CN108107146A - Oxide content assay method in improved naphtha - Google Patents
Oxide content assay method in improved naphtha Download PDFInfo
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- CN108107146A CN108107146A CN201711480050.4A CN201711480050A CN108107146A CN 108107146 A CN108107146 A CN 108107146A CN 201711480050 A CN201711480050 A CN 201711480050A CN 108107146 A CN108107146 A CN 108107146A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/38—Flow patterns
- G01N30/46—Flow patterns using more than one column
- G01N30/461—Flow patterns using more than one column with serial coupling of separation columns
- G01N30/463—Flow patterns using more than one column with serial coupling of separation columns for multidimensional chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/38—Flow patterns
- G01N30/40—Flow patterns using back flushing
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
Oxide content assay method in improved naphtha using there is valve multidimensional chromatography, is gas chromatograph using instrument, sets gas chromatograph parameter first；Sample introduction；Oil brain sample passes through TCEP columns；The component of detection outflow TCEP columns；It is characterized by comprising following steps：1）Standard specimen is prepared；2）Valve time range is cut in selection, and determines above-mentioned oxide component in the selected loss time cut in the valve time on TCEP columns；3）Naphtha sample is tested；4）Total oxide content determines；The present invention is changed to quantified by external standard method by inner mark method ration, and MTBE, DIPE content are first analyzed by sample introduction twice, then analyzes other oxide contents, solves the contradiction of peak interference and oxide loss so that low content of oxygen compound can be detected accurately in naphtha；Compensating for light components Interference Peaks in original cerebrol needs the longer valve time of cutting that could eliminate, and long cut the valve time that oxide can be caused in naphtha to cause is quantitatively relatively low.
Description
Technical field
The present invention relates to a kind of assay methods, are specifically related to oxide content assay method in improved naphtha, belong to
In analysis and testing technology field.
Background technology
Naphtha is a kind of extremely complex chemical mixture of composition, in chiral process, even if oxygenatedchemicals
It is horizontal in the presence of catalyst explanation poisoning may also be caused with PPM grades, catalyst life is reduced, production is caused to be unable to long period fortune
Row.At present in country's stone brain there are mainly three types of the assay methods of oxygenatedchemicals, first, single-column GC methods（OFID）, second is that multicolumn GC
Method, third, multi-dimensional chromatograph cuts backblowing.The switching of gas chromatographic column, which is divided to, in multi-dimensional chromatograph cutting backblowing two kinds of valve and valve,
Vavle switching is to connect pillar by the multiple-way valve of one or several rotations to form.In existing method, a certain purpose GC-2014
Oxide analysis system in hydrocarbon, the system are furnished with a TCEP column, and a RTX-1 column, sample is first through TCEP columns, when methyl ring
Pentane flows out and DIPE and MTBE when not flowing out, switching valve to RTX-1 post separations oxide, internal standard（DME）And heavy hydrocarbon, work as benzene
When being flowed out with TAME, switching valve to solid line blowback goes out heavy hydrocarbon.
Single-column GC methods provide preferable separation and important composition information, but as the increase of carbon number has a large amount of interference
Peak;Multicolumn PONA methods can be separated the hydro carbons in specified race from C3 to C10 by carbon number, when containing alcohols material in component
Can hydrocarbon component be mistakenly considered by the irreversible absorption of molecular sieve column, cause the presence of very big deviation;Multi-dimensional chromatograph column is cut
It cuts in backblowing, due to naphtha complicated components, the problem of light component interference is lost in oxide component is equally existed, so as to drop
Low measured value.
The content of the invention
In view of above-mentioned technical problem, the present invention, which mainly uses, valve multidimensional chromatography, after naphtha sample is by TCP columns,
It determines loss time of the different oxides on TCEP columns, 2 analyses of valve time progress is cut using change, to the different loss times
Oxide analyze respectively, so as to eliminate Interference Peaks, while ensure that oxide is not lost in, and then determine accurate oxide and contain
Amount.
