• Analytical Science and Technology
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• v.8 no.4
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• pp.427-434
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• 1995

Inductively coupled plasma mass spectrometry combined with the isotope dilution method is used for the determination of lithium. The isotope dilution method is based on the addition of a known amount of enriched isotope (spike) to a sample. The analyte concentration is obtained by measuring the altered isotope ratio. The spike solution is calibrated through so called reverse isotope dilution with a primary standard. The spike calibration is an important step to minimize error in the determined concentration. It has been found essential to add spike to a sample and the primary standard so that the two isotope ratios should be as dose as possible. Since lithium is neither corrosive nor toxic, lithium is used as a chemical tracer in the nuclear power plants to measure feedwater flow rate. 99.9% $^7Li$ was injected into a feedwater line of an experimental system and sample were taken downstream to be spiked with 95% $^6Li$ for the isotope dilution measurements. Effects of uncertainties in the spike enrichment and isotope ratio measurement error at various spike-to-sample ratios are presented together with the flow rate measurement results in comparison with a vortex flow meter.

• Analytical Science and Technology
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• v.13 no.6
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• pp.789-801
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• 2000

This analysis was conducted for PCDDs/PCDFs in sediment by isotope dilution HRGC/HRMS method. From the result, the mean recovery of surrogate standard was in the range of 70.1-80.8%. Among the distribution of 2, 3, 7, 8-substituted isomers, the concentration of OCDD represented almost 40.6-78.5% of total concentration and that of OCDF showed 6.6-14.7% and 1, 2, 3, 4, 6, 7, 8-HpCDD showed 5.1-7.7%. The portion of PCDDs represented 62.4-86.9% of total PCDDs/PCDFs. In the TEQ concentration 1, 2, 3, 4, 7, 8-PeCDF concentration represented 22.7-35.6 % of total TEQ concentration.

• Bulletin of the Korean Chemical Society
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• v.23 no.11
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• pp.1541-1544
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• 2002

The concentration of B in steels is important due to its influence on mechanical properties of steel such as hardenability, hot workability, and creep resistance. An analytical method has been developed to determine B in steel samples by high-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS). National Institute of Standard and Technology Standard Reference Material (NIST SRM) 348a was analyzed to validate the analytical method. The steel sample was digested in a centrifuge bottle with addition of aqua regia and $^{10}B$ spike isotope. Sample pH was then adjusted to higher than 10 to precipitate most matrix elements such as Fe, Cr, and Ni. After centrifugation, the supernatant solution was passed through a cation exchange column to enhance the matrix separation efficiency. B recovery efficiency was about 37%, while matrix removal efficiency was higher than 99.9% for major matrix elements. The isotope dilution method was used for quantification and the determined B concentration was in good agreement with the certified value.

• Mass Spectrometry Letters
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• v.2 no.2
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• pp.37-40
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• 2011

Saccharin is a commonly used artificial sweetener in foodstuffs. However, for its carcinogenic dispute, it has been regulated by government bodies. In this study, isotope dilution mass spectrometry (ID-MS) was introduced for the accurate quantification of saccharin. To employ ID-LC/MS, we obtained its isotope analogue, $^{13}C_1$-sodium saccharin, by customized synthesis. Samples were spiked with $^{13}C_1$-sodium saccharin and analyzed with LC/MS in negative mode. Chromatographic conditions were optimized for the adequate chromatographic retention and separation of saccharin with a $C_{18}$ column. MS was operated with electrospray ionization by the selected ion monitoring (SIM) mode of $[M-H]^-$ for saccharin (m/z 182) and $[M-Na]^-$ for its isotope analogue (m/z 183). To validate the ID-LC/MS method for accurate measurement, we prepared a batch of a candidate material by sortifying quasi-tea-drinks with saccharin and analyzed samples gravimetrically fortified in various levels of concentration. The repeatability and reproducibility of this method was tested by analyzing the reference material. Result show that ID-LC/MS is a reliable method for the quantitative analysis of saccharin.

