bluuebunny/crossref_metadata_2025 huggingface dataset:
Low-Frequency Vibrations of Some Organotrichlorosilanes
Authors: Durig J. R. , Hellams K. L.
Published: November 2005

The far infrared (33–500 cm−1) spectra of a series of organotrichlorosilanes have been recorded. The Raman spectra (0–600 cm−1) have also been measured and the relative intensity and depolarization values of lines are tabulated. The spectra have been interpreted in detail and some low-frequency “group frequencies” are proposed for the SiCl3 moiety. The infrared (3200–33 cm−1) and Raman (0–3200 cm−1) spectra of α-chlorovinyltrichlorosilane have been recorded and a complete vibrational assignment is presented. Torsional oscillations of the SiCl3 group were observed for two of the molecules; barriers of 1.7 kcal/mole and 2.7 kcal/mole were calculated for the motion around the C—Si bonds of the vinyltrichlorosilane and the ethyltrichlorosilane molecules, respectively. The results are briefly discussed. Thermodynamic properties have been calculated for the latter two molecules.
Infrared Absorption of the Carbonyl Group of Semicarbazides, Semicarbazones, and Pyrazolecarboxamides
Authors: Wang Tze Seng
Published: November 2005

The carbonyl frequency in semicarbazides, semicarbazones, and pyrazolecarboxamides is higher than that in ureas. A phenyl group attached to the third nitrogen atom of semicarbazides lowers the carbonyl frequency. A phenyl group substituted on the first nitrogen atom shifts the carbonyl absorption in semicarbazides to a higher frequency region than do alkyl groups.
Flame Photometer Specialized for Cesium
Authors: Folsom T. R. , Sreekumaran C. , Weitz W. E. , Tennant D. A.
Published: November 2005

A new photometer system is described that allows very small traces of an element, such as cesium, to be determined quantitatively with greater precision than previously possible with flame-emission spectra. For example, with the new system it is possible to replicate measurements of the cesium in quantities that are normally present in one liter of sea water (about 0.3 μg) with standard error less than two percent. Dilute cesium standard solutions can be compared significantly within a few parts per billion. This, apparently, has not been reported for any previous flame photometer. The system consists of two photomultiplier tubes observing a flame simultaneously, from the same aspect, but each having a different optical filter interposed. Use is made of a beam splitter and two interference filters, one filter passing only a narrow band centered at the 8521.1-Å line of cesium, the other filter passing a nearby band not containing much of this emission but rather passing a sample of the background of the flame that contributes much of the total statistical fluctuation. Signals from these two phototubes are compared by suitable differential circuits, and are continuously recorded. A specialized automatic sample-changing system was developed to provide for precise timing of the burning of the sample and the standard solutions and to carry out aspirator washings immediately following the burning of each sample. Finally, means are provided for continuously monitoring the aspiration rate by recording the brightness of the background (off-peak) signal independently.
Nuclear Magnetic Resonance Study of the Hydrolysis of Diethyl Methylphosphonite
Authors: Daugherty Kenneth E. , Eychaner William A. , Stevens John I.
Published: November 2005

The products of the hydrolysis reactions of diethyl methylphosphonite at room temperature have been elucidated by means of proton nuclear magnetic resonance. The reaction was followed by observing the methyl-hydrogen resonance, phosphorus-hydrogen resonance, methylenehydrogen resonance, and hydroxyl-hydrogen resonance. Upon addition of up to one mole of water per mole of diethyl methylphosphonite, ethyl hydrogen methylphosphinate was produced in a very rapid and complete reaction. Upon addition of greater than one mole of water—up to two moles of water per mole of diethyl methylphosphonite—the ethyl hydrogen methylphosphinate that was produced was further hydrolyzed to dihydrogen methylphosphinate in a very slow reaction. At ratios of two or more moles of water per mole of diethyl methylphosphonite, only dihydrogen methylphosphinate and ethanol were observed in solution after the reactions had come to completion. Trivalent phosphorus hydrolysis products were not observed in this reaction sequence. The chemical shifts, spin—spin coupling constants, and analytical data are described.
Determination of Total Bromine in Brines by X-Ray Fluorescence
Authors: Dunton Polly J.
Published: November 2005

Total bromine in brines may be determined directly by x-ray fluorescence by measuring the peak-to-background intensity ratio of the bromine K-alpha radiation. The accuracy of the determination is unaffected by wide differences in the specific gravity of the brines. Bromine concentrations of 1 to 1000 ppm may be determined in about one minute with an accuracy comparable to that of usual chemical methods.
Transmission and Attenuated Total Reflection (ATR) Infrared Spectra of Bone and Collagen
Authors: Furedi H. , Walton A. G.
Published: November 2005

Transmission and attenuated total reflection (ATR) spectra of collagen and normal, adult human bone have been compared with literature data and band assignments for bone spectra are given. Except for slight shifts in some absorption bands (the amide I band at 1650 cm−1 and some of the phosphate absorption bands), most frequencies of both spectra are in fair agreement with previously reported values for the individual components. An improvement in resolution of some protein bands was achieved with the ATR technique.
Characteristic Infrared Absorption Bands for Diels—Alder Quinone Adducts and Derivatives
Authors: Pollard G. E.
Published: November 2005

Extension of established correlations for carbonyl and carbon—carbon double bonds have been evolved for some Diels—Alder quinone adducts and derivatives. Some empirical correlations for novel nortricyclenic derivatives are discussed. These compounds have four possible stereoisomers and their infrared spectra provide a ready method of differentiation.
Spectroscopic Review of the Normal Vibrations of Metal Complexes with Nitrogen-Containing Ligands
Authors: Durig J. R. , Wertz D. W.
Published: November 2005

