• Nuclear Engineering and Technology
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• 제29권4호
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• pp.327-335
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• 1997

The correlation of isotope composition of uranium, plutonium and neodymium with the burnup in M uranium dioxide fuel has been investigated experimentally. The total and fractional($^{235}$ U) burnup were determined by Nd-148 and, U and Pu mass spectrometric method respectively. The isotope compositions of these elements, after their separation from the fuel samples were measured by mass spectrometric. The content of the elements in the irradiated fuel ore determined by isotope dilution mass spectrometric method using $^{233}$ U, $^{242}$ Pu and $^{150}$ Nd as spikes. The content of plutonium in the irradiated fuel was expressed by the correlation with uranium isotopes. The correlations between isotope compositions themselves and the total and fractional burnup ore compared with those calculated from ORIGEN2 code.

• Nuclear Engineering and Technology
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• 제47권7호
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• pp.924-933
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• 2015

The correlation of the isotopic composition of uranium, plutonium, neodymium, and cesium with the burnup for high burnup pressurized water reactor fuels irradiated in nuclear power reactors has been experimentally investigated. The total burnup was determined by Nd-148 and the fractional $^{235}U$ burnup was determined by U and Pu mass spectrometric methods. The isotopic compositions of U, Pu, Nd, and Cs after their separation from the irradiated fuel samples were measured using thermal ionization mass spectrometry. The contents of these elements in the irradiated fuel were determined through an isotope dilution mass spectrometric method using $^{233}U$, $^{242}Pu$, $^{150}Nd$, and $^{133}Cs$ as spikes. The activity ratios of Cs isotopes in the fuel samples were determined using gamma-ray spectrometry. The content of each element and its isotopic compositions in the irradiated fuel were expressed by their correlation with the total and fractional burnup, burnup parameters, and the isotopic compositions of different elements. The results obtained from the experimental methods were compared with those calculated using the ORIGEN-S code.

• Bulletin of the Korean Chemical Society
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• 제30권2호
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• pp.363-367
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• 2009

An isotope-dilution flow-injection electrospray/mass spectrometric method was developed for the accurate determination of glucosamine contents in pharmaceutical formulations. Samples were extracted by methanol. After spiking glucosamine-1-$^{13}C_1$ as an internal standard, the extracts were then analyzed by flow-injection ESI/MS in a selected ion monitoring (SIM) mode to detect [M+H]$^+$ ions of the analyte and its isotope analogue at m/z 180 and m/z 181, respectively. Confirmatory measurements were made by selectively monitoring the collisionally induced dissociation channels of m/z 180 $\rightarrow$ m/z 72 and m/z 181 $\rightarrow$73, respectively, to test the possibility of bias in the SIM method due to matrix interferences, but any significant bias in the SIM mode was not observed. Repeatability and reproducibility studies showed that the flow-injection ESI/MS method is a reliable and reproducible method which can provide a typical method precision of 1.0 %. Other results for the method validation are reported.

• Bulletin of the Korean Chemical Society
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• 제31권12호
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• pp.3663-3667
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• 2010

Acetaminophen (N-acetyl-p-aminophenol) is one of the most popular analgesic and antipyretic drugs. An isotope dilution mass spectrometric method based on LC/MS was developed as a candidate reference method for the accurate determination of acetaminophen in pharmaceutical product. After spiking an isotope labeled acetaminophen (acetyl-$^{13}C_2$, $^{15}N$-acetaminophen) as an internal standard, tablet extracts were analyzed by LC/MS in a selected reaction monitoring (SRM) mode to detect ions at m/z $152{\rightarrow}110$ and m/z $155{\rightarrow}111$ for acetaminophen and acetyl-$^{13}C_2$, $^{15}N$-acetaminophen, respectively. The repeatability and reproducibility of the developed ID/LC-MS method were tested for the validation and assessment of metrological quality of the method.

