
APPLIED
SPECTROSCOPY
Volume 4
edited by
Elwin N. Davis
Sinclair Research, Inc.
Harvey, Illinois
Proceedings of the
Fifteenth Annual Mid-America Spectroscopy Symposium
Held in Chicago, Illinois
June 2-5, 1964
Distributed by
PLENUM PRESS
NEW YORK
1965
ISBN 978-1-4684-8693-3 ISBN 978-1-4684-8691-9 (eBook)
DOI 10.1007/978-1-4684-8691-9
Library of Congress Catalog Card No. 61·17720
©1965 Chicago Section of the Society for Applied Spectroscopy
Softcover reprint oft he hardcover 1st edition 1965
All rights reserved
No part of this publication may be reproduced in any
form u'ithout written permission from the publisher
PREFACE
This volume presents some of the papers from the 15th
Mid-America Symposium on Spectroscopy held in Chicago on
June 2-5, 1964. 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, Indianapolis, and Milwaukee
sections of the Society and the Chicago Gas Chromatography
Discussion Group. Although basically a regional meeting, the
Symposium continues to draw enthusiastic attendance from
coast to coast and numerous foreign countries.
The present volume contains 45 of the 110 papers presented
at the Symposium. It is with some misgiving that we offer
this volume as the proceedings of the meeting with less than
half of the total papers included. However, it is the opinion of
the Symposium Committee that publication of the excellent
material available from the Symposium provides a valuable
addition to the literature in the field of spectroscopy. Response
to previous volumes of this series seems to verify this
opinion.
As Chairman of the Symposium and Editor of this volume,
I express my sincere appreciation to the authors whose
manuscripts make up this volume. I also extend my gratitude
to the following members of the Symposium Committee whose
time and effort made the 15th Mid-America Symposium a
success. Mr. Russell J. Hansen, Exhibits; Mr. Robert L.
Smick, Publicity; Mr. E. A. Piotrowski, Dr. L. S. Gray,
Infrared; Miss Joan Westermeyer, Dr. Emmett Kaelble, X-Ray;
Dr. E. L. Grove, Miss Vivian Biske, Emission; Dr. Herman
Szymanski, Mr. Stuart Armstrong, Nuclear Magnetic Reso
nance; Mr. George Kincaid, Dr. William Baer, Ultraviolet;
and Mr. Donald Ford, Mr. Jack O'Neil, Gas Chromatography.
EL WIN N. DAVIS
CONTENTS
X-Ray Spectroscopy
Soft and Very Soft Fluorescence Analysis: Spectro
graphic and Electronic Modifications for
Optimum, Automated Results
A. K. Baird, D. B. McIntyre, and E. E. Wei day . . . . 3
The Soft X-Ray Emission Band Spectra of Metals and
Alloys
Dr. Brian j. Thompson and Paul F. Kellen ..... . 23
Demountable X-Ray Tube for Light Element Fluores
cence Analysis
j. A. Dunne and W. R. Muller .............. . 33
Relationship Between X-Ray Tube Target Materials and
X-Ray Emission Intensities
F. Bernstein ......................... . 45
Applications of Chemical Precipitation Methods for Im
proving Sensitivity in X-Ray Fluorescent
Analysis
joseph S. Rudolph, Owen H. Kriege, and Robert J.
Nadalin ....................... . 57
X-Ray Spectrochemical Determination of Niobium and
Tantalum in High-Alloy and Stainless Steel
Roger W. Taylor .............•.....•... 65
Influence of the Origin of Raw Materials on the X-Ray
Analysis of Cements
H. T. Dryer and H. Renton ................ . 83
Scanning Electron-Probe Techniques for Diverse Non
metallurgical, Industrial Applications
T. E. Reichard and W. S. Coakley ........... . 91
Approximations for the Interpretations of X-Ray K
Absorption Spectra
George R. Mitchell. .. 109
vii
viii CONTENTS
Infrared and Raman Spectroscopy
Construction and Performance of Highly-Efficient Micro
Gas Cells for the Infrared Spectra
K. E. Stine, D. E. McCarthy, and H. J. Sloane. . . .. 121
Electronic Phase Null Photometric System of the Series
2000 Infrared Spectrophotometer
Charles W. Warren and Albert W. Chapple. . . . .. 133
The Identification of Fibers and Fabrics by Internal
Reflection Spectroscopy
Paul A. Wilks, Jr., and Mayhew R. Iszard . . . . .. 141
Multicomponent Infrared Analysis by the Absorbance
Ratio Method
Arthur S. Wexler. . . . . . . . . . . . . . . . . . . . . .. 151
Sensitivity of Calculated Wave Numbers of a Normal
Coordinate Treatment to Assumed Molecu-
lar Geometry
Robert R. Hart . . . . . . . . . . . . . . . . . . . . . . .. 171
Vibrational Spectra of ClOCl12 and CtoCllOO
S. Sundaram. . . . . . . . . . • . . . . . . . . . . . . . .. 179