The ir and Raman spectroscopic studies of metal complexes with nitrogen-containing ligands have been reviewed. A special emphasis has been placed on the stretching and bending fundamentals of the metal—ligand bond. The following ligands are included in the discussion: nitrosyl, nitro, nitrite, nitride, azido, molecular nitrogen, hydrazine, isocyanate, isothiocyanate, isoselenocyanate, pyridine, and ethylenediamine.
Absolute Disintegration Rate of Finite Gold Sample: Determination by Coincidence Techniques
Authors: Dooley John A.
Published: November 2005

A method has been developed for absolute disintegration rate determination of finite-sized, radioactive samples. Measurements were made on a 15-mg gold foil. The average disintegration rate was 2.163X105 for 24 determinations with a precision of 2.3%. Subsequent measurements yielded precisions as low as 0.5%. Conditions of bias settings, decay corrections, and coincidence resolving times were widely varied. The scintillation, coincidence equipment, including novel pulse timing, are mentioned. Data corrections, including accidentals and particle A in detector B are discussed. It is shown that the corrections are empirical and do not limit the absolute nature of the measurements. Some of the nuclear parameter requirements and spectroscopic implications are indicated.
Past Results and Future Prospects of the Far-Infrared Studies of Hydrogen Bonding
Authors: Jakobsen R. J. , Brasch J. W. , Mikawa Y.
Published: November 2005

In the past five years the number of papers concerned with far-ir studies of hydrogen bonding has increased by an order of magnitude. The results of some of these papers are presented in this review. Most of this work is concerned with the assignment of low frequency hydrogen bond vibrations. Since the major problem is reliable assignments, we discuss techniques used in making the assignments and emphasize the past work in which attempts have been made to substantiate those assignments. These assignments are discussed in terms of the different hydrogen bond vibrations associated with various types of hydrogen bonds. The main needs for future far ir hydrogen bond studies are listed.
Infrared Spectroscopy at Low Temperature for the Improved Resolution of Spectra
Authors: Caspary R.
Published: November 2005

The low-temperature technique in the normal ir region has proven to be a useful method for analytical purposes in distinguishing substances having similar spectra at room temperature.
Determination of 240Pu in Plutonium by Optical Emission Spectroscopy
Authors: Limpert John C.
Published: November 2005

The isotopic analysis for plutonium-240 in plutonium by optical emission spectroscopy has been studied. The choice of analytical and internal standard lines, wavelength measurement, the conditions for sample preparation, and excitation in a sustained ac arc is discussed. Data is presented concerning the determination of plutonium-240 over a range of 3%–17% with a relative precision of the order of ±1% at the 95% confidence level, in addition to optical emission vs mass spectrographic data.
Introduction to Fourier Transform Spectroscopy
Authors: Horlick Gary
Published: November 2005

This paper provides an introduction to Fourier transform spectroscopy. The basic concepts of the Fourier transform technique are reviewed. These include the characteristics and generation of interferograms and the generation of spectra by the Fourier transformation of interferograms. The multiplex and throughput advantages and the data handling disadvantages are also discussed. The optical, electronic, and data-handling instrumentation and techniques necessary for a Fourier transform spectrometer system are, in general, quite different from those of a conventional prism or grating spectrometer. The requirements of these areas are outlined and recent developments are reviewed. The Fourier transform technique has been successfully applied to a number of spectral measurements from the visible through to the far infrared. Some of the more recent applications are discussed.
Variable Temperature Raman Cell
Authors: Antion D. J. , Durig J. R.
Published: November 2005

A variable temperature cell for investigating the Raman spectra of solids, liquids, and condensed vapors is described. A special cradle for the cell is also described and spectra of various compounds recorded with the cell are presented. The variable temperature cell is designed for use with the Cary 81 Raman spectrophotometer equipped with the Spectra Physics helium—neon laser accessory.
Computerized Trace Impurity Measurement in Spark-Source Mass Spectrometry
Authors: Desjardins Michel , Moore John A.
Published: November 2005

An original computer program is applied to handle spark-source mass-spectrometry data. Computerized “Celidometry” (trace impurity measurement) increases the speed of data handling and also leaves complete freedom in interpretation of results. This article briefly describes the method utilized to obtain trace impurity concentrations by spark-source mass spectrometry and discusses in detail the computer program used to perform some of the operations. The computer program is written in DOS FORTRAN IV (E LEVEL SUBSET) supplied by IBM for System 360. The main program requires a card reader, a printer, and a 65K byte central processor. In addition, two magnetic tape drivers are used to provide off-line plotting of the calibration curve.
Simultaneous Determination of Several Elements by Spectrochemical Addition Method … (II) (Tabulation of Analytical Value)
Authors: Masuda Isoo , Inouye Tamon
Published: November 2005

An improved method for the tabulation of analytical data, obtained by addition and successive dilution procedures for spectrochemical analysis, is presented. The author's previous work shows that the solution of the first approximation diverges at some dilution factor smaller than unity when the slope of the working curve of added series is greater than that of unadded series. By obtaining the distance between this position and the origin, and taking it as a correction factor for zero-order approximation, tabulation of the analytical value, in the case of β>α, is carried out. One parameter of the calculation is deleted by normalizing the spectral intensity; therefore, the tabulation can be simplified.
Infrared-Pyrolysis Studies of Synthetic Fibers
Authors: Cassels John W.
Published: November 2005

