附近的新茶嫩茶

Designation: D4929 ? 17

Standard Test Method for

Determination of Organic Chloride Content in Crude  Oil

原油現貨中高分子氯化物含量測試的標準來嘗試體例


1. Scope 面積

1.1   The procedures in this test method cover the determination of organic chloride (above 1 μg/g organically-bound chlorine) in crude oils, using either distillation and sodium biphenyl reduction, distillation and microcoulometry, or distillation and x-ray fluorescence (XRF) spectrometry.

1.2   The procedures in this test method involve the distillation of crude oil test specimens to obtain a naphtha fraction     prior to chloride determination. The chloride content of the naphtha fraction of the whole crude oil can thereby be obtained. See Section 5 regarding potential interferences.


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1.5   Procedure C covers the determination of organic chloride in the washed naphtha fraction of crude oil by x-ray fluorescence spectrometry.

1.1 本嘗試體例中的法式包含利用蒸餾和聯苯鈉復原、蒸餾和微庫侖法或蒸餾和X射線熒光（XRF）光譜法測定原油中的無機氯化物（大于1μg/g無機連系氯）。             

1.2 本嘗試體例中的法式觸及蒸餾原油試樣，以在氯化物測定之前取得石腦油餾分。從而能夠取得全部原油石腦油餾分的氯化物含量。對潛伏攪擾，見第5節。             


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1.5 法式C包含用X射線熒光光譜法測定原油洗濯洗石腦油餾分中的無機氯。             


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4. Significance and Use 感覺和益處

4.1  Organic chlorides do not occur naturally in crude oil. When present, they result from contamination in some manner, such as disposal of chlorinated solvent used in many dewaxing pipeline or other equipment operations.

4.1.1   Uncontaminated crude oil will contain no detectable organic chloride, and most refineries can handle very small amounts without deleterious effects.

4.1.1.1  Most trade contracts specify that no organic chloride is present in the crude oil.

4.1.2   Several  pipelines  have  set  specification  limits  at <1 mg ?kg organic chlorides in the whole crude, and <5 mg ?kg in the light naphtha, on the basis of the naphtha fraction being 20 % of the original  sample.

4.1.2.1  To  ensure <1 mg ?kg organic chloride in the crude   oil, the amount measured in the naphtha fraction shall be <1/f (where f is the naphtha fraction calculated with Eq 3).

4.1.3   Organic chloride present in the crude oil (for example, methylene chloride, perchloroethylene, etc.) is usually distilled into the naphtha fraction. Some compounds break down during fractionation and produce hydrochloric acid, which has a corrosive effect. Some compounds survive fractionation and     are destroyed during hydro-treating (desulfurization of the naphtha).

4.2  Other halides can also be used for dewaxing crude oil; in such cases, any organic halides will have similar impact on the refining operations as the organic  chlorides.

4.3  Organic chloride species are potentially damaging to refinery processes. Hydrochloric acid can be produced in hydrotreating or reforming reactors and the acid accumulates in condensing regions of the refinery. Unexpected concentrations of organic chlorides cannot be effectively neutralized and damage can result. Organic chlorides are not known to be    naturally present in crude oils and usually result from cleaning operations at producing sites, pipelines, or tanks. It is important for the oil industry to have common methods available for the determination of organic chlorides in crude oil, particularly    when transfer of custody is  involved.

4.1 原油中不存在自然的無機氯化物。當存在時，它們以某種體例凈化形成，比方處置很多脫蠟管道或其余裝備操縱中利用的氯化溶劑。             

4.1.1 未受凈化的原油將不含可檢測的無機氯化物，大大都煉油廠能夠處置很是少許的無機氯化物，而不會發生無害影響。             

4.1.1.1 大大都商業條約劃定原油中不含有無機氯化物。             

4.1.2 在石腦油組分為原始樣品的20%的根本上，有幾條管道劃定了全部原油中<1 mg/kg和石腦油中<5 mg/kg的無機氯化物的規格限值。       

4.1.2.1 為確保原油中的無機氯化物含量<1 mg kg，石腦油中測得的含量應小于1/f（此中f是用式3計較的石腦油分數）。             

4.1.3 原油中的無機氯化物（如二氯甲烷、四氯乙烯等）凡是蒸餾成石腦油餾分。有些化合物在分餾進程中分化，發生鹽酸，有侵蝕感化。一些化合物在分餾進程中幸存上去，并在加氫處置（石腦油脫硫）進程中被粉碎。             

