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Title: Determination of radium-226 by high-resolution alpha spectrometry

Abstract

The determination of radium-226 by alpha spectrometry has been investigated critically to determine experimental conditions under which high resolution and accurate and reliable results can be obtained. Refractory solids such as soils, ores, and tailings from uranium mills are dissolved completely by fusion with potassium fluoride in the presence of barium-133 tracer. The fluoride cake is then transposed with sulfuric acid to a pyrosulfate fusion with simultaneous volatilization of all silica and fluoride. Radium is precipitated with barium already present in the sample by addition of lead perchlorate to a dilute hydrochloric acid solution of the pyrosulfate cake. The resulting insoluble sulfates are dissolved in an alkaline solution of diethylenetriaminepentaacetic acid, and the radium and barium sulfates are reprecipitated with acetic acid. The precipitate is mounted on a membrane filter and analyzed by alpha spectrometry. Water samples are partially evaporated and treated similarly. Resolution of the subsequent alpha spectra is much better than has been achieved previously from barium sulfate, and is almost as good as is obtainable with actinides electrodeposited on polished steel plates. The resolution is about 60 keV full-width-half-maximum with 100 ..mu..g of barium on a 1-inch filter with a 450 mm/sup 2/ detector at 20% countingmore » efficiency. Recovery is about 97% and accuracy is generally as good as the counting statistics obtained will permit. Grossly inaccurate results can be obtained under certain conditions when barium-133 tracer is used to determine the chemical yield of radium-226. Severe contamination of the surface-barrier detector by polonium-210 and by recoil products of the radium isotopes being counted is demonstrated, amd methods for virtual elimination of both problems are discussed.« less

Authors:
Publication Date:
Research Org.:
EG and G Idaho, Inc., Idaho Falls (USA)
OSTI Identifier:
5770824
Report Number(s):
EGG-M-00883; CONF-830695-7
ON: DE83014959
DOE Contract Number:  
AC07-76ID01570
Resource Type:
Conference
Resource Relation:
Conference: Health Physics Society annual meeting, Baltimore, MD, USA, 19 Jun 1983
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; 11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS; RADIUM 226; ALPHA SPECTROSCOPY; BARIUM 133; BARIUM SULFATES; ERRORS; FEED MATERIALS PLANTS; MILL TAILINGS; ORES; PRECIPITATION; RADIOCHEMICAL ANALYSIS; RADIUM SULFATES; SOILS; SULFATES; TRACER TECHNIQUES; WATER; ALKALINE EARTH ISOTOPES; ALKALINE EARTH METAL COMPOUNDS; ALPHA DECAY RADIOISOTOPES; BARIUM COMPOUNDS; BARIUM ISOTOPES; BETA DECAY RADIOISOTOPES; CHEMICAL ANALYSIS; DAYS LIVING RADIOISOTOPES; ELECTRON CAPTURE RADIOISOTOPES; EVEN-EVEN NUCLEI; EVEN-ODD NUCLEI; HEAVY NUCLEI; HYDROGEN COMPOUNDS; INDUSTRIAL PLANTS; INTERMEDIATE MASS NUCLEI; INTERNAL CONVERSION RADIOISOTOPES; ISOMERIC TRANSITION ISOTOPES; ISOTOPE APPLICATIONS; ISOTOPES; NUCLEAR FACILITIES; NUCLEI; OXYGEN COMPOUNDS; QUANTITATIVE CHEMICAL ANALYSIS; RADIOISOTOPES; RADIUM COMPOUNDS; RADIUM ISOTOPES; SEPARATION PROCESSES; SOLID WASTES; SPECTROSCOPY; SULFUR COMPOUNDS; TAILINGS; WASTES; YEARS LIVING RADIOISOTOPES; 400103* - Radiometric & Radiochemical Procedures- (-1987); 053000 - Nuclear Fuels- Environmental Aspects

Citation Formats

Sill, C W. Determination of radium-226 by high-resolution alpha spectrometry. United States: N. p., 1983. Web.
Sill, C W. Determination of radium-226 by high-resolution alpha spectrometry. United States.
Sill, C W. Sat . "Determination of radium-226 by high-resolution alpha spectrometry". United States.
@article{osti_5770824,
title = {Determination of radium-226 by high-resolution alpha spectrometry},
author = {Sill, C W},
abstractNote = {The determination of radium-226 by alpha spectrometry has been investigated critically to determine experimental conditions under which high resolution and accurate and reliable results can be obtained. Refractory solids such as soils, ores, and tailings from uranium mills are dissolved completely by fusion with potassium fluoride in the presence of barium-133 tracer. The fluoride cake is then transposed with sulfuric acid to a pyrosulfate fusion with simultaneous volatilization of all silica and fluoride. Radium is precipitated with barium already present in the sample by addition of lead perchlorate to a dilute hydrochloric acid solution of the pyrosulfate cake. The resulting insoluble sulfates are dissolved in an alkaline solution of diethylenetriaminepentaacetic acid, and the radium and barium sulfates are reprecipitated with acetic acid. The precipitate is mounted on a membrane filter and analyzed by alpha spectrometry. Water samples are partially evaporated and treated similarly. Resolution of the subsequent alpha spectra is much better than has been achieved previously from barium sulfate, and is almost as good as is obtainable with actinides electrodeposited on polished steel plates. The resolution is about 60 keV full-width-half-maximum with 100 ..mu..g of barium on a 1-inch filter with a 450 mm/sup 2/ detector at 20% counting efficiency. Recovery is about 97% and accuracy is generally as good as the counting statistics obtained will permit. Grossly inaccurate results can be obtained under certain conditions when barium-133 tracer is used to determine the chemical yield of radium-226. Severe contamination of the surface-barrier detector by polonium-210 and by recoil products of the radium isotopes being counted is demonstrated, amd methods for virtual elimination of both problems are discussed.},
doi = {},
journal = {},
number = ,
volume = ,
place = {United States},
year = {1983},
month = {1}
}

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