CN212008451U - High-purity gas oxygen content gas chromatograph - Google Patents
High-purity gas oxygen content gas chromatograph Download PDFInfo
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- CN212008451U CN212008451U CN202020610197.1U CN202020610197U CN212008451U CN 212008451 U CN212008451 U CN 212008451U CN 202020610197 U CN202020610197 U CN 202020610197U CN 212008451 U CN212008451 U CN 212008451U
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Abstract
The utility model relates to a high-purity gas oxygen content gas chromatograph, which comprises a detector and a ten-way valve, wherein ten through openings of the ten-way valve are numbered from one through ten clockwise in sequence; connect the dosing pipe between ten and seven openings of opening, opening one is connected with the three-way valve, and two other openings of three-way valve are connected with carrier gas respectively and advance the pipe and the reduction hydrogen advances the pipe, are connected with the adsorption desorption stove between two and six openings, and opening five is connected with the chromatographic column, and the chromatographic column connection detector, and opening eight is connected with the sample exit tube, and opening nine is connected with the sample and advances the pipe, and opening four is connected with carrier gas two and advances the pipe. The utility model discloses adsorb oxygen in the high-purity gas in the adsorption column in advance, thoroughly with oxygen argon separation back, improve the temperature of oxygen adsorption column, with absorbent miniflow oxygen release back in the adsorbent, send into the detector and detect, designed the activation device of adsorption column simultaneously, realized online activation adsorption column, trace oxygen in can the high-purity gas of rapid analysis.
Description
Technical Field
The utility model belongs to the technical field of gaseous detection, concretely relates to high-purity gaseous oxygen content gas chromatograph.
Background
In the analysis of high-purity gas, the measurement of the trace oxygen content is mostly carried out by an electrochemical method at present. Has the defects of short service life and low repeatability. When the traditional chromatography is used for analyzing the content of trace oxygen in high-purity gas, the oxygen and argon are difficult to separate, and the total data of the oxygen and argon are generally used for detection, so that the defect of large quantitative error exists.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a high-purity gas oxygen content gas chromatograph, when solving present chromatograph trace oxygen content's in high-purity gas analysis, because oxygen argon separation difficulty, generally detect with the data that oxygen argon adds up, have the problem of the big shortcoming of quantitative error.
The utility model discloses a high-purity gas oxygen content gas chromatograph, which comprises a detector and a ten-way valve, wherein ten through openings of the ten-way valve are numbered from one through ten clockwise in sequence; connect the dosing pipe between ten and seven openings of opening, opening one is connected with the three-way valve, and two other openings of three-way valve are connected with carrier gas respectively and advance the pipe and the reduction hydrogen advances the pipe, are connected with the adsorption desorption stove between two and six openings, and opening five is connected with the chromatographic column, and the chromatographic column connection detector, and opening eight is connected with the sample exit tube, and opening nine is connected with the sample and advances the pipe, and opening four is connected with carrier gas two and advances the pipe.
And the port III of the ten-way valve is connected with an emptying pipe, so that the gas can be emptied conveniently.
An adsorption column is arranged in the adsorption and desorption furnace, and a deoxidizer is filled in the adsorption column. The adsorption column is made of metal material with inner diameter of 4 mm and no catalytic activity, and 80-100 mesh 401 deoxidizer is filled in the adsorption column, so that the deoxidation effect is good.
Be equipped with heating rod and radiator fan in the adsorption and desorption stove, can realize rising fast and falling the temperature.
The length of the chromatographic column is 3 meters, the chromatographic column is a stainless steel pipe with the inner diameter of 2 millimeters, and a 60-80-mesh 13X molecular sieve is filled in the chromatographic column.
