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Standard Test Method for Elemental Analysis of Distillate Products by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) 用电感耦合等离子体质谱法(ICP-MS)对馏出物产品进行元素分析的标准试验方法
发布日期: 2017-05-01
1.1 本试验方法描述了使用电感耦合等离子体质谱(ICP-MS)测定轻馏分和中间馏分石油产品中微量元素的程序。 1.2 本试验方法应由在使用电感耦合等离子体质谱(ICP-MS)方面经验丰富的分析员使用,分析员应了解光谱、等压、多原子和基质干扰的解释,以及校正或减少干扰的程序。 1.3 中的表 6.1 列出了试验方法适用的元素以及推荐的同位素。实际工作检测限取决于样本,随着样本矩阵的变化,这些检测限也可能变化。 1.4 本试验方法的浓度范围通常为从低到亚纳克/克(ppb质量)到1000纳克/克(ppb质量),但是,根据ILS中分析的试验样品,针对较小的浓度范围规定了精度和偏差声明,见第节中的表 18 . 试验方法可用于该范围以外的浓度;但是,精度声明可能不适用。 1.4.1 应进一步开发该试验方法,以扩展该表,以包括其他元素。 1.5 本试验方法使用金属有机标准物(有机金属或有机可溶性金属络合物)进行校准,并不旨在定量测定不溶性颗粒。分析结果取决于粒径,对于大于几微米的颗粒,结果较低,因为这些颗粒可能在样品容器中沉淀,并且无法通过样品引入系统有效运输。 1.6 浓度高于校准曲线上限的元素可以通过额外的适当稀释确定,且精度不会降低。 1.7 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。 1.8 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和健康实践,并确定监管限制的适用性。 具体警告声明见 8.2 , 8.7 ,和截面 9 . 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====== 5.1 石油产品可能含有微量元素(例如,纳克/克(ppb质量))或微量到大量元素(ppm质量百分比)。 这些元素可能是原油的特征,或者可能来自添加剂的特定内含物,以便在精制产品中发挥有益作用。通常,此类添加剂具有产品规格,用于控制商业产品的质量。因此,尽可能准确地确定这些元素很重要。其他微量元素可能对内燃机有害,导致磨损或性能降低,可能导致催化剂中毒,或者可能与燃烧排放物一样引起环境问题。ICP-MS仪器非常适合测定这些元素,尤其适用于测定其他技术可能无法实现的微量元素。 5.2 各种元素分析技术,例如原子吸收光谱法(AAS),测试方法 D3605 和 D4628 ; 电感耦合等离子体原子发射光谱法(ICP-AES),例如,测试方法 D7111 , D4951 和 D5185 ; 例如,X射线荧光(XRF)实践 D7343 ,试验方法 D7220 ,试验方法 D4927 ,以及试验方法 D6443 ; 或石墨炉原子吸收光谱法(GFAAS),例如,测试方法 D6732 用于此目的。本试验方法是ICP-MS用于石油产品元素分析的第一个示例。 5.3 本试验方法涵盖馏出石油产品中七种元素的快速测定。每个试样的测试时间约为几分钟,大多数元素的定量在低至亚纳克/克(ppb质量)范围内。对于其他技术难以确定的某些元素,可以实现高分析灵敏度。
1.1 This test method describes the procedure for the determination of trace elements in light and middle distillate petroleum products using inductively coupled plasma mass spectrometry (ICP-MS). 1.2 This test method should be used by analysts experienced in the use of inductively coupled plasma mass spectrometry (ICP-MS) with knowledge of interpretation of spectral, isobaric, polyatomic, and matrix interferences, as well as procedures for their correction or reduction. 1.3 The table in 6.1 lists elements for which the test method applies along with recommended isotope. Actual working detection limits are sample dependent and, as the sample matrix varies, these detection limits may also vary. 1.4 The concentration range of this test method is typically from low to sub ng/g (ppb mass) to 1000 ng/g (ppb mass), however the precision and bias statement is specified for a smaller concentration range based on test samples analyzed in the ILS, see the table in Section 18 . The test method may be used for concentrations outside of this range; however, the precision statements may not be applicable. 1.4.1 This test method shall be further developed to extend that table to include additional elements. 1.5 This test method uses metallo-organic standards (organometallic or organosoluble metal complex) for calibration and does not purport to quantitatively determine insoluble particulates. Analytical results are particle size dependent, and low results are obtained for particles larger than a few micrometers as these particles may settle out in the sample container and are not effectively transported through the sample introduction system. 1.6 Elements present at concentrations above the upper limit of the calibration curves can be determined with additional, appropriate dilutions and with no degradation of precision. 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. Specific warning statements are given in 8.2 , 8.7 , and Section 9 . 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 ====== 5.1 Petroleum products may contain elements either in trace concentrations (for example, ng/g (ppb mass)) or in minor to major levels (ppm to mass %). These elements might be characteristic of the crude petroleum or might originate from specific inclusions of additives for beneficial effect in the refined product. Often, such additives have product specifications which control the quality of a product in commerce. Hence, it is important to determine these elements as accurately as possible. Other elements present at trace levels may be harmful to combustion engines causing wear or reduced performance, may cause poisoning of catalysts, or may be of environmental concern as combustion emissions. ICP-MS instrumentation is well-suited for determining these elements and is particularly useful for the determination of the trace level elements that may not be readily achieved by other techniques. 5.2 Various elemental analytical techniques such as atomic absorption spectrometry (AAS), for example, Test Method D3605 and D4628 ; inductively coupled plasma atomic emission spectrometry (ICP-AES), for example, Test Methods D7111 , D4951 , and D5185 ; X-ray fluorescence (XRF), for example, Practice D7343 , Test Method D7220 , Test Methods D4927 , and Test Method D6443 ; or graphite furnace atomic absorption spectrometry (GFAAS), for example, Test Method D6732 are used for this purpose. This test method is the first example where ICP-MS is used for elemental analysis of petroleum products. 5.3 This test method covers the rapid determination of seven elements in distillate petroleum products. Test times approximate a few minutes per test specimen, and quantification for most elements is in the low to sub ng/g (ppb mass) range. High analysis sensitivity can be achieved for some elements that are difficult to determine by other techniques.
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