CN204575606U - For the in-line analyzer of Analysis of Micro-amount Impurities In Liquid in electron level tungsten hexafluoride - Google Patents
For the in-line analyzer of Analysis of Micro-amount Impurities In Liquid in electron level tungsten hexafluoride Download PDFInfo
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- CN204575606U CN204575606U CN201520246286.1U CN201520246286U CN204575606U CN 204575606 U CN204575606 U CN 204575606U CN 201520246286 U CN201520246286 U CN 201520246286U CN 204575606 U CN204575606 U CN 204575606U
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- transfer valve
- valve
- number interface
- chromatographic column
- analysis
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- NXHILIPIEUBEPD-UHFFFAOYSA-H tungsten hexafluoride Chemical compound F[W](F)(F)(F)(F)F NXHILIPIEUBEPD-UHFFFAOYSA-H 0.000 title claims abstract description 36
- 238000004458 analytical method Methods 0.000 title claims abstract description 24
- 239000012535 impurity Substances 0.000 title claims abstract description 19
- 239000007788 liquid Substances 0.000 title claims abstract description 12
- 239000007789 gas Substances 0.000 claims description 22
- 239000012159 carrier gas Substances 0.000 claims description 14
- 206010037544 Purging Diseases 0.000 claims description 6
- 238000010926 purge Methods 0.000 claims description 6
- 238000005260 corrosion Methods 0.000 claims description 4
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002685 polymerization catalyst Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
The utility model is a kind of in-line analyzer for Analysis of Micro-amount Impurities In Liquid in electron level tungsten hexafluoride, comprise sample inlet gas circuit, sample export gas circuit, transfer valve, chromatographic column, emptying needle-valve and detecting device, it is characterized in that: the first transfer valve is provided with the first quantity tube, the first chromatographic column and the first emptying needle-valve, and the second transfer valve is provided with the second quantity tube, the 3rd transfer valve is provided with the second emptying needle-valve, the 3rd emptying needle-valve and detecting device; Be provided with the second chromatographic column between first transfer valve and the 3rd transfer valve, between the second transfer valve and the 3rd transfer valve, be provided with the 3rd chromatographic column.The utility model circulation sample introduction analysis mode, improves the stability of analysis result, reduces the failure rate of equipment, and the high sensitivity of the plasma emission detecting device adopted makes detectability of the present utility model can reach ppb rank.
Description
Technical field
The utility model relates to a kind of online analytical instrument, a kind of checkout equipment analyzed for electron level tungsten hexafluoride is particularly disclosed, realize robotization circulation sample introduction and analyze ppb rank impurity in tungsten hexafluoride, successfully realize the on-line analysis of trace impurity in tungsten hexafluoride.
Background technology
Tungsten hexafluoride (WF6) is at room temperature a kind of colourless, odorless gas or transparent liquid, and its density is maximum in known gas, and its molecule has symmetrical regular octahedron structure at normal temperatures, and has diamagnetism.Tungsten hexafluoride is toxic gas, has strong impulse and corrosive attack to respiratory tract, eyes and skin.Unstable in air and water, tungstic acid and hydrogen fluoride can be generated rapidly, similar hydrofluoric burn can be produced to skin.
In the fluoride of tungsten, tungsten hexafluoride is unique stable and by the kind of suitability for industrialized production.Its main application is in the electronics industry as the starting material of tungsten chemical vapor deposition (CVD) technique.It also can be used for manufacturing some tungsten member.In addition tungsten hexafluoride is also widely used as the raw material of fluorization agent, polymerization catalyst and optical material.Along with the develop rapidly of electronics industry, the demand expanding day of tungsten hexafluoride, but China not yet formulates the relevant criterion about electron level tungsten hexafluoride at present, due to the disappearance of related detecting method and standard, there is blind spot for the quality of tungsten hexafluoride in domestic manufacturers and user, causes very large impact to production and application.
Summary of the invention
The purpose of this utility model is to address the deficiencies of the prior art, design a kind of in-line analyzer for Analysis of Micro-amount Impurities In Liquid in electron level tungsten hexafluoride, there is dependable performance, the advantages such as continuous operation troubles rate is low, point in-line analyzer that be a set of applicable China's national situation, can accept for users.The utility model improves the security analyzing tungsten hexafluoride, can carry out on-line analysis, can detect the impurity of ppb rank in tungsten hexafluoride to the trace impurity in electron level tungsten hexafluoride.