Infrared spectra of the pyrolysis products of fifteen different synthetic fibers were examined and compared to the internal reflection spectra of the fibers. Valuable information was obtained, from both the vapor and condensed phases of the pyrolysis products, to qualitatively classify or identify the fibers. The spectra obtained also yielded information as to the characteristics of the thermal degradation of these polymers.
Micro X-Ray Fluorescence Spectroscopy: Selected Geochemical Applications
Authors: Cuttitta Frank , Rose Harry J.
Published: November 2005

Comprehensive and accurate data on the relative and absolute abundances of the elements are critical to a better understanding of the principles governing their crustal distribution and migration processes. Many geochemically coherent pairs or groups of elements (e.g., the halogens and the rare earths) are difficult to determine chemically. Microanalytical methods combining chemical and x-ray fluorescence techniques have been developed not only to determine these elements rapidly and accurately, but also to provide total analyses of milligram quantities of rare geologic specimens. One of these methods (solution—dilution) is virtually free of matrix effects and is adaptable to the analysis of trace or major constituents. These methods have proven invaluable in the microdetermination of Sc, Y, and the individual rare-earth elements in minerals or rare-earth separates on as little as 1 mg of total sample. Other applications have been the determination of iron in silicates, bromine and iodine in well waters, and the total analysis of small amounts of chromium, sulfide, and carbonate minerals.
Method to Determine all Detectable Exchangeable Cations Using X-Ray Emission and Optical Emission Spectroscopy
Authors: Cowgill Ursula M.
Published: November 2005

A method is described, employing as the sample bottom mud from Linsley Pond, North Branford, Connecticut, for the determination of all detectable exchangeable cations lying between lithium and uranium on the periodic table. Dried (48 h 110°C) and ground (200 mesh) lake mud samples are leached successively with IN, pH 6.9 ammonium acetate. Another set of similarly prepared samples are leached with doubly distilled deionized water. The leachate is made up to 100 ml. This volume is then added to a beaker containing two grams of terephthalic acid. The liquid is evaporated on to the water-insoluble terephthalic acid. The dried material is ground and pressed into a pellet. Another set of samples is treated in a similar fashion except that methyl cellulose is used as a substrate. The advantages and disadvantages of the two substrates are discussed. The pressed pellets containing the absorbed detectable exchangeable cations are examined with a G. E. x-ray emission spectroscope for those elements present between fluorine and uranium, and the lighter elements are examined by use of optical emission. The method in both cases is described.
Rare-Earth Analysis by a Rotating Platform, Silver-Spark Technique
Authors: Lyon Theodore R.
Published: November 2005

A rotating platform, silver-spark technique has been adapted for analysis of rare-earth elements directly, either as solutions or after coprecipitation with a carrier. The platform sample electrode is compared with the rod sample electrode conventionally used, and silver is shown to provide some advantages over copper as an electrode material. Observations are reported on conditions pertaining to the preparation and excitation of samples. Three varied applications of the method are briefly described, and matrix effects are discussed. Platform electrodes are found to be more convenient and adaptable than conventional rods, and the sensitivity of the method is comparable to the copper-spark method for small samples. When larger samples are used, the sensitivity decreases; however, good sensitivity can be obtained by properly selecting conditions or equipment.
Simple Photoelectric Laser Raman Spectrophotometer
Authors: Griffiths James E.
Published: November 2005

A Raman spectrophotometer employing He—Ne and argon ion laser light sources has been constructed. A three-tier platform configuration is used with the upper level supporting the source units, most of the optical components, the vacuum manifold, and the argon reservoir. A Czerny—Turner monochromator, the photoelectric detector, and the sample area are enclosed in the second level and the electronic components and pumping system are confined to the third level. Pertinent details of the instrument including optical, mechanical, and electronic components are described and discussed. Important features of the ac detection system are also given in some detail.
Analysis of Small Samples of Mixed Alkaline Earth Carbonates
Authors: Weberling R. P. , Cosgrove J. F. , Bracco D. J.
Published: November 2005

The application of instrumental techniques to the analysis of barium, calcium, and strontium in milligram-size samples of mixed alkaline earth carbonates was examined. The techniques investigated were atomic absorption spectroscopy, flame photometry, and x-ray fluorescence spectroscopy. The instrumental methods were evaluated on the basis of ease of manipulation, accuracy, and precision. Of the three methods, only atomic absorption spectroscopy fulfilled all the requirements. of precision and simplicity. It is a rapid analytical method which does not require chemical separations. Precision of 1% to 2% for each of the elements is obtainable with milligram-size samples.
Low-Temperature Grinding Technique for Infrared Analysis of Propellants and Binders in Potassium Bromide Disks
Authors: Tompa A. S.
Published: November 2005

A low-temperature grinding technique for the potassium bromide pressed-disk method was developed to obtain quantitative infrared spectra of propellants and propellant binders. The effects of grinding time and temperature on the intensities of infrared absorption bands were determined. The technique was applied to the study of the thermal degradation of a polyurethane propellant.
Infrared Spectra of the Nitration Products of Diphenylamine
Authors: Levitsky Harry , Norwitz George , Chasan David E.
Published: November 2005

