CN217180751U - A analytical equipment that is arranged in electron gas difluoromethane impurity to detect - Google Patents
A analytical equipment that is arranged in electron gas difluoromethane impurity to detect Download PDFInfo
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- CN217180751U CN217180751U CN202220751982.8U CN202220751982U CN217180751U CN 217180751 U CN217180751 U CN 217180751U CN 202220751982 U CN202220751982 U CN 202220751982U CN 217180751 U CN217180751 U CN 217180751U
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Abstract
The utility model discloses an analytical equipment that is arranged in electron gas difluoromethane impurity to detect, carry trachea, second year trachea, third year trachea, fourth year trachea, fifth year trachea, sixth year trachea, first switching valve, second diverter valve, third diverter valve, fourth diverter valve, fifth diverter valve, first quantitative ring, second ration ring, third ration ring, first chromatographic column, second chromatographic column, third chromatographic column, fourth chromatographic column, fifth chromatographic column, sixth chromatographic column, first needle valve, second needle valve, third needle valve, fourth needle valve, first helium ionization detector and second ionization detector including first. The utility model discloses realize once advancing the appearance simultaneously after, switch through the valve that optional puts into two helium ionization detectors respectively with required impurity, avoided the principal Components to disturb, realize the complete separation of target peak, increased the ration accuracy. The detection of trace impurities in the electronic gas difluoromethane is met.
Description
Technical Field
The utility model relates to an analytical equipment especially relates to an analytical equipment that is arranged in electron gas difluoromethane impurity to detect.
Background
Difluoromethane is a coolant with zero ozone loss potential, is a chlorofluorocarbon substitute in a new cooling system, and is widely applied to the refrigeration industry. Difluoromethane is also used in the manufacture of semiconductors and electronic products as a source of etching CF radicals during RF plasma processing as an etchant. The purity of difluoromethane will directly affect the yield and accuracy of electronic components. Thus, higher requirements are put on the impurity detection technology of the difluoromethane. However, the existing method for detecting difluoromethane impurities mainly uses a thermal conductivity detector and a hydrogen flame ionization detector, the sensitivity of the two detectors is difficult to meet the trace analysis requirement, and meanwhile, the problem that the quantitative result is inaccurate due to the fact that main components of difluoromethane cover adjacent impurity peaks exists. Therefore, it is an urgent problem for those skilled in the art to develop an analysis device for detecting impurities in electron gas difluoromethane.
SUMMERY OF THE UTILITY MODEL
The utility model provides a solve above-mentioned not enough, provide an analytical equipment that is arranged in electron gas difluoromethane impurity to detect.
The above object of the present invention is achieved by the following technical solutions: an analysis device for detecting impurities in electronic gas difluoromethane comprises a first gas carrying pipe, a second gas carrying pipe, a third gas carrying pipe, a fourth gas carrying pipe, a fifth gas carrying pipe, a sixth gas carrying pipe, a first switching valve, a second switching valve, a third switching valve, a fourth switching valve, a fifth switching valve, a first quantitative ring, a second quantitative ring, a third quantitative ring, a first chromatographic column, a second chromatographic column, a third chromatographic column, a fourth chromatographic column, a fifth chromatographic column, a sixth chromatographic column, a first needle valve, a second needle valve, a third needle valve, a fourth needle valve, a first helium ionization detector and a second helium ionization detector;
the first port of the first switching valve is an access end of a first gas carrying pipe, the second port of the first switching valve is connected with a first quantitative ring inlet, the third port of the first switching valve is a sample inlet, the fourth port of the first switching valve is connected with the third port of the second switching valve, the fifth port of the first switching valve is connected with a first quantitative ring outlet, the sixth port of the first switching valve is connected with a first chromatographic column outlet, the seventh port of the first switching valve is connected with a first needle valve, the eighth port of the first switching valve is an access end of a second gas carrying pipe, the ninth port of the first switching valve is connected with a second chromatographic column inlet, and the tenth port of the first switching valve is connected with a first chromatographic column inlet.
