The Analysis of Small Glass Fragments Using Inductively Coupled Plasma Mass Spectrometry

Abstract

Inductively coupled plasma mass spectrometry using solution nebulization has the ability to analyze up to 70 elements with good precision, accuracy, and sensitivity and is, therefore, well suited for the trace element analysis of glass. However, the technique places severe restrictions on sample preparation. High concentrations of acids or dissolved solids, changes in sample viscosity and molecular compound formation can cause physical, spectral and chemical interference. Solubilization of the glass samples based on a three acid digestion procedure (HF, HNO3, HCl 2:1:1) has been found to minimize these problems. Up to 62 elements have been determined in a range of glass samples. Glasses that could not be distinguished on the basis of refractive index measurement could be discriminated. A procedure of measuring a range of elemental ratios, which eliminated the need for weighing, was used to compare small samples typical of casework.

Forensic Discrimination of Tiny Glass Fragments with Non-flat Surface by Trace Elemental Analysis Using LA-ICP-MS

“…(2) SN ICP MS: To prepare a sample solution for SN ICP MS, small glass fragments from NIST 612 and theˆve sheet glass samples were digested by a procedure adapted from the work of Parouchais et al 20) . Approximately 2 mg of these fragments was accurately weighed, transferred into a 15 mL polypropylene tube, followed by addition of 300 mL of HF, 150 mL of HCl, and 150 mL of HNO 3 .…”

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

“…After being dried in an oven, this piece was crushed into smaller fragments of appropriate size (approximately 2 mg or smaller) with an agate mortar. These glass fragments were decomposed by a procedure adapted from the work of Parouchais et al 31 Approximately 2 mg of these fragments was accurately weighted, transferred into a polypropylene tube of 15 mL, followed by the addition of 300 mL of HF, 150 mL of HCl, and 150 mL of HNO3. After 2 h of ultrasonication with the cap closed, the tube was opened and heated at 80˚C on an aluminum block until the sample was completely dried so as to remove any Si and HF from the tube.…”

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

“…Various techniques of elemental analysis have been proposed for discrimination of glass samples, such as XRF, [2][3][4][5] EPMA, 6 AAS, 7 NAA, 8 ICP-AES, 2,9,10 ICP-MS, [11][12][13] and LA-ICP-MS. 14,15 For discrimination of glass, ICP-MS can widely be used to perform multielemental analysis with higher sensitivity than other techniques. However, it is difficult to apply ICP-MS for analysis of a small glass fragment, since glass samples found at crime scenes are often extremely small.…”