71.040.40 (Chemical analysis); 81.040.10 (Raw mate 标准查询与下载

ASTM E2927-13 鉴识比较用激光烧蚀感应耦合等离子体质谱法测定钠钙玻璃样品微量元素的标准试验方法

4.1 This test method is useful for the determination of elemental concentrations in the microgram per gram (µgg-1) to percent (%) levels in soda-lime glass samples. A standard test method can aid in the interchange of data between laboratories and in the creation and use of glass databases. 4.2 The determination of elemental concentrations in glass provides high discriminating value in the forensic comparison of glass fragments. 4.3 This test method produces minimal destruction of the sample. Microscopic craters of 50 to 100 µm in diameter by 80 to 150-µm deep are left in the glass fragment after analysis. The mass removed per replicate is approximately 0.4 to 3.1 µg. 4.4 Appropriate sampling techniques should be used to account for natural heterogeneity of the materials at a microscopic scale. 4.5 The precision, accuracy, and limits of detection of the method (for each element measured) should be established in each laboratory that employs the method. The measurement uncertainty of any concentration value used for a comparison should be recorded with the concentration. 4.6 Acid digestion of glass followed by either Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) or Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) may also be used for trace elemental analysis of glass, and offer similar detection levels and the ability for quantitative analysis. However, these methods are destructive, and require larger sample sizes and much longer sample preparation times (Test Method E2330). 4.7 Micro X-Ray Fluorescence (µ-XRF) uses comparable sample sizes to those used for LA-ICP-MS with the advantage of being non-destructive of the sample. Some of the drawbacks of µ-XRF are poorer sensitivity and precision, and longer analysis time. 4.8 Scanning Electron Microscopy with EDS (SEM-EDS) is also available for elemental analysis, but it is of limited use for forensic glass source discrimination due to poor detection limits for higher atomic number elements present in glass at trace concentration levels. However, distinguishing between sources having similar RIs and densities is possible. 1.1 This test method covers a procedure for the quantitative elemental analysis of the following seventeen elements: lithium (Li), magnesium (Mg), aluminum (Al), potassium (K), calcium (Ca), iron (Fe), titanium (Ti), manganese (Mn), rubidium (Rb), strontium (Sr), zirconium (Zr), barium (Ba), lanthanum (La), cerium (Ce), neodymium (Nd), hafnium (Hf) and lead (Pb) through the use of Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) for the forensic comparison of glass fragments. The potential of these elements to provide the best discrimination among different sources of soda-lime glasses has been published elsewhere (1-5).2 Silicon (Si) is also monitored for use as an internal standard. Additional elements can be added as needed, for example, tin (Sn) can be used to monitor the orientation of float glass fragments. 1.2 The method only consumes approximately 0.4 to 2 g of glass per replicate and is suitable for the analysis of full thickness samples as well as irregularly shaped fragments as small as 0.1 mm by 0.4 mm in dimension. The concentrations of the elements ......

Standard Test Method for Determination of Trace Elements in Soda-Lime Glass Samples Using Laser Ablation Inductively Coupled Plasma Mass Spectrometry for Forensic Comparisons

