CN104678049A - Method for determining diene value of hydrogenated gasoline - Google Patents
Method for determining diene value of hydrogenated gasoline Download PDFInfo
- Publication number
- CN104678049A CN104678049A CN201510057646.8A CN201510057646A CN104678049A CN 104678049 A CN104678049 A CN 104678049A CN 201510057646 A CN201510057646 A CN 201510057646A CN 104678049 A CN104678049 A CN 104678049A
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- CN
- China
- Prior art keywords
- sample
- titration
- maleic anhydride
- standard solution
- condenser
- Prior art date
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- 150000001993 dienes Chemical class 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 48
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000012086 standard solution Substances 0.000 claims abstract description 17
- 238000004448 titration Methods 0.000 claims abstract description 17
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 10
- 238000012360 testing method Methods 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 14
- 238000003556 assay Methods 0.000 claims description 11
- 239000012153 distilled water Substances 0.000 claims description 10
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 claims description 10
- 229910052740 iodine Inorganic materials 0.000 claims description 9
- 239000011630 iodine Substances 0.000 claims description 9
- 150000001336 alkenes Chemical class 0.000 claims description 8
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 5
- 238000012546 transfer Methods 0.000 claims description 5
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 4
- 239000011976 maleic acid Substances 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 150000008065 acid anhydrides Chemical class 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 235000013312 flour Nutrition 0.000 claims description 3
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims description 3
- 239000006210 lotion Substances 0.000 claims description 3
- 239000011541 reaction mixture Substances 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000003809 water extraction Methods 0.000 claims description 3
- 238000009835 boiling Methods 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 abstract 1
- 238000004458 analytical method Methods 0.000 description 8
- 238000013459 approach Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical group II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000010076 replication Effects 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for determining the diene value of hydrogenated gasoline. The method comprises the following steps: under a backflow condition, reacting a sample and maleic anhydride in a boiling methylbenzene solution, extracting unreacted maleic anhydride in a reaction mixed solution, titrating maleic anhydride by a sodium hydroxide standard solution, meanwhile performing a blank test, calculating the amount of maleic anhydride reacting with the sample by titration difference, and further calculating the diene value.
Description
Technical field
The present invention relates to a kind of assay method of hydrogasoline diadic alkene value.
Background technology
At present, the assay method of hydrogasoline diene value is in gasoline hydrogenation device technique correlation technique, and existing assay method has no.
Summary of the invention
The technical problem to be solved in the present invention overcomes existing defect, provides the assay method of a kind of simple, analytical approach short, hydrogasoline diadic alkene value that analysis cost is low consuming time.
Object of the present invention carrys out specific implementation by the following technical programs:
A kind of assay method of hydrogasoline diadic alkene value, under the condition of backflow, sample reacts in the toluene solution seethed with excitement with along determining enedioic acid acid anhydride, unreacted maleic anhydride is extracted from reaction mixture, with standard solution of sodium hydroxide titration maleic acid, do blank test simultaneously, utilize twice titration poor, calculate the amount with the maleic anhydride of example reaction, and then calculate diene value.
Concrete operation step is:
1) 5 ~ 20g sample is taken in 250 mL Inner ground conical flasks of drying, accurately add the toluene solution of the maleic anhydride after 20 mL filtrations, add several silicon carbide plates and prevent bumping, refined lead powder or the stone flour of thin layer is coated with at the interface of condenser, the Inner ground conical flask installing sample is connected in condenser, fix on hot plate, regulate the rate of heat addition, reflux 1 hour;
2) stop backflow, add 5 mL distilled water in conical flask by the top of condenser after cooling, then seethe with excitement 15 minutes, after being cooled to room temperature, add the distilled water of 5 mL ether and 20 mL again from top;
3) take off condenser, by the separating funnel of reactant transfer to 150 mL in conical flask or 250 mL, divide wash conical flask three times with the ether of 20 mL, then wash conical flasks three times with the moisture of 25 mL, washing lotion all adds as in separating funnel each time;
4) to vibrate in separating funnel 4 ~ 5 minutes, then leave standstill and make it layering, water is put into 250 mL conical flasks, then 250 mL are used successively, 10 mL, 10 mL distilled water extraction remaining liqs, pour into this aqueous solution liquid extracted several times in 250 mL conical flasks, take phenolphthalein as indicator, with the titration of NaOH standard solution.
5) do blank test simultaneously;
6) calculate
Diene value=(V-V1) × C × 126.9 × 100/m × 1000 (g iodine/100g)
In formula:
The volume mL of the NaOH standard solution that V----blank titration consumes
The volume mL of the NaOH standard solution that V1---titration sample consumes
The concentration mol/L of C-----NaOH standard solution
The quality g of m----sample
The atomic weight of 126.9-iodine.
