• 제목/요약/키워드: Inductively coupled plasma mass

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Determination of Bi Impurity in Lead Stock Standard Solutions by Hydride-generation Inductively Coupled Plasma Mass Spectrometry

  • Park, Chang J.
    • Bulletin of the Korean Chemical Society
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    • 제25권2호
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    • pp.233-236
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    • 2004
  • Total impurity analysis of a primary standard solution is one of the essential procedures to determine an accurate concentration of the standard solution by the gravimetry. Bi impurity is determined in Pb standard solutions by inductively coupled plasma mass spectrometry (ICP-MS). The direct nebulization of the Pb standard solution produces a significant amount of the Pb matrix-induced molecular ions which give rise to a serious spectral interference to the Bi determination. In order to avoid the spectral interference from the interferent $^{208}PbH^+$, the hydride generation method is employed for the matrix separation. The Bi hydride vapor is generated by reaction of the sample solution with 1% sodium borohydride solution. The vapor is then directed by argon carrier gas into the ICP after separation from the mixture solution in a liquid-gas separator made of a polytetrafluoroethylene membrane tube. The presence of 1000 ${\mu}$g/mL Pb matrix caused reduction of the bismuthine generation efficiency by about 40%. The standard addition method is used to overcome the chemical interference from the Pb matrix. Optimum conditions are investigated for the hydride-generation ICPMS. The detection limit of this method is 0.5 pg/mL for the sample solutions containing 1000 ${\mu}$g/mL Pb matrix.

유도결합플라스마 질량분석을 위한 사용후핵연료 중 테크네튬-99의 추출크로마토그래피 분리 (Extraction Chromatographic Separation of Technetium-99 from Spent Nuclear Fuels for Its Determination by Inductively Coupled Plasma-Mass Spectrometry)

  • 서무열;이창헌;한선호;박영재;지광용;김원호
    • 분석과학
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    • 제17권5호
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    • pp.438-442
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    • 2004
  • To determine the contents of $^{99}Tc$ in the spent PWR (pressurized water reactor) nuclear fuels by ICP-MS (inductively coupled plasma-mass spectrometry), a technetium separation method using an extraction chromatographic resin (TEVA Spec resin) has been established. $^{99}Tc$ was separated from a spent PWR nuclear fuel solution by this separation procedure and its concentration was determined by ICP-MS. The result agrees well with the value calculated by the program ORIGEN 2 and also the value measured by AG MP-1 resin/ICP-MS method described in our previous paper. It can be concluded that the present separation procedure is superior to the AG MP-1 resin procedure with respect to the time required for technetium separation as well as the efficiency of decontamination from other radioactive nuclides.

Nanometrology and its perspectives in environmental research

  • Kim, Hyun-A;Seo, Jung-Kwan;Kim, Taksoo;Lee, Byung-Tae
    • Environmental Analysis Health and Toxicology
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    • 제29권
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    • pp.16.1-16.9
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    • 2014
  • Objectives Rapid increase in engineered nanoparticles (ENPs) in many goods has raised significant concern about their environmental safety. Proper methodologies are therefore needed to conduct toxicity and exposure assessment of nanoparticles in the environment. This study reviews several analytical techniques for nanoparticles and summarizes their principles, advantages and disadvantages, reviews the state of the art, and offers the perspectives of nanometrology in relation to ENP studies. Methods Nanometrology is divided into five techniques with regard to the instrumental principle: microscopy, light scattering, spectroscopy, separation, and single particle inductively coupled plasma-mass spectrometry. Results Each analytical method has its own drawbacks, such as detection limit, ability to quantify or qualify ENPs, and matrix effects. More than two different analytical methods should be used to better characterize ENPs. Conclusions In characterizing ENPs, the researchers should understand the nanometrology and its demerits, as well as its merits, to properly interpret their experimental results. Challenges lie in the nanometrology and pretreatment of ENPs from various matrices; in the extraction without dissolution or aggregation, and concentration of ENPs to satisfy the instrumental detection limit.

유도결합 플라스마 질량분석법에 의한 모발의 다원소 분석 (Multi - elemental Analysis of Hair by Inductively Coupled Plasma/Mass Spectrometry)

  • 차명진;강준모;박창준
    • 분석과학
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    • 제15권4호
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    • pp.335-340
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    • 2002
  • 유도결합 플라스마 질량분석법 (ICP-MS)을 이용하여 모발 중 다원소 동시 정량법을 확립하였다. 0.05 g의 모발 시료에 내부표준물질인 In을 가하고 질산 1.5 mL와 함께 테플론 가압분해 용기에 넣어 마이크로파를 이용하여 분해하는 시료전처리법을 사용하였다. 측정값의 정확도 및 신뢰도를 확인하기 위하여 모발 인증표준물질인 GBW 09101을 반복 분석하였는데 측정값은 인증값과 불확도 범위 내에서 잘 일치하는 결과를 얻었다.

