bluuebunny/crossref_metadata_2025 huggingface dataset:
Optical Spectrographic Determination of Aluminum in a Titanium Alloy
Authors: Runge E. F. , Bryan F. R.
Published: November 2005

Although titanium alloy technology in general is advancing rapidly, the control analysis of these alloys has not reached the degree of speed and perfection possible with corresponding alloys of aluminum, magnesium, and steel. Thus far, nearly all reliable methods for titanium have necessitated reducing the samples to chips and dissolving the metal prior to either chemical or spectrochemical analysis These procedures are time consuming and costly. Most attempts to analyze titanium alloys by direct metal excitation have resulted in abnormally high errors frequently attributed to metal segregation. Results of experiments in this laboratory, however, indicate that acceptable precision can be obtained on a typical commercial alloy by direct excitation if certain precautionary techniques are employed. These techniques involve (I) selection of homologous line pairs, (2) choice of a reference line close to the element line in wavelength, (3) provision for flushing the analytical gap with an inert atmosphere during excitation, and (4) use of an adequate pre-exposure period to provide an equilibrium condition during exposure. The procedural considerations described, when applied to a direct spectrographic method, can reduce errors by an order of magnitude in the case of aluminum determinations in titanium alloy. The precision obtainable provides a coefficient of variation of 0.9%.
The Plate Characteristic: A Theory of the Linear Transform
Authors: Candler C.
Published: November 2005

Two variants of the Baker transform,

[Formula: see text]

introduced by Kaiser and Arrak, apply to a deep emulsion, not to a coating, since their curvature is positive at high densities.

In a deep emulsion, only two physical processes afreet the shape of the characteristics, absorption and polyphotonic fertilization. Since the (1-T) of the Kaiser transform is a measure of the number of silver grains formed, it should be replaced by the density. Thus the exposure equation demanded by theory is

[Formula: see text]

where P is the photon number, and K the ratio of the absorption cross sections of a crystal before and after development ‘A’ does not affect the shape of the characteristic, but only the speed.

This equation for a deep emulsion is generalized to cover a coating, and shown to fit two characteristics recorded in the Kodak laboratories. Further it is found to be valid in all the emulsions used in spectrochemical analysis down to 214 mμ, and in some sensitized plates up to 809 mμ. It is not valid in a few fast emulsions, and three of these are named
A Comparison of Precision for Solid, Liquid and Powder Sampling Techniques in the X-Ray Fluorescence Analysis of High Temperature Alloys
Authors: Friedlander Stanley , Goldblatt Alan
Published: November 2005

Data obtained in the routine use of a multi-channel x-ray spectrometer are presented to demonstrate precision on stainless steel, nickel and cobalt base alloys as solids, liquids and briquetted powders Coefficients of variation of 0.5% and less for the major constituents in high temperature alloys are readily attainable. The combination of liquid and powder techniques is particularly significant in that it provides an independent method for standardizing complex alloys by use of synthetic standards.
A “Vacuum Cup” Electrode for the Spectrochemical Analysis of Solutions
Authors: Zink Theodore H.
Published: November 2005

A new method is proposed for handling solution samples in spectro-chemical analysis. Speed, good sensitivity, short exposure times, and great ease of handling characterize the method. The rate of transfer of the solution into the analytical gap can be varied from less than 1 ml/100 sec to 1 ml/40 sec, and the total volume of sample carried in the electrode cup may range from 0.2 to 4 ml. The sample is presented to the excitation gap in the form of a very fine spray. The electrodes can be easily fabricated from pure copper, silver, graphite, or other materials.
Micro-Analysis of Metals by Optical Emission Spectroscopy
Authors: Runge E. F. , Bryan F. R.
Published: November 2005

The status of metallurgical micro-sampling and analysis is reviewed. Spectroscopic detectabilities for several metallic elements are found to be of the order of I × 10−9 gram when employing a quartz Littrow spectrograph together with arc excitation and Eastman 103-O emulsion. Techniques are described for the removal and identification of milli-microgram quantities of metallic constituents by means of drills as small as 6 3 microns diameter.
A Method for the Spectrographic Determination of Trace Impurities in Niobium
Authors: Fornwalt D. E. , Healy M. K.
Published: November 2005

Niobium is a member of a group of metals under investigation to evaluate their suitability for use in the nuclear reactor field Because of the complex chemistry involved in the determination of trace impurities in niobium by classical methods, spectrographic methods have been devised. This paper describes a method for the spectrographic determination of 14 elements present in niobium. The elements determined and their concentration ranges include boron, 0 0001 to 0 0015%, aluminum, cadmium, chromium, cobalt, iron, manganese, molybdenum, nickel, silicon, tin and titanium, 0.001 to 0.1%; tantalum, 0.025 to 1.5 percent; and zirconium, 0.001 to 1.5%.