The infrared spectra of the 19 nitration products of diphenylamine were established. A comparison was made of the spectra obtained and assignments were made to the principle bands. The compounds considered were diphenylamine, N-nitrosodiphenylamine, 4-nitrosodiphenylamine, 2-nitrodiphenylamine, 4-nitrodiphenylamine, N-nitroso-2-nitrodiphenylamine, N-nitroso-4-nitrodiphenylamine, 2,2′-dinitrodiphenylamine, 2,4-dinitrodiphenylamine, 2,4′-dinitrodiphenylamine, 4,4′-dinitrodiphenylamine, N-nitroso-2,4′-dinitrodiphenylamine, N-nitroso-4,4′-dinitrodiphenylamine, 2,2′,4-trinitrodiphenylamine, 2,4,4′-trinitrodiphenylamine, 2,4,6-trinitrodiphenylamine, 2,2′,4,4′-tetranitrodiphenylamine, 2,2′,4,4′,6-pentanitrodiphenylamine, 2,2′,4,4′,6,6′-hexanitrodiphenylamine, and picric acid (2,4,6-trinitrophenol).
Use of Multiple Internal Reflection Spectroscopy in the Study and Identification of Steroids
Authors: Saier Eleanor L.
Published: November 2005

Multiple internal reflection spectroscopy has been applied to the study and identification of microgram quantities of pure steroids. The methodology described is simple and requires a minimum of sample preparation. The steroid spectra which have been obtained on 20 to 100 μ g of sample are comparable to those obtained with KBr pellets. The steroids chosen to illustrate the method are of particular interest in assisting with the identification of the products of intermediary metabolism as it pertains to steroid hormones. The anomalous behavior of one of these steroids is discussed.
X-Ray Fluorescence of Rock Samples as Applied to Geological Problems
Authors: Laidley Richard A.
Published: November 2005

Three methods of sample preparation of rock specimens have been evaluated for precision and accuracy. A fusion technique was found to give the best precision. Standard deviations (1 σ) using this method and expressed as percent of the amount present for several elements are: Al 0.83, Si 0.64, K 0.43, Ca 0.43, Mn 0.48, Fe 0.24. Three recent studies of compositional variation were performed on volcanic rocks. Analyses of samples from the Hopi Buttes, Arizona, on obsidian flows from Newberry Caldera, Oregon, and on igneous rocks collected from grids or linear traverses give data which, in each case, are useful in making significant interpretations about the geologic history of the rocks concerned. These examples illustrate the rapidity and high quality of quantitative chemical analyses which can be obtained by application of x-ray fluorescence analytical techniques.
X-Ray Fluorescence Spectrometric Determination of Rare Earths in Plutonium
Authors: Hakkila E. A. , Hurley R. G. , Waterbury G. R.
Published: November 2005

Two methods were evaluated for determining rare earths in plutonium: (1) For the lighter rare earths ( Z≦66), or low concentrations of the heavier rare earths, an adjacent rare earth was added as a carrier and also as an internal standard, the rare earths were separated from plutonium by fluoride precipitation, and the measured intensity ratios for the sample and for solutions having known concentrations were compared. The Lβ1 x-rays were measured for the lighter rare earths and the Lα1 x rays for the remaining lanthanides. (2) For the heavier rare earths ( Z>66), the Lα1 x-ray intensities were measured from a nitric acid solution of the sample and compared to intensities obtained for solutions having known concentrations. The minimum concentrations that could be measured with a relative standard deviation no greater than 4% by the separation internal standard method varied from approximately 0.5% for lanthanum to 0.01% for lutetium. The direct measurement of x-ray intensity was much less sensitive. Applicability of the methods was shown by successful analyses of plutonium alloys containing dysprosium, thulium, or lutetium.
Absorption Spectroscopy of Fe(I) in Low-Pressure Oxyacetylene Flames
Authors: Bleekrode R.
Published: November 2005

The Fe atomic absorption spectrum of low-pressure oxyacetylene flames seeded with iron pentacarbonyl solutions in benzene is studied. In order to arrive at quantitative results a continuum source is used and the “total absorption” data are analyzed with the curve of growth for a single spectral line. Absorption is measured from four low-lying a5 D levels including the a5 D4 ground state and two a5 F levels, the latter lying almost 1 eV above the ground state.
Time-Programmed Mass Spectrometry
Authors: Brandt W. W. , Dovala D. L.
Published: November 2005

A 90°-sector mass spectrometer (Hitachi Perkin—Elmer Model RMU-6E) has been modified for continuous repeated scanning of the mass spectrum in up to seven separate steps of different duration. The detector sensitivity settings and scanning rates can be selected individually for each step so that precise scans of mass peaks in different parts of the spectrum can be obtained repetitively and with minimum supervision. The peak heights can be conveniently referenced to the mass peaks arising from suitable standard peaks, and a variety of kinetic measurements can thus be performed using this device. The programmer described here is very inexpensive, compared to certain other data acquisition systems, and it is probably useful in many other instrumental applications as well.
Application of Laser-Excited Raman Spectroscopy to Organic Chemistry I. Raman Spectra of Some Acyclic Monoterpenes
Authors: Freeman Stanley K. , Mayo Dana W.
Published: November 2005

Laser-Raman spectra of 12 acyclic terpenoids has been recorded. Assignments were made for stretching mode vibrations of carbon-carbon double bonds by comparison with infrared spectra. The results of intensity and depolarization studies are discussed.
Counting Strategy in X-Ray Emission Spectroscopy
Authors: Plummer L. N.
Published: November 2005

