bluuebunny/crossref_metadata_2025 huggingface dataset:
Soviet Spectrographic Equipment
Authors: Malinek M.
Published: November 2005

Standard Soviet spectrographic equipment is reviewed, and some of the properties of the newer Soviet spectrographic equipment are briefly discussed.
Pressure-Broadening Effects on Infrared Peak Intensities of Hydrocarbons
Authors: Altshuller A. P. , Wartburg A. F.
Published: November 2005

The pressure-broadening effects of one atmosphere of air or of carbon dioxide on various infrared bands of hydrocarbons have been investigated. Large pressure-broadening effects are shown by ethylene at 10 52 microns and acetylene at 3.1 and 13 7 microns, moderate effects by acetylene at 7.4 microns and propylene at 10 95 microns, and small effects by 1-butene at 10.85 microns, trans-2-butene at 10.375 microns, and benzene at 9.50 microns. The variation of absorbance at several of the infrared absorption maxima of ethylene and acetylene has been investigated using varying partial pressures of air or carbon dioxide at fixed partial pressures of the 2 hydrocarbons
Physico-Chemical Characterization of Some 5,5-Disubstituted 1:3-Dimethyl Barbituric Acids
Authors: Manson Jane M. , Cloutier J. A. R.
Published: November 2005

Infrared spectra and ultraviolet characteristics for nine 5,5-disubstituted 13-dimethyl barbituric acids are presented. X-ray diffraction powder data are given for 5 of these compounds
Infrared Spectral-Structural Correlations of Some Substituted Pyridines
Authors: Godar Edith M. , Mariella Raymond P.
Published: November 2005

Three series of substituted pyridines have been prepared having substituents in various positions on the ring. Although there were variations in the chemical nature and in the position of these substituents, it was found that certain fundamental absorption bands are typical of all the pyridines studied. The separation of the two bands in the 1600–1500 cm−1 region does not appear to be helpful in determining the position of substituents, but absorption in the 950–750 cm−1 region does give a clue as to the number of adjacent hydrogens on the pyridine ring There appears to be a band very characteristic of the cyclohexeno ring, thus confirming previous work. In addition, a band was found which is due to the cyclohexeno ring, as modified by the attached pyridine ring There seems to be absorption characteristic of the cyclohepteno ring Correlation is made of the several substituent groups when attached to the pyridine ring, as compared to the same groups attached to the benzene ring.
Emission Spectrographic Analysis of 65/35 and 50/50 Magnesium-Aluminum Alloys
Authors: Lader Seymour
Published: November 2005

An emission spectrographic method has been developed that has been found suitable for the determination of iron, silicon, chromium, lead, titanium, zinc, and tin in a concentration range of 0 07–1.0% The method consists of dissolving the sample in hydrochloric and sulfuric acids and converting it to the sulfate. One percent nickel is added as an internal standard and the sample is mixed with 2 parts of graphite. The procedure is found to have an average coefficient of variation of 5.1% for all determinations and has been found suitable is a rapid production control method for magnesium-aluminum alloys of 65/35 and 50/50 compositions.
Spectrographic Analysis of Hafnium by a Point-to-Plane Technique
Authors: Brayer R. C. , O'Connell R. F. , Powell A. S. , Gale R. H.
Published: November 2005

A method has been developed for the analysis of hafnium metal for aluminum, copper, iron, titanium, and tungsten in the ppm range and zirconium in the 1 0–4.0% range. Solid machined pieces 1 × 1 in. or larger are used. Spectra are excited with a low voltage ignited ac arc with low inductance and capacitance. Hafnium serves as the internal standard The method offers an increase in speed and improved precision over the carrier distillation technique which has been commonly used
Sensitometric Properties of a Polaroid Emulsion as Applied to Spectroscopic Analysis
Authors: Bryan F. R. , Runge E. F.
Published: November 2005

Polaroid-Land Type 46-L Projection Film is investigated as a medium for recording optical spectra for the purpose of qualitative and quantitative spectrochemical analysis The film's high spectral sensitivity extends from 3000 to 6000 A In the analytically important 3000–4000 A region, emulsion contrast is found to be adequate and reasonably constant, gamma averages to about 23 and is reproducible to within ±0 1 from frame to frame Speed is sufficient for nearly all spectrochemical purposes Resolution of at least 30 lines/mm is obtainable. Analytical precision resulting in a coefficient of variation of less than ±5% indicates that Polaroid films are likely to find some utility in quantitative as well as qualitative analysis.
Spectroscopic Standard Samples of Titanium and High-Temperature Alloys
Authors: Michaelis Robert E.
Published: November 2005

Ten new spectroscopic standard samples are now available from the National Bureau of Standards. These consist of three standards each for two titanium alloys and four standards for high-temperature alloys. The new standards are useful for both optical emission and x-ray methods of analysis.
The Quantitative Determination of Gallium in Micro Samples by the Graphite Spark
Authors: Murt E. M. , Bready J. C.
Published: November 2005

A quantitative spectrographic procedure is described for the determination of gallium in micro samples of indium-gallium alloys A solution procedure is employed with spark excitation and molybdenum as the internal standard The accuracy of the method ranges from 11% to 22% depending on the concentration level of interest
A Study of the Influence of Buffers on the Accuracy and Sensitivity of Spectrochemical Results
Authors: Holdt G.
Published: November 2005

