CN115032301A - Electron-level hydrogen chloride analysis device - Google Patents
Electron-level hydrogen chloride analysis device Download PDFInfo
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- CN115032301A CN115032301A CN202210659774.XA CN202210659774A CN115032301A CN 115032301 A CN115032301 A CN 115032301A CN 202210659774 A CN202210659774 A CN 202210659774A CN 115032301 A CN115032301 A CN 115032301A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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Abstract
The invention provides an electronic grade hydrogen chloride analysis device, which comprises: the separation device is used for separating substances in the carrier gas, the separation device is communicated with the detection device, and the detection device is used for analyzing the mole percentage of different substances in the carrier gas. Through setting up separator and detection device, can effectually detect out the content to impurity in the hydrogen chloride, and the precision is high, can very big avoid impurity gas to get into the problem that also can lead to final electronic components product quality to descend in the process.
Description
Technical Field
The invention relates to the technical field of gas chromatography analysis, in particular to an electronic grade hydrogen chloride analysis device.
Background
With the rapid development of the microelectronic industry towards large size, high integration, high uniformity and high integrity, there is also a new demand for electronic grade hydrogen chloride which is widely used in the gas phase polishing of single crystal silicon and the etching of epitaxial bases. Except that it should have a purity of 99.999% or more. It is also required that the lower the content of organic impurities such as THC, HO and metal ions of hydrogen chloride, the better. The electronic grade hydrogen chloride is mainly used for high-temperature gas phase etching of silicon and gallium arsenide before epitaxial growth to remove sodium ions. In addition, high-purity hydrogen chloride is also used for the surface chemical treatment of metal, the mixed gas for laser, the production of films and the surface treatment of carbon fibers.
At present, the purity of hydrogen chloride applied to the electronic industry is about 5N (99.999%), and even a very small amount of impurity gas enters a working procedure, the quality of a final electronic component product can be reduced, so that an electronic grade hydrogen chloride analysis device is needed for analyzing the impurities in the hydrogen chloride gas, and the problem that the very small amount of impurity gas in the hydrogen chloride gas enters a subsequent working procedure is solved.
Disclosure of Invention
The invention provides an electronic grade hydrogen chloride analysis device, which is used for solving the problems in the background technology.
In order to solve the technical problem, the invention discloses an electronic grade hydrogen chloride analysis device, which is characterized by comprising: the device comprises a separation device and a detection device, wherein carrier gas and sample gas are introduced into the separation device, the separation device is used for separating substances in the carrier gas, the separation device is communicated with the detection device, and the detection device is used for analyzing the mole percentages of different substances in the carrier gas.
Preferably, the detecting device is a DID detector, and the separating device includes: 4 diverter valves, 5 bellows valves, 2 quantitative rings, 4 chromatographic columns, 4 diverter valves include: 2 cross valves and 2 ten logical valves, 4 switching valves all have two states to be: CCW and CW, and the carrier gas is high purity helium.
Preferably, the carrier gas comprises: when the first four-way valve and the second four-way valve are in a CCW state and the first ten-way valve and the twenty-way valve are in a CW state, the first carrier gas is communicated with a No. 1 port of the first four-way valve through the first corrugated pipe valve, the No. 1 port of the first four-way valve is communicated with a No. 2 port of the first four-way valve, and the No. 2 port of the first four-way valve is communicated with the first vent port.
Preferably, the second path of carrier gas is communicated with the port 1 of the first ten-way valve through a second bellows valve, the port 1 of the first ten-way valve is communicated with the port 2 of the first ten-way valve, the port 2 of the first ten-way valve is communicated with a first analysis chromatographic column, the other end of the first analysis chromatographic column is communicated with the port 2 of the second four-way valve, the port 2 of the second four-way valve is communicated with the port 1 of the second four-way valve, and the port 1 of the second four-way valve is communicated with a DID detector;
the third path of carrier gas is communicated with a port 4 of the first ten-way valve through a third bellows valve, the port 4 of the first ten-way valve is communicated with a port 3 of the first ten-way valve, the port 3 of the first ten-way valve is communicated with the first pre-separation chromatographic column, the other end of the first pre-separation chromatographic column is communicated with a port 9 of the first ten-way valve, the port 9 of the first ten-way valve is communicated with a port 10 of the first ten-way valve, and the port 10 of the first ten-way valve is communicated with the second vent;
the fourth carrier gas channel is communicated with a port 1 of a twentieth through valve through a fourth corrugated pipe valve, the port 1 of the twentieth through valve is communicated with a port 2 of a second four-way valve, the port 2 of the twentieth through valve is communicated with a second analysis chromatographic column, the other end of the second analysis chromatographic column is communicated with a port 4 of the second four-way valve, the port 4 of the second four-way valve is communicated with a port 3 of the second four-way valve, and the port 3 of the second four-way valve is communicated with a fourth vent;
the fifth carrier gas channel is communicated with a port 4 of the twentieth valve through a fifth bellows valve, the port 4 of the twentieth valve is communicated with a port 3 of the twentieth valve, the port 3 of the twentieth valve is communicated with the second pre-separation chromatographic column, the other end of the second pre-separation chromatographic column is communicated with a port 9 of the twentieth valve, the port 9 of the twentieth valve is communicated with a port 10 of the twentieth valve, and the port 10 of the twentieth valve is communicated with the third vent.
Preferably, the sample gas is communicated with a port 3 of the first four-way valve, the port 3 of the first four-way valve is communicated with a port 4 of the first four-way valve, the port 4 of the first four-way valve is communicated with a port 7 of the first ten-way valve, the port 7 of the first ten-way valve is communicated with a port 8 of the first ten-way valve, the port 8 of the first ten-way valve is communicated with the first quantitative ring, the other end of the first quantitative ring is communicated with a port 5 of the first ten-way valve, the port 5 of the first ten-way valve is communicated with a port 6 of the first ten-way valve, the port 6 of the first ten-way valve is communicated with a port 6 of the twenty-way valve, the port 6 of the twenty-way valve is communicated with a port 5 of the twenty-way valve, the port 5 of the twenty-way valve is communicated with the second quantitative ring, the other end of the second quantitative ring is communicated with a port 8 of the twenty-way valve, and the port 8 of the twenty-way valve is communicated with a port 7 of the twenty-way valve, after which the sample gas is vented.
Preferably, the DID detector includes: the ionization chamber and the collecting chamber, the lower end of the ionization chamber is connected with a superfine pipeline in a through way, and the other end of the superfine pipeline is connected with the collecting chamber in a through way;
two bilaterally symmetrical discharge electrodes are fixedly arranged in the ionization cavity, and collectors are fixedly arranged in the collector cavities;
the separation device is in through connection with a first pipeline, the other end of the first pipeline is communicated with a second pipeline through a VCR connector, and the second pipeline is communicated with the ionization cavity of the DID detector.