To achieve these goals, the technical solution adopted in the present invention is：Oxide content is surveyed in improved naphtha
Determine method, using there is valve multidimensional chromatography, the use of instrument is gas chromatograph, sets gas chromatograph parameter first；Sample introduction
；Oil brain sample passes through TCEP columns；The component of detection outflow TCEP columns；It is characterized by comprising following steps：
1）Standard specimen is prepared
Choose oxide component and content
2）Valve time range is cut in selection, and determines above-mentioned oxide component in the selected stream cut in the valve time on TCEP columns
Lose the time；
3）Naphtha sample part component is tested
Determine the optimal content value for cutting the valve time of the respective ingredient of constituent part；
4）Total oxide content determines
The sum of optimal superposition of content value for cutting the valve time of respective ingredient.
Step 1）Middle selection oxide component and content（ppm）For：Ethyl alcohol 46；Isopropanol 285；The tert-butyl alcohol 155；Positive third
Alcohol 177；MTBE 485；Sec-butyl alcohol 265；DIPE 83；Isobutanol 320；Tert-pentyl alcohol 265；N-butanol 223.
Step 2）Loss time of the different oxide components on TCEP columns is determined in the range of middle selection 0.57-0.82min.
Step 3）In cut the valve time for 0.52min and 0.57min when to naphtha in DIPE components, MTBE components and uncle
Amylalcohol component is tested；Cut the valve time for 0.77min and 0.82min when again to naphtha in tert-pentyl alcohol component survey
Examination.
Description of the drawings
Fig. 1 is loss timetable of the different oxides of standard specimen on TCEP columns.
Fig. 2 is the test for cutting the valve time to DIPE components, MTBE components and tert-pentyl alcohol component in naphtha when being 0.52min
As a result chromatogram.
Fig. 3 is the test for cutting the valve time to DIPE components, MTBE components and tert-pentyl alcohol component in naphtha when being 0.57min
As a result chromatogram.
Fig. 4 for cut the valve time be 0.77min when to tert-pentyl alcohol component test result chromatogram in naphtha.
Fig. 5 for cut the valve time be 0.82min when to tert-pentyl alcohol component test result chromatogram in naphtha.
Present invention advantageous effect compared with the prior art is：The present invention is changed to quantified by external standard method by inner mark method ration, leads to
MTBE, DIPE content are first analyzed after sample introduction twice, then analyzes other oxide contents, solves what peak interference was lost in oxide
Contradiction so that low content of oxygen compound can be detected accurately in naphtha；Compensate for light components Interference Peaks in original cerebrol
Need the longer valve time of cutting that could eliminate, and the long valve time of cutting can cause oxide in naphtha to cause quantitatively partially
It is low.
Specific embodiment
Oxide content assay method in improved naphtha is gas phase color using instrument using there is valve multidimensional chromatography
Spectrometer sets gas chromatograph parameter first；Sample introduction；Oil brain sample passes through TCEP columns；Detection outflow TCEP columns
Component；It is characterized by comprising following steps：
1）Standard specimen is prepared
Choose oxide component and content；
Standard specimen is prepared, wherein all kinds of oxide contents（ppm）For：Ethyl alcohol 46；Isopropanol 285；The tert-butyl alcohol 155；Normal propyl alcohol 177；
MTBE 485；Sec-butyl alcohol 265；DIPE 83；Isobutanol 320；Tert-pentyl alcohol 265；N-butanol 223；
2）Valve time range is cut in selection, and determines above-mentioned oxide component in the selected stream cut in the valve time on TCEP columns
Lose the time；
It chooses and loss time of the different oxides on TCEP columns, such as Fig. 1 is determined in the range of 0.57-0.82min
Conclusion：DIPE components are cutting the valve time to start to be lost in during 0.62min, and MTBE components are when it is 0.72min to cut the valve time
Start to be lost in, other oxides cut the valve time reach 0.82min when be not lost in still；
