CN107505413A - For determining the gas chromatograph of propylene and propane content in insulating oil - Google Patents
For determining the gas chromatograph of propylene and propane content in insulating oil Download PDFInfo
- Publication number
- CN107505413A CN107505413A CN201710701195.6A CN201710701195A CN107505413A CN 107505413 A CN107505413 A CN 107505413A CN 201710701195 A CN201710701195 A CN 201710701195A CN 107505413 A CN107505413 A CN 107505413A
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- Prior art keywords
- propylene
- propane
- insulating oil
- chromatography column
- chromatographic separation
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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
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
-
- 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
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
- G01N2030/201—Injection using a sampling valve multiport valves, i.e. having more than two ports
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
It is used to determine the gas chromatograph of propylene and propane content in insulating oil the invention discloses a kind of, including carrier gas transfer passage, the first chromatographic separation device and the second chromatographic separation device, first chromatographic separation device and the second chromatographic separation device connect with carrier gas transfer passage；Second chromatographic separation device includes the second injection port, chromatography column and the second detector being sequentially connected, characterized in that, the chromatography column includes channel switching device, the second chromatography column and the 3rd chromatography column being both connected between channel switching device and the second injection port.The propylene and propane in Dissolved Gases in Insulating Oil can be fast and effectively separated using the device, improves the accuracy of detection of propylene and propane.
Description
Technical field
The present invention relates to gas chromatograph field, and in particular to a kind of to be used to determine propylene and propane content in insulating oil
Gas chromatograph.
Background technology
Transformer insulation oil will be cracked by under electricity, heat and stress, produce small-molecule substance, for example：Methane,
Ethane, ethene, acetylene, propylene and propane.Small-molecule substance in analysis transformer insulation oil can be found that and tracked transformer
Therefore failure, maintenance are also changed into repair based on condition of component by traditional periodic preventative maintenance.At present, using gas-chromatography
Instrument detects to gas content composition caused by insulation oil-breaking.Existing gas chromatograph includes two chromatographic separation devices,
One chromatographic separation device is used to separate hydrogen, oxygen and the nitrogen in Dissolved Gases in Insulating Oil, and another is used to separate absolutely
Methane, ethane, ethene, acetylene, carbon monoxide, carbon dioxide, propylene and propane in edge oil.But due to propylene and propane phase
Pair larger with gas component molecular weight, using existing gas chromatograph, when separating propylene and propane, its separating degree is small, and
Group separation delivery time length.
The content of the invention
In order to solve the above-mentioned technical problem the present invention provides a kind of for determining the gas of propylene and propane content in insulating oil
Chromatography.
The present invention is achieved through the following technical solutions：
For determining the gas chromatograph of propylene and propane content in insulating oil, including carrier gas transfer passage, the first chromatogram
Separator and the second chromatographic separation device, first chromatographic separation device and the second chromatographic separation device are and carrier gas transfer
Passage connects；The second injection port, the second chromatographic isolation passage, the passage that second chromatographic separation device includes being sequentially connected are cut
Changing device, nickel accelerant converter and fid detector, it is characterised in that the second chromatographic isolation passage is logical including being both connected to
It is used for separation of methane, ethane, ethene, acetylene, carbon monoxide and carbon dioxide between road switching device and the second injection port
Second chromatography column and the 3rd chromatography column for separating propylene and propane.
This programme makes improvements on the basis of existing gas chromatograph structure, by the second chromatographic separation device
The quantity of chromatography column is set up as 2, including the second chromatography column and the 3rd chromatography column, and uses channel switching device
Control its break-make with the second detector.Second chromatography column be used to separating methane in Dissolved Gases in Insulating Oil, ethane,
Ethene, acetylene, carbon monoxide and carbon dioxide, the 3rd chromatography column be used to separating propylene in Dissolved Gases in Insulating Oil and
Propane.The composition of gas is separated respectively using two chromatography columns, it can realize and efficiently separate.
Preferably, in order to improve the separating degree of propylene and propane, the length of the 3rd chromatography column is 4.5-5.5
Rice.
Further, the length of the 3rd chromatography column is 5 meters.
