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Standard Test Method for Sulfur in Petroleum and Petroleum Products by Energy Dispersive X-ray Fluorescence Spectrometry 用能量色散X射线荧光光谱法测定石油和石油产品中硫的标准试验方法
发布日期: 2021-12-01
1.1 本试验方法包括测定石油和石油产品中的总硫,这些石油和石油产品是单相的,在环境条件下为液态,可在中热下液化,或可溶于烃类溶剂。这些材料包括柴油、喷气燃料、煤油、其他馏出油、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(见 注释2 )和类似的石油产品。 注1: 乙醇或甲醇含量超过 表1 可以使用此测试方法处理,但精度和偏差声明不适用(参见 附录X3 ). 注2: 对于含氧量高(>3)的样品 % 按重量)样品稀释,如 1.3 或必须进行矩阵匹配以确保结果准确。 1.2 实验室间精密度研究显示范围为17 mg/kg至4。 6. % 按质量计算。本试验方法的混合定量限(PLOQ)估计为16.0 按实际程序计算的mg/kg D6259 . 然而,由于本试验方法涵盖的仪器灵敏度可能不同,因此必须单独确定硫浓度低于约20 mg/kg时试验方法的适用性。检测限的估计值是再现性标准差的三倍,定量限的估计值 2. 是再现性标准偏差的十倍。 1.3 含4.6以上的样品 % 可以按质量稀释硫,使稀释材料的硫浓度在本试验方法的范围内。稀释后的样品可能比第节中所示的误差更大 17 比非稀释样品。 1.4 挥发性样品(如高蒸气压汽油或轻烃)可能不符合规定的精度,因为在分析过程中会选择性损失轻物质。 1.5 本试验方法中的一个基本假设是,标准矩阵和样本矩阵匹配良好,或者考虑了矩阵差异(参见 6.2 ). 样品和标准品之间的C/H比差异可能导致基质不匹配(见第节) 6. )或者通过其他杂原子的存在。 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。 1.8 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》中确立的国际公认标准化原则制定的。 ====意义和用途====== 5.1 本试验方法提供了对石油和石油产品中总硫的快速准确测量,只需最少的样品制备。典型分析时间为1 最小值至5 每个样品的最小值。 5.2 许多石油产品的质量与含硫量有关。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 本试验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监管限制的方法。 5.4 当本试验方法适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. 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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