Application of Total Reflection X-ray Fluorescence Spectrometry to Small Glass Fragments

Abstract

Total reflection X-ray fluorescence spectrometry (TXRF) has been applied for trace elemental analysis of small glass fragments. A small glass sample (a fragment with weight less than 0.5 mg) was decomposed by 100 μl of HF/HNO3 acid; the material was condensed to 10 μl and was dried on a Si wafer. Since the size of the dried residue on the Si wafer was less than 1 cm in diameter, an incident X-ray beam with about 1 cm in width could effectively excite elemental components in such a small glass fragment. The precision of the present technique was checked by analyzing the glass fragments (< 0.5 mg) from NIST SRM612; the relative standard deviations (RSD) of less than 8.1% were achieved for elemental ratios that were normalized by Sr. Fragments (< 0.5 mg) obtained from 23 figured sheet glasses were used as samples for estimating the utility of this technique to forensic discrimination. Comparison of five elemental ratios of Ti/Sr, Mn/Sr, Zn/Sr, Rb/Sr, and Pb/Sr calculated from X-ray fluorescence spectra was effective in distinguishing glass fragments that could not be differentiated by their refractive indexes (RI).

Forensic Discrimination of Sheet Glass Exposed to High Temperature by the Determination of Trace Impurities Using ICP-MS

“…A number of studies have reported that comparisons of elemental compositions are useful for the forensic discrimination of glass fragments, 5,6,8,9,12,[15][16][17][18][19][20][21][22][23][24][25][26][27][28][29] and it is not pointed out again in this paper. What should be emphasized here is that a good correlation was observed in the elemental profiles between the non-heated and heated fragments in any of the 5 glasses.…”

“…If tiny glass fragments found on the clothes of a suspect can be proved to originate from the broken window glass, they can be valuable physical evidence to associate the suspect with the crime. [1][2][3][4][5][6] The forensic glass comparison mentioned above has been conducted by measuring the refractive index (RI) [5][6][7][8][9][10][11][12][13][14] and conducting an analysis of the elemental compositions using procedures such as X-ray fluorescence spectrometry (XRF), 6,8,12,[15][16][17][18][19][20][21][22] inductively coupled plasma atomic emission spectrometry (ICP-AES) 8,15,[23][24][25] and mass spectrometry (ICP-MS). 5,6,9,12,18,[26][27][28][29] An RI measurement can be applied to a glass fragment smaller than 0.1 mm in a maximum width without its destruction.…”

X‐Ray Fluorescence in Forensic ScienceUpdate based on the original article by Claude Roux and Chris Lennard,Encyclopedia of Analytical Chemistry, © 2000, John Wiley & Sons, Ltd.

“…However, since there are limitations regarding sample size, destruction of the glass fragment might be required. (1,61) Synchrotron radiation has been increasingly applied for the detection of trace elements to differentiate glass fragments. (58,59,62) amounts of heavy elements present in different samples; e.g.…”

Discrimination of side‐window glass of Korean autos by laser ablation inductively coupled plasma mass spectrometry

“…Glass fragments are often the most common pieces of trace evidence found at crime scenes, such as car accidents and burgled homes, which can be used to identify a suspect . Hence, previous studies have focused on distinguishing sources of broken glass using the physical and optical properties of the glass itself, such as color, thickness, and refractive index, because they involve simple preparation and short analysis time . With increased quality control in glass production, the physical and optical properties of glass have become regulated and now show less variation among products.…”

“…[1,2] Hence, previous studies have focused on distinguishing sources of broken glass using the physical and optical properties of the glass itself, such as color, thickness, and refractive index, because they involve simple preparation and short analysis time. [3][4][5][6][7] With increased quality control in glass production, the physical and optical properties of glass have become regulated and now show less variation among products. Therefore, recent studies have used elemental analysis as an alternative discrimination tool.…”