Compared with the prior art, the utility model has the advantages of:
the oxygen in the high-purity gas is adsorbed in the adsorption column in advance in the analysis process, the temperature of the oxygen adsorption column is improved after oxygen and argon are thoroughly separated, microflow oxygen adsorbed in the adsorbent is released and then sent to the detector for detection, meanwhile, the activation device of the adsorption column is designed, the on-line activation of the adsorption column is realized, the trace oxygen in the high-purity gas can be quickly analyzed, the separation is completed by adopting a method of adsorbing oxygen at low temperature and releasing oxygen at high temperature, and the oxygen content in the gas is quickly and accurately measured.
Drawings
FIG. 1 is a schematic structural view of the present invention;
in the figure: 1. a carrier gas inlet pipe, 2, a three-way valve, 3, an emptying pipe, 4, a carrier gas inlet pipe, 5, an adsorption column, 6, an adsorption and desorption furnace, 7, a detector, 8, a chromatographic column, 9, a ten-way valve, 10, a quantitative pipe, 11, a sample outlet pipe, 12, a sample inlet pipe, 13 and a reduction hydrogen inlet pipe.
Detailed Description
The following describes the embodiments of the present invention in further detail with reference to the accompanying drawings.
The high-purity gas oxygen content gas chromatograph shown in fig. 1 comprises a detector 7 and a ten-way valve 9, wherein ten ports of the ten-way valve 9 are numbered from one port to ten ports in a clockwise sequence; the valve disc mark is 1-10, has connect quantitative pipe 10 between ten and the seven opening of opening, and opening one is connected with three-way valve 2, and two other openings of three-way valve 2 are connected with carrier gas respectively and advance pipe 1 and reduction hydrogen and advance pipe 13, are connected with adsorption and desorption stove 6 between two openings and the six opening of opening, and opening five is connected with chromatographic column 8, and chromatographic column 8 connects detector 7, and opening eight is connected with sample exit tube 11, and opening nine is connected with the sample and advances pipe 12, and opening four is connected with carrier gas two and advances pipe 4.
And the port III of the ten-way valve 9 is connected with an emptying pipe 3.
An adsorption column 5 is arranged in the adsorption and desorption furnace 6, and a deoxidizer is filled in the adsorption column 5.
A heating rod and a cooling fan are arranged in the adsorption and desorption furnace 6. The adsorption column is made of metal material with length of 2 m and inner diameter of 4 mm and without catalytic activity, and is filled with 80-100 mesh 401 deoxidizer. The three-way valve is an electromagnetic stainless steel valve. The adsorption/desorption furnace has a heating rod and a heat radiation fan. Can realize rapid temperature rise and fall. The ten-way valve needs a valve body without dead volume and with a purging function. The length of the chromatographic column 8 is 3 meters, the chromatographic column 8 is a stainless steel pipe with the inner diameter of 2 millimeters, and the chromatographic column 8 is filled with a 60-80-mesh 13X molecular sieve at the use temperature of 50-80 ℃.
And (3) sample introduction: and the sample enters the nine port, the ten port, the quantitative tube, the seven port and the eight port of the ten-way valve through the sample inlet tube, and redundant sample is emptied through the sample outlet tube.
The analysis process comprises the following steps: the three-way valve connects the first carrier gas inlet pipe with the first port, the ten-way valve acts, and the first carrier gas passes through the first port, the tenth port, the quantitative pipe, the seventh port, the sixth port, the adsorption column, the second port and the third port of the ten-way valve; at the moment, oxygen in the sample in the quantitative pipe is adsorbed by the adsorption column, and other gases are discharged through the vent pipe. Meanwhile, the carrier gas II enters the port five through the port four and enters the chromatographic column, so that the purpose of protecting the chromatographic column is achieved, the effect of stably detecting the base flow is also achieved, and the fluctuation of a base line is prevented; and after the adsorption of the oxygen in the sample is finished, rapidly heating the adsorption and desorption furnace to 150 ℃, resetting the ten-way valve, and conveying the desorbed oxygen to the detector by the carrier gas I through the first port, the second port, the adsorption column, the sixth port, the fifth port and the chromatographic column of the ten-way valve. The detector uses a rapid temperature rise and fall multi-valve box multi-column box system of a gas chromatograph with application number 2017211636861 of the company to realize rapid and accurate determination of the oxygen content in the gas by adopting an external standard method for quantification.