The first port of the second switching valve is an access end of a third gas carrying pipe, the second port of the second switching valve is connected with an inlet of a second quantitative ring, the fourth port of the second switching valve is connected with the sixth port of the third switching valve, the fifth port of the second switching valve is connected with an outlet of the second quantitative ring, the sixth port of the second switching valve is connected with an outlet of a third chromatographic column, the seventh port of the second switching valve is connected with a third needle valve, the eighth port of the second switching valve is an access end of a fourth gas carrying pipe, the ninth port of the second switching valve is connected with an inlet of the fourth chromatographic column, and the tenth port of the second switching valve is connected with an inlet of the third chromatographic column.
The first port of the third switching valve is connected with the third quantitative ring inlet, the second port of the third switching valve is an access end of a fifth gas carrying pipe, the third port of the third switching valve is connected with the fifth chromatographic column inlet, the fourth port of the third switching valve is connected with the third quantitative ring outlet, and the fifth port of the third switching valve is a sample outlet.
And a first port of the fourth switching valve is connected with an outlet of the second chromatographic column, a second port of the fourth switching valve is connected with the second needle valve, a third port of the fourth switching valve is connected with a fourth port of the fourth switching valve, a fifth port of the fourth switching valve is connected with an outlet of the fourth chromatographic column, and a sixth port of the fourth switching valve is connected with the first helium ionization detector. And a first port of the fifth switching valve is connected with an outlet of the fifth chromatographic column, a second port of the fifth switching valve is connected with a fourth needle valve, a third port of the fifth switching valve is connected with a fourth port of the fifth switching valve, and a sixth port of the fifth switching valve is connected with an inlet of the sixth chromatographic column. And the second helium ionization detector is connected with an outlet of the sixth chromatographic column.
Further, the first switching valve and the second switching valve are ten-way valves, and the third switching valve, the fourth switching valve and the fifth switching valve are six-way valves.
Further, the first chromatographic column is a TDX-01 stainless steel packed column with the outer diameter of 1/8 inches and the length of 0.6m, the second chromatographic column is a 5A molecular sieve stainless steel packed column with the outer diameter of 1/8 inches and the length of 2m, the third chromatographic column and the fourth chromatographic column are Porapak-Q stainless steel packed columns with the outer diameter of 1/8 inches and the length of 2m, and the fifth chromatographic column and the sixth chromatographic column are GasPro fused silica capillary columns with the inner diameter of 0.32mm and the length of 30 m.
Furthermore, the carrier gas in the first carrier gas pipe, the second carrier gas pipe, the third carrier gas pipe, the fourth carrier gas pipe, the fifth carrier gas pipe and the sixth carrier gas pipe is helium.
The analysis method adopting the analysis device for detecting the impurities in the electronic gas difluoromethane comprises the following steps:
s1: under the reset state, difluoromethane sample gas flows into a third port of the first switching valve, a first quantitative ring, a fourth port of the first switching valve, a third port of the second switching valve, a second quantitative ring, a fourth port of the second switching valve, a sixth port of the third switching valve, a third quantitative ring and a fifth port of the third switching valve from the sample inlet in sequence, and finally flows out from the sample outlet.
S2: and switching the first switching valve to an analysis state, blowing the sample in the first quantitative ring by using first carrier gas in the first carrier gas pipe to enter a first chromatographic column for pre-separation, and switching the first switching valve to a reset state (figure 1) after H2, O2+ Ar, N2, CH4, CO and CF4 enter a second chromatographic column, so that difluoromethane and other impurities are blown back and emptied from the first needle valve. Further, H2, O2+ Ar, N2, CH4, CO, CF4 exit the second chromatography column into the first helium ionization detector.
