CN116148408A - On-line detection system and method for chlorosilane component - Google Patents
On-line detection system and method for chlorosilane component Download PDFInfo
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- CN116148408A CN116148408A CN202211595294.8A CN202211595294A CN116148408A CN 116148408 A CN116148408 A CN 116148408A CN 202211595294 A CN202211595294 A CN 202211595294A CN 116148408 A CN116148408 A CN 116148408A
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8804—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 automated systems
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/8859—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample inorganic compounds
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Abstract
The chlorosilane component online detection system comprises a chlorosilane storage tank, wherein the chlorosilane storage tank is connected with a first valve, a pipeline between the first valve and a filter is connected with an eighth valve, and the eighth valve is connected with a first recovery tank through a pipeline; the pipeline between the fourth valve and the fifth valve is connected with a sixth valve, and the sixth valve is connected with the second recovery tank through a pipeline; the pipeline between the second valve and the third valve is connected with a purging pipe, and a seventh valve is arranged on the purging pipe; the gas chromatograph is connected with a carrier gas pipeline, a driving gas pipeline and a tail gas absorption pipeline, and the tail gas absorption pipeline is sequentially provided with an alkali absorption tank and a flame arrester. In order to completely avoid links such as sampling, transferring samples, sampling and the like in the laboratory test process, the system is designed into a fully-closed system, and the accuracy of results is ensured.
Description
Technical Field
The invention belongs to the technical field of polysilicon production, and particularly relates to an online chlorosilane component detection system and method.
Background
In the production of chlorosilane (dichlorosilane, trichlorosilane, silicon tetrachloride) and in the production of chlorosilane serving as a raw material or a byproduct of chlorosilane, the chlorosilane is low in boiling point and easy to volatilize, is active in chemical property and easy to react with oxygen and water in the air, and the result error is large when components (hydrogen chloride, dichlorosilane, trichlorosilane, silicon tetrachloride, low-boiling-point substances, high-boiling-point substances and the like) are detected by a laboratory chromatograph, wherein the error mainly comes from the sampling and sample injection processes. For samples with too high content of dichlorosilane (such as more than or equal to 20 percent), the samples can be burnt on fire during conventional sampling and sample transferring, and the sampling is difficult to complete. At present, chlorosilane sampling generally adopts a sampling cabinet and a stainless steel sampling bottle for sampling, which takes a long time and is difficult to sample, so that the sampling times per day are limited, and enough detection results cannot be obtained. Meanwhile, safety accidents such as on-site smoke diffusion, even fire and material splashing injury caused by material leakage are easy to occur in the sampling process, and bad influence can be caused on production. Therefore, the technical problems to be solved by the technical scheme are as follows: the process of manually transferring the sampling bottle is omitted, manual sampling is changed into on-line sampling, and on-line inspection is realized.
Disclosure of Invention
In view of the technical problems in the background art, the chlorosilane component online detection system and the chlorosilane component online detection method provided by the invention are designed into a fully-closed system in order to completely avoid adverse effects such as volatilization of sample components in links such as sampling, sample transferring and sample feeding in a laboratory inspection process, reaction with oxygen and water in the air and the like, and ensure the accuracy of results.
In order to solve the technical problems, the invention adopts the following technical scheme:
the chlorosilane component online detection system comprises a chlorosilane storage tank, wherein the chlorosilane storage tank is sequentially connected with a first valve, a filter, a second valve, a third valve, a fourth valve, a fifth valve and a gas chromatograph through pipelines; the pipeline between the first valve and the filter is connected with an eighth valve, and the eighth valve is connected with the first recovery tank through a pipeline; the pipeline between the fourth valve and the fifth valve is connected with a sixth valve, and the sixth valve is connected with the second recovery tank through a pipeline; the pipeline between the second valve and the third valve is connected with a purging pipe, and a seventh valve is arranged on the purging pipe; the gas chromatograph is connected with a carrier gas pipeline, a driving gas pipeline and a tail gas absorption pipeline, and the tail gas absorption pipeline is sequentially provided with an alkali absorption tank and a flame arrester.
Preferably, the gas chromatograph is provided with a six-way valve, the six-way valve comprises a number A, a number B, a number C, a number D, a number E and a number F, a communicating pipe is arranged between the number B and the number E, a metering pipe is arranged on the communicating pipe, the number C is a sample inlet, the number D is a sample outlet, the number A is a carrier gas inlet, and the number F is a carrier gas outlet; in the sampling state, the A bit is conducted with the F bit, the B bit is conducted with the C bit, and the D bit is conducted with the E bit; under the sample injection state, the A bit is conducted with the B bit, the C bit is conducted with the D bit, and the E bit is conducted with the F bit.
Preferably, the fourth valve is an electrically heated pressure reducing valve.
