CN101000329A - Analytical investigating method of perfluor n-pro-pyl vinyl ether - Google Patents
Analytical investigating method of perfluor n-pro-pyl vinyl ether Download PDFInfo
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- CN101000329A CN101000329A CNA2006101710179A CN200610171017A CN101000329A CN 101000329 A CN101000329 A CN 101000329A CN A2006101710179 A CNA2006101710179 A CN A2006101710179A CN 200610171017 A CN200610171017 A CN 200610171017A CN 101000329 A CN101000329 A CN 101000329A
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- perfluor
- vinyl ether
- propyl vinyl
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Abstract
The invention discloses hexafluoro-Propoxyethylene analyzing and measuring method. It includes the following steps: processing gas-chromatography analysis for the hexafluoro-Propoxyethylene; using area normalization to directly measure its content; chromatographic analysis temperature is 40 degree centigrade; chromatographic column type is DB-17; liquid membrane is 1.0um; detector is flame ionization. The invention has reliable result, simple operation, can be used to guide hexafluoro-Propoxyethylene study and production.
Description
Technical field
The present invention relates to a kind of analysis determining method of perfluor n-propyl vinyl ether.
Background technology
The perfluor n-propyl vinyl ether is a kind of important fluorine-containing synthetic intermediate, and it is to be formed through addition, cracking, rectifying by hexafluoropropylene oxide, is the important source material of synthetic Meltability polytetrafluorethyletubular.In process of production, because the existence of minor amount of water can generate hydride and other impurity very approaching with perfluor n-propyl vinyl ether boiling point aborning, because the existence of these impurity can impact the quality of producing PFA.So need highly purified perfluor n-propyl vinyl ether on producing.But be difficult to it is carried out quantitative test with infrared analysis and nuclear magnetic resonance, and the price of instrument is also relatively more expensive, is not suitable for enterprise and does conventional analysis.
Summary of the invention
At the deficiencies in the prior art, the invention provides a kind of analysis determining method of perfluor n-propyl vinyl ether.
Technical scheme of the present invention is as follows:
A kind of analysis determining method of perfluor n-propyl vinyl ether carries out gas chromatographic analysis to the perfluor n-propyl vinyl ether, measures perfluor n-propyl vinyl ether content with the area normalization method direct quantitative.
The analysis determining method of above-mentioned perfluor n-propyl vinyl ether is got perfluor n-propyl vinyl ether sample 1uL, carries out stratographic analysis with chromatograph, tries to achieve the content of perfluor n-propyl vinyl ether by following formula.
In the formula: A is the peak area of perfluor n-propyl vinyl ether
∑ A is the total area at each peak.
The analysis determining method of above-mentioned perfluor n-propyl vinyl ether, preferred stratographic analysis temperature is 40 ℃.Be chromatograph column temperature when being 40 ℃, degree of separation is best.
The analysis determining method of above-mentioned perfluor n-propyl vinyl ether, preferred stratographic analysis is DB-17 with the chromatogram column type, liquid film is 1.0um.
The analysis determining method of above-mentioned perfluor n-propyl vinyl ether, preferred stratographic analysis chromatograph produces 6890 chromatographs for U.S.'s Agilent.
The analysis determining method of above-mentioned perfluor n-propyl vinyl ether, preferred stratographic analysis detecting device is a flame ionization detector.
Direct quantitative that the present invention set up is measured the chromatogram analysis method of perfluor n-propyl vinyl ether purity, obtains stable analysis result (seeing Table 1), can instruct the perfluor n-propyl vinyl ether research and production.This method is simple, reliable, has higher utility.
Description of drawings
Fig. 1 is the chromatographic fractionation figure of DB-17, and horizontal ordinate is the time, and ordinate is a peak value.Wherein, 4.720min hydride, 4.831min (summit) perfluor n-propyl vinyl ether.
Embodiment
The present invention will be further described below in conjunction with embodiment, but be not limited thereto.
Embodiment 1:
1.1 instrument
U.S.'s Agilent is produced 6890 chromatographs
1.2 chromatographic condition
Detecting device: FID (flame ionization detector)
Chromatographic column: DB-17
Column length: ￠ 0.25*30m
Column temperature: 40 ℃
Injector: 120 ℃
Detecting device: 300 ℃
1.3 sample analysis
Because the sample highly volatile, attention action is wanted rapidly when annotating sample.Sampling 1uL carries out stratographic analysis rapidly, tries to achieve the content of perfluor n-propyl vinyl ether by following formula.
In the formula: A is the peak area of perfluor n-propyl vinyl ether
∑ A is the total area at each peak.
In Fig. 1, the peak area of perfluor n-propyl vinyl ether is 658020, and the peak area of hydride is 263, and the content of perfluor n-propyl vinyl ether is so:
Be below present embodiment method to two kinds of samples respectively METHOD FOR CONTINUOUS DETERMINATION nine times the result relatively.
The result that table 1 sample METHOD FOR CONTINUOUS DETERMINATION is nine times relatively
| Sample | Measured value (%) | Mean value (%) | Relative average debiation (‰) |
| Perfluor n-propyl vinyl ether (99.99%) I number | 99.988 | 99.988 | 0.006 |
| 99.987 | |||
| 99.990 | |||
| 99.989 | |||
| 99.988 | |||
| 99.986 | |||
| 99.990 | |||
| 99.988 | |||
| 99.989 | |||
| Perfluor n-propyl vinyl ether II number | 99.941 | 99.944 | 0.006 |
| 99.963 | |||
| 99.954 | |||
| 99.922 | |||
| 99.935 | |||
| 99.973 | |||
| 99.934 | |||
| 99.924 | |||
| 99.955 |
Annotate: 1, " I number " be greater than 99.9% perfluor n-propyl vinyl ether from the purity of Daikin company purchase.
