The Journal of the Petrological Society of Korea (암석학회지)

The Petrological Society of Korea (한국암석학회)
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Low Dilution Glass Bead Digestion Technique for the Trace Element Analysis of Rock Samples

저희석 유리구 용해법에 의한 암석시료 미량원소 분석법

  • Park, Chan-Soo (Division of Earth and Environmental Science, Korea Basic Science Institute) ;
  • Shin, Hyung-Seon (Division of Earth and Environmental Science, Korea Basic Science Institute) ;
  • Oh, Hae-Young (Division of Earth and Environmental Science, Korea Basic Science Institute) ;
  • Moon, Jong-Hwa (Neutron Science Division, Korea Atomic Energy Research Institute) ;
  • Cheong, Chang-Sik (Division of Earth and Environmental Science, Korea Basic Science Institute)
  • 박찬수 (한국기초과학지원연구원 오창센터 환경과학연구부) ;
  • 신형선 (한국기초과학지원연구원 오창센터 환경과학연구부) ;
  • 오혜영 (한국기초과학지원연구원 오창센터 환경과학연구부) ;
  • 문종화 (한국원자력연구원 하나로이용연구본부) ;
  • 정창식 (한국기초과학지원연구원 오창센터 환경과학연구부)
  • Received : 2011.07.22
  • Accepted : 2011.08.25
  • Published : 2011.09.30
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Abstract

Open beaker digestion method is routinely used as the sample preparation technique for trace element determination of rock samples by inductively coupled plasma mass spectrometry, With this method, however, dissolution of Zr and Hf is not always guaranteed especially when the samples contain refractory minerals. In this study, glass bead digestion technique was compared with conventional open beaker digestion technique for the sample preparation of three USGS rock standards such as AGV-2, BHVO-2, and G-3. Thirty trace elements including rare earth elements were analysed by ICP-MS and ICP-AES. There were no clear differences in analytical results for the AGV-2 and BHVO-2 standards between the two techniques, but Zr, Hf, Y, and middle- to heavy- rare earth element concentrations of the G-3 standard prepared by open beaker digestion technique were significantly lower than the recommended values. This can be attributed to the presence of refractory mineral zircon. On the contrary, all the analytical results of the G-3 standard prepared by glass bead digestion technique were in good agreement with the recommended values, indicating complete dissolution of zircon. The analytical results show that the volatile elements such as Pb and Zn were not lost during the preparation of glass bead. Low dilution glass bead digestion technique described here will be very helpful to enhance precision and accuracy of trace element analysis for geological samples containing refractory minerals.

유도결합 플라즈마 질량분석법에 의한 암석 시료의 미량원소 정량분석을 위한 전처리 과정으로 통상 산분해법인 비이커-가열판 용해법이 사용된다. Zr과 Hf은 다른 비유동성 원소들과 함께 지구조 해석에 이용되는 중요한 원소이지만 암석 내에 이들을 농집시키는 불용성 광물이 있으면 비이커-가열판 용해법으로 완전히 용해되지 않는다. 이러한 불용성 광물을 용해시키기 위해 고압 테프론 용기법이나 알칼리 용융법을 이용하는데 전처리시간이 너무 오래 걸리거나 농도가 낮은 희토류원소 등의 분석 정확도가 감소하는 문제점이 있다. 이 연구에서는 자동 용융 기기를 사용하여 미국지질조사소의 암석 표준시료 3종(AGV-2, BHVO-2, G-3)을 저희석 유리구로 제작하고 이 유리구를 분말로 만들어 산분해를 거쳐 용해시킨 방법(유리구 용해법)으로 전처리한 후, 유도결합 플라즈마 질량분석기와 유도결합 플라즈마 원자방출분광기를 이용하여 희토류 원소를 포함한 30종의 미량원소 분석을 실시하였으며 시료에 대한 최종적인 희석비율은 1:2,000 이하로 유지하였다. 이 유리구 용해법에 의한 분석결과를 암석 분말시료를 이용한 비이커-가열판 용해법과 비교해 보았다. 대체적으로 Cr, Co, Ni, Cu, Zn, Pb 등의 원소분석 결과는 두 방법 모두 3종의 표준물질에서 추천치와 잘 부합되었으며 유리구 용해법을 이용한 분석에서 Pb, Zn 등 휘발성 원소의 손실은 나타나지 않았다. 저어콘을 많이 함유한 화강암 표준시료(G-3)의 Y, Zr, Hf과 중희토류원소에 대해서는 비이커-가열판 용해법의 경우 추천치에 비해 체계적으로 낮은 값을 보인 반면 유리구 용해법은 추천값에 잘 부합되는 결과를 얻었다. 이 연구의 유리구 용해법을 이용하면 불용성 원소를 포함한 미량원소 분석의 정확도가 크게 향상될 것으로 기대된다.

Keywords

Acknowledgement

Supported by : 한국연구재단

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