CN217638884U - Gas chromatography detection device for trace impurities in high-purity carbon monoxide - Google Patents
Gas chromatography detection device for trace impurities in high-purity carbon monoxide Download PDFInfo
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Abstract
The utility model provides a gas chromatography detection device of trace impurity in high-purity carbon monoxide, including pneumatic valve, sampling system, chromatographic column, evacuation needle valve, carrier gas system and detector, the pneumatic valve includes two pneumatic ten logical valves and two pneumatic cross valves, and sampling system includes sample import, two ration rings and sample outlet, and the chromatographic column includes four chromatographic columns, and the evacuation needle valve includes five evacuation needle valves, and the carrier gas system includes four carrier gas branch pipes, and the detector is helium ionization detector. The utility model discloses a gather the sample and get into the pneumatic valve, gaseous through the pneumatic valve flow in ration ring, switch the sampling valve, the sample gets into the chromatographic column under the drive of carrier gas and separates, and the gas after the separation is through the principal component cutting technique after unloading, gets into the detector in proper order and detects, adopts gas chromatography detection device to carry out the analysis to high-purity carbon monoxide, once advances the appearance and can accomplish the complete component analysis to trace impurity, has effectively promoted the sensitivity and the efficiency of analysis.
Description
Technical Field
The utility model belongs to the technical field of trace impurity detects in the carbon monoxide, concretely relates to gas chromatography detection device of trace impurity in high-purity carbon monoxide.
Background
Carbon monoxide is colorless, odorless and non-irritant toxic gas, is extremely insoluble in water and has stable chemical properties, is a main component of synthesis gas and various coal gases, is an important raw material of organic chemical engineering, is a C1 chemical basis, and is used as a fuel and a reducing agent for refining metals.
The high-purity carbon monoxide used for chemical synthesis can be purified and separated from synthesis gas and water gas converted from natural gas containing carbon monoxide and petroleum, and tail gas of steel plants, calcium carbide plants and the like, and along with the rapid development of semiconductor and electronic industries, the high-purity carbon monoxide electronic gas is widely used in semiconductor process technologies such as plasma-assisted vapor deposition cavity purging, etching and the like due to the characteristic that the high-purity carbon monoxide electronic gas forms low-boiling-point carbonyl complexes with various transition metals such as copper, molybdenum, tantalum, tungsten and the like, and in addition, the high-purity carbon monoxide is also widely applied to the fields of medical intermediates, standard gas preparation, carbon monoxide lasers, environmental monitoring, scientific research and the like.
Gas chromatography is the detection and analysis of gaseous substances or substances that can be converted to gases at a certain temperature. The distribution coefficients of each component in the sample between gas phase and fixed liquid phase are different due to different physical properties of the substances, when the gasified sample is carried into a chromatographic column by carrier gas to operate, the components are repeatedly distributed between the two phases, and after flowing for a certain time, the components are separated from each other and leave the chromatographic column in sequence to enter a detector due to different adsorption or dissolution capacities of the fixed components, generated signals are amplified, chromatographic peaks of the components are drawn on a recorder, and different detection devices for detecting samples are different.
At present, for the detection of trace impurities in high-purity carbon monoxide, a thermal conductivity detector or a hydrogen flame ionization detector is usually adopted, the sensitivity and the precision are very low, and the full-component analysis can be realized only by adopting a plurality of chromatographs, so that the manpower and the material resources are wasted, the operation is troublesome and the efficiency is too low.
SUMMERY OF THE UTILITY MODEL
The utility model aims to solve the technical problem that the not enough to above-mentioned prior art provides a gas chromatography detection device of trace impurity in high-purity carbon monoxide to solve the problem that proposes in the above-mentioned background art.
