CN101975830B - Gas chromatograph capable of simultaneously measuring oxygen and nitrogen in gas - Google Patents
Gas chromatograph capable of simultaneously measuring oxygen and nitrogen in gas Download PDFInfo
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- CN101975830B CN101975830B CN 201010530190 CN201010530190A CN101975830B CN 101975830 B CN101975830 B CN 101975830B CN 201010530190 CN201010530190 CN 201010530190 CN 201010530190 A CN201010530190 A CN 201010530190A CN 101975830 B CN101975830 B CN 101975830B
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Abstract
The invention relates to a gas chromatograph capable of simultaneously measuring oxygen and nitrogen in gas, comprising a chromatographic pre-column, an eleven-way draw bar valve, a chromatographic main-column, a thermal conductivity detector and a data processing system; the chromatographic pre-column, the eleven-way draw bar valve, the chromatographic main-column and the thermal conductivity detector are successively connected through a gas circuit connecting pipeline; and the data processing system is connected with the thermal conductivity detector through a network. According to the gas chromatograph capable of simultaneously measuring oxygen and nitrogen in gas, two different separation columns are combined to achieve the function of avoiding the interference of other gas, and the eleven-way draw bar valve is further arranged to switch introduce samples and analyze state and wash a gas circuit system while introducing the sample, thereby avoiding the pollution of residual gas in the gas circuit system and achieving the function of continuous real-time monitoring.
Description
Technical field
The present invention relates to a kind of gas chromatograph, the especially a kind of gas chromatograph that can measure simultaneously oxygen and nitrogen.
Background technology
Along with the development of new technology, gas chromatography analysis method is widely used as the gas determination method of maturation, can analyze simultaneously the multiple gases such as oxygen, nitrogen, and has played the effect of positive important.
In order to measure oxygen, nitrogen gas, as shown in Figure 1, conventional gas chromatograph comprises transfer valve 1, the chromatographic column 2 and detecting device 3 that connects by the gas circuit connecting pipe line, and connects the data handling system 4 of described detecting device 3 by the networking.This routine gas chromatograph adopts a root chromatogram column and a thermal conductivity detector (TCD) to detect, and utilizes chromatographic column that mixed gas is separated, and thermal conductivity detector (TCD) detects, and data handling system is carried out analyzing and processing and obtained determination data.The conventional assay method of gas chromatograph that adopts is: sample gas to be analyzed is cut in gas circuit by transfer valve 1, bring chromatographic column 2 into the sample gas that carrier gas will be cut in gas circuit, utilize the stalling characteristic of the composition to be measured in sample gas different, sample gas is analyzed, bringing the sample gas after separating into detecting device 3 detects, convert the signal record to, then by network transmission to data handling system, complete determination and analysis.But the gas that usually also has many other influences chromatographic columns to separate in sample gas, nitrogen oxygen just is not easy separated, and other gas also can disturb producing separating of nitrogen and oxygen.And the chromatographic column of this routine gas chromatograph exists the factors such as chromatographic column pollution when long-term work, can not carry out exactly the real-time analysis monitoring.
Summary of the invention
The purpose of this invention is to provide a kind of novel analysis oxygen, the gas chromatograph of nitrogen, can carry out the analysis mensuration of oxygen, nitrogen by real-time online, and avoid the existence of the gases such as carbon dioxide to the interference of chromatographic resolution.
In order to achieve the above object, the invention provides the gas chromatograph of oxygen and nitrogen in a kind of simultaneously mensurated gas composition, this gas chromatograph comprises: chromatogram pre-column, 11 logical pull bar valves, chromatogram principal post, thermal conductivity detector (TCD) and data handling system, and described chromatogram pre-column, 11 logical pull bar valves, chromatogram principal post, thermal conductivity detector (TCD) connect by the gas circuit connecting pipe line successively; Described data handling system is connected by the networking with described thermal conductivity detector (TCD).
The gas chromatograph of oxygen and nitrogen in above-mentioned mensurated gas composition simultaneously, wherein, described 11 logical pull bar valves comprise: the pull bar valve cage, and be set in the interior pull bar valve core of pull bar valve cage; Between described pull bar valve cage and described pull bar valve core, the space is arranged; Described pull bar valve cage is divided into 11 equidistant ring belt areas, and each ring belt area is provided with a hole, and the axial distance of described adjacent two ring belt areas is d; Described each hole connects a pipeline; Equidistantly be provided with 5 annular projections on described pull bar valve core, described annular projection can seal the space between pull bar valve cage and described pull bar valve core fully, plays the effect of similar dividing plate.
