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Standard Test Method for Determination of Concentrations of Elements in Glass Samples Using Inductively Coupled Plasma Mass Spectrometry (ICP-MS) for Forensic Comparisons 使用电感耦合等离子体质谱法(ICP-MS)进行法医比较的玻璃样品中元素浓度测定的标准测试方法
发布日期: 2019-12-01
1.1 法医玻璃检查的一个目标是比较玻璃样品,以确定是否可以使用其物理、光学或化学特性(例如,颜色、折射率(RI)、密度、元素组成)对其进行鉴别。如果样品在这些观察和测量的属性中可以区分,则可以得出结论,它们并非来自同一来源的碎玻璃。如果样品在所有这些观察和测量的特性中无法区分,则无法消除它们来自同一玻璃来源的可能性。使用元素分析方法(如电感耦合等离子体质谱法)可以在玻璃源之间产生高度的区分。 ( 1- 16 ) 2. 1.2 本试验方法涵盖了定量测定玻璃样品中镁(Mg)、铝(Al)、铁(Fe)、钛(Ti)、锰(Mn)、铷(Rb)、锶(Sr)、锆(Zr)、钡(Ba)、镧(La)、铈(Ce)、钕(Nd)、钐(Sm)和铅(Pb)浓度的程序。 1.3 该程序适用于小至200微克的不规则形状样品,用于将已知来源的碎片与来自可疑来源的回收碎片进行比较。这些元素以μg/L至%的水平存在于钠石灰和硼硅酸盐玻璃中。 1.4 本程序适用于其他元素、其他类型的玻璃和其他浓度范围,并适当修改消解程序(如果需要完全回收其他元素)、校准标准和质谱仪条件。 例如,可以在修改的分析方案中将钙和钾添加到分析物列表中。参考文献中列出了测定玻璃中元素浓度的替代方法。 1.5 对于任何给定的玻璃,使用该程序,只要稍加修改,大约40种元素可能以可检测浓度存在。这里所述的元素集是其中一些元素的示例,这些元素可以在玻璃中检测并用于法医学比较。 1.6 以国际单位制表示的数值应视为标准值。本标准不包括其他计量单位。 1.7 本标准不能取代通过教育、培训和经验获得的知识、技能或能力,并由具有此类纪律的个人结合专业判断使用- 特定的知识、技能和能力。 1.8 本标准并非旨在解决与其使用相关的所有安全问题(如有)。本标准的用户有责任在使用前制定适当的安全、健康和环境实践,并确定监管限制的适用性。 1.9 本国际标准是根据世界贸易组织技术性贸易壁垒(TBT)委员会发布的《关于制定国际标准、指南和建议的原则的决定》中确立的国际公认标准化原则制定的。 ====意义和用途====== 4.1 这种技术具有破坏性,因为玻璃碎片可能需要压碎,并在酸中消化。 4.2 尽管校准曲线的浓度范围如所示 附录X1 适用于钠钙和硼硅酸盐玻璃,该方法有助于从各种玻璃样品中准确测量元素浓度。 4.3 玻璃中元素浓度的测定产生了可用于比较碎片的数据。 4.4 应该认识到,该方法测量目标元素的体积浓度。玻璃上存在的任何外来物质在消化前未去除,可能会导致测量元素的浓度不准确。 4.5 应在使用该方法的每个实验室中确定该方法的精密度和准确度。
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- 16 ) 2 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 μg/L 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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.7 This standard cannot replace knowledge, skills, or abilities acquired through education, training, and experience and is to be used in conjunction with professional judgment by individuals with such discipline-specific knowledge, skills, and abilities. 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. 1.9 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee. ====== Significance And Use ====== 4.1 This technique is destructive, in that the glass fragments may need to be crushed, and digested in acid. 4.2 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. 4.3 The determination of the element concentrations in glass yields data that can be used to compare fragments. 4.4 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 can result in inaccurate concentrations of the measured elements. 4.5 The precision and accuracy of the method should be established in each laboratory that employs the method.
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发布单位或类别: 美国-美国材料与试验协会
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归口单位: E30.01
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