A method is described that allows the simultaneous estimation of buffer efficiency and loss of sensitivity caused by buffer dilution. The smallest amount of buffer, which is necessary to eliminate the effect of the matrices satisfactorily, can be determined. In this way an unnecessary loss of sensitivity due to too high a buffer dilution, can be avoided. The method is based on the study of the behaviour of the analysis lines of a number of elements present in two matrices with different behaviour and diluted with successively increasing buffer amounts. An application of this method is given for a specific rapid evaporation procedure using CuO and Li2CO3 as buffers. The dependence of the arc temperature on buffer type and concentration is discussed for both matrices. It is shown that the trend of the relative and of the absolute sensitivity limits with buffer concentration can be estimated from the behaviour of the log intensity value and of the log of the intensity/weight ratio. The smallest satisfactory buffer amounts established for CuO and Li2CO3, agree with recommendations in the literature.
Quality Control of Steel Using Clock and Chart Recording Photoelectric Spectrometers
Authors: Woodruff Joseph F. , Thomas Arba H.
Published: November 2005

A check analysis program initiated over twenty-five years ago is used to evaluate the performance of emission photoelectric spectrometers in five production control laboratories of the Armco Steel Corporation. For comparison, evaluation of analyses using conventional chemical methods by these same laboratories prior to instrumental analysis is also made The paper describes the check analysis program and presents analytical data used to evaluate the accuracies of the two types of photoelectric spectrometers and the conventional chemical methods used by the production laboratories.
Vibrational Spectra of Benzene Derivatives I. Para-Substituted Phenols
Authors: Jakobsen R. J. , Brewer E. J.
Published: November 2005

The infrared spectra of 16 para-substituted phenols have been recorded between 1600 and 300 cm−1. Assignments have been made for the frequencies of the p-X-C6H4-OH molecule where X is considered as a point-mass group. These assignments were made taking into account both the Raman spectra reported in the literature and Raman spectra obtained experimentally. Disregarding the four carbon-hydrogen stretching frequencies and the oxygen-hydrogen stretching frequency, 25 of the remaining 28 frequencies of the p-X-CoH-OH group have been assigned. Nine of the assigned frequencies were found to be either substituent sensitive or characteristic of para-substituted phenols.
High Resolution Infrared Spectroscopy in the Analysis of Liquids and Solutions
Authors: Sloane Howard J.
Published: November 2005

Careful examination of organic liquids and solutions at very narrow spectral slit widths indicates that many compounds exhibit several absorptions of half band width narrower than 5 cm−1, particularly at the medium and long wavelengths. This suggests that sodium chloride prism spectrophotometers are currently being operated under conditions which produce rather significant errors in intensity and band width on some narrow bands.

In order that this “finite slit error ‘be 3% or less in measuring peak absorbance, a spectral slit width about 1/5 of the natural half band width must be employed, e.g., a resolution of 1 cm−1 for a band of 5 cm−1 half band width The high resolution afforded by the grating instrument allows accurate intensity measurements on the typically narrow bands of such materials as indene at 1018 cm−1, cyclohexane at 861 and 903 cm−1 and acetonitrile at 2255 cm−1.

Other advantages of the high resolution grating spectrophotometer for solution spectroscopy are discussed
The Silicon-Phenyl Asymmetrical Stretching Vibration
Authors: Harvey Mack C. , Nebergall William H.
Published: November 2005

Calculations based on the assumption that the silicon-phenyl group is a simple harmonic oscillator and a study of the infrared spectra of tetraphenylmethane, tetraphenylsilane, tetraphenylgermane, tetraphenyltin, and tetraphenyllead indicate that the asymmetrical silicon-phenyl stretching vibration should occur near 515 cm−1. A strong infrared absorption band near 515 cm−1 has been observed in the infrared spectra of twenty-two phenylsilanes of the types (C6H5)4Si, (C6H5)3SiX, (C6H5)2SiX2, (C6H5)2SiXY, and C6H5SiX2Y and has been assigned to the silicon-phenyl asymmetrical stretching vibration.
The Spectrographic Determination of Trace Elements Using a Three-Step Filter and the Respektra Calculator
Authors: Chamberlain G. T.
Published: November 2005

A spectrochemical method has been evolved for the determination of trace elements in soils and plants with the objects of reducing the microphotometry involved in the variable internal standard method and of increasing the throughput of samples. A 3-step filter replaces the step sector and evaluation is achieved from an emulsion calibration curve prepared from step filter data using the Respektra calculator. The errors involved in certain stages are studied, and the resulting method shows an accuracy comparable to the original.
Analysis of Organic Reaction Products by Combined Infrared-Gas Chromatography Techniques
Authors: Grasselli Jeanette G. , Snavely Marcia K.
Published: November 2005

The combined use of infrared spectroscopy and gas-liquid chromatography provides a powerful analytical tool for solving a variety of problems. A simple trapping technique is described which allows 0 4 μl of liquid sample to be examined in the infrared without use of beam condensers. Examples are presented to show its usefulness in qualitative analysis. The trapping technique is efficient enough to allow quantitative collection for analysis by infrared spectroscopy of two-component, unresolved peaks on the gas Chromatograph. Application to dilute water solutions of acrolein and acetone is given
On Background Correction in Spectrum Line Photometry
Authors: Slavin Morris
Published: November 2005