The gas chromatograph of oxygen and nitrogen in above-mentioned mensurated gas composition simultaneously, wherein, described projection is arranged on the position apart from pull bar valve core end 1.5d, and the axial distance of described two adjacent protrusion is d1, and d1=3d.
The gas chromatograph of oxygen and nitrogen in above-mentioned mensurated gas composition simultaneously, wherein, described each hole can be arranged on the optional position of its ring belt area, place.
Gas chromatograph of the present invention is equipped with two different chromatographic columns simultaneously in a system; Utilize the gas that a root chromatogram column (being the chromatogram pre-column) separates needs analysis and impact analysis, use again the sample gas that an other root chromatogram column (being the chromatogram principal post) separates needs analysis, then, obtain the concentration of oxygen and nitrogen by thermal conductivity cell detector and chromatographic software (being data handling system) measurement and calculation; And, the present invention adopts the 11 logical pull bar valves can be when sample introduction, air-channel system to whole gas chromatograph carries out the carrier gas flushing, to avoid having in the chromatograph air-channel system residual contamination of a front sample gas, thereby realize the effect of real-time analysis monitoring, and can not be subject to the interference of other gases.
The present invention makes it compared with prior art owing to having adopted above-mentioned technical scheme, has following advantage and good effect:
1, by two kinds of different chromatography columns of coupling, separate and accept or reject various gaseous samples according to different characteristics, having avoided the gas interference;
2. two kinds of different chromatography columns of coupling, and 11 logical pull bar valves are set, switch sampling, analysis state, and simultaneously air-channel system is rinsed at sample introduction, thereby avoid the gas residue in air-channel system to pollute, realized the function of continuous real-time monitoring.
Description of drawings
Fig. 1 is the schematic diagram of the conventional gas chromatograph of prior art.
Fig. 2 is the schematic diagram of the system architecture of the gas chromatograph of oxygen and nitrogen in a kind of simultaneously mensurated gas composition of the present invention.
Fig. 3 is the structural representation of 11 logical pull bar valves of the gas chromatograph of oxygen and nitrogen in a kind of simultaneously mensurated gas composition of the present invention.
Fig. 4 A is the schematic flow sheet of the gas chromatograph analysis state of oxygen and nitrogen in a kind of simultaneously mensurated gas composition of the present invention.
Fig. 4 B is the schematic flow sheet of the gas chromatograph sampling state of oxygen and nitrogen in a kind of simultaneously mensurated gas composition of the present invention.
Embodiment
Describe the specific embodiment of the present invention in detail below in conjunction with accompanying drawing.
As shown in Figure 2, be the gas chromatograph of oxygen and nitrogen in a kind of mensurated gas composition simultaneously of the present invention, this gas chromatograph comprises: the chromatogram pre-column 10 that connects by the gas circuit connecting pipe line successively, 11 logical pull bar valves 20, chromatogram principal post 30, thermal conductivity detector (TCD) 40 and the data handling system 50 that is connected by the networking with thermal conductivity detector (TCD) 40.Detect when analyzing, sample gas goes out not have the sample gas of interference gas through 10 initial gross separations of chromatogram pre-column, then, switch by 11 logical pull bar valves 20, the sample gas of having removed interference gas is brought in chromatogram principal post 30 through carrier gas, again separates, then detect by thermal conductivity detector (TCD) 40, last detection signal enters data handling system 50 by the networking and carries out analyzing and processing, with the content of oxygen in mensurated gas composition and nitrogen.
As shown in Figure 3, be the structural representation of of the present invention 11 logical pull bar valves 20, this 11 logical pull bar valve 20 comprises: pull bar valve cage 21, and, be set in the pull bar valve core 22 in pull bar valve cage 21, between described pull bar valve cage 21 and described pull bar valve core 22, the space arranged; Described pull bar valve cage 21 is divided into 11 equidistant ring belt areas, and each ring belt area is provided with a hole a1-a11, and wherein, the axial distance between adjacent two ring belt areas is d, is d as the ring belt area distance at, described a9 and a10 place.Described each hole is communicated with a gas path pipe.
Equidistantly be provided with 5 annular projection b1-b5 on described pull bar valve core 22, these annular projections can seal the space between pull bar valve cage 21 and described pull bar valve core 22 fully.Wherein, described protruding b1 is arranged on the position apart from pull bar valve core 22 end 1.5d, and the axial distance of two adjacent protrusion is d1, and d1=3d.Described projection can be the ring of fixing welding, can be also the O-ring seals such as dismountable rubber washer.
