PNNL

Abstract

A rapid new method for determining the U and Th mass concentrations in high radiopurity plastics is described, consisting of 1) dry ashing the plastic sample and tracers in low mass crucibles made of ultra low background electroformed copper (ULB EF-Cu) foil cut and folded into boats, 2) dissolving both the ash and the boat in acid, 3) performing a column separation to remove copper, and 4) determining the elements of interest by isotope dilution mass spectrometry. This method was demonstrated on both unfluorinated and fluorinated plastics, demonstrating high tracer recoveries and detection limits to pg/g (i.e., parts per trillion) levels or below, corresponding to µBq/kg of material. Samples of biomedical polyester (Max-Prene® 955) and a fluoropolymer (polyvinylidene fluoride, PVDF) were analyzed in powder raw material forms as well as solids in the form of pellets or injection molded parts. The polyester powder contained 6 pg/g and 2 pg/g for Th and U respectively. These levels correspond to 25 and 25 µBq/kg radioactivity, respectively. Determinations on samples of PVDF powder were typically below 1 pg/g for Th and 2 pg/g for U, corresponding to 4 and 25 µBq/kg radioactivity, respectively. The use of low mass ULB EF-Cu boats for dry ashing successfully overcame the problem of crucible-generated contaminants in the analysis; absolute detection limits, calculated as 3 × standard deviation of the process blanks, were typically 20-100 fg within a sample set. Complete dissolution of the ash and low mass boat provided high tracer recoveries, and provides a convincing method to recover both the tracer and sample isotopes when full equilibration of tracer isotopes with sample isotopes is not possible prior to beginning chemical sample processing on solids.