• Analytical Science and Technology
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• v.29 no.4
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• pp.170-178
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• 2016

Accuracy and precision of ID methods for different spike isotopes of ⁷⁶Se, ⁷⁷Se, and ⁷⁸Se were compared for the analysis of Selenium using quadrupole ICP/MS equipped with Octopole reaction cell. From the analysis of Se inorganic standard solution, all of three spikes showed less than 1 % error and 1 % RSD for both short-term (a day) and long-term (several months) periods. They showed similar results with each other and ⁷⁸Se showed was a bit better than ⁷⁶Se and ⁷⁷Se. However, different spikes showed different results when NIST SRM 1568a and SRM 2967 were analyzed because of the several interferences on the m/z measured and calculated. Interferences due to the generation of SeH from ORC was considered as well as As and Br in matrix. The results showed similar accuracy and precisions against SRM 1568a, which has a simple background matrix, for all three spikes and the recovery rate was about 80% with steadiness. The %RSD was a bit higher than inorganic standard (1.8 %, 8.6 %, and 6.3 % for ⁷⁸Se, ⁷⁶Se and ⁷⁷Se, respectively) but low enough to conclude that this experiment is reliable. However, mussel tissue has a complex matrix showed inaccurate results in case of ⁷⁸Se isotope spike (over 100 % RSD). ⁷⁶Se and ⁷⁷Se showd relatively good results of around 98.6 % and 104.2 % recovery rate. The errors were less than 5 % but the precision was a bit higher value of 15 % RSD. This clearly shows that Br interferences are so large that a simple mathematical calibration is not enough for a complex-matrixed sample. In conclusion, all three spikes show similar results when matrix is simple. However, ⁷⁸Se should be avoided when large amount of Br exists in matrix. Either ⁷⁶Se or ⁷⁷Se would provide accurate results.

• Analytical Science and Technology
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• v.25 no.1
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• pp.25-32
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• 2012

Isotope dilution mass spectrometry (ID-MS) based on liquid chromatography tandem mass spectrometry (LC/MS/MS) was developed for the accurate determination of sorbic acid in tea-drink. An isotope analogue of sorbic acid, $^{13}C_2$-sorbic acid, was obtained by custom synthesis. MS was operated in the negative mode with selected reaction monitoring (SRM) mode of $[M-H]^-$ ${\rightarrow}$ $[M-CO_2H]^-$ channel at m/z 111 ${\rightarrow}$ 67 for sorbic acid and at m/z 113 ${\rightarrow}$ 68 for its isotope analogue. Chromatographic separation was accomplished with a C18 column and an isocratic mobile phase of 55% of 50 mM ammonium acetate (pH 4.5) and 45% of methanol. Homogeneous reference materials were prepared for validation of this method, including repeatability and reproducibility tests, by fortifying tea-drink with sorbic acid in our laboratory. Repeatability and reproducibility studies showed that the ID-LC/MS method is a reliable and reproducible method which provides less than 3.8% of relative standard deviation (RSD) for the analysis of sorbic acid.

• Journal of the Korean Chemical Society
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• v.37 no.9
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• pp.800-805
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• 1993

An analytical method has been developed to determine trace elements in biological samples. The biological samples are added to a laboratory-bulit Teflon bomb together with nitric acid-hydrogen peroxide mixture and enriched stable isotopes. The samples are decomposed in a microwave oven. The decomposed sample solutions are analyzed by isotope dilution inductively coupled plasma mass spectrometry. The analytical results of the biological samples agree well with the reference values.

• The Korean Journal of Zoology
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• v.3 no.1
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• pp.24-30
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• 1960

본실험의 목적은 탄산기에 방사성동위원소 C14를 표식한 sodium acetate ($CH_3$C14 OONA)를 사용하여 염소의 위내에 존재하는 acetate 의 위벽으로부터의 흡수율과 위의 acetate의 평균함량을 측정하는데 있다. C14 로 표식된 sodium acetate(specific activity 1.35$\times$108 cpm./g.)를 급사 3 시간후의 염소의 위내에 주입하고 주입 2분후부터 약 2분간격으로 위 내용물을 추울하여 column chromatograpy를 이용하여 acetate를 분리정량한 후 그의 specific activity를 측정하였다. 주입후 3 분경까지는 위내에 존재하는 acetate에 의한 표식 acetate의 희석으로 말미암아 specific activity 는 급격히 감소되어 갔고 3 분후부터는 감소도가 비교적 완만하였으나 역시 계속적으로 감소되어갔다. 희석완료후의 이 specific activity 감소는 위벽을 통한 acetate를 흡수와 위 내용물로부터의 acetate 생성으로 인한 것으로서, 이 감소율로부터 acetate의 위벽흡수속도를 추정할 수 있다. 상기 specific activity의 감소 graph 로부터 추정된 위내 acetate의 량은 본실험의 제조건하에서 약 30 g이었으며 위내 acetate 의 specific activity가 1/2 로 감소되는데 요하는 평균 시간은 약 4 분이었다. 이는 위내에 존재하는 acetate량의 약 절반은 4 분동안에 위벽을 통과함을 의미한다.