Preferably, the channel switching device is six direction changeover valves.
Preferably, the first chromatographic separation device includes the first chromatographic isolation passage and led to for detecting the first chromatographic isolation
The first detector of gas is isolated in road, and balance columns are additionally provided between the carrier gas transfer passage and the first detector.
The present invention compared with prior art, has the following advantages and advantages：
1st, the present invention sets up the 3rd chromatography column on the basis of existing gas chromatograph, can fast and effectively divide
From the propylene and propane in Dissolved Gases in Insulating Oil, the accuracy of detection of raising propylene and propane.
Brief description of the drawings
Accompanying drawing described herein is used for providing further understanding the embodiment of the present invention, forms one of the application
Point, do not form the restriction to the embodiment of the present invention.In the accompanying drawings：
Fig. 1 is schematic structural view of the invention.
Mark and corresponding parts title in accompanying drawing：
1st, carrier gas transfer passage, 2, balance columns, the 3, first detector, the 4, first injection port, the 5, first chromatography column, 6,
Second injection port, the 7, second chromatography column, the 8, the 3rd chromatography column, 9, channel switching device.
Embodiment
For the object, technical solutions and advantages of the present invention are more clearly understood, with reference to embodiment and accompanying drawing, to this
Invention is described in further detail, and exemplary embodiment of the invention and its explanation are only used for explaining the present invention, do not make
For limitation of the invention.
Embodiment 1
It is as shown in Figure 1 to be used to determine the gas chromatograph of propylene and propane content in insulating oil, including carrier gas transfer leads to
Road 1, the first chromatographic separation device and the second chromatographic separation device, the first chromatographic separation device and the second chromatographic separation device with
Carrier gas transfer passage 1 connects.First chromatographic separation device includes the first chromatographic isolation passage and for detecting the first chromatographic isolation
Channel separation goes out the first detector 3 of gas, is additionally provided with balance columns 2 between carrier gas transfer passage and the first detector 3, and first
Chromatographic isolation passage can use the first injection port 4, the first chromatography column 5 that are sequentially connected to realize that it is isolated in insulating oil
Hydrogen, oxygen and nitrogen in dissolved gas simultaneously detect；First detector 3 can use TCD detectors, for detecting the first chromatogram
The gas content that split tunnel is separated.Balance columns 2 are connected with the first detector 3, when detecting hydrogen, oxygen and nitrogen,
Play a part of reference.
Second chromatographic separation device includes the second injection port 6, the second chromatographic isolation passage, passage the switching dress being sequentially connected
Put, nickel accelerant converter and fid detector, the second chromatographic isolation passage include the second chromatography column 7 and the 3rd chromatographic isolation
Post 8, the second chromatography column 7 and the 3rd chromatography column 8 are connected by channel switching device 9 with nickel accelerant converter Ni.The
Two chromatographic isolation passages use two chromatography columns, separate different gas respectively, wherein one is used for propylene and propane
Measurement, switched by the passage of channel switching device, can be achieved to separate the second chromatography column 7 and the 3rd chromatography column 8
The detection respectively of gas out.Channel switching device can use six direction changeover valves to realize.
Second detector 10 can be realized using the nickel accelerant converter and fid detector that are sequentially connected.Nickel accelerant converts
Device main function be make carbon monoxide in Dissolved Gases in Insulating Oil and carbon dioxide in the case where nickel makees catalysts conditions with hydrogen
Reaction generation methane gas, then detects carbon monoxide and carbon dioxide content by fid detector.Fid detector is to examine
Survey methane, ethane, ethene, acetylene, carbon monoxide, carbon dioxide, propylene and propane content.When fid detector is completed to insulation
Methane, ethane, ethene, acetylene, carbon monoxide in oil, after the completion of the content detection of carbon dioxide, six direction changeover valves from
It is dynamic to switch to propylene and propane testing process.
Carrier gas can use Ar, Air, H2.First chromatographic isolation passage, the second chromatography column and the 3rd chromatography column structure
The chromatographic fractionation system of cost apparatus.Six direction changeover valves, nickel accelerant converter, TCD detectors, fid detector part form this
The component detecting system of device.