Beneficial effect of the present invention:
The assay method of hydrogasoline diene value provided by the invention, analytical approach titrimetry, guarantees accurate, the reliability of analysis result, and operating process is simple, thus plays promotion for the output and yield improving antioxidant.There is analysis principle novelty, advanced technology, the scope of application are wide; Step is simple, analytical approach consuming time short, analysis cost is low; The advantages such as analytical approach is high to analysis result accuracy, the range of linearity is wide, favorable reproducibility, analysis condition are stable.
Embodiment
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the present invention, is not intended to limit the present invention.
The assay method of hydrogasoline diadic alkene value
1 method summary
This standard defines a kind of assay method of hydrogasoline diadic alkene value.
This standard is applicable to the sample tests that hydrogasoline diene value is greater than 0.06g iodine/100g.
2 regulatory documents
Clause in the following files becomes the clause of this standard by quotation of this standard, every reference document with bearing date, all later amendment (do not comprise and help content) or revision version by mistake, all be not suitable for this standard, but, encourage each side of reaching an agreement according to this standard to examine whether to use the latest edition of these files, every reference document without bearing date, its latest edition is applicable to this standard.
GB/T4756 oil and liquid petroleum product sampling method
GB/T6682 use for laboratory water specification
3 Method And Principles
Under the condition of backflow, sample reacts in the toluene solution seethed with excitement with along determining enedioic acid acid anhydride, unreacted maleic anhydride (being hydrolyzed into maleic acid) is extracted from reaction mixture, with standard solution of sodium hydroxide titration maleic acid, do blank test simultaneously, utilize twice titration poor, calculate the amount with the maleic anhydride of example reaction, and then calculate diene value.
Diene value defines: in the toluene solution of boiling under the backflow special reaction condition of 3 hours, the amount of 100g sample and maleic acid anhydride reactant, the grams suitable with iodine, unit is: g iodine/100g
4 main materials and reagent
4.1 ether: AR
The toluene solution of 4.2 maleic anhydrides
60g maleic anhydride is dissolved in the toluene solution of heat, transfers to after cooling in 1000mL volumetric flask, and by dilution with toluene to scale, leave standstill more than one day, filter with quantitative filter paper before use.
4.3 phenolphthalein indicator
Dissolve the phenolphthalein of 1g in the alcohol of 100Ml30%.
4.4 NaOH standard solution: 1mol/L
4.5 distilled water: meet GB/T6682 tertiary effluent specification.
5 test apparatuses
5.1 Inner ground conical flasks: 250mL(is connected with condenser)
5.2 water condensers: outer grinding port (being connected with conical flask)
5.3 volumetric flasks: 1000 mL
5.4 separating funnel: 150mL or 250 mL
5.5 burets: alkali formula: 50 mL
5.6 conical flasks: 250 mL
5.7 graduated cylinders: 25 mL
5.8 transfer pipets: 5 mL, 10 mL
5.9 counter balance: 0-500g calibration is 0.5g
6 samplings
By the regulation of GB/TT4756 perform '
7 test procedures
7.1 take 5-20g sample in 250 mL Inner ground conical flasks of drying, accurately add the toluene solution of the maleic anhydride after 20 mL filtrations, add several silicon carbide plates and prevent bumping.Be coated with refined lead powder or the stone flour of thin layer at the interface of condenser, the Inner ground conical flask installing sample is connected in condenser, fix on hot plate, regulate the rate of heat addition, reflux 1 hour.
Note: if backflow 1 hour test findings with reflux 3 hours consistent time, can reflux 3 hours.
7.2 stop backflow, add 5 mL distilled water in conical flask, then seethe with excitement 15 minutes, add the distilled water of 5 mL ether and 20 mL after being cooled to room temperature again from top after cooling by the top of condenser.
7.3 take off condenser, by the separating funnel of reactant transfer to 150 mL in conical flask or 250 mL, divide wash conical flask three times with the ether of 20 mL, then wash conical flasks three times with the moisture of 25 mL, washing lotion all adds as in separating funnel each time.
4-5 minute in 7.4 vibration separating funnels, then leave standstill and make it layering, water is put into 250 mL conical flasks, then 250 mL are used successively, 10 mL, 10 mL distilled water extraction remaining liqs, pour into this aqueous solution liquid extracted several times in 250 mL conical flasks, take phenolphthalein as indicator, with the titration of NaOH standard solution.
