The determination of plutonium based on national bureau of standards potassium dichromate

Pietri, C.E.; Baglio, J.A.

doi:10.1016/0039-9140(60)80262-7

Cited by 11 publications

(5 citation statements)

References 3 publications

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“…Refs. [68][69][70][71][72][73]. Common reducing agents are liquid zinc amalgam, the Jones reductor, the lead reductor, Ti + , Cr + , and electrical methods.…”

Section: Chemical Analytical Methodsmentioning

confidence: 99%

Materials management in an internationally safeguarded fuels reprocessing plant

Hakkila¹,

Baker²,

Cobb³

1980

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Supporting information required for the design, evaluation, and implementation of an improved materials accounting system for reprocessing-conversion facilities is included in the third volume (the Appendices) of this report. Appendices A, B, and C include the basic process chemistry, descriptions of the reference facilities, and recommendations for possible process and facility modifications for improved materials accounting. The operator's safeguards system structure is reviewed in App. D. Appendices E-I review the tools used in the design and effectiveness evaluation studies, including the mathematical basis for international verification of the system. Measurement methodologies are reviewed in App. J-N. Appendix O considers the problem of integrating materials accounting and containment and surveillance measures.

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“…Refs. [68][69][70][71][72][73]. Common reducing agents are liquid zinc amalgam, the Jones reductor, the lead reductor, Ti + , Cr + , and electrical methods.…”

Section: Chemical Analytical Methodsmentioning

confidence: 99%

Materials management in an internationally safeguarded fuels reprocessing plant

Hakkila¹,

Baker²,

Cobb³

1980

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“…During the course of plutonium analyses for nearly three years the plutonium content for 28 samples from 3 lots of plutonium metal (99.96+% pure) and 35 samples from 9 lots of plutonium sulfate tetrahydrate (99.98+% pure) has been determined to be 99.97 ± 0.05% and 100.00 ± 0.05%., respectively, indicating plu-tonium sulfate tetrahydrate to be as reliable as plutonium metal when used for standardization purposes. Most of the above metal and salt samples were employed in verifying the standardization of potassium dichromate solutions subsequently used to titrate plutonium (11). Solutions accurately prepared from National Bureau of Standards potassium dichromate (Standard Sample No.…”

Section: Analytical Applicationsmentioning

confidence: 99%

Plutonium Sulfate Tetrahydrate, a Proposed Primary Analytical Standard for Plutonium.

Pietri¹

1962

Anal. Chem.

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Extraction, % 15 30 60 120 240 89.2 99.4 99.9 99.7 99.5 a Under conditions ae outlined in Procedure.The divalent CrO,-2 ion does not form an ion-association complex with the quaternary ammonium ion. Thus contact with caustic completely strips the chromium from the organic phase. Chromium could not be completely removed from methyl isobutyl ketone with the strip solution in the absence of the quaternary ammonium ion. This may be due to some type of solvation mechanism.Scavenging the strip phase with ferric hydroxide separates hydrolyzable ions that are coextracted with the chromium.Oxidization of the Cr(II1) in basic Plutonium Analytical solution appeared worthwhile and was investigated. A sample of aged fission products was treated according t o the first steps in the recommended procedure, followed by dissolution of the Cr(OH)a Mith 1 5 M NaOH. Sodium hypochlorite was added and after the oxidation was completed, an iron scavenging was performed. After filtering and acidifying, the Cr(Y1) n a s extracted according to the procedure. A ?-ray spectrum of the strip phase showed copious quantities of rutheniuni activity as well as some zirconiuniniobium activity in the final product. Apparently much of the ruthenium x i s in an extractable form and follon ed t!ie chrorniurn. Hence, in the recommended procedure, ruthenium is removed in the perchloric acid oxidation step. The yield is conveniently determined on a n aliquot of the strip phase by a spectrophotometric determination of chromate a t 370 mp.Decontamination by this procedure from 3-day and 3-month cooled fission product mixtures is shown in Figures 3 and 4, respectively. With irradiated stainless steel 300-type alloys, no foreign activity was found in the final chromium fraction.Six aliquots of chromium-51 activity were carried through the recommended procedure and the area under the 320k.e.17. photopeak m-as measured. The relative standard deviation was less than 1%. The average yield is 85% and the time of analysis is approvimately 1 hour. llTERATURE CITED(1) Dean, J. A., Beverlj-, lf. L., Ax41,.

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“…By the use of weight burets for both aliquoting and the addition of titrant a precision of ±0.05% is obtainable (8). Iron, the most common contaminant of plutonium metal and its compounds, interferes and a correction for the iron by means of a spectrophotometric determination is necessary, Several variations in the titration of the (III-IV) couple, such as photometric end point detection (2), and use of potassium dichromate as the titrant (10), have since been introduced.…”

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confidence: 99%