Equations are presented for obtaining greatest precision from available counting time, and minimum counting time for a specified precision in quantitative x-ray spectroscopic analyses. The equations are derived for analytical situations involving determination of the net peak intensity of a line above background and the ratio of the net peak intensities of two lines above one and two backgrounds. Graphical solutions are provided for some of the equations.
Electronic Absorption Spectra of Benzylchloride Vapor
Authors: Amma R. Ammini , Nair K. P. R. , Rai D. K.
Published: November 2005

The near-ultraviolet absorption spectra of benzylchloride vapor have been photographed on a medium quartz spectrograph. Two systems of bands have been observed, one at 37 115 cm−1 and the other at 41 748 cm−1, which correspond to B2 ↓ A1 and A1 ↓ A1 electronic transitions. The observed spectra have been analysed in terms of fundamentals and overtones.
The Effect of Ion Mass, Ion Energy, and Developing Time on the Sensitivity of Ilford Q Plates
Authors: Grais Khairi I.
Published: November 2005

An investigation has been made of Ilford Q as to the sensitivity dependence of the ion mass, ion energy, and the developing time, using a second order mass spectrometer with an electron impact source. Description and analysis of the results obtained are represented in this paper. It was found that the experimental data agree reasonably well with the suggested empirical equation.
Recent Trends in Analytical Atomic Absorption Spectroscopy
Authors: Slavin Walter , Slavin Sabina
Published: November 2005

Atomic absorption spectroscopy is reviewed especially as to the effect of developments in the past few years on analytical applications. Sources and sampling devices are given special attention. Atomic absorption, flame emission, and atomic fluorescence are compared as to their detection limits and their applicability to analysis. It is shown that the three methods are in many ways complementary rather than competing. The potentialities of resonance spectroscopy are examined and instrument systems utilizing resonance methods are described.
Infrared Spectroscopy at Sub-Ambient Temperatures: II. Pure Molecules
Authors: Hermann T. S. , Harvey S. R. , Honts C. N.
Published: November 2005

A great deal of research has been conducted on the infrared spectra of pure molecules at low temperatures. Only a limited amount of information can be acquired on molecules in the liquid, amorphous, and crystalline states. The theories describing the liquid and amorphous states are not yet completely adequate, whereas the theories describing the gaseous and crystalline states appear to be well established. The value of lowering the temperature of molecules appears to be that of simplifying their spectra by increasing the order of the system.
Computer Analysis of Photographed Optical Emission Spectra
Authors: Helz A. W. , Walthall F. G. , Berman Sol
Published: November 2005

A recording system and computer can be used for the complete spectrochemical analysis of photographed spectra. Transmission values, taken at equal intervals of travel along the spectrum are transferred to magnetic tape with high precision, high speed, and in a form suitable for computer processing. This processing may include wavelength determination, line identification, and plate calibration.
Rhodium Determination by Atomic Absorption Spectrometry Using the Nitrous Oxide—Acetylene Flame
Authors: Atwell M. G. , Hebert J. Y.
Published: November 2005

A study of the interferences encountered in determining rhodium in aqueous solutions by atomic absorption spectrometry is described. In this study, solutions containing rhodium and varying concentrations of a number of the more common elements and acids were aspirated into air—acetylene and nitrous oxide—acetylene flames. It was found that very serious interferences were encountered with the air—acetylene flame, while the nitrous oxide—acetylene flame was essentially free from such interferences. Optimum excitation parameters and the precision of replicate analyses are presented.
Determination of Antimony, Tin, and Arsenic in Antimonial Lead Alloys by X-Ray Fluorescence
Authors: Fillmore C. L. , Eckert A. C. , Scholle J. V.
Published: November 2005

Savings in man-hours of approximately 50% were gained with even greater reduction in elapsed time when fluorescent x-ray emission replaced classical wet methods to determine Sb (2%–7%), Sn (0.15%–0.75%) and As (0.05%–0.60%). No statistically significant differences were found in results, and scatter was less with the x-ray method. The problem of segregation in the sample was eliminated, and a surface of the required quality was obtained by a special method of sample preparation in which 5–20 ml of molten lead was poured into 1 liter of water, and the resulting granules were pressed to 95% density briquettes at 50 000 psi. The working curves, linear in the ranges stated, were established from alloys calibrated by the classical methods. Standard deviations were calculated from repeated x-ray determinations on a reference alloy (Sb: 5.89%±0.043; Sn: 0.36%±0.012; As: 0.175%±0.008).
Infrared Spectroscopy at Sub-Ambient Temperatures: IV. Sample Cells
Authors: Hermann T. S.
Published: November 2005

The design of cells is governed by the nature of the information desired from the experiments, the physical state, history and matrix of the sample, the longevity and cost of the cell, and the spectral region of interest. Several cells are described in this paper in four categories: conventional transmission cells; matrix-isolation cells; pseudo-matrix isolation cells; and multiple internal reflection cells.
Use of a Calculation Method for X-Ray Emission Analysis
Authors: Batt A.
Published: November 2005

The use of a fundamental parameter method for effecting matrix corrections in quantitative x-ray spectrochemical analysis is described. A versatile computer program calculates composition directly from measured intensities. Variations in the basic approach are employed in the analysis of a series of sulfide and oxide samples. The Applied Research Laboratories multi-channel x-ray quantometer (MXQ) is briefly described.
Historical Advances in Spark Emission Spectroscopy
Authors: Walters J. P.
Published: November 2005

