SPECTROSCOPIC TRICKS VOLUME 3 From: APPLIED SPECTROSCOPY Especially Reorganized and Rearranged for this Edition Volume 1: 1959-1965 Volume 2: 1966-1969 Volume 3: 1970-1973 SP ECTROSCO PIC TRICKS VOLUME 3 Edited by LEOPOLD MAY Department of Chemistry The Cmholic University of America Washington, D. C. Springer Science+Business Media, LLC Library of Congress Cataloging in Publication Data May, Leopold, comp. Spectroscopic tricks. Articles from Tricks and notes in Applied Spectroscopy selected from the periods: 1959-65, 1966-69, 1970-73, Includes bibliographical references. 1. Spectrum analysis. 1. Applied spectroscopy. II. Title. QC450.M38 53 5'.84 67-17377 The material contained in this volume originally appeared in AppJied SpectroscoP'Y from 1970 through 1973, and is reprinted here by permission of the Sodety for Applied Spectroscopy. ISBN 978-1-4684-2744-8 ISBN 978-1-4684-2742-4 (eBook) DOI 10.1007/978-1-4684-2742-4 ©1970-1973 Sodety for Applied Spectroscopy © 1974 Springer Science+Business Media New York Originally published by Plenum Press, New York in 1974 AH rights reserved No pact of this book may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying, microfilming, recording, or otherwise, without written permission from the Publisher FOREWORD This is the third volume of the collection of new devices, modifications of existing equipment, and other items of interest of this nature published in the journal Applied Spectroscopy. These tricks have proved of value since they first appeared in the journal in 1959. They give solutions to many problems of workers in the var- ious fields of spectroscopy. For the novice, the use of ali three vol- umes may provide insight into the improvements that have been made in the instruments and techniques that he is currently using. The novice may be saved the necessity of discovering some shortcut that many experienced spectroscopists are already using. The contributions in this third volume are selected from the years 1970 through 1973. The subject arrangement is the same as in Volumes 1 and 2 according to the area of spectroscopy. Those tricks concerned with the same device are placed together so that the reader can easily compare them. To maintain the advantages in- herent in a single collection of contributions, the subject index for this volume is cumulative including the tricks in the previous vol- umes. Both author and journal indices are provided for this vol- ume, the latter citing the original Applied Spectroscopy citation. The use of the contributions has been approved by the So- ciety for Applied Spectroscopy, whose cooperation in this matter is gratefully acknowledged. Leopold May v CONTENTS EMISSION ANO ATOMIC ABSORPTION SPECTROSCOPY 1.1 Rapid and Inexpensive Sampling Technique for Emission Spectroscopic Analysis of Thin Films, 1. Dieleman, A. W. Witmer, J. C. M. A. Ponsioen, and C. P. T. M. Damen ...... . 1.2 A Computer-Controlled Sampler for Atomic Flame Spec- troscopy, W. Sunderland, R. S. Hodge, W. G. Boyle, and E. Fisher . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . .. . . 5 1.3 The Preparation of Metal Ingots for Use as Chemical and Spectrographic Standards, S. L. Odess and G. S. Golden . . . . . . 9 1.4 Qualitative Analysis of Precipitates by Graphite Filter Meth- ods, M. S. Wang . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13 1.5 An Improved Spectrographic Evaporating Dish, R. E. Rainford . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 15 1.6 A Rotating-Disk Sample Holder for the Sparking of Flat- Metal-Disk Samples, P. E. Walters and T. Monaci .... . . . . 16 1.7 Vented Cupped Electrodes, L. Toft and G. A. Roworth .................................... 22 1.8 Suggestions and Comments on: "Vented Cup Electrodes." J. B. Marling . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 23 Reply to Dr. Marling, L. Toft and G. A. Roworth . . . . . . . . . .. 24 1.9 A Cylindrical Sector Driven by Either Water or Air, J. W. Mellichamp and L. L. Wilcox . . . . . . . . . . . . . . .. . . .. 