X射线荧光光谱法测定燃料中硫各标准的合并定量限（PLOQ），重复性，再现性 实验数据的再现性及重复性的计算 有关XRF的常见术语和问答（1） 有关XRF的常见术语和问答（2） 有关XRF的常见术语和问答（3） 有关XRF的常见术语和问答（4）

GB/T 17040—2019 石油和石油产品中硫含量的测定能量色散X射线荧光光谱法 NB/SH/T 0842—2017轻质液体燃料中硫含量的测定单波长色散X射线荧光光谱法 ASTM D7039 − 15a用单色波长色散X射线荧光光谱法测定汽油、柴油、航空燃料、煤油、生物柴油、生物柴油混合物和汽油-乙醇混合物中硫的标准试验方法-英中对照 GB/T 11140-2008石油产品硫含量的测定 波长色散X射线荧光光谱法 ASTM D2622 − 16波长色散x射线荧光光谱法测定石油产品中硫的标准试验方法-英中对照 ISO 20884石油产品–汽车燃料中硫含量的测定–波长色散X射线荧光光谱法 ASTM D7220 − 12 (Reapproved 2017)用单色能量色散x射线荧光光谱法测定汽车燃料、加热燃料和喷气燃料中硫的标准试验方法-英中对照 ASTM D7536 − 16用单色波长色散X射线荧光光谱法测定芳烃中氯的标准试验方法-英中对照 ASTM D4929 − 17原油中有机氯化物含量测定的标准试验方法-英中对照

技术简介 文档下载

Designation: D2622 − 16

Standard Test Method for

Sulfur in Petroleum Products by Wavelength Dispersive X-ray Fluorescence Spectrometry

波长色散x射线荧光光谱法测定石油产品中硫的标准试验方法

1.Scope* 范围

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, kerosene, other distillate oil, naphtha, residual oil, lubricating base oil, hydraulic oil, crude oil, unleaded gasoline, gasoline-ethanol blends, and biodiesel.

1.2 The range of this test method is between the PLOQ        value (calculated by procedures consistent with Practice D6259) of 3 mg/kg total sulfur and the highest level sample in the round robin, 4.6 weight % total sulfur.

N_OTE 1—Instrumentation covered by this test method can vary in sensitivity. The applicability of the test method at sulfur concentrations below 3 mg ⁄kg may be determined on an individual basis for WDXRF instruments capable of measuring lower levels, but precision in this test method does not apply.

1.2.1 The values of the limit of quantitation (LOQ) and    method precision for a specific laboratory’s instrument depends on instrument source power (low or high power), sample type, and the practices established by the laboratory to perform the method.

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，在环境条件下是液态的，可在中等温度下液化，或可溶于烃类溶剂。这些材料可以包括柴油、喷气燃料、煤油、其他馏出油、石脑油、残油、润滑基础油、液压油、原油、无铅汽油、汽油-乙醇混合物和生物柴油。

1.2 本试验方法的范围为3 mg/kg总硫的PLOQ值（按照与实施规程D6259一致的程序计算）与循环中的最高水平样品4.6 %（重量）总硫之间。

注1：本试验方法涵盖的仪器灵敏度可能不同。对于能够测量较低水平的WDXRF仪器，可单独确定硫浓度低于3 mg/kg时试验方法的适用性，但本试验方法中的精度不适用。

1.2.1 特定实验室仪器的定量限（LOQ）和方法精密度的值取决于仪器光源功率（低功率或高功率）、样品类型和实验室为执行该方法而建立的实施规程。

14.Precision and Bias 精度和偏差

14.1 The precision of the test method was determined by statistical analysis of results obtained an interlaboratory study⁶ that included 27 samples including gasolines, distillates, biodiesel, residual oils, and crude oils. A pooled limit of quantitation (PLOQ) of approximately 3 mg/kg S was determined for all sample types. Precision for gasoline and diesel samples for high-power source XRF instruments is included in Appendix X1. The ranges of sulfur concentrations represented by the sample sets, together with the precisions, are listed in 14.1.1 and 14.1.2. These statistics apply only to samples having less than the level of interfering materials present shown in Table 1 (see also 1.4).

14.1.1 Repeatability—The difference between successive test results obtained by the same operator with the same apparatus under constant operating conditions on identical test material would, in the long run, in the normal and correct   operation of the test method exceed the following values only in one case in twenty. Repeatability (r) may be calculated as shown in Eq 12 or Eq 13 for all materials covering the full       scope of this method. See Table 4 for calculated values.

14.1 通过对实验室间研究⁶所得结果的统计分析，确定试验方法的精密度，该研究包括27个样品，包括汽油、馏分油、生物柴油、渣油和原油。对所有样品类型确定了大约3 mg/kg S的合并定量限（PLOQ）。高功率光源X射线荧光仪器对汽油和柴油样品的精密度包含在附录X1中。14.1.1和14.1.2中列出了由样品组表示的硫浓度范围和精度。这些统计数据仅适用于小于表1所示干扰物质水平的样品（另见1.4）。

14.1.1 重复性--在长期运行中，在测试方法的正常和正确操作的情况下，由同一操作者在恒定操作条件下，对相同测试材料，使用同一仪器获得的连续结果之间的差异，二十个中仅有一个超过以下值。对于涵盖本方法全部范围的所有材料，可以如公式12或公式13所示计算重复性(r)。计算值见表4。

Repeatability（r）= 0.1462·X^0.8015 mg/kg       (12)

Repeatability（r）= （0.1462·（（Y·10000）^0.8015））/10000 mass %       (13)

where:

X =   sulfur concentration in mg/kg total sulfur, and

Y =   sulfur concentration in mass % total  sulfur.

式中：

X = 总硫的硫浓度,以mg/kg为单位，以及

Y = 总硫的硫浓度，以质量%为单位。

14.1.2 Reproducibility—The difference between two single and independent results obtained by different operators working in different laboratories on identical test material would, in the long run, in the normal and correct operation of the test  method exceed the following values only in one case in twenty. Reproducibility (R) may be calculated as shown in Eq 14 or Eq 15 for all materials covering the full scope of this method. See Table 4 for calculated values.

14.1.2 再现性--在长期运行中，在测试方法的正常和正确操作的情况下，由不同实验室的不同操作人员对相同测试材料获得的两个单独和独立结果之间的差异，二十个中仅有一个超过以下值。对于涵盖本方法全部范围的所有材料，可以如公式14或公式15所示计算再现性(R)。计算值见表4。

Repeatability（r）= 0.4273·X^0.8015 mg/kg       (14)

Repeatability（r）= （0.4273·（（Y·10000）^0.8015））/10000 mass %       (15)

where:

X =   sulfur concentration in mg/kg total sulfur, and

Y =   sulfur concentration in mass percent total  sulfur.

X = 总硫的硫浓度,以mg/kg为单位，以及

Y = 总硫的硫浓度，以质量%为单位。

TABLE 4 Precision Values, All Sample Types

表4 精度值（所有样品类型）

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