Designation: D2622 − 16

Standard TestMethod for

Sulfur inPetroleum 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 productsthat are single-phase and either liquid at ambient conditions, liquefiable withmoderate heat, or soluble in hydrocarbon solvents. These materials can includediesel 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 thePLOQ        value (calculated byprocedures consistent with Practice D6259) of 3 mg/kg total sulfur and the highest levelsample in the round robin, 4.6 weight % total sulfur.

N_OTE 1—Instrumentation covered by thistest method can vary in sensitivity. The applicability of the test method atsulfur concentrations below 3 mg ⁄kg may be determined on an individual basisfor WDXRF instruments capable of measuring lower levels, but precision in thistest 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 oninstrument source power (low or high power), sample type, and the practicesestablished 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.Precisionａnd Bias 精度和偏差

14.1The precision of the test method was determined by statistical analysis ofresults obtained an interlaboratory study⁶ that included 27 samplesincluding gasolines, distillates, biodiesel, residual oils, and crude oils. Apooled limit of quantitation (PLOQ) of approximately 3 mg/kg S was determinedfor all sample types. Precision for gasoline and diesel samples for high-powersource XRF instruments is included in Appendix X1. The ranges of sulfurconcentrations represented by the sample sets, togetherwith the precisions, are listed in 14.1.1 and 14.1.2. These statisticsapply only to samples having less than the level of interfering materialspresent shown in Table 1 (seealso 1.4).

14.1.1 Repeatability—Thedifference between successive test results obtained by the same operator withthe same apparatus under constant operating conditions on identical testmaterial would, in the long run, in the normal and correct   operation of the test method exceed the followingvalues only in one case in twenty. Repeatability (r) may be calculated as shown in Eq 12 or Eq 13 for allmaterials 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—Thedifference between two single and independent results obtained by differentoperators 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 calculatedas shown in Eq 14 or Eq 15 forall materials covering the full scope of this method. See Table 4 forcalculated 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 percenttotal  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。

TABLE4 Precision Values, All Sample Types

表4 精度值（所有样品类型）

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