The analysis involves the conversion of niobium to the oxide by heating the metal in platinum at 800°C until oxidation is complete. A 10 mg sample plus 10 mg of lithium carbonate, as a spectrographic buffer, and 25 μg of lanthanum, as an internal standard, is excited in a 20-ampere d.c. arc. The spectrogram obtained is used for the determination of all the elements listed with the exception of aluminum, boron, silicon, zirconium and tantalum'. The latter are determined from a spectrogram obtained by the excitation of a separate 20 mg sample of niobium oxide. The coefficient of variation is of the order of 10 percent for the various impurities.
Determination of Major Constituents in Alloy Steels by Spectrographic Solution Methods
Authors: Waggoner C. A.
Published: November 2005

A spectrographic solution technique utilizing either the porous cup or rotating disk electrode may be used to analyse high-alloy steels such as the corrosion and heat-resisting alloys, including the iron-chromium, iron-chromium-nickel, and iron-nickel-chromium groups Some types of low-alloy steel may also be analysed from the same analytical curves Cobalt is added as an internal standard, and iron, chromium, nickel, manganese, and molybdenum are determined with an accuracy in the order of ±2 to 3% of the amounts present. Interelement effects arising from wide variations in composition were indicated to be negligible. The procedure outlined is designed primarily for alloy identification or specification analysis, and is particularly useful where sample dimensions are not uniform
X-Ray Diffraction Patterns of p-Nitrobenzyl Derivatives of Barbituric Acids
Authors: Cloutier J. A. R. , Manson Jane M.
Published: November 2005

The x-ray powder diffraction patterns of p-nitrobenzyl derivatives of 20 clinically important barbituric acids have been obtained Data which can be used for identification purposes are presented
Determination of Zirconium in Plutonium by Ion Exchange and Spectrography
Authors: Ko Roy
Published: November 2005

The spectrographic analysis of plutonium for impurity elements is not without difficulties due to the complex emission spectrum of plutonium and to its toxicity. Separating the plutonium from the elements of interest would reduce the spectral interference and also the health hazard In the determination of zirconium in plutonium reported here, the plutonium was separated from zirconium by retaining the plutonium as a nitrate complex on the anion exchange resin, Dowex-1, while collecting the zirconium in the effluent and wash solution. The combined effluent and wash solutions were evaporated to a small volume and the resulting solution analyzed for zirconium by graphite spark, excitation using cobalt as the internal standard. Concentrations as low as 20 ppm of zirconium in plutonium have been determined with a precision of ± 17% (95% c.l.) for a single measurement.
The Spectrochemical Analysis of Solutions. A Comparison of Five Techniques
Authors: Baer William K. , Hodge Edwin S.
Published: November 2005

The spectrochemical analysis of solutions offers such a variety of advantages that a number of techniques have been developed and reported in the literature. There has been little or no intercomparison of the procedures or excitations, so it has been difficult to select one technique in preference to another. This paper describes studies of five different solution techniques and three excitation conditions A number of observations are reported regarding general conditions to give the best sensitivity and reproducibility. The effects of hydrochloric, nitric, sulfuric, and phosphoric acid on the spectra were also studied. The repression effects which were noted for some acids varied with the technique, acid concentration, and excitation potential of the line
The Photoelectric Theory of Photosynthesis. V. Further Correlation of the Absorption Spectrum of Chlorophyll with the Emission Spectrum of Magnesium
Authors: Levitt Leonard S.
Published: November 2005

The near infrared absorption spectrum of chlorophyll has been reexamined in an attempt to detect a possible weak absorption at around 881 mμ, corresponding to the only important emission line of Mg atoms above 655 mμ, and which is due to the transition 3p → 3d for Mg. Chlorophyll is found to exhibit such a band in the region 860–885 mμ. This is interpreted as further evidence for the author's photoelectric theory of photosynthesis, in which it is postulated that it is the Mg atom of chlorophyll which is electronically excited by light absorption. Seven new bands are predicted for chlorophyll in the far ultraviolet region of the spectrum, ranging from 273 to 123 mμ, and the ionization potential of chlorophyll is calculated to be 189 v.
X-Ray Diffraction Powder Data for Some 2,4,6-Substituted-1,3,5-Triazine Compounds
Authors: Baun William L.
Published: November 2005

X-ray powdei diffraction data are presented for fifteen polycrystalline 2,4,6-substituted-1,3,5-triazine compounds Methods of minimizing preferred orientation in pure compounds, and analysis of mixture and impure compounds are discussed The data presented permit rapid identification regardless of the complexity of the substitution
A Versatile 19 Cm. Diameter Low Temperature Debye-Scherrer Camera
Authors: Taylor A.
Published: November 2005

The camera described is designed for use with typical cylindrical powder specimens and also for bulky specimens frequently encountered in metallurgical research. Partly on account of its large radius, it is capable of yielding high spectral resolution and lattice parameters to an accuracy of approximately 0 002% in favorable cases. In its present form, the camera may be used with the specimen lying in the temperature range −190°C to 200°C.
A General Chemical-Spectrographic Method for the Determination of Boron in Iron and Nickel-Base Alloys
Authors: Anderson R. F.
Published: November 2005

A technique is presented that allows for the determination of boron in a great number of iron and nickel base alloys with the use of only one set of standards. Along with this advantage, another feature of the method is that the sensitivity can be increased in an alloy where an extremely low boron concentration is known to exist. The base metals of an alloy are removed by the use of the mercury cathode. To each of these stripped samples, copper is added to make up its new matrix. These samples are then compared to boron standards which have the same matrix. The technique greatly facilitates the speed at which boron can be determined in alloys that have varying matrices
Influence of Goniometric Arrangement and Absorption in Qualitative and Quantitative Analysis of Powders by X-Ray Diffractometry
Authors: Leroux J. , Mahmud M.
Published: November 2005

A theoretical approach to some factors influencing the intensity diffracted by a polycrystalline material at a definite Bragg angle has been confirmed by experimental data obtained with a High-Angle Norelco Diffractometer. The factors considered are mainly the focussing arrangement of the goniometer, which delineates the geometric shape of the volume fraction of the sample being irradiated, and the absorption of the latter.