3）Naphtha sample is tested
Determine the optimal content value for cutting the valve time of the respective ingredient of constituent part；
Cut the valve time for 0.52min and 0.57min when to naphtha in DIPE components, MTBE components and tert-pentyl alcohol component carry out
Test；
When cutting the valve time as 0.52min, MTBE concentration of component is 21.72354u/V, and peak value retention time is 13.374min, peak
A height of 196.3；DIPE concentration of component be 30.26490u/V, peak value retention time 16.566min, peak height 514.7；Tert-pentyl alcohol
Concentration of component be 347.39012 u/V, peak value retention time be 19.659min, peak height 3245.4；Chromatogram result such as Fig. 2；
When cutting the valve time as 0.57min, MTBE concentration of component is 21.52542u/V, and peak value retention time is 13.466min, peak
A height of 154.1；DIPE concentration of component be 30.3258u/V, peak value retention time 16.632min, peak height 311.5；Tert-pentyl alcohol group
Point concentration is 128.12375 u/V, and peak value retention time is 19.689min, peak height 1150.5；Chromatogram result such as Fig. 3；
Conclusion：MTBE, DIPE content do not change, it is seen that Interference Peaks have been removed in naphtha, therefore are cut the valve time and be set to 0.57min
When can accurately measure MTBE（21.5ppm）、DIPE（30.3ppm）Content.Tert-pentyl alcohol content is reduced to by 347.4ppm
128.1ppm illustrates still have Interference Peaks not cut completely by TCEP columns, continues adjustment and cuts the valve time；
Continue adjustment to tert-pentyl alcohol component and cut the valve time
Cut the valve time for 0.77min and 0.82min when to naphtha in tert-pentyl alcohol component test；
When it is 0.77min to cut the valve time, tert-pentyl alcohol concentration of component is 26.37020 u/V, and peak value retention time is
19.878min peak height 228.8；Chromatogram result such as Fig. 4
When it is 0.82min to cut the valve time, tert-pentyl alcohol concentration of component is 26.76550 u/V, and peak value retention time is
19.902min peak height 216.3；Chromatogram result such as Fig. 5
Conclusion：When cut the valve time 0.77min is adjusted to by 0.57min when tert-pentyl alcohol content continue to reduce, when cut the valve time by
0.77 when being adjusted to 0.82min, and tert-pentyl alcohol content no longer changes, and illustrates that Interference Peaks have been removed, and tert-pentyl alcohol is not lost in, therefore
Tert-pentyl alcohol content is 26.7ppm；
4）Total oxide content determines
The sum of optimal superposition of content value for cutting the valve time of respective ingredient.
Final conclusion：
When analyzing stone brain, DIPE, MTBE are measured when 0.57min cuts valve, is then changed and is cut the valve time and test other for 0.82min
Oxide content, result are the sum of measurement result twice, i.e., total oxide content is 26.7ppm (tert-pentyl alcohol content)+30.3
（DIPE contents）+21.5（MTBE contents）=83.7ppm.
Claims (4)
1. oxide content assay method in improved naphtha is gas-chromatography using instrument using there is valve multidimensional chromatography
Instrument sets gas chromatograph parameter first；Sample introduction；Oil brain sample passes through TCEP columns；Detection outflow TCEP columns
Component；It is characterized by comprising following steps：
1）Standard specimen is prepared
Choose oxide component and content
2）Valve time range is cut in selection, and determines above-mentioned oxide component in the selected stream cut in the valve time on TCEP columns
Lose the time；
3）Naphtha sample part component is tested
Determine the optimal content value for cutting the valve time of the respective ingredient of constituent part；
4）Total oxide content determines
The sum of optimal superposition of content value for cutting the valve time of respective ingredient.
2. oxide content assay method in improved naphtha according to claim 1, it is characterised in that step 1）In
Choose oxide component and content（ppm）For：Ethyl alcohol 46；Isopropanol 285；The tert-butyl alcohol 155；Normal propyl alcohol 177；MTBE 485；It is secondary
Butanol 265；DIPE 83；Isobutanol 320；Tert-pentyl alcohol 265；N-butanol 223.
