• Title/Summary/Keyword: 크로마토그래피-유도결합 플라스마

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Rare Earth Element Analysis with Chromatography-Inductively Coupled Plasma Atomic Emission Spectrometry and the Comparison of Cross Flow and Ultrasonic Nebulizers (크로마토그래피-유도 결합 플라스마 원자방출 분광법을 이용한 희토류 원소들의 연속적 분석 및 직교형과 초음파분무기의 비교)

Direct Determination of Tellurium in Simulated Nuclear Spent Fuels by Hydride Generation-Inductively Coupled Plasma Atomic Emission Spectrometry (수소화물 생성-유도결합플라스마 원자방출분광법을 이용한 모의사용후 핵연료 중의 텔루르 분석)

  • Choi, Kwang Soon;Lee, Chang Heon;Han, Sun Ho;Joe, Kih Soo;Kim, Won Ho
    • Analytical Science and Technology
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    • v.13 no.6
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    • pp.781-788
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    • 2000
  • Tellurium in simulated nuclear spent fuels (SIMFUEL) has been determined by hydride generation-inductively coupled plasma atomic emission spectrometry (HG-ICP-AES). Parameters such as concentrations of HCl and $NaBH_4$, flow rate of HCl and $NaBH_4$ were optimized and then the effects of U, Mo, Pd, Rh and Ru on the Te intensity were investigated. A thiourea as a masking agent was used to eliminate or minimize such interferences specially caused by palladium. Tellurium was measured by HG-ICP-AES and ICP-MS after separation of tellurium from SIMFUEL with cation exchange chromatography. The relative deviation between direct measurement and separation method was less than 6% based on the data by ICP-MS.

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Extraction Chromatographic Separation of Technetium-99 from Spent Nuclear Fuels for Its Determination by Inductively Coupled Plasma-Mass Spectrometry (유도결합플라스마 질량분석을 위한 사용후핵연료 중 테크네튬-99의 추출크로마토그래피 분리)

  • Suh, Moo-Yul;Lee, Chang-Heon;Han, Sun-Ho;Park, Yeong-Jae;Jee, Kwang-Yong;Kim, Won-Ho
    • Analytical Science and Technology
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    • v.17 no.5
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    • pp.438-442
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    • 2004
  • To determine the contents of $^{99}Tc$ in the spent PWR (pressurized water reactor) nuclear fuels by ICP-MS (inductively coupled plasma-mass spectrometry), a technetium separation method using an extraction chromatographic resin (TEVA Spec resin) has been established. $^{99}Tc$ was separated from a spent PWR nuclear fuel solution by this separation procedure and its concentration was determined by ICP-MS. The result agrees well with the value calculated by the program ORIGEN 2 and also the value measured by AG MP-1 resin/ICP-MS method described in our previous paper. It can be concluded that the present separation procedure is superior to the AG MP-1 resin procedure with respect to the time required for technetium separation as well as the efficiency of decontamination from other radioactive nuclides.

Determination of Fission Products in Simulated Nuclear Spent Fuels by Cation.Anion Exchange Chromatography and Inductively Coupled Plasma Atomic Emission Spectrometry (양.음이온교환 크로마토그래피와 유도결합플라스마 원자방출분광법을 이용한 모의 사용후핵연료 중 핵분열생성물 분석)

  • Choi, Kwang Soon;Sohn, Se Chul;Pyo, Hyung Yeol;Suh, Moo Yul;Kim, Do Yang;Park, Yang Soon;Jee, Kwang Yong
    • Analytical Science and Technology
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    • v.13 no.4
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    • pp.446-452
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    • 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.

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Separation of Fission Product Elements from Synthetic Dissolver Solutions of Spent Pressurized Water Reactor Fuels by $TBP/XAD-16/HNO_3$Extraction Chromatography ($TBP/XAD-16/HNO_3$추출 크로마토그래피에 의한 모의 사용후핵연료 용해용액 중 미량 핵분열생성물 원소의 분리)

  • Lee, Chang Heon;Choi, Kwang Soon;Kim, Jung Suk;Choi, Ke Chon;Jee, Kwang Yong;Kim, Won Ho
    • Journal of the Korean Chemical Society
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    • v.45 no.4
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    • pp.304-311
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    • 2001
  • A study has been carried out on the extraction chromatographic separation of fission products from spent pressurized water reactor (PWR) fuels for inductively coupled plasma atomic emission spectrometric analysis. Impregnation capacity of tri-n-butyl phosphate (TBP), which is well known as an extractant in the field of uranium separation from various nuclear grade materials, on Amberlite XAD polymeric macroporous support materials was measured. Amberlite XAD-16 of which the surface area is the highest was selected as a support material because its TBP impregnation capacity was the largest in Amberlite XADs. Sorption behaviour of this TBP impregnated resin was investigated for the fission product elements using acidic solutions simulated for dissolver solutions of spent PWR fuels. The parameters affecting the performance of the separation system were optimized. The fission product elements studied excluding Pd and Ru were quantitatively recovered with the precision of less than 3.1%.

