• Title/Summary/Keyword: spectrometry (ICP-MS)

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The Improved Method for Precise Determination of Pu Isotope Ratio using MC-ICP-MS (다중검출기유도결합플라즈마질량분석기를 이용한 Pu 동위원소비 정밀 분석법)

  • Yim, Seong-A;Han, Eun-Mi;Chae, Jung-Seok;Yun, Ju-Young
    • Journal of Radiation Protection and Research
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    • v.35 no.3
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    • pp.117-123
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    • 2010
  • Plutonium is by far the most important of the transuranic elements which have been released into the environment due to radio-toxicity and long term radiation effects on humans. And Pu isotope ratio ($^{240}Pu/^{239}Pu$) is of great interest because this ratio is used as a fingerprint for different sources. Mass spectrometry has been used as an useful atom counting technique with several advantages over decay counting techniques for the determination of Pu isotopes. It enables a determination of Pu isotope ratio in the environmental samples with a low detection limit and a short determination time. An ICP-MS is the representative mass spectrometry for Pu determination. In this study, the precision of $^{240}Pu/^{239}Pu$ isotope ratio was improved by using 4 multiple ion counters of MC-ICP-MS. The detection limit of $^{239}Pu$ and $^{240}Pu$ were $0.10\;fg\;ml^{-1}$ ($0.24\;{\mu}Bq\;ml^{-1}$), $0.12\;fg\;ml^{-1}$ ($0.97\;{\mu}Bq\;ml^{-1}$), respectively. The relative standard deviation of $^{240}Pu/^{239}Pu$ isotope ratio was less than 1 % in trace level. The various reference materials (seawater, soil and sediment) were analyzed to verify this method and their analytical results were in good agreement with the certified (or recommended value) value.

Quantitative analysis of selenium species in sea food using solid phase extraction and HPLC-ICP/MS (해산물 시료에서 solid-phase extraction 및 HPLC-ICP/MS를 이용한 셀레늄 화학종의 정량분석)

  • Kim, Eunju;Joo, Minkyu;Kwon, Hyosik;Pak, Yongnam
    • Analytical Science and Technology
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    • v.26 no.5
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    • pp.307-314
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    • 2013
  • Selenium exists in various forms of chemical species. The activity and bioavailability is strongly dependent on its chemical form and concentration. Consequently the information on each selenium species and its concentration must be exactly determined for the food we take in. In this study, selenium species in seafood were separated and quantified by RP (reversed phase) HPLC (high performance liquid chromatography) coupled with ICP-MS (inductively coupled plasma mass spectrometry) using post-column isotope dilution. $^{79}Br$, which interferes on $^{80}Se$, has mostly been removed by solid phase extraction and then mathematical correction has been applied for the more accurate correction. The experimental result for CRM (certified reference material) DOLT-4 agreed well with the certified value but each selenium species could not be compared. SeCys (selenocysteine) and SeMet (selenomethionine) were the major species detected in seafood such as belt fish, spanish mackerel, and squid that have been serving as Korean diet. The concentrations found in Korean sea food for SeCys and SeMet were in the range of 0-661.6 mg/kg and 137.3-462.7 mg/kg, respectively.

A Study on the Migration of Heavy Metals from Polycarbonate Food Contact Materials Using an Inductively Coupled Plasma Mass Spectrometry (ICP-MS) (식품용 폴리카보네이트 기구류 중 ICP-MS를 이용한 중금속 이행량 조사)

  • Park, Se-Jong;Park, So-Ra;Kim, MeeKyung;Choi, Jae Chun
    • KOREAN JOURNAL OF PACKAGING SCIENCE & TECHNOLOGY
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    • v.24 no.3
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    • pp.107-112
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    • 2018
  • The purpose of this study was to investigate the migration levels of lead (Pb), cadmium (Cd) and arsenic (As) from polycarbonate food contact materials into food simulant at different temperatures ($70^{\circ}C$ and $100^{\circ}C$). The method was validated by linearity of calibration curves, limit of detection (LOD), limit of quantification (LOQ), recovery, precision and uncertainty. All of 200 samples, including bottles, cups, containers, ladles, spoons and tongs were purchased from domestic markets and analyzed by inductively coupled plasma mass spectrometry (ICP-MS). Mean concentrations of positive samples were higher at $100^{\circ}C$ than $70^{\circ}C$ as showing a dependency of migration temperature. The migration concentrations ranged from not-detected (ND) to $4.67{\mu}g/L$, ND to $0.49{\mu}g/L$L and ND to $2.91{\mu}g/L$ for Pb, Cd and As, respectively, which were far below the migration limits of Korea standards and specifications for food utensils, containers and packages.

