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(se)波長色(se)散X射線熒光光譜(pu)法測(ce)定汽油(you)(you)(you)(you)、柴油(you)(you)(you)(you)、航空燃(ran)料、煤油(you)(you)(you)(you)、生物(wu)柴油(you)(you)(you)(you)、生物(wu)柴油(you)(you)(you)(you)混合(he)物(wu)和汽油(you)(you)(you)(you)-乙醇(chun)混(hun)合物中硫(liu)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(shi)驗方法包括(kuo)用單(dan)色波長色散X射線熒光（(MWDXRF）光譜法測定(ding)單相汽(qi)油(you)(you)(you)、柴(chai)油(you)(you)(you)、用于混(hun)(hun)合汽(qi)油(you)(you)(you)和柴(chai)油(you)(you)(you)的煉(lian)油(you)(you)(you)工(gong)藝流、噴氣燃(ran)料、煤油(you)(you)(you)、生物(wu)柴(chai)油(you)(you)(you)、生物(wu)柴(chai)油(you)(you)(you)混(hun)(hun)合物(wu)和汽(qi)油(you)(you)(you)乙醇混(hun)(hun)合物(wu)中的總硫。
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——由于分析過程(cheng)中輕(qing)組分的蒸發(fa)，高蒸氣(qi)壓汽油或輕(qing)烴等揮發(fa)性樣品可能(neng)不符合(he)規定(ding)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(de)程(cheng)序計算）的(de)總(zong)硫(liu)含量為3.2 mg / kg和循環(huan)中最(zui)高含(han)量(liang)的樣品，總硫含(han)量(liang)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(gai)測試方法(fa)的精確度是根(gen)據實施規程D6300在實驗室間研(yan)究7中獲得的(de)(de)結果(guo)的(de)(de)統計(ji)分(fen)析(xi)(xi)確定(ding)的(de)(de)。通過使(shi)(shi)用(yong)九(jiu)個不同(tong)實(shi)驗室的(de)(de)九(jiu)個分(fen)析(xi)(xi)儀(yi)的(de)(de)數據計(ji)算精確度(du)。每(mei)個實(shi)驗室分(fen)析(xi)(xi)一(yi)組盲目復制樣本(ben)。通過使(shi)(shi)用(yong)來自(zi)22種(zhong)(zhong)(zhong)含硫材料(liao)的數據計(ji)算(suan)精確度，所述材料(liao)包括五種(zhong)(zhong)(zhong)汽(qi)油(you)，七種(zhong)(zhong)(zhong)柴(chai)(chai)油(you)和生物(wu)柴(chai)(chai)油(you)混合(he)物(wu)，三種(zhong)(zhong)(zhong)航空燃料(liao)，一種(zhong)(zhong)(zhong)煤油(you)，三種(zhong)(zhong)(zhong)生物(wu)柴(chai)(chai)油(you)和三種(zhong)(zhong)(zhong)汽(qi)油(you)-乙醇混合物。測(ce)得的平均硫含(han)量范圍為1.1mg / kg至2822mg / kg。確定(ding)了硫的合并定(ding)量限（PLOQ）（通過與實施規程D6259一致的程序計算(suan)）為3.2 mg / kg。
15.1.1 重復性(xing) - 在長期運行(xing)中(zhong)，在測(ce)試方(fang)法(fa)(fa)的(de)(de)正常和正確操作的(de)(de)情況下(xia)(xia)，由(you)同(tong)一操作者在恒定操作條(tiao)件(jian)下(xia)(xia)，對(dui)相同(tong)測(ce)試材料(liao)，使(shi)用同(tong)一儀器(qi)獲得的(de)(de)連續結果之間(jian)的(de)(de)差異，二十個(ge)中(zhong)僅有一個(ge)超(chao)過以下(xia)(xia)值。對(dui)于涵蓋本方(fang)法(fa)(fa)的(de)(de)全(quan)部范圍的(de)(de)所有材料(liao)，可以如公式7所示計算重復性（r）。有(you)關計算值，請參閱表6。
Repeatability (r)=0.49987X0.54 …………(7)
where:
X = the average sulfur concentration of two results in mg/kg.
式中(zhong)：
X = 兩(liang)個結(jie)果的平均硫濃(nong)度，以(yi)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(xian)性 - 在(zai)長(chang)期運行中(zhong)，在(zai)測試(shi)方法(fa)的(de)正(zheng)常和正(zheng)確(que)操作的(de)情況下，由(you)不(bu)同實驗室的(de)不(bu)同操作人員對(dui)相(xiang)同測試(shi)材(cai)料獲得的(de)兩個單獨和獨立結果之間的(de)差異，二十(shi)個中(zhong)僅有(you)一個超過以(yi)(yi)下值。對(dui)于涵蓋本方法(fa)的(de)全部范圍(wei)的(de)所有(you)材(cai)料，可以(yi)(yi)如公(gong)式(shi)8所示計算再現性（R）。有(you)關計算值(zhi)，請(qing)參閱表(biao)6。
Reproducibility (R)=0.7384X0.54 …………(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(yang)品(pin)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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