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Standard Test Method for Sulfur in Petroleum and Petroleum Products by Energy Dispersive X-ray Fluorescence Spectrometry 石油和石油产品中硫的能量分散X射线荧光光谱法的标准测试方法
发布日期: 2024-12-01
1.1 本试验方法涵盖了石油和石油产品中总硫的测定,这些石油和石油产品是单相的,在环境条件下为液体,可在中等热量下液化,或可溶于烃类溶剂。这些材料可以包括柴油、喷气燃料、煤油、其它馏分油、石脑油、渣油、润滑基础油、液压油、原油、无铅汽油、汽油-乙醇混合物、生物柴油(参见 附注2 )和类似的石油产品。 附注1: 乙醇或甲醇含量超过中规定限值的含氧燃料 表1 可以使用该测试方法进行处理,但精密度和偏倚声明不适用(参见 附录X3 ). 附注2: 对于氧含量高(>3%重量)的样品,样品稀释如中所述 1.3 或必须执行矩阵匹配以确保准确的结果。1.2 实验室间精密度研究显示范围为17 mg/kg至4.6%(质量)。根据实际操作程序计算,该检测方法的合并定量限(PLOQ)估计值为16.0 mg/kg D6259 然而,由于该测试方法所涵盖的仪器的灵敏度可能不同,因此必须在个体基础上确定该测试方法在硫浓度低于约20 mg/kg时的适用性。检测限的估计值是重现性标准偏差的三倍,定量限的估计值 2 是重现性标准偏差的十倍。 1.3 含硫超过4.6质量%的样品可以稀释,使稀释后材料的硫浓度在本试验方法的范围内。稀释后的样品可能具有比第节所示更高的误差 17 比未稀释的样品。 1.4 挥发性样品(如高蒸气压汽油或轻质碳氢化合物)可能不符合规定的精密度,因为在分析过程中轻质物质的选择性损失。 1.5 该测试方法的一个基本假设是标准和样品基质匹配良好,或者基质差异得到考虑(见 6.2 ).基质不匹配可能是由样品和标准品之间的C/H比差异引起的(参见第节 6 )或通过其它杂原子的存在。 1.6 以SI单位表示的值将被视为标准值。本标准不包括其他计量单位。 1.7 本标准并不旨在解决与其使用相关的所有安全性问题(如果有)。本标准的使用者有责任在使用前建立适当的安全、健康和环境实践并确定法规限制的适用性。 1.8 本国际标准是根据世界贸易组织技术性贸易壁垒(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》中确立的国际公认的标准化原则制定的。 ======意义和用途====== 5.1 该测试方法只需最少的样品制备即可快速、精确地测量石油和石油产品中的总硫。每个样品的典型分析时间为1分钟至5分钟。 5.2 许多石油产品的质量与硫的含量有关。硫浓度的知识对于加工目的是必要的。联邦、州和地方机构也颁布了限制某些燃料中硫含量的法规。 5.3 该测试方法提供了一种确定石油或石油产品的硫含量是否符合规范或法规限值的方法。 5.4 当本试验方法应用于基质与中规定的校准材料显著不同的石油材料时 10.1 ,第节中的注意事项和建议 6 在解释结果时应遵守。
1.1 This test method covers the determination of total sulfur in petroleum and petroleum products that are single-phase and either liquid at ambient conditions, liquefiable with moderate heat, or soluble in hydrocarbon solvents. These materials can include diesel fuel, jet fuel, kerosine, other distillate oil, naphtha, residual oil, lubricating base oil, hydraulic oil, crude oil, unleaded gasoline, gasoline-ethanol blends, biodiesel (see Note 2 ), and similar petroleum products. Note 1: Oxygenated fuels with ethanol or methanol contents exceeding the limits given in Table 1 can be dealt with using this test method, but the precision and bias statements do not apply (see Appendix X3 ). Note 2: For samples with high oxygen contents (>3 % by weight) sample dilution as described in 1.3 or matrix matching must be performed to assure accurate results. 1.2 Interlaboratory studies on precision revealed the scope to be 17 mg/kg to 4.6 % by mass. An estimate of this test method’s pooled limit of quantitation (PLOQ) is 16.0 mg/kg as calculated by the procedures in Practice D6259 . However, because instrumentation covered by this test method can vary in sensitivity, the applicability of the test method at sulfur concentrations below approximately 20 mg/kg must be determined on an individual basis. An estimate of the limit of detection is three times the reproducibility standard deviation, and an estimate of the limit of quantitation 2 is ten times the reproducibility standard deviation. 1.3 Samples containing more than 4.6 % by mass sulfur can be diluted to bring the sulfur concentration of the diluted material within the scope of this test method. Samples that are diluted can have higher errors than indicated in Section 17 than non-diluted samples. 1.4 Volatile samples (such as high vapor pressure gasolines or light hydrocarbons) may not meet the stated precision because of selective loss of light materials during the analysis. 1.5 A fundamental assumption in this test method is that the standard and sample matrices are well matched, or that the matrix differences are accounted for (see 6.2 ). Matrix mismatch can be caused by C/H ratio differences between samples and standards (see Section 6 ) or by the presence of other heteroatoms. 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 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 This test method provides rapid and precise measurement of total sulfur in petroleum and petroleum products with a minimum of sample preparation. A typical analysis time is 1 min to 5 min per sample. 5.2 The quality of many petroleum products is related to the amount of sulfur present. Knowledge of sulfur concentration is necessary for processing purposes. There are also regulations promulgated in federal, state, and local agencies that restrict the amount of sulfur present in some fuels. 5.3 This test method provides a means of determining whether the sulfur content of petroleum or a petroleum product meets specification or regulatory limits. 5.4 When this test method is applied to petroleum materials with matrices significantly different from the calibration materials specified in 10.1 , the cautions and recommendations in Section 6 should be observed when interpreting results.
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归口单位: D02.03
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