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(dan)色波(bo)長色散X射(she)線熒光(guang)光(guang)譜(pu)法(fa)測定(ding)汽油(you)(you)(you)、柴油(you)(you)(you)、航空燃料、煤(mei)油(you)(you)(you)、生(sheng)物柴油(you)(you)(you)、生(sheng)物柴油(you)(you)(you)混合(he)物和汽油(you)(you)(you)-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(bao)括用單色波長(chang)色散(san)X射線熒光（(MWDXRF）光譜法測定單相汽油、柴(chai)(chai)油、用于混(hun)合汽油和柴(chai)(chai)油的(de)煉油工藝(yi)流、噴氣燃料(liao)、煤油、生物(wu)柴(chai)(chai)油、生物(wu)柴(chai)(chai)油混(hun)合物(wu)和汽油乙(yi)醇混(hun)合物(wu)中的(de)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(cheng)中輕(qing)組分的蒸發，高蒸氣壓汽油或輕(qing)烴(jing)等揮發性樣品可能(neng)不(bu)符合規定的精度。

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(fa)的范(fan)圍介(jie)于(yu)合(he)并(bing)定量(liang)限（PLOQ）值（通過(guo)與實踐D6259一致的程序計算）的總硫含量為3.2 mg / kg和循(xun)環中最高含(han)量的(de)樣品，總硫含(han)量為2822 mg / kg。

15.     Precision and Bias 精度和(he)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(que)度 - 該測試方法的精確度是(shi)根據實施規程D6300在實驗(yan)室間研究(jiu)⁷中獲(huo)得的結果的統計分析確(que)定的。通過使用(yong)九個(ge)(ge)不同實(shi)驗(yan)室(shi)的九個(ge)(ge)分析儀(yi)的數據(ju)計算精(jing)確(que)度。每(mei)個(ge)(ge)實(shi)驗(yan)室(shi)分析一組盲(mang)目(mu)復制樣本。通過使用(yong)來自22種(zhong)含硫材料的(de)數(shu)據計算精確度(du)，所(suo)述(shu)材料包括五種(zhong)汽(qi)油，七種(zhong)柴油和(he)生物柴油混合(he)物，三種(zhong)航空燃料，一種(zhong)煤油，三種(zhong)生物柴油和(he)三種(zhong)汽(qi)油-乙醇(chun)混合物。測(ce)得的平均硫含量范(fan)圍為1.1mg / kg至2822mg / kg。確(que)定了硫(liu)的合并定量限（PLOQ）（通過與實施規程D6259一致(zhi)的程(cheng)序計算(suan)）為3.2 mg / kg。

15.1.1 重復性 - 在長期運行(xing)中，在測試方法的(de)正常和正確操(cao)作(zuo)的(de)情況(kuang)下，由同(tong)一操(cao)作(zuo)者在恒定操(cao)作(zuo)條(tiao)件(jian)下，對相同(tong)測試材料(liao)(liao)，使(shi)用(yong)同(tong)一儀器獲得的(de)連(lian)續結果之間的(de)差異，二十個中僅有一個超過以下值。對于涵蓋(gai)本方法的(de)全部(bu)范圍的(de)所有材料(liao)(liao)，可以如(ru)公(gong)式7所示計算(suan)重復性（r）。有(you)關(guan)計算值(zhi)，請參閱(yue)表6。

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

where:

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

式中(zhong)：

X = 兩個(ge)結(jie)果(guo)的(de)平均硫濃度，以mg / kg表(biao)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(xian)性(xing) - 在長期運行(xing)中，在測(ce)試(shi)方(fang)(fang)法(fa)的正常(chang)和(he)正確操作(zuo)的情(qing)況(kuang)下，由不(bu)同實(shi)驗室的不(bu)同操作(zuo)人(ren)員對相同測(ce)試(shi)材(cai)料(liao)獲得的兩個(ge)(ge)單獨和(he)獨立結果(guo)之間的差(cha)異，二(er)十個(ge)(ge)中僅有(you)(you)一(yi)個(ge)(ge)超(chao)過以下值。對于涵(han)蓋本(ben)方(fang)(fang)法(fa)的全部范圍的所有(you)(you)材(cai)料(liao)，可(ke)以如公式8所示計算(suan)再(zai)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(liang)個結果的平均硫濃度，以mg / kg表示。

TABLE 6 Precision Values, All Sample Types

表(biao)6 精度值(zhi)（所有樣品類型）

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