S3: and switching the second switching valve to an analysis state, blowing a third carrier gas in a third carrier gas pipe to carry a sample in a second quantitative ring to enter a third chromatographic column for pre-separation, switching the second switching valve to a reset state after H2, O2+ Ar, N2, CH4, CO, CF4 and CO2 flow into a fourth chromatographic column, blowing difluoromethane and other impurities out of the third needle valve, and switching the fourth switching valve to enable CO2 to enter the first ionization detector after H2, O2+ Ar, N2, CH4, CO and CF4 flow out of the fourth chromatographic column and are blown out of the second needle valve.
S4: switching the third switching valve to an analysis state, switching the fifth switching valve 15 to a venting state, blowing a sample in a third quantitative ring by using fifth carrier gas in a fifth carrier gas pipe to enter a fifth chromatographic column for pre-separation, venting the H2, O2+ Ar, N2, CH4, CO, CF4 and CO2 which flow out firstly through a fourth needle valve, switching the third switching valve and the fifth switching valve to a reset state, putting the trifluoromethane into a sixth chromatographic column, switching the fifth switching valve to a venting state, when a large amount of main component difluoromethane is vented through a fourth needle valve, and simultaneously, when the difluoro dichloromethane does not flow out of the fifth chromatographic column, switching the fifth switching valve to a reset state, so that the remaining small amount of main components of the difluoro methane, the difluoro dichloromethane, the difluoro monochloromethane, the fluoro dichloromethane and the dichloromethane flow into the sixth chromatographic column for re-separation, and then enter the second helium ionization detector.
Further, in step S2, the first switching valve is switched to the analysis state, the third switching valve is switched to the analysis state, and the fourth switching valve is switched to the analysis state.
Compared with the prior art, the utility model the advantage be: the utility model discloses a two helium ionization detectors of high sensitivity, five diverter valves, three ration ring, six chromatographic columns constitute an analytic system. After one-time simultaneous sample introduction is realized, the required impurities are selectively and respectively placed into the two helium ionization detectors through valve switching, so that the interference of main components is avoided, the complete separation of target peaks is realized, and the quantitative accuracy is increased. The detection of trace impurities in the electronic gas difluoromethane is met.
Drawings
Fig. 1 is a schematic structural diagram of the present invention in a reset state.
Fig. 2 is a schematic structural diagram of the present invention in an analysis state.
Fig. 3 is a schematic structural diagram of the present invention in the emptying state.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
As shown in fig. 1, fig. 2 and fig. 3, an analysis device for detecting impurities in electronic gas difluoromethane of the present invention includes a first gas carrying pipe 1, a second gas carrying pipe 2, a third gas carrying pipe 3, a fourth gas carrying pipe 4, a fifth gas carrying pipe 5, a sixth gas carrying pipe 6, a first switching valve 12, a second switching valve 13, a third switching valve 14, a fourth switching valve 15, a fifth switching valve 16, a first quantitative ring 9, a second quantitative ring 10, a third quantitative ring 11, a first chromatographic column 21, a second chromatographic column 22, a third chromatographic column 23, a fourth chromatographic column 24, a fifth chromatographic column 25, a sixth chromatographic column 26, a first needle valve 17, a second needle valve 18, a third needle valve 19, a fourth needle valve 20, a first helium ionization detector 27 and a second helium ionization detector 28;
the first port of the first switching valve 12 is an access end of the first gas carrying pipe 1, the second port of the first switching valve 12 is connected with an inlet of the first quantitative ring 9, the third port of the first switching valve 12 is a sample inlet 7, the fourth port of the first switching valve 12 is connected with the third port of the second switching valve 13, the fifth port of the first switching valve 12 is connected with an outlet of the first quantitative ring 9, the sixth port of the first switching valve 12 is connected with an outlet of the first chromatographic column 21, the seventh port of the first switching valve 12 is connected with the first needle valve 17, the eighth port of the first switching valve 12 is an access end of the second gas carrying pipe 2, the ninth port of the first switching valve 12 is connected with an inlet of the second chromatographic column 22, and the tenth port of the first switching valve 12 is connected with an inlet of the first chromatographic column 21.
