CN207215766U - The gas-chromatography valve path system that a kind of high-purity Nitrogen trifluoride analysis is adsorbed with anaerobic - Google Patents
The gas-chromatography valve path system that a kind of high-purity Nitrogen trifluoride analysis is adsorbed with anaerobic Download PDFInfo
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- CN207215766U CN207215766U CN201720771875.0U CN201720771875U CN207215766U CN 207215766 U CN207215766 U CN 207215766U CN 201720771875 U CN201720771875 U CN 201720771875U CN 207215766 U CN207215766 U CN 207215766U
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Abstract
The utility model discloses the gas-chromatography valve path system that a kind of high-purity Nitrogen trifluoride analysis is adsorbed with anaerobic, using the valve path system of the post of four valve four, including 2 four-way valves, 2 ten-way valves, 2 quantitative loops, 4 root chromatogram columns, 11 pressure balance regulating valves and 1 chromatography with discharge ionization detector, system carrier gas is more than 99.9999% high-purity helium, the simple system, easy to operate, analysis is accurate.
Description
Technical field
It the utility model is related to the analytical equipment of Nitrogen trifluoride.
Background technology
Nitrogen trifluoride (NF3) because it has that etch-rate is fast, selectivity is high and does not stay residue being etched material surface
The advantages of matter, in field extensive applications such as integrated circuit, photovoltaic and displays (TFT-LCD).Due to the height of its purity,
It is larger to material etch influential effect, therefore accurately analyze NF3Main gaseous impurities O2、N2、CO、CO2、N2O and SF6Content show
Obtain particularly important.
CN102636598A discloses a kind of gas chromatographic valve road system for the fluorine-containing electronic gas analysis of a variety of high-purities
System and its application method, using the post of five valve four, single injected sampling can be completed to include NF3The fluorine-containing electronics spy gas of a variety of high-purities inside
Gaseous impurities measure, but its system complex, and because pre-separation post can adsorb micro amount of oxygen, therefore inevitable influence
High-purity N F3The degree of accuracy of middle micro amount of oxygen component analysis measure.
Utility model content
The technical problems to be solved in the utility model is to provide a kind of gas phase of high-purity Nitrogen trifluoride analysis anaerobic absorption
Chromatogram valve path system, the simple system is easy to operate, and analysis is accurate.
In order to solve the above technical problems, the bright valve path system using the post of four valve four of the utility model, including 2 four-way valves, 2
Individual ten-way valve, 2 quantitative loops, 4 root chromatogram columns, 11 pressure balance regulating valves and 1 chromatography with discharge ionization detector, system carrier gas
For more than 99.9999% high-purity helium；
Connect after the 1st interface connection pressure balance regulating valve 2 10 of first four-way valve 1 with helium gas source, the connection of the 2nd interface
Pressure balance regulating valve 11 is followed by gas vent, and interface 3 is connected with the 2nd interface of the second ten-way valve 3, and the 4th interface connects
Connect the 4th interface that the second analysis chromatographic column 8 is followed by the second four-way valve 4；
1st interface of the first ten-way valve 2 is communicated by pressure balance regulating valve 3 11 with helium gas source, the 2nd interface connection the
One analysis chromatographic column 6 is followed by the 2nd interface of the second four-way valve 4, and the first preseparation chromatography is connected between interface 3 and the 9th interface
The interface of post the 5, the 4th is communicated by pressure balance regulating valve 4 12 with helium gas source, and it is fixed that first is connected between the 5th interface and the 8th interface
The amount interface of ring the 20, the 6th is connected with the 6th interface of the second ten-way valve 3, the 7th interface connection sample inlet, the 10th interface connection pressure
Balance regulating valve 10 is followed by gas vent；
1st interface of the second ten-way valve 3 is communicated by pressure balance regulating valve 5 13 with helium gas source, and interface 3 and the 9th connects
The interface of the second preseparation chromatography post the 7, the 4th is connected between mouthful to communicate with helium gas source by pressure balance regulating valve 6 14, the 5th connects
The second quantitative loop 21, the 7th interface connection sample export, the connection pressure balance regulation of the 10th interface are connected between mouth and the 8th interface
Valve 9 17 is followed by gas vent；
The 1st interface connection chromatography with discharge ionization detector 22 of second four-way valve 4, interface 3 connection pressure balance regulating valve
8 16 are followed by gas vent.
