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Designation: D2622 ? 16
Standard Test Method for
Sulfur in Petroleum Products by Wavelength Dispersive X-ray Fluorescence Spectrometry
波長(chang)色散x射線熒光光譜法(fa)測(ce)定石油產品(pin)中硫的標(biao)準試(shi)驗方法(fa)
1.Scope* 范圍
1.1 This test method covers the determination of total sulfur in petroleum and petroleum products that are single-phase and either liquid at ambient conditions, liquefiable with moderate heat, or soluble in hydrocarbon solvents. These materials can include diesel fuel, jet fuel, kerosene, other distillate oil, naphtha, residual oil, lubricating base oil, hydraulic oil, crude oil, unleaded gasoline, gasoline-ethanol blends, and biodiesel.
1.2 The range of this test method is between the PLOQ value (calculated by procedures consistent with Practice D6259) of 3 mg/kg total sulfur and the highest level sample in the round robin, 4.6 weight % total sulfur.
NOTE 1—Instrumentation covered by this test method can vary in sensitivity. The applicability of the test method at sulfur concentrations below 3 mg ?kg may be determined on an individual basis for WDXRF instruments capable of measuring lower levels, but precision in this test method does not apply.
1.2.1 The values of the limit of quantitation (LOQ) and method precision for a specific laboratory’s instrument depends on instrument source power (low or high power), sample type, and the practices established by the laboratory to perform the method.
1.1 本試(shi)驗方法包括(kuo)測定石(shi)油(you)(you)(you)和石(shi)油(you)(you)(you)產品(pin)中(zhong)的總硫，這些(xie)石(shi)油(you)(you)(you)和石(shi)油(you)(you)(you)產品(pin)是單相的，在環(huan)境條件(jian)下是液(ye)(ye)態的，可(ke)(ke)在中(zhong)等溫度下液(ye)(ye)化，或可(ke)(ke)溶于烴類溶劑。這些(xie)材料可(ke)(ke)以包括(kuo)柴油(you)(you)(you)、噴(pen)氣(qi)燃料、煤油(you)(you)(you)、其(qi)他(ta)餾出油(you)(you)(you)、石(shi)腦(nao)油(you)(you)(you)、殘油(you)(you)(you)、潤(run)滑基礎油(you)(you)(you)、液(ye)(ye)壓(ya)油(you)(you)(you)、原(yuan)油(you)(you)(you)、無鉛(qian)汽(qi)油(you)(you)(you)、汽(qi)油(you)(you)(you)-乙醇混(hun)合(he)物和生物柴油。
1.2 本試(shi)驗(yan)方(fang)法的范圍(wei)為3 mg/kg總硫的PLOQ值（按(an)照與實施規程D6259一致的(de)程序(xu)計算(suan)）與(yu)循(xun)環(huan)中的(de)最高(gao)水平樣品4.6 %（重量）總硫之間。
注(zhu)1：本試驗方法涵蓋的儀(yi)器靈敏(min)度(du)可能不同。對于能夠(gou)測量較低水平的WDXRF儀(yi)器，可(ke)單獨(du)確定硫濃度低于3 mg/kg時試驗方(fang)法(fa)的(de)適用性，但(dan)本(ben)試驗方(fang)法(fa)中的(de)精度(du)不適用。
1.2.1 特(te)定(ding)實驗(yan)室儀(yi)器(qi)的定(ding)量限(xian)（LOQ）和方(fang)(fang)法精密度的(de)值取(qu)決于儀(yi)器光源功率(lv)（低功率(lv)或高功率(lv)）、樣品類型和實驗室為執行該(gai)方(fang)(fang)法而建立的(de)實施(shi)規(gui)程。
14.Precision and Bias 精度和偏差
14.1 The precision of the test method was determined by statistical analysis of results obtained an interlaboratory study6 that included 27 samples including gasolines, distillates, biodiesel, residual oils, and crude oils. A pooled limit of quantitation (PLOQ) of approximately 3 mg/kg S was determined for all sample types. Precision for gasoline and diesel samples for high-power source XRF instruments is included in Appendix X1. The ranges of sulfur concentrations represented by the sample sets, together with the precisions, are listed in 14.1.1 and 14.1.2. These statistics apply only to samples having less than the level of interfering materials present shown in Table 1 (see also 1.4).
