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Elemental Analysis of Glass and Paint Materials by Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) for Forensic Application

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Elemental Analysis of Glass and Paint Materials by Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) for Forensic Application The author(s) shown below used Federal funds provided by the U.S. Department of Justice and prepared the following final report: Document Title: Elemental Analysis of Glass and Paint Materials by Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) for Forensic Application Author: Tatiana Trejos, Waleska Castro and Jose R. Almirall Document No.: 232133 Date Received: October 2010 Award Number: 2003-IJ-CX-K004 This report has not been published by the U.S. Department of Justice. To provide better customer service, NCJRS has made this Federally- funded grant final report available electronically in addition to traditional paper copies. Opinions or points of view expressed are those of the author(s) and do not necessarily reflect the official position or policies of the U.S. Department of Justice. This document is a research report submitted to the U.S. Department of Justice. This report has not been published by the Department. Opinions or points of view expressed are those of the author(s) and do not necessarily reflect the official position or policies of the U.S. Department of Justice. ELEMENTAL ANALYSIS OF GLASS AND PAINT MATERIALS BY LASER ABLATION INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY (LA-ICP-MS) FOR FORENSIC APPLICATION Award No. 2003-IJ-CX-K004 NIJ TECHNICAL REPORT 2006 Tatiana Trejos, Waleska Castro and Jose R. Almirall, Research Programs Coordinator, Doctoral Student and Associate Professor Department of Chemistry and Biochemistry and International Forensic Research Institute Florida International University Miami, Florida August 2006 This document is a research report submitted to the U.S. Department of Justice. This report has not been published by the Department. Opinions or points of view expressed are those of the author(s) and do not necessarily reflect the official position or policies of the U.S. Department of Justice. ABSTRACT Abstract: The elemental analysis of materials has become an important yet underutilized type of evidence at many crime scenes, including scenes of hit-and-run accidents. Although the utility of trace elemental analyses and comparisons for glass or paint fragments has been shown to offer a high degree of discrimination between different sources of these materials, the lack of method development, validation of methods and publication of the results in the open literature have limited the adoption of this technology by the typical forensic laboratory. The proposed research has expanded on prior work in our group (TSWG contract with end date of December 2002) to develop a solution analysis-based standard method for the elemental analysis of glass from a large number of sources and develop a database of data from the analysis of a large number of glasses. One significant disadvantage to solution analysis is the time consuming nature of the sample preparation, using acid digestion of the glasses for metal analysis. The methodology described within this report utilizes a laser ablation-sampling source prior to the ICP-MS analyte detection. A direct comparison of the results for solution and laser ablation analyses also provides additional data to pursue a more comprehensive study of the LA method development for glass comparisons. The results of the studies described within this report and the results of several groups (ie. NITECRIME network) yields excellent precision and low bias for the analysis of glass samples encountered in forensic casework. Glass sample size and sample heterogeneity/homogeneity considerations are also addressed. The results from the analysis of paint samples for forensic purposes are also described. 2 This document is a research report submitted to the U.S. Department of Justice. This report has not been published by the Department. Opinions or points of view expressed are those of the author(s) and do not necessarily reflect the official position or policies of the U.S. Department of Justice. TABLE OF CONTENTS SECTION PAGE SECTION I. INTRODUCTION AND OBJECTIVES................................................. 7 1.1. THE ROLE OF TRACE EVIDENCE IN FORENSIC SCIENCE.............................. 7 1.2. FORENSIC SIGNIFICANCE OF EXAMINATION OF GLASS FRAGMENTS..... 9 1.2.1. History of the glass industry ............................................................. 9 1.2.2. Formulations and raw materials .................................................... 10 1.2.3. Manufacture of glass....................................................................... 13 1.2.4 Transfer and persistence of glass .................................................... 15 1.2.5. Glass Analysis: from physical to elemental analysis...................... 17 1.2.5.1. Physical Examinations..................................................... 17 1.2.5.2. Density ............................................................................. 18 1.2.5.3. Refractive Index............................................................... 19 1.2.5.4. Elemental analysis ........................................................... 19 1.3. FORENSIC EXAMINATION AND COMPARISON OF PAINTS......................... 21 1.3.1 Chemical composition of paint ........................................................ 21 1.3.1.1. Automotive paint ............................................................. 22 1.3.2. Comparison of Analytical Methods for Paint Examinations: Strengths and Limitations ......................................................................... 24 1.3.2.1. Visual and microscopic examination............................... 25 1.3.2.2. Infrared and GC- Pyrolisis............................................... 25 1.3.2.3. Elemental analysis ........................................................... 26 1.3.3. New developments in forensic analysis of paints............................ 26 1.4. ELEMENTAL ANALYSIS OF TRACE EVIDENCE AND ITS SIGNIFICANCE IN COURT............................................................................................................................. 27 1.4.1.Statistical Tools for the evaluation of evidence comparisons.......... 27 1.4.1.1. Descriptive Statistics........................................................ 28 1.4.2. Match criterion for comparisons .................................................... 29 1.4.3. Discrimination potential of elemental analysis .............................. 30 1.5. LASER ABLATION INDUCTIVELY COUPLED MASS SPECTROMETRY ..... 32 1.5.1. Laser Ablation Systems................................................................... 32 1.5.1.1 History of Lasers............................................................... 32 1.5.1.2 Laser Principles................................................................. 33 1.5.1.3 Solid State Lasers.............................................................. 35 1.5.1.4. Principles of LA-ICP-MS ................................................ 37 1.5.3 Optimization and quantification strategies...................................... 39 1.5.3.1 Internal standardization..................................................... 39 1.5.3.2. Calibration curves and single standard calibrations......... 41 1.5.4. Elemental fractionation .................................................................. 42 1.6. LA-ICP-MS OF GLASS AND PAINTS: OBJECTIVES ......................................... 43 3 This document is a research report submitted to the U.S. Department of Justice. This report has not been published by the Department. Opinions or points of view expressed are those of the author(s) and do not necessarily reflect the official position or policies of the U.S. Department of Justice. SECTION II. LA-ICP-MS for GLASS ANALYSIS.................................................. 46 2.1 COMPARISON OF THREE DIFFERENT Nd:YAG LASER SYSTEMS: LSX 200 AND LSX 200+ AND NEW WAVE UP213 ................................................................... 46 2.1.1 Instruments description.................................................................... 46 2.1.1.1 Cetac LSX-200 Plus and LSX 200 ................................... 46 2.1.1.2 New Wave UP213............................................................. 47 2.1.1.2 ICP-MS System ................................................................ 47 2.1.2. Methodology ................................................................................... 48 2.1.2.1 LA-ICP-MS Optimization ................................................ 48 2.1.2.2 LA-ICP-MS Quantification .............................................. 51 2.1.3. Results and Discussion ................................................................... 56 2.1.3.1 Comparison of the two laser systems LSX 200 vs. LSX 200+ .............................................................................................. 56 2.1.4. Conclusions..................................................................................... 66 2.1.4.1 LSX 200 vs. LSX 200+..................................................... 66 2.1.4.2 New Wave UP213 vs. LSX 200+ ..................................... 67 2.2. ANALYSIS OF GLASSES TYPICALLY FOUND IN CRIME SCENES (AUTOMOBILE, CONTAINERS AND HEADLAMPS)............................................... 68 2.2.1. Methodology ................................................................................... 68 2.2.1.1. Sampling Sets .................................................................. 68 2.2.1.2. Samples for homogeneity studies .................................... 70 2.2.1.3. Evaluation of the analytical performance of LA-ICP-MS72 2.2.2. Results and
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