Preferably, the VCR joint comprises: the leakage testing device comprises an internal thread sleeve and an external thread sleeve, wherein the internal thread sleeve is in threaded connection with the external thread sleeve, a leakage testing hole is formed in the internal thread sleeve, a first pipeline penetrates through the external thread sleeve and is attached to the inner wall of the external thread sleeve, a gasket is fixedly connected to the left side of the first pipeline, the right end of the gasket is attached to the left end of the external thread sleeve, the gasket is arranged in the internal thread sleeve and is attached to the inner wall of the internal thread sleeve;
the second pipeline right side extends into the internal thread sleeve, just the second pipeline right side is fixed and is equipped with the stopper, stopper and the laminating of internal thread sleeve left side wall, just the stopper right side contacts the cooperation with the packing ring.
Preferably, still be equipped with locking device on the internal thread sleeve, locking device includes: the left side of the installation box is detachably connected with the internal thread sleeve, and the clamping mechanism is clamped on the external thread sleeve;
the installation box is internally provided with: the upper end of the driving motor is fixedly arranged on the inner wall of the upper side of the installation box, the lower end of the driving motor is fixedly connected with a first rotating rod through an output shaft, and a first gear is fixedly arranged at the lower end of the first rotating rod;
the left end and the right end of the first mounting plate are fixedly connected with the inner walls of the left side and the right side of the mounting box respectively, and the first mounting plate is provided with a jog button which is electrically connected with a driving motor;
a first moving rod is fixedly arranged on the lower surface of the first gear, a first extension rod is fixedly arranged at the lower end of the first moving rod, and the first extension rod is positioned on the front side of the inching button;
preferably, the clamping mechanism includes: the centre gripping case, centre gripping case centre gripping is in external screw thread sleeve week side, just be equipped with a plurality of spouts on the centre gripping case, the centre gripping incasement is equipped with: the periphery of the rotating plate is in contact fit with the inner wall of the clamping box, a hexagonal groove is formed in the rotating plate, a pushing block is further fixedly arranged on the rotating plate, and a first opening is formed in the clamping box;
the clamping blocks are arranged in the clamping box, a sliding block is fixedly arranged on one side, close to the rotating plate, of each clamping block, the sliding block is arranged in the groove in a sliding mode, a first sliding rod is fixedly connected to one end, far away from the sliding block, of each clamping block, and the first sliding rod extends into the sliding groove;
a limiting box is fixedly arranged at the first opening, a second opening is arranged on the limiting box, the pushing block passes through the first opening and the second opening to extend out of the clamping box, a plurality of limiting grooves are formed in the inner walls of the upper side and the lower side of the limiting box, clamping springs are symmetrically arranged in the limiting box and clamped on the pushing block, a limiting block is fixedly arranged at one end, far away from the pushing block, of each clamping spring, and the limiting blocks are in contact fit with the limiting grooves;
one end of the clamping box, which is far away from the pushing block, is fixedly connected with a first arc-shaped rack, a third opening is formed in the left wall of the installation box, and the right end of the first arc-shaped rack penetrates through the third opening to be meshed with the first gear.
Preferably, a safety device is further fixedly arranged on the housing of the DID detector, and the safety device includes: the upper ends of the safety boxes are fixedly arranged on a shell of the DID detector, and a first connecting block is fixedly arranged at one end, far away from the first pipeline, of each safety box;
the upper ends of the buffer springs are fixedly connected with a shell of the DID detector;
the second connecting block is arranged in a triangular shape, one corner of the second connecting block is fixedly connected with the lower end of the buffer spring, one corner of the second connecting block, which is close to the first pipeline, is hinged with the first connecting block, and one corner of the second connecting block, which is far away from the first pipeline, is hinged with the buffer rod;
the left end and the right end of the fixing piece are respectively hinged with a first fastening ring and a second fastening ring, one end, far away from the fixing piece, of the first fastening ring is hinged with a fifth connecting rod, one end, far away from the first fastening ring, of the fifth connecting rod is fixedly connected with a pressing rod, one end, far away from the fixing piece, of the second fastening ring is hinged with a sixth connecting rod, one end, far away from the second fastening ring, of the sixth connecting rod is hinged with one end, far away from the first fastening ring, of the fifth connecting rod, and a ring formed by the fixing piece, the first fastening ring and the second fastening ring is sleeved on the outer wall of the first pipeline;
second fixing blocks are symmetrically arranged on the left side of the first fastening ring and the right side of the second fastening ring, and the second fixing blocks are hinged to one end, far away from the second connecting block, of the buffer rod;
the safety box is equipped with ratchet subassembly around the symmetry in the safety box, ratchet subassembly includes: the ratchet wheel is rotationally connected to the inner wall of the safety box, and a plurality of teeth of the ratchet wheel are provided with stop rods;
the safety box comprises an arc-shaped mounting plate, wherein the arc-shaped mounting plate is fixedly arranged on the inner wall of the lower side of the safety box, a hinge head is fixedly arranged on the arc-shaped mounting plate, a stopping plate is hinged to the hinge head, a third sliding groove is formed in the stopping plate, and the right end of the stopping plate is in contact fit with a ratchet wheel;
an arc stopping block is arranged on the upper surface of the arc mounting plate in a sliding mode, a second sliding rod is arranged on the arc stopping block and is arranged in a third sliding groove in a sliding mode, one end, far away from the first pipeline, of the arc stopping block is in contact fit with the stopping rod, a limiting plate is fixedly arranged at the upper end of the arc mounting plate, and one end, close to the first pipeline, of the arc stopping block is in contact fit with the limiting plate;
the ratchet is provided with two, two fixed connection reel between the ratchet, just around being equipped with the rope on the reel, the rope is kept away from reel one end run through the safety box outer wall and with first pipeline outer wall fixed connection keep away from the one end fixed connection damping spring's of first pipeline one end on the rope, damping spring's other end fixed connection buffer beam.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic diagram of the gas circuit of the present invention;
FIG. 2 is a schematic diagram of a DID detector according to the present invention;
FIG. 3 is a schematic view of the structure of a VCR adapter of the present invention;
FIG. 4 is a schematic structural view of the anti-loosening device of the present invention;
FIG. 5 is a schematic view of the clamping mechanism of the present invention;
FIG. 6 is a schematic view of a rotating plate according to the present invention;
FIG. 7 is a schematic view of a clamping block according to the present invention;
FIG. 8 is a schematic view of the structure of the spacing box of the present invention;
FIG. 9 is a top view of FIG. 5 of the present invention;
FIG. 10 is a schematic view of the safety device of the present invention;
FIG. 11 is a schematic view of the connection of a first fastening ring and a second fastening ring of the present invention;
FIG. 12 is an enlarged view taken at A of FIG. 10 in accordance with the present invention;
FIG. 13 is a schematic view of the ratchet assembly of the present invention.