• Analytical Science and Technology
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• v.12 no.6
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• pp.550-557
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• 1999

This Analysis was conducted for 13 toxic-PCBs having TEF value among 209 PCBs isomers in sediment by isotope dilution HRGC/HRMS method. From the result, the recovery of surrogate standard was in the range of 71~99%. The concentration range for 13 toxic-PCBs in sediment was found to be 0.84~2.49 ng/g, among them the concentration levels of 2,2',3,3',4,4',5-HpCB(IUPAC No. 170) and 2,2',3,4,4',5,5'-HpCB(IUPAC No. 180) represented almost 50% of total concentrarion and that of 2,3,4,4,5-PeCB(IUPAC No. 114) showed over 10%. The TEQ concentration levelwas in the range of 0.38~2.63 pg-TEQ/g and 3,3',4,4',5-PeCB(IUPAC No. 126) concentration represented over 50% of total TEQ concentration.

• Bulletin of the Korean Chemical Society
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• v.35 no.12
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• pp.3482-3488
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• 2014

Matrix-induced mass bias and its effect on the accuracy of isotope ratio measurements have been examined for a quadrupole-based inductively coupled plasma-mass spectrometer (Q ICP-MS). Matrix-induced mass bias effect was directly proportional to % mass difference, and its magnitude varied for element and nebulizer flow rate. For a given element and conditions in a day, the effect was consistent. The isotope ratio of Cd106/Cd114 under $200{\mu}g\;g^{-1}$ U matrix deviated from the natural value significantly by 3.5%. When Cd 111 and Cd114 were used for the quantification of Cd with isotope dilution (ID) method, the average of differences between the calculated and measured concentrations was -0.034% for samples without matrix ($0.076{\mu}g\;g^{-1}$ to $0.21{\mu}g\;g^{-1}$ for the period of 6 months). However, the error was as large as 1.5% for samples with $200{\mu}g\;g^{-1}$ U. The error in ID caused by matrix could be larger when larger mass difference isotopes are used.

• Analytical Science and Technology
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• v.16 no.6
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• pp.450-457
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• 2003

The determination of uranium and its isotopes in spent nuclear fuels by isotope dilution mass spectrometry (IDMS) has been studied. The spent fuel samples were dissolved in 8 M $HNO_3$ or its mixture with 14 M $HNO_3-0.05M$ HF. The dissolved solutions were filterred on membrane filter with $1.2{\mu}m$ pore size. The uraniums in the spiked and unspiked sample solutions were quantitatively adsorbed by anion exchange resin, AG 1X8 and eluted with 0.1 M HCl. The contents of uranium and its isotopes ($^{234}U$, $^{235}U$, $^{236}U$ 및 $^{238}U$) in the spent fuel samples were determined by isotope dilution mass spectrometric method using $^{233}U$ as spike. The spike reference solution was standarized by reverse isotope dilution mass spectrometry (R-IDMS) using natural and depleted uranium. The results from IDMS were in average relative difference of 0.34% when compared with those by the potentiometric titration method.

• Mass Spectrometry Letters
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• v.5 no.2
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• pp.52-56
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• 2014

Glycated hemoglobin (HbA1c) is used as an index of mean glycemia over prolonged periods. This study describes an optimization of enzyme digestion conditions for quantification of non-glycated hemoglobin (HbA0) and HbA1c as diagnostic markers of diabetes mellitus. Both HbA0 and HbA1c were quantitatively determined followed by enzyme digestion using isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) with synthesized N-terminal hexapeptides as standards and synthesized isotope labeled hexapeptides as internal standards. Prior to quantification, each peptide was additionally quantified by amino acid composition analysis using ID-LC-MS/MS via acid hydrolysis. Each parameter was considered strictly as a means to improve digestion efficiency and repeatability. Digestion of hemoglobin was optimized when using 100 mM ammonium acetate (pH 4.2) and a Glu-C-to-HbA1c ratio of 1:50 at $37^{\circ}C$ for 20 h. Quantification was satisfactorily reproducible with a 2.6% relative standard deviation. These conditions were recommended for a primary reference method of HbA1c quantification and for the certification of HbA1c reference material.

• Bulletin of the Korean Chemical Society
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• v.29 no.11
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• pp.2125-2128
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• 2008

• Journal of the Korean Chemical Society
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• v.63 no.5
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• pp.387-391
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• 2019