20th Mid-America Symposium on Spectroscopy - Analytical Chemistry

May 23, 2012 - 20th Mid-America Symposium on Spectroscopy. Anal. Chem. , 1969, 41 (4), pp 48A–65A. DOI: 10.1021/ac60273a741. Publication Date: April...
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A CORCO

FIRST

News

20th Mid-America Symposium on Spectroscopy Chicago, Ill., May 12 to 15, 1969

THE

CHICAGO SECTION in cooperation

• Easier and safer disposal of empties.

with other Mid-America Sections of the Society of Applied Spectroscopy and the Chicago Gas Chromatography Discussion Group will sponsor the 20th Mid-America Symposium on Spectroscopy. All of the program, including the exhibits, will be held in the Sheraton-Chicago Hotel in Chicago, 111., May 12 through 15, 1969. The technical program presently includes 180 papers from various fields of spectroscopy and gas chromatography. These include arc-spark-flame emission, atomic absorption, X-ray, N M R EPR, Raman, infrared absorption, and nuclear particle spectroscopy. Sessions on air-water pollution, computer, and biochemicah-toxicological applications are included. New for this year are sessions in Mossbauer and electron spectroscopy for chemical analyses. Symposia on trace element analyses, silicate analyses, and spectroscopy of materials under high pressure are included in the program. An exhibit of scientific instruments, laboratory supplies, and books is part of the program. The detailed technical program given below is a tentative program. Papers, authors, and authors' addresses are given under the general subject title and not by date of presentation. The condensed program summarizes the technical program. For further information on the meeting write to W. A. Loseke, H T Research Institute, 10 W. 35th St., Chicago, 111. 60616.

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CONDENSED PROGRAM Emission Spectroscopy Gas Chromatography-Mass Spectrometry N u c l e a r Particle Spectroscopy Mossbauer Spectroscopy of Materials at High Pressure

Tuesday, May 13, 1969 Emission Spectroscopy Trace Analysis Gas C h r o m a t o g r a p h y A i r - W a t e r Pollution Studies Mossbauer Raman Instrumentation and Techniques

Wednesday, May 1 4 , 1 9 6 9 Flame-Atomic Absorption Biochemical-Toxicological Applications Electron Spectroscopy f o r Chemical Analysis Computer Applications Study of Molecular Spectra Thursday, May 15, 1 9 6 9 X-Ray Spectroscopy B i o c h e m i c a l - T o x i c o l o g i c a l Applications S y m p o s i u m o n Silicate Analyses Computer Applications Matrix Isolation NMR-EPR

PROGRAM EMISSION SPECTROSCOPY Carbon and Graphite Spectroscopic Electrodes. J . Weinard, U n i o n Carbide Corp., Parma, Ohio Arc Stabilization with Cored Graphite Electrodes. J . W. M e l l i c h a m p , U.S. A r m y Electronics C o m m a n d , Fort M o n m o u t h , N. J . Silica in Xylene by Direct Reading Emission Spectroscopy Using a Plasma Jet. W. T. Engelskirchen, F. E. Lichte, Sinclair Research, Inc., Harvey, III. Alternate Methods for t h e Determination of Boron in Silicates. J o h n A. Schleicher, David B. Heck, Illinois State Geological Survey, U r b a n a , III. Spectroscopy Measurements on a HighPressure Uranium Arc. Richard R. Schneider, George R. S h i p m a n , Art h u r G. Randol I I , U n i v e r s i t y o f Florida, Gainesville, Fla. Time-Resolved Radial Intensity Distributions in a High Voltage Spark Discharge. R. D. Sacks, J . P. Walt e r s , University of W i s c o n s i n , Madison, Wis. The Effects of Source Parameters on Excitation in a High Voltage Spark Discharge. J . P. Walters, University of Wisconsin, M a d i s o n , Wis. Studies of Phenomena Associated with Electrode Sampling in High Voltage, Oscillating Spark Discharge. Stephen W. Brewer, Jr., J o h n P. Walters, University o f Wisconsin, M a d i s o n , Wis. An Electronically-Ignited Current Injection Spark Source. J . P. Walters, T h o m a s V. B r u h n s , University of Wisc o n s i n , M a d i s o n , Wis. A Review of Recent Achievements in Analytical Emission Spectroscopy. Anna M . Y o a k u m , Oak Ridge N a t i o n a l Laboratory, Oak Ridge, T e n n . Spectral Response for Hollow Cathode Excitation of Some Binary and Ternary Gas Mixtures. E. L. Grove, W. A. Loseke, 1 IT Research I n s t i t u t e , Chi-

News cago. III.; I. Kaleps, Wright-Patterson Air Force Base Study of the Hollow Cathode Sources for Gas Monitoring in the 25 km to 65 km Altitude Region. G. L. Johnson, J. Reich, E. L. Grove, I IT Research Institute, Chicago, III. Recent Advances in Glow-Discharge Emission for Spectrochemical Analysis. J. Loeb, Dr. H. Ritzl, RSV Spectroscopy Division of Carl Zeiss, Hechendorf, West Germany Simplified Computer Operations in Spectrochemical Analyses. Harry Dryer, Applied Research Laboratories, Detroit, Mich. Analytical Usage of the New Small Crater Laser Microprobe. Fredrick Breck, Fisher Research Laboratories, Waltham, Mass.