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Determination of the Trace Elements in $UO_2$ Powder by ICP-AES Directyl Coupled with Extraction Chromatography (추출크로마토그래피와 유도결합플라스마 원자방출분광법을 이용한 이산화우라늄분말 중 미량금속불순물 분석)

  • Choi, Kwang-Soon;Lee, Chang-Heon;Pyo, Hyung-Yeal;Han, Sun-Ho;Suh, Moo-Yul;Eom, Tae-Yoon;Lee, Gae-Ho
    • Journal of the Korean Chemical Society
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    • v.37 no.9
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    • pp.813-819
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    • 1993
  • An ICP-AES system directly connected with a separation column was used in order to determine the trace elements in $UO_2$ powder promptly and reduce the volume of the waste solution. The outlet of a separation column, which was filled with Teflon powder ($330\;{\mu}m$) coated with tri-n-butyl phosphate (TBP) as extractant, was directly connected with sample injection tube of ICP-AES. Eleven elements including molybdenum in $UO_2$ powder were separated and determined simultaneously. Recoveries of these elements were $91{\sim}110%$ and these results were agreed with those of solvent extraction methods. This method was applicable to quality control in manufacturing nuclear fuel.

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Sonication in the Analysis of Hexavalent Chromium in Welding Fume (초음파 전처리에 의한 용접 흄 중 6가 크롬의 분석)

  • Yoon, Chung-Sik;Paik, Nam-Won;Kim, Jeong-Han;Park, Dong-Uk;Choi, Sang-Jun;Kim, Shin-Bum;Chae, Hyun-Byung
    • Analytical Science and Technology
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    • v.12 no.5
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    • pp.447-459
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    • 1999
  • A study was conducted to compare three analytical methods for determination of hexavalent chromium in the welding fume. Precision and accuracy arc documented for colorimetric, ion chromatographic, and inductively coupled plasma-optical emission spectroscopic method. Evidence is presented that welding fume can affect the oxidation of trivalent chromium. A simple sonication extraction method, proposed in this study, instead of hot alkaline extraction has the advantage of minimizing the potential for chromium oxidation.

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Quantification of seleno proteins in Korean blood serum using solid phase extraction and affinity chromatography-inductively coupled plasma/mass spectrometry (고체상 추출과 친화 크로마토 그라피-유도결합 플라즈마 질량분석법을 이용한 한국인 혈청에서의 셀레노 단백질 정량)

  • Ahn, Ji-Yun;Kwon, Hyo-Sik;Pak, Yong-Nam
    • Analytical Science and Technology
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    • v.27 no.2
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    • pp.92-99
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    • 2014
  • Interferences were removed using anion exchange solid phase extraction (AE SPE) in quantification of selenoproteins in Korean human blood serum with affinity high performance liquid chromatography (AF HPLC)-inductively coupled plasma/mass spectrometry (ICP/MS). The average selenium level obtained for healthy Koreans was $94.3{\pm}2.3ngg^{-1}$ using isotope dilution method. AE SPE was coupled to AF column to separate 3 selenoproteins, glutathione peroxidase GPx, selenoprotein SelP, and selenoalbumin SeAlb. Post column isotope dilution was employed to quantify the proteins. The certified reference material of human blood serum BCR-637 was analyzed to give total selenoprotein concentration of $85.4{\pm}3.4ngg^{-1}$, which agreed well with the reference value of $81{\pm}7ngg^{-1}$. The pooled concentration of GPx, SelP, and SeAlb from healthy Koreans (n=20) was $12.1{\pm}1.4ngg^{-1}$, $57.2{\pm}2.0ngg^{-1}$, and $20.0{\pm}1.9ngg^{-1}$, respectively. The sum of selenoproteins is $89.3ngg^{-1}$, which is about the same as the total selenium concentration of $94.3ngg^{-1}$. The fact suggests that selenium in blood serum is mostly consisted of selenoproteins. After the removal of interference, GPx showed a significant decrease (more than 50%) from $25.0ngg^{-1}$ to $12.1ngg^{-1}$. It was identified that the interference in blood serum was mostly from GPx and the use of AE SPE was proven to be efficient in eliminating Cl and Br that cause interference to GPx.

The measurement of oxygen and metal ratio of simulated spent fuels by wet and dry chemical analysis (습식 및 건식법에 의한 모의 사용후핵연료의 O/M비 측정)

  • Choi, Ke Chon;Lee, Chang Heon;Kim, Won Ho
    • Analytical Science and Technology
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    • v.16 no.2
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    • pp.117-124
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    • 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.