In order to solve the technical problem, the utility model adopts the technical scheme that: a gas chromatography detection device for trace impurities in high-purity carbon monoxide comprises a pneumatic valve, a sample introduction system, a chromatographic column, an air release needle valve, a gas carrier system and a detector, wherein the pneumatic valve comprises a first pneumatic ten-way valve, a second pneumatic ten-way valve, a first pneumatic four-way valve and a second pneumatic four-way valve; the sample introduction system comprises a sample inlet, a first quantitative ring, a second quantitative ring and a sample outlet; the chromatographic columns comprise a first chromatographic column, a second chromatographic column, a third chromatographic column and a fourth chromatographic column; the emptying needle valve comprises a first emptying needle valve, a second emptying needle valve, a third emptying needle valve, a fourth emptying needle valve and a fifth emptying needle valve; the carrier gas system comprises a first carrier gas branch pipe, a second carrier gas branch pipe, a third carrier gas branch pipe and a fourth carrier gas branch pipe; the detector is a helium ionization detector.
Further, a first port, a second port, a third port, a fourth port, a fifth port, a sixth port, a seventh port, an eighth port, a ninth port and a tenth port which are distributed in sequence anticlockwise are arranged on the first pneumatic ten-way valve and the second pneumatic ten-way valve, wherein the first port and the second port are communicated with each other, the third port and the fourth port are communicated with each other, the fifth port and the sixth port are communicated with each other, the seventh port and the eighth port are communicated with each other, the ninth port and the tenth port are communicated with each other, a first quantitative ring is connected between the first port and the fourth port on the first pneumatic ten-way valve, the second port on the first pneumatic ten-way valve is connected with a sample inlet, the third port on the first pneumatic ten-way valve is connected with the second port on the second pneumatic ten-way valve, the tenth port on the first pneumatic ten-way valve is connected with a first branch pipe, the seventh port on the first pneumatic ten-way valve is connected with a second carrier gas, the fifth port on the first pneumatic ten-way valve is connected with a first color spectrum releasing valve, and the eighth port on the first pneumatic ten-way valve are connected with a first color spectrum releasing valve.
Furthermore, a second quantitative ring is connected between a first port and a fourth port on the second pneumatic ten-way valve, a third gas-carrying branch pipe is connected to a tenth port on the second pneumatic ten-way valve, a fourth gas-carrying branch pipe is connected to a seventh port on the second pneumatic ten-way valve, a third chromatographic column is connected between a fifth port and an eighth port on the second pneumatic ten-way valve, a second emptying needle valve is connected to a sixth port on the second pneumatic ten-way valve, and a sample outlet is connected to a third port on the second pneumatic ten-way valve.
Further, all be equipped with a mouthful, no. two mouthful, no. three mouthful and No. four mouths that are anticlockwise and distribute in proper order on first pneumatic cross valve and the pneumatic cross valve of second, wherein a mouthful and No. two mouthful intercommunication, no. three mouthful and No. four mouthful intercommunication each other, be connected with the fourth chromatographic column between a mouthful on the first pneumatic cross valve and No. four mouths on the pneumatic cross valve of second, no. two mouths on the first pneumatic cross valve and No. nine mouths on the pneumatic ten way valve of second are connected, no. three mouthful connection third air needle valve on the first pneumatic cross valve, no. four mouths on the first pneumatic cross valve connect the fourth air needle valve, no. one mouth on the pneumatic cross valve of second is connected with the ionization detector, be connected with the second chromatographic column between No. two mouths on the pneumatic cross valve of second and No. nine mouths on the pneumatic ten way valve of first, no. three mouths on the pneumatic cross valve of second is connected with the fifth air needle valve.
Further, the first chromatographic column is a carbon molecular sieve chromatographic column, the second chromatographic column is a 5A molecular sieve chromatographic column, the third chromatographic column is a Hayesep R chromatographic column, and the fourth chromatographic column is a Hayesep Q chromatographic column.
Further, the volumes of the first quantitative ring and the second quantitative ring are 0.2-1ml.