Determination of Cd and Pb in Human Blood by Isotope Dilution Inductively Coupled Plasma Mass Spectrometry : International Comparison (동위원소희석 질량분석법에 의한 혈액 중 Cd, Pb 성분의 측정 : 국제공동분석)

  • Park, C.J.;Suh, J.K.;Lee, S.H.
    • Analytical Science and Technology
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    • v.9 no.2
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    • pp.145-160
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    • 1996
  • Inorganic analytical laboratory of Korea Research Institute of Standards and Science participated in an interlaboratory comparison program operated by Quebec Toxicology Centre of Canada in 1994 and again in 1995. The objective of this program is to enable participating laboratories to assess reproducibility and accuracy of their analytical results for trace toxic elements in human biological fluids. This laboratory determined Cd and Pb concentrations in 3 levels of human blood samples by isotope dilution inductively coupled plasma mass spectrometry. 0.5mL of blood sample is added to the digestion bomb together with 2mL of nitric acid and enriched spike isotopes and then decomposed in the microwave digestion system. The decomposed sample is diluted to 10mL and nebulized into ICP-MS. The Cd and Pb values reported by all participating laboratories are presented and compared. The values reported by this laboratory are within the acceptable range of target values.

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Development and Validation of the Simultaneous Analytical Method of Urinary Metals and Metalloids for the National Biomonitoring Programs (국가 바이오모니터링 프로그램을 위한 소변 중 금속류 동시분석법 개발 및 검증)

  • Cho, Yong Min;Yang, Minho;Im, Hosub;Cha, Sangwon;Lee, Jaeick;Kim, Ki Hun;Han, Sang Beom
    • Journal of Environmental Health Sciences
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    • v.45 no.6
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    • pp.594-604
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    • 2019
  • Objectives: This study developed and validated an analysis method of urinary metals and metalloids that can be applied inductively with coupled plasma mass spectrometry (ICP-MS). Methods: 0.3 mL of urine was used to analyze 25 metal and metalloid compounds using ICP-MS. The validation of the analytical method included linearity, accuracy, precision, and the calculation of detection limits. In addition, a comparison test was performed with the graphite furnace atomic absorption spectrometry (GF-AAS) method, which is the current standard method, with urine samples of 66 healthy subjects. Results: The linearities (R2) of calibration curves of all 25 compounds were ≥ 0.999. Of the 25 compounds, the intra-day and inter-day accuracy% of 17 and 20 met ≤15%, respectively. In addition, fifteen compounds showed ≤15% recovery% for certificated reference materials. Intraclass correlation coefficients of the comparison between the current methods and new methods in this study were 0.952 (p-value<0.001) and 0.911 (p-value<0.001) for urinary cadmium and mercury, respectively. Conclusion: This study proposes an efficient simultaneous methodology that can analyze multi elements in smaller sample amounts. More reproduction experiments are needed in the future.

Recovery of Copper from Spent Photovoltaic Ribbon in Solar Module (폐태양전지(廢太陽電池)용 솔라리본으로부터 구리회수(回收)에 관한 연구(硏究))

  • Lee, Jin-Seok;Jang, Bo-Yun;Kim, Joon-Soo;Ahn, Young-Soo;Kang, Gi-Hwan;Wang, Jei-Pil
    • Resources Recycling
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    • v.22 no.5
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    • pp.50-55
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    • 2013
  • The recovery of copper from spent photovoltaic ribbon was conducted using thermal treatment method at the range of temperature of $300^{\circ}C$ to $600^{\circ}C$ under inert atmosphere. The coating layer consisted of lead of 68.99 wt.% and tin of 31.21 wt.% was melted down at elevated temperatures and was collected on the bottom of crucible. The chemical composition of copper ribbon after thermal treatment was analyzed by ICP-MS (Inductively coupled plasma mass spectrometry) and the purity of copper was found to be obtained up to about 96 wt.% regardless of temperatures. The cross-sectional area of the specimen was also examined by SEM (scanning electron microscopy) and EDX (energy dispersive X-ray microscopy).