ASTM E2330-12 使用法医比对用电感耦合等离子体质量色谱法 (ICP-MS) 测定玻璃样品中元素含量的标准试验方法

This technique is destructive, in that the glass fragments may need to be crushed, and must be digested in acid. Although the concentration ranges of the calibration curves shown in Appendix X1 are applicable to soda lime and borosilicate glass, this method is useful for the accurate measurement of element concentrations from a wide variety of glass samples. The determination of the element concentrations in glass yields data that can be used to compare fragments. It should be recognized that the method measures the bulk concentration of the target elements. Any extraneous material present on the glass that is not removed before digestion may result in inaccurate concentrations of the measured elements. The precision and accuracy of the method should be established in each laboratory that employs the method. 1.1 One objective of a forensic glass examination is to compare glass samples to determine if they can be discriminated using their physical, optical or chemical properties (for example, color, refractive index (RI), density, elemental composition). If the samples are distinguishable in any of these observed and measured properties, it may be concluded that they did not originate from the same source of broken glass. If the samples are indistinguishable in all of these observed and measured properties, the possibility that they originated from the same source of glass cannot be eliminated. The use of an elemental analysis method such as inductively coupled plasma mass spectrometry yields high discrimination among sources of glass. 1.2 This test method covers a procedure for quantitative determination of the concentrations of magnesium (Mg), aluminum (Al), iron (Fe), titanium (Ti), manganese (Mn), rubidium (Rb), strontium (Sr), zirconium (Zr), barium (Ba), lanthanum (La), cerium (Ce), neodymium (Nd), samarium (Sm), and lead (Pb) in glass samples. 1.3 This procedure is applicable to irregularly shaped samples as small as 200 micrograms, for the comparison of fragments of a known source to the recovered fragments from a questioned source. These elements are present in soda lime and borosilicate glass in ppb to % levels 1.4 This procedure is applicable to other elements, other types of glass, and other concentration ranges with appropriate modifications of the digestion procedure (if needed for full recovery of the additional elements), calibration standards and the mass spectrometer conditions. Calcium and potassium, for example, could be added to the list of analytes in a modified analysis scheme. Alternative methods for the determination of concentrations of elements in glass are listed in the references. 1.5 For any given glass, approximately 40 elements are likely to be present at detectable concentrations using this procedure with minor modifications. The element set stated here is an example of some of these elements that can be detected in glass and used for forensic comparisons. 1.6 This guide cannot replace knowledge, skill, or ability acquired through appropriate education, training, and experience and should be used in conjunction with sound professional judgment. 1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.8 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

Standard Test Method for Determination of Concentrations of Elements in Glass Samples Using Inductively Coupled Plasma Mass Spectrometry (ICP-MS) for Forensic Comparisons

ASTM E2330-04 用感应耦合等离子体质谱法(ICP-MS)测定玻璃样品中痕量元素的标准试验方法

This technique is destructive, in that the glass fragments may need to be crushed, and must be digested in acid. Although the concentration ranges of the calibration curves shown in Appendix X1 are applicable to soda lime and borosilicate glass, this method is useful for the accurate measurement of trace elements from a wide variety of glass samples. The determination the elemental concentrations in glass allows for additional data that can be compared between fragments. A standardized, validated method can aid in the interchange of data between laboratories. It should be recognized that the method measures the bulk concentration of the target elements. Any extraneous material present on the glass that is not removed before digestion may result in a measurably different concentration of the elements. The precision and accuracy of the method should be established in each laboratory that employs the method. Confidence intervals or a similar statistical quality statement should be quoted along with any reported concentration value.1.1 This test method covers a procedure for elemental analysis of magnesium (Mg), aluminum (Al, titanium (Ti), manganese (Mn), gallium (Ga), rubidium (Rb), strontium (Sr), zirconium (Zr), antimony (Sb), barium (Ba), lanthanum (La), cerium (Ce), samarium (Sm), hafnium (Hf) and lead (Pb) in the bulk of glass samples (irregularly shaped and as small as 200 micrograms) for the comparison of fragments of a known source to the recovered fragments from a questioned source. These elements are present in soda lime and borosilicate glass in ngg-1 to % levels. Alternative methods for the determination of elemental analysis of glass are listed in the references. This procedure may also be applicable to other elements, other types of glass, or other concentration ranges with appropriate modifications of the digestion procedure (if needed for full recovery of the additional elements) and the mass spectrometer conditions. The addition of calcium and potassium, for example, could be added to the list of analytes in a modified analysis scheme.This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

Standard Test Method for Determination of Trace Elements in Glass Samples Using Inductively Coupled Plasma Mass Spectrometry (ICP-MS)