Embodiment 2
Through substantial amounts of experimental study, the present embodiment optimizes on the basis of above-described embodiment, i.e. the 3rd chromatographic isolation
The length of post is 4.5-5.5 rice.
By the experimental study of the length to the 3rd chromatography column, find its length being arranged on 4.5-5.5 rice, propylene
It is greatly improved with the separating degree of propane, reaches application requirement.And when the length of the 3rd chromatography column is arranged into 5 meters, most
To be suitable, its separating degree R=1.5, can be achieved to be kept completely separate.
The operating process to the present apparatus illustrates below：
Gas propylene and propane measure：
Ar, H2, Air three channel gas source are opened, starts heating after the 5min that ventilates；
Chromatographic work station is opened, sets work station standard factors；
Temperature is run to the temperature of setting, by " hydrogen flame "+" igniting "；Then " thermal conductivity "+" RUN " is pressed；
Instrument runs 30min, and after baseline stability, propane and propylene 1ml gases that metrological service of learning from else's experience was detected are injected into
Second injection port, start standard specimen collection；
Gas respectively enters the second chromatography column after once shunting and the 3rd chromatography column carries out component separation,
Six direction changeover valves switch to propylene and propane testing process after 6min, and 17min begins to flow out propylene peak, propylene appearance after 19min
Completely, 19.5min begins to flow out propane peak, and propane peak flows completely out after 23min, and demarcation terminates, and preserves gas chromatographic peak；
Twice, the repeatability demarcated twice should be ± more than the 2% of its average value for continuous demarcation.
Sample propylene and propane measure：
After the sample gas for taking 1ml to be measured is injected into the second injection port, starts sample measure, treat that sample peak is covered completely
Afterwards.Propylene and propane content are quantitatively calculated, continuous measurement twice, calculates its average value.
Above-described embodiment, the purpose of the present invention, technical scheme and beneficial effect are carried out further
Describe in detail, should be understood that the embodiment that the foregoing is only the present invention, be not intended to limit the present invention
Protection domain, within the spirit and principles of the invention, any modification, equivalent substitution and improvements done etc., all should include
Within protection scope of the present invention.
Claims (5)
1. for determining the gas chromatograph of propylene and propane content in insulating oil, including carrier gas transfer passage, the first chromatogram point
From device and the second chromatographic separation device, first chromatographic separation device and the second chromatographic separation device lead to carrier gas transfer
Road connects；Second chromatographic separation device includes the second injection port, the second chromatographic isolation passage, the passage switching being sequentially connected
Device, nickel accelerant converter and fid detector, it is characterised in that the second chromatographic isolation passage includes being both connected to passage
It is used for separation of methane, ethane, ethene, acetylene, the of carbon monoxide and carbon dioxide between switching device and the second injection port
Two chromatography columns and the 3rd chromatography column for separating propylene and propane.
2. according to claim 1 be used to determine the device of propylene and propane content in insulating oil, it is characterised in that described
The length of 3rd chromatography column is 4.5-5.5 rice.
3. according to claim 2 be used to determine the device of propylene and propane content in insulating oil, it is characterised in that described
The length of 3rd chromatography column is 5 meters.
4. according to claim 1 be used to determine the device of propylene and propane content in insulating oil, it is characterised in that described
Channel switching device is six direction changeover valves.