In the figure: 1. a first four-way valve; 2. a first ten-way valve; 3. a twentieth valve; 4. a second four-way valve; 5. a first bellows valve; 6. a second bellows valve; 7. a third bellows valve; 8. a fourth bellows valve; 9. a fifth bellows valve; 10. a first pre-separation chromatography column; 11. a second pre-separation chromatography column; 12. a first analytical chromatographic column; 13. a second analytical chromatographic column; 14. a first quantitative ring; 15. a second dosing ring; 16. a DID detector; 17. a collector; 18. a superfine pipeline; 19. a discharge electrode; 20. an ionization chamber; 21. a current collection chamber; 22. a gasket; 23. a first pipeline; 24. an externally threaded sleeve; 25. a leak test hole; 26. a second pipeline; 27. an internally threaded sleeve; 28. a locking device; 29. installing a box; 30. a first gear; 31. a first moving bar; 32. a first mounting plate; 33. a drive motor; 34. a first arc-shaped rack; 35. a clamping mechanism; 36. a clamping box; 37. a clamping block; 38. a limiting box; 39. a pushing block; 40. a chute; 41. a first slide bar; 42. a rotating plate; 43. a groove; 44. a slider; 45. a clamp spring; 46. a limiting block; 47. a limiting groove; 48. clicking a button; 49. a first rotating lever; 50. a safety box; 51. a buffer spring; 52. a first connection block; 53. a damping spring; 54. a connecting rod; 55. a second fixed block; 56. a buffer rod; 57. a rope; 58. a second connecting block; 59. a safety device; 60. a ratchet assembly; 61. a limiting plate; 62. a third sliding groove; 63. an arc-shaped stop block; 64. a second slide bar; 65. a hinge joint; 66. a stop plate; 67. an arc-shaped mounting plate; 68. a stop lever; 70. a ratchet wheel; 71. a reel; 72. a fixing sheet; 73. a first fastening ring; 74. a second fastening ring; 75. a sixth link; 76. a fifth link; 77. the lever is pressed.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
In addition, the descriptions related to "first", "second", etc. in the present invention are used for descriptive purposes only, do not specifically refer to an order or sequence, and do not limit the present invention, but merely distinguish components or operations described in the same technical terms, and are not to be construed as indicating or implying any relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, technical solutions and technical features between various embodiments can be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent and not be within the protection scope of the present invention.
Example 1
An embodiment of the present invention provides an electronic-grade hydrogen chloride analysis apparatus, as shown in fig. 1, including: the device comprises a separation device and a detection device, wherein carrier gas and sample gas are introduced into the separation device, the separation device is used for separating substances in the carrier gas, the separation device is communicated with the detection device, and the detection device is used for analyzing the mole percentages of different substances in the carrier gas.
The working principle and the beneficial effects of the technical scheme are as follows: firstly, introducing sample gas and carrier gas into a separation device, purging the separation device for a period of time and collecting a sample to be detected, separating a plurality of impurities through a partial structure in the separation device, and detecting components of the impurities through a detection device; through setting up separator and detection device, can effectually detect out the content to impurity in the hydrogen chloride, and the precision is high, can very big avoid impurity gas to get into the problem that also can lead to final electronic components product quality to descend in the process.
Example 2
On the basis of the above embodiment 1, as shown in fig. 1, the detecting device is a DID detector 16, and the separating device includes: 4 diverter valves, 5 bellows valves, 2 quantitative rings, 4 chromatographic columns, 4 diverter valves include: 2 cross valves and 2 ten logical valves, 4 all have two states to be by the diverter valve: CCW and CW, and the carrier gas is high purity helium.
Wherein, preferably, the carrier gas comprises: when the first four-way valve 1 and the second four-way valve 4 are in a CCW state and the first ten-way valve 2 and the twentieth-way valve 3 are in a CW state, the first carrier gas is communicated with a port 1 of the first four-way valve 1 through a first bellows valve 5, the port 1 of the first four-way valve 1 is communicated with a port 2 of the first four-way valve 1, and the port 2 of the first four-way valve 1 is communicated with a first vent hole.
Preferably, the second path of carrier gas is communicated with the port 1 of the first ten-way valve 2 through the second bellows valve 6, the port 1 of the first ten-way valve 2 is communicated with the port 2 of the first ten-way valve 2, the port 2 of the first ten-way valve 2 is communicated with the first analytical chromatographic column 12, the other end of the first analytical chromatographic column 12 is communicated with the port 2 of the second four-way valve 4, the port 2 of the second four-way valve 4 is communicated with the port 1 of the second four-way valve 4, and the port 1 of the second four-way valve 4 is communicated with the DID detector 16;
the third path of carrier gas is communicated with a port 4 of the first ten-way valve 2 through a third bellows valve 7, the port 4 of the first ten-way valve 2 is communicated with a port 3 of the first ten-way valve 2, the port 3 of the first ten-way valve 2 is communicated with a first pre-separation chromatographic column 10, the other end of the first pre-separation chromatographic column 10 is communicated with a port 9 of the first ten-way valve 2, the port 9 of the first ten-way valve 2 is communicated with a port 10 of the first ten-way valve 2, and the port 10 of the first ten-way valve 2 is communicated with a second vent;
the fourth carrier gas is communicated with the port 1 of the twentieth through valve 3 through a fourth bellows valve 8, the port 1 of the twentieth through valve 3 is communicated with the port 2 of the second four-way valve 3, the port 2 of the twentieth through valve 3 is communicated with a second analysis chromatographic column 13, the other end of the second analysis chromatographic column 13 is communicated with the port 4 of the second four-way valve 4, the port 4 of the second four-way valve 4 is communicated with the port 3 of the second four-way valve 4, and the port 3 of the second four-way valve 4 is communicated with a fourth vent;
the fifth carrier gas is communicated with the port 4 of the twentieth valve 3 through a fifth bellows valve 9, the port 4 of the twentieth valve 3 is communicated with the port 3 of the twentieth valve 3, the port 3 of the twentieth valve 3 is communicated with a second pre-separation chromatographic column 11, the other end of the second pre-separation chromatographic column 11 is communicated with the port 9 of the twentieth valve 3, the port 9 of the twentieth valve 3 is communicated with the port 10 of the twentieth valve 3, and the port 10 of the twentieth valve 3 is communicated with a third vent.
Preferably, the sample gas is communicated with a port 3 of the first four-way valve 1, the port 3 of the first four-way valve 1 is communicated with a port 4 of the first four-way valve 1, the port 4 of the first four-way valve 1 is communicated with a port 7 of the first ten-way valve 2, the port 7 of the first ten-way valve 2 is communicated with a port 8 of the first ten-way valve 2, the port 8 of the first ten-way valve 2 is communicated with the first quantitative ring 14, the other end of the first quantitative ring 14 is communicated with a port 5 of the first ten-way valve 2, the port 5 of the first ten-way valve 2 is communicated with a port 6 of the first ten-way valve 2, the port 6 of the first ten-way valve 2 is communicated with a port 6 of the twenty-way valve 3, the port 6 of the twenty-way valve 3 is communicated with a port 5 of the twenty-way valve 3, the port 5 of the twenty-way valve 3 is communicated with the second quantitative ring 15, and the other end of the second quantitative ring 15 is communicated with a port 8 of the twenty-way valve 3, and the No. 8 port of the twentieth valve 3 is communicated with the No. 7 port of the twentieth valve 3, and then the sample gas is discharged.
Wherein, the CW state of the valve is positive air intake, and the CCW state is reverse air intake.