• The Journal of the Petrological Society of Korea
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• v.10 no.3
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• pp.172-178
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• 2001

K-Ar dating system of Korea Basic Science Institute (KBSI) was installed in 1997 and has been used since then. The system consists of high temperature graphite furnace, gas purification system, and mass spectrometer with data acquisition system. K-Ar age is determined by the measurement of the concentrations of Ar and K through isotope dilution method using $^{38}Ar$ as spike and flame spectroscopy, respectively. The accuracy and reliability for the K-Ar age are checked using the several K-Ar standard materials. Although the exact age determination for young samples of less than 1 Ma is hampered by small fluctuations of sensitivity and mass discrimination, the present system yields the reliable K-Ar age compared to the standard materials of Tertiary and Mesozoic age. The measurements for the SORI93 biotite with the recommended K-Ar age of $92.6\pm$0.6 Ma and Bern4M muscovite of $18.5\pm$0.6 Ma yield the reliable age of $92.1\pm$1.1 Ma and $17.8\pm$0.2 Ma, respectively.

• Proceedings of the Korean Nuclear Society Conference
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• 1995.05b
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• pp.1047-1051
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• 1995

수소동위원소의 분리공정은 월성원자력발전소의 보충용 중수제조공정에 필수적이며 백금촉매를 이용한 교환반응공정이 가장 경제적인 것으로 알려져 있다. 본고에서는 백금촉매 개발의 일환으로 담체로서 실리카라이트를 제조하여 결정성을 X선 회절분석기를 이용하여 측정하였으며 이 담체에 일반적인 함침법으로 백금을 담지시켜 처리한 Pt/Silicalite 촉매의 백금분산도를 수소 흡착법을 이용하여 측정하였다. 측정실험 결과 다공성의 실리카라이트가 제조되었고 일반적인 함침법에 의해 제조된 촉매의 백금분산도는 매우 낮음을 확인하였다.

• The Journal of the Petrological Society of Korea
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• v.13 no.4
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• pp.238-243
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• 2004

Duwon meteorite was fallen on 23 November 1943 in Duwonmyeon, Goheung, Jeolanam-Do. We measured rare earth element abundance of Duwon meteorite by isotope dilution thermal ion mass spectrometry (ID-TIMS) and ICP-MS. As a result, except La and Ce, abundance of other rare earth element show a correspondence within 10％ of error range. However, La and Ce show more than 70％ in abundance, which is considered due to 1) experimental procedure or 2) inhomogeneity of sample. Leedey meteorite was fallen on 25 November 1943 in Dewey County, Oklahoma, USA. which suggested that fallen difference between Leedey and Duwon meteorites is only 2 days. Leedey and Duwon meteorites are classified as ordinary chondrite of L6 type. In Leedey chondrite-normalized REE pattern, Duwon meteorite shows nearly flattened, which suggests close relationship between Leedey and Duwon meteorites meteoritically or cosmochemically.

• Applied Chemistry for Engineering
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• v.9 no.1
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• pp.121-128
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• 1998

In fields of operating or handling a hydrogen isotope facility, and of the technology for nuclear fusion source management, gas chromatography has been used as one of the practical techniques lot separation and enrichment of hydrogen isotopic gases including tritium. Chromatographic separation experiments of the hydrogen isotope mixture (hydrogen, deuterium and tritium) were carried out by use of a commercially available gas chromatograph. An aliquot of gas sample was injected by a specially designed vacuum sampler into the stream of inert carrier gas which went through the separation column under liquid nitrogen temperature. The complete separation of hydrogen isotopic molecules was observed with an alumina adsorbent partially deactivated by coating with 10% manganese chlorine. In addition, fairly good separation conditions were obtained without any appearance of nuclear spin isomers with shorter retention time, which would be available for the practical applications of the hydrogen isotope separation and enrichment.

• Analytical Science and Technology
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• v.19 no.1
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• pp.1-8
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• 2006

The isotope dilution method was used for the determination of Br impurity in $1000{\mu}g/g$ Cl standard solution. Since relatively pure KCl salt was used for the preparation of the Cl standard solution, the Br impurity determination suffers from both spectral and non-spectral interferences due to the presence of a large amount of K and Cl matrices. AG2-X8 anion-exchange resin was employed to separate the Br analyte from the matrices, and RF power was raised to 1500 W and nebulizer gas flow rate was lowered to 0.77 L/min to reduce background from the $ArArH^+$ molecular ions. The Br impurity in the $1000{\mu}g/g$ Cl standard solution was determined to be 43.7 ng/g with the standard addition method. The analytical result was in good agreement with 41.2 ng/g (RSD 1.6%) determined by the isotope dilution method to lower uncertainty from poor reproducibility of the anion-exchange process.

• Analytical Science and Technology
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• v.31 no.6
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• pp.225-231
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• 2018

Benzoic acid, methyl paraben, and butyl paraben are preservatives that have been used in pharmaceutical, cosmetic, and food products. However, as their toxicities for human have been reported, many nations and organizations including Korea have established a regulation limit for thier usage of these preservatives in food products. The present study developed the isotope dilution liquid chromatography mass spectrometry method for accurate determination of three target preseratives in soysauce. In this study, the isotope dilution liquid chromatography mass spectrometry method was developed for accurate determination of three target preservatives in soy sauce. LC separation was optimized considering the pKa of benzoic acid which is lower than those of methyl and butyl parabens. A C18 column was used with 5 mM ammonium acetate and methanol as mobile phases. Mass spectrometry was operated in negative mode and selected reaction monitoring mode (SRM). Soy sauce sample was cleaned-up with C18 SPE cartridge for removing matrix inferences and color material. Optimized conditions and the method were validated with soy sauce reference materials for the analysis of food preservatives from Health Science Authority in Singapore. The measured values of benzoic acid, methyl and butyl paraben agreed well with reference values within their uncertainties.