• Analytical Science and Technology
• /
• v.16 no.2
• /
• pp.117-124
• /
• 2003

Oxygen to metal ratio has been measured by wet and dry chemical analysis to study the properties of sintered $UO_2$ pellets and $U_3O_8$ in the lithium reduction process of spent pressurized water reactor fuels. Uranium dioxide pellets simulated for the spent PWR fuels with burnup values of 20,000~60,000 MWd/MtU were prepared by mixing $UO_2$ powder and oxides of fission product elements, pelleting the powder mixture and sintering it at $1,700^{\circ}C$ under a hydrogen atmosphere. For wet chemical analysis, the simulated spent fuels were dissolved with mixed acid (10 M HCl : 8 M $HNO_3$, 2.5 : 1, v/v) using acid digestion bomb technique. The total amount of uranium and fission products added in the simulated spent fuels were measured using inductively coupled plasma atomic emission spectrometry. Weight change of the simulated fuel during its oxydation was measured by thermogravimetry and then the O/M ratio result was compared to that obtained by wet chemical analysis. Influence of $Mo_{0.4}-Ru_{0.4}-Rh_{0.1}-Pd_{0.1}$, quaternary alloy, on the determination of O/M ratio was investigated.

• Analytical Science and Technology
• /
• v.13 no.4
• /
• pp.446-452
• /
• 2000

The simulated nuclear spent fuel (SIMFUEL) containing the platinum group elements which will not be dissolved in a nitric acid was completely dissolved with a acid digestion bomb. The metallic elements separated in the SIMFUEL were measured by inductively coupled plasma atomic emission spectrometry (ICP-AES). Because the peaks of metallic elements were spectrally interfered by uranium spectrum, uranium and metallic elements were separated by cation exchange resin for Mo, Pd, Rh and Ru and by anion exchange resin for Ba, Ce, La, Nd, Rh, Sr, Y and Zr, respectively. The recovery of Mo, Pd, Rh and Ru after separation by cation exchange chromatography found to be 99-103% and anion exchange separation showed 96.5-107% of recovery except Y with the simulated solution whose concentration was similar to the spent nuclear fuel. The relative standard deviation of this method showed 1.3-6.7% in the SIMFUEL whose concentrations of metallic elements were between several $10^2-10^3$ppm.

• Analytical Science and Technology
• /
• v.12 no.6
• /
• pp.484-489
• /
• 1999

The extraction of trace amounts of Se in volcanic rock was investigated using the hydride generation method and atomic absorption spectrophotometry. The powdered rock, 1.0 g, was decomposed with the mixture of $HClO_4$, $HNO_3$ and HF in an acid digestion bomb at $140^{\circ}C$ for 2 hours. For the reduction of Se(VI) to Se(IV) in the solution, 10 mL of 6 M HCl and 0.2 mL of 1 M KBr were added to the solution and the mixture was heated for 30~45 minutes. $H_2Se$ was produced by adding 3% $NaBH_4$ as a strong reducing agent, extracted by nitrogen gas, and was absorbed twice into $KMnO_4$solution. The contents of Se in the solution were determined by generation/AAS. According to the proposed method, 1.0 ng or more of Se was quantitatively extracted and Se levels of 2.5 ng/g or more in rock samples could be determined. For example, Se in a rhyolite was determined with the precision of $19.5{\pm}1.3ng/g$(95% confidence, n=6).

• Analytical Science and Technology
• /
• v.13 no.3
• /
• pp.291-296
• /
• 2000

The SIMFUEL which composition is similar to PWR nuclear spent fuels was dissolved with a acid digestion bomb. An analytical conditions of ICP-AES for the direct determination of molybdenum in the uranium matrices without separation process were investigated. Based on the effect of uranium on molybdenum intensity. the most optimum wavelengths of molybdenum were found to be 202.030 and 203.844 nm. However, the method of standard additions is applied to overcome the effects of changing background caused by analyzing the sample solutions containing high concentration of uranium and the standard calibration solutions. The relative error of two methods, direct and indirect measurements with cation exchange resin separation procedures, was less than 5%. Therefore it was possible for this procedure to directly measure molybdenum in uranium matrices without separation. And this method was also applied to the determination of several percent of molybdenum in a U-Mo alloy.