The first port of the second switching valve 13 is an inlet end of the third gas carrying pipe 3, the second port of the second switching valve 13 is connected with an inlet of the second quantitative ring 10, the fourth port of the second switching valve 13 is connected with the sixth port of the third switching valve 14, the fifth port of the second switching valve 13 is connected with an outlet of the second quantitative ring 10, the sixth port of the second switching valve 13 is connected with an outlet of the third chromatographic column 23, the seventh port of the second switching valve 13 is connected with the third needle valve 19, the eighth port of the second switching valve 13 is an inlet end of the fourth gas carrying pipe 4, the ninth port of the second switching valve 13 is connected with an inlet of the fourth chromatographic column 24, and the tenth port of the second switching valve 13 is connected with an inlet of the third chromatographic column 23.
The first port of the third switching valve 14 is connected with the inlet of the third quantitative ring 11, the second port of the third switching valve 14 is the inlet of the fifth carrier gas pipe 5, the third port of the third switching valve 14 is connected with the inlet of the fifth chromatographic column 25, the fourth port of the third switching valve 14 is connected with the outlet of the third quantitative ring 11, and the fifth port of the third switching valve 14 is the sample outlet 8.
And a first port of the fourth switching valve 15 is connected with an outlet of the second chromatographic column 22, a second port of the fourth switching valve 15 is connected with the second needle valve 18, a third port of the fourth switching valve 15 is connected with a fourth port of the fourth switching valve 15, a fifth port of the fourth switching valve 15 is connected with an outlet of the fourth chromatographic column 24, and a sixth port of the fourth switching valve 15 is connected with the first helium ionization detector 27. And a first port of the fifth switching valve 16 is connected with an outlet of a fifth chromatographic column 25, a second port of the fifth switching valve 16 is connected with a fourth needle valve 20, a third port of the fifth switching valve 16 is connected with a fourth port of the fifth switching valve 16, and a sixth port of the fifth switching valve 16 is connected with an inlet of a sixth chromatographic column 26. The second helium ionization detector 28 is connected to the outlet of the sixth chromatographic column 26.
Further, the first switching valve 12 and the second switching valve 13 are ten-way valves, and the third switching valve 14, the fourth switching valve 15, and the fifth switching valve 16 are six-way valves.
Further, the first column 21 was a TDX-01 stainless steel packed column with an outer diameter of 1/8 inches and a length of 0.6m, the second column 22 was a 5A molecular sieve stainless steel packed column with an outer diameter of 1/8 inches and a length of 2m, the third and fourth columns 23 and 24 were Porapak-Q stainless steel packed columns with an outer diameter of 1/8 inches and a length of 2m, and the fifth and sixth columns 25 and 26 were GasPro fused silica capillary columns with an inner diameter of 0.32mm and a length of 30 m.
Furthermore, the carrier gas in the first carrier gas pipe 1, the second carrier gas pipe 2, the third carrier gas pipe 3, the fourth carrier gas pipe 4, the fifth carrier gas pipe 5 and the sixth carrier gas pipe 6 is helium.
The analysis method adopting the analysis device for detecting the impurities in the electron gas difluoromethane comprises the following steps:
s1: in the reset state (fig. 1), the difluoromethane sample gas flows into the third port of the first switching valve 12, the first quantitative ring 9, the fourth port of the first switching valve 12, the third port of the second switching valve 13, the second quantitative ring 10, the fourth port of the second switching valve 13, the sixth port of the third switching valve 14, the third quantitative ring 11 and the fifth port of the third switching valve 14 in sequence from the sample inlet 7, and finally flows out from the sample outlet 8.
S2: the first switching valve 12 is switched to an analysis state (figure 2), the first carrier gas in the first carrier gas pipe 1 blows the sample in the first quantitative ring 9 to enter the first chromatographic column 21 for pre-separation, and after H2, O2+ Ar, N2, CH4, CO and CF4 enter the second chromatographic column 22, the first switching valve 12 is switched to a reset state (figure 1), so that difluoromethane and other impurities are blown back and emptied from the first needle valve 17. Further, H2, O2+ Ar, N2, CH4, CO, CF4 exit the second chromatography column 22 to the first helium ionization detector 27.
