주사전자 현미경/에너지 분산형 X-선 검출 분광기(SEM/EDS)를 이용한 뇌관화약 잔사분석법의 유효성 확인
Internal Validation of the Primer Residue Analysis by Scanning Electron Microscope/Energy Dispersive X-ray Spectrometry
1
조회
0
다운로드
5
인용
0
참고문헌
키워드
초록
본 실험은 총기 사고에서 중요한 증거물 중 하나인 뇌관 화약잔사에 대한 분석법을 확립하고자하였고, 이 시험방법에 대한 유효성 및 신뢰성을 확보하기 위하여 선택성, 감도, 재현성을 성능 특성들로선정하여 확인하였다. SEM/EDS분석 변수인자 중 스테이지 Z축(14.5 mm), 최종 aperture와 시료 표면간의 거리 즉, 작업거리(10.8 mm), 탐침전류(1500 pA), 탐색입자의 최저크기(0.4 μm) 및 최저 탐색한계값(10)에 대하여 최적화 하였고 이러한 변수값을 기본으로 하여 뇌관화약 잔사 분석에 대한 연구소 자체분석법을 확립하였다. 총기 발사 시 생성되어 검출 가능한 42개의 구성 성분이 모두 검출되도록 조건을설정하여 확인한 결과 뇌관화약 고유의 특정성분인 Pb-Ba-Sb, Ba-Sb, Pb-Sb 및 Pb-Ba 성분들이 뚜렷이구별되어 검출되었다. 1.0 μm 이상의 크기에서 검출된 입자의 수는 표준편차 ±2개 이내로 재현성 있는분석결과를 얻었으며 90%이상의 검출율을 확인하였다.
Abstract
This study aims to establish an analytical method for primer residue, one of the most significant evidence in firearm accidents. Selectivity, sensitivity, robustness and repeatability were chosen as characteristics to ensure validity and reliability of the experiment. Optimal results were obtained when stage z-axis was set on 14.5 mm, working distance on 10.8 mm, i probe of 1500 pA, minimum size of particle searched on 0.4 μm and lower threshold on 10. These values served as a basis for for the development of SIL's self-analysis method. The experiment was set to detect all 42 components created from bullet discharge, and the analysis indicated a distinct existence of Pb-Ba-Sb, Ba-Sb, Pb-Sb and Pb-Ba, the characteristic components of primer residue. The analysis yielded repeatable results, with the number of particles detected from evidence larger than 1.0ߦ consistent with standard deviation within 2 units and the detection rate of over 90%.
참고문헌 (23)
- F Saverio Romolo, "Identification of gunshot residue: a critical review", Forensic Sci Int, 119, pp.195~211 (2001)
- M Grima, "Firework displays as sources of particles similar to gunshot residue", Science and Justice, 52, pp.49~57 (2012)
- G Wolten, "Particle analysis for the detection of gunshot residue II: occupational and environmental particles", J Forensic Sci, 24(2), pp.423~430 (1979)
- J Wallace, "Discharge residues from cartridge-operated industrial tools", J Forensic Sci Soc, 24(5), pp.495~508 (1984)
- O Salles, "A forensic study: Lead determination in gunshot residues", Microchemical Journal, 101, pp.49~53 (2012)
- AJ Schwoeble, "Current Method in Forensic Gunshot Residue Analysis", pp.11~18 (2000), CRC Press
- ASTM E1588-10, "Standard Guide for Gunshot Residue Analysis by Scanning Electron Microscopy", Energy Dispersive X-ray Spectrometry, 2010
- C Torre, "Brake linings: a source of non-GSR particles containing lead, barium, and antimony", J Forensic Sci, 47(3), pp.494~504 (2002)
- B Matthew, "Determining the Lifetime of Detectable Amounts of Gunshot Residue on the Hands of a Shooter Using Laser-Induced Breakdown Spectroscopy", APPLIED SPECTROSCOPY, 62(11), pp.1238~1241 (2008)
- GD Renshaw, "The Quantitative Estimation of Lead, Antimony and Barium in Gunshot Residues by Non-Flame Atomic Absorption Spectrophotometry", Atomic Absorption Newsletter, 12, pp.55~57 (1973)
- E Reis, "Identification of gunshot residues by high resolution inductively coupled plasma massspectrometry", QUIM. Nova, 27(3), pp.409~413 (2004)
- J Souza Sarkis, "Measurements of gunshot residues by sector field inductively coupled plasma mass spectrometry-Further studies with pistols", Forensic Sci Int, 172, pp.63~66 (2007)
- A Berendes, "A versatile technique for the investigation of gunshot residue patterns on fabrics and other surfaces: m-XRF", J Forensic Sci, 51(5), pp.1085~1090 (2006)
- J Flynn, "Evaluation of X-ray microfluorescence spectrometry for the elemental analysis of firearm discharge residues", Forensic Sci Int, 97, pp.21~36 (1998)
- J Brazeau, "Analysis of gunshot residues on human tissues and clothing by Xray microfluorescence", J Forensic Sci, 42(3), pp.424~428 (1997)
- A Martiny, "SEM", EDS analysis and characterization of gunshot residues from Brazilian lead-free ammunition, 2008, pp.177(1), 9~17
- 전충현, "SEM", EDX에 의한 뇌관화약 잔사분석, 2009, pp.3(2), 166~172
- 임봉환, "총기별 발사 후 뇌관 화약류 잔사물의 분포특성", 과학수사학, 7(1), pp.1~8 (2013), 한국과학수사학회
- M Pechnikova, "Detection of metal residues on bone using SEM", EDS. Part I: Blunt force injury, 2012, pp.223, 87~90
- L Niewoehner, "ENFSI proficiency test program on identification of GSR by SEMEDX", J Forensic Sci, 48(4), pp.786~792 (2003)
- V Kocman, "Analysis of a bulk coal-tar reference pitch sample by neutron and photon activation analysis, X-Ray fluorescence spectrometry, and atomic absorption spectroscopy", J Carbon, 27(2), pp.185~190 (1989)
- Y Osin, "SEM and X-ray analysis of surface microstructure of a natural leather processed in a low temperature plasma", J Vacuum, 51(2), pp.221~225
- G Kotula, "Automated Analysis of SEM X-Ray Spectral Images: A Powerful New Microanalysis Tool", Microscopy and Microanalysis, 9(1), pp.1~17 (2003)