분석과학 (Analytical Science and Technology)

  • 제15권2호
  • /
  • Pages.127-134
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  • 2002
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  • 1225-0163(pISSN)
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  • 2288-8985(eISSN)
한국분석과학회 (The Korean Society of Analytical Sciences)
권호 표지

초음파 분무기를 이용한 유기상의 주입에 의한 희토류 원소의 유도결합 플라스마 질량분석법적 정량

Determination of Rare Earth Elements by Inductively Coupled Plasma Mass Spectrometry with Introduction of Organic Phase Using Ultrasonic Nebulizer

  • 이상학 (경북대학교 자연과학대학 화학과) ;
  • 손범목 (경북대학교 자연과학대학 화학과)
  • Lee, Sang Hak (Department of Chemistry, Kyungpook National University) ;
  • Son, Bum Mok (Department of Chemistry, Kyungpook National University)
  • 투고 : 2002.01.24
  • 발행 : 2002.04.25
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초록

추출한 유기상 속의 희토류 원소를 유도결합 플라스마 질량분석법(inductively coupled plasma mass spectrometry, ICP-MS)으로 정량하는 방법에 대하여 연구하였다. 희토류 원소를 추출한 유기상의 과다한 도입을 방지하기 위하여 탈용매화장치를 장착한 초음파 분무기를 이용하여 ICP-MS에 주입하였다. 에탄올(EtOH)에 MIBK(methyl isobutyl ketone)를 섞은 용매를 도입하였을때, 계수율(count rate)이 증가하였고, 여기에 0.03 M의 추출제 HEH(2-ethylhexyl-2-ethylhexyl phosphonic acid, P507, PC88A)를 섞었을 때는 감소하였다. 탈용매화장치의 냉각장치(condenser)의 최적온도는 -10 $^{\circ}C$이었고, 가열관(heating tube)의 최적온도는 150 $^{\circ}C$이었다. 계수율이 최대이고, 반사파(reflect power)가 최소인 최적 운반기체의 흐름속도는 0.7 L/min이었다. MIBK에 추출제 HEH가 0.03 M이 섞여있는 추출용매로 추출을 행하였을 때, 최적 pH는 4.3이었고, 추출시간은 10 분이었다. 최적조건에서 0.2 ${\sim}$ 20 ng/mL의 표준용액으로 얻은 검정곡선으로부터 구한 검출 한계는 0.02 ${\sim}$ 0.05 ng/mL 이었다.

Analytical method to determine rare earth elements which were extracted to organic phase by inductively coupled plasma mass spectrometry(ICP-MS) was investigated. Organic phase which had extracted rare earth elements was directly aspirated into ICP-MS by ultrasonic nebulizer(USN) in order to reduce solvent load to the plasma. Then, the count rate increased when MIBK(methyl isobutyl ketone) was added to EtOH(ethanol) but decreased when 0.03 M HEH(2-ethylhexyl-2-ethylhexyl phosphonic acid, $P_{507}$, PC88A) was added to solvent which mixed MIBK with EtOH. The optimal temperatures of desolvation system were -10 $^{\circ}C$ for the condenser and 150 $^{\circ}C$ for the heating tube. The optimal nebulizer flow rate which gave maximum count rate and minimum reflect power was 0.7 L/min. The optimal pH and extraction time were 4.3 and 10 min for MIBK-0.03 M HEH system. Detection limits which were obtained through calibration curves at the range of 0.2 ${\sim}$ 20 ng/mL were 0.02 ${\sim}$ 0.05 ng/mL under the optimal experimental conditions.

키워드

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