Preferably, the output end of the fifth valve is provided with a flowmeter, and the output end of the sixth valve is provided with a flowmeter.
Preferably, electric tracing pipes are arranged on the pipelines between the chlorosilane storage tank and the gas chromatograph.
Preferably, the collecting method of the chlorosilane component on-line detecting system is characterized by comprising the following working conditions:
working condition one, sampling and detecting process:
step one, a first valve, an eighth valve are opened, a second valve is closed, chlorosilane passes through the first valve and the eighth valve from a chlorosilane storage tank to a first recovery tank, replacement of the front section of a pipeline is completed, and then the eighth valve is closed;
step two, the first valve, the second valve, the third valve, the fourth valve, the fifth valve and the sixth valve are opened, the seventh valve is closed, chlorosilane is led out from a chlorosilane storage tank through the first valve and a filter and then is led out from a pipeline, a heat tracing pipe is attached to the pipeline to heat a chlorosilane sample, the chlorosilane sample is heated through the second valve and the third valve, and is decompressed after the fourth valve is heated and gasified into gas, and the pressure is regulated and then is divided into two paths, and the two paths are heated and kept warm; one path of the gas flow is regulated by a sixth valve and a flowmeter to a second recovery tank, the other path of the gas flow is regulated by a fifth valve and a flowmeter to a six-way valve of the gas chromatograph,
step three, the gaseous sample starts to the C position of a six-way valve of the chromatograph, and the six-way valve is in a sampling state and is discharged to a third recovery tank through the B position, the metering tube, the E position and the D position of the six-way valve, wherein the third recovery tank is used for being arranged at a sample outlet;
step four, a sample replacement system is used for ensuring that the system is cleaned for a period of time, after the sample at the moment can represent a tested sample, a gas is driven to drive a six-way valve to shift, at the moment, sampling is completed, the six-way valve is in a sample injection state, carrier gas helium enters from a number A, passes through a number B, drives sample gas in a quantitative pipe to enter a chromatographic column of a gas chromatograph through a number E and a number F, and after components of the sample gas are separated by the chromatographic column, the components enter a TCD detector to be detected; the gas from the TCD detector is absorbed by an alkali absorption tank and then is exhausted by a high-level blow-down pipe, and after sample injection is completed, the six-way valve is automatically switched to a sampling state;
step five, after the replacement of the pipeline rear section and the chromatographic six-way valve is completed, closing a fifth valve and a sixth valve and starting detection;
working condition II, pipeline purging flow:
the seventh valve, the third valve, the fourth valve, the fifth valve and the sixth valve are opened, the second valve is closed, the purging nitrogen flows through the seventh valve, the third valve, the fourth valve and the sixth valve to the second recovery tank, and flows through the seventh valve, the third valve, the fourth valve and the fifth valve to the sixth valve to the third recovery tank, so that the sample in the pipeline is thoroughly blown away, and then the seventh valve is closed;
working condition three, standard gas correction: and opening the ninth valve, closing the fifth valve, and allowing standard gas to enter the gas chromatograph through the ninth valve for sampling, sample introduction and detection.
Preferably, the chromatographic column is a 316L stainless steel packed column and is subjected to passivation treatment, and the stationary phase is OV-1; the chromatographic conditions are as follows: sample injection temperature is 80 ℃, column temperature is 40 ℃, detector temperature is 110 ℃, and carrier gas flow rate is 20mL/min.
The following beneficial effects can be achieved in this patent:
1. in order to completely avoid the adverse effects of volatilization of sample components, reaction with oxygen and water in the air and the like in the links of sampling, transferring samples, sampling and the like in the laboratory test process, the system is designed into a fully-closed system, and the accuracy of results is ensured.
2. In order to completely vaporize the sample, the sample transmission pipeline of the system is provided with a heat tracing pipeline on the outer surface of the pipeline behind the filter, so as to heat the sample. The liquid sample is vaporized by a heating and pressure reducing valve, and is reduced to a proper pressure, and then is heated and kept warm.
3. The system is connected with the gas chromatograph and a remote computer through optical fibers, and the gas chromatograph is controlled to run according to a program through control software installed on the computer. Personnel can not read the detection result in the explosion-proof cabinet, if 4-20 mA or modbus is adopted to transmit data, the method is inconvenient, and chromatograms and other specific chromatographic information can not be transmitted. In order to solve the problem, the system is connected with the gas chromatograph and the remote computer through the optical fiber, the chromatograph detection data and the chromatograms are transmitted to the computer of the central control room, and the data are checked and edited at the computer end. The effect is good.
