Designation: D7039 - 15a


Standard Test Method for

Sulfur in Gasoline, Diesel Fuel, Jet Fuel, Kerosine, Biodiesel, Biodiesel Blends, and Gasoline-Ethanol Blends by Monochromatic Wavelength Dispersive X-ray Fluorescence Spectrometry

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




1.    Scope* 范围*

1.1   This test method covers the determination of total sulfur by monochromatic wavelength-dispersive X-ray fluorescence (MWDXRF) spectrometry in single-phase gasoline, dieselfuel, refinery process streams used to blend gasoline and diesel, jet fuel, kerosine, biodiesel, biodiesel blends, and gasoline-ethanol blends.

1.1 本试验方法包括用单色波长色散X射线荧光((MWDXRF)光谱法测定单相汽油、柴油、用于混合汽油和柴油的炼油工艺流、喷气燃料、煤油、生物柴油、生物柴油混合物和汽油乙醇混合物中的总硫。

NOTE 1—Volatile samples such as high-vapor-pressure gasolines or light hydrocarbons might not meet the stated precision because of the evaporation of light components during the analysis.

1——由于分析过程中轻组分的蒸发,高蒸气压汽油或轻烃等挥发性样品可能不符合规定的精度。

1.2   The range of this test method is between the pooled limit of quantitation (PLOQ) value (calculated by procedures consistent with Practice D6259) of 3.2 mg /kg total sulfur and the highest level sample in the round robin, 2822 mg /kg total sulfur.

1.2 本试验方法的范围介于合并定量限(PLOQ)值(通过与实践D6259一致的程序计算)的总硫含量为3.2 mg / kg和循环中最高含量的样品,总硫含量为2822 mg / kg



15.     Precision and Bias 精度和偏差

15.1 Precision—The precision of this test method was determined by statistical analysis of results obtained in an interlaboratory study7 in accordance with Practice D6300. Precision was calculated by using data from nine analyzers at nine different laboratories. Each laboratory analyzed a sample set in blind duplicate. Precision was calculated by using data from 22 sulfur-containing materials, including five gasolines, seven diesel and biodiesel blends, three jet fuels, one kerosine, three biodiesels, and three gasoline-ethanol blends. The range of the measured average sulfur levels was 1.1 mg/kg to 2822 mg/kg. A pooled limit of quantitation (PLOQ) (calculated by procedures consistent with Practice D6259) of 3.2 mg/kg sulfur was determined.

15.1.1 Repeatability—The  difference  between successive 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 Eq7for all materials covering the full scope of this method. See Table  6 for calculated values.

15.1 精确度 - 该测试方法的精确度是根据实施规程D6300在实验室间研究7中获得的结果的统计分析确定的。通过使用九个不同实验室的九个分析仪的数据计算精确度。每个实验室分析一组盲目复制样本。通过使用来自22种含硫材料的数据计算精确度,所述材料包括五种汽油,七种柴油和生物柴油混合物,三种航空燃料,一种煤油,三种生物柴油和三种汽油-乙醇混合物。测得的平均硫含量范围为1.1mg / kg2822mg / kg。确定了硫的合并定量限(PLOQ)(通过与实施规程D6259一致的程序计算)为3.2 mg / kg

15.1.1 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。对于涵盖本方法的全部范围的所有材料,可以如公式7所示计算重复性(r)。有关计算值,请参阅表6

Repeatability (r)=0.49987X0.54 …………(7)

where:

      X =  the average sulfur concentration of two results in mg/kg.

式中:

X = 两个结果的平均硫浓度,以mg / kg表示。

15.1.2 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 Eq8 for all materials covering the full scope of this method. See Table 6 for calculated values.

15.1.2 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。对于涵盖本方法的全部范围的所有材料,可以如公式8所示计算再现性(R)。有关计算值,请参阅表6

Reproducibility (R)=0.7384X0.54 …………(8)

where:

X =  the average sulfur concentration of two results in mg/kg.

式中:

X = 两个结果的平均硫浓度,以mg / kg表示。

TABLE 6 Precision Values, All Sample Types

6 精度值(所有样品类型)

S,mg/kg

Repeatability r,mg/kg

Eq7values

Reproducibility R, mg/kg

Eq 8values

3.2

0.9

1.4

5.0

1.2

1.8

10.0

1.7

2.6

15.0

2.2

3.2

25.0

2.8

4.2

50.0

4.1

6.1

100

6

9

250

10

15

500

14

21

1000

21

31

2000

30

45

2822

36

54





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