GAS CHROMATOGRAPHYMASS SPECTROMETRY Study of Carbohydrates by Silylation. Charles R. Sweeley, Dept. of Biochemistry, Michigan State University, Lansing, Mich. (Awards Address: Chicago Gas Chromatography Discussion Group Award for outstanding work in gas chromatography) Quantitative Aspects of the Flame Ionization Detector in Flow Programmed Gas Chromatography. Ram Levy, John Q. Walker, Clarence J. Wolf, Research Division, McDonnell Douglas Corp., St. Louis, Mo. Determination of Components in Cough Syrups. Joseph Martin, Abbott Labs, North Chicago, III. Analysis of Polymers by Gas-Liquid Chromatography. Michael Kulisz, V. Vincent Watson, Richardson Co., Melrose Park, III. The Use of Gas—Liquid Chromatography in the Printing Industry. J. B. Himes, E. S. Derzko, Richardson Co., Melrose Park, III. Isolation of Gas—Liquid Chromatographic Determination of Trace Amounts of Amines in Related Compounds. L. L. Metcalfe, Armour Industrial Chemicals, McCook, III. Capillary Gas Chromatography Analysis of Isomeric Amines in Related Compounds. D. Martin, Armour Industrial Chemicals, McCook, III. Gas Chromatography Analysis of Perfume Compounds. A. Modestas, Armour Dial, Inc. Molecular Characterization of Silicones by Gel Permeation Chromatography. Fred Larson, Bendix Corp., Kansas City, Mo. Gas Chromatographic Analysis of Vaporous Contaminants in Living Spaces. J. P. Hoeppesch, E. Lanterman, BorgWarner, Des Plaines, III. Limiting Factors Involving Analysis by Gel Permeation Chromatography. J. Armstrong, Arro Laboratories, Joliet, III. Functional Analysis by Combination Reaction Gas Chromatography-Mass Spectroscopy. F. E. Régnier, J. Huang, Purdue University, Lafayette, Ind. Gel Permeation Chromatography Calibration of Normal Paraffins by Carbon Number. R. E. Thompson, D. C. Ford, E. G. Sweeney, Sinclair Research, Harvey, III. VPC Analysis of Water in Chlorophyll. T. M. Cotton, K. Ballschmiter, J. J. ^

Circle No. 17 on Readers' Service Card

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2-69G

Circle No. 23 on Readers' Service Card

VOL. 4 1 , NO. 4, APRIL 1969

·

51 A

Determine surface area easily and economically. With t h e Perkin-Elmer-Shell Model 212D Sorptometer, it's easy and inexpensive t o determine surface areas. It's fast—several times faster than conventional surface area measurement. This latest model handles three samples simultaneously, tripling t h e speed over past models. (The 212D is a third-generation instrument, so it's thoroughly proven.) It's accurate. Even hard-to-measure samples of low surface area can be analyzed. It's sturdy. Construction is of metal with a minimum of glass, so there's no breakage problem. Sample requirements are modest. Measurements can be made with as little as 0.02 grams — certainly no more than 5 grams. Results are o b tainable over a very broad range of surface areas. A n d t h e cost is l o w — w e l l below that of conventional techniques. W e ' d like t o send you a brochure and reprints of articles w h i c h d e s c r i b e the Sorptometer and its a p p l i cations. Write t o Instrument Group, Perkin-Elmer C o r p o r a t i o n , 7 0 2 Main Avenue, Norwalk, C o n n . 06852.

PERKIN-ELMER

News Katz, Argonne National Laboratory, 1043 S. LaGrange Rd., LaGrange, III. 60525 Solubility Studies of Testosterone in Organic Solvents Using Gas-Liquid Chromatography. Maryon W. Ruchelman, Jon T. Watson, The University of Texas; M. D. Anderson, Anderson Hospital and Tumor Institute at Houston, 6723 Bertner Ave., Houston, Texas 77025 Mass Spectral Analysis of Mandelic Acid Esters. Kenneth E. Daugherty, Technical Center, American Cement Corp., 1229 Monte Vista Drive, Riverside, Calif. 92507; John I. Stevens, Walter H. Neville, Dept. of the Army, Weapons Development and Engineering Laboratories, Chemical Process Laboratory, Edgewood Arsenal, Md.

NUCLEAR PARTICLE SPECTROSCOPY Gamma Ray Spectrometer-Computer System. J. R. Vogt, Research Reactor Facility, University of Missouri, Columbia, Mo. Neutron Activation Analysis of Rare Earth Impurities in Scandium Metal. J. J. Hines, M. A. Wahlgren, Argonne National Labs, Argonne, III.; C. A. Edwards, Western College for Women, Oxford, Ohio Radiochemical Separation of Gallium by Amalgam Exchange. R. R. Ruch, Illinois State Geological Survey, 1821 Maynard Dr., Champaign, III. 61820 A Key-Lock System Based on Nuclear Radiation Spectrometry. James Wing, Argonne National Laboratory, 9700 S. Cass Ave., Argonne, III. 60439 The Effect of Channeling on the ChargeChanging Collisions of Energetic 'He* Ions Penetrating through Au(100) Monocrystals. Manfred Kaminsky, Argonne National Laboratory, 9700 S. Cass Ave., Argonne, III. 60439 General Aspects of Nuclear GammaRay Resonance (NGR). Stanley Ruby, Argonne National Laboratory, Argonne, III. Multiple Linear Regression Analysis of Scintillation Gamma-Ray Spectra: Automatic Candidate Selection. M. A. Hogan, Hogan Associates; S. Yamamoto, D. F. Covell, Naval Radiological Defense Laboratory, San Francisco, Calif. A New Combustion Method for Collecting Tritiated Water from Organic Samples for Liquid Scintillation Counting. Niilo Kaartinen, University of Turku, Finland A Commercial Version of Kaartinen Sample Preparation Apparatus. D. W. Sher, A. G. Schrodt, Packard Instrument Co., Downers Grove, III.; Niilo Kaartinen, University of Turku, Finland

MÖSSBAUER SPECTROSCOPY

Circle No. 173 on Readers' Service Card See ACS Laboratory Guide for All Products/Sales Office 52 A

·

ANALYTICAL CHEMISTRY

Application of Môssbauer Spectroscopy to Coordination and Biological Chemistry. Leopold May, The Catholic University of America, Washington, D.C. On the Distinction Between MassChange Shift and Second-Order Doppler Shift in the Môssbauer Effect. J. T. Dehn, U.S.A. Ballistic Research Laboratories, Md. The Point Charge Model for Quadrupole Splitting in 11BSn in Môssbauer Spec-

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ioaggka»*· Circle No. 48 on Readers' Service Card

