1.1 本试验方法包括通过电感耦合等离子体原子发射光谱法（ICP-AES）技术测定未使用润滑脂中的铝、锑、钡、钙、铁、锂、镁、钼、磷、硅、钠、硫和锌等多种金属。 1.1.1 该试验方法的适用范围基于2005年进行的实验室间研究， 2. 是铝（10至600）、锑（10至2300）、钡（50至800）、钙（20至50 000）、铁（10至360）、锂（300至3200）、镁（30至10 000）、钼（50至22 000）、磷（50至2000）、硅（10至15 000）、钠（30-1500）、硫（1600-28 000）和锌（300至2200），全部以mg/kg为单位。 较低水平的元素可通过使用较大的样品重量来确定，而较高水平的元素可以通过使用较小量的样品或通过在样品溶解后使用较大的稀释因子来确定。然而，这种情况下的测试精度尚未确定，可能与表3中给出的精度不同。 1.1.2 还可以通过该技术测定其他金属，如铋、硼、镉、铬、铜、铅、锰、钾、钛等。然而，没有足够的数据来指定后一种测定的精度。 这些金属可能通过污染或作为添加剂元素来源于润滑脂。 1.1.3 在样品制备过程中，润滑脂样品被各种酸混合物分解。为样品中存在的所有可能的金属组合指定合适的酸混合物超出了本试验方法的范围。但是，如果灰分溶解导致任何可见的不溶性物质，假设不溶性材料含有一些感兴趣的分析物，则该测试方法可能不适用于所分析的润滑脂类型。 1.2 浓度高于校准曲线上限的元素可以通过对溶解样品进行额外的适当稀释来确定，并且不会降低精度。 1.3 福克斯记录了这种测试方法背后技术的发展。 3. 1.4 以国际单位制表示的数值应视为标准。括号中给出的值仅供参考。 1.5 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。 具体警告说明见第节 8. 和 10 。 1. 6. 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 润滑脂几乎用于任何机械中使用的所有轴承。润滑脂由~90组成 % 添加的油和肥皂或其他增稠剂。润滑脂中存在十几种金属元素，它们要么作为添加剂混合以提高性能，要么作为增稠剂，要么在使用过的润滑脂中作为污染物和磨损金属存在。 确定它们的浓度可能是润滑脂制造的一个重要方面。金属含量还可以指示润滑脂中增稠剂的量。此外，可靠的分析技术也可以帮助解决现场新润滑脂和旧润滑脂的故障。 5.2 尽管在石油工业的其他部门广泛用于金属分析，但基于ICP-AES的测试方法 D4951 或 D5185 不能用于分析润滑脂，因为它们在这些测试方法中使用的有机溶剂中不溶。因此，在ICP之前，需要通过酸分解将润滑脂样品带入水溶液中- AES测量。 5.3 试验方法 D3340 已用于使用火焰光度法测定润滑脂中的锂和钠含量。这种技术不再被广泛使用。这种新的测试方法为油脂样品的多元分析提供了一种测试方法。这是第一个可用于润滑脂多元素同时分析的D02标准。

1.1 This test method covers the determination of a number of metals such as aluminum, antimony, barium, calcium, iron, lithium, magnesium, molybdenum, phosphorus, silicon, sodium, sulfur, and zinc in unused lubricating greases by inductively coupled plasma atomic emission spectrometry (ICP-AES) technique. 1.1.1 The range of applicability for this test method, based on the interlaboratory study conducted in 2005, 2 is aluminum (10 to 600), antimony (10 to 2300), barium (50 to 800), calcium (20 to 50 000), iron (10 to 360), lithium (300 to 3200), magnesium (30 to 10 000), molybdenum (50 to 22 000), phosphorus (50 to 2000), silicon (10 to 15 000), sodium (30 to 1500), sulfur (1600 to 28 000), and zinc (300 to 2200), all in mg/kg. Lower levels of elements may be determined by using larger sample weights, and higher levels of elements may be determined by using smaller amounts of sample or by using a larger dilution factor after sample dissolution. However, the test precision in such cases has not been determined, and may be different than the ones given in Table 3. 1.1.2 It may also be possible to determine additional metals such as bismuth, boron, cadmium, chromium, copper, lead, manganese, potassium, titanium, etc. by this technique. However, not enough data is available to specify the precision for these latter determinations. These metals may originate into greases through contamination or as additive elements. 1.1.3 During sample preparation, the grease samples are decomposed with a variety of acid mixture(s). It is beyond the scope of this test method to specify appropriate acid mixtures for all possible combination of metals present in the sample. But if the ash dissolution results in any visible insoluble material, the test method may not be applicable for the type of grease being analyzed, assuming the insoluble material contains some of the analytes of interest. 1.2 Elements present at concentrations above the upper limit of the calibration curves can be determined with additional appropriate dilutions of dissolved samples and with no degradation of precision. 1.3 The development of the technique behind this test method is documented by Fox. 3 1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only. 1.5 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. Specific warning statements are given in Sections 8 and 10 . 1.6 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 greases are used in almost all bearings used in any machinery. Lubricating grease is composed of ~90 % additized oil and soap or other thickening agent. There are over a dozen metallic elements present in greases, either blended as additives for performance enhancements or as thickeners, or in used greases present as contaminants and wear metals. Determining their concentrations can be an important aspect of grease manufacture. The metal content can also indicate the amount of thickeners in the grease. Additionally, a reliable analysis technique can also assist in the process of trouble shooting problems with new and used grease in the field. 5.2 Although widely used in other sectors of the oil industry for metal analysis, ICP-AES based Test Methods D4951 or D5185 cannot be used for analyzing greases because of their insolubility in organic solvents used in these test methods. Hence, grease samples need to be brought into aqueous solution by acid decomposition before ICP-AES measurements. 5.3 Test Method D3340 has been used to determine lithium and sodium content of lubricating greases using flame photometry. This technique is no longer widely used. This new test method provides a test method for multi-element analysis of grease samples. This is the first D02 standard available for simultaneous multi-element analysis of lubricating greases.