Determination of Zirconium in Uranium Fissium Alloys

Evans, H. B.; Hrobar, A. M.; Patterson, Joshua T.

doi:10.1021/ac60160a008

Cited by 13 publications

(3 citation statements)

References 11 publications

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“…Preliminary precipitation of the rare earths as fluorides has been recommended in solutions containing iron, but with the high iron to rare earth ratio encountered here precipitation would be incomplete ( 1 ) . However, Lerner and Pinto (6) coprecipitated rare earth fluorides and oxalates with a thorium carrier from stainless steel solutions which contained ammonium fluoride and obtained high recoveries.…”

Section: Spectrophotometric Determination Of Yttrium and Rare Earths mentioning

confidence: 99%

Spectrophotometric Determination of Iron in Uranium-Fission Element Alloys.

McCown¹,

Kudera²

1962

Anal. Chem.

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Figure 1 . Effect of flash heater temperature on chromatograms of loganberry extract Flash heater: Chromatogram A, 205' C.; chromatogram 6, 100' C.of charged samples were a factor, the area of peak X, identified by infrared spectra as a-terpineol (p-menth-l-en-8-01), would be the reverse of that shown in Figure 1.Comparison of chromatograms A and B of Figure 2 shows that a-terpineol is aImost completely destroyed in A , whereas only slight decomposition was noted in B. The only difference in operating conditions for the two chromatograms was the flash heater tempera-CHROMATOGRAM ( A ) 6 12 18 24 x) 56 di 42 46 L TIME (MIN) Figure 2. Effect of flash heater temperature on chromatograms of a-terpineol Flash heater: Chromatogram A, 205' C.; chromatogram B, 100' C.ture. The fact that some decomposition was still evident, even at 100" C.emphasizes the thermal lability of the compound. Similar results were observed for linalool. Oxygenated terpenes are not peculiar in this respect and, like many compounds, they present a problem in achieving plug flow because of their relatively high boiling points. Evaluation of flash heater temperatures for unknown mixtures, to avoid decomposition, may prove desirable in most cases. While low flash heater temperatures tend to give undesirable skewed peaks (Figure 1, chromatogram B ) , these are less objectionable than to devote time to the analyses of thermal artifacts.SIR: In studies connected with the processing of fuels for the Second Experimental Breeder Reactor (ERB-11)) it has been necessary to determine less than 0.01% of iron in uranium alloys containing moIybdenum, ruthenium, palladium, rhodium, and zirconium.A simplified procedure for the spectrophotometric determination of iron in metallic uranium reported by Tomida and Takenchi (3) appeared to be adaptable for use on such samples.In Tomida's procedure, iron in a uranyl chloride solution of 7.5N hydrochloric acid was extracted into butyl acetate. After washing the organic layer twice with 7.5N hydrochloric acid, the butyl acetate phase was diluted with an equal volume of methyl isobutyl ketone (hexone) and the mixed solvent layer was contacted with a 20% aqueous solution of ammonium thiocyanate. The absorbance of the iron thiocyanate complex was measured directly in the organic solution.A procedure reported by Evans, Hrobar, and Patterson ( I ) utilized an ammonium hydroxide precipitation of uranium and zirconium to separate zirconium from palladium and molybdenum contained in uranium-fission element dloys. Because molybdenum was considered a possible interference in the iron thiocyanate procedure, it appeared that an ammonium hydroxide precipitation using uranium as a carrier for iron would serve a two-fold purpose:It would separate the iron from molybdenum and it would also furnish a precipitate which could be dissolved in 7.5N hydrochloric acid prior to the extraction with butyl acetate.As very little information was available on the details of the Japanese work, a study was made of the absorption spectra of the complex ...

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Section: Spectrophotometric Determination Of Yttrium and Rare Earths mentioning

confidence: 99%

Spectrophotometric Determination of Iron in Uranium-Fission Element Alloys.

McCown¹,

Kudera²

1962

Anal. Chem.

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“…Evans, Hrobar, and Patterson have developed two separation methods for zirconium in uranium alloys using cupferron and p-chloromandelic acid. The final measurement was made colorimetrically as the alizarin sulfonate lake (83). Rare Earths.…”

Section: Nbmentioning

confidence: 99%

Nonferrous Metallurgy

Leftault¹,

Moss²

1961

Anal. Chem.

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“…21 Subsequently, many other precipitants were used for the gravimetric analysis of Zr. [22][23][24] The procedure usually takes two to three hours to form a complete precipitation and then filtered out followed by ignition. The trace amount of Zr can be estimated by electrochemical techniques such as voltammetry, impedance spectroscopy, potentiometry, and ion selective electrodes.…”

Section: Introductionmentioning

confidence: 99%

Method to Eliminate Fluoride Interference in the Spectrophotometric Estimation of Zirconium: Application to U–Zr Alloys

2022

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In the estimation of Zr by UV-visible spectrophotometric technique, fluoride interference is a decade old unsolved problem. The process of repeated fuming with strong acids is often used to remove fluoride from the solution in order to estimate Zr by spectrophotometry analysis. For the first time, in this work, a simple use of AlCl3 is reported as a suppressing reagent to eliminate the interference of fluoride in the estimation of Zr. Xylenol orange in HCl medium is used as a complexing reagent. Linearity in the datum acquired from absorbance at 551 nm (λmax) is achieved over the concentration range 0.25-4.5 µg mL-1 of Zr with a molar absorptivity of 35030 L.mol-1.cm-1 and Sandell’s sensitivity of 0.003 µg.cm-2. Zr is quantified in the variety of U-Zr alloys and various water samples by using spectrophotometric detection with a classical univariate calibration with suppressing of fluoride-interference through AlCl3. Results from this novel analytical method herein developed for the first time are compared with those achieved from gravimetric analysis.

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Determination of Zirconium in Uranium Fissium Alloys

Cited by 13 publications

References 11 publications

Spectrophotometric Determination of Iron in Uranium-Fission Element Alloys.

Spectrophotometric Determination of Iron in Uranium-Fission Element Alloys.

Nonferrous Metallurgy

Method to Eliminate Fluoride Interference in the Spectrophotometric Estimation of Zirconium: Application to U–Zr Alloys

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