The pipeline design avoids acute-angle bending as much as possible, and vortex and residue are not easy to form on the pipeline. The material of the pipeline adopts EP grade 316L stainless steel, and the pipeline is not easy to absorb hydrogen chloride and does not react with the hydrogen chloride after electrochemical polishing and passivation treatment. The pipelines and valves through which hydrogen chloride gas flows in large quantity are made of Hastelloy materials, so that the corrosion resistance of the related pipelines is further ensured.
The gas circuit design strictly controls the flow of each carrier gas, the back flushing flow is also controlled, and the balance of the gas circuit is guaranteed.
The DID detector adopts a platinum electrode, is corrosion-resistant, adopts a double-cavity design in an internal cavity structure, and reduces the interference of hydrogen chloride on the discharge electrode because a discharge chamber and an ionization chamber are separated.
Wherein, four chromatographic columns are respectively:
first pre-separation chromatography column 10: 4' x1/8 "silica gel;
first analytical chromatography column 12: 6' X1/8 "13X;
second pre-separation column 11: 10' x1/8 "hayesep R (Nickle);
a second analytical column 13: 15' x1/8 "hayesep Q (Nickle).
The working principle of the technical scheme is as follows:
1. opening the first ten-way valve 2 to realize the collection of the measured sample in the first quantitative ring 14; opening the twentieth valve 3 to realize the collection of the tested sample in the second quantitative ring 15;
2. the first ten-way valve 2 and the second four-way valve 4 are closed, and the sample collected by the first quantitative ring 20 is blown into the first pre-separation chromatographic column 10 by the carrier gas of the third bellows valve 7;
3. after being pre-separated by a first pre-separation chromatographic column 10, pre-separated components such as H2, O2+ Ar + CO, N2, CH4 and the like enter a first analysis chromatographic column 12; opening the first ten-way valve 2, and blowing back and emptying other components;
4. h2, O2+ Ar, N2, CH4, CO separated by the first analytical chromatographic column 12
The components are equal, and the detection of the detected components is realized from the second four-way valve 4 to the DID detector 16;
5. the twentieth valve 3 is closed, the first four-way valve 1 is opened, and the carrier gas at the outlet of the fifth pressure balance regulating valve 9 blows the sample collected in the second quantitative ring 15 into the second pre-separation chromatographic column 11;
6. after pre-separation by a second pre-separation chromatographic column 11, pre-separated components such as CO2 enter the second analysis chromatographic column, a twentieth valve is opened, and other components are blown back and emptied;
7. and (3) opening the second four-way valve 4, and detecting the detected component by the CO2 component separated by the second analytical chromatographic column 13 from the second four-way valve 4 to the detector 22.
The beneficial effects of the above technical scheme are: through setting up 4 diverter valves, 5 bellows valves, 2 quantitative rings, 4 chromatographic columns and DID detector, the content of impurity in can effectual separation and the analysis HCL, the precision is high, can effectively avoid impurity to electrical components product quality's influence, has improved the convenience of device.
Wherein, 1, the chromatographic column has good separation effect, which not only ensures the effective separation of the impurity components (H2, O2+ Ar, N2, CH4, CO2) and the main component (hydrogen chloride), but also ensures that the hydrogen chloride does not remain in the pre-separation column for too long time and can be quickly and cleanly blown back.
2. The first pre-separation chromatographic column 10 is matched with a first analysis chromatographic column 12, and the second analysis chromatographic column 11 is matched with a second analysis chromatographic column 13, the pre-separation chromatographic columns 10 and 11 completely separate six components (H2, O2+ Ar, N2, CH4, CO2) from main component hydrogen chloride, and the separation chromatographic columns 12 and 13 completely separate the six components (H2, O2+ Ar, N2, CH4, CO2) again and mutually.
And the hydrogen chloride in the first pre-separation chromatographic column and the hydrogen chloride in the second analysis chromatographic column 11 are respectively prevented from entering a separation column and a detector at the rear end by the third carrier gas and the fifth carrier gas through the second vent and the third vent by switching to the CW state through the first ten-way valve 2 and the twenty-way valve 3.
3. And the good gas path design ensures that the hydrogen chloride is not left in the pipeline.
Setting instrument parameters:
the set temperature of the column box is 60 ℃, the set temperature of the detector is 23 ℃, the discharge voltage is 525V DC, and the polarization voltage is 160V DC.
The pressure of carrier gas (high-purity helium) is 6bar, the pressure of driving gas (high-purity helium) is 3bar, and the pressure of sample gas (helium standard gas or high-purity hydrogen chloride gas) is 2 bar.
The flow rates of the first path of carrier gas, the second path of carrier gas, the third path of carrier gas, the fourth path of carrier gas and the fifth path of carrier gas are all 30ml/min, the flow rate of the discharge gas Detector He is 30ml/min, and the flow rate of the valve box Purge gas is as follows: 2 ml/min.
The first ten-way valve 2 and the twenty-way valve 3 are sampling/back-flushing valves, and when the first ten-way valve 2 and the twentieth-way valve 3 are in a CW state, the back-flushing flow is also controlled at 30ml/min by adjusting external damping valves Restrictor1 and Restrictor2 (not marked in a gas path diagram) at the second vent and the third vent, so that the balance of carrier gas flow during valve switching is ensured.
The gas at each inlet of the first carrier gas and the fifth carrier gas is helium and cannot be changed.
The Detector He is not shown on the gas path diagram, and is not shown, but is shown on the Detector structure diagram.
Example 3
On the basis of the above-described embodiments 1-2, as shown in fig. 2, the DID detector 16 includes: the ionization chamber 20 and the collecting chamber 21, the lower end of the ionization chamber 20 is connected with one superfine pipeline 18 in a penetrating way, and the other end of the superfine pipeline 18 is connected with the collecting chamber 21 in a penetrating way;
two bilaterally symmetrical discharge electrodes 19 are fixedly arranged in the ionization cavity 20, and a collector 17 is fixedly arranged in the collector cavity 21;
the separating device is connected with a first pipeline 23 in a penetrating way, the other end of the first pipeline 23 is communicated with a second pipeline 26 through a VCR joint, and the second pipeline 26 is communicated with the DID detector 16.
The working principle of the technical scheme is as follows: when purified ultra-pure helium gas is applied to two discharge electrodes 19 in the ionization chamber 20 with appropriate high voltage, discharge is generated between the two electrodes, thereby obtaining a beam of high-energy ultraviolet radiation (400-. The ultra-high energy ultraviolet light is introduced into a collector 17 in a collecting cavity 21 through an ultra-fine pipeline 18, in the process, high-energy photons directly irradiate impurity molecules to be detected in sample components, all components in the sample gas brought by ultra-high purity carrier gas are ionized, meanwhile, the high-energy photons firstly excite helium ions in the carrier gas to a metastable state (He), and then the He with higher energy generates inelastic collision with the impurity molecules in the sample and ionizes the He. At this time, proper voltage is applied to the collector to collect ionized impurity molecules, and the signal is amplified and recorded to obtain the spectrum peak of the component to be measured.
The beneficial effects of the above technical scheme are: through setting up the DID detector, impurity molecule in can effectual detection sample composition can obtain the spectral peak of surveyed composition simultaneously, and the precision is higher, and effectual completion detects the task, very big improvement the validity and the functionality of device, improved the availability factor.