A general equation and experimental conditions, suitable for qualitative and quantitative analysis when these factors have to be taken into consideration, are proposed and a new type of sample holder for obtaining more accuracy in the measurement of lattice spacings is discussed.
Infrared Analysis of Phenylchlorosilanes in the CsBr Region
Authors: Grenoble Maurice E. , Launer Philip J.
Published: November 2005

The infrared spectra of seven phenylchlorosilanes have been meassured from 2 to 30 microns The spectra of certain phenylchlorosilanes are very similar in the 2–15 micron wavelength region but show marked differences in the 15–30 micron range, where there are Si-Cl stretching and aromatic-ring deformation vibrations. Based on these differences, methods for the quantitative analysis of mixtures of phenylchlorosilanes have been developed using a double-beam, double-pass spectrometer equipped with a CsBr prism and a new, low-cost KBr spectrometer With double-beam compensation, low concentrations of phenyltrichlorosilane in diphenyldichlorosilane can be determined Techniques for the quantitative analysis of mixtures of phenyltrichlorosilane, diphenyldichlorosilane, and chlorobenzene are described. Because atmospheric water vapor absorbs strongly in the CsBr region, flushing the spectrometer with dry air or nitrogen improves the accuracy of absorbance measurements.
Spectroscopic Analysis of Polyvinyl Chloride Compounds
Authors: Bennett W. J. , Law E. M.
Published: November 2005

An emission spectrographic method for the determination of stabilizers and fillers in polyvinyl chloride compounds is described. In conjunction with infrared methods, the plasticizer is ether extracted and the resin dissolved in tetrachloroethane. The stabilizer and filler are removed from the dissolved resin by centrifuging The resultant powder is mixed with cupric oxide and graphite powder. The mixture is pelletized on the end of a graphite electrode. A Multisource discharge is used to determine lead, aluminum, silicon, calcium and antimony as percent oxides The concentration of stabilizers and fillers may then be calculated The emission spectrographic analysis can be performed in duplicate on 8 mg of stabilizer and filler from the compound.
Ten Years of Aid to Applied Absorption Spectroscopy by A.S.T.M. Committee E-13
Authors: Robey R. F.
Published: November 2005

To mark the tenth anniversary of the founding of the committee, the scope of activity, organization, accomplishments, current programs, and unsolved problems are reviewed Outstanding accomplishments of sub-committees include publication of (a) recommended nomenclature, (b) methods for objectively evaluating the performance of spectrophotometers, (c) general techniques of infrared and ultraviolet quantitative analysis, (d) a recommended form of ASTM methods involving absorption spectroscopy, and (e) an ever-expanding index of absorption spectral data now comprising almost 100,000 cards designed for machine sorting, encompassing the ultraviolet, visible, near-infrared, and infrared ranges. The nature, uses, and advantages of the index are described briefly

In recent months, new subcommittees were established to serve the fields of molecular fluorescence and nuclear magnetic resonance spectroscopy These subcommittees are active in sponsoring symposia. The unsolved problems of committee activity in the newer and older fields of spectroscopy are summarized.
Spectrochemical Rubidium-Strontium Method for Geological Age Determination
Authors: Eichhoff Hans-J.
Published: November 2005

The age values of lepidolites from South Africa and from Varutrask as well as that of a microcline from Varutrask have been determined and are discussed in connection with determination according to the potassium-argon method, applied to the same materials

A method is suggested which allows the spectrochemical determination of Rb and Sr with sufficient accuracy. The isotopic composition is determined by means of a Fabry-Perot etalon and hollow-cathode excitation, investigating the hyper-fine structure of the Sr line at 4078 A.
The Use of Scatter Diagrams in Emission Spectroscopy
Authors: Holdt G. , Strasheim A.
Published: November 2005

The necessity to employ two-dimensional statistical methods in emission spectroscopy and the dependence of variance of ΔY, i.e. of the logarithm of the intensity ratio of an analysis-internal standard line pair, on correlation and regression are pointed out. To investigate the statistical behaviour of intensity ratios or the correlation of other quantities the scatter diagram method and its improvement by the contour ellipse are described. Examples of various applications are given and the calculation of the “Complete Statistical Analysis” is described. Finally the completion of the scatter diagram method by statistical test methods is illustrated by examples.
The Effect of Absorbance on Raman Intensities in Solids
Authors: Vratny F. , Fischer R. B.
Published: November 2005

