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Title: A STUDY OF SPECTROPHOTOMETRIC METHODS FOR THE DETERMINATION OF OSMIUM (thesis)

Abstract

The development of rapid, selective, and sensitive methods for the determination of osmium in liquid samples is reported. The specific application of primary interest was the estimation of microgram or milligram quantities of osmium in homogeneous reactcr fuel solutions which contain uranyl sulfate as the major component and corrosion products of stainless steel as minor components. (W.L.H.)

Authors:
Publication Date:
Research Org.:
Oak Ridge National Lab., Tenn.
OSTI Identifier:
4194413
Report Number(s):
ORNL-2862
NSA Number:
NSA-14-006256
DOE Contract Number:
W-7405-ENG-26
Resource Type:
Technical Report
Resource Relation:
Other Information: Submitted to the Univ. of Tennessee. Orig. Receipt Date: 31-DEC-60
Country of Publication:
United States
Language:
English
Subject:
CHEMISTRY; CORROSION; FUELS; HOMOGENEOUS REACTORS; LIQUIDS; OSMIUM; PHOTOMETRY; QUANTITATIVE ANALYSIS; REACTORS; SAMPLING; SOLUTIONS; SPECTRA; STAINLESS STEELS; SULFATES; TRACE AMOUNTS; URANYL COMPOUNDS

Citation Formats

Goldstein, G. A STUDY OF SPECTROPHOTOMETRIC METHODS FOR THE DETERMINATION OF OSMIUM (thesis). United States: N. p., 1960. Web. doi:10.2172/4194413.
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Goldstein, G. A STUDY OF SPECTROPHOTOMETRIC METHODS FOR THE DETERMINATION OF OSMIUM (thesis). United States. doi:10.2172/4194413.
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Goldstein, G. Wed . "A STUDY OF SPECTROPHOTOMETRIC METHODS FOR THE DETERMINATION OF OSMIUM (thesis)". United States. doi:10.2172/4194413. https://www.osti.gov/servlets/purl/4194413.
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@article{osti_4194413,
title = {A STUDY OF SPECTROPHOTOMETRIC METHODS FOR THE DETERMINATION OF OSMIUM (thesis)},
author = {Goldstein, G.},
abstractNote = {The development of rapid, selective, and sensitive methods for the determination of osmium in liquid samples is reported. The specific application of primary interest was the estimation of microgram or milligram quantities of osmium in homogeneous reactcr fuel solutions which contain uranyl sulfate as the major component and corrosion products of stainless steel as minor components. (W.L.H.)},
doi = {10.2172/4194413},
journal = {},
number = ,
volume = ,
place = {United States},
year = {Wed Jan 20 00:00:00 EST 1960},
month = {Wed Jan 20 00:00:00 EST 1960}
}
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Technical Report:
View Technical Report (2.81 MB)
DOI:  10.2172/4194413
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  • A method was developed for the spectrophotometric determination of 30 to 100 mu g of osmium. The osmium as OsO/sub 4/ is extracted with CHCl/sub 3/ and diphenylcarbazide is then added to the organic extract. A blue-violet reaction product is formed, the absorbancy of which is measured at 560 m mu . A suitable reagent concentration is from 3 to 5 ml of 0.2% diphenylcarbazide in a volume of 25 ml and the preferred solvent for the reagent is ethanol. Beer's law is followed over a range of 8 to 130 mu g of osmium with a coefficient of variationmore » of about 4 After a 2-hr color-development period the molar absorbancy index is 31,300. Attempts to achieve reproducible measurements of absorbancy in less than 2 hr were unsuccessful. A study was made of the effects of foreign elements and only Ru(VIII) was found to interfere. (auth)« less

  • A method was developed for the determination of osmium by measuring the absorbancy of osmium tetroxide in CHCl/sub 3/. The osmium is first oxidized to the octavalent state and the osmium tetroxide which is formed is extracted selectively with CHCl/sub 3/. The ultraviolet absorption spectrum of OsO/sub 4/ in CHCl/sub 3/ has a series of absorption bands with peak absorbancies at 282, 289. 297, 304, and 312 m mu , and molar absorbancy indices of 1870. 1760, 1640, 1400, and 1000, respectively. For each wavelength the optimum concentration range for the determination of osmium was evaluated by the method ofmore » Ringbom. Only chloride and octavalent ruthenium interfere in the determination. By this method, from 0.4 to 3 mg of osmium can be determined with a coefficient of variation of 3%. (auth)« less

  • ; ; ; ... - Talanta (England)
    An ultraviolet spectrophotometric method is presented for the determination of milllgram quantities of osmium in solutions of uranyl suifate. Osmium is first oxidized to the octovalent state, and the osmium tetroxide which ls formed is selectively extracted with chloroform. The ultraviolet absorption spectrum of osmium tetroxide in chloroform has a series of absorptlon bands with peak absorbancies at 282, 289, 297, 304, and 312 m mu and molar absorbancy indexes of 1870, 1760, 1640, 1400 and 1000, respectively. For each wavelength, the optimum concentration range for the determination of osmium was evaluated. From 0.4 to 3.3 mg of osmium canmore » be determined with a coefficient of variation of 3%. Of the elements tested only chloride and octovalent ruthenium interfere; however, both of these interferences can be eliminated. (auth)« less

  • New spectrophotometric methods for the determination of scandium, yttrium, and bromate, respectively. have been developed. Scandium and yttrium react non-selectively with anthrarufin-2,6-disuifonic acid (disodium salt) to give one to one complexes which obey Beer's law. The sensitivity of the scandium reaction is one part in 250 million and that for yttrium is one part in 200 million. Ion exchange with Dowex-1 X 8 and solvent extraction with dibutyl phosphate, tributyl phosphate, and thenoyltrifluoroacetone were investigated. Separation procedures were developed for scandium and yttrium. The scandium separation procedure was successfully applied to six salt solutions containing various trace amounts of thismore » element. Bromate reacts with o-arsanilic acid to give a reddish-brown color. This reaction, though somewhat unstable, was developed into a spectrophotometric method for traces of bromate. The method is sensitive to one part of bromate in 20 million parts of solution. The effects of pH, time, and temperature are critical and must be carefully controlled. (A.G.W.)« less

  • ; ; ; ... - Talanta (England)
    A method has been developed for the spectrophotometric determination of microgram quantlties of osmium in uranyl sulfate solutions. The osmium is oxidized to osmium tetroxide, then extracted wtth chloroform. The extracts are added to an ethanolic solutlon of 1:5diphenylcarbchydrazide. A blue-violet colored reaction product is formed which exhibits maximum absorbancy at 560 m mu . After a period of 2 hr for color development the molar absorbancy index is about 31,000. Beer's law is adnered to over a range of 30 to 100 mu g of osmium with a coefficient of variatlon of about 4%. A study was made ofmore » the effects of foreign substances and only chloride and octovalent ruthenium were found to interfere. Both of these lnterfering ions can be eliminated. (auth)« less