The process of subtracting background exposure from line exposure, as a means of correcting for the effect of background, has been investigated. Of two lines of equal exposure, one in a clear ground (and presumably requiring no correction) and the other in a measurable background, which had been subtracted, the energy of the former is greater. This difference is constant and independent of both line and background densities. As the addition of photographic exposures is not open to question, the probable cause of this difference is the less than inertial exposure the emulsion received, here called the subliminal exposure, either as scattered light in the spectrograph or during manufacture. Its effect on the emulsion characteristic is to reduce the contrast. This subliminal exposure is ordinarily not subtracted. Although the resulting error from these two causes is small for dense lines, for light lines it can amount to 50%. In view of these findings, changes in the standard photometric procedure are suggested.
The Reflectance Spectra of Metallic Oxides in the 300 to 1000 Millimicron Region
Authors: Vratny F. , Kokalas J. J.
Published: November 2005

The reflectance spectra of forty metallic oxides and oxide-like materials have been obtained in the spectral region from 300 to 1000 millimicrons. The data are discussed in relation to the electronic structure of the materials.
A Digital Printer for Use with the Cary Model 11 Spectrophotometer
Authors: Jones J. H. , Clark G. R. , Heine K. S. , Williams R. F.
Published: November 2005

This paper describes an attachment for the Cary model 11 spectrophotometer that will print out the absorbance and wavelength at any number of preselected wavelengths, while the instrument is drawing the usual absorbance—wavelength curve Bidirectional revolut'on counters with electrical readout are used to digitize the wavelength and absorbance data; the digitized data are used to operate a parallel entry printer The program, i.e., wavelengths at which data are to be printed, is controlled by the data from the wavelength digitizer The printer will give absorbance data precise to 0.01 absorbance units when the spectrophotometer is scanning at the rate of 2 1/2 millimicrons/sec.
X-Ray Fluorescence Analysis of Light Elements, Aluminum-Chromium
Authors: Carter G. F.
Published: November 2005

The best conditions obtainable from available equipment for x-ray fluorescence analysis of the elements aluminum through chromium are presented. Approximate limits of detection of aluminum, silicon, and titanium in iron alloys are given. A chromium target tube was compared with a tungsten tube and was found to give a several-fold improvement over the tungsten tube in the analysis of the elements aluminum through titanium. A lithium fluoride analyzing crystal has been shown to be superior to an ethylenediamine ditartrate crystal for the elements from chromium to potassium, the lightest element that may be analyzed with a LiF crystal.
Ion Exchange-Spectrographic Determination of Thorium in Uranium Ores
Authors: Ko R.
Published: November 2005

The determination of 0.01 ppm of thorium in 1 g of uranium ore by a combined ion exchange-spectrographic analysis is presented. Thorium is separated from the chemically complex ore solution by anion exchange in hydrochloric and nitric acid media and determined spectrographically using zirconium as the internal standard. The precision of the method expressed as a coefficient of variation is estimated to be ±6%.
Use of a High-Voltage AC Arc Source for the Spectrochemical Analysis of Plant Tissue
Authors: Connor Jane , Bass S. T.
Published: November 2005

A method for the spectrochemical analysis of plant tissue, designed principally for use by graduate students with minimum guidance from the spectrographer, has been devised. The method is designed to eliminate or reduce at least the many matrix problems of biological systems The ash of plant tissue is mixed with the buffer powder (K2SO4-graphite) in portions determined by the amount of ash and potassium present in the plants.
Determination of Lead in Leaded Steels by X-Ray Spectroscopy
Authors: Kilday Betty Ann , Michaelis Robert E.
Published: November 2005

The determination of lead in leaded steel by x-ray spectroscopy is highly dependent on proper surface preparation because of the tendency toward smearing or removal of the lead. A metallographic preparation technique using diamond dust as the abrasive is shown to provide reproducible and accurate results even with appreciable changes in the particle size of the lead. This work is part of a cooperative program with the United States Steel Corporation in the preparation of a leaded-steel spectrochemical standard. Although certain inhomogeneities, both linear and radial, were observed by x-ray spectroscopy in the rods tested, suitable material has been selected for use as the National Bureau of Standards spectroscopic standard
An Appearance Potential Recorder
Authors: Caldecourt V. J.
Published: November 2005

A circuit has been developed that records the electron accelerating potential required to generate a barely detectable ion current at each mass in a mass spectrum. The level of electron accelerating potential attained for each ion peak approaches the true appearance potential for the instrument when the ion peak is one which would be large with 70 v electrons The device is useful to select operating conditions for analyses at low electron accelerating potentials.
Effect of Slit Width on Background Correction in Photographic Photometry
Authors: Slavin Morris
Published: November 2005

Slope of the characteristic curve drawn from measurements of a narrow-lined spectrum is less than that of a curve drawn from broad lines or from continua This is due to. 1) the lateral diffusion of lines within the emulsion, 2) narrow lines being subject to Schwarzschild-Villiger Effect in the densitometer, which particularly tends to change the shape of the toe. (This effect is minimized in dense lines due to diffusion), and 3) the spreading of dense lines, which causes errors in reading background if the area read is too close to the line. Each of the three effects lowers the line-to-background ratio.
The Determination of Lead, Copper and Zinc in Wines by Atomic Absorption Spectroscopy
Authors: Zeeman P. B. , Butler L. R. P.
Published: November 2005

