CN103424490A - Gas chromatograph with plasma emission detector - Google Patents

Gas chromatograph with plasma emission detector Download PDF

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Publication number
CN103424490A
CN103424490A CN2013103706854A CN201310370685A CN103424490A CN 103424490 A CN103424490 A CN 103424490A CN 2013103706854 A CN2013103706854 A CN 2013103706854A CN 201310370685 A CN201310370685 A CN 201310370685A CN 103424490 A CN103424490 A CN 103424490A
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CN
China
Prior art keywords
plasma emission
detecting device
gas
emission detecting
gas chromatograph
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Pending
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CN2013103706854A
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Chinese (zh)
Inventor
方华
李建浩
庄鸿涛
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SHANGHAI HUAAI CHROMATOGRAPHIC ANALYSIS CO Ltd
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SHANGHAI HUAAI CHROMATOGRAPHIC ANALYSIS CO Ltd
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Priority to CN2013103706854A priority Critical patent/CN103424490A/en
Publication of CN103424490A publication Critical patent/CN103424490A/en
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Abstract

The invention relates to a gas chromatograph with a plasma emission detector. The gas chromatograph is characterized by comprising an internal purifier, an oxygen adsorption preventer, a six-way valve, an oxygen-argon separator, the plasma emission detector, and a digital voltage output device. The plasma emission detector comprises a selective filter. Carrier gas to be detected flows out of a steel cylinder and passes the internal purifier and the oxygen adsorption preventer before entering the six-way valve; when the six-way valve switches to the mode of sample introduction, the carrier gas carries sample gas to enter the oxygen-argon separator; after the sample gas is separated completely, components enter the plasma emission detector successively and are subjected to selective filtering by the selective filter; an optical signal is converted into an electrical signal; finally, the digital electronic signal is output by the digital voltage output device. The gas chromatograph is simple in structure, low in cost and convenient to operate.

