• Title/Summary/Keyword: M-ICP

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INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY FOR THE DETERMINATION OF 237Np IN SPENT NUCLEAR FUEL SAMPLES BY ISOTOPE DILUTION METHOD USING 239Np AS A SPIKE

  • Joe, Kihsoo;Han, Sun-Ho;Song, Byung-Chul;Lee, Chang-Heon;Ha, Yeong-Keong;Song, Kyuseok
    • Nuclear Engineering and Technology
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    • v.45 no.3
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    • pp.415-420
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    • 2013
  • A determination method for $^{237}Np$ in spent nuclear fuel samples was developed using an isotope dilution method with $^{239}Np$ as a spike. In this method, inductively coupled plasma mass spectrometry (ICP-MS) was taken for the $^{237}Np$ instead of the previously used alpha spectrometry. $^{237}Np$ and $^{239}Np$ were measured by ICP-MS and gamma spectrometry, respectively. The recovery yield of $^{237}Np$ in synthetic samples was $95.9{\pm}9.7$% (1S, n=4). The $^{237}Np$ contents in the spent fuel samples were 0.15, 0.25, and $1.06{\mu}g/mgU$ and these values were compared with those from ORIGEN-2 code. A fairly good agreement between the measurements (m) and calculations (c) was obtained, giving ratios (m/c) of 0.93, 1.12 and 1.25 for the three PWR spent fuel samples with burnups of 16.7, 19.0, and 55.9 GWd/MtU, respectively.

Comparison of Multi-element Extraction Methods to Determine Available Phosphate and Exchangeable Cations of Korean Soils (토양의 유효태 인산과 치환성 양이온의 다성분동시추출 분석방법 비교)

  • Kim, Myung-Sook;Yang, Jae Eui;Kim, Yoo-hak;Yoon, Jung-Hui;Zhang, Yong-Seon;Kwak, Han-Gang;Ha, Sang-Keon;Hyun, Byung-Keun
    • Korean Journal of Soil Science and Fertilizer
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    • v.42 no.3
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    • pp.192-200
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    • 2009
  • Soil testing is one of the best management practices for sustainable agriculture. Recently, as increasing soil testing needs, simplification of soil analytical procedure has been required. To determine recommendable multi-element extractant, the soil testing results of available phosphate and exchangeable cations between the conventional methods (Lancaster and 1M $NH_4OAc) and multi-element extraction methods such as Mehlich III, Modified Morgan and Kelowna methods were compared. There were highly significant correlation between the conventional methods and multi-element extraction methods (Mehlich III, Modified Morgan and Kelowna) for available phosphate and exchangeable K, Ca, Mg and Na. The coefficients of determination ($R^2) between available phosphate extracted by Lancaster method and multielement extraction methods were in the order of Mehlich III ($0.979^{***}$) > Kelowna ($0.977^{***}$) > Modified(Mod.). Morgan ($0.553^{***}$). For exchangeable cations, there were highly significant correlations between 1M $NH_4OAc method and Mehlich III, Mod. Morgan and Kelowna. However, exchangeable K, Ca and Mg by Mehlich III method were more highly correlated with conventional method than other methods. Therefore, Mehlich III extraction method could be recommended as a single extractant for simultaneous measurement using ICP in the analysis of avaliable phosphate and exchangeable cations.

Determination of La in $U_3Si/Al$ Spent Nuclear Fuel by Ion Chromatography-Inductively Coupled Plasma-Mass Spectrometry (Ion Chromatography-Inductively Coupled Plasma-Mass Spectrometry에 의한 $U_3Si/Al$ 사용후핵연료 중 La의 분리 및 정량)

  • Han, Sun Ho;Choi, Kwang Soon;Kim, Jung Suk;Jeon, Young Shin;Park, Yang Soon;Jee, Kwang Yong;Kim, Won Ho
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.601-607
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    • 2000
  • Lanthanum has been used as one of the burnup monitor in spent nuclear fuel. $U_3Si/Al$ spent nuclear fuel contains small amount of La in high concentration of U and Al. Therefore, chemical separation of La is required to remove matrix elements. At first, ion chromatography (IC) and inductively coupled plasma systems were installed in radiation shielded glove box to handle the radioactive samples. Retention behavior of uranium, aluminum, lanthanum and some interesting fission products (Sr, Zr, Y, Mo, Ru, Pd, Rh, Cs, Ba, Ce, Pr, Nd, Sm, Eu and Cd) was investigated using the CG10 column and ${\alpha}$-HiBA eluent. As all elements were eluted earlier than lanthanum in 0.2 M ${\alpha}$-HiBA eluent, a portion of U and Al was directly passed to waste using a three way valve between the column and the nebulizer. Thus it was possible to determine the lanthanum in a high concentration of U and Al matrix. Retention time of La was about 12 minutes in this separation condition. Optimum range for the determination of La in $U_3Si/Al$ spent nuclear fuel was $1-10{\mu}g/L$ (ppb) with this system and detection limit was $0.25{\mu}g/L$ in case of $200{\mu}L$ of sample volume.