The operation of the device comprises the following steps:
s1, sample gas to be detected sequentially passes through a second port, a first quantitative ring, a fourth port and a third port on a first pneumatic ten-way valve through a sample inlet, then flows to the second port, the first port, a second quantitative ring, the fourth port and the third port on a second pneumatic ten-way valve, and finally flows to a sample outlet, wherein the first quantitative ring and the second quantitative ring are filled with the sample gas in the process;
s2, starting sample introduction, switching a first pneumatic ten-way valve, enabling carrier gas of a first carrier gas branch pipe to sequentially pass through a ten-port and a nine-port, carrying the sample gas into a second chromatographic column by the carrier gas for pre-separation, and enabling H to flow out of the pre-separation at first 2 +O 2 +Ar+N 2 The gas in the second port flows into the first port and then enters a helium ionization detector for detection;
s3, the first pneumatic ten-way valve is reset, the second carrier gas branch pipe passes through the seventh port and the eighth port of the first pneumatic ten-way valve, then the carrier gas brings the sample gas into the first chromatographic column for back flushing and outflow, and the outflow H is 2 +O 2 +Ar+N 2 The combined peak flows into a fifth port and a sixth port on the first pneumatic ten-way valve to a first emptying needle valve for emptying;
s4, starting to sample, and switching a second pneumatic ten-way valve and a third valveThe carrier gas of the carrier gas branch pipe sequentially passes through a tenth port, a ninth port, a second port and a first port on the first pneumatic four-way valve, at the moment, the carrier gas brings the sample gas into a fourth chromatographic column for pre-separation, and H which flows out firstly in the pre-separation 2 +O 2 +Ar+N 2 +CO+CH4+CO 2 The combined peak of the first pneumatic four-way valve flows into a fourth port on the second pneumatic four-way valve, the second pneumatic four-way valve rotates, gas in the fourth port flows into a third port, and then the fifth venting needle valve is vented;
s5, the second pneumatic ten-way valve is reset, the fourth carrier gas branch pipe passes through the seventh port and the eighth port of the second pneumatic ten-way valve, then the carrier gas brings the sample gas into the third chromatographic column for back flushing and outflow, and the outflow CH4+ CO is 2 The combined peak flows into a fifth port and a sixth port on the second pneumatic ten-way valve to a second emptying needle valve for emptying;
s6, separating the effluent H by using a second chromatographic column 2 +O 2 +Ar+N 2 The gas flows into a second port on a second pneumatic four-way valve, the second pneumatic four-way valve rotates, the gas in the second port flows into a first port, then the gas enters a helium ionization detector for detection, and the second pneumatic four-way valve is switched to enable a fourth chromatographic column to separate the flowing CH4+ CO 2 And entering a helium ionization detector for detection.
Compared with the prior art, the utility model has the following advantage:
the utility model discloses a gather the sample and get into the pneumatic valve, the pneumatic valve can realize admitting air as gas circuit control element, the sample gas flows into quantitative ring through the pneumatic valve, the ration that admits air can be realized to quantitative ring, switch the admission valve, the sample separates in getting into the chromatographic column respectively under the drive of carrier gas, gas after the separation is again through principal component cutting technique evacuation back, it obtains to get into the detector detection in proper order, adopt helium ionization gas chromatography detection device to micro-impurity H in to high-purity carbon monoxide 2 +O 2 +Ar+N 2 +CH 4 +CO 2 The analysis is carried out, the full component analysis of trace impurities can be completed by one-time sample injection, and the sensitivity and the efficiency of the analysis are effectively improved.
Drawings
Fig. 1 is a schematic view of the overall structure of the present invention.