Methods are described for the determination of Pb, Cu, and Zn in wine products. A lead lamp with demountable cathode is described as well as a new type of burner with an eight in absorbing path and a slotted top. The temperature and height of the flame could be adjusted by means of an extra air current fed into the burner through the ordinary acetylene nozzle of a Zeiss atomizer. Heated air was used to atomize the solutions, and the efficiency of the burner was approximately 22%. Concentrated H2SO4 was used to dehydrate the samples before ashing at 500°C Recovery tests for lead were carried out at various temperatures The results for lead are compared for a number of samples with those obtained by chemical analyses. Similar work is described for Cu and Zn. The coefficient of variation for Pb, Cu, and Zn was respectively 3.7%, 4.23%, and 4.11%. The results for Cu and Zn for a large number of wine samples are given.
Spectrographic Analysis of Gold Alloys Used in Semiconductor Devices
Authors: Hyman H. M.
Published: November 2005

A quantitative spectrographic method has been developed for the determination of the following alloying constituents in gold within the concentration range 0.1 to 2.0%: Al, Sb, As, B, Ga, Ge, In, and Sn The method utilizes a rotating-disc solution technique with internal standard control and ac spark excitation The minimum sample requirement for a single exposure is 2.5 mg of gold alloy in a 0 25 ml solution volume Extension of the method to include higher or lower concentration levels or other elements of interest is feasible in most cases. The accuracy of the method ranges from 5 8 to 10.7% at the 95% confidence level.
Spectrochemical Analysis for Some Major and Minor Elements in Rocks
Authors: Webber G. R. , Jellema J. U.
Published: November 2005

Analytical results are reported for a dc arc method of quantitative spectrochemical analysis for major and minor elements in silicate rocks The procedure involves a fusion method of sample preparation with lithium metaborate as flux. Analysis elements are Si, Al, Fe, Mg, Ca, Ti, Mn, and Ba.
Burning Properties of Electrodes for DC Arc Analysis
Authors: Mellichamp J. W. , Buder R. K.
Published: November 2005

A series of tests have been made using two spectrographic electrode materials to evaluate differences in response to the dc arc over a wide variation in current (6 to 38 amp) Carbon anodes burn at a faster rate than graphite, but carbon is overloaded at a lower current density At high currents both materials approach the same burning rate The burning rates are dependent on the arc current, the cross sectional area, and the properties of the grade used Any one of the three variables can be partially compensated for by an equivalent change in the other two. The effects of burning rates on analytical results are discussed
The Mass Spectrum of Tetrachloro Copper Phthalocyanine
Authors: Beynon J. H. , Saunders R. A. , Williams A. E.
Published: November 2005

A method is described by which it has been possible to obtain the mass spectrum of organic compounds of low volatility. The spectrum of tetrachloro copper phthalocyanine is given and the main features are discussed including the isotopic abundance ratios of the molecular ions.
Spectrographic Determination of Trace Amounts of Rare Earths. II. Analysis of Lanthanum, Yttrium, Europium, Prasedymium, Neodymium, and Samarium by the Carrier Distillation Method
Authors: Radwan Z. , Strzyzewska B. , Minczewski J.
Published: November 2005

A method for the spectrographic determination of trace amounts of Eu, La, Y, Nd, Pr, and Sm in the 5 N HCl solution has been developed. The solution is evaporated on graphite powder and excited in the craters of graphite electrodes in a dc arc using the carrier distillation method CsF is used as the carrier. Excitation is made in the special atmosphere of 80% oxygen and 20% argon. For Y and La, the range of determination is from 0.25 to 10 μg/ml and for Eu, Nd, Pr, and Sm the range is from 0 5 to 20 μ g/ml. The average coefficient of variation amounts to ± 10%. It has been found that in the investigated concentration range the influence of some rare earth elements on excitation of the others is negligible This method can be applied also to the analysis of other rare earth elements
Analysis of o-Xylene Oxidation Products by Combined Gas Chromatographic and Spectroscopic Techniques
Authors: Brown R. A. , Quiram E. R.
Published: November 2005

Seventeen hydrocarbons and fifteen oxygenated compounds were identified as products from mild oxidation of o-xylene. These compounds generally had boiling points at 220°C or lower and varied in concentration from 0 003 to 3.5 wt %. What would normally have been a formidable analytical problem was solved with comparative ease using a gas Chromatograph augmented by infrared spectral examination of chromatographic fractions and high molecular-weight mass spectrometry. The gas chromatograph-mass spectrometer apparatus was improved so that it can measure the mass spectra of compounds boiling as high as 350°C.
A Method for Matrix Correction in the Spectrographic Determination of Uranium
Authors: Dennen W. H. , Sankaran A. V.
Published: November 2005

The differences of relative intensity of U 4241A in various matrices is a thermal effect, which can be corrected by use of a temperature sensitive pair of titanium lines. This is illustrated using rock samples.
Physical State Influences on the Intensity of Infrared Absorption Bands
Authors: Sharpless Norman E. , Gregory Dolores A.
Published: November 2005