3. oxide content assay method in improved naphtha according to claim 1, it is characterised in that step 2）In
It chooses and loss time of the different oxide components on TCEP columns is determined in the range of 0.57-0.82min.
4. oxide content assay method in improved naphtha according to claim 1, it is characterised in that step 3）In
Cut the valve time for 0.52min and 0.57min when to naphtha in DIPE components, MTBE components and tert-pentyl alcohol component survey
Examination；Cut the valve time for 0.77min and 0.82min when again to naphtha in tert-pentyl alcohol component test.
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| CN201711480050.4A CN108107146A (en) | 2017-12-29 | 2017-12-29 | Oxide content assay method in improved naphtha |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0088439A2 (en) * | 1982-03-10 | 1983-09-14 | Hitachi, Ltd. | Gas chromatographic apparatus |
| JPS62167475A (en) * | 1985-12-03 | 1987-07-23 | Shimadzu Corp | Method for analyzing oil-soluble vitamin |
| US20030079523A1 (en) * | 2001-10-29 | 2003-05-01 | Teresa Lechner-Fish | Carrier gas pre-heat system for gas chromatograph |
| CN104569241A (en) * | 2013-10-25 | 2015-04-29 | 中国石油化工股份有限公司 | Method for determining oxygenated compound of C6 in gasoline or micro-reaction product by gas chromatography |
| CN105259265A (en) * | 2015-10-26 | 2016-01-20 | 大连福佳·大化石油化工有限公司 | Detection method for ppm-level oxygen-containing compound in naphtha |
| CN104422739B (en) * | 2013-08-28 | 2017-04-26 | 中国石油化工股份有限公司 | Instrument for quantitatively analyzing trace oxide in petroleum hydrocarbon and method for quantitatively analyzing trace oxide in petroleum hydrocarbon |
| CN206235602U (en) * | 2016-09-29 | 2017-06-09 | 新疆广汇新能源有限公司 | A kind of detecting system of oxygenatedchemicals |
-
2017
- 2017-12-29 CN CN201711480050.4A patent/CN108107146A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0088439A2 (en) * | 1982-03-10 | 1983-09-14 | Hitachi, Ltd. | Gas chromatographic apparatus |
| JPS62167475A (en) * | 1985-12-03 | 1987-07-23 | Shimadzu Corp | Method for analyzing oil-soluble vitamin |
| US20030079523A1 (en) * | 2001-10-29 | 2003-05-01 | Teresa Lechner-Fish | Carrier gas pre-heat system for gas chromatograph |
| CN104422739B (en) * | 2013-08-28 | 2017-04-26 | 中国石油化工股份有限公司 | Instrument for quantitatively analyzing trace oxide in petroleum hydrocarbon and method for quantitatively analyzing trace oxide in petroleum hydrocarbon |
| CN104569241A (en) * | 2013-10-25 | 2015-04-29 | 中国石油化工股份有限公司 | Method for determining oxygenated compound of C6 in gasoline or micro-reaction product by gas chromatography |
| CN105259265A (en) * | 2015-10-26 | 2016-01-20 | 大连福佳·大化石油化工有限公司 | Detection method for ppm-level oxygen-containing compound in naphtha |
| CN206235602U (en) * | 2016-09-29 | 2017-06-09 | 新疆广汇新能源有限公司 | A kind of detecting system of oxygenatedchemicals |
Non-Patent Citations (3)
| Title |
|---|
| DANILO SCIARRONE 等: "Multidimensional GC coupled to MS for the simultaneous determination of oxygenate compounds and BTEX in gasoline", 《J. SEP. SCI.》 * |
| 童玲 等: "乙烯裂解原料中常量含氧化合物的分析方法", 《石化技术》 * |
| 黄河柳 等: "多维气相色谱法测定车用汽油含氧化合物方法改进研究", 《广东化工》 * |
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