News troscopy. N. W. G. Debye, J. J. Zuckerman, State University of New York, Albany, Ν. Υ. Mossbauer Spectroscopic Studies of Iron Diffusion in Rutile (TiO«). Paul P. Stampfl, John C. Travis, NASA/ Goddard Space Flight Center, Greenbelt, Md. The Use of Mossbauer Spectroscopy on the Lanthanide Elements and Their Compounds. Alan F. Clifford, Vir­ ginia Polytechnic Institute, Blacksburg, Va. Sample Preparation Methods for Over­ coming Resolution Limitations in ITFe Mossbauer Patterns Obtained on Steels. B. W. Christ, National Bureau of Standards, Washington, D.C. Mossbauer Studies of Tin Compounds with Quadrupole Splittings in Ex­ ternally Applied Magnetic Fields. Ν. Ε. Erickson, Brookhaven National Laboratory. Mossbauer Spectra of Some Tellurium Compounds. Columba Curran, Thomas G. Krivak, University of Notre Dame, Notre Dame, Ind. Magnetic Ordering in Dilute Alloys of Iron in Gold. C. E. Violett, University of California, Livermore, Calif. The Study of Retained Austenite by Means of Mossbauer Scattering Spec­ troscopy. H. K. Chow, R. L. Bogner, International Chemical and Nuclear Corp., Pittsburgh, Pa. 15236 Standard Reference Materials for Spec­ trometer Calibration and Correlation of Chemical Shifts of Iron and Tin Compounds. James R. DeVoe, J. J. Spijkerman, National Bureau of Stan­ dards, Washington, D.C. 20234

Look what $325 buys in a ljJV Full Scale DC Null Deffector/Microvoltmeter It buys you a portable

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It's

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Model 155—the lowest-priced elec­ tronic null d e t e c t o r on t h e

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a null detector, it doubles as a 1 μν to 1000 volt microvoltmeter with 19 zero center ranges. Use it for measuring thermocouple and ther­ mopile potentials, contact resis­ tance, making Hall Effect studies, or whatever. See this little giant perform. Call your Keithley Sales Engineer for your demonstration. Or contact Keithley Instruments, Inc. for com­ plete details—28775 Aurora Road, Cleveland, Ohio 44139. In Europe: 14, Ave. Villardin, 1009 Pully, Suisse. Prices slightly higher outside the U.S.A. and Canada.

circuits.

When t h e Model 155 i s n ' t w o r k i n g as

Circle No. 91 on Readers' Service Card

54 A ·

ANALYTICAL CHEMISTRY

KEITHLEY

See ACS Laboratory Guide for All Products/Sales Office

SPECTROSCOPY OF MATERIALS UNDER HIGH PRESSURE Raman Spectra of Solids Under Pres­ sure. S. S. Mitra, University of Rhode Island, Kingston, R. I. Pressure Dependencies of the Infrared Active Optical Phonons in Mixed Crystals ZnSiSei-*. J. R. Ferraro, C. Postmus, Argon ne National Lab­ oratory, Argonne, III.; S. S. Mitra, University of Rhode Island, Kingston, R. I.; C. J. Hoskins, University of Kentucky, Lexington, Ky. Pressure Dependencies of the Infrared Active Optical Phonons in Mixed Crystals KCI*Bri_*. C. Postmus, J. R. Ferraro, Argonne National Labora­ tory, Argonne, III.; S. S. Mitra, Uni­ versity of Rhode Island, Kingston, R. I.; C. J. Hoskins, University of Kentucky, Lexington, Ky. Interferometric Measurement of Ma­ terials Under High Pressure. J. Hiraishi, W. Fateley, Carnegie-Mellon University, Pittsburgh, Pa. The Effect of Pressure Upon the Opti­ cal Absorption Spectra of Silver Chloride and Silver Bromide. Richard B. Aust, Eastman Kodak Co., Roch­ ester, Ν. Υ. Putting the Squeeze on at Maryland. J. W. Brasch, A. J. Melveger, E. R. Lippincott, Center of Materials Re­ search, University of Maryland, Col­ lege Park, Md. 20742 High Pressure Studies of Hydrogen Bonding. R. Jakobsen, Y. Mikawa, Battelle Memorial Institute, Colum­ bus, Ohio Panel Discussion

BURRELL "WRIST-ACTION" LABORATORY SHAKERS

News TRACE ELEMENT SYMPOSIUM Determination of Traces of Light Ele­ ments in Inorganic and Organic Ma­ terials by X-Ray Fluorescence Spec­ troscopy. C. L. Luke, Bell Telephone Laboratories, Murray Hill, N. J . Direct Spectrographic Determination of Trace Impurities in High Purity Silver Nitrate Crystals. A. J . Kincoln, V. LeRoy, Engelhard Industries, Inc., Newark, N. J. Sampling and Preparation Errors in Trace Analyses. C. L. Grant, Uni­ versity of New Hampshire, Durham, Ν. Η. Use of Sampling Boat Techniques for Trace Analysis of Lead. D. C. Hi Idesbrand, E. E. Pickett, S. R. Koirtyohann, University of Missouri, Colum­ bia, Mo. Electrodes for Trace Impurity Analysis and Determination of Traces in Gal­ lium Metal. M. S. Wang, Monsanto Co., St. Louis, Mo. Ultratrace Quantitative Metal Analysis by Mass Spectrometry of /3-Diketonates. T. L. Isenhour, University of Washington, Seattle, Wash.; B. R. Kowalski, R. E. Sievers, Wright-Pat­ terson Air Force Base, Ohio

AIR POLLUTION STUDIES

The same complete mixing swirl you get with your own hand and wrist has been copied mechanically in Burrell shakers. Then, superior t o human wrist-action, the shaking motion operates at a constant speed— for as long as is required. You control procedures from gentle agitation t o violent swirling and repeat any operation at another time. The degree of shaking is controlled mechanically with an adjustable knob. The full torque of the constant speed motor is always applied to the oscillating mechanism. Loads need not be equalized or balanced. Shaking degrees are set, and repeated exactly at another time, to a scale graduated from 0 to 10. A built-in timer will automatically stop the shaker at any desired time up t o 5 5 minutes or may be set t o operate continuously.

B U I L D - U P

DESIGN

You Build-Up to suit your requirements. Starting with a standard shaker base unit, consisting of motor, oscillator and controls; you add a plat­ form that accommodates Separatory Funnel Clamps or 8 Erienmeyer flasks; and side-arms for 8, 12 or 16 flasks or bottles. Users may start with any Build-Up size and add or modify later, as all parts are inter­ changeable.

