You need JavaScript to view this

The MacDonald and savage titrimetric procedure for plutonium scaled-down to the milligram level: Automated procedure for routine analysis of safeguards samples containing 2 to 5 mg plutonium

Technical Report:

Abstract

A selective titrimetric procedure directly applicable to both input and product solutions from fast reactor fuel reprocessing was set up by MacDonald and Savage and scaled down to 3 mg of plutonium in sample aliquots at the request of the Safeguards Analytical Laboratory (SAL) of the International Atomic Energy Agency (IAEA), which needed to replace its silver (II) oxide titration procedure by a more selective electrochemical method. Although the procedure is very selective the following species still interfere: Vanadates (almost quantitatively), Neptunium (one electron exchange per mole); Nitrites, Fluorosilicates and Iodates present in mg amount yield slight biases. This paper describes the fully automatized procedure presently applied in SAL for the routine determination of 2 to 5 mg plutonium dissolved in nitric acid solution. The method allows the unattended analysis of 20 aliquots within a five hour period. The equipment including the reagent distribution system, the sample changer and the control units are introduced and the principle design of the software is shortly described. Safety requirements have been addressed and are also reviewed in the report. Results obtained on standard reference materials, international intercomparison samples and actual safeguards samples routinely analyzed with the proposed procedure are presented and compared with  More>>
Authors:
Ronesch, K; Jammet, G; Berger, J; Doubek, N; Bagliano, G; Deron, S; [1]  Kuvik, V [2] 
  1. International Atomic Energy Agency, Seibersdorf (Austria). Safeguards Analytical Lab.
  2. Central Control Lab., NRI, Rez (Czechoslovakia)
Publication Date:
Aug 01, 1992
Product Type:
Technical Report
Report Number:
IAEA-AL-059
Reference Number:
SCA: 400102; PA: AIX-24:000051; SN: 93000912510
Resource Relation:
Other Information: PBD: Aug 1992
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; PLUTONIUM; POTENTIOMETRY; TITRATION; REPROCESSING; VERIFICATION; ACCURACY; CERIUM NITRATES; CHEMICAL PREPARATION; INTERFERING ELEMENTS; INTERLABORATORY COMPARISONS; NITRIC ACID; OXIDATION; QUANTITATIVE CHEMICAL ANALYSIS; SAFEGUARDS; 400102; CHEMICAL AND SPECTRAL PROCEDURES
OSTI ID:
10108599
Research Organizations:
International Atomic Energy Agency, Seibersdorf (Austria). Safeguards Analytical Lab.
Country of Origin:
IAEA
Language:
English
Other Identifying Numbers:
Other: ON: DE93608774; TRN: XA9232923000051
Availability:
OSTI; NTIS (US Sales Only); INIS
Submitting Site:
INIS
Size:
[29] p.
Announcement Date:
Jun 30, 2005

Technical Report:

Citation Formats

Ronesch, K, Jammet, G, Berger, J, Doubek, N, Bagliano, G, Deron, S, and Kuvik, V. The MacDonald and savage titrimetric procedure for plutonium scaled-down to the milligram level: Automated procedure for routine analysis of safeguards samples containing 2 to 5 mg plutonium. IAEA: N. p., 1992. Web.
Ronesch, K, Jammet, G, Berger, J, Doubek, N, Bagliano, G, Deron, S, & Kuvik, V. The MacDonald and savage titrimetric procedure for plutonium scaled-down to the milligram level: Automated procedure for routine analysis of safeguards samples containing 2 to 5 mg plutonium. IAEA.
Ronesch, K, Jammet, G, Berger, J, Doubek, N, Bagliano, G, Deron, S, and Kuvik, V. 1992. "The MacDonald and savage titrimetric procedure for plutonium scaled-down to the milligram level: Automated procedure for routine analysis of safeguards samples containing 2 to 5 mg plutonium." IAEA.
@misc{etde_10108599,
title = {The MacDonald and savage titrimetric procedure for plutonium scaled-down to the milligram level: Automated procedure for routine analysis of safeguards samples containing 2 to 5 mg plutonium}
author = {Ronesch, K, Jammet, G, Berger, J, Doubek, N, Bagliano, G, Deron, S, and Kuvik, V}
abstractNote = {A selective titrimetric procedure directly applicable to both input and product solutions from fast reactor fuel reprocessing was set up by MacDonald and Savage and scaled down to 3 mg of plutonium in sample aliquots at the request of the Safeguards Analytical Laboratory (SAL) of the International Atomic Energy Agency (IAEA), which needed to replace its silver (II) oxide titration procedure by a more selective electrochemical method. Although the procedure is very selective the following species still interfere: Vanadates (almost quantitatively), Neptunium (one electron exchange per mole); Nitrites, Fluorosilicates and Iodates present in mg amount yield slight biases. This paper describes the fully automatized procedure presently applied in SAL for the routine determination of 2 to 5 mg plutonium dissolved in nitric acid solution. The method allows the unattended analysis of 20 aliquots within a five hour period. The equipment including the reagent distribution system, the sample changer and the control units are introduced and the principle design of the software is shortly described. Safety requirements have been addressed and are also reviewed in the report. Results obtained on standard reference materials, international intercomparison samples and actual safeguards samples routinely analyzed with the proposed procedure are presented and compared with results achieved with the semiautomatic mode to demonstrate the performance. International requirements to reduce the amount of radioactive materials in waste will certainly lead to a further reduction of the amount of plutonium in one aliquot. Some future perspective to titrate 1 mg samples are presented in the discussion. 12 refs, 10 figs, 8 tabs.}
place = {IAEA}
year = {1992}
month = {Aug}
}