• Title, Summary, Keyword: isotope dilution method

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Determination of Li by Isotope Dilution Inductively Coupled Plasma Mass Spectrometry

  • Park, Chang J.;Chung, Bag S.
    • 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.

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Determination of Boron Steel by Isotope-Dilution Inductively Coupled Plasma Mass Spectrometry after Matrix Separation

  • Park, Chang-J.
    • 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.

Accurate Quantification of Saccharin Using Isotope Dilution Liquid Chromatography Mass Spectrometry (ID-LC/MS)

  • Lee, Yun-Jung;Kim, Byung-Joo;Kim, Jeong-Kwon;Ahn, Seong-Hee
    • 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.

Analysis of PCDDs/PCDFs in Sediment by Isotope Dilution HRGC/HRMS (Isotope Dilution HRGC/HRMS 방법을 이용한 저니토중의 PCDDs/PCDFs 분석)

  • Jang, Seong Ki
    • 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.

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Errors in Isotope Dilution Caused by Matrix-induced Mass Bias Effect in Quadrupole Inductively Coupled Plasma-Mass Spectrometry

  • Pak, Yong-Nam
    • 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.

Development of an Isotope-Dilution Liquid Chromatography/Mass Spectrometric Method for the Accurate Determination of Acetaminophen in Tablets

  • Shin, Hyun-Ju;Kim, Byung-Joo;Lee, Joon-Hee;Hwang, Eui-Jin
    • Bulletin of the Korean Chemical Society
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    • v.31 no.12
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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.

Determination of Polybrominated Diphenyl Ethers(PBDEs) in Soil using Gas Chromatography/Isotope Dilution Mass Spectrometry (기체크로마토그래피/동위원소 희석 질량분석법을 이용한 토양 중 폴리브롬화 디페닐에테르의 분석법)

  • Na, Yuncheol;Chang, Yoon-Seok;Kim, Hai-Dong;Hong, Jongki
    • Analytical Science and Technology
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    • v.17 no.1
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    • pp.29-36
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    • 2004
  • An analytical method of polybrominated diphenyl ethers in soil samples by isotope dilution method using gas chromatography/mass spectrometry (GC/MS)-selected ion monitoring (SIM) was described. PBDEs in soil were extracted with soxhlet extractor and then silica and florisil solid phase extraction (SPE) methods as purification of extract were compared. After clean-up, the extractions were analyzed by GC/MS with SIM mode. Quantitation was performed isotope dilution method using four $^{13}C$ isotopically labeled PBDEs as internal standards. This developed method was validated for eight congeners of PBDEs in the concentration range 0.04~4 ng/g in soil and the average recovery of the analytes ranged 30.8~110.8% for florisil and 44.4~110.7% for silica, respectively. The method detection limits of PBDEs were 0.04~0.3 ng/g.

Inspection of the Fragmentation Pathway for Thiamethoxam

  • Son, Sunwoong;Kim, Byungjoo;Ahn, Soenghee
    • Mass Spectrometry Letters
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    • v.8 no.3
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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.

Development of an Isotope Dilution Mass Spectrometry (IDMS)-Based Method for the Analysis of Ibuprofen

  • Lee, Joonhee;Kim, Byungjoo
    • Mass Spectrometry Letters
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    • v.8 no.3
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    • pp.49-52
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    • 2017
  • Ibuprofen is one of the most popular analgesic and antipyretic drugs. An isotope dilution mass spectrometry method based on LC/MS was developed as a candidate reference method for the accurate determination of ibuprofen in pharmaceutical tablets. Isotope labelled ibuprofen, $ibuprofen-d_3$, was added as an internal standard into sample extracts. Ibuprofen and $ibuprofen-d_3$, was analysed by LC/MS in a selected ion monitoring (SIM) mode to detect ions at m/z 205 and 208, 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.

Determination of Uranium Isotopes in Spent Nuclear Fuels by Isotope Dilution Mass Spectrometry (동위원소희석 질량분석법을 이용한 사용후핵연료 중 우라늄 동위원소 정량)

  • Kim, Jung Suk;Jeon, Young Shin;Son, Se Chul;Park, Soon Dal;Kim, Jong Goo;Kim, Won Ho
    • 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$$^{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.