Burrell Shaker B U I L D - U P

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SCIENTIFIC INSTRUMENTS AND LABORATORY SUPPLIES 2 2 2 3 FIFTH AVENUE, PITTSBURGH, PA. 15219 Circle No. 102 on Readers' Service Card

56A

·

ANALYTICAL CHEMISTRY

Industrial Pollution Control Equipment. Charles Skinner, Consulting Engi­ neer, Skinner Engineering, 1301 W. 22 St., Oakbrook, III. Air Pollution and Analytical Chemist. George Morgan, Acting Director, Division of Air Quality and Emission Data, National Air Pollution Control Administration, Cincinnati, Ohio

WATER POLLUTION STUDIES Gas Chromatographic Analysis of Toxaphene in Natural Waters, Fish and Lake Sediments. Robert A. Hughes, Gilman Veith, G. Fred Lee, Water Chemistry Laboratory, University of Wisconsin, Madison, Wis. Investigation of Solid Surfaces and Optically Opaque Systems by In­ ternal Reflection Spectroscopy: Ex­ perimental Considerations. James S. Mattson, Harry B. Mark, Jr., Walter J. Weber, Jr., Water Resources Sci­ ence, University of Michigan, Ann Arbor, Mich. Status of Instrumentation in Pollution Analysis. Alfred M. Tenny, Tenco Hydro/Aerosciences Pesticide Analyses by Gas Chromatog­ raphy at Lake Michigan Basin Office. W. DeWitt Johnson, Frederic D. Fuller, LeRoy E. Scarce, U.S. Depart­ ment of the Interior, Federal Water Pollution Control Administration, Great Lakes Region, Lake Michigan Basin Office

FLAME-ATOMIC ABSORPTION SPECTROSCOPY A Silicon Specific Detector Based on Interfacing a Gas Chromatograph and a Flame Emission or an Atomic Ab­ sorption Spectrometer. J . A. Dean, Roy W. Morrow, W. D. Shultz, Uni­ versity of Tennessee, Knoxville, Tenn. An Evaluation of the Hydrogen-Argon Entrained Air Flame in Atomic Ab-

News

ALCHEMY 1969...

CORNING Labtop from Fisher transmutes old workbench surfaces into brand-new supertops. Just cement CORNING™ Labtop to any benchtop mate­ rial. At once, that worn, scarred, burned or gouged surface is covered with a Space Age glass-ceramic in handsome matte gray. Permanently. Labtop is tough as case-hardened steel (it can't dent), has a mechanical strength about 20 times greater than conventional stone tops. It's extremely resistant to acids, alkalies and solvents, abrasion, and thermal shock (it's recommended for fume hoods). High in stain resistance too, and itwipes clean for a crisp new look, year in, yearout. Corning Labtop comes in 20 stock sizes for benchtops, three additional ones for reagent shelves (special sizes on request). Bulletin? Write Fisher Scientific Company, 1003 Fisher Building, Pittsburgh, Pennsylvania 15219. Or phone your Fisher representative—he can give you the details, plus a free Labtop sample that you can put through the paces for yourself. j. 7 „

F I S H E R S C I E N T I F I C CO.

Circle No. 43 on Readers' Service Card 58A

·

ANALYTICAL CHEMISTRY

See ACS Laboratory Guide for All Products/Sales Office

sorption Spectroscopy. Keith E. B u r k e , C. H. A l b r i g h t , I n t e r n a t i o n a l Nickel Co., Inc., Suffern, Ν. Υ. Some Improved Turbulent Flames and Their Use in Atomic Fluorescence Spectroscopy. R. M. Dagnall, M. P. Bratzel, J . D. W i n e f o r d n e r , University of Florida, Gainesville, Fla. Digital Data Handling for Atomic Ab­ sorption Spectrophotometry. J . E. Schallis, H. L. K a h n , Perkin-Elmer Corp., N o r w a l k , C o n n . Measurement of the Degree of Atomization of Elements in an Air-Acetylene Flame. W. P. T o w n s e n d , P. T. Zeegers, J . D. W i n e f o r d n e r , Univer­ sity of Florida, Gainesville, Fla. Recent Developments in Flame Emis­ sion, Absorption, and Fluorescence Methods. R. N. Kniseley, Iowa State U n i v e r s i t y , A m e s , Iowa Determination of Calcium in Atmo­ spheric Particulate Samples by Atomic Absorption Spectroscopy Util­ izing an Internal Standard. Jae Y. H w a n g , Frederic F e l d m a n , I n s t r u ­ m e n t a l Laboratory, Inc., L e x i n g t o n , Mass. The Analysis of Electric Furnace Slags by Atomic Absorption Spectropho­ tometry. W. H. Scheub, C. J . S t r o m sky, T i m k e n Roller Bearing Co., Can­ t o n , Ohio Performance Features and Application of New Atomic Absorption Instrumen­ tation. N. S h i f r i n , J . R a m i r e z - M u n o z , D. Barber, B e c k m a n Instruments, Inc., F u l l e r t o n , Calif. Sprayer and Burner Units for Flame Emission and Atomic Absorption Measurements. R. Mavrodineanu, Philips Laboratories, Briarcliff M a n o r , Ν. Υ. Internal Standardization Philosophy in Flame Spectroscopy. Frederic J . F e l d m a n , Stanley B. S m i t h , Jr., In­ s t r u m e n t a t i o n Laboratory, Inc., Lex­ i n g t o n , Mass. Determination, by Atomic Absorption Spectroscopy, of Lead and Copper Contents of Particulate Samples Col­ lected from Air over Morton Grove, Illinois. C. D. B u r n h a m , C. E. M o o r e , T. Kowalski, J . K r a s n i e w s k i , Loyola University, Chicago, III.

BIOMEDICAL-TOXICOLOGICAL APPLICATIONS Optimization of a Spectrophotometer for the Measurements of Enzyme Re­ action Rates. Robert J . M a n n i n g , B e c k m a n I n s t r u m e n t s , Inc., Fullert o n , Calif. Rat Liver Subcellular Trace Metal Al­ terations Resulting from Exposure to Low Concentrations ( 5 0 ppm) of Car­ bon Monoxide. Stanely C. Mazaleski, W a s h i n g t o n University School of In­ t e r n a l Medicine, St. Louis, M o . ; Carl A. N a u , Robert C. D u n c a n , Ronald L. C o l e m a n , O k l a h o m a University School of Medicine Uses of the Laser Microprobe in Biomedicine. I. H a r d i n g - B a r l o w , NASA, Palo A l t o , Calif. New Methods for the Analysis of Hu­ man Skin and Perspiration by Infra­ red Spectroscopy. Β. Μ. A l l i s o n , Biology D e p a r t m e n t , M i c h i g a n Tech­ nological University; W. T. M. J o h n ­ s o n , R. P. Harroff, A. M. Collings, W. W. J o h n s o n , C h e m i s t r y Dept., Lincoln University, Pa.