Determination of Li by Isotope Dilution Inductively Coupled Plasma Mass Spectrometry

  • Park, Chang J.;Chung, Bag S.
    • 분석과학
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    • 제8권4호
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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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유도결합 플라스마 질량 분석법(ICP-MS)을 이용한 음용수 중의 전체 비소의 정량 (Determination of Total Arsenic in Drinking Water by Inductively Coupled Plasma-Mass Spectrometry)

  • 임유리;박경수;윤양희;김선태;정진호
    • 분석과학
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    • 제13권4호
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    • pp.423-427
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    • 2000
  • 유도결합 플라스마 질량 분석법(ICP-MS)을 이용하여 음용수 중의 전체비소를 정량하였다. 지하수 및 간이 상수도와 시판되는 먹는 물에 질산을 첨가하여 1%로 산성화한 후에 ICP-MS로 전제비소의 함량을 분석하였다. 그 결과 음용수 중의 전체 비소는 $30{\mu}g/L$ 이하로서 수질 기준치인 $50{\mu}g/L$ 이하의 값을 나타내었다.

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Attenuation of Background Molecular Ions and Determination of Isotope Ratios by Inductively Coupled Plasma Mass Spectrometry at Cool Plasma Condition

  • 박창준
    • Bulletin of the Korean Chemical Society
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    • 제18권7호
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    • pp.706-710
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    • 1997
  • Isotope ratios of K, Ca, Cr and Fe are measured at cool plasma condition generated using high carrier flow rate and relatively low RF power of 900 W. Background molecular ions are suppressed to below 100 counts which give isobaric interference to the analytes. The background ions show different attenuation characteristics at increased carrier flow rate and hence for each element different carrier flow rate should be used to measure isotope ratios without isobaric interference. Isotope ratios are measured at both scan and peak-hopping modes and compared with certified or accepted ratios. The measured isotope ratios show some mass discrimination against low mass due to low ion energy induced from a copper shield to eliminate capacitive coupling of plasma with load coil.

Determination of Isotopic Ratios for Ca in Inductively Coupled Plasma Mass Spectrometry (ICPMS) by Removing Water Related Molecules

  • 박용남;S. R. Koirtyohann
    • Bulletin of the Korean Chemical Society
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    • 제18권11호
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    • pp.1172-1175
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    • 1997
  • Calcium isotopic ratios are precisely measured by removing isobaric interferences originated from water in the plasma. Liquid Ar cryogenic trap combined with membrane desolvator could eliminate backgrounds at m/z 42 and 44. Slow drift of ICP-MS is corrected by the frequent running of the standards. It is found necessary to separate Ca from the sample matrix using Ca oxalate precipitation technique. Currently, the RSD is 0.5-1.0% for 2 minutes of measurement but is expected to be improved if the measurement time is increased. The technique was applied to 42Ca enriched baby fecal samples and successfully determined 42Ca/44Ca ratio changes.

Isotope Measurement of Uranium at Ultratrace Levels Using Multicollector Inductively Coupled Plasma Mass Spectrometry

  • Oh, Seong-Y.;Lee, Seon-A.;Park, Jong-Ho;Lee, Myung-Ho;Song, Kyu-Seok
    • Mass Spectrometry Letters
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    • 제3권2호
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    • pp.54-57
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    • 2012
  • Mass spectrometric analysis was carried out using multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) for the precise and accurate determination of the isotope ratios of ultratrace levels of uranium dissolved in 3% $HNO_3$. We used the certified reference material (CRM) 112-A at a trace level of 100 pg/mL for the uranium isotopic measurement. Multiple collectors were utilized for the simultaneous measurement of uranium isotopes to reduce the signal uncertainty due to variations in the ion beam intensity over time. Mass bias correction was applied to the measured U isotopes to improve the precision and accuracy. Furthermore, elemental standard solution with certified values of platinum, iridium, gold, and thallium dissolved in 3% $HNO_3$ were analyzed to investigate the formation rates of the polyatomic ions of $Ir^{40}$ $Ar^+$, $Pt^{40}$ $Ar^+$, $Tl^{40}$ $Ar^+$, $Au^{40}$ $Ar^+$ for the concentration range of 50-400 pg/mL. Those polyatomic ions have mass-to-charge ratios in the 230-245 m/z region that it would contribute to the increase of background intensity of uranium, thorium, plutonium, and americium isotopes. The effect of the polyatomic ion interference on uranium isotope measurement has been estimated.

MgO 증착을 위한 유도결합 플라즈마 마그네트론 스퍼터링에서 실시간 공정 진단 (A Real-Time Diagnostic Study of MgO Thin Film Deposition Process by ICP Magnetron Sputtering Method)

  • 주정훈
    • 한국표면공학회지
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    • 제38권2호
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    • pp.73-78
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    • 2005
  • A real-time monitoring of ICP(inductively coupled plasma) assisted magnetron sputtering of MgO was carried out using a QMS(quadrupole mass spectrometer), an OES(optical emission spectrometer), and a digital oscilloscope with a high voltage probe and a current monitor. At the time of ICP ignition, the most distinct impurity was OH emission (308.9 nm) which was dissociated from water molecules. For reactive deposition oxygen was added to Ar and the OH emission intensity was reduced abruptly When the discharge voltage was regulated by a PID controller from 240V(metallic mode) to 120V(oxide mode), the emission intensity from Mg (285.2 nm) changed proportionally to the discharge voltage, but the intensity of Ar I(811.6 nm) was constant. At 100V of discharge voltage, Mg sputtering was almost stopped. Emissions from Ar I(420.1 nm) and Mg I were dropped down to 1/10, but Ar I(811.6 nm) didn't change. And the emission from atomic oxygen (O I, 777.3 nm) was increased to 10 times. These results are compatible with those from QMS study.