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

用單色波長色散X射線熒光光譜法測定汽油、柴油、航空燃料、煤油、生物柴油、生物柴油混合物和汽油-乙醇混合物中硫的標準試驗方法

1.    Scope* 范圍*

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 本試驗方法包括用單色波長色散X射線熒光（(MWDXRF）光譜法測定單相汽油、柴油、用于混合汽油和柴油的煉油工藝流、噴氣燃料、煤油、生物柴油、生物柴油混合物和汽油乙醇混合物中的總硫。

N_OTE 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.

注1——由于分析過程中輕組分的蒸發(fā)，高蒸氣壓汽油或輕烴等揮發(fā)性樣品可能不符合規(guī)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 本試驗方法的范圍介于合并定量限（PLOQ）值（通過與實踐D6259一致的程序計算）的總硫含量為3.2 mg / kg和循環(huán)中最高含量的樣品，總硫含量為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 精確度 - 該測試方法的精確度是根據實施規(guī)程D6300在實驗室間研究⁷中獲得的結果的統(tǒng)計分析確定的。通過使用九個不同實驗室的九個分析儀的數據計算精確度。每個實驗室分析一組盲目復制樣本。通過使用來自22種含硫材料的數據計算精確度，所述材料包括五種汽油，七種柴油和生物柴油混合物，三種航空燃料，一種煤油，三種生物柴油和三種汽油-乙醇混合物。測得的平均硫含量范圍為1.1mg / kg至2822mg / kg。確定了硫的合并定量限（PLOQ）（通過與實施規(guī)程D6259一致的程序計算）為3.2 mg / kg。

15.1.1 重復性 - 在長期運行中，在測試方法的正常和正確操作的情況下，由同一操作者在恒定操作條件下，對相同測試材料，使用同一儀器獲得的連續(xù)結果之間的差異，二十個中僅有一個超過以下值。對于涵蓋本方法的全部范圍的所有材料，可以如公式7所示計算重復性（r）。有關計算值，請參閱表6。

Repeatability (r)=0.49987X^0.54 …………(7)

where:

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

式中：

X = 兩個結果的平均硫濃度，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 再現性 - 在長期運行中，在測試方法的正常和正確操作的情況下，由不同實驗室的不同操作人員對相同測試材料獲得的兩個單獨和獨立結果之間的差異，二十個中僅有一個超過以下值。對于涵蓋本方法的全部范圍的所有材料，可以如公式8所示計算再現性（R）。有關計算值，請參閱表6。

Reproducibility (R)=0.7384X^{0.54 …………(8)}

where:

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

式中：

X = 兩個結果的平均硫濃度，以mg / kg表示。

TABLE 6 Precision Values, All Sample Types

表6 精度值（所有樣品類型）

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