Description of reference numerals:
1-a first carrier gas manifold; 2-a sample inlet; 3-a first quantitative ring; 4-a first pneumatic ten-way valve; 5-a second carrier gas manifold; 6-a third carrier gas branch pipe; 7-a second quantification loop; 8-a sample outlet; 9-a fourth carrier gas manifold; 10-a second vent needle valve; 11-a first vent needle valve; 12-a first chromatography column; 13-a second pneumatic ten way valve; 14-a third chromatographic column; 15-second chromatography column; 16-a third vent needle valve; 17-a fourth vent needle valve; 18-a first pneumatic four-way valve; 19-fourth chromatography column; 20-a fifth vent needle valve; 21-a second pneumatic four-way valve; 22-helium ionization detector.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
As shown in fig. 1, the utility model provides a technical solution: a gas chromatography detection device for trace impurities in high-purity carbon monoxide comprises a pneumatic valve, a sample introduction system, a chromatographic column, an emptying needle valve, a carrier gas system and a detector, wherein the pneumatic valve comprises a first pneumatic ten-way valve 4, a second pneumatic ten-way valve 13, a first pneumatic four-way valve 18 and a second pneumatic four-way valve 21, and the pneumatic valve adjusts the flow of gas by controlling the magnitude of signal pressure; the sample introduction system comprises a sample inlet 2, a first quantitative ring 3, a second quantitative ring 7 and a sample outlet 8, wherein the sample is fed from the sample inlet 2, gas enters the first quantitative ring 3 and the second quantitative ring 7, and a certain amount of sample in the quantitative rings is brought into the chromatographic column by a mobile phase through the switching of a pneumatic ten-way valve; the chromatographic columns comprise a first chromatographic column 12, a second chromatographic column 15, a third chromatographic column 14 and a fourth chromatographic column 19, and the chromatographic columns are used for separating and analyzing the sample gas; the emptying needle valves comprise a first emptying needle valve 11, a second emptying needle valve 10, a third emptying needle valve 16, a fourth emptying needle valve 17 and a fifth emptying needle valve 20, and the emptying needle valves mainly adjust the gas flow, so that the gas flowing out of the chromatographic column is emptied due to high adjustment precision; the carrier gas system comprises a first carrier gas branch pipe 1, a second carrier gas branch pipe 5, a third carrier gas branch pipe 6 and a fourth carrier gas branch pipe 9, and the carrier gas branch pipes provide stable and adjustable gas flow to ensure the normal operation of the gas chromatography detection device; the detector is a helium ionization detector 22 which serves to perform analytical detection of the gas.
The first pneumatic ten-way valve 4 and the second pneumatic ten-way valve 13 are respectively provided with a first port, a second port, a third port, a fourth port, a fifth port, a sixth port, a seventh port, an eighth port, a ninth port and a tenth port which are distributed in sequence in an anticlockwise mode, wherein the first port and the second port are communicated with each other, the third port and the fourth port are communicated with each other, the fifth port and the sixth port are communicated with each other, the seventh port and the eighth port are communicated with each other, the ninth port and the tenth port are communicated with each other, a first quantitative ring 3 is connected between the first port and the fourth port on the first pneumatic ten-way valve 4, the second port on the first pneumatic ten-way valve 4 is connected with a sample inlet 2, sample injection gas enters from the sample inlet 2, the sample inlet 2 is connected with the second port on the first pneumatic ten-way valve 4, the second port is connected with the first port, the first pneumatic ten-way valve 4 starts to operate, and the sample gas flows to the first quantitative ring 3;
the third port on the first pneumatic ten-way valve 4 and the second port on the second pneumatic ten-way valve 13 are connected with each other, the tenth port on the first pneumatic ten-way valve 4 is connected with a first carrier gas branch pipe 1, the seventh port on the first pneumatic ten-way valve 4 is connected with a second carrier gas branch pipe 5, a first chromatographic column 12 is connected between the fifth port and the eighth port on the first pneumatic ten-way valve 4, the sixth port on the first pneumatic ten-way valve 4 is connected with a first vent needle valve 11, the second carrier gas branch pipe 5 carries the gasified sample gas at a certain flow rate to enter the first chromatographic column 12 for separation, the separated components flow through the fifth port on the first pneumatic ten-way valve 4, the first pneumatic ten-way valve 4 operates, the gas in the fifth port flows into the sixth port, and then the gas in the sixth port flows to the first vent needle valve 11 for venting.