S3: the second switching valve 13 is switched to the analysis state (fig. 2), the third carrier gas in the third carrier gas pipe 3 blows the sample in the second quantitative loop 10 into the third chromatographic column 23 for pre-separation, after H2, O2+ Ar, N2, CH4, CO, CF4 and CO2 flow into the fourth chromatographic column 24, the second switching valve 13 is switched to the reset state (fig. 1), difluoromethane and other impurities are blown back and emptied from the third needle valve 19, and after H2, O2+ Ar, N2, CH4, CO and CF4 flow out of the fourth chromatographic column 24 and are emptied by the second needle valve 18, the fourth switching valve 15 is switched to allow CO2 to enter the first helium ionization detector 27.
S4: switching the third switching valve 14 to an analysis state (fig. 2), switching the fifth switching valve 15 to an emptying state (fig. 3), blowing a fifth carrier gas in the fifth carrier gas pipe 5 to bring a sample in the third quantitative ring 11 into the fifth chromatographic column 25 for pre-separation, discharging H2, O2+ Ar, N2, CH4, CO, CF4 and CO2 through a fourth needle valve 20, switching the third switching valve 14 and the fifth switching valve 16 to a reset state (fig. 1), discharging trifluoromethane into the sixth chromatographic column 26, switching the fifth switching valve 16 to the emptying state (fig. 3), discharging a large amount of main component difluoromethane through the fourth needle valve while difluorodichloromethane does not flow out of the fifth chromatographic column, switching the fifth switching valve to the reset state (fig. 1), and allowing a small amount of main components difluoromethane, difluorodichloromethane, chlorochloromethane, monofluoromethane, fluorodichloromethane, the dichloromethane flows into a sixth chromatographic column for re-separation and then enters a second helium ionization detector.
Further, in step S2, the first switching valve 12 is switched to the analysis state, the third switching valve 13 is switched to the analysis state, and the fourth switching valve 14 is switched to the analysis state, as shown in fig. 2.
The above only is the embodiment of the present invention, not limiting the patent scope of the present invention, all the equivalent structures or equivalent processes that are used in the specification and the attached drawings or directly or indirectly applied to other related technical fields are included in the patent protection scope of the present invention.
Claims (4)
1. An analytical equipment that impurity detected in was used for electron gas difluoromethane, its characterized in that: the device comprises a first gas carrying pipe, a second gas carrying pipe, a third gas carrying pipe, a fourth gas carrying pipe, a fifth gas carrying pipe, a sixth gas carrying pipe, a first switching valve, a second switching valve, a third switching valve, a fourth switching valve, a fifth switching valve, a first quantitative ring, a second quantitative ring, a third quantitative ring, a first chromatographic column, a second chromatographic column, a third chromatographic column, a fourth chromatographic column, a fifth chromatographic column, a sixth chromatographic column, a first needle valve, a second needle valve, a third needle valve, a fourth needle valve, a first helium ionization detector and a second helium ionization detector;
the first port of the first switching valve is an access end of a first gas carrying pipe, the second port of the first switching valve is connected with a first quantitative ring inlet, the third port of the first switching valve is a sample inlet, the fourth port of the first switching valve is connected with the third port of the second switching valve, the fifth port of the first switching valve is connected with a first quantitative ring outlet, the sixth port of the first switching valve is connected with a first chromatographic column outlet, the seventh port of the first switching valve is connected with a first needle valve, the eighth port of the first switching valve is an access end of a second gas carrying pipe, the ninth port of the first switching valve is connected with a second chromatographic column inlet, and the tenth port of the first switching valve is connected with a first chromatographic column inlet;