First preseparation chromatography post, 5 preferred carbon molecular sieve (CST) chromatographic column.
The first analysis preferred 13X chromatographic columns of chromatographic column 6.
Second preseparation chromatography post, 7 preferred Hayesep D chromatographic columns.
The second analysis preferred Hayesep DB chromatographic columns of chromatographic column 8.
This valve path system includes three parts：Carrier gas regulating system, component separation system and detector.
1. carrier gas regulating system includes 11 pressure balance regulating valves and its carrier connecting line.Adjusted by pressure balance
Valve 9 introduces high-purity helium to valve path system, and pressure balance regulating valve 10~14 controls respectively enters the first four-way valve the 1, the 10th
The pressure and flow velocity of port valve 2, the second ten-way valve 3 and the carrier gas of the second four-way valve 4；Pressure balance regulating valve 15 control enter electric discharge from
The pressure and flow speed stability of the carrier gas of sonization detector 22；Pressure balance regulating valve 16~19 controls the first four-way valve 1, first respectively
The pressure and flow velocity of ten-way valve 2, the second ten-way valve 3 and the gas vent of the second four-way valve 4.
2. component separation system includes 2 four-way valves, 2 ten-way valves, 2 preseparation chromatography posts and 2 analysis chromatographic columns；
3. detector is chromatography with discharge ionization detector 22；
The utility model device has the characteristics that：
1. the device includes two groups of sample collection-pre-separation-piece-rate systems, the first ten-way valve 2, the first quantitative loop 20,
One preseparation chromatography post 5 and the first analysis chromatographic column 6 are first group；Second ten-way valve 3, the second quantitative loop 21, the second pre-separation
It is second group that chromatographic column 7 and second, which analyzes chromatographic column 8,.After single injected sampling, the sample collected in two quantitative loops can respectively enter
Respective preseparation chromatography post and analysis chromatographic column.
2. the system has blowback and heartcut function.The sample of the pre-separated pre-separation of chromatographic column 5 all the way, by cutting
Change the blowback of the first ten-way valve 2 and remove substrate NF3；Sample of the another way through the pre-separation of the second preseparation chromatography post 7, passes through the one or four
The heartcut substrate NF of port valve 13, influence of the substrate components to trace impurity content analysis is eliminated, avoids polluting and damages inspection
Survey device.
3. avoid oxygen to adsorb as preseparation chromatography post using carbon molecular sieve (CST) chromatographic column, improve oxygen analysis
The degree of accuracy, reduce systematic error.The accurate quantitative analysis of all dirt component including oxygen can be achieved.
System mode as shown in Figure 1, the application method of the utility model device include：
1. each valve of diagram is in "On" state, "Off" state is in after a valve actuation, is in "ON" shape after valve actuation again
State；
2. opening the first ten-way valve 2, collection of the sample in the first quantitative loop 20 is realized；The second ten-way valve 3 is opened,
Realize collection of the sample in the second quantitative loop 21；
3. close the first ten-way valve 2 and the second four-way valve 4, by the carrier gas of pressure balance regulating valve 12 by the first quantitative loop
The sample of 20 collections is blown into the first preseparation chromatography post 5；
4. after the pre-separation of the first preseparation chromatography post 5, pre-separation component O2、N2, CO enter first analysis chromatographic column 6；Beat
The first ten-way valve 2 is opened, other components are vented by blowback；
5. the O separated through the first analysis chromatographic column 62、N2, CO components, realized by the second four-way valve 4 to detector 22 tested
The detection of component；
6. closing the second ten-way valve 3, the first four-way valve 1 is opened, pressure balance regulating valve 14 exports carrier gas and quantified second
The sample gathered in ring 21 is blown into the second preseparation chromatography post 7；
7. after the pre-separation of the second preseparation chromatography post 7, pre-separation component N2、O2, CO is through the second ten-way valve 3 to the 1st
Port valve 1 is vented；
8. closing the first four-way valve 1, the second four-way valve 4 is opened, through the pre-separation component CF of the second preseparation chromatography post 74With
A small amount of NF3The second analysis chromatographic column 8 is entered through the first four-way valve 1, after the second analysis chromatographic column 8 separates, by the second four-way
Valve 4 realizes the detection of tested component to detector 22；
9. open the first four-way valve 1, a large amount of major constituent NF through the pre-separation of the second preseparation chromatography post 73Through the first four-way
Valve 1 is vented；
10. close the first four-way valve 1, the CO through the pre-separation of the second preseparation chromatography post 72、N2O、SF6With a small amount of NF3Through
One four-way valve 1 enters the second analysis chromatographic column 8, after the second analysis chromatographic column 8 separates, by the second four-way valve 4 to detector
22 realize the detection of tested component.
