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(dan)色(se)波長色(se)散X射線熒光(guang)光(guang)譜(pu)法(fa)測定汽油(you)、柴油(you)、航空燃料(liao)、煤(mei)油(you)、生(sheng)物柴油(you)、生(sheng)物柴油(you)混合物和汽油(you)-乙(yi)醇混(hun)合物中硫的標(biao)準試驗(yan)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(yan)方法包括用單色(se)波長色(se)散X射線熒光（(MWDXRF）光譜法測定單相汽(qi)油(you)、柴(chai)油(you)、用于(yu)混合汽(qi)油(you)和(he)柴(chai)油(you)的(de)(de)煉油(you)工藝流、噴氣(qi)燃料、煤油(you)、生物柴(chai)油(you)、生物柴(chai)油(you)混合物和(he)汽(qi)油(you)乙醇混合物中的(de)(de)總(zong)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)于分(fen)析過(guo)程(cheng)中輕(qing)組分(fen)的蒸發(fa)，高蒸氣壓汽油或(huo)輕(qing)烴等揮發(fa)性樣品可能不符合規定的精度(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(ben)試驗方法(fa)的范圍介于合(he)并定量限（PLOQ）值(zhi)（通過(guo)與實(shi)踐D6259一致的程序計算）的總硫含量為3.2 mg / kg和循環中最(zui)高含量(liang)的樣品，總硫含量(liang)為2822 mg / kg。
15. Precision and Bias 精度(du)和偏差(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 - 該測(ce)試方法的(de)精確(que)度是根(gen)據實施規程D6300在實驗室(shi)間研(yan)究7中獲(huo)得的(de)(de)(de)結(jie)果的(de)(de)(de)統計分(fen)析確定(ding)的(de)(de)(de)。通(tong)(tong)過(guo)使(shi)用九個不同(tong)實(shi)驗室(shi)(shi)的(de)(de)(de)九個分(fen)析儀的(de)(de)(de)數(shu)據(ju)計算精確度。每個實(shi)驗室(shi)(shi)分(fen)析一組盲目(mu)復制樣本。通(tong)(tong)過(guo)使(shi)用來自(zi)22種(zhong)含(han)硫材料的(de)數據(ju)計算精確(que)度(du)，所述材料包括(kuo)五(wu)種(zhong)汽(qi)油(you)(you)，七種(zhong)柴油(you)(you)和(he)生物柴油(you)(you)混合物，三(san)種(zhong)航空(kong)燃料，一種(zhong)煤油(you)(you)，三(san)種(zhong)生物柴油(you)(you)和(he)三(san)種(zhong)汽(qi)油(you)(you)-乙醇混合(he)物(wu)。測得的平均硫含量范圍為1.1mg / kg至2822mg / kg。確定(ding)了(le)硫的合并定(ding)量限（PLOQ）（通過與實(shi)施規程D6259一(yi)致的(de)程序計算）為3.2 mg / kg。
15.1.1 重(zhong)復性 - 在(zai)長(chang)期運行中，在(zai)測試方法的(de)(de)(de)正常和(he)正確操作(zuo)(zuo)的(de)(de)(de)情況下，由同一(yi)(yi)(yi)操作(zuo)(zuo)者在(zai)恒(heng)定操作(zuo)(zuo)條件下，對(dui)相同測試材料(liao)，使用同一(yi)(yi)(yi)儀器獲(huo)得的(de)(de)(de)連續結(jie)果之間的(de)(de)(de)差異，二十個(ge)中僅(jin)有一(yi)(yi)(yi)個(ge)超(chao)過(guo)以下值。對(dui)于涵(han)蓋本方法的(de)(de)(de)全部范(fan)圍的(de)(de)(de)所有材料(liao)，可以如(ru)公式(shi)7所示計算(suan)重復(fu)性（r）。有關(guan)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：
X = 兩個結果的平均硫濃度(du)，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(xing) - 在長(chang)期運(yun)行(xing)中(zhong)，在測(ce)試方(fang)法(fa)的正常和正確操(cao)作的情況下，由不同(tong)實驗室的不同(tong)操(cao)作人員對相同(tong)測(ce)試材料獲得的兩個(ge)單獨和獨立結果之間的差異，二十個(ge)中(zhong)僅有一(yi)個(ge)超過以下值。對于涵(han)蓋(gai)本方(fang)法(fa)的全部范圍(wei)的所有材料，可以如(ru)公式8所示計算(suan)再現性（R）。有(you)關計算(suan)值，請參閱表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(biao)示。
TABLE 6 Precision Values, All Sample Types
表(biao)6 精度(du)值（所有(you)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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