Using chloranil as a model, the intensities of various bands in the infrared spectrum have been investigated as functions of the particle size of the crystals. As the particles become larger, the values of molar absorptivity appear to approach the value found for a single crystal As the particle size approaches zero, the values increase. The molar absorptivities in solution are higher than those observed for the smallest particles investigated, and the plots of molar absorptivity as function of size may be extrapolated to the solution values as possible limits It appears that there is no orientation of particles in the pellets, while x-ray diffraction data indicate no changes in crystal structure but do show some evidence of the formation of a solid solution. The frequencies of the various bands are independent of the sizes of the particles.
The X-Ray Emission Analysis of Thin Films Produced by Lubricating Oil Additives
Authors: Schreiber T. P. , Ottolini A. C. , Johnson J. L.
Published: November 2005

X-ray emission techniques have proven feasible for the analysis of thin films produced by the reaction of lubricating oil additives with metal parts The method was found applicable to the determination of Zn, Ba, P, S, and Cl in the concentration range of zero to 75 μg/cm2. Standard films were prepared synthetically from standard solutions of the elements of interest.
Solvent Effects on the Infrared Spectra of Organophosphorus Compounds
Authors: Ferraro John R.
Published: November 2005

Solvent effects on the P → O and [p → 0]G absorptions in organophosphorus compounds of the type (GO)3P → O, (GO)3G'P→ O, [(GO)G'PO(OH)]2, [(GO)3PO(OH)]2, and G3P → O are described, where G is an alkyl or aryl group. The unassociated phosphoryl dipoles are affected by solvents in a manner similar to the carbonyl dipole The consequences of the solvent effects on the physical properties of these compounds are discussed.
Improved Methods for the Measurement of Spectral Line Intensities
Authors: Boswell Colin R. , Brooks Robert R.
Published: November 2005

Improved methods for the measurement of spectral line intensities have been developed. Such techniques are based on the authors' modification of the partial Seidel function, referred to as B-functions. A conversion table for these is given. A scale calibrated in B-functions has been incorporated into a Hilger microphotometer enabling such values to be obtained directly without the use of conversion tables. B-values can be plotted directly on to the linear co-ordinate of semilog graph paper if the self-calibration method is used for evaluating line intensities, there is an attendant time saving and improvement in the accuracy of background extrapolation. A nomographic technique developed for use in conjunction with this scale, results in a rapid evaluation of line intensities but with some loss of precision. It is concluded that the technique will result in an improvement of some existing photometric methods.
The Nuclear Magnetic Resonance Spectra of Compounds Related to DDT. I. Non-Aromatic Protons
Authors: Sharpless Norman E. , Bradley Robert B.
Published: November 2005

The nuclear magnetic resonance spectra of a series of compounds related to DDT have been studied as they are influenced by ring or aliphatic substituents or by aliphatic structural changes

The chemical shift of the benzylic or α proton follows the Hammett equation for ring substituents and the Taft variation of this equation for aliphatic substituents. Alkoxy substituents on the ring show alternation of chemical shift of the —OCH2— group protons with chain length and limiting behavior of the terminal methyl group with chain length.

Dehydrochlorination of o,p-DDD produces cis-trans isomers.

Coupling constants are shown to be influenced by ring substitution, particularly ortho chlorine.
Atomic-Absorption Spectroscopy—A Critical Review
Authors: Slavin Walter
Published: November 2005

Atomic-absorption spectroscopy is reviewed as an analytical technique. The effect of recent instrumental advances on analytical procedures is reported. It is now possible to determine every metal and semimetal for which lamps have been made. Analytical procedures by atomic absorption are generalized and limitations of the technique stated. The various instrumental techniques for metal analysis are compared to show for what purposes atomic absorption is useful. Applications in various analytical fields are mentioned briefly.
Investigation of Cleaning Procedures for Agate Mortars and Plastic Tubes with the Aid of a Radioactive Tracer
Authors: Havre Gustav N.
Published: November 2005

Cleaning of agate mortars and plastic vials in the Wig-L-Bug mixer mill was studied by radioactive-tracer technique using 32P as sodium orthophosphate as a tracer. It was found for agate mortars that cleaning with aluminia followed by acid is adequate for preventing contamination of the next sample. Plastic vials used in the Wig-L-Bug mixer are difficult to clean and can hardly be reused more than once.
Determination of Certain Noble Metals in Solution by Means of X-ray Fluorescence Spectroscopy. 2. Determination of Palladium, Rhodium, and Ruthenium
Authors: Wybenga F. T. , Strasheim A.
Published: November 2005

Methods are described for the determination of palladium, rhodium, and ruthenium in matte solutions by means of x-ray fluorescence. The best results for palladium determinations were obtained using background measurements to calculate absorption effects. Palladium was used as a variable internal standard for the determination of rhodium and ruthenium. Coefficients of variation of the order of 1% were obtained throughout.
Analysis of Magnesium and Aluminum Alloys by Atomic-Absorption Spectroscopy
Authors: Mansell Ralph E. , Emmel Herbert W. , McLaughlin Ernest L.
Published: November 2005