2, " II number " be the perfluor n-propyl vinyl ether that Donggue Shenzhou New Material Co., Ltd., Shandong produces.
3, " measured value " is the result with analytical of the present invention.
" mean value " is the average result of continuous nine sample introduction analysis results.
" relative average debiation " is the average absolute of absolute deviation of each time mensuration shared thousand marks in the mean value of each time mensuration.It is used for representing the degree of reliability of analysis result, can embody the degree near each other of same sample income value in repeatedly measuring.
(see Table 1) as can be known from the sample analysis result, can obtain more stable analysis result with this law.
Embodiment 2: the selection of chromatographic condition
Be liquid film respectively the DB-1 of 0.32um, DB-200, DB-17 and liquid film are the DB-1 of 1.0um, DB-200, two groups of also aging good capillary chromatographic columns of DB-17 are installed on Agilent 6890 chromatographs, (column temperature) carried out the test of degree of separation under different temperature, the results are shown in Table 2, table 3.Described DB-1, DB-200, DB-17 are the chromatographic column type.
Table 2 thickness of liquid film is the degree of separation under the chromatographic column different temperatures of 1.0um
Annotate: degree of separation can show each component situation separated from one another in chromatographic column.When degree of separation adjacent two chromatographic peaks greater than 1.5 time could separate fully.Degree of separation has been got well, and measurement result can have enough good collimation and accuracy.
Table 3 thickness of liquid film is the degree of separation of chromatographic column under different temperatures of 0.32um
Annotate: "----" can not separate for the peak.
By table 2, table 3 as can be seen liquid film be that obviously to be better than liquid film under each temperature be a group of 0.32um for one group of degree of separation of 1.0um, and liquid film is that the degree of separation of DB-17 in a group of 1.0um is apparently higher than DB-1 and DB-200, wherein DB-17 is when the chromatograph column temperature is 40 ℃, and degree of separation can reach best effects.
In sum, selecting liquid film as can be seen is the DB-17 of 1.0um, and degree of separation was best when analysis temperature was 40 ℃.
Claims (6)
1, a kind of analysis determining method of perfluor n-propyl vinyl ether is characterized in that the perfluor n-propyl vinyl ether is carried out gas chromatographic analysis, measures perfluor n-propyl vinyl ether content with the area normalization method direct quantitative.
2, the analysis determining method of perfluor n-propyl vinyl ether as claimed in claim 1 is characterized in that getting perfluor n-propyl vinyl ether sample 1uL, carries out stratographic analysis with chromatograph, tries to achieve the content of perfluor n-propyl vinyl ether by following formula:
In the formula: A is the peak area of perfluor n-propyl vinyl ether
∑ A is the total area at each peak.
3, the analysis determining method of perfluor n-propyl vinyl ether as claimed in claim 1 is characterized in that described stratographic analysis temperature is 40 ℃.
4, the analysis determining method of perfluor n-propyl vinyl ether as claimed in claim 1 is characterized in that described stratographic analysis is DB-17 with the chromatogram column type, and liquid film is 1.0um.
5, the analysis determining method of perfluor n-propyl vinyl ether as claimed in claim 1 is characterized in that described stratographic analysis chromatograph produces 6890 chromatographs for U.S.'s Agilent.
6, the analysis determining method of perfluor n-propyl vinyl ether as claimed in claim 1 is characterized in that described stratographic analysis detecting device is a flame ionization detector.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101710179A CN100489521C (en) | 2006-12-29 | 2006-12-29 | Analysis and determination method of perfluor n-pro-pyl vinyl ether |
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|---|---|---|---|
| CNB2006101710179A CN100489521C (en) | 2006-12-29 | 2006-12-29 | Analysis and determination method of perfluor n-pro-pyl vinyl ether |
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| CN101000329A true CN101000329A (en) | 2007-07-18 |
| CN100489521C CN100489521C (en) | 2009-05-20 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105319290A (en) * | 2014-08-04 | 2016-02-10 | 天津市长芦盐业总公司化工新材料工程技术中心 | Method for analyzing and measuring heptafluoropropyl trifluorovinyl ether |
| CN111398481A (en) * | 2020-04-22 | 2020-07-10 | 上海汽车集团股份有限公司 | Analysis test method of perfluorosulfonyl fluoroolefin ether |
-
2006
- 2006-12-29 CN CNB2006101710179A patent/CN100489521C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105319290A (en) * | 2014-08-04 | 2016-02-10 | 天津市长芦盐业总公司化工新材料工程技术中心 | Method for analyzing and measuring heptafluoropropyl trifluorovinyl ether |
| CN111398481A (en) * | 2020-04-22 | 2020-07-10 | 上海汽车集团股份有限公司 | Analysis test method of perfluorosulfonyl fluoroolefin ether |
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|---|---|
| CN100489521C (en) | 2009-05-20 |
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Owner name: SHANDONG HUAXIA SHENZHOU NEW MATERIAL CO., LTD. Free format text: FORMER NAME: DONGGUE SHENZHOU NEW MATERIAL CO., LTD., SHANDONG |
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Address after: 256401 Tangshan Town, Huantai County, Shandong Province Patentee after: Shandong Dongyue Shenzhou New Material Co., Ltd. Address before: 256401 Tangshan Town, Huantai County, Shandong Province Patentee before: Donggue Shenzhou New Material Co., Ltd., Shandong |
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Granted publication date: 20090520 Termination date: 20111229 |