Raman, spectra have been observed for several simple systems as powders in the solid state. The (measured) intensities of the Raman bands appear to be functions which are dependent upon the concentration and the particle size of the Raman scattering material. A significant effect on the Raman intensity was noted as a result of the “effective absorptivity” of the material, defined as the combined effect of absorbance and the scattering of the material Sample thickness and materials of high, low and intermediate effective absorptivity are considered to demonstrate their effects on the Raman intensities.
Determination of Trace Elements in Lignite Ashes
Authors: O'Neil Robert L. , Suhr Norman H.
Published: November 2005

Two spectrographic methods for the quantitative determination of trace elements in lignite ashes and shales are described. The involatile elements are determined in a controlled atmospher of carbon dioxide gas that suppresses cyanogen bands, improves line to background ratio, and provides a more precise technique for the simultaneous determination of a large number of elements. Lutecium oxide in calcium carbonate and fused potassium sulfate (1 + 1) is used as the internal standard The volatile elements are determined in an ordinary d.c. arc, using a pellet technique to increase the limit of detection and rate of volatilization. Antimony and cadmium potassium sulfate are used as internal standards. Analyses of U. S. Geological Survey standard rock samples G1 and W1 show that the method can be extended to other silicate rocks. An additional application of the controlled carbon dioxide atmosphere is the determination of boron and gallium.
Determination of Traces of Certain Rare Earths in Uranium Compounds by Ion Exchange and Spectrography
Authors: Carter Joel A. , Dean John A.
Published: November 2005

An ion exchange separation followed by a spectrographic determination has been developed for certain of the rare earths present in uranium compounds. This method permits the determination of dysprosium, erbium, europium, gadolinium, neodymium, samarium, and ytterbium at concentrations as low as 0.01 to 1 ppm. Hydrofluoric acid solutions of uranium containing the rare earth elements, with yttrium as an internal standard, were passed through a cation exchanger. The negatively charged uranium fluoride complex passed through the column while the rare earths were retained. After the residual uranium was completely removed by eluting with 2.5 M hydrofluoric acid, the resin bed was ignited, and the resulting ash analyzed spectrographically for the individual rare earth elements. Other cations which separate with the rare earths were easily separated, when necessary, by standard, wet chemical, group separations The standard deviation for the method was about 10%.
Some Results of Resonance Raman Spectroscopy
Authors: Maier Werner , Dörr Friedrich
Published: November 2005

The intensity of scattered Raman radiation increases greatly as the exciting frequency approaches an absorption band of the molecule. This phenomenon, termed “Resonance Raman Effect”, permits new spectroscopic applications. For instance, a red cyanine dye absorbing strongly at 542 mμ was successfully investigated, using the 5461 line of Hg for irradiation, at dye concentrations as low as 10−6 mole/liter. Shifts in absorption due to solvent or substituent effects show great influence upon line intensities, as demonstrated with p-nitroso-dimethylaniline. There is no evidence of n → π* bands also causing the effect. According to theoretical aspects by Behringer, selection rules based on the Franck-Condon principle are valid. This makes for relatively simple resonance Raman spectra.
A Limit on the Accuracy of Photographic Radiometry
Authors: Eyer James A.
Published: November 2005

The granular nature of the photographic emulsion places a limit on the accuracy with which the density of a small area on the film can be defined. This in turn limits the accuracy with which incident exposures can be calculated when, for example, a spectrograph is employed for radiometric measurements. The quantity of information conveyed by a single density measurement is estimated for a particular emulsion and microdensitometer scanning aperture.
The Application of Statistical Methods to a Problem in Spectrochemical Analysis
Authors: Keeler Barbara T.
Published: November 2005

An R chart, analysis of means charts, and the range square ratio test, are applied to spectrographic data to compare two internal standards and two different buffer salts in the analysis of solutions of organic ash. The range square ratio test confirms the indications derived from the graphical methods that cobalt is a better standard for manganese, molybdenum is better for lead, and that sodium silicate is superior to lithium chloride as a buffer salt.
Infrared and Ultraviolet Absorption Spectra of Alpha-Azido Ethers and Amines
Authors: Lieber Eugene , Thomas Alexander E.
Published: November 2005

The ultraviolet absorption spectra of a series of alpha- azido ethers, alpha- azido thioethers, and alpha- azido amines exhibited extinction coefficient maxima in the region 264–300 mμ A shift to the lower wavelength was found to occur in the order S>O>N when these atoms are substituted alpha to an azido- group.

Infrared absorption spectra were recorded in the 2 to IS micron region, and assignments made for the asymmetric and symmetric N3 stretching vibrations. The N3 asymmetric vibration occurred in the range 2141–2090 cm−1 for the azides examined. The N3 symmetric vibration was more variable. Tentative assignments were made lor this absorption occurring for alpha- azido ethers and alpha- azido thioethers. However, no assignment was made for this vibration for the alpha-azido amines due to the complicated spectra in this region. The N3 asymmetric vibration for azidomethyl methyl ether, azidomethyl methyl sulfide and N-azidomethyl phthalimide exhibited a doublet while other azides exhibited a single absorption for this mode.
X-Ray Spectrographic Determination of Thorium in Low Concentrations
Authors: van Niekerk J. N. , Strelow F. W. E. , Wybenga F. T.
Published: November 2005