4.2 其余鹵化物也可用于原油脫蠟；在這類環境下，任何無機鹵化物對煉油功課的影響與無機氯化物類似。             

4.3 無機氯化物對煉油進程有潛伏風險。鹽酸可在加氫處置或重整反映器中發生，并在煉油廠的冷凝區儲蓄積累。不測濃度的無機氯化物沒法有用中和，能夠形成侵害。已知原油中不存在自然的無機氯化物，凡是是出產現場、管道或儲罐潔凈功課的成果。對火油產業來講，有配合的體例來測定原油中的無機氯化物是很重要的，出格是在觸及移交保存的環境下。


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 32. Precision  and Bias  精度和誤差

32.1.1  Repeatability—The difference between successive results obtained by the same operator with the same apparatus under constant operating conditions on identical test materials would, in the long run, in the normal and correct operation, exceed the following values only in one case in twenty.

32.1.1.3  Procedure C—Values can be obtained for organically-bound chlorine for any given concentration above 1 mg/kg Cl (in the original crude oil specimen) as specified in Table 2. See Table 3 for calculated values. See Note 8 for details of the ILS.

32.1.1  反復性—從持久來看，在一般和準確的操縱中，統一操縱員在不異的嘗試資料上利用不異的儀器在恒定操縱前提下取得的持續成果之間的差別僅在二非常之一的環境下跨越以下值。

32.1.1.3  法式C—如表2所示，任何給定濃度跨越1 mg/kg Cl（在原始原油樣品中）時，可取得無機連系氯的值。計較值見表3。ILS概況見注8。   

32.1.2  Reproducibility—The difference between two single and independent results obtained by different operators working in different laboratories on identical material would, in the long run, exceed the following values only in one case in twenty.

32.1.2.1  Procedure C—Values can be obtained for organically-bound chlorine for any given concentration above  1 mg/kg Cl (in the original crude oil specimen) as specified in Table  2. See Table  3 for calculated values. See Note 8 for    details of the ILS.

32.1.2  再現性—從久遠來看，在差別嘗試室任務的差別操縱員在不異資料上取得的兩個零丁和自力成果之間的差別在二非常之一的環境下僅會跨越以下值。

32.1.2.1 法式C—如表2所示，任何給定濃度跨越1 mg/kg Cl（在原始原油樣品中）時，可取得無機連系氯的值計較值見表3。ILS概況見注8。


TABLE 2 Precision Equations, Procedure C XRF

表 2  密封方程式式，法式風格C XRF

Repeatability  r, mg/kgA

MWDXRF               r = 0.643*X0.44                (19)

MEDXRF                r =  0.591*X0.44              (20)

EDXRF                r =  0.934（X  + 0.4）0.48    (21)

Reproducibility R, mg/kgA

MWDXRF              R= 1.235*X0.44                (22)

MEDXRF               R = 1.500*X0.44               (23)

EDXRFB             R =  2.000（X  + 0.4）0.48              (24)

AWhere X = mg/kg chloride

A式中 x=mg/kg氯化物


TABLE 3 Calculated Precision Values, Procedure C XRF

表 3  斤斤計較高精度值，法式風格C XRF

Cl，

Repeatability r, mg/kgA

Reproducibility R, mg/kgB

mg/kg

MWDXRF

MEDXRF

EDXRF

MWDXRF

MEDXRF

EDXRF

1

0.6

0.6

1.1

1.2

1.5

2.4

2

0.9

0.8

1.4

1.7

2.0

3.0

3

1.0

1.0

1.7

2.0

2.4

3.6

4

1.2

1.1

1.9

2.3

2.8

4.1

5

1.3

1.2

2.1

2.5

3.0

4.5

6

1.4

1.3

2.3

2.7

3.3

4.9

8

1.6

1.5

2.6

3.1

3.7

5.6

10

1.8

1.6

2.9

3.4

4.1

6.2

12

1.9

1.8

3.1

3.7

4.5

6.7

AValues calculated from Eq 19 for MWDXRF, Eq 20 for MEDXRF, and Eq 21 for EDXRF.

BValues calculated from Eq 22 for MWDXRF, Eq 23 for MEDXRF, and Eq 24 for EDXRF.


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