the first port of the second switching valve is an access end of a third gas carrying pipe, the second port of the second switching valve is connected with an inlet of a second quantitative ring, the fourth port of the second switching valve is connected with the sixth port of the third switching valve, the fifth port of the second switching valve is connected with an outlet of the second quantitative ring, the sixth port of the second switching valve is connected with an outlet of a third chromatographic column, the seventh port of the second switching valve is connected with a third needle valve, the eighth port of the second switching valve is an access end of a fourth gas carrying pipe, the ninth port of the second switching valve is connected with an inlet of the fourth chromatographic column, and the tenth port of the second switching valve is connected with an inlet of the third chromatographic column;
the first port of the third switching valve is connected with the inlet of the third quantitative ring, the second port of the third switching valve is the inlet end of the fifth gas carrying pipe, the third port of the third switching valve is connected with the inlet of the fifth chromatographic column, the fourth port of the third switching valve is connected with the outlet of the third quantitative ring, and the fifth port of the third switching valve is the sample outlet;
a first port of the fourth switching valve is connected with an outlet of the second chromatographic column, a second port of the fourth switching valve is connected with the second needle valve, a third port of the fourth switching valve is connected with a fourth port of the fourth switching valve, a fifth port of the fourth switching valve is connected with an outlet of the fourth chromatographic column, and a sixth port of the fourth switching valve is connected with the first helium ionization detector; a first port of the fifth switching valve is connected with an outlet of the fifth chromatographic column, a second port of the fifth switching valve is connected with a fourth needle valve, a third port of the fifth switching valve is connected with a fourth port of the fifth switching valve, and a sixth port of the fifth switching valve is connected with an inlet of the sixth chromatographic column; and the second helium ionization detector is connected with an outlet of the sixth chromatographic column.
2. The apparatus of claim 1, wherein the apparatus comprises: the first switching valve and the second switching valve are ten-way valves, and the third switching valve, the fourth switching valve and the fifth switching valve are six-way valves.
3. The apparatus of claim 1, wherein the apparatus comprises: the first chromatographic column is a TDX-01 stainless steel packed column with the outer diameter of 1/8 inches and the length of 0.6m, the second chromatographic column is a 5A molecular sieve stainless steel packed column with the outer diameter of 1/8 inches and the length of 2m, the third chromatographic column and the fourth chromatographic column are Porapak-Q stainless steel packed columns with the outer diameter of 1/8 inches and the length of 2m, and the fifth chromatographic column and the sixth chromatographic column are GasPro fused silica capillary columns with the inner diameter of 0.32mm and the length of 30 m.
4. The apparatus of claim 1, wherein the apparatus comprises: and helium is used as carrier gas in the first carrier gas pipe, the second carrier gas pipe, the third carrier gas pipe, the fourth carrier gas pipe, the fifth carrier gas pipe and the sixth carrier gas pipe.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202220751982.8U CN217180751U (en) | 2022-04-02 | 2022-04-02 | A analytical equipment that is arranged in electron gas difluoromethane impurity to detect |
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| CN202220751982.8U CN217180751U (en) | 2022-04-02 | 2022-04-02 | A analytical equipment that is arranged in electron gas difluoromethane impurity to detect |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115166103A (en) * | 2022-08-19 | 2022-10-11 | 大连大特气体有限公司 | System and method for analyzing impurities in diborane-containing feed gas |
| CN115236244A (en) * | 2022-09-01 | 2022-10-25 | 中船(邯郸)派瑞特种气体股份有限公司 | Gas chromatography detection system and method for analyzing impurities in molybdenum hexafluoride product |
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- 2022-04-02 CN CN202220751982.8U patent/CN217180751U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115166103A (en) * | 2022-08-19 | 2022-10-11 | 大连大特气体有限公司 | System and method for analyzing impurities in diborane-containing feed gas |
| CN115236244A (en) * | 2022-09-01 | 2022-10-25 | 中船(邯郸)派瑞特种气体股份有限公司 | Gas chromatography detection system and method for analyzing impurities in molybdenum hexafluoride product |
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