The utility model is achieved in that a kind of in-line analyzer for Analysis of Micro-amount Impurities In Liquid in electron level tungsten hexafluoride, comprise sample inlet gas circuit, sample export gas circuit, transfer valve, chromatographic column, emptying needle-valve and detecting device, it is characterized in that: the first transfer valve is provided with the first quantity tube, the first chromatographic column and the first emptying needle-valve, and the second transfer valve is provided with the second quantity tube, the 3rd transfer valve is provided with the second emptying needle-valve, the 3rd emptying needle-valve and detecting device; Be provided with the second chromatographic column between first transfer valve and the 3rd transfer valve, between the second transfer valve and the 3rd transfer valve, be provided with the 3rd chromatographic column.
As preferably, the first carrier gas gas circuit is connected with the 4. number interface of the first transfer valve, the second carrier gas gas circuit is connected with a 7. number interface for the first transfer valve; Sample inlet gas circuit is connected with a 2. number interface for the first transfer valve, and the 1. number interface of the first transfer valve is connected with a 5. number interface for the second transfer valve; 3. number interface of the first transfer valve is provided with the first quantity tube with the pipeline that 10. number interface is connected; 5. number interface of the first transfer valve is provided with the first chromatographic column with the pipeline that 9. number interface is connected; 6. number interface of the first transfer valve is provided with the second chromatographic column with the pipeline that 5. number interface is connected of the 3rd transfer valve.
As preferably, the 3rd carrier gas gas circuit is connected with a 3. number interface for the second transfer valve; Second transfer valve) 1. number interface be provided with the second quantity tube with the pipeline that 4. number interface is connected, the 2. number interface of the second transfer valve is provided with the 3rd chromatographic column with the pipeline that 3. number interface is connected of the 3rd transfer valve.
As preferably, the 3rd emptying needle-valve is connected with a 6. number interface for the 3rd transfer valve, and the second emptying needle-valve is connected with a 2. number interface for the 3rd transfer valve; Detecting device is connected with a 4. number interface for the 3rd transfer valve.
As preferably, first transfer valve is the pneumatic transfer valve of ten logical purgings, second transfer valve, the 3rd transfer valve are the pneumatic transfer valve of six logical purgings, and detecting device using plasma emission detector (PED detecting device), all connecting tubes and chromatographic column all adopt the parts through anti-corrosion treatment.
The beneficial effects of the utility model are: the utility model is analyzed for trace impurity in electron level tungsten hexafluoride, adopt on-line analysis, circulation input mode, selected and heartcut method by the stratographic analysis flow process that redesigns, chromatographic column, realize once online sample introduction and can complete inorganic impurity (H in tungsten hexafluoride
2, O
2+ Ar, N
2, CF
4, CO
2, CO, N
2o, SF
6) total analysis.The utility model also adopts anti-corrosion treatment to all connecting tubes and chromatographic column, improve the security of the analysis of tungsten hexafluoride, and circulation sample introduction analysis mode of the present utility model, improve the stability of analysis result, reduce the failure rate of equipment, the high sensitivity of the plasma emission detecting device adopted makes detectability of the present utility model can reach ppb rank, have highly sensitive, reproducible, the advantage that degree of safety is high.
Accompanying drawing explanation
Fig. 1 is the sample introduction analysis process schematic diagram of the utility model in-line analyzer.
Fig. 2 is the first transfer valve of the present utility model and the second transfer valve sampling flowsheet schematic diagram.
Fig. 3 is the second chromatographic column of the present utility model and the 3rd chromatographic column heartcut schematic flow sheet.
In figure: 1, the first transfer valve; 2, the second transfer valve; 3, the 3rd transfer valve; 4, detecting device; 5, the first quantity tube; 6, the second quantity tube; 7, the first chromatographic column; 8, the second chromatographic column; 9, the 3rd chromatographic column; 11, the first carrier gas; 12, the second carrier gas; 13, the 3rd carrier gas; 14, sample inlet gas circuit; 15, sample export gas circuit; 16, the first emptying needle-valve; 17, the second emptying needle-valve; 18, the 3rd emptying needle-valve.
Embodiment
Below in conjunction with the drawings and the specific embodiments, the utility model is described in further detail.
