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(zhǎng)色散X射線熒光光譜法測(cè)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(biāo)準(zhǔn)試驗(yàn)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(yàn)方法包括用單色波長(zhǎng)色散X射線熒光（(MWDXRF）光譜法測(cè)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(yàn)方法的范圍介于合并定量限（PLOQ）值（通過與實(shí)踐D6259一致的程序計(jì)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(cè)試方法的精確度是根據(jù)實(shí)施規(guī)程D6300在實(shí)驗(yàn)室間研究⁷中獲得的結(jié)果的統(tǒng)計(jì)分析確定的。通過使用九個(gè)不同實(shí)驗(yàn)室的九個(gè)分析儀的數(shù)據(jù)計(jì)算精確度。每個(gè)實(shí)驗(yàn)室分析一組盲目復(fù)制樣本。通過使用來自22種含硫材料的數(shù)據(jù)計(jì)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(cè)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(shí)施規(guī)程D6259一致的程序計(jì)算）為3.2 mg / kg。

15.1.1 重復(fù)性 - 在長(zhǎng)期運(yùn)行中，在測(cè)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(duì)相同測(cè)試材料，使用同一儀器獲得的連續(xù)結(jié)果之間的差異，二十個(gè)中僅有一個(gè)超過以下值。對(duì)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(jì)算重復(fù)性（r）。有關(guān)計(jì)算值，請(qǐng)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(gè)結(jié)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(xiàn)性 - 在長(zhǎng)期運(yùn)行中，在測(cè)試方法的正常和正確操作的情況下，由不同實(shí)驗(yàn)室的不同操作人員對(duì)相同測(cè)試材料獲得的兩個(gè)單獨(dú)和獨(dú)立結(jié)果之間的差異，二十個(gè)中僅有一個(gè)超過以下值。對(duì)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(jì)算再現(xiàn)性（R）。有關(guān)計(jì)算值，請(qǐng)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(gè)結(jié)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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