The application of atomic absorption spectroscopy to the analysis of magnesium alloys and scrap aluminum is described. Ca, Cu, Mn, and Zn are determined in Mg alloys, while Cu, Fe, Mg, and Zn in the alloy range are determined in the aluminum samples. In aluminum analysis, synthetic standards and a spiking procedure are employed to compensate for matrix effects. Comparison with chemical results shows AA (atomic absorption) to be a reliable analytical tool in these applications.
Approximate Half-Intensity Widths of a Number of Atomic Spectral Lines Used in Atomic-Emission and Atomic-Absorption Flame Spectrometry
Authors: Parsons M. L. , McCarthy W. J. , Winefordner J. D.
Published: November 2005

A Fortran program was written to calculate the approximate total half-intensity linewidths of several spectral lines for a number of atoms in some common analytical flames. By means of this program, total half-intensity linewidths of any atomic spectral line can be calculated if sufficient spectral and flame compositional data are available. Calculations have been made for 136 lines of 60 elements, and the data have been tabulated.
Determination of Calcium and Magnesium in Plant Material and Culture Solutions, Using Atomic-Absorption Spectroscopy
Authors: Berry Wade L. , Johnson C. M.
Published: November 2005

Interferences in the atomic-absorption spectroscopy of cultures and plant materials for Ca and Mg are eliminated by addition of Sr and HClO4. The method described yields good accuracy and precision, and is suitable for routine analysis of large numbers of samples containing widely varying concentrations of unknown and interfering ions.
Direct Determination of Nickel in Catalytic-Cracking Feedstocks by Atomic-Absorption Spectrophotometry
Authors: Kerber J. D.
Published: November 2005

Nickel in catalytic-cracking feedstocks is determined by atomic-absorption spectrophotometry with no sample preparation other than dilution in p–xylene. A modification of the method of additions permits rapid testing with a detection limit of 0.05 ppm Ni and a precision of 0.05 ppm.
Interferences Associated with the Determination of Calcium by Atomic Absorption
Authors: Dickson Richard E. , Johnson C. M.
Published: November 2005

The determination of calcium in solution by atomic absorption is quite satisfactory, provided that potential interferences are overcome. Ionization enhancements and refractory-compound formations are the most important interferences found in the analysis for calcium. Protecting agents and the method of additions can both be used to overcome these interferences.
Determination of Manganese and Zinc in Aluminous Materials, Using Atomic-Absorption Spectrophotometry
Authors: Calkins R. C.
Published: November 2005

Mn and Zn are determinable in Al ores, intermediates, and finished metal by atomic-absorption spectrophotometry, using a particular burner, if suitable separation procedures are employed. Zn may be separated by chloro—anion exchange. Mn is conveniently extracted into chloroform by complexing with 8–hydroxyquinaldine at pH 12. Results from analyses of known samples show that the method is suitable for the calibration of emission spectrographs.
Investigation of Spectral Sensitization III. A Study of the Visible and Infrared Spectra of Some Very Pure Bis-Thiazolinyl and Bis-Thiazolyl Cyanine Iodides
Authors: Leifer A. , Boedner M. , Dougherty P. , Fusco A. , Koral M. , LuValle J. E.
Published: November 2005

A detailed study of the visible spectra in solution and the infrared spectra of the dyes in the solid state have been made for the following vinylogous series of cyanine dyes: [2-bis(3-ethylthiazolinyl)] cyanine iodides, I; [2-bis(3-ethyl-4-methylthiazolyl)] cyanine iodides, II; and [2-bis(3-ethyl-4,5-diphenylthiozolyl] cyanine iodides, III. Each dye, to be acceptable for study, had to be chromatographically pure, give a correct microchemical elemental analysis, and be free of electron-spin resonance (free radical) signals. These vinylogous series of dyes form a systematic group. That is, in series I there is only a resonant conjugated chain of alternate single and double bonds present between the two nitrogen atoms; in series II there are additional olefinic unsaturated bonds which are in conjugation with the resonant conjugated chain; and in series III there are additional phenyl rings in conjugation with the entire pi bond system present in II. The characteristic red shift of the principal absorption maxima was observed for these dyes in the visible as the number of methine linkages increased. Furthermore, a small relative red shift of the absorption maxima has been observed for this group of dyes and has been interpreted on the basis of the type of unsaturation present in conjugation with the resonant conjugated chain. Assignments of vibrational modes to separate absorption regions have been made for these vinylogous series of dyes. A correlation of the dye structure with the absorption bands has been made. Each vinylog gave rise to a characteristic pattern of resonant conjugated stretching modes in the region 1600 to 1400 cm−1. These modes exhibited a low frequency shift as the resonant conjugated chain-length increased. For a constant number of polymethine linkages these modes are a function of the type of unsaturation present which is in conjugation with the resonant conjugated chain.
Characteristics of Ion-Sensitive Emulsions for Mass Spectrography. I
Authors: McCrea J. M.
Published: November 2005

As part of a research program in spark-source solids mass spectrometry, the photon and ion response characteristics of various types of detector plates have been determined. Outgassing behavior of the plates in high-vacuum service has also been evaluated by empirical tests in a mass-spectrometer system. Conventional ion-sensitive plates are compared and contrasted on the basis of log-probability response curves. Various development procedures are classified by the nature of the response curves and by the extent of processing fog. Coating analyses and microstructure are related to the response properties of some emulsions. Development of an emulsion with much higher ion sensitivities than the present SWR and Q plates is forecast.
Determination of Alloy Composition in the GaAs—InAs System by Reflectivity
Authors: Jones Charlie E.
Published: November 2005