14.1.1 Repeatability—The difference between successive test 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 Eq 12 or Eq 13 for all materials covering the full scope of this method. See Table 4 for calculated values.
14.1 通過對實驗室間(jian)研究6所得(de)結果(guo)的(de)統計分析，確(que)定(ding)試驗方法的(de)精密度，該研究包(bao)括27個樣品(pin)，包括(kuo)汽油(you)(you)、餾分油(you)(you)、生物柴油(you)(you)、渣(zha)油(you)(you)和(he)原油(you)(you)。對所有(you)樣品(pin)類型確定了大約3 mg/kg S的(de)合(he)并定(ding)量限(xian)（PLOQ）。高(gao)功率光源X射線熒光儀器對汽油和柴油樣品的精密(mi)度(du)包含在附錄(lu)X1中。14.1.1和14.1.2中列出了由樣品組表示(shi)的硫濃度(du)范(fan)圍(wei)和精度(du)。這些統計數據僅(jin)適用(yong)于小于表1所示(shi)干(gan)擾物質(zhi)水平的(de)樣(yang)品（另見(jian)1.4）。
14.1.1 重(zhong)復性--在長期運行中，在測(ce)試方法的(de)正(zheng)常和正(zheng)確操作(zuo)的(de)情(qing)況下(xia)，由同(tong)一操作(zuo)者在恒定(ding)操作(zuo)條件(jian)下(xia)，對相(xiang)同(tong)測(ce)試材料，使(shi)用(yong)同(tong)一儀(yi)器獲得的(de)連續結果之間的(de)差(cha)異，二十個中僅有一個超過以下(xia)值。對于涵蓋(gai)本方法全(quan)部(bu)范圍的(de)所有材料，可以如(ru)公式12或公式13所示計算(suan)重復(fu)性(r)。計算值見表4。
Repeatability（r）= 0.1462·X0.8015 mg/kg (12)
Repeatability（r）= （0.1462·（（Y·10000）0.8015））/10000 mass % (13)
where:
X = sulfur concentration in mg/kg total sulfur, and
Y = sulfur concentration in mass % total sulfur.
式中：
X = 總硫(liu)的硫(liu)濃度,以(yi)mg/kg為單位，以及
Y = 總硫的硫濃度(du)，以質量%為單位。
14.1.2 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 Eq 14 or Eq 15 for all materials covering the full scope of this method. See Table 4 for calculated values.
14.1.2 再現性--在(zai)長期運行中，在(zai)測(ce)試方法(fa)的(de)正常和(he)正確(que)操(cao)作的(de)情況下，由不同(tong)實驗(yan)室的(de)不同(tong)操(cao)作人員對(dui)相同(tong)測(ce)試材料獲得(de)的(de)兩個單獨和(he)獨立結果之間的(de)差(cha)異，二(er)十個中僅有(you)一個超(chao)過以(yi)(yi)下值(zhi)。對(dui)于涵蓋本方法(fa)全部范圍的(de)所有(you)材料，可以(yi)(yi)如公式14或公式15所(suo)示計算再現性(R)。計算(suan)值見表(biao)4。
Repeatability（r）= 0.4273·X0.8015 mg/kg (14)
Repeatability（r）= （0.4273·（（Y·10000）0.8015））/10000 mass % (15)
where:
X = sulfur concentration in mg/kg total sulfur, and
Y = sulfur concentration in mass percent total sulfur.
X = 總硫的硫濃度(du),以(yi)mg/kg為單位，以及
Y = 總硫的硫濃(nong)度，以(yi)質量(liang)%為單位。
TABLE 4 Precision Values, All Sample Types
表4 精度值（所(suo)有樣品類(lei)型）
|
S,mg/kg |
Repeatability r,mg/kg Eq 12 values |
Reproducibility R, mg/kg Eq 14 values |
|
3.0 |
0.4 |
1.0 |
|
5.0 |
0.5 |
1.6 |
|
10.0 |
0.9 |
2.7 |
|
25.0 |
1.9 |
5.6 |
|
50.0 |
3.4 |
9.8 |
|
100.0 |
5.9 |
17.1 |
|
500 |
21 |
62 |
|
1000 |
37 |
108 |
|
5000 |
135 |
394 |
|
10 000 |
235 |
687 |
|
46 000 |
798 |
2333 |
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