Description

Gas chromatograph with the plasma emission detecting device
Technical field
The present invention relates to a kind of gas chromatograph, particularly disclose a kind of gas chromatograph with the plasma emission detecting device for high-purity gas and electronics industry field of gas detection.
Background technology
For the chromatograph of high-purity gas and electronics industry gas, all there is many disadvantages in the market.Although traditional hydrogen flame detector is highly sensitive, can only measure hydrocarbon, can measure carbon monoxide and carbon dioxide in the situation that install reburner additional.And the sensitivity of thermal conductivity detector (TCD) mensuration inorganic component is too low.In recent years, also there were some highly sensitive instruments to occur, as Zirconia detector, the argon ion detecting device, although sensitivity is very high, because there is selectivity, can only detects a certain gas or coordinate and just can complete the mensuration of all impurity components with other analytical instrument.Also having a kind of helium ionization detector, is a kind of common detector, and sensitivity is also higher, but must use expensive helium as carrier gas, and use cost is higher.In addition, during current gas chromatograph analysing impurity content, can only analysing impurity content under existing condition higher than the sample more than the ppm rank, the sample of low content can't detect; Need to reduce the chromatograph box temperature when oxygen separates with argon gas, will drop to even below 0 degree centigrade, with liquid nitrogen and solid carbon dioxide cooling, complicated operation, waste energy usually; When measuring other oxygen of ppm level, usually adopt macromolecule bead or molecular sieve chromatography post to be separated, according to the character of these two kinds of carriers, when oxygen content is very low, chromatographic column can be adsorbed a certain amount of oxygen content, thereby can't detect the oxygen of the low content in sample.And the purification devices of existing instrument and instrument split, transport very inconveniently, increases cost.
Summary of the invention
The objective of the invention is to address the deficiencies of the prior art, design a kind of gas chromatograph with the plasma emission detecting device, detectable substance content is at other impurity of ppt level, the problem of chromatographic column oxygen uptake when having solved existing chromatograph box temperature argon gas and oxygen separation and oxygen are at micro-content in the time of 50-60 ℃.
The present invention is achieved in that a kind of gas chromatograph with the plasma emission detecting device, it is characterized in that: described gas chromatograph comprises the built-in purifier connected successively, anti-block adsorbent equipment, six-way valve, oxygen argon tripping device, plasma emission detecting device and digital voltage output unit; Described plasma emission detecting device comprises the selection filtering apparatus; Tested carrier gas is flowed out from steel cylinder, enter six-way valve respectively after built-in purifier and anti-block adsorbent equipment, when six-way valve switches to the sample introduction state, carrier gas is carried sample gas and is entered oxygen argon tripping device, after sample gas completes separation, each component enters respectively the plasma emission detecting device, after selecting filtering apparatus to carry out the selectivity optical filtering, optical signalling is converted into electric signal, finally by the digital voltage output unit, digital electronic signal is exported.
Described plasma emission detecting device is outsourcing piece, originate from Canadian LDetek company, comprise radio-frequency generator, quartz ampoule, selection filtering apparatus and signal amplifier that order is installed in described plasma emission detecting device, described selection filtering apparatus is comprised of optical filter, photodiode; The working mechanism of described gas chromatograph mainly completes in this plasma emission detector, carrier gas is carried sample gas and is entered the plasma emission detecting device, effect through radio-frequency generator, sample gas forms emission spectrum, enter optical filter through quartz ampoule again, every kind of material forms after spectrum the wavelength that oneself is arranged, select the optical filter of different wave length according to the needs of analyzing, the material of mating plate is converted into electric signal to light signal by photodiode after filtration, and electric signal is directly exported to the digital voltage output unit by signal amplifier.
Described built-in purifier is also outsourcing piece, originates from Canadian LDetek company, and described built-in purifier contains two air-breathing beds, working temperature is 350 ℃ and 200 ℃, when carrier gas is passed through first air-breathing, the impurity except hydrogen all is adsorbed totally, and hydrogen is by the second air-breathing bed absorption.
The length of described oxygen argon tripping device is that 2m, bore are 3.2mm, and inside filling out can oxygen separation, the chromatographic column of the stainless steel of the 5A carrier of argon gas.Described anti-block adsorbent equipment length is that 2m, bore are 3.2mm, fills the chromatographic column of the stainless steel of active passivation chromatographic column carrier.Described digital voltage output unit, comprise a circuit board, directly exports digital voltage signal.
High performance plasmas emission detector of the present invention is a kind of common detector, it has very high response to inorganic and organic component, the above-mentioned any detecting device of remolding sensitivity all will exceed at least 2 orders of magnitude, and can use nitrogen, argon gas or helium as carrier gas, the relative usage cost is lower.
The invention has the beneficial effects as follows: the present invention is a kind of for analyzing the gas chromatograph of high-purity gas Analysis of Micro-amount Impurities In Liquid, can analyze quantitatively content ppt level Trace Components, solved the difficult problem that the analysis of ppt level Trace Components is separated with the lower oxygen argon of chromatograph box 50 degrees celsius, purifier and chromatographic apparatus one, structure is simpler, and digital voltage signal is directly exported, without the micro-current magnification version, and with low cost, easy to operate.
The advantage that the present invention compared with prior art had is:
1, solved the detection of ppt rank foreign gas content;
2, solved the chromatograph box difficult problem that oxygen separates with argon gas under normal temperature control;
3, solved the difficult problem that trace oxygen can't detect due to the absorption of chromatographic column.
The accompanying drawing explanation
Fig. 1 is the structural representation of gas chromatograph of the present invention.
Fig. 2 is gas chromatograph principle of work schematic diagram of the present invention.
In figure: 1, built-in purifier; 2, anti-block adsorbent equipment; 3, six-way valve; 4, oxygen argon tripping device; 5, select filtering apparatus; 6, plasma emission detecting device; 7, digital voltage output unit; 601, radio-frequency generator; 602, quartz ampoule; 603, optical filter; 604, photodiode; 605, signal amplifier.
Embodiment
With reference to the accompanying drawings 1 and accompanying drawing 2, a kind of gas chromatograph with the plasma emission detecting device of the present invention, comprise the built-in purifier 1 connected successively, anti-block adsorbent equipment 2, six-way valve 3, oxygen argon tripping device 4, plasma emission detecting device 6 and digital voltage output unit 7, plasma emission detecting device 6 comprises selects filtering apparatus 5.
Tested carrier gas is carried sample gas and is flowed out from steel cylinder, first pass through built-in purifier 1 and anti-block adsorbent equipment 2, effectively remove the content of foreign gas in carrier gas, then pass into the six-way valve 3 for gas sampling, when six-way valve 3 switches to the sample introduction state, make trace oxygen pass through rapidly the III mouth of six-way valve 3, enter the oxygen argon separating column of oxygen argon tripping device 4.After sample gas completes oxygen and argon gas detachment process, each component enters respectively plasma emission detecting device 6.
Plasma emission detecting device 6 is outsourcing piece, originates from Canadian LDetek company.Comprise radio-frequency generator 601, quartz ampoule 602, selection filtering apparatus and signal amplifier 605 that order is installed in plasma emission detecting device 6, select filtering apparatus to be formed by optical filter 603 and photodiode 604.The working mechanism of gas chromatograph mainly completes in this plasma emission detector 6, after carrier gas is carried sample gas and is entered plasma emission detecting device 6, through the effect of radio-frequency generator 601, sample gas forms emission spectrum, then enters optical filter 603 through quartz ampoule 602.Every kind of material forms after spectrum the wavelength that oneself is arranged, select the optical filter 603 of different wave length according to the needs of analyzing, the material of mating plate 603 is converted into electric signal to light signal by photodiode 604 after filtration, electric signal is directly exported to digital voltage output unit 7 by signal amplifier 605 again, thereby completes whole detection.
Built-in purifier 1 of the present invention is also outsourcing piece, originates from Canadian LDetek company, and built-in purifier 1 contains two air-breathing beds, working temperature is 350 ℃ and 200 ℃, when carrier gas is passed through first air-breathing, the impurity except hydrogen all is adsorbed totally, and hydrogen is by the second air-breathing bed absorption.
The length of oxygen argon tripping device 4 of the present invention is that 2m, bore are 3.2mm, and inside filling out can oxygen separation, the chromatographic column of the stainless steel of the 5A carrier of argon gas.Anti-block adsorbent equipment 2 length are that 2m, bore are 3.2mm, fill the chromatographic column of the stainless steel of active passivation chromatographic column carrier.Digital voltage output unit 7, comprise a circuit board, directly exports digital voltage signal.
But the present invention's detection level is in other foreign gas of ppt level, realize separating of oxygen and argon gas under the normal temperature control of chromatograph box, purifier and chromatograph are integrated, structure is simpler, directly exports digital voltage signal, without the micro-current magnification version, with low cost, easy to operate.