5. according to claim 1 be used to determine the device of propylene and propane content in insulating oil, it is characterised in that described
First chromatographic separation device include the first chromatographic isolation passage and go out gas for detecting the first chromatographic isolation channel separation the
One detector, balance columns are additionally provided between the carrier gas transfer passage and the first detector.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710701195.6A CN107505413A (en) | 2017-08-16 | 2017-08-16 | For determining the gas chromatograph of propylene and propane content in insulating oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710701195.6A CN107505413A (en) | 2017-08-16 | 2017-08-16 | For determining the gas chromatograph of propylene and propane content in insulating oil |
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| Publication Number | Publication Date |
|---|---|
| CN107505413A true CN107505413A (en) | 2017-12-22 |
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|---|---|---|---|
| CN201710701195.6A Pending CN107505413A (en) | 2017-08-16 | 2017-08-16 | For determining the gas chromatograph of propylene and propane content in insulating oil |
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Citations (9)
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|---|---|---|---|---|
| CN1158421A (en) * | 1996-02-28 | 1997-09-03 | 沈阳电业局 | On-line analyser for dissolved gas color spectrum in transformer oil |
| CN2616907Y (en) * | 2003-05-07 | 2004-05-19 | 上海海欣色谱仪器有限公司 | Gaseous phase chromatograph with three detectors |
| CN1687769A (en) * | 2005-04-25 | 2005-10-26 | 湖北省电力试验研究院 | Gas chromatography for measuring gas content and characteristic gas in insulating oil completed at one time of sample injection |
| CN1967241A (en) * | 2006-11-20 | 2007-05-23 | 河南省中分仪器有限公司 | A multifunctional gas chromatographic device gas circuit flow |
| CN200944098Y (en) * | 2006-07-12 | 2007-09-05 | 徐明远 | Transformer oil chromatogram analytical equipment |
| CN101320025A (en) * | 2008-07-18 | 2008-12-10 | 上海市计算技术研究所 | Gas-chromatography detection method used for power transformer oil |
| CN201440135U (en) * | 2009-06-26 | 2010-04-21 | 河南省电力公司商丘供电公司 | Multifunctional gas chromatograph gas path flow |
| CN106124676A (en) * | 2016-09-08 | 2016-11-16 | 国网上海市电力公司 | A kind of for measuring the gas chromatograph of solution gas in transformer oil |
| CN106370746A (en) * | 2016-08-26 | 2017-02-01 | 湖南大学 | Gas-dissolved-in-vegetable-insulating-oil analyzer with oil-gas separation function and detecting method |
-
2017
- 2017-08-16 CN CN201710701195.6A patent/CN107505413A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1158421A (en) * | 1996-02-28 | 1997-09-03 | 沈阳电业局 | On-line analyser for dissolved gas color spectrum in transformer oil |
| CN2616907Y (en) * | 2003-05-07 | 2004-05-19 | 上海海欣色谱仪器有限公司 | Gaseous phase chromatograph with three detectors |
| CN1687769A (en) * | 2005-04-25 | 2005-10-26 | 湖北省电力试验研究院 | Gas chromatography for measuring gas content and characteristic gas in insulating oil completed at one time of sample injection |
| CN200944098Y (en) * | 2006-07-12 | 2007-09-05 | 徐明远 | Transformer oil chromatogram analytical equipment |
| CN1967241A (en) * | 2006-11-20 | 2007-05-23 | 河南省中分仪器有限公司 | A multifunctional gas chromatographic device gas circuit flow |
| CN101320025A (en) * | 2008-07-18 | 2008-12-10 | 上海市计算技术研究所 | Gas-chromatography detection method used for power transformer oil |
| CN201440135U (en) * | 2009-06-26 | 2010-04-21 | 河南省电力公司商丘供电公司 | Multifunctional gas chromatograph gas path flow |
| CN106370746A (en) * | 2016-08-26 | 2017-02-01 | 湖南大学 | Gas-dissolved-in-vegetable-insulating-oil analyzer with oil-gas separation function and detecting method |
| CN106124676A (en) * | 2016-09-08 | 2016-11-16 | 国网上海市电力公司 | A kind of for measuring the gas chromatograph of solution gas in transformer oil |
Non-Patent Citations (4)
| Title |
|---|
| V. G. ARAKELIAN: "The Long Way to the Automatic Chromatographic Analysis of Gases Dissolved in Insulating Oil", 《IEEE ELECTRICAL INSULATION MAGAZINE》 * |
| 中华人民共和国国家质量监督检验检疫总局 等: "《GB/T 17623-2017 绝缘油中溶解气体组分含量的气相色谱测定法》", 12 May 2017 * |
| 徐懿俊: "变压器油中溶解性气体（DGA）检测方法的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 郭景云 等: "液化石油气组成色谱分析技术探讨", 《石油与天然气化工》 * |
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Application publication date: 20171222 |
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