News Determination of Metals in Biological Samples with an Induction-Coupled Radio-Frequency Plasma Torch. C. L. Grant, Donald Macnaughtan, Jr., Engineering Experiment Station, Uni­ versity of New Hampshire, Durham, Ν. Η., Merle Thorpe, Humphreys Corp., Concord, Ν. Η. Long Term Studies of Elemental Intake and Excretion of Three Adult Male Subjects. Isabel H. Tipton, University of Tennessee, Knoxville, Tenn.; Peggy L. Stewart, University of Tennessee and Stewart Laboratories, Inc. Atmospheric Monitoring for Vapors of 1, 1-Dimethylhydrazine with a Porta­ ble Automatic Colorimetric Instru­ ment. Alfred M. Grosso, Manfred J. Prager, Joseph L. Kalinsky, Naval Ap­ plied Science Laboratory, Brooklyn, Ν. Υ. ATR Infrared Spectroscopy of Biochemi­ cal Substances at Liquid-Nitrogen Temperature. Frank S. Parker, New York Medical College, New York City, Ν. Υ. Odor Threshold and Gas Chromato­ graphic Assays of Vaginal Odors dur­ ing Nitrofurazone Treatment. Louis Keith, Irving Bush, Cook County Hos­ pital, Chicago, III.; Andrew Dravnieks, B. K. Krotoszynski, NT Research In­ stitute, Chicago, III. Patterns of Urinary Copper Excretion in Patients with and without Urinary Tract Disease. Jose A. Berrios, Frances Alexander, AI Dubin, George C. Baumgartner, Irving Bush, Hektoen Institute of Medical Research of Cook County Hospital and Chicago Medical School, Chicago, III. Dietary Zinc Intake in Man. Dace Osis, Emily Wiatrowski, Joseph Samachson, Herta Spencer, Veterans Admin­ istration Hospital, Hines, III. Instrumentation in a Hospital Labora­ tory. Alvin Dubin, Hektoen Institute for Medical Research, Chicago, III. Isolation and Identification of Morphine in Biological Material by Spectrome­ try and Gas Chromatography. George Christopoulos, Cook County Coro­ ner's Laboratory, Chicago, III. Applications of Instrumentation in Clini­ cal Toxicology. Eleanor Berman, Hektoen Institute for Medical Re­ search, Chicago, ill. Fluorometric Analysis of Serum and Tis­ sue Lipids on TLC Scanner. Donald Silverman, Hektoen Institute, Chi­ cago, III. Fractional Vacuum Sublimation and Mass Spectrometry. Part I. Applica­ tion in Toxicological Studies. Paritosh K. De, Charles J. Umberger, Department of Forensic Medicine, New York University Medical Center and Department of Toxicology, Office of Chief Medical Examiner, New York Analysis of Corneal Tissue with an Elec­ tron Microprobe. Mary Jo Ingram, Department of Physiology and Bio­ physics, Donald R. Doughman, M.D., Department of Ophthalmology, Uni­ versity of Iowa, 240 Medical Labs., Iowa City, Iowa 52240 Quantification of Tricarboxylic Acid Cy­ cle and Related Acids in Human Urine by Gas-Liquid Chromatog­ raphy. Diane S. Zaura, Jack Metcoff, Michael Reese Hospital and Medical Center, 2901 S. Ellis Ave., Chicago, III. 60616 Data Acquisition and Data Processing

Separate amines easily, efficiently with

New Chromosorb* 103 Separation of nine amines in dilute aqueous solution 4-ft χ 4 - m m I.D. glass coil, 1 0 0 / 1 2 0 mesh Chromosorb 103, 35 m l / m i n , FID. Sample size: 0.1 J . Column p r o g r a m : 200-250° C, 1 5 ° / m i n . 1. Methylamine 2. Ethylamine 3. iso-propylamine 4. n-propylamine 5. sec-butylamine 6. n-butylamine 7. jsio-penty lamine 8. ji-penty lamine 9. j]-hexylamine

Chromosorb 103 is a polyaromatic porous resin de­ veloped by Johns-Manville as a solid-type support for the separation of amines and basic compounds. Until now, amine separation has been both labo­ rious and difficult. With new highly selective Chromo­ sorb 103, it's fast and easy. For more specific information, write for our bulletin FF-181. Johns-Manville, Box 290-C, Trenton, New Jersey.

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VOL. 4 1 , NO. 4, APRIL 1969

.

59 A

News in Automatic Clinical Chemistry. R. L. Faley a n d W. S l a v i n , Perkin-Elmer Corp., Norwalk, Conn. Evaluation of Succinyl Choline by Chemical and Instrumental Means. Frank Fiorese, J o h n M a c D o n a l d , B u reau of Toxicology, Illinois Departm e n t of Public H e a l t h , Chicago, III. 60612

ELECTRON SPECTROSCOPY FOR CHEMICAL ANALYSIS Introduction to ESCA. Royal A l b r i d g e , Vanderbilt University, Nashville, Tenn. Applications of ESCA. Ragnar N o r d berg, U n i v e r s i t y o f U p p s a l a , Sweden Use of Electron Spectroscopy in Determination of Electronic Structure in Molecules. T. A. C a r l s o n , O R N L , Oak Ridge, T e n n . Fundamentals of Electron Spectrometer Design. C. E. K u y a t t , N a t i o n a l B u r e a u of S t a n d a r d s , G a i t h e r s b u r g , Md. Inelastic Electronic Scattering by Molecular Gases. Edwin M. Lassettre, M e l l o n I n s t i t u t e , P i t t s b u r g h , Pa. Design and Performance of t h e NBS Electron Impact Spectrometer. J. Arol S i m p s o n , N B S , G a i t h e r s b u r g , Md. Auger Spectroscopy for Surface Chemical Analysis. R. E. Weber, U n i v e r s i t y of M i n n e s o t a , M i n n e a p o l i s , M i n n .