A method is described for the rapid determination of small concentrations of thorium The thorium is first concentrated on a suitable cation exchange resin and then measured directly on an x-ray spectrograph With the experimental conditions employed it is shown that the extraction of thorium is practically quantitative Both column and batch extraction methods were investigated, and it is shown that the latter technique is superior both as regards reproducibility and time of analysis. It is further shown how interference effects due to co-adsorbed elements, such as iron, can be overcome by the use of a suitable internal standard. From calibration curves so obtained the thorium concentration in three unknown samples was determined, and the results are compared with those obtained by chemical analysis.
A Technique for Obtaining the Ultraviolet Absorption Spectrum of Solid Keratin
Authors: Bendit E. G. , Ross D.
Published: November 2005

A technique is described for obtaining spectra of solid keratin in the form of thin sections of horse tail hair. The method of sectioning, mounting the specimen, and positioning it in the beam of the spectrophotometer is given. The application of a correction procedure for scattering, which his previously been described by other authors, and a corrected ultraviolet absorption spectrum of keratin are included in the report
The Spectrographic Determination of Uranium 235. Part IV. Using a Direct Reading, Littrow, Grating Spectrograph and a Hollow Cathode
Authors: Lee Ted , Killeen Owen P. , MacIntyre S. A.
Published: November 2005

This report, the fourth of a related series dealing with the isotopic analysis of uranium, describes the use of a hollow cathode source and a 4-m, direct-reading, Bausch and Lomb high-resolution spectrograph. A relative precision of ±3.0%, expressed at the 95% confidence level, was obtained with naturally occurring uranium for a single cathode determination of U235 measured in twenty min. Evidence for a weak uranium line structure interfering with the U235 measurement is presented

Minor isotopes, U231 and U236, present up to a few percent at the higher U235 concentrations, did not interfere with U235 measurements. Measurements of U234, however, could not be made in the presence of high U235 concentrations, thereby limiting the determination of total uranium necessary for calculating the percent U235. At the lower U235 concentrations, the concentrations of minor isotopes are generally too small to significantly affect the total uranium content of the sample.
Use of Low Molecular Weight Polyethylene in Ultraviolet Spectroscopy
Authors: McDonald F. R. , Cook G. L.
Published: November 2005

The ultraviolet spectra of high-molecular-weight materials were obtained by dispersing them in polyethylene, which had a negligible contribution to the spectrum between 2200 and 4000 A. The spectra of reference compounds as well as asphaltenes and polymers are given. The sample is stirred into melted polyethylene, and a portion of the dispersion is pressed between sheets of metal foil in a heated laboratory press to form a film. A circular plate cut from the film and mounted between two metal rings is inserted into the spectrophotometer to obtain a spectrum.
The Analysis of Unirradiated “Fissium” Alloy by Optical Emission Spectroscopy
Authors: Goleb Joseph A.
Published: November 2005

An optical emission spectrographic method has been developed for the quantitative determination of molybdenum, ruthenium, rhodium, palladium, and zirconium in normal uranium metal in the range of 2.5%, 2.0%, 0.30%, 0.20%, and 2.5%, respectively. The precision of the spectrographic method for molybdenum is ±1.0%, ruthenium ±18%, rhodium ±17%, palladium ±21%, and zirconium ± 2.2% of the amounts present The comparison of spectrographic and chemical results on 24 “fissium” alloy samples for molybdenum, ruthenium, rhodium, palladium, and zirconium shows a standard relative deviation from the chemical results of ±3.9%, ±4.3%, ±7.2%, ±6.6% and ±7.5%, respectively. These samples were chosen at random from ingots by using routine sampling procedures
Identification of Barbiturates by X-ray Diffraction Powder Patterns of Their p-Nitrobenzyl Derivatives
Authors: Cloutier J. A. R. , Manson Jane M.
Published: November 2005

The identification of barbituric acids by the x-ray powder diffraction method is discussed from the practical point of view. Data are presented showing the advantage of preparing the p-nitrobenzyl derivative whenever identification of the isolated free acid is either doubtful or considered impossible. A detailed account of the experimental micro technique is given and the applicability of the technique to pharmaceutical products as forensic specimens is discussed.
The Spectrochemical Analysis of Magnesium and its Alloys for Beryllium, Lead, and other Trace Elements by Solution and Salt-Cap Techniques
Authors: Mansell R. E.
Published: November 2005

Spectrographic solution and salt-cap techniques are described for the determination of beryllium, lead, and other trace elements in magnesium alloys in the range 0.0001–0 3%. Beryllium is determined with a precision within ±4% between 0 0001 and 0 01% with a high voltage spark source and a rotating disk electrode method. Comparative sensitivity and precision results are given for Al, Ca, Cu, Fe, Mn, Pb, Ni, Sn, and Zn with a high voltage spark condition using the rotating disk electrode and an ac arc salt-cap technique. Considerable improvement in sensitivity for Al, Ca, and Pb is demonstrated with use of an argon atmosphere in the ac arc work.
Light Source, Excitation, and High Temperature Cell Assembly for Raman Spectroscopy
Authors: Janz George J. , Mikawa Yukio , James David W.
Published: November 2005

