聯系我們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(chang)色散X射(she)線熒光光譜法測定汽油、柴(chai)油、航(hang)空燃料、煤油、生物(wu)柴(chai)油、生物(wu)柴(chai)油混合物(wu)和汽油-乙醇混合物中硫的(de)標準(zhun)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(ben)試驗(yan)方法包括用單色波長(chang)色散(san)X射線熒光(guang)（(MWDXRF）光譜法測定單相汽油、柴(chai)油、用于混(hun)合汽油和(he)柴(chai)油的(de)煉油工藝(yi)流、噴(pen)氣燃(ran)料、煤油、生(sheng)物(wu)柴(chai)油、生(sheng)物(wu)柴(chai)油混(hun)合物(wu)和(he)汽油乙醇混(hun)合物(wu)中的(de)總硫。
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.
注1——由(you)于(yu)分析過程中輕組分的蒸發(fa)(fa)，高(gao)蒸氣(qi)壓汽油(you)或輕烴等揮發(fa)(fa)性樣品(pin)可(ke)能(neng)不符合規(gui)定的精(jing)度(du)。
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)的范圍介于合并定量限（PLOQ）值（通過與實(shi)踐D6259一致的(de)程序計算(suan)）的(de)總(zong)硫(liu)含(han)量為3.2 mg / kg和循環中(zhong)最高含(han)(han)量(liang)的樣(yang)品，總硫含(han)(han)量(liang)為2822 mg / kg。
15. Precision and Bias 精度和(he)偏(pian)差(cha)
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(du) - 該測試方(fang)法的精確度是(shi)根據(ju)實施(shi)規(gui)程(cheng)D6300在(zai)實驗(yan)室間(jian)研(yan)究7中(zhong)獲(huo)得(de)的結果的統計(ji)分析確(que)定的。通過使用九個(ge)不(bu)同實驗(yan)室的九個(ge)分析儀的數據計(ji)算(suan)精確(que)度。每個(ge)實驗(yan)室分析一(yi)組盲目復制樣本。通過使用來自22種(zhong)(zhong)(zhong)含硫材料(liao)(liao)的(de)數據(ju)計算(suan)精確度，所述材料(liao)(liao)包括五種(zhong)(zhong)(zhong)汽油，七(qi)種(zhong)(zhong)(zhong)柴油和(he)生(sheng)物柴油混合(he)物，三(san)種(zhong)(zhong)(zhong)航空燃料(liao)(liao)，一種(zhong)(zhong)(zhong)煤油，三(san)種(zhong)(zhong)(zhong)生(sheng)物柴油和(he)三(san)種(zhong)(zhong)(zhong)汽油-乙醇混合物(wu)。測得的(de)平均(jun)硫(liu)含量(liang)范圍為1.1mg / kg至2822mg / kg。確定(ding)了硫的合(he)并定(ding)量限（PLOQ）（通過(guo)與實施規(gui)程D6259一(yi)致的(de)程(cheng)序計算(suan)）為3.2 mg / kg。
15.1.1 重復性 - 在(zai)(zai)長期(qi)運行(xing)中，在(zai)(zai)測試方(fang)法(fa)的(de)正常和正確操作的(de)情況下(xia)(xia)，由同(tong)一操作者在(zai)(zai)恒(heng)定操作條件下(xia)(xia)，對相同(tong)測試材料，使用同(tong)一儀器獲得的(de)連續結果之間的(de)差異，二十個中僅有(you)一個超(chao)過以(yi)下(xia)(xia)值。對于(yu)涵蓋本方(fang)法(fa)的(de)全部范圍的(de)所有(you)材料，可以(yi)如公式7所示計算重復性（r）。有(you)關(guan)計算值，請(qing)參閱表6。
Repeatability (r)=0.49987X0.54 …………(7)
where:
X = the average sulfur concentration of two results in mg/kg.
式(shi)中(zhong)：
X = 兩個結(jie)果的(de)平(ping)均硫(liu)濃(nong)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 再現性 - 在長(chang)期(qi)運行中(zhong)(zhong)，在測試方法的(de)正常和正確操(cao)作的(de)情況下(xia)，由不同實驗(yan)室的(de)不同操(cao)作人(ren)員對(dui)相同測試材料(liao)獲得(de)的(de)兩個單獨(du)和獨(du)立(li)結果之間的(de)差異，二十(shi)個中(zhong)(zhong)僅有(you)一(yi)個超過以下(xia)值。對(dui)于涵(han)蓋本方法的(de)全部范圍的(de)所有(you)材料(liao)，可以如公(gong)式8所示計算再現(xian)性（R）。有關(guan)計(ji)算(suan)值(zhi)，請參閱表(biao)6。
Reproducibility (R)=0.7384X0.54 …………(8)
where:
X = the average sulfur concentration of two results in mg/kg.
式(shi)中：
X = 兩(liang)個結果的(de)平均硫濃度(du)，以mg / kg表(biao)示。
TABLE 6 Precision Values, All Sample Types
表6 精度值(zhi)（所有樣品類型）
|
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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