In the decommissioning process of nuclear power plants, Ni-59, Ni-63 and Fe-55 present in radioactive waste are crucial radionuclides used as fundamental indicators in determining waste treatment methods. However, due to their low-energy emissions, the chemical separation of these two radionuclides is essential compared to others. Therefore, this study aims to evaluate the suitability of various pre-treatment methods for decommissioning waste materials by conducting characteristic assessments at each chemical separation stage. The goal is to find the most optimized pre-treatment method for the analysis of Ni-59, Ni-63 and Fe-55 in decommissioning waste. The comparative evaluation results confirm that the chemical separation procedures for Fe and Ni are very stable in terms of stepwise recovery rates and the removal of interfering radionuclides. However, decommissioning waste materials, which mainly consist of concrete, metals, etc., possess unique properties, and a significant portion may be low-radioactivity waste suitable for on-site disposal. Considering that the chemical behavior and reaction characteristics may vary at each chemical separation stage depending on the matrix properties of the materials, it is considered necessary to apply cascading chemical separation or develop and apply individual chemical separation methods. This should be done by verifying and validating their effectiveness on actual decommissioning waste materials.

According to the Nuclear Safety and Security Commission (NSSC) Notice No. 2021-26 “Delivery Regulations for the Low- and Intermediate Level Radioactive Waste (LILW)”, the activity of 3H, 14C, 55Fe, 58Co, 60Co, 59Ni, 63Ni, 90Sr, 94Nb, 99Tc, 129I, 137Cs, 144Ce, and gross alpha must be identified. Currently, the scaling factor of the dry active waste (DAW) for LILW is applied as an indirect evaluation method in Korea. The analyses are used the destructive methods and 55Fe, 60Co, 59Ni, 63Ni, 90Sr, 94Nb, 99Tc, and 137Cs, which are classified as nonvolatile nuclides, are separated through sequential separation and then measured by gamma detector, liquid scintillation counter (LSC), alpha/beta total counter (Gas Proportional Counter, GPC), and ICP-MS. We will introduce how to apply the existing nuclide separation method and improve the measurement method to supplement it.

Radioactive wastes that are generated as a result of operating NPPs, contain 63Ni and 59Ni that should be analyzed in accordance with the notice of Nuclear Safety and Security Commission (NSSC) for the acceptance of Korea Radioactive Waste Agency (KORAD). Analyzing 63Ni and 59Ni has few challenges to determine activities of each nuclide in radioactive waste sample that contains both nuclides. As is well known, 63Ni can be analyzed by liquid scintillation counter (LSC) detecting its emitted beta rays, however, beta rays emitted from 59Ni are overlapped on the spectrum. Therefore, to discriminate those two nuclides, spectrum channel should be divided according to its dedicating part of the spectrum. For instance, 59Ni contribute to spectrum channel 30–250, on the other hand, 63Ni contributes to spectrum channel 30–450. In other word, 63Ni solely can be analyzed on the channel from 260 to 450. To analyze both 63Ni and 59Ni using this channel division method, detection efficiency must be measured in advance; efficiency of 63Ni and 59Ni at ch. 30–250, and efficiency of 63Ni at ch. 260–450, then the activity can be calculated using the corresponding efficiency. In this study, for verifying the feasibility of channel division method, 5 simulated samples were prepared with different ratio of 63Ni/59Ni. The ratio varies as 1, 2, 10, 20 and 100 spiking standard source of 63Ni and 59Ni. Each sample was mixed with scintillation cocktail and detected for 90 minutes by LSC (300SL, Hidex) after the stabilization of solutions. As a result, calculated 63Ni activities for all sample were averaged as 97% of spiked activity. However, calculated 59Ni activity were 101%, 103%, 128%, 140%, 260%, respectively. The result indicates that 59Ni cannot be discriminated by channel division method when it exists in the sample with high 63Ni over 10 times then 59Ni such as radioactive waste sample. However, the results also show that the channel division method for analyzing 63Ni activity was successful verifying it can determine the activity of 63Ni regardless of the affect of 59Ni on the spectrum.

방사성 폐기물 핵종 재고량 평가에 필요한 핵종분석을 위하여 다양한 매질의 방사성 폐기물 시료로부터 및 의 분리에 관한 연구가 수행되고 있다. Ni은 음이온교환 수지와 Sr-Spec 추출 크로마토그래피 수지로 Re(의 대용물), Nb, Fe 및 Sr을 차례로 분리하는 과정에서 Ca, Mg, Al, Cr, Ti, Mn, Ce, Na, K 및 Cu와 함께 회수되었다. 본 연구에서는 Ni의 선택적 분리기술을 확립하기 위하여 Ni-Spec 추출 크로마토그래피 및 양이온교환수지법으로 이들의 분리거동을 비교하였다. 또한 Ni의 정제와 기체비례계수법으로 방사능을 측정하기에 적합한 계측시료 준비를 위하여 ammonium 및 tartaric 에서 dimethylglyoxime(DMG)에 의한 Ni의 침전거동을 조사하였다 원자력발전소로부터 채취한 폐이온교환수지 시료 용해용액의 화학조성을 모사하여 만든 모의 폐이온교환수지 용액을 사용하여 Re, Nb, Fe 및 Sr 분리과정을 거쳐 최종적으로 분리한 Ni의 회수율은 이었다. 또한 tartaric 에서 DMG에 의한 Ni의 회수율은 이었다.