• Mass Spectrometry Letters
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• 제8권3호
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• pp.65-68
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• 2017

Thiamethoxam is one of the main suspect in honeybee colony collapse disorder (CCD). Due to this reason, thiamethoxam including imidacloprid and clothianidin has been banned for two years in some Europe countries. The CCD phenomenon has also been reported in Korea. Regarding this issue and needs, a new project has started to develop the method for the quatitation of thiamethoxam using isotope dilution mass spectrometry (IDMS). In the process of optimization for the IDMS method with thiamethoxam and $thiamethoxam-d_3$, we observed that the fragment peaks did not correspond to the fragmentation pathway as published elsewhere. Here, we proposed a candidate fragmentation pathway. To validate the proposed fragmentation pathway, another isotope analogue, $thiamethoxam-d_4$, was introduced and the MS/MS spectra of both isotope analogues were compared. In addition, the MS/MS/MS spectra of thiamethoxam were inspected for more evidence of the candidate pathway. Those spectra indicated that the proposed fragmentation pathway could be used to assign the fragment peaks of thiamethoxam.

• Mass Spectrometry Letters
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• 제3권2호
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• pp.58-61
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• 2012

A method based on flow injection-isotope dilution-cold vapor-inductively coupled plasma mass spectrometry (FI-IDCV-ICP/MS) has been applied to determine trace level of mercury in fly ash. $^{200}Hg$ isotopic spike was added to 0.25 g of BCR176R fly ash and then decomposed by microwave digestion procedure with acid mixture A (8 mL $HNO_3$ + 2 mL HCl + 2 mL HF) and acid mixture B (8 mL $HNO_3$ + 2 mL $HClO_4$ + 2 mL HF) for applying IDMS. Mercury cold vapor was generated by using reductant solution of 0.2% (w/w) $NaBH_4$ and 0.05% (w/w) NaOH. The measurements of n($^{200}Hg$)/n($^{202}Hg$) isotope ratio was made using a quadrupole ICP/MS system. The accuracy in this method was verified by the analysis of certified reference material (CRM) of fly ash (BCR 176R). The indicative value of Hg in BCR 176R fly ash was $1.60{\pm}0.23$ mg/kg (k = 2). The determined values of Hg in BCR 176R fly ash by the method of FI-CV-ID-ICP/MS described in this paper were $1.60{\pm}0.24$ mg/kg (k = 3.18) and the analysis results were in well agreement with the indicative value within the range of uncertainty.

• 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.

• 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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• 제16권1호
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• pp.82-89
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• 2003

Isotope dilution mass spectrometry (IDMS) was applied to the determination of Ni, Cr, Mo in low alloy steel reference materials. The Mo isotope ratio measurement was performed by dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP/MS) using ammonia as a reaction cell gas. In the case of Ni and Cr measurement, all data were obtained at medium resolution mode (m/${\Delta}m=3000$) of double focusing sector field high resolution inductively coupled plasma mass spectrometry (HR-ICP/MS). For the method validation of the technique was assessed using the certified reference materials such as NIST SRM 361, NIST SRM 362, NIST SRM 363, NIST SRM 364, NIST SRM 36b. This method was applied to the determination of Ni, Cr and Mo in low alloy steel sample (CCQM-P25) provided by NMIJ for international comparison study.

• 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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• 제14권6호
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• pp.696-700
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• 1993

Gold bonding wire of 0.076 mm in diameter used in semiconductor industry, is dissoved in aqua regia. The solution is then evaporated to near dryness several times with a few drops of HCl added to prepare the final sample solution in 5% HCl. The gold matrix is separated from trace impurities by controlled potential deposition. The whole electrolysis has been carried out inside a clean bench. An optimum potential is found to be +0.25 V to give more than 99.9% Au matrix removal with better than 90 analytes remaining in the electrolyte solution. Isotope dilution calibration is employed to get the best accuracy and precision. Analytical results are presented with determination limits of the analytical method.

• Bulletin of the Korean Chemical Society
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• 제20권8호
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• pp.910-916
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• 1999

A current interest in chemistry concerns traceability of analytical measurements to the International System of Units (SI) and the proper estimation of their uncertainties in accordance with the internationally agreed guide provided by the International Organization for Standardization (ISO). Isotope dilution mass spectrometry (IDMS) is regarded as a primary method, which make the measurement results traceable to SI units without significant empirical correction factors. Our laboratory, as the national standards institute of Korea, participated in an intercomparison of environmental analysis, pp'-DDE in corn oil, which was organized by the CCQM under supervision of the CIPM to test feasibility of IDMS as a primary method for the trace analysis of organic compounds. In this report, we provide basic equations used for the calculation of the concentration of the analyte in a sample and a precise description of the processes for the evaluation of the uncertainties of the measurement results. Also, we report the experimental conditions adopted to improve the accuracy of the IDMS measurement. The principles contained in ？？Guide to the Expression of Uncertainty in Measurement'' provided by ISO are followed for the uncertainty evaluation.

• Nuclear Engineering and Technology
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• 제52권12호
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• pp.2867-2873
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• 2020

In reprocessed uranium, derived from an impoverished fuel of light-water moderated reactors, there are isotopes of ^{232, 234, 236}U, which make its recycling remarkably difficult. A method of concentration of ²³⁵U target isotope in cascade's additional product was proposed to recover the isotopic composition of reprocessed uranium. A general calculation procedure is presented and a parameters' optimization of multi-flow cascades with additional products. For the first time a numeric model of a cascade that uses the cuts of partial flows of stages with relatively high separation factors was applied in this procedure. A novel computing experiment is carried out on separation of reprocessed uranium hexafluoride with providing a high concentration of ²³⁵U in cascade's additional product with subsequent dilution. The parameters of cascades' stages are determined so as to allow reducing the ^{232, 234, 236}U isotope content up to the acceptable. It was demonstrated that the dilution of selected products by the natural waste makes it possible to receive a low enriched uranium hexafluoride that meets the ASTM C996-15 specification for commercial grade.