With reference to the accompanying drawings 1 ~ 3, a kind of in-line analyzer for Analysis of Micro-amount Impurities In Liquid in electron level tungsten hexafluoride of the utility model, comprises sample inlet gas circuit 14, sample export gas circuit 15, transfer valve, chromatographic column, emptying needle-valve and detecting device.First transfer valve 1 is provided with the first quantity tube 5, first chromatographic column 7 and the first emptying needle-valve 16, second transfer valve 2 and is provided with the second quantity tube the 6, three transfer valve 3 and is provided with the second emptying needle-valve 17, the 3rd emptying needle-valve 18 and detecting device 4; Be provided with between first transfer valve 1 and the 3rd transfer valve 3 between second chromatographic column 8, second transfer valve 2 and the 3rd transfer valve 3 and be provided with the 3rd chromatographic column 9.
First carrier gas 11 gas circuit is connected with the 4. number interface of the first transfer valve 1, the second carrier gas 12 gas circuit is connected with a 7. number interface for the first transfer valve 1; Sample inlet gas circuit 14 is connected with a 2. number interface for the first transfer valve 1, and the 1. number interface of the first transfer valve 1 is connected with a 5. number interface for the second transfer valve 2; 3. number interface of the first transfer valve 1 is provided with the first quantity tube 5 with the pipeline that 10. number interface is connected; 5. number interface of the first transfer valve 1 is provided with the first chromatographic column 7 with the pipeline that 9. number interface is connected; 6. number interface of the first transfer valve 1 is provided with the second chromatographic column 8 with the pipeline that 5. number interface is connected of the 3rd transfer valve 3.
3rd carrier gas 13 gas circuit is connected with a 3. number interface for the second transfer valve 2; 1. the 2. number interface that number interface and the pipeline that 4. number interface is connected of the second transfer valve 2 are provided with the second quantity tube 6, second transfer valve 2 is provided with the 3rd chromatographic column 9 with the pipeline that 3. number interface is connected of the 3rd transfer valve 3.
3rd emptying needle-valve 18 is connected with a 6. number interface for the 3rd transfer valve 3, and the second emptying needle-valve 17 is connected with a 2. number interface for the 3rd transfer valve 3; Detecting device 4 is connected with a 4. number interface for the 3rd transfer valve 3.
First transfer valve is the pneumatic transfer valve of ten logical purgings, second transfer valve, the 3rd transfer valve are the pneumatic transfer valve of six logical purgings, detecting device using plasma emission detector (PED detecting device), all connecting tubes and chromatographic column all adopt the parts through anti-corrosion treatment.
The utility model is adopted heartcut, blowback and is realized being separated completely of tungsten hexafluoride and other impurity by emptying needle-valve emptying tungsten hexafluoride.Concrete steps are as follows:
1, the first transfer valve 1 adopts blowback flow process, and when sample introduction starts, the first carrier gas 11 enters the first chromatographic column 7 with the tungsten hexafluoride of the first quantity tube 5 and realizes pre-separation, makes H
2, O
2+ Ar, N
2, CO enters the second chromatographic column 8 and analyzes.As shown in Figure 2.
2, H is worked as
2, O
2+ Ar, N
2, after CO enters the second chromatographic column 8, switch first transfer valve 1 blowback tungsten hexafluoride etc. from the first emptying needle-valve 16 safety vent.As shown in Figure 1.
3, the second transfer valve 2 adopts six logical sample introduction flow processs, and the second carrier gas 12 enters the 3rd chromatographic column 9 with the tungsten hexafluoride of the second quantity tube 6 and analyzes.As shown in Figure 2.
4, the 3rd transfer valve 3 is that component in the second chromatographic column 8 and the 3rd chromatographic column 9 goes out peak transfer valve, utilizes the second emptying needle-valve 17 to control the appearance time of component in the 3rd chromatographic column 9, when the 3rd chromatographic column 9 realizes H
2, O
2+ Ar, N
2, after CO goes out peak, switch the 3rd transfer valve accurately, make CF
4, CO
2, N
2o, SF
6go out peak.As shown in Figure 3.
5, make tungsten hexafluoride by the second emptying needle-valve 17 safety vent when said components switches the 3rd transfer valve 3 after rolling.As shown in Figure 1.
The utility model achieves the on-line analysis of inorganic impurity in tungsten hexafluoride by above-mentioned steps, completes the online total analysis to electron level tungsten hexafluoride.
The above is preferred embodiment of the present utility model, allly describes equalization change that scope does according to patent disclosed in the utility model application and modifies, and all should belong to the scope of the utility model patent requirements protection.