Spectroscopic Study of the Molecular Complex HMX:
DMF
Alex Castelli and Delbert J. Cragle. . . . . . . . . .. 187
Intramolecular NH'" Halogen Hydrogen-Bond Strengths
in Five- and Six-Membered Chelate Rings
P. J. Krueger and D. W. Smith . . . . . . . . . . . . .. 197
Ultraviolet and Visible Spectroscopy
A New Molybdenum-Blue Method for Silicon in Steel
Uno T. Hill. . . . . . . . . . . . . . . . . . . . . . . . . .. 215
Theory and Applications of Diffuse Reflectance Spec
troscopy
Audrey L. Companion. . . . . . . . . . . . . . . . . . .. 221
Adaptation of an Inexpensive Ultraviolet-Visible Spec
trophotometer for Enzyme Kinetic Work
David L. Heyse. . . . . . . . . . . . . . . . . . . . . . .. 235
CONTENTS ~
Investigation of Cathodo-Luminescence with the Petro
graphic Microscope
Paul Weiblen. . . . . . . . . . . . . . . . . . . . . . . . .. 245
Gas Chromatography
The Detection of Submicrogram Quantities of Carcino
genic Polynuclear Hydrocarbons Using
Electron Capture
William Lijinsky and Irving Domsky . . . . . . . . .. 255
Chromatographic Analysis of Evolved Contaminants
From Spacecraft Materials
Normal T. Gonnella. . . . • . . . . . . . . . . . . . . .. 265
A Novel Method for Collecting Samples for Infrared
Identification
Lillian Churchill . . . . . . . . . . . . . . . . . . . . . .. 283
Determination of Traces of Glycols by Gas Chromatog-
raphy
Abram Davis, Arthur Roaldi, and Lewis E. Tufts.. 289
Gas Chromatographic Analysis of Alpha-Hydroxy Car
boxylic Acids
Norman E. Hoffman and Peter J. Conigliaro. . . .. 299
The Direct Gas Chromatographic Determination of Low
Molecular Weight Fatty Acids in Rumen Fluid
J. B. Martin, Jr. . . . . . . . . . . . . . . . . . . . . . .. 313
Simultaneous Gas Chromatography and Radioactivity
Analysis: Instrumentation, Calibration,
and Application
D. C. Nelson, R. C. Hawes, D. Paull, and P. C.
Ressler, Jr. . . . . . . . . . . . . . . . . . . . .. 323
An Inexpensive, Dual-Detector Gas Chromatograph Suit
able for Temperature Programming
John A. Perry. . . . . . . . . . . . . . . . . . . . . . . .. 347
A New Method of Pyrolysis
Theron Johns and Robert A. Morris . . . . . . . . .. 361
Gas Chromatographic Determination of Total Oxygen in
Organic Materials
F. L. Boys and D. D. Dworak. . . . . . . . . . . . . .. 369
x CONTENTS
Gas Chromatographic Methods for the Detailed Study of
Controlled-Temperature Polymer Degra
dation
Robert T. Conley. . . . . . . . . . . . . . . . . . . . • .• 377
NMR Spectroscopy
NMR-Fun Chemistry
C. L. McGehee and C. H. Summers 405
Emission, Flame, and Atomic Absorption Spectroscopy
Extraction and Flame Spectrophotometric Determina
tion of Palladium and Rhodium
Howard C. Eshelman, John Dyer, and James
Armentor. . . . . . . . . . . . . . . . . . . . . .. 419
The Determination of Copper, Nickel, Cobalt, Manga
nese, and Magnesium in Irons and Steels
by Atomic Absorption Spectrophotometry
Sabina Sprague and Walter Slavin ........... , 433
Developments in Flame Emission and Flame Absorption
Photometry
John A. Dean. . . . . . . . . . . . . . . . . . . . . . . . .. 443
The Future of Atomic Absorption Spectroscopy
J. W. Robinson. . . . . . . . . . . . . . . . . . . . . . . .. 455
A Plasma-Arc Technique for the Spectrochemical
Determination of Titanium and Zirconium
in Molybdenum
James H. Muntz. . . . . . . . . . . . . . . . . . . . . . .. 461
The Performance of the Interrupted Discharge in Argon
H. T. Dryer and F. Borile . . . . . . . . . . . . . . . .. 469
Spark Excitation in Inert Atmospheres
Arno Arrak. . . . . . . . . . . . . . . . . . . . . . . . . .. 481
The Interferometric Control System of the Diffraction
Product's Ruling Engine
Edward Leibhardt and John DuBois. . . . . . . . . .. 495
CONTENTS xi
Transformation Functions for Photographic Response in
Spectrography
J. M. McCrea . • . . . • • • . • • • • • . • • • . • • . . .. 501
Spectrographic Determination of Rhenium in Molybdenite
with the DC Arc
W. G. Schrenk and Show-jy Ho . . . . . . . . . . . . .. 517
The Determination of Boron in Metal Particles Using
the Copper Fluoride Evaluation Technique
M. E. Waitlevertch, Jr., K. W. Guardipee, J. E.
Paterson and A. L. Wolfe . . . . . . . . . . .. 527
l
The Influence of the Thermal Conductivity of Electrodes
on the Spectrochemical AnalYSis of Small
Samples and Trace Concentrations
F. J. Haftka. . . . . . . . . . . . . . . . . . . . . . . . . .. 533
X-Ray Spectroscopy