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A Study to Recover Si from End-of-Life Solar Cells using Ultrasonic Cleaning Method (초음파 세척법을 이용한 사용 후 태양광 셀로부터 Si 회수 연구)

  • Lee, Dong-Hun;Go, Min-Seok;Wang, Jei-Pil
    • Resources Recycling
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    • v.30 no.5
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    • pp.38-48
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    • 2021
  • In this study, we determine the optimal process conditions for selectively recovering Si from a solar cell surface by removal of impurities (Al, Zn, Ag, etc.). To selectively recover Si from solar cells, leaching is performed using HCl solution and an ultrasonic cleaner. After leaching, the solar cells are washed using distilled water and dried in an oven. Decompression filtration is performed on the HCl solution, and ICP-OES (Inductively Coupled Plasma Optical Emission spectroscopy) full scan analysis is performed on the filtered solution. Furthermore, XRD (X-ray powder diffraction), XRF (X-ray fluorescence), and ICP-OES are performed on the dried solar cells after crushing, and the purity and recovery rate of Si are obtained. In this experiment, the concentration of acid solution, reaction temperature, reaction time, and ultrasonic intensity are considered as variables. The results show that the optimal process conditions for the selective recovery of Si from the solar cells are as follows: the concentration of acid solution = 3 M HCl, reaction temperature = 60℃, reaction time = 120 min, and ultrasonic intensity = 150 W. Further, the Si purity and recovery rate are 99.85 and 99.24%, respectively.

Optimization for I-129 analytical method of radioactive waste sample using a high-temperature combustion tube furnace (고온연소로를 이용한 방사성 폐기물 내 I-129 정량 분석법 최적화 연구)

  • Chae-yeon, Lee;Jong-Myoung, Lim;Hyuncheol, Kim;Ji-Young, Park;Jin-Hong, Lee
    • Analytical Science and Technology
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    • v.35 no.6
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    • pp.256-266
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    • 2022
  • It is important to determine the concentration of long-lived radionuclides (e.g., 129I) in nuclear waste to ensure safety when handling it. To analyze nuclides in a solid sample (e.g., concrete and soil), it is essential to effectively separate and purify the nuclides of interest in the sample. This study reports the comprehensive efforts made to validate the analytical procedure for 129I detection in solid samples, using a high-temperature combustion furnace. 129I volatilized from the sample collected in 0.01 M HNO3 solution with a reducing agent (e.g., NaHSO3) and was rapidly measured by ICP-MS. Analytical conditions, such as pyrolysis temperature and types of mobile phase gas, catalyst, and trapping solution, were optimized to obtain a high recovery rate of spiked 129I. Finally, the optimized method was applied for the simultaneous analysis of other volatile radionuclides, such as 3H and 14C. The performance test results for the optimized method confirmed that the LSC (for 3H and 14C) and ICP-MS (for 129I) measurements, with the separation of volatile nuclides using a high-temperature combustion furnace, were reliable.

Separation of High Purity Terbium Using Extraction Chromatography (추출 크로마토그래피를 이용한 고순도 테르븀의 분리)

  • Lee, Kwang-Pill;Park, Myoung-Jin;Park, Keung-Shik;Lee, Hueng-Lark;Piao, Zhexiu
    • Analytical Science and Technology
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    • v.12 no.5
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    • pp.370-374
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    • 1999
  • Extraction chromatography was used to scarch optimum separation conditions of terbium. Stationary phase was 2-ethylhexyl-2-ethylhexyl phosphonic acid(HEH[EHP])levextrel (-100~+150 mesh), column size was ${\Phi}20{\times}530mm$ and kept constantly temperature at $50^{\circ}C$, adsorption flow rate of $0.2mL/cm^2{\cdot}min$, elution flow rate of $1.0mL/cm^2{\cdot}min$, column diameter to packing height of 1:15. But to search optimum separation conditions of terbium, it changed the eluent acidity, the loading weight of sample. the composition of sample. In conclusion, acidity was 0.6 N HCl, loading weight of sample was about 5% and composition of sample was $Gd_2O_3(20%)+Tb_4O_7(60%)+Dy_2O_3(20%)$. Moreover purity of separated terbium by ICP-AES analysis was 99.98% in yield of 99.99%.