7.5 do blank test simultaneously
8 calculate
Diene value=(V-V1) × C × 126.9 × 100/m × 1000 (g iodine/100g)
In formula:
The volume mL of the NaOH standard solution that V----blank titration consumes
The volume mL of the NaOH standard solution that V1---titration sample consumes
The concentration mol/L of C-----NaOH standard solution
The quality g of m----sample
The atomic weight of 126.9-iodine
9 expression of results
9.1 analysis result
Using the arithmetic mean of twice replication as its analysis result, result retains one decimal place, and unit is g iodine/100g
9.2 repeated
Real in same lab technician in same experiment, with same test method and instrument, do double repeated experiment to same sample is continuous mutually.The difference of acquired results should be not more than the setting listed by table 1 in 95% confidence level:
Table 1
。
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. the assay method of a hydrogasoline diadic alkene value, it is characterized in that: under the condition of backflow, sample reacts in the toluene solution seethed with excitement with along determining enedioic acid acid anhydride, unreacted maleic anhydride is extracted from reaction mixture, with standard solution of sodium hydroxide titration maleic acid, do blank test simultaneously, utilize twice titration poor, calculate the amount with the maleic anhydride of example reaction, and then calculate diene value.
2. the assay method of hydrogasoline diadic alkene value according to claim 1, is characterized in that: concrete operation step is:
1) 5 ~ 20g sample is taken in 250 mL Inner ground conical flasks of drying, accurately add the toluene solution of the maleic anhydride after 20 mL filtrations, add several silicon carbide plates and prevent bumping, refined lead powder or the stone flour of thin layer is coated with at the interface of condenser, the Inner ground conical flask installing sample is connected in condenser, fix on hot plate, regulate the rate of heat addition, reflux 1 hour;
2) stop backflow, add 5 mL distilled water in conical flask by the top of condenser after cooling, then seethe with excitement 15 minutes, after being cooled to room temperature, add the distilled water of 5 mL ether and 20 mL again from top;
3) take off condenser, by the separating funnel of reactant transfer to 150 mL in conical flask or 250 mL, divide wash conical flask three times with the ether of 20 mL, then wash conical flasks three times with the moisture of 25 mL, washing lotion all adds as in separating funnel each time;
4) to vibrate in separating funnel 4 ~ 5 minutes, then leave standstill and make it layering, water is put into 250 mL conical flasks, then 250 mL are used successively, 10 mL, 10 mL distilled water extraction remaining liqs, pour into this aqueous solution liquid extracted several times in 250 mL conical flasks, take phenolphthalein as indicator, with the titration of NaOH standard solution;
5) do blank test simultaneously;
6) calculate
Diene value=(V-V1) × C × 126.9 × 100/m × 1000 (g iodine/100g)
In formula:
The volume mL of the NaOH standard solution that V----blank titration consumes
The volume mL of the NaOH standard solution that V1---titration sample consumes
The concentration mol/L of C-----NaOH standard solution
The quality g of m----sample
The atomic weight of 126.9-iodine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510057646.8A CN104678049A (en) | 2015-02-04 | 2015-02-04 | Method for determining diene value of hydrogenated gasoline |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510057646.8A CN104678049A (en) | 2015-02-04 | 2015-02-04 | Method for determining diene value of hydrogenated gasoline |
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| Publication Number | Publication Date |
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| CN201510057646.8A Pending CN104678049A (en) | 2015-02-04 | 2015-02-04 | Method for determining diene value of hydrogenated gasoline |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115598285A (en) * | 2022-10-09 | 2023-01-13 | 苏州恒润商品检验有限公司（Cn） | A kind of iodized catalyst test method that can improve the detection speed of diene value |
-
2015
- 2015-02-04 CN CN201510057646.8A patent/CN104678049A/en active Pending
Non-Patent Citations (6)
| Title |
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| 张坤: "近红外光谱法快速测定加氢物料的双烯含量", 《石化技术》 * |
| 张帆: "声化学法用于测定裂解汽油的双烯值", 《广东化工》 * |
| 张继忠等: "红外光谱透射法测定裂解汽油二烯值", 《石油化工》 * |
| 彭少逸等: "测定油品中共轭双烯含量的新方法", 《燃料化学学报》 * |
| 徐亚贤: "油品中共扼二烯烃的测定", 《石油化工高等学校学报》 * |
| 王小伟等: "极谱法测定汽油中共轭二烯烃的含量", 《石油炼制与化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115598285A (en) * | 2022-10-09 | 2023-01-13 | 苏州恒润商品检验有限公司（Cn） | A kind of iodized catalyst test method that can improve the detection speed of diene value |
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Application publication date: 20150603 |