A second quantitative ring 7 is connected between the first port and the fourth port of the second pneumatic ten-way valve 13, the gas flowing out of the first quantitative ring 3 flows to the second port and the first port of the second pneumatic ten-way valve 13 through the third port and the fourth port of the first pneumatic ten-way valve 4 and then flows into the second quantitative ring 7, and the gas in the second quantitative ring 7 flows to the sample outlet 8 through the third port and the fourth port of the second pneumatic ten-way valve 13; the ten-port of the second pneumatic ten-way valve 13 is connected with a third gas carrying branch pipe 6, the seventh port of the second pneumatic ten-way valve 13 is connected with a fourth gas carrying branch pipe 9, a third chromatographic column 14 is connected between the fifth port and the eighth port of the second pneumatic ten-way valve 13, the sixth port of the second pneumatic ten-way valve 13 is connected with a second vent needle valve 10, the fourth gas carrying branch pipe carries the gasified sample gas at a certain flow rate and enters the third chromatographic column 14 for separation, the separated component gas flows through the fifth port of the second pneumatic ten-way valve 13, the second pneumatic ten-way valve 13 rotates, the gas in the fifth port flows to the sixth port, and then the gas in the sixth port is vented to the second vent needle valve 10.
The first pneumatic four-way valve 18 and the second pneumatic four-way valve 21 are respectively provided with a first port, a second port, a third port and a fourth port which are distributed anticlockwise, the first port is communicated with the second port, the third port is communicated with the fourth port, a fourth chromatographic column 19 is connected between the first port on the first pneumatic four-way valve 18 and the fourth port on the second pneumatic four-way valve 21, the second port on the first pneumatic four-way valve 18 is connected with the ninth port on the second pneumatic ten-way valve 13, the third pneumatic branch pipe 6 carries the gasified sample gas into the tenth port and the ninth port on the second pneumatic ten-way valve 13 at a certain flow rate, the second port on the first pneumatic four-way valve 18 is operated, the gas in the second port flows into the fourth chromatographic column 19 through the first port for separation, the separated gas in each component flows through the fourth port on the second pneumatic four-way valve 21, the second pneumatic four-way valve 21 rotates, the gas in the fourth port flows into the third port, and the third port flows into the fifth port for back flushing of the needle valve 20.
A third port on the first pneumatic four-way valve 18 is connected with a third venting needle valve 16, a fourth port on the first pneumatic four-way valve 18 is connected with a fourth venting needle valve 17, a first port on the second pneumatic four-way valve 21 is connected with a helium ionization detector 22, a second chromatographic column 15 is connected between a second port on the second pneumatic four-way valve 21 and a ninth port on the first pneumatic ten-way valve 4, the first carrier gas branch pipe 1 carries the gasified sample gas at a certain flow rate to enter the tenth port on the first pneumatic ten-way valve 4, the first pneumatic ten-way valve 4 operates, the gas in the tenth port flows into the ninth port, then the sample gas in the ninth port flows into the second chromatographic column 15 for separation, each separated component gas flows to a second port on the second pneumatic four-way valve 21, the second pneumatic four-way valve 21 rotates, the gas in the second port flows to the first port, and then the separated and flowed gas enters the helium ionization detector 22 for analysis and detection.
The first chromatographic column 12 is a carbon molecular sieve chromatographic column, and has an inner diameter: 3mm, length: 0.6cm, the second chromatography column 15 is a 5A molecular sieve chromatography column, inner diameter: 3mm, length: 2cm, the third column 14 is a Hayesep R column, internal diameter: 3mm, length: 4cm, the fourth chromatographic column 19 is a Hayesep Q chromatographic column, internal diameter: 3mm, length: 4cm, separation is the core, the chromatographic column is the heart of a chromatographic system, the chromatographic column has the requirements of high column efficiency, good selectivity and high analysis speed, and the length of the chromatographic column can meet the requirement of trace impurity analysis.
The quantitative rings are communicated in the pneumatic valve to ensure the accuracy and consistency of sample injection, the volumes of the first quantitative ring 3 and the second quantitative ring 7 are 0.2-1ml, and if the accurate quantification is required and the importance is required, the sample injection is required to be carried out by multiple times of the volumes of the quantitative rings.