COMPUTER APPLICATIONS The Use of a Small Computer for OnLine Processing of Mass Spectrome-

try Data. A. L. H a r k n e s s , W. A. Svec, A r g o n n e N a t i o n a l Labs, A r g o n n e , III. Computerized Spectrometry Analysis. Chester D. Kylstra, Richard T. Schneider, Dept. of N u c l e a r Engineeri n g Sciences, U n i v e r s i t y of Florida, Gainesville, Fla. SpectroPlan—A Modular Approach to Computerized-Aided Spectroscopy Systems. Richard R a b i n , Varian Associates, San Carlos, Calif. The Impact of the Computer on Access to Chemical Information. R. E. O ' D e t t e , F. A. Tape, C h e m i c a l Abs t r a c t s Service, C o l u m b u s , Ohio A Computer Automated Diffraction Syst e m . Larry A m i o t , A r g o n n e N a t i o n a l Laboratory, A r g o n n e , III. Analytical Laboratory Instrumentation and a Shared T i m e Computer. Karl F. W e i h m a n , Elwin N. Davis, Richard Wertzler, Sinclair Oil C o r p . , Research D i v i s i o n , 3 0 8 E. 1 4 8 t h PI., Harvey, III. 6 0 4 2 6 Laboratory Data Acquisition and Computation. A b r a h a m Savitzky, PerkinElmer Corp., 1 8 8 Perry Ave., Norwalk, C o n n . 0 6 8 5 0 On-Line Computer Analysis of Gas Chromatograph Data. W. R. O l s o n , C o n t r o l Data Corp., 6 4 6 7 Lake A t h a baska, San Diego, Calif. 9 2 1 1 9 ; S. E. S u n d e r l a n d , Goodyear T i r e a n d Rubber, A k r o n , Ohio A Computer System for t h e Automation of Spectrometers. C. H. S e d e r h o l m , I B M Scientific Center, 2 6 7 0 Hanover St., Palo A l t o , Calif. 9 4 3 0 4 The Collection of Cristallographie Structural Data Using Automated Diffrac-

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MOLECULAR SPECTROSCOPY I. RAMAN SPECTROSCOPY Tensorial Properties of the Vibrational Raman Effect. J . A. K o n i n g s t e i n , C a r l e t o n University, O t t a w a , Canada Theory of Raman and Infrared Processes in Crystals: Selection Rules in Cuprite. J o s e p h S. Z i o m e k , NT Research I n s t i t u t e , Chicago, III. 6 0 6 1 6 Laser-Excited Raman Scattering in Gases. J . J . B a r r e t t , Perkin-Elmer Corp., N o r w a l k , C o n n . 0 6 8 5 2 Remote Raman Spectroscopy. T o m a s H i r s c h f e l d , Stanley M. Klainer, Block Engineering, Inc., 19 B l a c k s t o n e St., C a m b r i d g e , Mass. 0 2 1 3 9 Design Considerations for Routine Raman Spectrophotometers. Frank M. D u n n i n g t o n , Hans N e u m a n n , Spectra-Physics, Inc., 1 2 5 0 W. M i d d l e f i e l d Rd., M o u n t a i n View, Calif. 9 4 0 4 0 Raman Study of Selenium Oxychloride. J . E. Griffiths, Bell T e l e p h o n e Labs, M u r r a y Hill, N. J . 0 7 9 7 4 Raman Spectra of Organic Molecules in the Vapor Phase. Donald O. L a n d o n , J . R. A l l k i n s , Spex I n d u s t r i e s , Inc., 3 8 8 0 Park Ave., M e t u c h e n , N. J . 08840

MOLECULAR SPECTROSCOPY II. TECHNIQUES Breakthroughs in Fourier Transform Spectroscopy. P. R. Griffiths, J . O. L e p h a r d t , U n i v e r s i t y of M a r y l a n d , College Park, M d . ; S. T. D u n n , D u n n Associates, Inc., Silver S p r i n g , M d . Electrical Ratio Recording IR Spectrophotometer, 2 . 5 to 2 5 Microns with Ge:Cu Photodetector. L. W. Herscher, F. J . Karle, Dow C h e m i c a l Co., 4 0 0 1 Oak C o u r t , M i d l a n d , M i c h . 4 8 6 4 0 Environmental Particle Identification by Means of Monochromatic Radiative Scattering. Firouz S h a h r o k h i , Fred M. Shofner, U n i v e r s i t y of Tennessee Space I n s t i t u t e , T u l l a h o m a , T e n n . 37388 Degradation of Laser Optics. T e d L. Barber, U.S. A r m y W h i t e Sands Missile Range

MOLECULAR SPECTROSCOPY III. STUDY OF SPECTRA AND CHARACTERIZATION

MANOSTAT

Circle No. 119 on Readers' Service Card 60 A

tometers. J . B e n s o n , R. A. J a c o b s o n , A m e s L a b o r a t o r y , A.E.C., 1 1 0 5 Garf i e l d , A m e s , Iowa 5 0 0 1 0 On-Line Experiments in Spectroscopy. W i l l i a m D. G w i n n , U n i v e r s i t y of Calif o r n i a , Berkeley, Calif. 9 4 7 2 0 Preliminary Attempts in Computer Simulation of Chemical Reactions. Enrico C l e m e n t i , IBM Research Labs Conversational Time Sharing Computer Calculations of Purity from Differential Scan Calorimetry Data. J . G. K a r o h l , A. P. Gray, L. R. Scott, Perkin-Elmer Corp., N o r w a l k , C o n n . Computer Application t o an Automated Direct Reading Emission Spectrometer. J . J . Lowe, R. J . M a r t i n , Gulf Research a n d D e v e l o p m e n t Co., P.O. Drawer 2 0 3 8 , P i t t s b u r g h , Pa. 1 5 2 3 0

Infrared Spectra of Group VI Metal Carbonyls Containing Heterocyclic Diamines. B e n n e t t H u t c h i n s o n , Kasuo

News

Generation Gap

The Wang 700 Calculator is a whole lot smarter than its predecessors. It's the first of a new breed, a third generation programmable calculator. The difference is more revolutionary than evolutionary. It's ten times faster and more powerful than the best of the 2nd generation machines. It handles far longer programs (learns on a built-in 8192-bit core and stores permanently up to 10 blocks of 960 steps each on snap-in magnetic tape cassettes), has many more data storage registers (up to 120), and provides more hardware operations (like logs to base e and base 10, -, e x , 10 x , etc. ), than any existing calculator or so-called desk-top computer. Execution speeds for various functions range from 300 ,«sec for + and — to 250 msec for trig functions. A dual Nixie-type display produces 12. digit answers plus 2-digit (—98 to + 9 9 ) exponents each register. The Wang 700 has commands for loops, branches and subroutines, unmatched power for matrix and array operations. Exclusive integrated circuit design concentrates all these capabilities into a self-contained, convenient desk-top package. It's the logical heir to Wang leadership in high performance problem-solving.