• 분석과학
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• 제16권6호
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• pp.450-457
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• 2003

사용후핵연료 내 U 및 동위원소 정량분석을 동위원소 희석 질량분석법 (isotope dilution mass spectrometry, IDMS)으로 수행하였다. 시료는 산화우라늄 사용후핵연료 시료를 $HNO_3$(1+1) 또는 이 용액과 14 M $HNO_3-0.05M$ HF 혼합용액으로 용해한 후 막 거르게 ($1.2{\mu}m$)로 여과하여 준비하였다. 시료 및 스파이크를 첨가한 시료 중의 U은 AG lX8 음이온교환 수지관에서 0.1 M HCl 용액으로 용리하였다. 시료 중의 총 U 량과 성분 동위원소 ($^{234}U$, $^{235}U$, $^{236}U$ 및 $^{238}U$)의 조성은 $^{233}U$을 스파이크로 이용하는 동위원소 희석 질량분석법으로 정량하였다. 제조한 U-233 스파이크 용액은 천연 및 감손 U을 이용한 역동위원소 희석 질량분석법 (reverse isotope dilution mass spectrometry, R-IDMS)으로 표정하였다. 동위원소 희석 질량분석법에 의한 핵연료시료 중의 총 U 량 측정결과를 전위차 적정으로 측정한 결과와 비교하였을 때 0.34% 평균 상대오차 범위에서 일치하였다.

• Bulletin of the Korean Chemical Society
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• 제28권5호
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• pp.745-750
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• 2007

An isotope dilution-liquid chromatography/tandem mass spectrometric method was developed as a candidate reference method for the accurate determination of folic acid in infant milk formula. Sample was spiked with 13C5-folic acid and then extracted with phosphate buffer (pH 6) solution. The extract was further cleaned up by deproteinization followed by a C18 solid-phase extraction cartridge. The extract was analyzed by using LC/ ESI/MS/MS with selectively monitoring the collisionally induced dissociation channels of m/z 442 → m/z 295 and m/z 447 → m/z 295, which are the neutral glutamyl loss from the [M+H]+ ions of folic acid and 13C5-folic acid, respectively. LC/MS/MS chromatograms showed substantially reduced background from chemical noises compared to LC/MS chromatograms. Repeatability and reproducibility studies showed that the LC/MS/ MS method is a reliable and reproducible method which can provide less than 1.5 relative percentage of method precision.

• 한국해양학회지:바다
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• 제27권3호
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• pp.144-157
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• 2022

비활성기체는 화학적, 생물학적 반응을 하지 않는 보존적인 특성을 가지고 있어 해양에서 수온과 염분 변화, 기체 주입, 해수의 혼합과 빙하 융해수의 분포와 같은 물리적인 변화의 추적자로 활용되고 있다. Ne, Ar과 Kr을 정밀하게 분석하기 위해 사중극자 질량 분석기, 고진공 전처리 라인, 초저온 냉각 트랩과 동위원소 표준기체로 구성된 분석 시스템을 제작했다. 고진공 라인은 시료의 용존 기체를 추출하여 동위원소 표준기체와 혼합하는 시료추출부, 합금 물질을 이용하여 반응성 기체를 제거하고 초저온 냉각 트랩으로 비활성기체를 기화점에 따라 분별 증류하는 기체 준비부, 비활성기체를 원소별로 측정하는 기체 측정부로 구성하였다. 기체준비부에 결합한 초저온 냉각 트랩은 질량분석기 내 Ar와 CO₂의 부분압을 현저히 낮추어 Ne 동위원소 분석의 오차를 감소시켰다. 동위원소 표준기체는 ²²Ne, ³⁶Ar과 ⁸⁶Kr를 혼합하여 제작하였고, 혼합 표준 기체의 원소별 양은 대기를 반복 측정하여 역동위원소 희석법으로 결정했다. 대기 평형수 반복 분석의 상대 오차는 Ne, Ar과 Kr에 대해 각각 0.7%, 0.7%, 0.4%이었다. 반복 측정한 대기 평형수의 농도와 포화 농도의 차이로 확인한 분석시스템의 정확도는 Ne, Ar, Kr에 대해 각각 0.5%, 1.0%, 1.7%이었다.