A Toronto-style light source and the excitation circuit designed for use with a Hilger E612 recording Raman spectrometer in this laboratory are described. The electrical circuits and accessories are designed for automatic or manual start and with safety devices for protection in event of various component failures. For measurements on specimens at elevated temperatures, a simple cell assembly capable of use at temperatures up to 575 °C with a gradient of not more than ±5°C at the maximum temperature limit is described.
The Spectrographic Determination of Uranium 235. Part III. Use of a Multiple Hollow Cathode Source Assembly and a 22 Foot Direct Reading Eagle Spectrograph
Authors: Lee Ted , Maclntyre S. A.
Published: November 2005

This report, the third of a series dealing with the isotopic analysis of uranium, describes the work done with a 22-ft Eagle mounted, direct-reading spectrograph using 5 in. of a 15,000 lines/in. concave grating in the second order. The samples were excited in a multiple source assembly consisting of 4 hollow cathode source lamps and an automatically positioned selector mirror. This arrangement allowed close comparison of unknown and standard, minimized the effect of exit slit misalignment, and allowed large number of routine samples to be handled economically A complete analysis in duplicate, including comparison standards, was made in less than 20 min.

Measurements on 4 standards having U235 concentrations between 10 and 51% showed average external and internal precisions of ±0.23% and ±0.048% U235 for a single cathode determination Analyses of 32 unknown samples containing 10–85% U235 determined independently on the optical spectrograph and the mass spectrometer, showed good agreement Comparative measurements on 65 unknown samples in the range of 30–40% U235 showed an agreement of ±0.17% U235 with no significant bias All precisions were expressed at the 95% confidence level The factor limiting the precision—a weak line interfering with the U235 measurement, and the effect of U234 and U236 on the analysis are discussed.
X-ray Powder Diffraction Data for 2,4-Dinitrophenylhydrazones of Aldehydes and Ketones
Authors: Calvert L. D. , Przybylska Maria
Published: November 2005

In order to extend the data available for the identification of carbonyl compounds, the x-ray powder diffraction patterns of sixty-four 2,4-dinitrophenylhydrazones of aldehydes and ketones were determined. An alphabetical table includes 39 additional compounds found in the literature. A second numerical table indexes the spacing and intensities of the three strongest lines in Hanawalt groups. The complete new diffraction pattern data are available from the American Documentation Institute.
Comparison of Ignited Arc Sources
Authors: Schreiber T. P. , Joseph B. W.
Published: November 2005

A Bardócz BIG 210 ignited arc source was compared with a conventional ignited unidirectional arc and a Multisource for the analysis of lead alloys and the determination of boron in steel. The sources performed similarly except for the lead alloy analysis where the Bardócz source proved superior in repeatability and line-to-background ratio
A Spark Spectrographic Procedure for the Determination of Boron in Sheet Steel
Authors: Runge E. F. , Bryan F. R.
Published: November 2005

Sheet metal is directly analyzed for boron by means of spark excitation. Source inductance of 200 to 300 μh, together with rotation of the specimen during excitation, provides detectability an order of magnitude better than conventional spark excitation of steel. Sheet material of 0 050 in thickness and containing a nominal 0.004% boron is analyzed with a coefficient of variation of 3.2%.
The Spectrographic Determination of Uranium 235. Part II. Using a Direct-Reading Attachment and a Hollow Cathode Source
Authors: Lee Ted , Rogers Lewis H.
Published: November 2005

This report, the second of a series associated with the development of the spectrographic determination of U235 at the Oak Ridge Gaseous Diffusion Plant, describes the development of the direct-reading scanning technique, using a Jarrell-Ash 21-foot Wadsworth spectrograph with a hollow cathode discharge tube to excite the uranium samples For a determination consisting of ten scans on a single cathode containing the unknown, and ten scans on a single cathode containing a comparison standard, the precision obtained was from ±12 to 18% of the amount present over a concentration range of 8–12% U235. All precisions are expressed at the 95% confidence level
The Spectrographic Determination of Uranium 235. V. Routine Application of a Multiple Hollow Cathode Source Assembly and a Direct-Reading, Littrow Grating Spectrograph
Authors: Lee Ted , Katz Sidney , Maclntyre S. A.
Published: November 2005

This paper, the fifth of a related series, describes the routine application of a rapid, high-precision procedure and a high resolution spectrograph to the isotopic analysis of uranium. The procedure, which evolved from the development described in previous papers of this series, includes a simple sample preparation and a hollow cathode source designed for rapid sample changing. The procedure also involves a high degree of automation and eliminates the reference measurement and background correction The precision at the level of naturally occurring uranium (0.7115% U235) measured under routine conditions, is ±2.1% of the amount present for a single cathode determination expressed at the 95% confidence interval. In the vicinity of 90% U235 the precision is 0 07% of the amount present for a single cathode determination. Approximately 7½ min is required for a determination, including sample preparation, measurement, and calculations The maximum capacity of the instrument is over 60 samples per 8 hr day, the instrument is presently applied to a routine load varying from 20 to 5 0 samples per day. In addition to the U235 determination, a preliminary calibration and evaluation for U236 is included
The Shape of Working Curves Using Photometric Line Width
Authors: Rubeska I. , Polej B.
Published: November 2005