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N a k a m o t o , Illinois I n s t i t u t e of Technology, Chicago, III. 6 0 6 1 6 Infrared and Raman Spectra of Cyclopentadienyltrichlorotitanium ( I V ) , Dicyclopentadienyldichlorotitanium(IV), and Related Compounds. Edward Maslowsky, Jr., Kazuo N a k a m o t o , Illinois I n s t i t u t e of T e c h n o l o g y , Chicago, III. 6 0 6 1 6 Raman and Infrared Spectra and Assignment of BFsNCCHa. D. F. Shriver, Basil S w a n s o n , N o r t h w e s t e r n University, 2 1 4 5 Sheridan R d . , Evanston, III. 6 0 2 0 1 Substitutional Effects on t h e IR Absorption Spectra of Apatites. R. Z. LeGeros, O. R. Trautz, J . P. LeGeros, E. Klein, A. T h e i n , New York University, 3 3 9 East 2 5 t h St., N e w York, Ν. Υ. 1 0 0 1 0 Low Frequency Vibrational Spectra of Several Potassium Para-Substituted Tetraarylborate Compounds. J o h n T. Vandeberg, Carl E. M o o r e , Frank P. Cassaretto, Loyola U n i v e r s i t y , 2 4 0 6 K e n n i c o t t Dr., A r l i n g t o n H e i g h t s , III. 60004. Characterization of Carbonate Minerals in Oil Shales and Coals by Infrared Spectroscopy. Patricia A. Estep, J o h n J . K o v a c h , A r t h u r L. Hiser, Clarence Karr, Jr., U.S. D e p a r t m e n t of t h e Interior, Bureau of M i n e s , M o r g a n t o w n Coal Research Center, M o r g a n t o w n , W. Va. 2 6 5 0 5 Material Identification by a Nondestruc­ tive Infrared Technique—External ATR. Jesse M. H o w a r d I I I , General Electric C o . , Appliance Park, Louis­ ville, Ky. 4 0 2 2 5 Spectroscopic Properties of Some Metal Complexes of Gossypol. H. N. Ramas w a m y , R. T. O'Connor, S o u t h e r n Utilization Research a n d Develop­ m e n t D i v i s i o n , A.R.S., U.S.D.A., 1 1 0 0 Robert E. Lee B o u l e v a r d , P. O. Box 1 9 6 8 7 , New Orleans, La. 7 0 1 1 9 Optically Active Crystal Vibrations of the Alkali Metal Nitrates. Rev. J . L. Walter, University of N o t r e D a m e , Notre Dame, I n d . Site Preference for Manganese in Flame-Fusion Spinel. Carl A. Pitha, J o s e p h A. A d a m s k i , Air Force C a m ­ bridge Research Laboratories, Hanscorn Field, B e d f o r d , Mass. 0 1 7 3 0 ; Charles S. N a i m a n , MITHRAS Divi­ sion of Sanders A s s o c , Inc.

X-RAY SPECTROSCOPY The Aging of Solder Standards. H. R. Post, International Business Ma­ c h i n e s , Essex J u n c t i o n , Vt. X-Ray Methods for t h e Analysis of So­ lutions. T h o m a s J . C u l l e n , Sel-Rex Corp., N u t l e y , N. J . Applications of t h e Cold Cathode Dis­ charge X-Ray Source. W i l l i a m L. Baun, Materials Physics Division (MAYA) Air Force M a t e r i a l s Labora­ tory, Wright-Patterson Air Force Base, Ohio; J a m e s S. S o l o m o n , Uni­ versity of C i n c i n n a t i , Ohio The Low Energy Absorption M a x i m u m in X-Ray K-Absorption Spectra of Transition Metal Complexes. G. L. Glen, Owens-Illinois, Inc., T o l e d o , Ohio A Study on t h e Change of Water of Crystallization by X-Ray Diffraction Data Stored in ASTM Magnetic Tape. Frank L. C h a n , Aerospace Research Laboratories, Wright-Patterson Air

News Force Base, Ohio; G. G. Johnson, Jr., Pennsylvania State University, Uni­ versity Park, Pa. Multielement Analysis With an Im­ proved X-Ray Quantometer. Fred W. Johannsen, Applied Research Labo­ ratories, Sunland, Calif. Application of a Computer Controlled Automatic X-Ray Spectrometer. John Croke, Rus Westberg, Philips Elec­ tronics, Mount Vernon, Ν. Υ. X-Ray Analysis of Stainless Steel and Low Alloy Steel. Harry Dryer, Applied Research Laboratories, Detroit, Mich. Applications of X-Ray Emission to Coat­ ings Analyses. Richard W. Scott, James D. McGinness, Sherwin-Wil­ liams Research Center, Chicago, III. A Chemical Concentration X-Ray De­ termination of Cerium in Iron and Steels. C H. Albright, Michael M. Yanak, International Nickel Co., Inc., Sterling Forest, Suffern, Ν. Υ. 10901 A Novel Technique for the Preparation of Solid Spectrographic Standards Used in the XRF Calibration for Cata­ lyst. John R. Polky, Catalyst Division, Nalco Chemical Co., Chicago, III.