Claims (5)
1. the in-line analyzer for Analysis of Micro-amount Impurities In Liquid in electron level tungsten hexafluoride, comprise sample inlet gas circuit, sample export gas circuit, transfer valve, chromatographic column, emptying needle-valve and detecting device, it is characterized in that: the first transfer valve (1) is provided with the first quantity tube (5), the first chromatographic column (7) and the first emptying needle-valve (16), second transfer valve (2) is provided with the second quantity tube (6), and the 3rd transfer valve (3) is provided with the second emptying needle-valve (17), the 3rd emptying needle-valve (18) and detecting device (4); Be provided with the second chromatographic column (8) between first transfer valve (1) and the 3rd transfer valve (3), between the second transfer valve (2) and the 3rd transfer valve (3), be provided with the 3rd chromatographic column (9).
2. according to the in-line analyzer for Analysis of Micro-amount Impurities In Liquid in electron level tungsten hexafluoride described in claim 1, it is characterized in that: the first carrier gas (11) gas circuit is connected with the 4. number interface of described first transfer valve (1), the second carrier gas (12) gas circuit is connected with a 7. number interface for described first transfer valve (1); Sample inlet gas circuit (14) is connected with a 2. number interface for described first transfer valve (1), and the 1. number interface of described first transfer valve (1) is connected with a 5. number interface for the second transfer valve (2); 3. number interface of described first transfer valve (1) is provided with the first quantity tube (5) with the pipeline that 10. number interface is connected; 5. number interface of described first transfer valve (1) is provided with the first chromatographic column (7) with the pipeline that 9. number interface is connected; 6. number interface of described first transfer valve (1) is provided with the second chromatographic column (8) with the pipeline that 5. number interface is connected of the 3rd transfer valve (3).
3. according to the in-line analyzer for Analysis of Micro-amount Impurities In Liquid in electron level tungsten hexafluoride described in claim 1, it is characterized in that: the 3rd carrier gas (13) gas circuit is connected with a 3. number interface for described second transfer valve (2); 1. number interface of described second transfer valve (2) is provided with the second quantity tube (6) with the pipeline that 4. number interface is connected, and the 2. number interface of described second transfer valve (2) is provided with the 3rd chromatographic column (9) with the pipeline that 3. number interface is connected of the 3rd transfer valve (3).
4. according to the in-line analyzer for Analysis of Micro-amount Impurities In Liquid in electron level tungsten hexafluoride described in claim 1, it is characterized in that: the 3rd described emptying needle-valve (18) is connected with a 6. number interface for the 3rd transfer valve (3), the second described emptying needle-valve (17) is connected with a 2. number interface for the 3rd transfer valve (3); Described detecting device (4) is connected with a 4. number interface for the 3rd transfer valve (3).
5. according to the in-line analyzer for Analysis of Micro-amount Impurities In Liquid in electron level tungsten hexafluoride described in claim 1, it is characterized in that: the first described transfer valve is the pneumatic transfer valve of ten logical purgings, second transfer valve, the 3rd transfer valve are the pneumatic transfer valve of six logical purgings, detecting device using plasma emission detector, all connecting tubes and chromatographic column all adopt the part through anti-corrosion treatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520246286.1U CN204575606U (en) | 2015-04-22 | 2015-04-22 | For the in-line analyzer of Analysis of Micro-amount Impurities In Liquid in electron level tungsten hexafluoride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520246286.1U CN204575606U (en) | 2015-04-22 | 2015-04-22 | For the in-line analyzer of Analysis of Micro-amount Impurities In Liquid in electron level tungsten hexafluoride |
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| Publication Number | Publication Date |
|---|---|
| CN204575606U true CN204575606U (en) | 2015-08-19 |
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|---|---|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106370746A (en) * | 2016-08-26 | 2017-02-01 | 湖南大学 | Gas-dissolved-in-vegetable-insulating-oil analyzer with oil-gas separation function and detecting method |
-
2015
- 2015-04-22 CN CN201520246286.1U patent/CN204575606U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106370746A (en) * | 2016-08-26 | 2017-02-01 | 湖南大学 | Gas-dissolved-in-vegetable-insulating-oil analyzer with oil-gas separation function and detecting method |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20191224 Address after: 201404 room 1087, building 2, No.228, Jinqian Road, Fengxian District, Shanghai Patentee after: Shengyu (Shanghai) Electronic Technology Co.,Ltd. Address before: 200436, room 13-14, No. 1577, Lane 201, West Road, Zhabei District, Shanghai Patentee before: SHANGHAI FULAOSI DETECTION TECHNOLOGY CO.,LTD. |
|
| TR01 | Transfer of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150819 |