Example 4
On the basis of the above embodiments 1 to 3, as shown in fig. 3, the VCR joint comprises: the leakage testing device comprises an internal thread sleeve 27 and an external thread sleeve 24, wherein the internal thread sleeve 27 is in threaded connection with the external thread sleeve 24, a leakage testing hole 25 is formed in the internal thread sleeve 27, the first pipeline 23 penetrates through the external thread sleeve 24, the first pipeline 23 is attached to the inner wall of the external thread sleeve 24, the left side of the first pipeline 23 is fixedly connected with a gasket 22, the right end of the gasket 22 is attached to the left end of the external thread sleeve 24, the gasket 22 is arranged in the internal thread sleeve 27, and the gasket 22 is attached to the inner wall of the internal thread sleeve 27;
the right side of the second pipeline 26 extends into the inner thread sleeve 27, a limiting block is fixedly arranged on the right side of the second pipeline 26, the limiting block is attached to the left side wall of the inner thread sleeve 27, and the right side of the limiting block is in contact fit with the gasket 22.
The working principle of the technical scheme is as follows: the second conduit 26 is first placed into the internally threaded sleeve 27, then the gasket 22 and the first conduit 23 are placed, and then the externally threaded sleeve 24 is threadedly connected to the internally threaded sleeve 27.
The beneficial effects of the above technical scheme are: use threaded connection, the steadiness that can effectual increase connection, inside simultaneously is equipped with packing ring 22, can the effectual connection leakproofness that improves the device, has improved the result of use of device, has increased life.
Example 5
On the basis of the above embodiments 1 to 4, as shown in fig. 4 to 9, the internally threaded sleeve 27 is further provided with a locking device 28, and the locking device 28 includes: the mounting box 29 and the clamping mechanism 35, the left side of the mounting box 29 is detachably connected with the internal thread sleeve 27, and the clamping mechanism 35 is clamped on the external thread sleeve 24;
the installation box 29 is internally provided with: the upper end of the driving motor 33 is fixedly arranged on the inner wall of the upper side of the installation box 29, the lower end of the driving motor 33 is fixedly connected with a first rotating rod 49 through an output shaft, and a first gear 30 is fixedly arranged at the lower end of the first rotating rod 49;
the left end and the right end of the first mounting plate 32 are fixedly connected with the inner walls of the left side and the right side of the mounting box 29 respectively, the inching button 48 is arranged on the first mounting plate 32, and the inching button 48 is electrically connected with the driving motor 33;
the lower surface of the first gear 30 is fixedly provided with a first moving rod 31, the lower end of the first moving rod 31 is fixedly provided with a first extending rod, and the first extending rod is positioned on the front side of the inching button 48.
The working principle of the technical scheme is as follows: the clamping mechanism 35 is clamped on the first pipeline 23, when the first gear 30 rotates under the action of external force, the first gear 30 drives the first extending rod on the first moving rod 31 to press the inching button 45, so that the driving motor 33 is started, the first gear 30 is driven to rotate reversely, the clamping mechanism 35 is clamped, and when the first extending rod on the first moving rod 31 leaves the inching button 48, the driving motor 33 is powered off.
The beneficial effects of the above technical scheme are: through setting up inching button 48, can make when the button is pressed, driving motor 33 starts, when loosening the button, driving motor 33 closes, when the circumstances such as take place the pine of external screw thread sleeve 24, driving motor 33 can start under the effect of inching button 48, and after external screw thread sleeve 24 fastens, driving motor 33 can stop, the effectual functionality and the security that has improved the device.
Example 6
On the basis of the above embodiments 1 to 5, as shown in fig. 4 to 9, the clamping mechanism 35 includes: centre gripping case 36, centre gripping case 36 centre gripping is in outer screw sleeve 24 week side, just be equipped with a plurality of spouts 40 on the centre gripping case 36, be equipped with in the centre gripping case 36: the periphery of the rotating plate 42 is in contact fit with the inner wall of the clamping box 36, a hexagonal groove 43 is formed in the rotating plate 42, a pushing block 39 is further fixedly arranged on the rotating plate 42, and a first opening is formed in the clamping box 36;
the clamping blocks 37 are arranged in the clamping box 36, a sliding block 44 is fixedly arranged on one side, close to the rotating plate 42, of each clamping block 37, the sliding block 44 is arranged in the groove 43 in a sliding mode, a first sliding rod 41 is fixedly connected to one end, far away from the sliding block 44, of each clamping block 37, and the first sliding rod 41 extends into the sliding groove 40;
a limiting box 38 is fixedly arranged at the first opening, a second opening is arranged on the limiting box 38, the pushing block 39 passes through the first opening and the second opening to extend out of the clamping box 36, a plurality of limiting grooves 47 are arranged on the inner walls of the upper side and the lower side of the limiting box 38, clamping springs 45 are symmetrically arranged in the limiting box 38, the clamping springs 45 are clamped on the pushing block 39, a limiting block 46 is fixedly arranged at one end, far away from the pushing block 39, of each clamping spring 45, and the limiting blocks 46 are in contact fit with the limiting grooves 47;
one end of the clamping box 36 far away from the pushing block 39 is fixedly connected with a first arc-shaped rack 34, the left wall of the installation box 29 is provided with a third opening, and the right end of the first arc-shaped rack 34 penetrates through the third opening to be meshed and connected with the first gear 30.
The working principle of the technical scheme is as follows: clamping mechanism 35 presss from both sides on external screw thread sleeve 24, promote and promote piece 39, make rotor plate 42 rotatory, slider 44 on driving a plurality of grip blocks 37 slides in recess 43, first slide bar 41 slides in spout 40, and when grip blocks 37 press from both sides tight back to external screw thread sleeve 24, it does not remove in spacing case 38 to promote piece 39, press from both sides spring 45 and drive stopper 46 card in a plurality of spacing grooves 47, it is spacing to promote piece 39, grip blocks 37 press from both sides tight external screw thread sleeve 24, when external screw thread sleeve 24 pine takes off, it is rotatory that grip case 36 rotates and drives first arc rack 34, it is rotatory to drive first gear 30.
The beneficial effects of the above technical scheme are: through setting up double-layered spring 45 and stopper 46, can effectual restriction promote the removal of piece 39 for grip block 37 presss from both sides tight external screw thread sleeve 24, sets up recess 43 and spout 40 and can effectually make the removal of grip block 37 in centre gripping case 36 more convenient, the effectual functionality that improves the device.
