Determination of In and Ga in plutonium oxide matrix by ICP-AES after chemical separation

Abstract

An analytical method was developed for the determination of indium and gallium in plutonium samples. A solvent extraction technique was employed by using 30% TBP in CCl 4 for the quantitative separation of plutonium from the sample solution and subsequent determination by radial inductively coupled plasma atomic emission spectrometry (ICP-AES). The quantitative recovery of In and Ga in the separated samples was confirmed from radiometric/tracer studies. Recording of spectral profile at 303.396 nm for In and 403.298 nm for Ga has clearly indicated that the determination of Ga and In at lower concentrations will be affected by the presence of significant amounts of residual Pu in the aqueous phase due to spectral interference. These elements can be determined from ppm to % levels by proper dilution with 1 M HNO 3 and appropriate (100 mg and 1 g) sample size. The analytical range obtained for Ga and In was 0.1-1000 µg/mL and 0.05-500 µg/mL respectively by ICP-AES. Synthetic samples of plutonium containing indium and gallium in the range of 50-20 000 ppm were analyzed.

ICP-AES determination of trace metallic constituents in thorium matrix after preferential extraction of thorium using TBP, TOPO and DHOA: a comparative study

“…Tri-n-butyl phosphate (TBP) is known as work-horse for nuclear industries in Plutonium Uranium Reduction Extraction (PUREX) process and its analytical applications [22][23][24][25]. Cyanex 923 has also been utilized for preferential extraction of thorium for the determination of trace analytes [26].…”

Characterization of wastes pertaining to naturally occurring radioactive materials (NORM) and the nuclear fuel cycle

“…Determination of the concentration of gallium (Ga) metal in Pu-bearing nuclear materials is recognized as an important analytical parameter of interest to the nuclear power industry and for nuclear forensic analysis of materials. 5,[52][53][54][55][56][57] For nuclear forensic analysis of suspect plutoniumcontaining materials, the value of this parameter arises from the use of Ga as an alloy constituent to impart properties to Pu metal that render the material suitable for fabrication of preciselyengineered weapons related devices. 5 For example, so-called Pu "pits" originating from the Manhattan project in the United States, were alloyed with Ga metal primarily to stabilize the δphase crystal-structure of Pu metal.…”

“…Previous method development for the analysis of actinides and metal impurities in Pu materials by ion-exchange combined with mass spectrometric techniques in the absence of a yield monitors proved problematic for some metals and for the analysis of U and Th. 55 Previous methods specifically designed for the analysis of stable Ga in these materials have employed radiometric determination of Ga chemical yield using gamma-emitting radionuclide 68 Ga. 52 However, no readily-available commercial source of this radionuclide is available and manufacturing requires reactor facilities with high neutron flux capabilities. 52 In addition, previous methods involved the use of cumbersome liquid-liquid extraction techniques, which can potentially involve large volumes of radioactive organic solvent waste.…”

“…55 Previous methods specifically designed for the analysis of stable Ga in these materials have employed radiometric determination of Ga chemical yield using gamma-emitting radionuclide 68 Ga. 52 However, no readily-available commercial source of this radionuclide is available and manufacturing requires reactor facilities with high neutron flux capabilities. 52 In addition, previous methods involved the use of cumbersome liquid-liquid extraction techniques, which can potentially involve large volumes of radioactive organic solvent waste. 52 On the other hand, the use of positron emitter 68 Ga is on the rise for medical applications and the availability of commercial 68 Ga generators is expanding commercially from several sources.…”

“…52 In addition, previous methods involved the use of cumbersome liquid-liquid extraction techniques, which can potentially involve large volumes of radioactive organic solvent waste. 52 On the other hand, the use of positron emitter 68 Ga is on the rise for medical applications and the availability of commercial 68 Ga generators is expanding commercially from several sources. 19 Thus, 68 Ga is a promising alternative for yield monitoring of the analysis of complex Pu-bearing materials where the chemical yield is required for an accurate determination of stable Ga concentration.…”