Standard Test Method for Determination of Uranium or Plutonium Isotopic Composition or Concentration by the Total Evaporation Method Using a Thermal Ionization Mass Spectrometer

1.1 This method describes the determination of the isotopic composition and/or the concentration of uranium and plutonium as nitrate solutions by the thermal ionization mass spectrometric (TIMS) total evaporation method. Purified uranium or plutonium nitrate solutions are loaded onto a degassed metal filament and placed in the mass spectrometer. Under computer control, ion currents are generated by heating of the filament(s). The ion beams are continually measured until the sample is exhausted. The measured ion currents are integrated over the course of the run, and normalized to a reference isotope ion current to yield isotopic ratios.

1.2 In principle, the total evaporation method should yield isotopic ratios that do not require mass bias correction. In practice, some samples may require this bias correction. When compared to the conventional TIMS method, the total evaporation method is approximately two times faster, improves precision from two to four fold, and utilizes smaller sample sizes.

1.3 The total evaporation method may lead to biases in minor isotope ratios due to peak tailing from adjacent major isotopes, depending on sample characteristics. The use of an electron multiplier equipped with an energy filter may eliminate or diminish peak tailing effects. Measurement of instrument abundance sensitivity may be used to ensure that such biases are negligible, or may be used to bias correct minor isotope ratios.

1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.