Example 7
On the basis of the above embodiments 1 to 6, as shown in fig. 10 to 13, a safety device 59 is further fixed on the housing of the DID detector 16, and the safety device 59 includes: the DID detector comprises two bilaterally symmetrical safety boxes 50, wherein the upper ends of the safety boxes 50 are fixedly provided with shells of the DID detector 16, and one end of each safety box 50, which is far away from the first pipeline 23, is fixedly provided with a first connecting block 52;
the upper ends of the buffer springs 51 are fixedly connected with the shell of the DID detector 16;
a second connecting block 58, wherein the second connecting block 58 is triangular, one corner of the second connecting block 58 is fixedly connected with the lower end of the buffer spring 51, one corner of the second connecting block 58 close to the first pipeline 23 is hinged with the first connecting block 52, and one corner of the second connecting block 58 far away from the first pipeline 23 is hinged with the buffer rod 56;
the left end and the right end of the fixing plate 72 are respectively hinged with a first fastening ring 73 and a second fastening ring 74, one end of the first fastening ring 73, which is far away from the fixing plate 72, is hinged with a fifth connecting rod 76, one end of the fifth connecting rod 76, which is far away from the first fastening ring 73, is fixedly connected with a pressing rod 77, one end of the second fastening ring 74, which is far away from the fixing plate 72, is hinged with a sixth connecting rod 75, one end of the sixth connecting rod 75, which is far away from the second fastening ring 74, is hinged with one end, which is far away from the first fastening ring 73, of the fifth connecting rod 76, and circular rings formed by the fixing plate 72, the first fastening ring 73 and the second fastening ring 74 are sleeved on the outer wall of the first pipeline 23;
a second fixing block 55 is symmetrically arranged on the left side of the first fastening ring 73 and the right side of the second fastening ring 74, and the second fixing block 55 is hinged with one end, far away from the second connecting block 58, of the buffer rod 56;
ratchet assemblies 60 are symmetrically arranged in the safety box 50 from front to back, and each ratchet assembly 60 comprises: the ratchet wheel 70 is rotationally connected to the inner wall of the safety box 50, and stop rods 68 are arranged on a plurality of teeth of the ratchet wheel 70;
the arc-shaped mounting plate 67 is fixedly arranged on the inner wall of the lower side of the safety box 50, a hinge joint 65 is fixedly arranged on the arc-shaped mounting plate 67, a stopping plate 66 is hinged to the hinge joint 65, a third sliding groove 62 is formed in the stopping plate 66, and the right end of the stopping plate 66 is in contact fit with the ratchet wheel 70;
an arc-shaped stopping block 63 is arranged on the upper surface of the arc-shaped mounting plate 67 in a sliding manner, a second sliding rod 64 is arranged on the arc-shaped stopping block 63, the second sliding rod 64 is arranged in a third sliding groove 62 in a sliding manner, one end, far away from the first pipeline 23, of the arc-shaped stopping block 63 is in contact fit with the stopping rod 68, a limiting plate 61 is fixedly arranged at the upper end of the arc-shaped mounting plate 67, and one end, close to the first pipeline 23, of the arc-shaped stopping block 63 is in contact fit with the limiting plate 61;
ratchet 70 is provided with two fixed connection reel 71 between the two ratchet 70, just the reel 71 is gone up around being equipped with rope 57, rope 57 is kept away from reel 71 one end runs through safety box 50 outer wall and with first pipeline 23 outer wall fixed connection one end fixed connection damping spring 53's one end that keeps away from first pipeline 23 on the rope 57, damping spring 53's other end fixed connection buffer beam 56.
The working principle of the technical scheme is as follows: the fixing plate 72, the first fastening ring 73 and the second fastening ring 74 are attached to the first pipeline 23, the pressing rod 77 is pressed, the fifth connecting rod 76 and the sixth connecting rod 75 move, so that the first fastening ring 73 and the second fastening ring 74 are fastened with the first pipeline 23, when the first pipeline 23 passes through gas with larger pressure inside and swings or moves, the second fixing blocks 55 on the first fastening ring 73 and the second fastening ring 74 drive the buffer rods 56 to move, the second connecting block 58 is driven to rotate on the first connecting block 52, and the buffer springs 51 are compressed or extended continuously;
one end of the rope 57 is fixed on the first pipeline 23, the other end of the rope is wound on the winding drum 71, when one end of the first pipeline 23 is separated from the VCR connector, the rope 57 can drive the winding drum 71 to rotate, the ratchet 70 is driven to rotate, the stop rod 68 on the ratchet 70 can be thrown outwards under the action of centrifugal force, the stop rod 68 drives the arc-shaped stop block 63 to slide on the arc-shaped mounting plate 67, the second sliding rod 64 is driven to move in the third sliding groove 62, the stop plate 66 is driven to move, and the ratchet 70 is clamped.
The beneficial effects of the above technical scheme are: by arranging the buffer spring 51, the stress of the first pipeline 23 during swinging can be effectively relieved, the buffer and shock absorption effects are achieved, and by arranging the second connecting block 58 to be triangular, the stability of the device can be improved, the possibility of breakage of the first pipeline 23 is effectively reduced, and the service life of the first pipeline 23 is prolonged;
through setting up ratchet assembly 60, the effectual security that has improved first pipeline 23 when the fracture, and through setting up stop lever 68, arc stop block 63 and stop plate 66, can effectively restrict the removal of first pipeline 23, avoided first pipeline 23 to connect the separation with the VCR, and set up damping spring 53, also can effectually play the effect of buffering to first pipeline 23, improved the security of device.
Example 8
On the basis of any one of the above embodiments 1 to 7, the electronic-grade hydrogen chloride analysis apparatus further includes:
a pressure sensor: mounted within the internally threaded sleeve 27 for sensing the gas pressure at the VCR joint;
a volume flow meter: is arranged in the first pipeline 23 and is used for detecting the volume flow in the first pipeline 23;
a timer: the device is arranged at the joint of the VCR and is used for detecting the total time of gas passing;
controller, alarm install respectively in VCR joint department, the controller with pressure sensor, volumetric flowmeter, time-recorder and alarm electricity are connected, the controller is based on pressure sensor, volumetric flowmeter, time-recorder control the alarm work, including following step:
step 1: the controller obtains the gas permeability index of the VCR joint based on the pressure sensor, the volume flow meter, the timer and the formula (1):
wherein K is the gas permeability index of the VCR joint; q is a detection value of the mass flowmeter; λ is the kinetic viscosity of the gas in the first conduit 23; l is the length of the first conduit 23; s is the cross-sectional area within the internally threaded sleeve 27; p 1 Is the pressure at the inlet of the separation device; p 2 Is the detection value of the pressure sensor; e is a natural constant(ii) a T is a timer detection value; t is a unit time;
step 2: and (3) comparing the gas permeability index of the VCR connector calculated by the formula (1) with a preset gas permeability index, and controlling an alarm to give an alarm by the controller when the gas permeability index of the VCR connector calculated by the formula (1) is greater than the preset gas permeability index.
In the formula
When the pressure difference is increased, the gas permeability index of the VCR joint is increased, which easily causes gas leakage in the pipeline, and at this time, acute-angled bending of the pipeline is avoided as much as possible during connection, and when the volume flow in the first pipeline 23 is gradually increased, the gas permeability index is also increased, which easily causes gas leakage, so that a proper gas pressure and gas flow rate are selected;
assume that the volume flow Q in the first line 23 is 30cm 3 Min; the kinetic viscosity λ of the gas in the first line 23 is 22.624pa · s; the length L of the first line 23 is 0.5 m; the cross-sectional area S in the internally threaded sleeve 27 is 3cm 2 (ii) a Pressure P at the inlet of the separating device 1 0.6 Mpa; gas pressure P at VCR connection 2 0.59 Mpa; e is a natural constant; the total time T of gas passing is 3 h; the unit time t is 1 h; the gas permeability index K of the VCR joint can be calculated as 0.67, if the preset gas permeability index is 1, then the alarm will not give an alarm.
