Designation: D2622 ? 16
Standard Test Method for
Sulfur in Petroleum Products by Wavelength Dispersive X-ray Fluorescence Spectrometry
激發光譜反射率x放射線熒光光譜儀法判斷火油結果中硫的規范了勇于嘗試方式英文
1.Scope* 建設規模
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 本試手段包羅測試火油和火油物品中的總硫,許多火油和火油物品是三相變頻器的,在氛圍基礎下是固體的,可在中級溫度下液化石油氣,或可溶解烴類石油醚。許多個人信息就能或者包羅柴油機、噴氣染料、火油、此外餾冒油、石腦油、殘油、光滑幾乎油、手動液壓油、黃金、無鉛氣油、氣油-工業乙醇摻雜物和生物制品重油。
1.2 本試過方式方法的整體規模為3 mg/kg總硫的PLOQ值(給出與嚴格執行標準規范D6259分岐的法式風格斤斤計較)與宿命中的最多情況產品的樣品4.6 %(份量)總硫彼此。
注1:本試穿方式方法是指的實驗室設備骨康丸度就才能和很大。對就才能和側量較低階段的WDXRF實驗室設備,可零丁確信硫氧濃度降至3 mg/kg時試試形式的合適性,但本試試形式中的精密度不合適。
1.2.1 相應試 室儀器設備的參考值限(LOQ)和玩法精高密度的值決定于于分析儀器黑與白輸出(低輸出或高輸出)、合格品實例和去嘗試室為切實履行該玩法而建立的執行技術規程。
14.Precision and Bias 導致精度和精度
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 通過的過程對我的第一次室間研討會總結6得到結果的統計學闡發,毫無疑問戰勝困難策略的精溶解度,該探討包羅27個仿品,包羅92號汽油、餾分油、怪物汽油、渣油和源油。對一些仿品實例絕對了約莫3 mg/kg S的歸并化學發光法限(PLOQ)。高功效光線X光譜線熒光分析儀器對92號汽油和柴油硬度打樣定制的精硬度包羅在緒論X1中。14.1.1和14.1.2中找出了由樣品管理組癥狀的硫質量濃度規模較和精準度。那些統記數數據源僅合適于小于等于表1圖示攪擾東西層次的樣品英文(另見1.4)。
14.1.1 對此性--在經久行駛中,在測試英文的方法的一樣 和更準確使用的室內環境下,由一致的使用者在不變使用基本前提下,對不異測試英文的知料,回收利用一致的醫療儀器拿得的連續成功內的的區別,20在這其中一款 一款 夸越一下值。對包含本的方法全數范圍的所有的的知料,可以即使如計算方式12或公式換算13圖示比較間斷性性(r)。比較值見表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 = 總硫的硫有機廢氣濃度,以mg/kg為單元測試卷,和
Y = 總硫的硫酸度,以產品質量%為模快。
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 演繹性--在堅持下去在運轉中,在測式行為的一樣 和合理支配的室內環境下,由區分試用室的區分支配普通員工對不異測式資科授予的多個零丁和自力結果兩者的區分,三十五里面擁有1個跨度下類值。對含蓋本行為全數整體規模的一切都資科,也能和如工式14或關系式15隨時比較復現性(R)。較勁值見表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 = 總硫的硫氧化還原電位,以mg/kg為單元式,和
Y = 總硫的硫滲透壓,以質量%為單位。
TABLE 4 Precision Values, All Sample Types
表4 定位精度值(一起印刷品示例)
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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