The operation of the device comprises the following steps:
s1, sample gas to be detected sequentially passes through a second port, a first quantitative ring 3, a fourth port and a third port on a first pneumatic ten-way valve 4 through a sample inlet 2, then flows to the second port, the first port, a second quantitative ring 7, the fourth port and the third port on a second pneumatic ten-way valve 13, and finally flows to a sample outlet 8, wherein the first quantitative ring 3 and the second quantitative ring 7 are filled with the sample gas in the process;
s2, starting to sample, switching the first pneumatic ten-way valve 4, enabling the carrier gas of the first carrier gas branch pipe 1 to sequentially pass through a No. ten port and a No. nine port, carrying the sample gas into the second chromatographic column 15 by the carrier gas for pre-separation, and enabling the pre-separation to flow out H firstly 2 +O 2 +Ar+N 2 The combined peak of the two-way valve (21) flows into a second port on the second pneumatic four-way valve (21), the second pneumatic four-way valve (21) operates, and the gas in the second port flows into a first port and then enters a helium ionization detector (22) for detection;
s3, resetting the first pneumatic ten-way valve 4, enabling the second carrier gas branch pipe 5 to pass through a seventh port and an eighth port on the first pneumatic ten-way valve 4, then enabling the carrier gas to bring the sample gas into the first chromatographic column 12 for back flushing and outflow, and enabling the outflow H to be back-flushed 2 +O 2 +Ar+N 2 The peak closing valve discharges the air from a fifth port and a sixth port on the first pneumatic ten-way valve 4 to the first emptying needle valve 11;
s4, starting sample introduction and switching the second pneumatic ten-way valve 13, enabling carrier gas of the third gas-carrying branch pipe 6 to sequentially pass through a No. ten port, a No. nine port and a No. two port and a No. one port on the first pneumatic four-way valve 18, enabling the carrier gas to bring sample gas into a fourth chromatographic column 19 for pre-separation, and pre-separating H flowing out first 2 +O 2 +Ar+N 2 +CO+CH4+CO 2 The peak closing signal of the second pneumatic four-way valve 21 flows into a fourth port on the second pneumatic four-way valve 21, the second pneumatic four-way valve 21 rotates, and the gas in the fourth port flows into a third port and then is discharged to a fifth discharge needle valve 20;
s5, resetting the second pneumatic ten-way valve 13, enabling the fourth carrier gas branch pipe 9 to pass through a seventh port and an eighth port on the second pneumatic ten-way valve 13, then enabling the carrier gas to bring the sample gas into a third chromatographic column 14 for back flushing and outflow, and enabling the outflow CH4+ CO to be discharged 2 The combined peak flows into a fifth port and a sixth port on the second pneumatic ten-way valve 13 to a second emptying needle valve 10 for emptying;
s6, separating the effluent H by the second chromatographic column 15 2 +O 2 +Ar+N 2 Flows into the second port of the second pneumatic four-way valve 21, the second pneumatic four-way valve 21 rotates, and the gas in the second port flows intoThe first port is connected with a helium ionization detector 22 for detection, and then a second pneumatic four-way valve 21 is switched to enable a fourth chromatographic column 19 to separate the flowing CH4+ CO 2 And enters a helium ionization detector 22 for detection.
It should be noted that, in this document, relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. The utility model provides a gas chromatography detection device of trace impurity in high-purity carbon monoxide which characterized in that: the system comprises a pneumatic valve, a sample introduction system, a chromatographic column, an emptying needle valve, a carrier gas system and a detector, wherein the pneumatic valve comprises a first pneumatic ten-way valve (4), a second pneumatic ten-way valve (13), a first pneumatic four-way valve (18) and a second pneumatic four-way valve (21); the sample introduction system comprises a sample inlet (2), a first quantitative ring (3), a second quantitative ring (7) and a sample outlet (8); the chromatographic columns comprise a first chromatographic column (12), a second chromatographic column (15), a third chromatographic column (14) and a fourth chromatographic column (19); the emptying needle valve comprises a first emptying needle valve (11), a second emptying needle valve (10), a third emptying needle valve (16), a fourth emptying needle valve (17) and a fifth emptying needle valve (20); the carrier gas system comprises a first carrier gas branch pipe (1), a second carrier gas branch pipe (5), a third carrier gas branch pipe (6) and a fourth carrier gas branch pipe (9); the detector is a helium ionization detector (22).