The working principle and the beneficial effects of the calculation scheme are as follows: utilize formula (1) to calculate the gas permeability index that VCR connects earlier, the controller with formula (1) calculate the gas permeability index that VCR connects and predetermine the gas permeability index and contrast, when the gas permeability index that VCR that formula (1) calculated connects is greater than when predetermineeing gas permeability index 1, controller control alarm reports to the police, and suggestion personnel VCR joint department takes place unusually, in time inspects the connection condition that VCR connects, realizes unusually reporting to the police and reminds personnel to check the problem through setting up the alarm, can effectual improvement security.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. It is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.
Claims (10)
1. An electronic grade hydrogen chloride analysis device, comprising: the device comprises a separation device and a detection device, wherein carrier gas and sample gas are introduced into the separation device, the separation device is used for separating substances in the carrier gas, the separation device is communicated with the detection device, and the detection device is used for analyzing the mole percentages of different substances in the carrier gas.
2. An electronic grade hydrogen chloride analysis device according to claim 1, wherein the detection device is a DID detector (16), and the separation device comprises: 4 diverter valves, 5 bellows valves, 2 quantitative rings, 4 chromatographic columns, 4 diverter valves include: 2 cross valves and 2 ten logical valves, 4 all have two states to be by the diverter valve: CCW and CW, and the carrier gas is high purity helium.
3. An electronic grade hydrogen chloride analysis apparatus according to claim 2, wherein the carrier gas comprises: the first way of carrier gas, the second way of carrier gas, the third way of carrier gas, the fourth way of carrier gas and the fifth way of carrier gas are in a CCW state at a first four-way valve (1) and a second four-way valve (4), and when a first ten-way valve (2) and a twenty-way valve (3) are in a CW state, the first way of carrier gas is communicated with a port 1 of the first four-way valve (1) through a first corrugated pipe valve (5), the port 1 of the first four-way valve (1) is communicated with a port 2 of the first four-way valve (1), and the port 2 of the first four-way valve (1) is communicated with a first vent.
4. An electronic grade hydrogen chloride analysis device according to claim 3, wherein the second path of carrier gas is communicated with the port 1 of the first ten-way valve (2) through the second bellows valve (6), the port 1 of the first ten-way valve (2) is communicated with the port 2 of the first ten-way valve (2), the port 2 of the first ten-way valve (2) is communicated with the first analysis chromatographic column (12), the other end of the first analysis chromatographic column (12) is communicated with the port 2 of the second four-way valve (4), the port 2 of the second four-way valve (4) is communicated with the port 1 of the second four-way valve (4), and the port 1 of the second four-way valve (4) is communicated with the DID detector (16);
the third path of carrier gas is communicated with a port 4 of the first ten-way valve (2) through a third bellows valve (7), the port 4 of the first ten-way valve (2) is communicated with a port 3 of the first ten-way valve (2), the port 3 of the first ten-way valve (2) is communicated with a first pre-separation chromatographic column (10), the other end of the first pre-separation chromatographic column (10) is communicated with a port 9 of the first ten-way valve (2), the port 9 of the first ten-way valve (2) is communicated with a port 10 of the first ten-way valve (2), and the port 10 of the first ten-way valve (2) is communicated with a vent hole;
the fourth carrier gas channel is communicated with a port 1 of a twentieth through valve (3) through a fourth bellows valve (8), the port 1 of the twentieth through valve (3) is communicated with a port 2 of a second four-way valve (3), the port 2 of the twentieth through valve (3) is communicated with a second analysis chromatographic column (13), the other end of the second analysis chromatographic column (13) is communicated with a port 4 of the second four-way valve (4), the port 4 of the second four-way valve (4) is communicated with a port 3 of the second four-way valve (4), and the port 3 of the second four-way valve (4) is communicated with a fourth vent;
the fifth carrier gas is communicated with a port 4 of the twentieth valve (3) through a fifth bellows valve (9), the port 4 of the twentieth valve (3) is communicated with a port 3 of the twentieth valve (3), the port 3 of the twentieth valve (3) is communicated with a second pre-separation chromatographic column (11), the other end of the second pre-separation chromatographic column (11) is communicated with a port 9 of the twentieth valve (3), the port 9 of the twentieth valve (3) is communicated with a port 10 of the twentieth valve (3), and the port 10 of the twentieth valve (3) is communicated with a vent hole.
5. The electronic grade hydrogen chloride analysis device according to claim 2, wherein the sample gas is communicated with the port 3 of the first four-way valve (1), the port 3 of the first four-way valve (1) is communicated with the port 4 of the first four-way valve (1), the port 4 of the first four-way valve (1) is communicated with the port 7 of the first ten-way valve (2), the port 7 of the first ten-way valve (2) is communicated with the port 8 of the first ten-way valve (2), the port 8 of the first ten-way valve (2) is communicated with the first quantitative ring (14), the other end of the first quantitative ring (14) is communicated with the port 5 of the first ten-way valve (2), the port 5 of the first ten-way valve (2) is communicated with the port 6 of the first ten-way valve (2), the port 6 of the first ten-way valve (2) is communicated with the port 6 of the twenty-way valve (3), and the port 6 of the twenty-way valve (3) is communicated with the port 5 of the twenty-way valve (3), no. 5 port of the twentieth valve (3) is communicated with a second quantitative ring (15), the other end of the second quantitative ring (15) is communicated with No. 8 port of the twentieth valve (3), No. 8 port of the twentieth valve (3) is communicated with No. 7 port of the twentieth valve (3), and then the sample gas is discharged.
6. An electronic grade hydrogen chloride analysis device according to claim 2, wherein said DID detector (16) comprises: the ionization chamber (20) and the current collection chamber (21), the lower end of the ionization chamber (20) is connected with one superfine pipeline (18) in a penetrating way, and the other end of the superfine pipeline (18) is connected with the current collection chamber (21) in a penetrating way;
two bilaterally symmetrical discharge electrodes (19) are fixedly arranged in the ionization cavity (20), and a collector (17) is fixedly arranged in the collector cavity (21);
the separating device is connected with a first pipeline (23) in a penetrating way, the other end of the first pipeline (23) is communicated with a second pipeline (26) through a VCR joint, and the second pipeline (26) is communicated with the ionization cavity (20) of the DID detector (16).
7. An electronic grade hydrogen chloride analysis apparatus according to claim 6, wherein the VCR adapter comprises: the pipeline testing device comprises an internal thread sleeve (27) and an external thread sleeve (24), wherein the internal thread sleeve (27) is in threaded connection with the external thread sleeve (24), a leakage testing hole (25) is formed in the internal thread sleeve (27), a first pipeline (23) penetrates through the external thread sleeve (24), the first pipeline (23) is attached to the inner wall of the external thread sleeve (24), a gasket (22) is fixedly connected to the left side of the first pipeline (23), the right end of the gasket (22) is attached to the left end of the external thread sleeve (24), the gasket (22) is arranged in the internal thread sleeve (27), and the gasket (22) is attached to the inner wall of the internal thread sleeve (27);
second pipeline (26) right side extends into in interior screw sleeve (27), just second pipeline (26) right side is fixed and is equipped with the stopper, stopper and the laminating of interior screw sleeve (27) left side wall, just the stopper right side contacts cooperation with packing ring (22).