Claims (6)

1. the gas chromatograph with the plasma emission detecting device is characterized in that: described gas chromatograph comprises the built-in purifier connected successively, anti-block adsorbent equipment, six-way valve, oxygen argon tripping device, plasma emission detecting device and digital voltage output unit; Described plasma emission detecting device comprises the selection filtering apparatus; Tested carrier gas is flowed out from steel cylinder, enter six-way valve respectively after built-in purifier and anti-block adsorbent equipment, when six-way valve switches to the sample introduction state, carrier gas is carried sample gas and is entered oxygen argon tripping device, after sample gas completes separation, each component enters respectively the plasma emission detecting device, after selecting filtering apparatus to carry out the selectivity optical filtering, optical signalling is converted into electric signal, finally by the digital voltage output unit, digital electronic signal is exported.
2. according to the described gas chromatograph with the plasma emission detecting device of claim 1, it is characterized in that: described plasma emission detecting device is outsourcing piece, originate from Canadian LDetek company, comprise radio-frequency generator, quartz ampoule, selection filtering apparatus and signal amplifier that order is installed in described plasma emission detecting device, described selection filtering apparatus is comprised of optical filter, photodiode; The working mechanism of described gas chromatograph mainly completes in this plasma emission detector, carrier gas is carried sample gas and is entered the plasma emission detecting device, effect through radio-frequency generator, sample gas forms emission spectrum, enter optical filter through quartz ampoule again, every kind of material forms after spectrum the wavelength that oneself is arranged, select the optical filter of different wave length according to the needs of analyzing, the material of mating plate is converted into electric signal to light signal by photodiode after filtration, and electric signal is directly exported to the digital voltage output unit by signal amplifier.
3. according to the described gas chromatograph with the plasma emission detecting device of claim 1, it is characterized in that: described built-in purifier is also outsourcing piece, originate from Canadian LDetek company, described built-in purifier contains two air-breathing beds, working temperature is 350 ℃ and 200 ℃, when carrier gas is passed through first air-breathing, the impurity except hydrogen all is adsorbed totally, and hydrogen is by the second air-breathing bed absorption.
4. according to the described gas chromatograph with the plasma emission detecting device of claim 1, it is characterized in that: the length of described oxygen argon tripping device is that 2m, bore are 3.2mm, and inside filling out can oxygen separation, the chromatographic column of the stainless steel of the 5A carrier of argon gas.
5. according to the described gas chromatograph with the plasma emission detecting device of claim 1, it is characterized in that: described anti-block adsorbent equipment length is that 2m, bore are 3.2mm, fills the chromatographic column of the stainless steel of active passivation chromatographic column carrier.
6. according to the described gas chromatograph with the plasma emission detecting device of claim 1, it is characterized in that: described digital voltage output unit comprises a circuit board, directly exports digital voltage signal.
CN2013103706854A 2013-08-23 2013-08-23 Gas chromatograph with plasma emission detector Pending CN103424490A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105758965A (en) * 2016-03-10 2016-07-13 上海福劳斯检测技术有限公司 Plasma emission detector based food-grade carbon dioxide online analyzer
CN110736794A (en) * 2019-09-25 2020-01-31 浙江汇泽医药科技有限公司 two-dimensional gas chromatograph system and detection method applying same
CN113156008A (en) * 2021-04-19 2021-07-23 广西电网有限责任公司电力科学研究院 Analysis device for dissolved gas in insulating oil

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CN203490201U (en) * 2013-08-23 2014-03-19 上海华爱色谱分析技术有限公司 Gas chromatograph with plasma emission detector

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
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CN201637728U (en) * 2010-02-26 2010-11-17 沈阳洪生气体有限公司 Device for rapidly detecting constituents of hydrogen
CN101915811A (en) * 2010-07-16 2010-12-15 上海炫一电子科技有限公司 Universal device and method for analyzing impurities in high-purity non-corrosive gas
CN203490201U (en) * 2013-08-23 2014-03-19 上海华爱色谱分析技术有限公司 Gas chromatograph with plasma emission detector

Non-Patent Citations (3)

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Title
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105758965A (en) * 2016-03-10 2016-07-13 上海福劳斯检测技术有限公司 Plasma emission detector based food-grade carbon dioxide online analyzer
CN110736794A (en) * 2019-09-25 2020-01-31 浙江汇泽医药科技有限公司 two-dimensional gas chromatograph system and detection method applying same
CN113156008A (en) * 2021-04-19 2021-07-23 广西电网有限责任公司电力科学研究院 Analysis device for dissolved gas in insulating oil

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Application publication date: 20131204