The analysis of impurities in rare earth oxide for fluorescent substance by ICP-MS (ICP-MS에 의한 형광체용 $(Y,\;Eu)_2O_3$ 중 불순물 분석 연구)

  • Kim, Sang-Kyoung;Jang, Seung-Kyu
    • Analytical Science and Technology
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    • v.7 no.1
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    • pp.1-10
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    • 1994
  • A survey was made on detection limit, reproducibility, matrix effect, linear dynamic range and the memory effect of yttrium and europium in order to analyze rare earth elements which exist as impurities in the rare earth oxide which is raw materials of fluorescent substance. When analysing a certain amount of thulium quantitatively using inductively coupled plasma mass spectrometry, it was found that the analysis was interfered with $EuO^+$ which is one of polyatomic ions caused by plasma. As the intensity of thulium linearly proportional to the europium concentration, it was possible to the determine the actual concentration of thulium.

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RRT Study for the Quantitative Analysis of Boron in Silicon (실리콘에 도핑된 붕소의 정량분석에 대한 공동분석연구)

  • 김경중;김현경;문대원;홍태은;정칠성;김이경;김재남;임철호;김정호
    • Journal of the Korean Vacuum Society
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    • v.11 no.4
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    • pp.218-224
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    • 2002
  • A domestic round robin test(RRT) for the quantitative analysis of minor impurities was performed by a standard procedure and standard reference material. The certified reference material(CRM)s for B-doped Si thin film and analysis specimens and the analysis specimens were prepared by an ion beam sputter deposition method. These samples were certified by inductively coupled plasma mass spectrometry(ICP-MS) with isotope dilution method which il one of the most quantitative methods in chemical analysis. By using an international standard procedure(ISO/DIS-l4237) for the quantitative analysis of B in Si by SIMS, a domestic RRT was performed for these specimens. Although only a few laboratories participated in this RRT, the average B concentration well agreed with the certified value within 2% error.

Investigation on Dissolution and Removal of Adhered LiCl-KCl-UCl3 Salt From Electrodeposited Uranium Dendrites using Deionized Water, Methanol, and Ethanol

  • Killinger, Dimitris Payton;Phongikaroon, Supathorn
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.18 no.4
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    • pp.549-562
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    • 2020
  • Deionized water, methanol, and ethanol were investigated for their effectiveness at dissolving LiCl-KCl-UCl3 at 25, 35, and 50℃ using inductively coupled plasma mass spectrometry (ICP-MS) to study the concentration evolution of uranium and mass ratio evolutions of lithium and potassium in these solvents. A visualization experiment of the dissolution of the ternary salt in solvents was performed at 25℃ for 2 min to gain further understanding of the reactions. Aforementioned solvents were evaluated for their performance on removing the adhered ternary salt from uranium dendrites that were electrochemically separated in a molten LiCl-KCl-UCl3 electrolyte (500℃) using scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS). Findings indicate that deionized water is best suited for dissolving the ternary salt and removing adhered salt from electrodeposits. The maximum uranium concentrations detected in deionized water, methanol, and ethanol for the different temperature conditions were 8.33, 5.67, 2.79 μg·L-1 for 25℃, 10.62, 5.73, 2.50 μg·L-1 for 35℃, and 11.55, 6.75, and 4.73 μg·L-1 for 50℃. ICP-MS analysis indicates that ethanol did not take up any KCl during dissolutions investigated. SEM-EDS analysis of ethanol washed uranium dendrites confirmed that KCl was still adhered to the surface. Saturation criteria is also proposed and utilized to approximate the state of saturation of the solvents used in the dissolution trials.

Analysis of multi-layered Surface with Glow Discharge-Mass Spectrometry (글로우방전 질량분석법을 이용한 다층박막의 표면 분석)

  • Pak, Yong-Nam;Lee, Gae-Ho;Kim, Hyo Jin
    • Analytical Science and Technology
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    • v.10 no.5
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    • pp.357-361
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    • 1997
  • A Griemm type Glow Discharge cell is attached to a commercial quadrapole based ICP-MS and used for the analysis of surface analysis. By employing 2.0mm diameter, mode and proper experimental conditions, several layers of few ${\mu}m$ thickness are analysed within 30 minutes. Multi-layers of Cu-Ni, Fe-Ni are analyzed with the resolution of 10nm by GDMS. Proper experimental conditions make a flat bottom crater shape and good resolution for multi-layer depth profile study.

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