Brief description of the drawings
Fig. 1 is the utility model chromatogram valve path system schematic diagram.
Wherein：1. the first four-way valve；2. the first ten-way valve；3. the second ten-way valve；4. the second four-way valve；5. first pre- point
From chromatographic column；6. the first analysis chromatographic column；7. the second preseparation chromatography post；8. the second analysis chromatographic column；9~19. pressure balances
Regulating valve
Embodiment
To introduce technical scheme provided by the utility model in more detail, it is illustrated with reference to embodiment.
Embodiment 1
Gas-chromatography valve path system as shown in Figure 1, the separation detection for trace impurity in Nitrogen trifluoride.
The Nitrogen trifluoride trace impurity of purity more than 99.99% mainly includes：Oxygen (O2), nitrogen (N2), carbon monoxide (CO),
Carbon tetrafluoride (CF4), carbon dioxide (CO2), nitrous oxide (N2) and sulfur hexafluoride (SF O6)。
Carbon molecular sieve (CST) chromatographic column of first preseparation chromatography post 5 from long 2m.
13X molecular sieve chromatography post of the first analysis chromatographic column 6 from long 3m.
Hayesep D chromatographic column of the second preseparation chromatography post 7 from long 5m.
Hayesep DB chromatographic column of the second analysis chromatographic column 8 from long 5m.
1. as shown in Figure 1, each valve is in "On" state.
2. open the first ten-way valve 2 and the second ten-way valve 3, sample enter the first quantitative loop 20 and the second quantitative loop along pipeline
In 21, the collection of two quantitative loop samples is realized.
3. the first ten-way valve 2 and the second four-way valve 4 are closed, by the carrier gas of pressure balance regulating valve 12 through the first ten-way valve
The preseparation chromatography post 5 of the interface of the interface of 2 the 4th interface → the 5th → interface of the first quantitative loop the 20 → the 8th → the 9th → first, is realized miscellaneous
Matter component O2、N2, CO and other components pre-separation.
4. after the pre-separation of the first preseparation chromatography post 5, pre-separation component O2、N2, interface 3s of the CO through the first ten-way valve 2
→ the 2 interface → first analyzes chromatographic column 6；Open the first ten-way valve 2, the CF through the pre-separation of the first preseparation chromatography post 54、CO2、
N2O、SF6With major constituent NF3The interface of the 9th interface through the first ten-way valve 2 → the 10th, is vented by blowback；
5. the O separated through the first analysis chromatographic column 62、N2, CO components, by the interface of the interface of the second four-way valve 4 the 2nd → the 1st →
Detector 22, realizes the detection of tested component, and peak sequence is followed successively by O2、N2、CO；
6. closing the second ten-way valve 3, the second four-way valve 4 is opened, it is logical through the 20th that pressure balance regulating valve 14 exports carrier gas
The interface of the interface of 4th interface of valve 3 → the 5th → interface of the second quantitative loop the 21 → the 8th → the 9th, the second pre-separation color is blown into by sample
Compose post 7；
7. after the pre-separation of the second preseparation chromatography post 7, pre-separation component N2、O2, interface 3s of the CO through the second ten-way valve 3
Interface 3 → 2 interfaces → equilibrated valve 19 of the four-way valve 1 of → the 2 interface → first is vented；
8. closing the first four-way valve 1, the second four-way valve 4 is opened, through the pre-separation component CF of the second preseparation chromatography post 74With
A small amount of NF3The analysis chromatographic column 8 of the interface of interface 3 through the first four-way valve 1 → the 4th → second, is separated through the second analysis chromatographic column 8
Afterwards, by the 4th interface → 1 interface → detector 22 of the second four-way valve 4, the detection of tested component is realized；
9. the first four-way valve 1 is opened, a large amount of major constituent NF separated through the second preseparation chromatography post 73Through the first four-way valve 1
Interface 3 → 2 interfaces → equilibrated valve 19 be vented；
10. close the first four-way valve 1, the CO through the pre-separation of the second preseparation chromatography post 72、N2O、SF6With a small amount of NF3Through
The analysis chromatographic column 8 of the interface of the interface 3 of one four-way valve 1 → the 4th → second, after the second analysis chromatographic column 8 separates, by the two or four
The 4th interface → 1 interface → detector 22 of port valve 4, realizes the detection of tested component, and peak sequence is followed successively by CO2、N2O、
SF6。
After sample introduction, the final peak sequence of impurity is in Nitrogen trifluoride：O2、N2、CO、CF4、CO2、 N2O, SF6.During appearance
Between be respectively：2.45min, 3.03min, 4.81min, 8.01min, 15.44min, 17.91min, 21.83min.