Major developments in the understanding of the physics and chemistry of the atmospheric pressure spark discharge are presented and commented upon. These include work in the areas of equipment, initial gap breakdown, spark channel formation, electrode sampling phenomena, sample propagation phenomena, excited state production, related plasma physics, and counter electrode phenomena.
Digestion of Sugar Beet Leaves for Atomic Absorption Spectroscopy
Authors: Harrison Merle , Andre Charles
Published: November 2005

A modified digestion mixture utilizing sodium molybdate as a catalyst is described for plant materials. In atomic absorption spectroscopy, special attention is given to calcium analyses using this mixture, because of various interfering ions. The digestion mixture is suitable for numerous other cation determinations. Also, a method of increasing the sensitivity for copper by adding methanol is described.
Improving the Diffracting Properties of LiF: Comparison with Graphite
Authors: Vierling J. , Gilfrich J. V. , Birks L. S.
Published: November 2005

The integral reflection coefficient R was measured for the (200) planes in LiF using a double crystal spectrometer over the wavelength range 0.7–2.1 Å. For cleaved LiF, R was about 0.7 × 10−4 rads compared to 0.3 × 10−4 calculated for the theoretically perfect crystal case. After abrading with 1.5–20 μ carborundum, R increased to 2.90 × 10−4 at the 0.7-Å end of the range and to 3.68 × 10−4 at the 2.1-Å end. For a flexed and reflattened crystal, R increased further to 9.45X10−4 at the 0.7-Å end of the range but was not improved over the abraded crystal at the 2.1-Å end. Theoretical R values for mosaic graphite were compared with LiF. The value for graphite at 1.66 Å was 4.5 times higher than that calculated for mosaic LiF and 1.3 times higher than the measured graphite values of Gould, Bates, and Sparks. It appears that one can approximate theoretical mosaic crystals by either distorting a nearly perfect crystal such as LiF or by orienting powder crystallites as in the case of graphite.
Recent Results with a Nitrous Oxide—Acetylene Burner in Atomic-Absorption Flame Photometry
Authors: Shifrin N. , Hell A. , Ramírez-Muñoz J.
Published: November 2005

Performance data are presented for several elements determined by atomic-absorption flame photometry with the use of a high sensitivity nitrous oxide—acetylene burner. Utilizing the specific advantages of this flame, the effect of gas mixtures, feeding rate, and the height of reaction zone on the sensitivities achieved are presented. Flame profiles of several elements studied will be discussed with emphasis on using multiple-pass optics for increased sensitivities. Information will be presented on the problems of this type of flame. Results are presented in terms of the precision and accuracy of routine determinations under selected optimum system conditions and will be discussed.
A Direct-Reading Polychromator for Emission Spectroscopy
Authors: Beatrice Edwin S. , Glick David
Published: November 2005

Construction and use of a photomultiplier-tube direct-reading polychromator for emission spectroscopy is described for application to measurement of spectral line intensities from plumes generated by a ruby laser microprobe. Simultaneous correction for background adjacent to each spectral line measured is provided. Advantages include capability of external precision alignment and the use of optically and electronically matched components for recording the line and background intensities. Although the unit is adaptable to commercial spectrographs, the polychromator constructed was made to fit a Czerny-Turner, f/6.3, emission spectrograph (Jarrell-Ash Co., Waltham, Mass.) which had been designed for photographic recording.
Photographic Emulsion Calibration with the Use of a Digital Computer
Authors: Boswell C. R. , Berman S. S. , Russell D. S.
Published: November 2005

A computer program, written in Fortran IV, has been developed for the calibration of photographic emulsions using the two-step method of Churchill. Innovations in this program are: (1) the proportional weighting of all points used in the construction of the preliminary curve to their precision of determination; (2) the examination of the preliminary curve of best fit with the rejection of spurious values; and (3) an automatic increase of the degree of the equation used if a random scatter of points about the preliminary curve has not been found. A table relating relative intensities to percent transmittance is printed and a data card containing the coefficients of the emulsion calibration curve is punched.
Vacuum Ultraviolet Spectroscopy
Authors: Milazzo Giulio , Cecchetti Gaetano
Published: November 2005

A review is presented on vuv spectroscopy, discussing the optics necessary, instrumentation used in absorption and emission vuv, and measurement of wavelength and intensities. Finally, several applications of the technique of interest to the chemist are presented.
Use of the Direct Current Arc Voltage in Determining the Carbonate Content of Bone
Authors: Spadaro Joseph A.
Published: November 2005

An example is presented of the usefulness of arc voltage recordings in the design of a synthetic matrix for the trace analysis of bone ash and bone mineral. In particular, the sensitivity of the voltage patterns of calcium phosphate to carbonate concentration enabled a simple quantitative estimate of the carbonate content of bone to be made, and measurement of the average arc temperatures substantiated the result. A method is therefore suggested for the determination of percent amounts of carbonate in similar materials which requires but a few milligrams of sample. This determination is important in the study of the nature, deposition, and crystallization of bone mineral and other biological calcifications. It may also be useful in the analysis of the various geological apatites.
Investigation into Increasing the Precision of a Rotating Disk-Solution Technique for the Analysis of Silicates
Authors: Ondrick C. W. , Suhr N. H. , Medlin J. H.
Published: November 2005

