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Title: The comparison of sample preparation techniques for the determination of technetium-99 in pure uranium compounds and subsequent analysis by inductively coupled plasma-mass spectrometry (ICP-MS)

Abstract

In this presentation, a procedure for the determination of ng/g levels of technetium-99 in uranium dioxide powder, hydrolyzed uranium hexafluoride (Hex), and uranyl nitrate liquor (UNL) is discussed, and three methods for the dissolution of uranium dioxide are compared. Digestion of uranium dioxide using concentrated nitric acid in a stoppered glass tube gives variable results. A concentrated hydrochloric acid dissolution using microwave digestion in sealed TFE-fluorocarbon PFA digestion vessels gives reproducible results, as does the digestion using dilute nitric acid in open beakers. The effects of the isobaric interference of ruthenium-99 and the molecular interference of {sup 98}MoH and the use of suitable algorithms to correct for such interferences are discussed. Compensation of signal suppression due to the uranium matrix is made by the use of matrix-matched calibration standard solutions and instrumental drift is monitored and corrected by the addition of rhodium as an internal standard. A detection limit (2 s) of 0.3 ng g{sup {minus}1} U is achieved using a solution containing 2 g of uranium per liter and a 30-s per isotope acquisition time, using peak jump mode.

Authors:
 [1]
  1. British Nuclear Fuels PLC, Preston (United Kingdom). Chemical and Metallurgical Services Dept.
Publication Date:
OSTI Identifier:
409710
Report Number(s):
CONF-9410207-
ISBN 0-8031-2034-6; TRN: 97:000712
Resource Type:
Book
Resource Relation:
Conference: Symposium on applications of inductively coupled plasma mass spectrometry (ICP-MS) to radionuclide determinations, Gatlinburg, TN (United States), 11-13 Oct 1994; Other Information: PBD: 1995; Related Information: Is Part Of Applications of inductively coupled plasma-mass spectrometry to radionuclide determinations; Morrow, R.W. [ed.] [Lockheed-Martin Energy Systems, Oak Ridge, TN (United States)]; Crain, J.S. [ed.] [Argonne National Lab., IL (United States)]; PB: 149 p.; ASTM STP 1291
Country of Publication:
United States
Language:
English
Subject:
40 CHEMISTRY; TECHNETIUM 99; QUANTITATIVE CHEMICAL ANALYSIS; URANIUM DIOXIDE; URANIUM HEXAFLUORIDE; URANYL NITRATES; DISSOLUTION; NITRIC ACID; HYDROCHLORIC ACID; MICROWAVE HEATING; CALIBRATION; STANDARDS; ACCURACY; EXPERIMENTAL DATA

Citation Formats

Makinson, P R. The comparison of sample preparation techniques for the determination of technetium-99 in pure uranium compounds and subsequent analysis by inductively coupled plasma-mass spectrometry (ICP-MS). United States: N. p., 1995. Web.
Makinson, P R. The comparison of sample preparation techniques for the determination of technetium-99 in pure uranium compounds and subsequent analysis by inductively coupled plasma-mass spectrometry (ICP-MS). United States.
Makinson, P R. 1995. "The comparison of sample preparation techniques for the determination of technetium-99 in pure uranium compounds and subsequent analysis by inductively coupled plasma-mass spectrometry (ICP-MS)". United States.
@article{osti_409710,
title = {The comparison of sample preparation techniques for the determination of technetium-99 in pure uranium compounds and subsequent analysis by inductively coupled plasma-mass spectrometry (ICP-MS)},
author = {Makinson, P R},
abstractNote = {In this presentation, a procedure for the determination of ng/g levels of technetium-99 in uranium dioxide powder, hydrolyzed uranium hexafluoride (Hex), and uranyl nitrate liquor (UNL) is discussed, and three methods for the dissolution of uranium dioxide are compared. Digestion of uranium dioxide using concentrated nitric acid in a stoppered glass tube gives variable results. A concentrated hydrochloric acid dissolution using microwave digestion in sealed TFE-fluorocarbon PFA digestion vessels gives reproducible results, as does the digestion using dilute nitric acid in open beakers. The effects of the isobaric interference of ruthenium-99 and the molecular interference of {sup 98}MoH and the use of suitable algorithms to correct for such interferences are discussed. Compensation of signal suppression due to the uranium matrix is made by the use of matrix-matched calibration standard solutions and instrumental drift is monitored and corrected by the addition of rhodium as an internal standard. A detection limit (2 s) of 0.3 ng g{sup {minus}1} U is achieved using a solution containing 2 g of uranium per liter and a 30-s per isotope acquisition time, using peak jump mode.},
doi = {},
url = {https://www.osti.gov/biblio/409710}, journal = {},
number = ,
volume = ,
place = {United States},
year = {Sun Dec 31 00:00:00 EST 1995},
month = {Sun Dec 31 00:00:00 EST 1995}
}

Book:
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