A separation scheme for the analysis of multicomponent samples

A sequential separation scheme has been devised for the quantitative analytical separation of 27 different metal ions. Five different Chromatographic and ion-exchange columns are used to separate the metal ions into groups. The metal ions of each group are eluted separately from each column by means of selective eluents. Following separation, the metal ions are determined by titrimetry, flame spectrometry or other appropriate analytical methods. The reliability of the proposed scheme has been demonstrated by extensive testing, including the analysis of U.S. National Bureau of Standards samples. The scheme can be used for macro or micro quantities.     

A systematic scheme of qualitative analysis for anions : A simplified scheme for the detection of common anions

The original comprehensive scheme for the detection of anions has been simplified for the systematic detection of common anions     

A rapid fire-assay/atomic-absorption method for the determination of platinum, palladium and gold in ores and concentrates: A modification of the tin-collection scheme

The tin-collection scheme of fire-assaying has been simplified to permit the rapid and accurate determination of platinum, palladium and gold in ores and related materials. The presence of tellurium in the charge ensures that the precious metals remain insoluble during the parting of the tin button with hydrochloric acid. The residue is easily collected and dissolved and the resultant solution analysed for the precious metals by AAS. The accuracy of the method has been established by application to five diverse certified reference materials.     

A systematic scheme of qualitative analysis for cations and anions

The behaviour of different elements towards sodium hydroxide and sodium carbonate is reviewed. Detailed procedures for the complete analysis of a mixture containing anions and cations are given.     

A systematic scheme of qualitative analysis for anions.IV

A comprehensive investigation has been undertaken to ascertain how the basic radicals that pass into the sodium carbonate filtrate arc distributed among the various groups for the detection of anions. Methods for the detection of these basic radicals in the presence of the anions have been worked out in detail. It was found that the scheme for the detection of anions put forward previously remains unaffected by the presence of these basic radicals. It has been shown that the scheme for the detection of anions can be integrated with the comprehensive schemes for the detection of basic radicals and insoluble substances.     

A systematic scheme of qualitative analysis for anions. III

The completeness of precipitation of anions and basic radicals by the two group reagents, zinc acetate and cadmium nitrate, has been investigated. It has been shown that the two reagents precipitate many of the anions quantitatively and can thus be used for their gravimetric estimation.     

Spectrophotometric determination of uranium application of the method to the analysis of leach solutions and monazite

Uranyl thiocyanate complex is extracted from a slightly acid solution, using tributyl phosphate-carbon tetrachloride as solvent. The effect of various factors on the extraction of uranium and the interference of a number of cations and anions was studied. After extraction, uranium is determined spectrophotometrically in the organic solvent.     

Dry-column chromatography of uranium. Application to chemical analysis of monazite and phosphate rock for uranium

Summary A dry-column Chromatographic technique has been applied to the separation of uranium from complicated matrices. It has been demonstrated that operating parameters of thin-layer chromatography on silanized silica gel in isopropyl ether-tetrahydrofuran-nitric acid (65203) can be transferred to this technique. Chromatograms are thus easily developed on dry packed column with the solvent system of the type used in the TLC. Uranium is eluted off the column and determined with Arsenazo III spectrophotometrically. The technique is successfully applied to the determination of uranium in monazite and phosphate rock samples with good precision and accuracy.

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Trockensäulenchromatographie des Urans. Anwendung zur chemischen Analyse von Monazit und Phosphorit

Zusammenfassung Zur Abtrennung des Urans aus komplizierten Matrices wurde die Trockensäulenchromatographie verwendet. Wie gezeigt werden konnte, lassen sich die Bedingungen der Dünnschichtchromatographie (DSC) auf silanisiertem Silikagel mit Isopropylether-Tetrahydrofuran-Salpetersäure (65203) auf das genannte Verfahren übertragen. Chromatogramme sind daher auf trocken geschichteten Säulen mit Lösungsmittelsystemen der DSC herstellbar. Uran wird eluiert und mit Arsenazo III spektrophotometrisch bestimmt. Das Verfahren wurde zur Uranbestimmung in Monazit und Phosphorit erfolgreich angewendet.

     

Improved scheme for the analysis of high-purity talc

An improved method is proposed for the determination of silica, magnesium oxide, R(2)O(3), ferric oxide, calcium oxide, and aluminium oxide in high-purity talc. In the method for silica and magnesium oxide, the sample is fused with sodium carbonate and the cooled melt is dissolved with perchloric acid in such a manner that it floats free from the crucible (in previous schemes for the analysis of talc there are frequently mechanical losses due to the difficulty of removing the magnesium silicate melt from the crucible). The solution is then evaporated to fumes of perchloric acid and the silica is filtered off and ignited. The magnesium oxide is determined in the filtrate by precipitation as magnesium ammonium phosphate and a correction is made for the calcium which is precipitated along with the magnesium ammonium phosphate. R(2)O(3) is determined after treatment of the sample with nitric and hydrofluoric acids and evaporation to fumes of perchloric acid. Iron oxide and calcium oxide are determined by atomic absorption, after treatment with nitric and hydrofluoric acids and evaporation to fumes of perchloric acid. Al(2)O(3) is calculated by difference.     