2. The gas chromatography detection device for trace impurities in high-purity carbon monoxide as claimed in claim 1, wherein the first pneumatic ten-way valve (4) and the second pneumatic ten-way valve (13) are respectively provided with a first port, a second port, a third port, a fourth port, a fifth port, a sixth port, a seventh port, an eighth port, a ninth port and a tenth port which are distributed in a counterclockwise sequence, wherein the first port and the second port are communicated with each other, the third port and the fourth port are communicated with each other, the fifth port and the sixth port are communicated with each other, the seventh port and the eighth port are communicated with each other, the ninth port and the tenth port are communicated with each other, a first quantitative ring (3) is connected between the first port and the fourth port on the first pneumatic ten-way valve (4), the second port on the first pneumatic ten-way valve (4) is connected with a sample inlet (2), the third port on the first pneumatic ten-way valve (4) and the second port on the second pneumatic ten-way valve (13) are connected with a carrier gas inlet (2), the third port on the first pneumatic ten-way valve (4) and the second pneumatic needle valve (11) are connected with a carrier gas branch (11) on the first pneumatic ten-way valve (4), and the tenth pneumatic needle valve (11) are connected with a carrier gas branch (11).
3. The gas chromatography detection device for trace impurities in high-purity carbon monoxide according to claim 2, wherein one of the first port and the fourth port of the second pneumatic ten-way valve (13)
The spacing second ration ring (7) that is connected with, the ten number mouth on the pneumatic ten logical valve of second (13) is connected with third carrier gas branch pipe (6), the seven number mouth on the pneumatic ten logical valve of second (13) is connected with fourth carrier gas branch pipe (9), be connected with third chromatography post (14) between the five number mouth and the eight number mouth on the pneumatic ten logical valve of second (13), the six number mouth on the pneumatic ten logical valve of second (13) is connected with second and puts empty needle valve (10), no. three mouth on the pneumatic ten logical valve of second (13) is connected with sample export (8).
4. The gas chromatography detection device for trace impurities in high-purity carbon monoxide according to claim 1, wherein a first port, a second port, a third port and a fourth port which are distributed in turn counterclockwise are arranged on the first pneumatic four-way valve (18) and the second pneumatic four-way valve (21), the first port and the second port are communicated with each other, the third port and the fourth port are communicated with each other, a fourth chromatographic column (19) is connected between the first port on the first pneumatic four-way valve (18) and the fourth port on the second pneumatic four-way valve (21), the second port on the first pneumatic four-way valve (18) and the ninth port on the second pneumatic ten-way valve (13) are connected, the third port on the first pneumatic four-way valve (18) is connected with the third venting needle valve (16), the fourth port on the first pneumatic four-way valve (18) is connected with the fourth venting needle valve (17), the first port on the second pneumatic four-way valve (21) is connected with the helium detector (22), the second port on the second pneumatic four-way valve (21) is connected with the ninth port on the second pneumatic four-way valve (15), and the ninth port on the second pneumatic four-way valve (20) is connected with the ninth port on the fifth pneumatic ten-way valve (15).
5. The gas chromatography detection device for trace impurities in high-purity carbon monoxide according to claim 1, wherein the first chromatographic column (12) is a carbon molecular sieve chromatographic column, the second chromatographic column (15) is a 5A molecular sieve chromatographic column, the third chromatographic column (14) is a Hayesep R chromatographic column, and the fourth chromatographic column (19) is a Hayesep Q chromatographic column.
6. The gas chromatography detection device for trace impurities in high-purity carbon monoxide according to claim 1, wherein the volumes of the first quantitative ring (3) and the second quantitative ring (7) are 0.2-1ml.
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CN117890492A (en) * | 2023-12-08 | 2024-04-16 | 江苏南大光电材料股份有限公司 | Chromatographic Fourier infrared combined analysis system and method |
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