25 1.10 A Symmetrical Cylindrical Rotating Step Sector, H. G. Yuster . ........... . . . . . . . . . . . ............... 28 1.11 Prevention of Laser Microprobe Staining of Analyzed Metals, H. N. Barton and J. Benallo ....... -. . . . . . . . . . . .. . . .. 35 1.12 A Simple Multiport Atomic Absorption Burner Head, M. S. Wang .... . . . . . . . . . . . . . . . . . . . . . . . . . . . ....... 37 vii viii CONTENTS 1.13 Modification of a Commercial Carbon Rod Flameless Atom- izer to Accept Graphite Tubes, R. W. Morrow and R. J. McElhaney ................................. 39 1.14 Tuning Stubs as an Aid to Coupling RF Energy to Electrode- less Discharge Lamps, W. G. Schrenk, S. E. Valente, and K. E. Smith .................................... 44 1.15 A Compact Gas Jet for Optica1 Emission Spectroscopy, K. J. Curry and E. F. Cooley. . . . . . . • . • • . . . . . . . . . . . . . .. 52 1.16 Electrode Heater, P. B. Adams, E. C. Goodrich, and J. S. Sterlace . . . . . . . . . . . . . . . . . . . . . . . . . . . . • . . . . . .. 58 1.17 A Simple Modification of a Flame Photometer for Routine Trace Potassium Analysis, W. R. Knolle ..... . . . . . . . . .. 59 1.18 Mounting for New Safety Door for Perkin-Elmer Model 303 Atomic Absroption Spectrophotometer, L. T. Sennello ..... 62 1.19 Selective Filtration in Optica1 Emission Spectroscopy, A. Szule . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. .. 65 1.20 Simple Inexpensive Method of Time Resolved Spectroscopy, R. A. Koehler and F. J. Morgan. . . . . . . . . . . . . . . . . . . . .. 69 1.21 Photoelectric Time Differentiation in Laser Microprobe Optical Emission Spectroscopy, W. J. Treyt1, J. B. Orenberg, K. W. Marich, and D. Glick . . . . . . . . . . . . . . . . . . . . . . . . 74 1.22 A Photographic Plate Processing System, T. B. Griswold, W. H. Dennen, and W. H. Blackburn. . . . . . . . . . . . . . . . .. 81 1.23 A Microphotometer Digital Readout System, R. E. Mason .................................... 86 INFRARED SPECTROSCOPY 2.1 Microsampling for Infrared and Emission Analyses, P. W. H. Schuessler ..•.••...•••....••••....... . . .. 93 2.2 Cold Pressing Solid Samples in a Wax Disk for Far Infrared Analysis, M. E. Peterkin . . . . . . . . . . . . . . . . . . . . . . . . .. 95 2.3 A Manual Rectangu1ar KBr Pellet Press, M. Van Swaay and E. M. Winkler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 97 2.4 An Improved Infrared Microcell, E. C. Sunas, J. F. Williams, C. Walker, and D. Kidd .............................. 104 2.5 Infrared Cells for Salt Solutions, W. F. Edgell ............. 108 2.6 Far Infrared Sealed Liquid Cell with Polyethylene Windows, A. T. Tsatsas and W. M. Risen, Jr. ..................... 111 2.7 An Inert Infrared Cell for Measuring Quantitative Solution Spectra of Carbonium Ions and Other Reactive Species, T. J. Broxton, J. Chippindall, L. W. Deady, and R. Topsom ......................................... 115 2.8 A Simple Evacuable, Double-Beam Infrared Hot Cell As- sembly, H. W. Wilson ............................... 118 CONTENTS ix 2.9 A Novel Infrared Gas Cell, A. B. Harvey, F. E. Saalfeld, and C. W. Sink ........................................ 124 2.10 A Diamond-Window Infrared Short Path Length Cell for Corrosive Liquids, H. H. Hyman, T. Surles, L. A. Quarterman, and A. 1. Popov ................................... 127 2.11 A New Gasketing Technique for Studies with the High-Pres- sure Diamond Anvil Cell, J. R. Ferraro and A. Quat- trochi ........................................... 130 2.12 The Application of the Quartz Crystal Microbalance for Monitoring Rates of Deposition of High Temperature Species in Matrix Isolation Infrared and Raman Spectroscopy, M. Moskovits and G. A. Ozin ........................... 133 2.13 Internal Reflectance Spectroscopy. III. Micro Sampling, A. C. Gilby, J. Cassels, and P. A. Wilks, Jr. . ............. 135 2.14 Infrared Spectra of Deuterated Solvents, N. L. McNiven and R. Court ........................................ 