A systematic scheme of qualitative analysis for anions. part II

Procedures for the separation of amons into groups and the detailed analysis of groups are given     

Non-volatile organic analysis of uranium ore concentrates

In support of nuclear safeguards and non-proliferation efforts, Oak Ridge National Laboratory is responsible for characterizing uranium ore concentrate (UOC) samples obtained from two ore mining and milling sites. A sorptive extraction method has been developed for analysis of non-volatile organic compounds that might be used to identify characteristics of the purification process by which uranium was separated from these ores. This method utilizes Gerstel Twister^® stir bars coated with polydimethylsiloxane to extract organic components from aqueous media. A slurry of UOC is extracted with the Twister^® stir bar in 20 % methanol/80 % water containing deuterated internal hydrocarbon standards. Following extraction of non-volatile organics, the Twister^® stir bar is analyzed directly in the inlet of a gas chromatograph fitted with a quadrupole mass spectrometric detector. Results have been consistent and have shown excellent recoveries of internal standards, with the average recovery being 97.5 %. Both qualitative and quantitative differences have been identified between the two sources of UOC utilizing this method. One source contained an increased concentration of amines which commonly are used in the recovery and purification of ores. Amines that were identified in this UOC source include dioctylamine, triisoctylamine, and Alamine^® 336, a common industrial complexant. Also, when comparing both sources, the same UOC source contained various decanol and C20 compounds. Based on the results from this study, non-volatile organic analysis of UOC using sorptive extraction with Twister^® stir bars and GC–MS is a tool that can be used to facilitate sourcing of unknown UOC.     

An investigation of methods for the analysis of zinc concentrates for their total fluoride contents

Accurate determination of trace fluoride down to 6.6 mug/g in zinc concentrate samples is found to be most expediently performed potentiometrically with a fluoride ion-selective electrode and a single-point standard addition after decomposition of the sample by potassium hydroxide fusion. The lower limit of measurement may be reduced to 1.8 mug/g if distillation from tungsten oxide flux is used in place of the fusion, but the analysis takes longer. The need for reliable fluoride data for zinc concentrate standard reference materials is exemplified and results for CANMET zinc concentrate MP-1 are given. The failure of some of the methods used to analyse standard siliceous materials is discussed.     

Fast neutron activation analysis of rare-earth elements in monazite from Korea

The relative ans single comparator methods have been applied to determine 7 rare-earth elements and U, Th in Korean Monazites by 14.5 MeV neutron activation analysis. The (n, 2n) nuclear reactions are used for all elements except La, for which (n, p) reaction is used. Al is used as a flux monitor for the relative method and as a singlle comparator for the single comparator method. The analytical results obtained by the two methods agree well within 3% deviation except for Sm and Gd. These results are also compared with the result obtained by a single comparator method using reactor neutron.     

A systematic scheme of qualitative analysis for anions. part I

A new and comprehensive scheme for the systematic detection of anions has been put forward. This scheme is based on the precipitation of difficultly soluble salts of anions in groups by basic group reagents in sodium carbonate solution and the subsequent analysis of cach group precipitate or filtrate for the detection of individual members of the group     

A systematic scheme for the analysis of common anions using the Weisz ring oven technique

Summary A systematic scheme for the identification of the common anions: sulphate, sulphite, nitrate, nitrite, fluoride, chloride, bromide, iodide, ferricyanide, ferrocyanide, thiocyanate, phosphate, sulphide, thiosulphate and borate in a mixture by the ring oven technique has been described.

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Zusammenfassung Ein systematischer Analysengang zum Nachweis folgender Anionen mit Hilfe des Ringofens wurde beschrieben: Sulfat, Sulfit, Nitrat, Nitrit, Fluorid, Chlorid, Bromid, Jodid, Cyanoferrat(III), Cyanoferrat (II), Rhodanid, Phosphat, Sulfid, Thiosulfat und Borat.

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Résumé On a décrit un plan d'identification systématique des anions usuels dans leurs mélanges: sulfate, sulfite, nitrate, nitrite, fluorure, chlorure, bromure, iodure, ferricyanure, ferrocyanure, thiocyanate, phosphate, sulfure, thiosulfate et borate, au moyen de la technique du four annulaire.

     

A simplified and extended scheme of analysis for the common cations,based on paper chromatography

The chromatogram-comparison method has been extended to include the elements Li, Be, Ce, Ti, V, Mo, Th and U. The technique was simplified through the use of six drops of the original solution, two on each of the general solvent mixtures. The method was also made more accurate through the application of selected specific sprays.     

A new method - based on paper chromotography - for the estimation of thorium and uranium in monazite

A dioxan-antipyrine solvent mixture is used to separate thorium and uranium — on sheet chromatograms — from the monazite sand solution. Thorium is estimated by an indirect EDTA titration method, using pyrocatechol violet, Uranium is estimated spectrophotometrically by the hydrogen peroxide method.     

Determination of rare earth elements in Taiwan monazite by chemical neutron activation analysis

Taiwan monazite is a unique mineral obtained from the heavy sand found in the river floor of Tzuo-suei river and En-suei river. Both rivers are flowing parallel with separated narrow area into the sea at southwestern coast of Taiwan. The characteristic of monazite is that it contains considerable rare earth elements (REEs). REEs are considered very useful elements in the local industries and scientific researches such as ceramic, semiconductors, and glass optics. In this study, chemical neutron activation analysis (CNAA) was used to determine the contents of REEs in Taiwan monazite. A few milligram of monazite was digested in the microwave oven for 25 minutes with mixed acid (conc. HNO₃ and HClO₄). REEs were preconcentrated by hydrated magnesium oxide and CNAA was performed.