ASTM C1672-07(2014)

5.1 The total evaporation method is used to measure the isotopic composition of uranium and plutonium materials, and may be used to measure the elemental concentrations of the two elements when employing the IDMS technique.

5.2 Uranium and plutonium compounds are used as nuclear reactor fuels. In order to be suitable for use as a nuclear fuel the starting material must meet certain specifications, such as found in Specifications C757, C833, C753, C776, C787, C967, C996, C1008, or as specified by the purchaser. The uranium and/or plutonium concentration and isotopic abundances are measured by mass spectrometry following this method.

5.3 The total evaporation method allows for a wide range of sample loading with no loss in precision or accuracy, and is also suitable for trace-level loadings with consequent loss of precision. Typical uranium analyses are conducted using sample loadings between 10 nanograms and several micrograms. Plutonium analyses are generally conducted using between five and 200 nanograms of plutonium per filament. The total evaporation method and modern instrumentation allow for the measurement of minor isotopes using ion counting detectors, while the major isotopes are simultaneously measured using Faraday cup detectors.

5.4 New generations of miniaturized ion counters now allow extremely small samples, in the picogram to femtogram range, to be measured via total evaporation methods. The method may be employed for measuring environmental or safeguards inspection samples containing very small quantities of uranium or plutonium. Very small loadings require special sample handling and analysis techniques, and careful evaluation of measurement uncertainty contributors.

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.