SILICATE ANALYSES SYMPOSIUM Silicate Analysis—A Glance Backward and a Look Forward. Irving May, U.S.G.S., Washington, D.C. Rapid Rock Analysis Today. Leonard Shapiro, U.S.G.S., Washington, D.C. Electron Microprobe Analysis of Sili­ cates. A. A. Chodos, California In­ stitute of Technology, Pasadena, Calif. Laser Microprobe of Minerals—Aero Measurements on Micro Samples. Fred Ward, U.S.G.S., Denver, Col. Semiquant X-Ray Spectrographic Analy­ sis of Silicate Materials. Merlin Sal­ mon, Fluo-X-Spec Analytical Labora­ tory, Denver, Col. Reference Standards in the Use of Geo­ logic Materials. A. T. Myers, R. G. Havens, U.S.G.S., Denver, Col. Silicate Analysis as Viewed by the Geo­ logical Surveys. Neil Shimp, Illinois State Geological Survey, Urbana, III. An Evaluation of the Problem of Chemi­ cal Analysis of Trace Coloring Oxides in Optical Glasses. D. E. Campbell, P. B. Adams, Corning Glass Works, Corning, Ν. Υ. A Method for Analyzing Geologic Ma­ terial by a New Mobile Direct Read­ ing Spectrometer. K. J. Curry, D. J. Grimes, U.S.G.S., Denver, Col. Computer Analysis of Optical Emission Spectra. Armand W. Helz, F. G. Wal­ thall, S. Berman, U.S.G.S., Washing­ ton, D. C. Neutron Activation Analysis: The Value of the Technique to Geochemical Studies. Hugh Millard, Jr., P. J. Aruscavage, U.S.G.S., Denver, Col.

MATRIX ISOLATION The Evolution of Matrix Isolation. M. M. Rochkind, Bell Telephone Labora­ tories, Mountain Ave., Murray Hill, N. J. 07974 A Simple Radical Source for Matrix Iso­ lation Studies. Alan Snelson, I IT Re­ search Institute, 10 W. 35th St., Chi­ cago, III. 60616 64 A .

ANALYTICAL CHEMISTRY

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Same plant has to put only one layer on each of these. Ought to be pretty dependable sheet for your thin-layer chromatography.

Fluorescence and Absorption Spectra of Matrix Isolated Cobalt Dichloride Molecules. J . R. C l i f t o n , D. M. G r u e n , A r g o n n e N a t i o n a l L a b o r a t o r y , 9 7 0 0 S. Cass Ave., A r g o n n e , III. 6 0 4 3 9 Optical and EPR Spectroscopy of HighTemperature Molecules at 4 ° K . W. Weltner, Jr., U n i v e r s i t y of Florida, Gainesville, Fla. Laser Excited Fluorescence. Arnold Bass, N a t i o n a l B u r e a u of S t a n d a r d s , W a s h i n g t o n , D. C. Generation and Study of ESR of Charged Species in Matrices at 4 K. Paul Kasai, D. M c L e o d , U n i o n Car­ bide Research I n s t i t u t e , T a r r y t o w n , N.Y. Study of Copper Atoms in Rare Gas Matrices at 4 ° K . Paul Kasai, U n i o n C a r b i d e Research I n s t i t u t e , Tarryt o w n , Ν. Υ. ESR Study of Reaction Products of Dis­ charge Gases. Paul Kasai, U n i o n C a r b i d e Research I n s t i t u t e , Tarryt o w n , Ν. Υ. Environmental Effects on Intersystems Crossing in Matrix Isolated Mole­ cules. J . J . S m i t h , B. Meyer, Uni­ v e r s i t y of W a s h i n g t o n , Seattle, W a s h . Effects of Temperature on the Spectra of Matrix Isolated Molecules. J . J . Smith B. Meyer, University of W a s h i n g t o n , Seattle, W a s h .

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oping Jar, small and inexpensive, right for pre-testing and for the shorter migrations.

While thinking of TLC, send off a request for the detailed recipe book "EASTMAN TLC Visualization Reagents" to Eastman Kodak Company, Eastman Organic Chemicals, Rochester, N.Y. 14650.

Whole-Body N M R Spectrometer. Jasper A. J a c k s o n , W r i g h t H. L a n g h a m , Los A l a m o s Scientific L a b o r a t o r y , Los A l a m o s , Ν. Μ. Hydration Numbers of Strong Electro­ lytes from Temperature Dependence of Proton Shifts. E d m u n d R. Malin o w s k i , Stevens I n s t i t u t e of T e c h n o l ­ ogy, H o b o k e n , N. J . Correlations of Chemical Shifts of Sub­ stituted Norbornenes with Taft's Sigma Function. M a r t h a C. T h o r p e , W. C. C o b u r n , Jr., S o u t h e r n Research I n s t i t u t e , B i r m i n g h a m , Ala. Ν Chemical Shifts of Aqueous Alkyl A m m o n i u m Chlorides. Bruce E. W e n zel, A m e r i c a n Oil Co., W h i t i n g , I n d . , Max T. Rogers, M i c h i g a n State Uni­ versity, L a n s i n g , M i c h . Nuclear Magnetic Resonance in Crystal­ line Choline Chloride. Ralph H. H a n n o n , J o h n D. G r a h a m , N o r t h e r n Illi­ nois U n i v e r s i t y , DeKalb, III. Electron Spin Resonance Studies of the Reactions of Tris (1-Naphthyl) Phosphine and its Oxide, Sulfide and Selenide with Alkali Metals in Tetrahydrofuran and 1 , 2-Dimethoxyethane. M a h d y H. H n o o s h , A s h l a n d C h e m i ­ cal Co., H o u s t o n , Texas; Ralph A. Z i n g a r o , D e p a r t m e n t of C h e m i s t r y , Texas A and M U n i v e r s i t y , College S t a t i o n , Texas Experimental Nuclear Magnetic Multi­ ple Resonance. M. I. Levenberg, Richard S. Eagan, A b b o t t Laborato­ ries, N o r t h C h i c a g o , III. N M R and Gel Permeation Chromatogra­ phy Characterization of Etherified Melamine-Formaldehyde Resins. Dan­ iel A. Netzel, Dennis G. A n d e r s o n , DeSoto Inc., Des Plaines, III. 6 0 0 1 8 EPR in Irradiated Zinc Orthotitanate. N. A. A s h f o r d , NT Research I n s t i t u t e , C h i c a g o , III. 6 0 6 1 6

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