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Standard Test Method for Determination of Calcium, Chlorine, Copper, Magnesium, Phosphorus, Sulfur, and Zinc in Unused Lubricating Oils and Additives by Wavelength Dispersive X-ray Fluorescence Spectrometry (Mathematical Correction Procedure) 用波长分散X射线荧光光谱法测定未使用的润滑油和添加剂中钙、氯、铜、镁、磷、硫和锌的标准试验方法(数学校正程序)
发布日期: 2024-05-01
1.1 本试验方法包括通过波长色散X射线荧光光谱法测定未使用的润滑油、添加剂和添加剂包装中的钙、氯、铜、镁、磷、硫和锌。矩阵效果是通过数学校正来处理的。 1.2 对于每种元素,本试验方法所涵盖的浓度范围的上限由中列出的最高浓度定义 表1 含有较高浓度的样品可以在稀释后进行分析。 1.3 对于每种元素,该测试方法所涵盖的浓度范围的下限可以通过检测限(LOD)来估计 2. (另见40 CFR 136附录B)或定量限(LOQ), 2. 两者都可以从S估计 r ,重复性标准偏差。LOD和LOQ值,根据实验室间精密度研究的结果确定,列于 表2 . 1.3.1 LOD和LOQ不是本试验方法的固有常数。LOD和LOQ取决于实验室在使用该测试方法时可达到的精度。 1.4 该测试方法使用回归软件来确定校准参数,其中可以包括影响系数(即元素间效应系数)(指南 E1361 ),在本文中被称为字母。字母表也可以使用相关软件从理论上确定。 1.5 本测试方法的设置适用于接受过X射线光谱法实践培训的人员。设置之后,可以常规使用此测试方法。 1.6 以SI单位或埃(Å)单位表示的值应单独视为标准。 1.7 本标准并不旨在解决与其使用相关的所有安全问题(如有)。本标准的使用者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。 1.8 本国际标准是根据世界贸易组织技术性贸易壁垒委员会发布的《关于制定国际标准、指南和建议的原则的决定》中确立的国际公认的标准化原则制定的。 ====意义和用途====== 5.1 润滑油可以与添加剂配制,添加剂可以用作清洁剂、抗氧化剂、抗磨剂等。一些添加剂可以含有钙、铜、镁、磷、硫和锌中的一种或多种。该试验方法可用于确定油、添加剂和添加剂包是否符合这些元素含量的规范。 5.2 润滑油中添加了几种添加元素及其化合物,以提供有益的性能( 表3 ). 5.3 该试验方法也可用于确定润滑油、添加剂和添加剂包是否符合氯浓度规范。在这种情况下,规范可以指污染。 5.4 本试验方法不适用于含有严重干扰范围内规定元素分析的某些成分的样品。 5.5 该试验方法可补充润滑油和添加剂的其他试验方法,包括试验方法 D4628 , D4927 , D4951 和 D5185 .
1.1 This test method covers the determination of calcium, chlorine, copper, magnesium, phosphorus, sulfur, and zinc in unused lubricating oils, additives, and additive packages by wavelength dispersive X-ray fluorescence spectrometry. Matrix effects are handled with mathematical corrections. 1.2 For each element, the upper limit of the concentration range covered by this test method is defined by the highest concentration listed in Table 1 . Samples containing higher concentrations can be analyzed following dilution. 1.3 For each element, the lower limit of the concentration range covered by this test method can be estimated by the limit of detection (LOD) 2 (see also 40 CFR 136 Appendix B) or limit of quantification (LOQ), 2 both of which can be estimated from S r , the repeatability standard deviation. LOD and LOQ values, determined from results obtained in the interlaboratory study on precision, are listed in Table 2 . 1.3.1 LOD and LOQ are not intrinsic constants of this test method. LOD and LOQ depend upon the precision attainable by a laboratory when using this test method. 1.4 This test method uses regression software to determine calibration parameters, which can include influence coefficients (that is, interelement effect coefficients) (Guide E1361 ), herein referenced as alphas. Alphas can also be determined from theory using relevant software. 1.5 Setup of this test method is intended for persons trained in the practice of X-ray spectrometry. Following setup, this test method can be used routinely. 1.6 The values stated in either SI units or angstrom (Å) units are to be regarded separately as standard. 1.7 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. 1.8 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 Lubricating oils can be formulated with additives, which can act as detergents, anti-oxidants, anti-wear agents, and so forth. Some additives can contain one or more of calcium, copper, magnesium, phosphorus, sulfur, and zinc. This test method can be used to determine if the oils, additives, and additive packages meet specification with respect to content of these elements. 5.2 Several additive elements and their compounds are added to the lubricating oils to give beneficial performance ( Table 3 ). 5.3 This test method can also be used to determine if lubricating oils, additives, and additive packages meet specification with respect to chlorine concentration. In this context, specification can refer to contamination. 5.4 This test method is not intended for use on samples that contain some component that significantly interferes with the analysis of the elements specified in the scope. 5.5 This test method can complement other test methods for lube oils and additives, including Test Methods D4628 , D4927 , D4951 , and D5185 .
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归口单位: D02.03
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