The composition of GaAs—InAs alloys can be determined by measuring the position of the E1 reflection maximum in the visible spectrum range. The composition is directly related to the energy value associated with the reflection peak. The reflection technique is rapid and nondestructive. The precision and accuracy of the method is good.
Characteristics of a Controlled Atmosphere ac Arc
Authors: Boettner E. A. , Grunder F. I.
Published: November 2005

A study was carried out to determine the characteristics of the ac arc when using various controlled atmospheres. This research was instigated because our laboratory makes extensive use of the ac arc for the analysis of air particulate matter and of body tissues and fluids. Although controlled atmosphere sources have been widely investigated, they have generally been with the dc arc. The atmospheres were evaluated by measuring the background, precision, and sensitivity of various elements using 3 matrices (graphite, lithium carbonate—graphite, and lithium fluoride—graphite). The conclusions reached were (1) the limit of detection for 21 elements was determined for each matrix. In each case, 7 elements were more sensitive by a factor of two or better in the oxygen—argon mixture than in air. The other elements showed no improvement: (2) the standard deviations obtained on 30 or more repeat analyses on each of 6 elements showed the precision of analysis of the 2 lithium—graphite matrices to be better by as much as a factor of three than the graphite matrix in both air and the oxygen—argon mixture. (3) Only the lithium carbonate—graphite matrix showed any improvement in precision when using the oxygen—argon mixture, but the results were not appreciably better than those of the lithium fluoride—graphite mixture in air.
Digital Computer Calculation and Correction of Matrix Effects in X-Ray Spectroscopy
Authors: Mitchell Betty J. , Hopper F. Noel
Published: November 2005

A multiple regression technique has been employed to calculate equations correlating x-ray fluorescent intensities with composition for complex sample matrices. The technique has been applied to a variety of materials containing major and minor components with a wide range of atomic numbers. Equations for the concentration of elements as functions of the fluorescent intensities of the sample constituents are developed to calculate concentrations without the need for calibration curves. The equations themselves are programmed for computer calculation, permitting complete computer determination of sample composition from measured intensities. In order to predict matrix effects, equations are also developed for the fluorescent intensities of elements as a function of the sample composition.
Polarization of the Energy Beam in Perkin-Elmer Infrared Grating Spectrophotometers
Authors: George Raymond S.
Published: November 2005

An account is given of the polarization occurring within the Perkin-Elmer models 421 and 521 infrared grating spectrophotometers. It is shown that the use of gratings in these instruments results in considerable polarization of the energy beam. The efficiency curves and the degree of polarization curves for the two components of polarization are given as a function of frequency. The polarization properties of the microsampling unit and the attenuated total reflectance accessory are also investigated.
Infrared Spectra of Phenoxarsine Derivatives
Authors: Nyquist R. A. , Sloane H. J. , Dunbar J. E. , Strycker S. J.
Published: November 2005

Certain well-known infrared frequencies were studied in new derivatives of 10-substituted phenoxarsine, and the effect of arsenic on vC=O, vSO2(sym), vP=O, and vP=S are explained in terms of simple electronic theory. No explanation is given for vC=S in the xanthate derivatives.
Suppression of Selective Volatilization in a Method for the Spectrographic Analysis of Lanthanum
Authors: Whitehead A. B. , Piper B. C. , Heady H. H.
Published: November 2005

The effects of electrode type, arc current, and the Stallwood Jet on selective distillation of impurities other than rare earths in La2O3 are evaluated. Selective volatilization is reduced by use of a 20-A dc arc with a ⅛-in.-diam electrode. An analytical method incorporating these operating conditions is presented for 19 impurity elements in La2O3 prepared from the lanthanum metal sample. The overall precision is about ±14% relative standard deviation over the concentration range of 30 to 1000 parts per million.
Analysis of Beryllium Metal and its Compounds by Optical Emission Spectrography
Authors: Carpenter L. , Lewis R. W. , Hazen K. A.
Published: November 2005

Eighteen elements are determined in beryllium from 5 to 1000 ppm by a dc-arc method. Samples are dissolved in hydrochloric acid, converted thermally to beryllium oxide, then mixed with graphite and barium carbonate for determining calcium, mixed with cupric oxide for determining boron and molybdenum, and mixed with graphite and germanium oxide for determining the other 15 elements. Spectral transmittances of analytical and internal standard lines are converted to relative-intensity ratios which are plotted against concentrations of standards to form curves from which concentrations of impurities are read.
Determination of Optimum Operating Conditions in Atomic Absorption Spectroscopy
Authors: Cellier K. M. , Stace H. C. T.
Published: November 2005

A statistical technique for the simultaneous study of response to several variables has been used in the estimation of “optimum„ operating conditions for the element Calcium in atomic absorption spectroscopy. The method is based on “response surface„ exploration, originally due to G.E.P. Box. This technique has several advantages over the traditional method of varying “one factor at a time.„ Direct estimates of the magnitude of the effects of changes in each instrumental variable are obtained, together with estimates of the interactions between two or more variables. The method leads to the efficient estimation of “optimum„ operating conditions, i.e., those levels of the instrumental variables at which percent transmission is a minimum and also the estimation of alternative levels of the several variables at which transmission can be maintained at a minimum. The results showed that, for the estimation of Ca, the four variables air pressure, air flow, gas flow, and “height above the blue cone„ are compensating in the sense that departure from minimum transmission due to change in one variable can be compensated by a suitable change in the other variables. In the absence of a theoretical solution to the problem of estimating “optimum„ operating conditions, it would seem that this method is the best available at the present time.
Some Spectroscopic Measurements of a Supersonic Plasmajet
Authors: Shipley K. L.
Published: November 2005

