CN101949909A - Connector for connecting capillary column with ceramic tube in individual hydrocarbon test system - Google Patents
Connector for connecting capillary column with ceramic tube in individual hydrocarbon test system Download PDFInfo
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- CN101949909A CN101949909A CN2010102571803A CN201010257180A CN101949909A CN 101949909 A CN101949909 A CN 101949909A CN 2010102571803 A CN2010102571803 A CN 2010102571803A CN 201010257180 A CN201010257180 A CN 201010257180A CN 101949909 A CN101949909 A CN 101949909A
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Abstract
The invention relates to a connector for connecting a capillary column with a ceramic tube, in particular to a connector which is arranged in an individual hydrocarbon carbon/hydrogen isotope test system and used for connecting a quartz capillary column with a ceramic reaction tube. The connector is implemented directly through high temperature silica gels, and has the advantages of good tightness, high elongation rate, good aging resistance, low loss, translucence, easy operation, and the like. The maximum operating temperature of the sealing connector can reach 300 DEG C, therefore, the accuracy of the connector as an important system component for testing values can be improved effectively; meanwhile, the connector has the characteristics of low cost, long service time, and good application and generalization values; and the invention is simple in structure and easy to replace, and reduces the overall investment funds in the process of operating the equipment.
Description
Technical field
The present invention relates to the important accessory in the hydrocarbon isotope test macro of a kind of detailed hydrocarbon, is a kind of interface that connects between gas-phase chromatographic capillary column and the micropore ceramic tube specifically.
Background technology
The hydrocarbon isotopic ratio of detailed hydrocarbon is in the important effect that has aspect the researchs such as geoscience, ecology, environmental science.The hydrocarbon isotope test macro of detailed hydrocarbon mainly comprises gas chromatography (GC), oxidation reaction apparatus or elevated temperature heat conversion equipment (C/TC) and isotopic ratio mass spectrum (IRMS) (IRMS) three parts composition, and system is called for short GC-C/TC-IRMS.Wherein gas chromatography is mainly used to hydrocarbon mixture is separated into the unimolecule compound, and its core is a capillary chromatographic column; The core of oxidation reaction apparatus or high temperature pyrolysis device is that an internal diameter is a 0.4mm micropore alundum (Al ceramic pipe.In the process of isotope test, the minor leakage of interface all may cause isotope fractionation in various degree and make measurement result deviation occur, and the leakproofness that therefore guarantees interface is one of pacing items of the hydrocarbon isotope test of detailed hydrocarbon.Present widely used connected mode is that the metal pressure ring is connected with graphite gasket, and the interface of capillary chromatographic column and ceramic reaction tube is positioned at chromatograph box, because the thermal expansivity difference between the different materials, frequent periodicity temperature variation is as easy as rolling off a log to make graphite pads loosening and produce seepage in various degree and cause test result deviation to occur, in addition, the attended operation of traditional approach is comparatively complicated, therefore be easy to cause the damage of micropore ceramic tube, how develop a kind of not easy to leak and the convenient interface that connects and then seem extremely important for the more hydrocarbon isotope of test unit hydrocarbon.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of not easy to leak is provided, the convenient connection, low-cost, the effective interface structure of seamless link capillary column ceramic pipe, this syndeton can more accurately be measured the hydrocarbon isotope value of detailed hydrocarbon.
In order to solve the problems of the technologies described above, the present invention is achieved by the following technical solutions:
The interface that connects capillary column and ceramic pipe in a kind of detailed hydrocarbon test macro, described interface comprises body, this body is arranged on the reaction tube that runs through the elevated temperature heat reacting furnace, and the input end of described reaction tube and output terminal are respectively by body and the mutual socket of capillary column; Second cavity body that described body is provided with first cavity body that the caliber with reaction tube adapts and adapts with the caliber of capillary column, described first cavity body runs through mutually with second cavity body and is connected.
Further, described body is a column structure, and the xsect of described column structure is annular, equilateral triangle or polygon annular.
As preferred version, can select to make things convenient for volume production lower-cost cylindrical structural for use.
Further, the diameter of described body cross-section is the 10-20 millimeter, and the length of body is the 20-30 millimeter.
As best design, the diameter of described xsect is 10 millimeters, and the optimum length of body is 20 millimeters.
Further, described body is to be made by silica gel, and the silica gel of employing is to have the good high temperature resistant type silica gel of elasticity.The good airproof performance of this kind silica gel, the extensibility height, high temperature resistant, resistance to ag(e)ing is good, low-bleed, and have advantages such as translucent, easy operation.
More specifically, described reaction tube is the micropore ceramics reaction tube.
More specifically, described capillary column is a quartz capillary column.
In sum, better elastic and the leakproofness thereof of this interface by utilizing silica gel realized seamless link between quartz capillary column and the micropore ceramic tube.