The precision of major—minor silicate analyses employing a rotating disk-solution technique may be improved upon by restricting the number of sparkings on each end of the counter electrode to no more than two times; and by placing a more rigid control on disk weight than presently supplied by the manufacturer, i.e., prior to sparking, weigh the disks and place them in weight categories with a range of no greater than 30 mg. Boom temperature fluctuations of 5°F or less are enough to decrease precision of the analysis; therefore, in order to maintain maximum precision, a tighter control on room temperature is required. Changes in barometric pressure affect the precision of certain major and minor oxides, therefore, during periods of stable barometric pressure the precision of the analysis is at an optimum. Relative humidity in the range of 40%–60% and minor shifts in the optical alignment of the grating appears to have little effect on the precision of the analyses.
Adjustment of a Grazing Incidence Spectrometer for Maximum Resolution
Authors: Alexander E. , Fraenkel B. S.
Published: November 2005

A routine method to adjust a grazing incidence spectrometer for maximum resolution is described. The trial and error method uses as variable, the distance of the slit from the Rowland circle. Examples of resolved doublets are shown.
Mass Spectra of Organometallic Compounds. V. Some Π-Cyclopentadienyl Derivatives Not Containing Carbonyl Groups
Authors: King R. B.
Published: November 2005

The mass spectra of the following compounds are reported: (1) the π-eycloheptatrienyl derivatives C5H5 MC7H7, ( M = V and Cr); (2) the π-pyrrolyl derivative C5H5FeC4H4N; (3) the ethylene derivative C5H5Rh(C2H4)2; (4) the 1,5-cyclooctadiene derivatives C5H6 MC8H12 ( M = Rh or Ir); (5) the trimethylplatinum derivative (CH3)3PtC5H5; (6) the nickel and palladium complexes C3H5PdC5H5, C10H12OCH3PdC5H5, and C5H5NiC13H17. The following features of particular interest were observed: (1) evidence for elimination of neutral C6H6 fragments from the C5H5- MC7H7 compounds; (2) evidence for elimination of C2H2, HCN, C2H2N, C4H4N, and Fe fragments from the parent ion of C5H5FeC4H4N; (3) evidence for stepwise elimination of ethylene ligands from C6H5Rh(C2H4)2; (4) evidence for relatively weak metal–π-cyclopentadienyl bonds in the nickel and palladium derivatives.
Activation Analysis of Normal and Atherosclerotic Aortas
Authors: Strain W. H. , Rob C. G. , Pories W. J. , Childers R. C. , Thompson M. F. , Hennessen J. A. , Graber F. M.
Published: November 2005

Normal and atherosclerotic aortas from rats and man have been analyzed by neutron activation to determine changes in the content of Ca, Cd, Co, Cu, Mg, Mn, Se, V, and Zn with the development of degenerative changes. Samples of aortic tissue were weighed, dried at 110°C overnight, and irradiated for 30 min in a thermal neutron flux of 1.8X1012 n/cm2-sec in a TRIGA Mark I reactor. Immediately after irradiation, the samples were wet-ashed in the presence of carriers, the various elements were then radiochemically separated, and the separated fractions were counted by multichannel gamma-ray spectrometry. Definite values, or firm upper limits, for the elements were calculated by computer. With increasing degree of atherosclerosis, the Ca content rose from <350 to 36 000±2000 ppm; Co from undetectable to 0.34 ppm; Mg from <110 to 880 ppm; Mn from 0.34 to 1.26 ppm; and Zn from 37 to 152 ppm. Significant changes could not be detected in Cd, Se, and V; changes in Cu were not consistent. These results are discussed in relation to the pathological changes and to zinc therapy in the treatment of atherosclerosis.
Effect of Halogen Compounds on the Molecular Spectra of Air
Authors: Nelson Gary O.
Published: November 2005

Airborne halogen compounds have been found to greatly increase the intensity of the N2 and NO molecular spectra of air in an ac spark. Chlorinated materials cause the largest enhancement followed by brominated, iodinated, and fluorinated compounds. This phenomenon can effectively be used to measure the presence of many volatilized halogen compounds present in concentrations as low as 1 ppm.
Mass Spectra of Organometallic Compounds. IV. Some Mononuclear Fluorocarbon Derivatives of Transition Metals
Authors: King R. B.
Published: November 2005

The mass spectra of the following fluorocarbon derivatives of transition metals have been investigated: (a) the perfluoroalkyl derivatives RfMo (CO)3C5H5 ( Rf = CF3 and C3F7); (b) the perfluoroacyl derivatives CF3COM(CO)3C6H5 (M = Mo and W), C3F7COM(CO)3C5H5 (M = Mo and W), and C3F7COFe(CO)2C6H6; (c) the perfluoraryl derivatives RfFe(CO)2C5H5 ( Rf/ = C6F5, p-HC6F4, 3, 4-H2C6F3, and p-CF3C6F4); (d) the hexafluorobutyne derivatives [(CF3)2C]3 MNCCH3 (M = Mo and W); and (e) the bis (trifluoromethyl)tetramethylbicyclo-[2.2,2] octatriene complexes C14H14F6Fe (CO)3 and C5H5CoC14H14F6. Unusual features observed in these mass spectra include the following: (a) Evidence for elimination of the neutral metal fluoride fragments FeF2 and C5H5CoF; (b) evidence for the elimination of neutral HF and CF2 fragments; (c) evidence for the elimination of a bridge in the bicyclo [2,2,2] octatriene derivatives; (d) decarbonylation of RfCOMo (CO)3C5H5 compounds, but not their tungsten analogs, in the mass spectrometer; and (e) evidence for the eliminations of C4F4 and CH3CN fragments in the mass spectra of the [(CF3)2C2]3MNCCH3 complexes.
Optimal Detection Sensitivities in Activation with Fast Neutrons from an 241Am-242Cm—Be Source
Authors: Wing James , Wahlgren Morris A.
Published: November 2005