8. An electronic grade hydrogen chloride analysis device according to claim 7, wherein the internally threaded sleeve (27) is further provided with a locking device (28), and the locking device (28) comprises: the left side of the mounting box (29) is detachably connected with the internal thread sleeve (27), and the clamping mechanism (35) is clamped on the external thread sleeve (24);
the installation box (29) is internally provided with: the upper end of the driving motor (33) is fixedly arranged on the inner wall of the upper side of the mounting box (29), the lower end of the driving motor (33) is fixedly connected with a first rotating rod (49) through an output shaft, and a first gear (30) is fixedly arranged at the lower end of the first rotating rod (49);
the left end and the right end of the first mounting plate (32) are fixedly connected with the inner walls of the left side and the right side of the mounting box (29) respectively, a jog button (48) is arranged on the first mounting plate (32), and the jog button (48) is electrically connected with a driving motor (33);
the lower surface of the first gear (30) is fixedly provided with a first moving rod (31), the lower end of the first moving rod (31) is fixedly provided with a first extension rod, and the first extension rod is located on the front side of the inching button (48).
9. An electronic grade hydrogen chloride analysis device according to claim 8, wherein said clamping mechanism (35) comprises: centre gripping case (36), centre gripping case (36) centre gripping is in external screw sleeve (24) week side, just be equipped with a plurality of spouts (40) on centre gripping case (36), be equipped with in centre gripping case (36): the periphery of the rotating plate (42) is in contact fit with the inner wall of the clamping box (36), a hexagonal groove (43) is formed in the rotating plate (42), a pushing block (39) is further fixedly arranged on the rotating plate (42), and a first opening is formed in the clamping box (36);
the clamping blocks (37) are arranged in the clamping box (36), a sliding block (44) is fixedly arranged on one side, close to the rotating plate (42), of each clamping block (37), the sliding block (44) is arranged in the groove (43) in a sliding mode, a first sliding rod (41) is fixedly connected to one end, far away from the sliding block (44), of each clamping block (37), and the first sliding rod (41) extends into the sliding groove (40);
a limiting box (38) is fixedly arranged at the first opening, a second opening is formed in the limiting box (38), the pushing block (39) penetrates through the first opening and the second opening to extend out of the clamping box (36), a plurality of limiting grooves (47) are formed in the inner walls of the upper side and the lower side of the limiting box (38), clamping springs (45) are symmetrically arranged in the limiting box (38), the clamping springs (45) are clamped on the pushing block (39), a limiting block (46) is fixedly arranged at one end, far away from the pushing block (39), of each clamping spring (45), and the limiting block (46) is in contact fit with the limiting grooves (47);
one end, far away from the pushing block (39), of the clamping box (36) is fixedly connected with a first arc-shaped rack (34), a third opening is formed in the left wall of the installation box (29), and the right end of the first arc-shaped rack (34) penetrates through the third opening to be connected with the first gear (30) in a meshed mode.
10. An electronic grade hydrogen chloride analysis device according to claim 7, wherein a safety device (59) is further fixed on the housing of the DID detector (16), the safety device (59) comprises: the upper ends of the safety boxes (50) are fixedly arranged on a shell of the DID detector (16), and one end, far away from the first pipeline (23), of each safety box (50) is fixedly provided with a first connecting block (52);
the upper ends of the buffer springs (51) are fixedly connected with a shell of the DID detector (16);
the second connecting block (58) is arranged in a triangular shape, one corner of the second connecting block (58) is fixedly connected with the lower end of the buffer spring (51), one corner of the second connecting block (58), which is close to the first pipeline (23), is hinged to the first connecting block (52), and one corner of the second connecting block (58), which is far away from the first pipeline (23), is hinged to the buffer rod (56);
the left end and the right end of the fixing plate (72) are respectively hinged with a first fastening ring (73) and a second fastening ring (74), one end, far away from the fixing plate (72), of the first fastening ring (73) is hinged with a fifth connecting rod (76), one end, far away from the first fastening ring (73), of the fifth connecting rod (76) is fixedly connected with a pressing rod (77), one end, far away from the fixing plate (72), of the second fastening ring (74) is hinged with a sixth connecting rod (75), one end, far away from the second fastening ring (74), of the sixth connecting rod (75) is hinged with one end, far away from the first fastening ring (73), of the fifth connecting rod (76), and a circular ring formed by the fixing plate (72), the first fastening ring (73) and the second fastening ring (74) is sleeved on the outer wall of the first pipeline (23);
a second fixing block (55) is symmetrically arranged on the left side of the first fastening ring (73) and the right side of the second fastening ring (74), and the second fixing block (55) is hinged with one end, far away from the second connecting block (58), of the buffer rod (56);
ratchet wheel subassembly (60) are equipped with to the front and back symmetry in safety box (50), ratchet wheel subassembly (60) include: the ratchet wheel (70) is rotationally connected to the inner wall of the safety box (50), and stop rods (68) are arranged on a plurality of teeth of the ratchet wheel (70);
the safety box comprises an arc-shaped mounting plate (67), wherein the arc-shaped mounting plate (67) is fixedly arranged on the inner wall of the lower side of the safety box (50), a hinge head (65) is fixedly arranged on the arc-shaped mounting plate (67), a stopping plate (66) is hinged to the hinge head (65), a third sliding groove (62) is formed in the stopping plate (66), and the right end of the stopping plate (66) is in contact fit with a ratchet wheel (70);
an arc stopping block (63) is arranged on the upper surface of the arc mounting plate (67) in a sliding mode, a second sliding rod (64) is arranged on the arc stopping block (63), the second sliding rod (64) is arranged in a third sliding groove (62) in a sliding mode, one end, far away from the first pipeline (23), of the arc stopping block (63) is in contact fit with the stopping rod (68), a limiting plate (61) is fixedly arranged at the upper end of the arc mounting plate (67), and one end, close to the first pipeline (23), of the arc stopping block (63) is in contact fit with the limiting plate (61);
ratchet (70) are provided with two, two fixed connection reel (71) between ratchet (70), just around being equipped with rope (57) on reel (71), rope (57) are kept away from reel (71) one end is run through safety box (50) outer wall and with first pipeline (23) outer wall fixed connection keep away from the one end of the one end fixed connection damping spring (53) of first pipeline (23) on rope (57), the other end fixed connection buffer beam (56) of damping spring (53).
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| CN202210659774.XA CN115032301B (en) | 2022-06-13 | 2022-06-13 | Electronic grade hydrogen chloride analysis device |
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| CN202210659774.XA CN115032301B (en) | 2022-06-13 | 2022-06-13 | Electronic grade hydrogen chloride analysis device |
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| CN115032301B (en) | 2023-10-13 |
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