Typical results of spectroscopic data from argon and nitrogen supersonic plasmajets are presented. The purpose of this study was to determine which of these spectroscopic data give suitable information for temperature determination. Spectral-line-intensity and hydrogen-line broadening techniques were used. For the argon jet, the results from line-intensity measurements of ionized and un-ionized atoms generally give reliable information; results from hydrogen-line broadening measurements indicate temperatures from 6% to 20% less than intensity measurements. Spectrographic data are compared with enthalpy measurements. For the nitrogen plasmajet, the N2+ (0,0) band was used to determine a rotational temperature.
Evaluation of Solid Metal Specimens Produced for Spectrographic Analysis by the Inert-Gas dc-Arc Fusion of Wire and Chips
Authors: Prince L. A. , Ellgren A. J. , DeGlopper T. J.
Published: November 2005

A study has been made of the chemical composition of solid-metal buttons of low-alloy steel, stainless steel, high-temperature alloys, and copper-base and aluminum-base alloys produced by the dc-arc fusion of wire and chips under argon shielding. The effect of fusion on 22 elements commonly encountered in these alloys has been determined quantitatively. A correlation has been shown between boiling points and element losses. With the exception of zirconium, no significant changes in the composition of metallic elements having boiling points greater than manganese (2150° C) were noted while using the recommended procedures for button preparation. Steels showed consistent, slight losses of manganese and occasional loss of zirconium. Losses of lead in copper-base alloys and of magnesium, lead and manganese in aluminum-base alloys, which occur with high currents, may be eliminated by first briquetting the chips, then fusing at relatively low amperage. Consistent and significant losses of zinc were noted. Carbon pickup from the graphite electrode is slight, but inconsequential. Copper pickup from the water-cooled copper cup is usually negligible.
Spectrometric Investigation of Complexes of Copper(II) and anti-2-Aminobenzophenone Oximes, and Characterization of the syn and anti Forms
Authors: Pritchard J. G. , Field G. F. , Koch K. , Raymond G. , Sternbach L. H. , Toome V. , Traiman S.
Published: November 2005

Nine bivalent cations were examined spectrophotometrically for a color reaction with anti-2-amino-5-chlorobenzophenone oxime, using aqueous ethanol as solvent. Only Cu++ gave a positive color change owing to the formation of complexes. The syn isomer gave a negative result with all of the cations. This test also distinguished the two isomeric forms of eight additional pairs of analogous oximes. In the case of the anti-2-amino-5-chloro-derivative, the nature of the copper complexes in solution was explored; a crystalline complex, formulated as [(C13H11CIN2O)2Cu.H2O]2++2SO4−, was isolated. The proton-resonance signals given by the hydroxyl and amino groups for the whole set of oximes provide evidence for a significant structural difference between the two isomeric forms. The infrared spectra show lower symmetric NH stretching frequencies for the anti forms than for the syn forms. These differences are attributed to the presence of an intramolecular N-H…N=C hydrogen bond in the anti forms and to its absence in the case of the syn forms. The ultraviolet spectra of the anti forms show an increased intensity of absorption and a maximum at lower wavelength in the 220–250 mμ, range when compared to the syn forms. The situation is similar with regard to intensity, but there is a shift to a higher wavelength, for the broad absorption maximum in the 300–350 mμ range. It is concluded that these latter two regularities stem mostly from the differences in molecular geometry of the anti and syn isomers, with only a small contribution resulting specifically from the difference in hydrogen bonding.
Controlled-Atmosphere dc Arc for the Quantitative Determination of Rare Earths in Calcium Fluoride
Authors: Nash D. L.
Published: November 2005

This paper discusses the investigation of optimum controlled-atmosphere conditions for the analysis of rare earths in calcium fluoride and describes the specific technique evolved for the determination of terbium and holmium. The limits of detection and precision of the method are given.
Atomic-Absorption Characteristics of Rhenium
Authors: Schrenk W. G. , Lehman D. A. , Neufeld Lorin
Published: November 2005

Rhenium can be determined by atomic absorption in a fuel-rich acetylene-oxygen flame, using either de or ac electronics. Use of an organic solvent increases the sensitivity. Proper burner placement in the optical path is critical. Using three burners in a single-pass optical system, with optimum conditions, 1–2 ppm rhenium is readily detectable.
Automatic Filter Method in Spectrophotometry
Authors: Thekaekara Matthew P. , MacKenzie Donald
Published: November 2005

A filter method of radiometry has been developed which gives a relatively high degree of accuracy and spectral resolution, A set of 34 interference filters covering the range 2800 A-27 000 Å is used. All stages of data reduction are handled automatically by a computer and the final results are presented as a spectral radiance curve. The relative advantages of the automatic filter method and its range of applicability are discussed.