The detection sensitivities of 60 chemical elements in activation with the fast neutrons from an 241Am-242Cm—Be source have been measured. The source consisted of six slugs with a total output of 4.8X109 unmoderated neutrons/sec, and a flux of 1.4×108 fast neutrons/sec-cm2. In general, the sensitivity (counts in a selected photopeak per gram of target element) for each element was obtained with irradiation for two to three half-lives of the short product nuclide, and counting for the same length of time. Neither irradiation nor counting was longer than 1 h. The detector was a cylindrical thallium-activated sodium iodide crystal 10 cm long and 10 cm in diam. The measured sensitivities are compared with reported sensitivities in activation with thermal neutrons.
Infrared Spectra of Some Perfluoroalkyl-Substituted Fluoro-s-Triazines
Authors: Sawodny Wolfgang , Hynes John B. , Dawson John W. , Niedenzu Kurt
Published: November 2005

The infrared spectra in the sodium chloride region of the series trifluoro- s-triazine tris (trifluoromethyl)- s-triazine and trifluoro- s-triazinetris(perfluoroethyl)- s-triazine have been recorded and normal vibrations were assigned. The transitions of characteristic frequencies are discussed.
Raman Apparatus Using Laser Excitation and Polarization Measurements. Rotational Spectrum of Fluorine
Authors: Claassen Howard H. , Selig Henry , Shamir Jacob
Published: November 2005

Various schemes are compared for measuring depolarization factors in Raman spectra with laser excitation. Optical systems are discussed for producing a laser beam free of unwanted emission lines and for focusing scattered light on the slit and on the detector. The rotational spectrum of gaseous F2 has been used to determine a rotational constant of Bo=0.8841 ±0.0006 cm−1, corresponding to r0=1.4168±0.0005 Å.
Some Parameters Affecting Auger and Photoelectron Spectroscopy as an Analytical Technique
Authors: Yin L. I. , Adler I. , Lamothe R.
Published: November 2005

Various possibilities of Auger and photoelectron spectroscopy as an analytical technique are discussed. In some applications simple electrostatic analyzers with coarse resolution may suffice and even be preferable. Typical spectra obtained with a hemispherical electrostatic analyzer of 0.6% energy resolution are presented and discussed. Such factors as sample thickness, sample potential, surface contamination, and incident angle of the exciting x rays have been found to affect the quality and character of the observed spectra. These results characterize some of the features, problems, and capabilities of applied Auger and photoelectron spectroscopy.
Zinc-secreting Paneth Cells Studied by ZP Fluorescence
Authors: Giblin Leonard J. , Chang Christopher J. , Bentley Anthony F. , Frederickson Cathleen , Lippard Stephen J. , Frederickson Christopher J.
Published: November 2005

We have used a new family of zinc-specific-responsive fluorescent dyes (ZPs) to study the sequestration and secretion of zinc from Paneth cells, which are located in the bases of the crypts of Lieberkühn within the rat small intestine. Vivid ZP fluorescence zinc staining of Paneth cell secretory granules is seen in both cryostat sections and isolated crypts, providing firm evidence for a pool of labile (rapidly exchangeable) zinc within these cells. We further demonstrate that this ionic zinc pool is secreted under physiological conditions. In vivo stimulation of the small intestine by IP injection of the secretagogue pilocarpine results in discrete zinc staining within the lumens of subsequently isolated crypts, concomitant with a decrease in the zinc staining of Paneth cell granules located within the same crypts. In contrast, the secretion of zinc into the lumens of isolated crypts stimulated in vitro with either carbachol or LPS (lipopolysaccharide) is not observed. However, a distinct change in Paneth cell morphology, suggesting attempted secretion, is seen in response to the direct application of cholinergics but not LPS. These findings suggest that zinc is coreleased with other Paneth cell anti-microbials, and that the intact intestine is necessary for secretion into the crypt lumen.
Ontogeny and cellular localization of SRY transcripts in the human testes and its detection in spermatozoa
Authors: Modi D , Shah C , Sachdeva G , Gadkar S , Bhartiya D , Puri C
Published: November 2005

The sex-determining region on the Y (SRY) gene is unequivocally designated as the testis-determining factor in mammals; however, its roles beyond sex determination, if any, have been hitherto unknown. To determine whether SRY has any roles beyond sex determination, herein the expression of SRY mRNA was investigated in the midtrimester human fetal, infantile and adult testes as well as in ejaculated spermatozoa. High levels of SRY transcripts werein situlocalized to the Sertoli cells of the developing testis at 9 weeks of gestation, and the expression persisted at comparable levels throughout the midtrimester (until 22 weeks) and also in the testis of an infant at 3 months of age. The germ cells and other somatic cells in the testes of fetuses and the infant were negative for SRY expression. The mRNA for SRY was detected in the spermatogenic cells, particularly the spermatogonia and the round spermatids; the expression was negligible in the meiotic stages. A single transcript of ~1.2 kb was detected in the adult testes and isolated spermatogonial cells. In the adult testis,in situhybridization (ISH) studies revealed a switch in the cellular localization of SRY transcripts. SRY transcripts were also demonstrable by RT-PCR of RNA from ejaculated human spermatozoa. ISH revealed the presence of SRY transcripts in the midpiece of 50% of ejaculated sperm. These results suggest that SRY may have extensive roles in male reproductive physiology, such as maturation of fetal testis, spermatogenesis, sperm maturation and early embryonic development.