The invention has the beneficial effects as follows:
(1) its maximum operating temperature can reach 300 ℃, in this temperature range, detect to prove whether the m/z=40 of seepage sign signal is arranged by isotopic ratio mass spectrum (IRMS), and utilized the metallic graphite carbon packing ring to compare originally not detect tangible signal lifting, show that the sealing of this invention is good;
(2) reduce operation experiments (n 〉=150) by continuing repeatedly the temperature rising, do not find the lifting of m/z=40 signal equally, significantly loosening phenomenon then appears in the metallic graphite carbon packing ring under the same terms, and show the significantly lifting of m/z=40 baseline, show that sealing of the present invention is more reliable;
(3) the selection of material of the present invention is simple, easy to connect, because permeability is low, better elastic, good seal performance is enough continued under temperature variation condition repeatedly, thereby can improve the accuracy of utilizing the present invention to be used for test unit hydrocarbon carbon/hydrogen isotope numerical value;
(4) cost of manufacture is lower, and long service life has good use and promotional value.
Description of drawings
Fig. 1 is the one-piece construction synoptic diagram that connects the interface of capillary column and ceramic pipe in a kind of detailed hydrocarbon test macro of the present invention;
Fig. 2 is the enlarged diagram of A shown in Figure 1 of the present invention portion.
The division mark is as follows in the accompanying drawing: 1, body; 101, first cavity body; 102, second cavity body; 2, reaction tube; 3, capillary column; 4, gas chromatography; 5, isotopic ratio mass spectrum (IRMS) meter; 6, elevated temperature heat reacting furnace.
Embodiment
The interface that connects capillary column and ceramic pipe in a kind of detailed hydrocarbon test macro, described interface comprises body 1, this body 1 is arranged on the reaction tube 2 that runs through elevated temperature heat reacting furnace 6, and the input end of described reaction tube 2 and output terminal are respectively by body 1 and capillary column 3 mutual sockets; Second cavity body 102 that described body 1 is provided with first cavity body 101 that the caliber with reaction tube 2 adapts and adapts with the caliber of capillary column 3, described first cavity body 101 runs through mutually with second cavity body 102 and is connected.
It is the column structure of annular that body 1 adopts xsect, and the diameter of this circular cylindrical cross-section is 10 millimeters, and the length of body 1 is 20 millimeters.Described body 1 adopts silica gel to make, and this kind silica gel is to have the good high temperature resistant type silica gel of elasticity.The good airproof performance of this kind silica gel, the extensibility height, high temperature resistant, resistance to ag(e)ing is good, low-bleed, and have advantages such as translucent, easy operation.It is the micropore ceramics reaction tube that reaction tube 2 in the present embodiment adopts, and it is quartz capillary column that capillary column 3 adopts.
As further technological improvement to the interface of connection capillary column and ceramic pipe in embodiment 1 described a kind of detailed hydrocarbon test macro, it is the column structure of equilateral triangle that described body 1 can also be selected xsect for use, the diameter of this equilateral triangle xsect is 12 millimeters, and the length of body 1 is 25 millimeters.
Present embodiment adopts detailed hydrocarbon hydrogen isotope test macro that this kind interface is tested, described test macro mainly comprises: gas chromatography 4, elevated temperature heat reacting furnace 6 and isotopic ratio mass spectrum (IRMS) meter 5 three parts, unimolecule compound hydrogen isotope testing process is as follows, potpourri to be analyzed at first separates by gas chromatography 4, the unimolecule compound that flows out enters in the elevated temperature heat reburner 6 successively and is cracked into hydrogen, and its cracking process carries out in a high temperature micropore ceramic tube.By cracking, the unimolecule hydrocarbon compound at high temperature is converted into the hydrogen that isotope mass spectrometry can be analyzed.In this course, organic matter need carry out under up to the high temperature more than 1400 ℃, and when test macro was worked, sample at first was admitted to injector, is carried by carrier gas then and enters chromatographic column.Since in the sample each component in chromatographic column moving phase and stationary phase between distribute or the difference of adsorption coefficient, under the flushing of carrier gas, each component distributes in two-phase intercropping repeated multiple times, make each component in chromatographic column, obtain separating, after gas after separated enters elevated temperature heat reacting furnace 6 by quartz capillary column, by the high temperature micropore ceramics reaction tube that is arranged in the elevated temperature heat reburner hydrocarbon compound at high temperature is cracked into hydrogen again.Second cavity body 102 that interface described in the utility model is provided with first cavity body 101 that the caliber with reaction tube 2 adapts and adapts with the caliber of capillary column 3, described first cavity body 101 runs through mutually with second cavity body 102 and is connected.In test process, the maximum operating temperature of this interface can reach 300 ℃, in this temperature range, detect to prove whether the m/z=40 of seepage sign signal is arranged by isotopic ratio mass spectrum (IRMS), with utilized the metallic graphite carbon packing ring to compare originally not detect tangible signal lifting, the sealing that shows this kind structure is good, by continuing repeatedly temperature rising-reduction operation experiments (n 〉=150), do not find the lifting of m/z=40 signal equally, significantly loosening phenomenon then appears in the old metallic graphite carbon gasket construction under the same terms, and shows the significantly lifting of m/z=40 baseline.