As shown in Fig. 4 A and Fig. 4 B, be the gas path analysis process flow diagram of analysis state of the present invention and sample introduction state, wherein, the dotted line between two holes of adjacent ring region represents that the ring belt area at this place, two holes is in connected state; Carrier gas 70 herein is hydrogen.Described each hole a1 ~ a11 is in communication with the outside by gas path pipe respectively.Described a1, a8, a11 are communicated with carrier gas 70 by pipeline respectively, form the first path p1, alternate path p2 and three-way p3; Described a2, a5 are communicated with quantity tube 60 respectively; Described a3 is communicated with sample gas 80; Described a4, a7 are communicated with atmosphere respectively; Described a6, a9 are communicated with chromatogram pre-column 10 respectively, and described a10 is communicated with chromatogram principal post 30.
as shown in Fig. 4 A, at this moment, the spool 22 of 11 logical pull bar valves 20 is in the state of pulling out, beginning sample gas analysis: the first path p1 of carrier gas 70, a1 by 11 logical pull bar valves 20, a2, with the sample gas in quantity tube 60, a5 by 11 logical pull bar valves 20, a6 is brought into chromatogram pre-column 10 and carries out initial gross separation, then, removed the sample gas of interference gas, a9 by 11 logical pull bar valves 20, a10 is brought in chromatogram principal post 30 and again separates, the gas that separates enters thermal conductivity detector (TCD) 40 and detects, then by data handling system, detection signal is carried out analyzing and processing, complete the mensuration to oxygen in sample gas and nitrogen content, the alternate path p2 of carrier gas 70, by a8, the a7 of 11 logical pull bar valves 20, directly emptying, at this moment, the three-way p3 of carrier gas 70 is in closed state, sample gas 80 is by the direct emptying of a3, a4 of 11 logical pull bar valves 20.Then, pull bar valve core 22 is advanced, make it reach the state shown in Fig. 4 B, begin whole gas chromatograph is rinsed, and the beginning sample introduction.
As shown in Figure 4 B, be at this moment the sample introduction state: the first path p1 of carrier gas 70 is airtight; The alternate path p2 of carrier gas 70 enters chromatogram pre-column 10 by a8, the a9 of 11 logical pull bar valves 20, again by 11 a6, the a7 emptying of leading to valves 20, complete the blowback of chromatogram pre-column 10 is rinsed, residual to remove previous sample gas, avoid contaminate subsequent testing sample gas, be convenient to continuous real-time monitoring; The three-way p3 of carrier gas 70 opens, and a11, a10 by 11 logical pull bar valves 20 rinse chromatogram principal post 30, and be residual to remove previous sample gas, is convenient to continuous real-time monitoring; Sample gas 80 to be detected enters quantity tube 60 by a3, the a2 of 11 logical pull bar valves 20, carry out emptying by a5, a4 by 11 logical pull bar valves 20 again, complete the sample gas in quantity tube is rinsed, removing last residual sample gas, and quantity tube is carried out new sample gas fill.Then, pull out pull bar valve core 22, complete new sample gas to be determined to the filling of quantity tube.At this moment, be in the sample analysis state, as shown in Fig. 4 A.
By the way, by advancing or pull out 11 logical pull bar valve cores, repeat analysis of shift state, sample introduction state, thereby periodically carry out sample introduction, analysis, sample introduction, the cyclic process of analysis more again, realize the measurement function of continuous real-time monitoring of the present invention.
In sum, the present invention carries out initial gross separation by increase chromatogram pre-column nitrogen and oxygen is measured the gas that causes interference, then, complete the switching of analysis, sample introduction by 11 logical pull bar valves, and can carry out carrier gas to whole gas chromatograph before sample introduction and rinse, avoid the residual error that causes of a front sample gas, thereby, realize the measurement function of METHOD FOR CONTINUOUS DETERMINATION oxygen and nitrogen, in sample gas real-time analysis monitoring, positive effect is arranged.