148 2.15 Measurement of Aqueous Solution Temperatures in Infra- red Spectroscopy, M. Cormier and J. L. Thompson ......... 159 2.16 Ultrahigh Sensitivity Detection System for Far Infrared Spectrophotometers, W. M. Poteet and R. D. Feltham . . . . . . . . . . . . . . . . . . . . . . . . . . . . • . . . . . . . . . . .. 162 2.17 Derivative Traces in Infrared Fourier Transform Spectros- copy, M. J. D. Low and H. Mark ...................... 167 2.18 On Resolution Enhancement af Line Spectra by Decan- volution, A. Goldman and P. Alon ..................... 173 2.19 Negative Skin Sensitization Text with KRS-5, R. P. Oertel and E. A. Newmann ................................ 177 MASS SPECTROSCOPY 3.1 Trapping Volatiles from GLC for Injection into a Mass Spectrometer, M. G. Moshonas and P. E. Shaw ........•.... 181 3.2 A Simple System for Transferring Air-Sensitive Compounds into Capillaries from Schlenk Tubes, W. G. Eggerman ........ 184 3.3 Construction of a Leak-Inlet System for the LKB 9000 Gas Chromatograph-Mass Spectrometer, R. E. Hawk and R. W. Jennings ......................................... 186 NUCLEAR MAGNETIC RESONANCE 4.1 A New NMR Microtechnique, L. V. Haynes and C. D. Sazavsky . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 191 4.2 A Nonbreakable Nuclear Magnetic Resonance Sample Con- tainer for Radioactive Materials, L. R. Crisler .............. 198 4.3 A Convenient Device for Removing Dissolved Oxygen from NMR Samples, N. Mandava ...................•...... 202 x CONTENTS 4.4 A Method for Capping Nuclear Magnetic Resonance Tubes, R. Foester ..•...............•..•.................. 20S 4.S Nuclear Magnetic Resonance Tube Washer, D. W. Mastbrook and E. A. Hansen .................................. 207 RAMAN SPECTROSCOPY S.l SampHng Techniques for Raman Spectroscopy of Minerals, L. E. Makovsky .................................... 211 5.2 Aluminum Metaphosphate as a Hydrofluoric Acid Resistant Raman Cell Materials, J. E. Griffiths .............•....... 21S S.3 A CeH for Resonance Rarnan Excitation with Lasers in Liq- uids, W. Kiefer and H. J. Bemstein •.................... 219 S.4 MultipleSampHng RamanCold Cell,J. B. Bates ....•....... 223 5.S A Windowless Cell for Laser-Raman Spectroscopy of Molten Fluorides, A. S. Quist ............................... 226 5.6 A Laser-Raman Cell for Pressurized Corrosive Gas and Liq- uids, J. C. Cornut and P. V. Huong ..................... 232 S.7 Thermostating Capillary Cells for a Laser-Raman Spectro- photometer, G. J. Thomas, Jr. and J. R. Barylski ...•.... 236 S.8 Low Temperature CeH for Measurement of Raman Spectra, 1. Stokr and B. Schneider ............................ 239 5.9 Variable Temperature Sample Holder for Raman Spectros- copy, F. A. MiIler and B. M. Haney ........ '" .•........ 243 5.10 A Fumace for Molten Salt Rarnan Spectroscopy to 800°C, A. S. Quist ....................................... 24S 5.11 A Simple Furnace for Obtaining High Temperature Rarnan Spectra, G. M. B~gun .............................. 252 5.12 Modification of a Commercial Argon Ion Laser for Enhance- ment of Gas Phase Raman Scattering, G. O. Neely, L. Y. Nelson, and A. B. Harvey .....•.•.•...........•...... 256 S.13 Polarized Raman Scattering from Small Singie Crystals, B. 1. Swanson •...••..•.......................•........ 262 S.14 On "Scrambler Plates" Used to Depolarize Visible Radiation, L. A. Rabn, P. A. Temple, and C. E. Hathaway ............. 269 5.1S On "Scrambler Plates" Used to Depolarize Visible Radiation P. R. Reed and D. O. Landon . . . . . . • • . . . . . . . . . • . . . . . .. 276 S.16 AConstantSpectraiSHtWidthServo,C.D.Allemand ....... 278 5.17 A Method for EHminating Resonance Fluorescence Ef- fects in Raman Studies of Some High Temperature Vapors: Raman Spectra of BiG3 from 450 to 800°C, P. T. Cun- ningham and V. A. Maroni .....................•..... 283 5.18 Computer Time Averaging of Laser Raman Spectra for Matrix-Isolated Species, D. A. Hatzenbuhler, R. R. Smard- zewski, and L. Andrews . . . . . • . . . . . . . . . . . . . . . . . . . . . .. 287