In sum, the present invention has above-mentioned plurality of advantages and practical value, no matter it all has bigger improvement on product structure or function, obvious improvement is arranged technically, and produced good and practical effect, and meet current market demand, really be a new and innovative, progressive, practical new design.Have handled easily, practical safety, advantage such as cost is lower is convenient to promote and is made, and has wide research application prospect.
Obviously the foregoing description is not a limitation of the present invention, and the interface that connects capillary column and ceramic pipe in above-mentioned a kind of detailed hydrocarbon test macro can also have other many variations.Though gone through the present invention in conjunction with above-mentioned example, some that should be understood that professional person in the industry can expect apparently are identical, and alternative scheme is within the protection domain that all falls into claim of the present invention and limited.
Claims (7)
1. the interface that connects capillary column and ceramic pipe in the detailed hydrocarbon test macro, it is characterized in that, comprise body (1), described body (1) is arranged on the reaction tube (2) that runs through elevated temperature heat reacting furnace (6), and the input end of described reaction tube (2) and output terminal are respectively by body (1) and capillary column (3) socket mutually; Second cavity body (102) that described body (1) is provided with first cavity body (101) that the caliber with reaction tube (2) adapts and adapts with the caliber of capillary column (3), described first cavity body (101) runs through mutually with second cavity body (102) and is connected.
2. interface according to claim 1 is characterized in that, described body (1) is a column structure, and the xsect of described column structure is annular, equilateral triangle or polygon annular.
3. interface according to claim 2 is characterized in that, the diameter of described body (1) xsect is the 10-20 millimeter, and the length of described body (1) is the 20-30 millimeter.
4. interface according to claim 3 is characterized in that, the optimum diameter of described body (1) xsect is 10 millimeters, and the optimum length of described body (1) is 20 millimeters.
5. interface according to claim 4 is characterized in that, described body (1) is to be made by silica gel.
6. interface according to claim 5 is characterized in that, described reaction tube (2) is the micropore ceramics reaction tube.
7. interface according to claim 6 is characterized in that, described capillary column (3) is a quartz capillary column.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102571803A CN101949909A (en) | 2010-08-19 | 2010-08-19 | Connector for connecting capillary column with ceramic tube in individual hydrocarbon test system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102571803A CN101949909A (en) | 2010-08-19 | 2010-08-19 | Connector for connecting capillary column with ceramic tube in individual hydrocarbon test system |
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| Publication Number | Publication Date |
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| CN101949909A true CN101949909A (en) | 2011-01-19 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2010102571803A Pending CN101949909A (en) | 2010-08-19 | 2010-08-19 | Connector for connecting capillary column with ceramic tube in individual hydrocarbon test system |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109557217A (en) * | 2019-01-27 | 2019-04-02 | 广西科技大学鹿山学院 | A kind of gas-chromatography --- mass spectrometer interface seal joint pressing device |
| CN113916949A (en) * | 2021-09-30 | 2022-01-11 | 中国科学院西北生态环境资源研究院 | A catalytic cracking device and method for the determination of monomolecular hydrogen isotopes of hydrocarbon compounds |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2226768Y (en) * | 1994-05-12 | 1996-05-08 | 中国石化扬子石油化工公司 | Aluminium trioxide filling capillary chromatographic column |
-
2010
- 2010-08-19 CN CN2010102571803A patent/CN101949909A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2226768Y (en) * | 1994-05-12 | 1996-05-08 | 中国石化扬子石油化工公司 | Aluminium trioxide filling capillary chromatographic column |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109557217A (en) * | 2019-01-27 | 2019-04-02 | 广西科技大学鹿山学院 | A kind of gas-chromatography --- mass spectrometer interface seal joint pressing device |
| CN113916949A (en) * | 2021-09-30 | 2022-01-11 | 中国科学院西北生态环境资源研究院 | A catalytic cracking device and method for the determination of monomolecular hydrogen isotopes of hydrocarbon compounds |
| CN113916949B (en) * | 2021-09-30 | 2024-01-26 | 中国科学院西北生态环境资源研究院 | Catalytic cracking device and method for hydrocarbon compound single-molecule hydrogen isotope determination |
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Application publication date: 20110119 |