• Nuclear Engineering and Technology
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• 제33권4호
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• pp.375-385
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• 2001

The total burnup in the spent U$_3$Si/Al fuel samples from Hanaro reactor was determined by destructive methods using $^{148}$ Nd, the sum of $^{143}$ Nd and $^{144}$ Nd, the sum of $^{145}$ Nd and $^{146}$ Nd, and the sum of total Nd isotopes($^{143}$ Nd, $^{144}$ Nd, $^{145}$ Nd, $^{146}$ Nd, $^{148}$ Nd and $^{150}$ Nd) monitors. The fractional($^{235}$ U) turnup in the spent fuel samples was also determined by U and Pu mass spectrometric method. The samples were dissolved in a mixture of 4 M HCI and 10 M HNO$_3$ without any catalyst. The separation of U, Pu and Nd from the spiked and unspiked sample solutions was achieved by two sequential anion exchange separation methods. The isotope compositions of these elements, after their separation from the fuel samples were measured by mass spectrometry. The contents of the elements in the spent fuel samples were determined by isotope dilution mass spectrometric method(IDMS) using $^{233}$ U, $^{242}$ Pu and $^{150}$ Nd as spikes. The effective fission yield was calculated from the weighted fission yields averaged over the irradiation period. The difference between total turnup values determined by various Nd monitors were in the range of 1.8%.

• Nuclear Engineering and Technology
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• 제38권3호
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• pp.301-310
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• 2006

Destructive methods were used for the burnup determination of U-Zr alloy nuclear fuel irradiated in the High-flux Advanced Neutron Application Reactor (HANARO) at KAERI. The dissolution rate of unirradiated U-Zr alloy fuel in $HNO_3$/HF mixtures was investigated for the experimental conditions of a different temperature, and initial concentrations of HF and $HNO_3$. The irradiated U-Zr alloy fuel specimen was dissolved in a mixed acid condition of 3 M HNO3 and 1 M HF at $90^{\circ}C$ for 8 hours under reflux. The total burnup was determined from measurement of the Nd isotope burnup monitors. The method includes U, Pu, $^{148}Nd,\;^P{145}Nd+^{146}Nd,\;^{144}Nd+^{143}Nd$ and total Nd isotopes determination by the isotope dilution mass spectrometric method (IDMS) using triple spikes $(^{233}U,\;^{242}Pu\;and\;^{150}Nd)$. The effective fission yield was calculated from the weighted fission yields averaged over the irradiation period. The results are compared with that obtained by the destructive -spectrometric measurement of the $^{137}Cs$ monitor.

• Bulletin of the Korean Chemical Society
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• 제28권5호
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• pp.737-744
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• 2007

An isotope dilution-liquid chromatography/tandem mass spectrometric method was developed as a candidate reference method for the accurate determination of acrylamide in potato chips, starch-rich foodstuff cooked at high temperature. Sample was spiked with 13C3-acrylamide and then extracted with water. The extract was further cleaned up with an Oasis HLB solid-phase extraction (SPE) cartridge and an Oasis mixed-phase cation exchange (MCX) SPE cartridge. The extract was analyzed by using LC/ESI/Tandem MS in positive ion mode. LC with a medium reversed-phase (C4) column was optimized to obtain adequate chromatographic retention and separation of acrylamide. MS was operated to selectively monitor [M+H]+ ions of the analyte and its isotope analogue at m/z 72 and m/z 75, respectively. Sample was also analyzed by the LC/MS with selectively monitoring the collisionally induced dissociation channels of m/z 72 → m/z 55 and m/z 75 → 58. Compared to the LC/MS chromatograms, the LC/MS/MS chromatograms showed substantially reduced background chemical noises coming from solvent clusters formed during ESI spray processes and interferences from sample matrix. Repeatability and reproducibility studies showed that the LC/MS/MS method is a reliable and reproducible method which can provide a typical method precision of 1.0% while the LC/MS results are influenced by chemical interferences.