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Inductively coupled plasma - mass spectrometer (ICPMS)

Inductively coupled plasma - mass spectrometer (ICPMS). 발표자 : 백 지 훈 (석사1기) 발표일 : 2000.06.17. ICPMS 개요. ICPMS as a chromatographic detector was first described in the late 1980s. A useful and powerful technique for the detection of trace elements in chromatographic eluents.

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Inductively coupled plasma - mass spectrometer (ICPMS)

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  1. Inductively coupled plasma - mass spectrometer (ICPMS) 발표자 : 백 지 훈 (석사1기) 발표일 : 2000.06.17

  2. ICPMS 개요 • ICPMS as a chromatographic detector was first described in the late 1980s. • A useful and powerful technique for the detection of trace elements in chromatographic eluents. • The analysis of both metals and non-metalss

  3. Advantages • 60여종 이상의 원소에 대해 ppb이하의 분석이 가능 • 희토류원소 분석이 용이 • 1분정도의 시간에 70여개 원소의 동시분석이 가능 • ppt에서 ppm에 이르는 농도범위에서 주성분, 미량성분 및 흔적원소 등을 동시에 분석 • 동위원소비(정밀도: 약 0.2%)를 측정할 수 있다

  4. Components of a mass spectrometer

  5. Schematic of an ICPMS system

  6. Inductively Coupled Plasma Mass Spectrometer (유도결합 플라즈마 질량분석) • Ar 가스를 induction coil로 둘러쌓인 Torch로 흘려보내고 고주파를 걸어주면 고온(최대 약 8000K)의 Ar 플라즈마 형성. • 이 플라즈마에 용액시료를 작은 입자상태로 분무. • 이 때 전 원소중 약 70%에 해당되는 원소들은 90% 이상의 효율로 1가의 양이온으로 하전됨. • 하전된 입자는 단계적으로 진공도가 낮아지도록 설계된 경계역을 지나 종국에는 진공도가 약 10-6mbar에 달하는 질량분석기에 연결되어 분석됨.

  7. Plasma • 물질의 제 4의 상태. • 고도로 이온화 된 가스로 약 4,000℃ ~ 12,000℃사이에 존재. • 생성과정에서 전광을 방출. • 우주 구정물질은 99% 이상이 plasma 상태. • 지구상에서는 거의 존재하지 않음. • 전기아크, 번개, 형광등, 네온사인, 태양풍, 태양 그자체, 성간물질 및 별과 성운

  8. Chromium speciationusing an automated liquid handling system with inductively coupled plasma - mass spectrometric detection

  9. Abstract • The speciation of inorganic chromium in environmental samples is required for accurate assessment of pollution levels. • Cr(Ⅵ) is a known carcinogen, while Cr(Ⅲ) is an essential element. • An automated liquid handling system, the PrepLabTM, can be used with an ICP-MS to quantify CR(Ⅲ) and Cr(Ⅵ) in liquid samples.

  10. Introduction • Chromium is a naturally occurring element. • Daily intake from air, water, and food. • Two major valence states, trivalent chromiumCr(Ⅲ) and hexavalent chromium Cr(Ⅵ). • The body is capable of detoxifying some Cr(Ⅵ) to Cr(Ⅲ).

  11. Experimental section • Sample loading solutions, eluting solutions and test solutions • Ion chromatography : the PrepLabTM, a metal-free, automated, liquid handling system • Inductively coupled plasma-mass spectrometry : A PlasmaQuad 3TM ICP-MS instrument

  12. PrepLabTM automated liquid handling system

  13. Implementation of PrepLabTM for separation of Cr(Ⅲ) and Cr(Ⅵ) • A 0.5 ml sample loop is filled with sample while the loading solution flows through the column to the ICP-MS. • The six-port valve is then switched so that the sample flows through the column. • During this step, the chelation resin must have specificity in the solvent or buffer for one Cr species but not the other, such that one species remains bound to the resin while the other flows through to the ICP-MS. • Switching of the mobile phase to an eluting solution then removes the species bound to the resin so that it flows to the ICP-MS for detection.

  14. Result 1 Chromatography of a mixture of Cr(Ⅲ) from Cr(Ⅵ) using Prosep-Chelating Ⅰ.

  15. Result 2 Chromatography of individual Cr(Ⅲ) and Cr(Ⅵ) runs using Prosep-Chelating Ⅰ. The small amount of Cr(Ⅲ) detected during the analysis of the Cr(Ⅵ) solution could be caused by either Cr(Ⅲ) contamination in the Cr(Ⅵ) solution or inter-conversion of Cr(Ⅵ) to Cr(Ⅲ) during the analysis.

  16. Discussion • Upon testing the pH of the standard solution it was determined to be acidic(<pH3.5). Under these acidic conditions, Cr(Ⅵ) can be converted to Cr(Ⅲ) and thus create Cr(Ⅲ) contamination in the certified Cr(Ⅵ) solution. • The basic conditions (pH 9.0) used during steps 1 and 2 the IC-ICP-MS method would discourage the conversion of Cr(Ⅵ) to Cr(Ⅲ). • Further studies using SIDMS at each step of the analysis procedure are planned in order to determine definitively the source of the Cr(Ⅲ) contamination.

  17. ICPMS의 적용분야 • 환경 분야 (음료수의 불순물분석, 독성폐기물의 중금속분석, 지질학 및 해양학 분야,주성분, 미량성분 및 흔적원소 등의 정량분석, 전처리과정을 거치지 않는 희토류원소분석, 동위원소의 분석, 암석 및 광물의 화학조성분석, 금속에 대한 speciation연구) • 화학분야 (원료분석, 생산품에 대한 품질검사, 유기물의 극미량원소분석) • 반도체분야 (원료의 순도분석, 품질검사, 가스 순도분석, 초순수시약의 순도분석) • 금속분야 (고순도금속의 불순물검사, 합금에 함유된 원소분석) • 원자력분야 (핵연료의 순도분석, 저농도의 우라늄계열 원소분석) • 생물학분야 (동위원소를 추적자로 이용하는 연구, 금속-단백질의 speciation, 대사과정 추적을 위한 혈액중의 납, 아연 등의 분석) • 핵융합발전, 신물질의 합성 및 고분자와 금속의 표면처리, 조명 및 정보표시 장치, 환경정화

  18. 경희대학교 중앙기기센터 ICP Emission Spectrometer (유도결합 플라즈마 방출분광기) 제조사 및 MODEL 명 :U.S.A. Thermo Jarrell Ash ARIS-AP Solid State Detector Type : Charge Injection Detector Pixels : 512*512 Wavelength : 170 - 800 nm RF Generator Maximum output power : 2.0 KW Frequency : 27.12 MHz Tuning : Autotuning

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