The shape of working curves using photometric line widths is derived using simplifying assumptions. Their shape is influenced by different effects of line image broadening, and it depends upon the working conditions, which of these will prevail. For small and medium spectrographs, linear working curves given by the light diffusion in the photographic emulsion are most likely to appear. For spectrographs with greater linear dispersion it is the physical line shape or the apparatus function which make themselves evident. In these cases the working curves should be curved.
Equations for Working Curves in Emission Spectroscopy
Authors: Pitwell L. R.
Published: November 2005

From consideration of the theory of emission, the causes of interference, and the effects of segregation and self absorption, complex equations can be derived relating observable measurements of line intensity ratio to the concentration of the element being determined and the other elements present. These equations are capable of graphical solution and can be used to make working curves and predict the limits of analysis As actual working curves are of the predicted shapes, these theoretically obtained curves can be used as guides when correcting for interference effects, thus reducing the number of standards required for such analysis.
Spectrochemical Analysis of Rocks, Minerals and Related Materials
Authors: Joensuu Oiva I. , Suhr Norman H.
Published: November 2005

A spectrochemical method for the determination of major constituents in rocks, minerals, and related materials is described The samples are fused with lithium or sodium borate and burned with a Stallwood jet in carbon dioxide Cobalt is used as the internal standard Comparisons with chemically analysed samples show good accuracy and reproducibility.
Emission Spectrographic Analysis of Fused Aluminum Oxide and Fused Tin Oxide Crystals
Authors: Owens E. B.
Published: November 2005

A method is described for the analysis of fused aluminum oxide and fused tin oxide crystals in which the treatment of the samples and standards removes the effects which sample form might have on spectral excitation. The crystal sample is ground and then dissolved in a molten sodium carbonate-tetraborate flux. The cooled cake is dissolved in dilute hydrochloric acid, and an internal standard is added. A drop of the solution is dried on the flat end of a graphite electrode, and the spectra are excited with an ac arc. The elements Cr, Co, Cu, Fe, Mn, Ni. and V have been determined with the lower limits ranging from 0.001 to 0.05%. The method is applicable to many other elements over wide concentration ranges because of the convenient method of standardization.
Direct-Reading Semi-Quantitative Spectrochemical Analysis of Non-Metallics
Authors: Lemieux P. E.
Published: November 2005

A method in which samples are mixed with CuO and graphite in the proportions 1920 has been tested on a wide variety of non-metallics using an ARL Quantometer The technique yields results accurate within a factor of 1.2 for a majority of determinations ranging from traces (0 01% level) to major constituents. When applied to one class of material, bauxites of different origins having varied mineral structures, the method gives much improved accuracy without evidence of appreciable matrix effects. Advantages and limitations of direct-reading instrumentation for semi-quantitative analysis are presented
The Infrared Spectra of Metal Dialkylphosphorodithioates
Authors: Rockett Jack
Published: November 2005

The infrared spectra of eight zinc dialkylphosphorodithioates and four potassium dialkylphosphorodithioates have been examined The infrared spectra of the zinc, cadmium, copper, nickel, and potassium salts of a mixed dialkylphosphorodithioate have been studied and compared to the spectrum of the parent acid. The P-O-C absorption of all of these compounds is found to occur about 25 cm−1 lower in frequency than in compounds containing the P = 0 group. The thiophosphoryl group (P = S) is found to occur at 635–668 cm−1 both for the free acid and the covalent salts. It occurs at a higher frequency, 675–702 cm−1 for the more ionic potassium salt. The P— S—(M) absorption occurs at 510–556 cm−1.
Preparation of Graphite Electrodes for Spectrographic Analysis of Acid Solutions
Authors: Zotov G. , Jarbo G. J.
Published: November 2005

A procedure is described for the treatment of graphite electrodes to make them impervious to acids. Elimination of loss of sample due to random seepage into the body of the electrode results in high sensitivity and good reproducibility. Sample volume required is 0 1 ml. Reproducibility obtained is within 25% of the amount present at 0.04 μg/ml level; 0.02 μg/ml is readily detectable for most elements. The electrodes are excited in flowing oxygen. A new compact chamber is also described in which the electrodes are sparked.
The Spectrochemical Determination of Trace Impurities in Graphite
Authors: Goleb J. A. , Faris J. P. , Meng B. H.
Published: November 2005

Optical emission spectrographic procedures are described for the estimation of some 60 elements in graphite. Using sodium fluoride as a carrier, the dc arc is employed for a direct examination of powdered graphite, while the copper spark method is used for analysis of the residue after ashing the sample.
Analysis of Air Samples for Beryllium by the Rotating Platform Spectrographic Technique
Authors: Wheeler G. V. , Ryder W. A. , Arnold K. R.
Published: November 2005

Beryllium is determined spectrographically on air sample filter papers by direct sparking of the filter paper mounted on a silver disk which revolves on a rotating platform electrode apparatus eccentric from a silver counter electrode. The procedure is fast and precise, with a minimum of sample handling and can be used with samples containing as little as one mμg of beryllium
Direct Spectrographic Determination of Trace Metals in Food Products by the Rotating Disc Technique
Authors: Paolini A. , Kennedy R. M.
Published: November 2005