Although content of the present invention has been done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple modification of the present invention with to substitute will be all apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (3)
1. gas chromatograph of oxygen and nitrogen in mensurated gas composition simultaneously, it is characterized in that, this gas chromatograph comprises: chromatogram pre-column (10), 11 logical pull bar valves (20), chromatogram principal post (30), thermal conductivity detector (TCD) (40) and data handling system (50)
Described chromatogram pre-column (10), 11 logical pull bar valves (20), chromatogram principal post (30), thermal conductivity detector (TCD) (40) connect by the gas circuit connecting pipe line successively;
Described data handling system (50) is connected by the networking with described thermal conductivity detector (TCD) (40);
Described 11 logical pull bar valves (20) comprise: pull bar valve cage (21), and be set in the interior pull bar valve core (22) of pull bar valve cage (21);
Between described pull bar valve cage (21) and described pull bar valve core (22), the space is arranged;
Described pull bar valve cage (21) is divided into 11 equidistant ring belt areas, each ring belt area is provided with the hole, be respectively the first hole (a1), the second hole (a2), the 3rd hole (a3), the 4th hole (a4), the 5th hole (a5), the 6th hole (a6), seven apertures in the human head (a7), octal (a8), the 9th hole (a9), the tenth hole (a10) and 11-holes (a11), the axial distance of described adjacent two ring belt areas is d; Described each hole all connects a pipeline;
Equidistantly be provided with 5 annular projections (b1-b5) on described pull bar valve core (22), described annular projection can seal the space between pull bar valve cage (21) and described pull bar valve core (22) fully;
Described the first hole (a1), octal (a8) and 11-holes (a11) are communicated with carrier gas (70) by pipeline respectively, form the first path p1, alternate path p2 and three-way p3; Described the second hole (a2), the 5th hole (a5) are communicated with quantity tube (60) respectively; Described the 3rd hole (a3) is communicated with sample gas (80); Described the 4th hole (a4), seven apertures in the human head (a7) are communicated with atmosphere respectively; Described the 6th hole (a6), the 9th hole (a9) are communicated with chromatogram pre-column (10) respectively, and described the tenth hole (a10) is communicated with chromatogram principal post (30).
2. the gas chromatograph of oxygen and nitrogen in simultaneously mensurated gas composition as claimed in claim 1, it is characterized in that, described projection (b1) is arranged on the position apart from pull bar valve core (22) end 1.5d, and the axial distance of described two adjacent protrusion is d1, and d1=3d.
3. the gas chromatograph of oxygen and nitrogen in mensurated gas composition simultaneously as claimed in claim 1, is characterized in that, described each hole can be arranged on the optional position of its ring belt area, place.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010530190 CN101975830B (en) | 2010-11-03 | 2010-11-03 | Gas chromatograph capable of simultaneously measuring oxygen and nitrogen in gas |
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| CN 201010530190 CN101975830B (en) | 2010-11-03 | 2010-11-03 | Gas chromatograph capable of simultaneously measuring oxygen and nitrogen in gas |
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| CN101975830A CN101975830A (en) | 2011-02-16 |
| CN101975830B true CN101975830B (en) | 2013-06-05 |
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| CN106290623B (en) * | 2016-07-29 | 2019-04-02 | 黑龙江省劳动安全科学技术研究中心 | A kind of detection method of content of oxygen in air |
| CN108827949B (en) * | 2018-08-14 | 2023-06-02 | 四川理工学院 | Nitrogen dioxide and ozone combined online detection device and method |
| CN114113429A (en) * | 2021-11-26 | 2022-03-01 | 厦门埃癸斯流体控制设备有限公司 | Sample injection valve of gas chromatograph |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2468050Y (en) * | 2000-05-31 | 2001-12-26 | 中国石油化工集团公司 | Gas chromatograph for analyzing aromatic hydrocarbon content of alcohol |
| CN201837614U (en) * | 2010-11-03 | 2011-05-18 | 上海神开石油化工装备股份有限公司 | Gas chromatograph capable of simultaneously measuring oxygen and nitrogen in gas |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2468050Y (en) * | 2000-05-31 | 2001-12-26 | 中国石油化工集团公司 | Gas chromatograph for analyzing aromatic hydrocarbon content of alcohol |
| CN201837614U (en) * | 2010-11-03 | 2011-05-18 | 上海神开石油化工装备股份有限公司 | Gas chromatograph capable of simultaneously measuring oxygen and nitrogen in gas |
Non-Patent Citations (2)
| Title |
|---|
| 中国科学院化学物理研究所色谱组.大气成分和大气中某些污染物的气相色谱分析.《分析化学》.1977,第1卷(第1期),52-63. |
| 大气成分和大气中某些污染物的气相色谱分析;中国科学院化学物理研究所色谱组;《分析化学》;19770131;第1卷(第1期);52-63 * |
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