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Health Risk Assessment of Airborne Toxic Metals in Taejon Third and Fourth Industrial Complexes (대전 3, 4 공단지역의 대기중 독성금속의 인체 위해도 평가)

  • Lee, Jin-Hong;Jang, Mi-Suk;Lim, Joung-Myung;Ku, Bu-Mi
    • Journal of Environmental Impact Assessment
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    • v.9 no.4
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    • pp.271-276
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    • 2000
  • The research centers on the health risk assessment of airborne toxic metals in Taejon third and fourth industrial complexes. Total suspended particulates were collected on glass microfibre filters by high volume air samplers. Fifteen toxic metals including 6 carcinogenic metals were analyzed by ICP-MS and ICP-AES after the pre-treatment of mixed acid extraction. The following results were summarized from the research : 1) the concentrations of TSPs were $17.7{\sim}219.6{\mu}g/m^3$ while the arithmetic mean concentration was $101.7{\mu}g/m^3$; 2) the arithmetic mean concentrations of human carcinogens such as arsenic, hexavalent chromium and nickel subsulfide were 10.22, 6.96 and 6.42 $ng/m^3$, respectively while those of probable human carcinogens such as beryllium, cadmium and lead were 0.13, 3.41, 97.65 $ng/m^3$, respectively; 3) the point risk estimate for the inhalation of carcinogenic metals was $1.5{\times}10^{-4}$, which was much higher than a risk standard of $10^{-5}$; 4) approximately 93% of the cancer risk were to the inhalation of human carcinogens, arsenic and hexavalent chromium, which should be properly managed in Taejon third and fourth industrial complexes.

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Kinetics of the Oxidation of Substituted Benzyl Alcohols with 4-(Dimethylamino)pyridinium Dichromate (4-(Dimethylamino)pyridinium Dichromate를 이용한 치환 벤질 알코올류의 산화반응 속도)

  • Choi, Sun do;Park, Young Cho
    • Applied Chemistry for Engineering
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    • v.16 no.1
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    • pp.153-157
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    • 2005
  • 4-(Dimethylamino)pyridinium dichromate was synthesized by the reaction of 4-(dimethylamino)pyridine with chromium(VI)trioxide in $H_2O$, and characterized by IR, EA and ICP. The oxidation of benzyl alcohol using 4-(dimethylamino)pyridinium dichromate in various solvents showed that the reactivity increased with the increase of the dielectric constant, in the order: cyclohexen < chloroform < acetone < N,N-dimethylformamide. In the presence of hydrochloric acid(HCl), 4-(dimethylamino)pyridinium dichromate oxidized benzyl alcohol and its derivatives ($p-CH_3$, H, m-Br, $m-NO_2$) smoothly in N,N-dimethylformamide. Electron-donating substituents accelerated the reaction, whereas electron-withdrawing groups retarded the reaction. The Hammett reaction constant($\rho$) was -0.70 at 303K. The observed experimental data have been rationalized as follows: the proton transfer occurs after the prior formation of a chromate ester in the rate-determining step.

Determination of Lead in Steels by Hydride generation-Inductively Coupled Plama/Mass Spectrometry (수소화물 발생-유도결합플라스마 질량분석법에 의한 철강 중의 납의 정량)

  • Park, Chang Joon;Song, Sun Jin;Lee, Dong Soo
    • Analytical Science and Technology
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    • v.14 no.5
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    • pp.410-415
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    • 2001
  • An analytical method has been developed which determines lead in steel samples by inductively coupled plasma mass spectrometry (ICP-MS) with sample introduction by the hydride generation. The lead hydride is not stable and requires and oxidant for the oxidation into metastable Pb(IV) before reduction to $PbH_4$ with $NaBH_4$. A study was carried out to find and optimum lead hydride generation condition for a sample solution with more than $1000{\mu}g/mL$ Fe matrix. $K_2Cr_2O_7$ was found to work as an efficient oxidant when more than $10{\mu}g/mL$ Fe matrix was present. Lactic acid was used with the oxidant as a complexing agent of the metastable Pb(IV) to enhance sensitivity. Optimum concentrations of the sample acidity, oxidant and lactic acid were different depending on the matrix concentration. The isotope dilution method was employed for the quantitation of lead. The determined Pb concentrations of the NIST steel SRM 361 and 362 were in good agreement with the certified values within the uncertainty range.

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Color enhancement and characteristics of natural rubies originated in Africa by the hydrothermal treatment method (수열처리법에 의한 아프리카산 천연루비의 색상개선 및 특성평가)

  • Park, Chun-Won
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.15 no.4
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    • pp.145-151
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    • 2005
  • Color enhancement of African rubies with dark red was carried out by the heat treatment and the hydrothermal treatment method respectively. The heat treatment method brought about an adverse effect causing the color to be deteriorated. However, the hydrothermal treatment method enhanced its color and clarity. The hydrothermal treatment conditions for color enhancement of them were as follows: solvent: 0.9M $Na_2CO_3-1M\;K_2CO_3$, temperature: $450^{\circ}C$, duration: 48 hrs, filling: $30\%$, pressure: 375 atm. As the results of characteristics for African rubies obtained under these conditions, it was known that the amount of $Cr^{3+},\;Fe^{3+},\;Ti^{4+}$ was reduced after the hydrothermal treatment from the ICP/MS and XRF analyses. Also, it was found that the red color from the colorimeter analyses was getting lighter. These results were consistent with the PL analysis showing that the intensity of the luminescence peak generated by the electron transition of $Cr^{3+}$ ion became lower after the hydrothermal treatment compared with the non-treated rubies.