Claims (2)
- A kind of 1. gas-chromatography valve path system that high-purity Nitrogen trifluoride analysis is adsorbed with anaerobic, using the Zhu Fa roads system of four valve four System, including 2 four-way valves, 2 ten-way valves, 2 quantitative loops, 4 root chromatogram columns, 11 pressure balance regulating valves and 1 discharge from Sonization detector, system carrier gas are more than 99.9999% high-purity helium；The 1st interface connection pressure balance regulating valve two (10) of first four-way valve (1) connects with helium gas source afterwards, the connection of the 2nd interface Pressure balance regulating valve 11 (19) is followed by gas vent, and interface 3 is connected with the 2nd interface of the second ten-way valve (3), and the 4th connects The analysis chromatographic column (8) of mouth connection second is followed by the 4th interface of the second four-way valve (4)；1st interface of the first ten-way valve (2) is communicated by pressure balance regulating valve three (11) with helium gas source, the 2nd interface connection the One analysis chromatographic column (6) is followed by the 2nd interface of the second four-way valve (4), and the first pre-separation is connected between interface 3 and the 9th interface Chromatographic column (5), the 4th interface are communicated by pressure balance regulating valve four (12) with helium gas source, are connected between the 5th interface and the 8th interface The first quantitative loop (20) is connect, the 6th interface is connected with the 6th interface of the second ten-way valve (3), the 7th interface connection sample inlet, and the 10th Interface connection pressure balance regulating valve ten (18) is followed by gas vent；First preseparation chromatography post (5) is carbon molecular sieve (CST) color Compose post；1st interface of the second ten-way valve (3) is communicated by pressure balance regulating valve five (13) with helium gas source, and interface 3 and the 9th connects The second preseparation chromatography post (7) is connected between mouthful, the 4th interface is communicated by pressure balance regulating valve six (14) with helium gas source, and the 5th The second quantitative loop (21), the 7th interface connection sample export, the connection pressure balance of the 10th interface are connected between interface and the 8th interface Regulating valve nine (17) is followed by gas vent；The 1st interface connection chromatography with discharge ionization detector (22) of second four-way valve (4), interface 3 connection pressure balance regulating valve Eight (16) are followed by gas vent.
- 2. gas-chromatography valve path system according to claim 1, it is characterized in that：First analysis chromatographic column (6) is 13X chromatograms Post；Second preseparation chromatography post (7) is Hayesep D chromatographic columns；Second analysis chromatographic column (8) is Hayesep DB chromatographic columns.
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| CN201720771875.0U CN207215766U (en) | 2017-06-23 | 2017-06-23 | The gas-chromatography valve path system that a kind of high-purity Nitrogen trifluoride analysis is adsorbed with anaerobic |
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| CN201720771875.0U CN207215766U (en) | 2017-06-23 | 2017-06-23 | The gas-chromatography valve path system that a kind of high-purity Nitrogen trifluoride analysis is adsorbed with anaerobic |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113063874A (en) * | 2021-04-02 | 2021-07-02 | 中国神华煤制油化工有限公司 | Device and method for analyzing impurities in air separation liquid oxygen |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113063874A (en) * | 2021-04-02 | 2021-07-02 | 中国神华煤制油化工有限公司 | Device and method for analyzing impurities in air separation liquid oxygen |
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Address after: 471012 room 103, office building, Geely Industrial Park, liming research and Design Institute of chemical industry, South Road, Geely science and Technology Park, Geely District, Luoyang City, Henan Province Patentee after: Luoyang Haohua Gas Technology Co.,Ltd. Address before: 471012 room 103, office building, Geely Industrial Park, liming research and Design Institute of chemical industry, South Road, Geely science and Technology Park, Geely District, Luoyang City, Henan Province Patentee before: LUOYANG DAWN DACHENG FLUORINE CHEMICAL Co.,Ltd. |