And (3) activating an adsorption column: after a period of use, the adsorption column becomes saturated, and at this time, the adsorption column needs to be activated. The three-way valve is used for connecting the reducing hydrogen inlet pipe with the first port of the ten-way valve, the adsorption and desorption furnace is heated to 180 degrees, the ten-way valve acts, and the reducing hydrogen is discharged through the first port, the ten port, the quantitative pipe, the seventh port, the sixth port, the adsorption column, the second port and the third port of the ten-way valve. After 4 hours, the hydrogen gas activates the adsorption column completely.
The second carrier gas is used for providing shielding gas for the first chromatographic column 8.
To sum up, the utility model discloses adsorb oxygen in the high-purity gas in the adsorption column in advance, thoroughly with oxygen argon separation back, improve the temperature of oxygen adsorption column, with absorbent miniflow oxygen release back in the adsorbent, send into the detector and detect, designed the activation device of adsorption column simultaneously, realized online activation adsorption column, trace oxygen in can the high-purity gas of rapid analysis adopts cryosorption oxygen, and the separation is accomplished to the method of high temperature release oxygen, realizes fast, the oxygen content in the accurate survey gas.
In the description of the present invention, the terms "inside", "outside", "longitudinal", "lateral", "up", "down", "top", "bottom", etc. indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only for convenience of description of the present invention rather than requiring the present invention to be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention.
Claims (5)
1. A high-purity gas oxygen content gas chromatograph comprises a detector (7) and a ten-way valve (9), wherein ten ports of the ten-way valve (9) are numbered from one port to ten ports clockwise in sequence; the method is characterized in that: connect quantitative pipe (10) between ten and the seven ports of port, port one is connected with three-way valve (2), two other mouths of three-way valve (2) are connected with carrier gas respectively and advance pipe (1) and reduction hydrogen and advance pipe (13), be connected with between two and the six ports of port and inhale desorption stove (6), port five is connected with chromatographic column (8), detector (7) are connected to chromatographic column (8), port eight is connected with sample exit tube (11), port nine is connected with the sample and advances pipe (12), port four is connected with carrier gas two and advances pipe (4).
2. The high purity gas oxygen content gas chromatograph of claim 1, wherein: and the third port of the ten-way valve (9) is connected with an emptying pipe (3).
3. The high purity gas oxygen content gas chromatograph of claim 2, wherein: an adsorption column (5) is arranged in the adsorption and desorption furnace (6), and a deoxidizer is filled in the adsorption column (5).
4. The high purity gas oxygen content gas chromatograph of claim 2, wherein: and a heating rod and a cooling fan are arranged in the adsorption and desorption furnace (6).
5. The high purity gas oxygen content gas chromatograph of claim 2, wherein: the length of the chromatographic column (8) is 3 meters, the chromatographic column (8) is a stainless steel pipe with the inner diameter of 2 millimeters, and the chromatographic column (8) is filled with a 60-80-mesh 13X molecular sieve.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202020610197.1U CN212008451U (en) | 2020-04-22 | 2020-04-22 | High-purity gas oxygen content gas chromatograph |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202020610197.1U CN212008451U (en) | 2020-04-22 | 2020-04-22 | High-purity gas oxygen content gas chromatograph |
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| CN212008451U true CN212008451U (en) | 2020-11-24 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113058379A (en) * | 2021-03-04 | 2021-07-02 | 北京高麦克仪器科技有限公司 | Oxygen-argon separator |
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2020
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113058379A (en) * | 2021-03-04 | 2021-07-02 | 北京高麦克仪器科技有限公司 | Oxygen-argon separator |
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