A rapid, direct method for the determination of trace metals in food products by emission spectroscopy is described. This procedure permits the simultaneous determination of metals such as Ca, Cu, Fe, P, and Sn in food without time-consuming wet or dry ashing of the samples. It is applicable to fresh as well as canned or processed foods. The food is blended with water and an internal standard to a smooth consistency The sample is then sparked directly using the rotating disc technique. Concentrations from 1 to 1,000 ppm can be determined with good accuracy and reproducibility.
Spectrochemical Analysis of Iron Ores by the Solution-Spark-Rotating Disk Technique
Authors: Wilkinson Lex P.
Published: November 2005

A method is designed to provide for the spectrochemical analysis of iron ore for the following elements, reported as oxides in the ranges indicated: S1O2, 4.0–20.0%, and Al2O3, CaO, MgO, 1 0–6 0% each The solution and rotating disk technique is applied to a sample which has been treated to yield a dilute hydrochloric acid solution containing all of the four elements to be determined. A solution containing titanium and zinc for internal standard use is added. The spectrograms resulting from, a high voltage excitation of these sample solutions have given analytical results with an average precision of 3.0% expressed as the coefficient of variation.
Time-Intensity Characteristics of a Single-Discharge Emission Source
Authors: Runge E. F. , Forgacs R. L. , Bryan F. R.
Published: November 2005

Spectral line intensity vs time measurements were obtained from single, high-energy discharges by means of a photo-multiplier and cathode ray oscillograph. Effects of small changes in current pulse shape upon line intensities are observed for lines representing the first, second, and third spectra of aluminum. Line intensity peaks are observed in the spectra of ionized atoms, especially during the initial steep current rise of short duration pulses It is concluded that an improvement in the spectrographic sensitivity of spectra of ionized atoms can be achieved by employing an electrical pulse of extremely short duration in combination with detectors, which will resolve and record intensity maxima.
The Effect of Ion Mass and Ion Energy on the Sensitivity of Ilford Q2 Plates as Ion Detectors in Mass Spectrography
Authors: Owens Edward B.
Published: November 2005

The sensitivity of llford Q2 photographic plates as detectors in mass spectrography has been investigated. The dependence of the sensitivity on the mass and energy of the impinging ions has been determined from the relative darkening of the emulsion produced by a fixed number of ions of mass 13 through 198 accelerated by voltages between 1.88 and 15 kv The sensitivity was found to increase with increasing ion energy and to decrease with ion mass.
Spectrographic Analysis of Micro Samples of Tin-Cadmium Electroplated Alloys
Authors: Murt E. M. , Corson I.
Published: November 2005

A quantitative spectrographic procedure is described for the determination of cadmium in micro samples of tin-cadmium electroplated alloys. The porous cup solution procedure is employed with spark excitation. Tin is used as the internal standard. Cadmium is determined with an accuracy of ± 40 to 7.2% of the amount present depending on the concentration level, which extended from 10 to 30%.
The Atomic Absorption Determination of Some Noble Metals
Authors: Strasheim A. , Wessels G. J.
Published: November 2005

Methods for the atomic absorption determination of Pt, Pd, Rh, and Au in the presence of one or all of the other noble metals were developed. The reproducibility of the analytical results was satisfactory. The effect of various interfering solutions on the analytical results were examined
X-Ray Spectrographic Analysis of Silica and Alumina Base Catalyst by a Fusion-Cast Disc Technique
Authors: Townsend J. E.
Published: November 2005

An x-ray spectrographic analytical method has been developed using a fusion-cast disc technique based on that described by Claisse. This method eliminates the necessity of having chemically analyzed samples or synthetic samples for use as a calibration media and uses instead, an easily compounded mixture of metallic oxides diluted with lithium carbonate. Presently, the method is set up for the analysis of elements of atomic weight 23 through 42 but may be extended by use of other accessories in the optical system. The extreme dilution and subsequent fusion with sodium borate destroys sample identity and reduces matrix effects to such an extent that working curves may be used for a variety of sample types. The resultant cast disc may be retained and reused indefinitely.
A Cascade Mass Spectrometer
Authors: White F. A. , Sheffield J. C. , Rourke F. M.
Published: November 2005

A cascade spectrometer has been designed and constructed in which the ion beam traverses two successive 180° trajectories. This instrument differs from previous two-stage mass spectrometers in that a large single magnet (rather than tandem magnets) is utilized. Designed as a research rather than an analytical instrument, it provides for not only the analysis of ions from a primary source but also the identification of primary, secondary, or dissociated ions after the primary ion beam has interacted with a suitable target at the focal point of the first 180° 12-in. radius trajectory. Reflected and/or sputtered ions from the target traverse a second 180° trajectory and are detected by a semiconductor magnetic multiplier, which scans the entire focal plane. Isotopically resolved mass spectra of ions sputtered from pure metals and alloys have been obtained.
Identification of Rubber Polymers by Mass Spectrometry
Authors: Phillips J. K.
Published: November 2005

The identity of an elastomer or elastomers in a rubber compound can be determined within a few min by the use of a new analytical procedure described in this article It involves high temperature pyrolysis for two sec, tn vacuo, with an arc imaging furnace and subsequent analysis of the gaseous pyrolyzate with a mass spectrometer Numerical values derived from the mass spectra of standards permit semi-quantitative analyses of some mixtures of elastomers in cured products. Qualitative analyses have also been made on most of the common textile polymers and a small number of miscellaneous polymers.