- P-ISSN 1225-0163
- E-ISSN 2288-8985
제조 공장의 구분이 가능한지 검토하기 위하여 LA-ICP-MS를 이용한 한국 자동차 전면 유리의 미량원소 분석을 실시하였다. 먼저 Si를 내부 표준물질로 하여 표준품 NIST 610, 612, 614과 616을 분석하여 검량선을 작성하였다. 시료와 표준품은 24원소에 대해 정량을 실시하였고 LOQ는 0.11 mg/kg(Ti)-4.91 mg/kg(Ca) 였다. 2개 공장의 11개 시료에 대하여 각각 5개씩의 위치에 따른 부시료를 분석하였다. 검출한계이하의 원소들(Cu, Cr, Cd와 Ni), 표준품에 존재하지 않는 원소들(Ti, Pr, Mg, Nb, Nd)과 균질성에 문제가 있는 원소들(Pb와 Sn)은 분석 대상 원소에서 제외하였다. 제조공장과 제조년도와 관련하여 삼각 다이어그램을 그려 본 결과 구별의 가능성을 볼 수 있었으며 Mn, Ce와 Rb를 토대로 한 정준 판별 분석식에 의해 제조공장의 구별이 가능하였다.
The analyses of minor and trace elements in glass debris were performed using LA-ICP-MS in order to identify manufacturers using real commercial samples. At first, a calibration curve was made using standard glass samples of NIST 610, 612, 614 and 616. 29Si was used as an internal standard, and the ratios of metal/Si for each metal were compared with their concentrations. Based on elements in each sample and standard materials, 24 metals were quantified and the LOD in analysis, according to the blank sample, was in the range of 0.11 mg/kg (Ti)- 4.91 mg/kg (Ca). Eleven samples from two manufacturers were collected and five sub-samples were taken from each sample for analysis. 15 elements (Co, Ce, Ca, Mn, Sr, Ba, Li, Rb, U, La, Th, Na, Al, Zr and Hf) were selected to identify manufacturers because some elements (Cu, Cr, Cd and Ni) were below the detection limit and some elements (Ti, Pr, Mg, Nb, Nd) were absent in the analysis of standards and others (Pb and Sn) had a problem of homogeneity. The attempts to identify manufacturers and the manufacturing period were performed through a triangular diagram. In the manufacturer discrimination by discriminant analysis, a canonical discriminant function was made based on Mn, Ce and Rb, and each sample could be identified.
1. (a) A. M. Dobney, W. Wiarda, P. de Joode and G. van der Peijl, J. Anal. At. Spectrom., 17, 478-484(2002).
(b) R. J. Watling, 1998. J. Anal. At. Spectrom., 13, 917-926.
2. (a) D. C. Duckworth, S. J. Morton, C. K. Bayne, S. Montero, R. D. Koons, R. D. and J. R. Almirall, J. Anal. At. Spectrom., 17, 662-668(2002).
(b) S. Branch, S. Burke, P. Evans, B. Fairman, and C. S. J. W. Bricher, J. Anal. At. Spectrom., 18, 17-22(2003).
(c) Pierce, D.S., J. Forensic Ident., 40, 51-59(1990).
3. (a) Tatiana Trejos, Shirly Montero and Jose R. Almirall, Anal. Bioanal. Chem., 376, 1255-1264(2003).
(b) Christopher Latkoczy, Marc Duecking, Stefan Becker, Detlef Guenther, Jurian A. Hoogewerff, Jose, R. Almirall, JoAnn Buscaglia, Andrew Dobney, Robert D. Koons, Shirly Montero, Gerard, J. Q. van der Peijl, Wilfried R.
4. (a) Klaus Bange, Hartmut Mueller, and Christine Strubel, Mikrochim. Acta, 132, 493-503(2000).
(b) Hans-Rudolf Kuhn, Marcel Guillong and Detlef Guenther, Anal. Bioanal. Chem., 378, 1069-1074(2004).
5. (a) Armand Zurhaar and Lindsay Mullings, J. Anal. At. Spectrom. 5, 611-617(1990).
(b) R. J. Watling, B. F. Lynch and D. Herring, J. Anal. At. Spectrom., 12, 195- 203(1997).
(c) D.C. Duckworth, C. K. Bayne, Shelby J. Morton and Jose Almirall, J. Anal. At. Spectrom., 15, 821-828(2000).
(d) Ludwik Halicz and Detlef Guenther, J. Anal. At. Spectrom., 19, 1539-1545(2004).
(e) Shirly Berends-Montero, Wim Wiarda, Peter de Joode and Gerard van der Peijl, J. Anal. At. Spectrom., 21, 1185- 1193(2006).
6. Montero, S., 2005. NFI scientific report, 47pp
7. The use of Statistics in Forensic Science C. G. G. Aitken and D. A. Stoney Tayler & Francis 1991, Forensic Interpretation of Glass Evidence James Michael Curran, Tacha Natalie Hicks, John S. Buckleton Taylor & Francis 2000.
8. Pearce, N. J. G., Perkins, W. T., Westgate, J. A., Gorton, M. P., Jackson, S. E., Neal, C. R., and Chenery, S. P., Geostandards Newsletter, 21(1), 115-144(1997).