Drawings
The invention is further illustrated by the following examples in conjunction with the accompanying drawings:
FIG. 1 is a process diagram of the present invention;
FIG. 2 is a sample view of a six-way valve of the present invention;
FIG. 3 is a six-way valve sample of the present invention;
FIG. 4 is a diagram of a high purity trichlorosilane according to the present invention;
FIG. 5 is a graph of chlorosilanes according to the invention.
In the figure: a first valve 1, a second valve 2, a third valve 3, a fourth valve 4, a fifth valve 5, a sixth valve 6, a seventh valve 7, an eighth valve 8, a ninth valve 9, a gas chromatograph 10, a first recovery tank 11, a second recovery tank 12, a flowmeter 13, a chlorosilane storage tank 14, a filter 15, an alkali absorption tank 16, and a flame arrester 17; PG represents an in-situ pressure gauge.
Detailed Description
Example 1:
the preferred scheme is as shown in figures 1-3, and a chlorosilane component online detection system is characterized in that a chlorosilane storage tank 14 is sequentially connected with a first valve 1, a filter 15, a second valve 2, a third valve 3, a fourth valve 4, a fifth valve 5 and a gas chromatograph 10 through pipelines; the pipeline between the first valve 1 and the filter 15 is connected with an eighth valve 8, and the eighth valve 8 is connected with the first recovery tank 11 through the pipeline; the pipeline between the fourth valve 4 and the fifth valve 5 is connected with a sixth valve 6, and the sixth valve 6 is connected with a second recovery tank 12 through the pipeline; the pipeline between the second valve 2 and the third valve 3 is connected with a purging pipe, and a seventh valve 7 is arranged on the purging pipe; the gas chromatograph 10 is connected with a carrier gas pipeline, a driving gas pipeline and a tail gas absorption pipeline, and the tail gas absorption pipeline is sequentially provided with an alkali absorption tank and a flame arrester. The output end of the fifth valve 5 is provided with a flowmeter 13, and the output end of the sixth valve 6 is provided with a flowmeter 13. Electric tracing pipes are arranged on the pipelines from the chlorosilane storage tank 14 to the gas chromatograph 10. And electrically heating and vaporizing the sample, decompressing, and completing gas sample injection after flow adjustment.
The carrier gas line in this embodiment is fed with high purity helium. And the air which is introduced into the driving air pipeline is used for driving the switching action of the six-way valve. Flame arrestor 17 is located above alkali absorption tank 16, and alkali absorption tank 16 is connected with flame arrestor 17 through the high-order blow-down pipe. The chlorosilane and helium mixture passing through the reference cell and the sample cell of the detector is absorbed by sodium hydroxide through the alkali solution tank, and the rest gas is emptied through the high-altitude discharge pipe.
The gas chromatograph 10 is provided with a six-way valve, the six-way valve comprises a number A, a number B, a number C, a number D, a number E and a number F, a communicating pipe is arranged between the number B and the number E, a metering pipe is arranged on the communicating pipe, the number C is a sample inlet, the number D is a sample outlet, the number A is a carrier gas inlet, and the number F is a carrier gas outlet; in the sampling state, the A bit is conducted with the F bit, the B bit is conducted with the C bit, and the D bit is conducted with the E bit; under the sample injection state, the A bit is conducted with the B bit, the C bit is conducted with the D bit, and the E bit is conducted with the F bit.
The acquisition method of the chlorosilane component on-line detection system comprises the following steps:
working condition one, sampling and detecting process:
step one, a first valve, an eighth valve are opened, a second valve is closed, chlorosilane passes through the first valve and the eighth valve from a chlorosilane storage tank to a first recovery tank, replacement of the front section of a pipeline is completed, and then the eighth valve is closed;
step two, the first valve, the second valve, the third valve, the fourth valve, the fifth valve and the sixth valve are opened, the seventh valve is closed, chlorosilane is led out from a chlorosilane storage tank through the first valve and a filter and then is led out from a pipeline, a heat tracing pipe is attached to the pipeline to heat a chlorosilane sample, the chlorosilane sample is heated through the second valve and the third valve, and is decompressed after the fourth valve is heated and gasified into gas, and the pressure is regulated and then is divided into two paths, and the two paths are heated and kept warm; one path of the gas flow is regulated by a sixth valve and a flowmeter to a second recovery tank, the other path of the gas flow is regulated by a fifth valve and a flowmeter to a six-way valve of the gas chromatograph,
step three, the gaseous sample starts to the C position of a six-way valve of the chromatograph, and the six-way valve is in a sampling state and is discharged to a third recovery tank through the B position, the metering tube, the E position and the D position of the six-way valve, wherein the third recovery tank is used for being arranged at a sample outlet;
step four, a sample replacement system is used for ensuring that the system is cleaned for a period of time, after the sample at the moment can represent a tested sample, a gas is driven to drive a six-way valve to shift, at the moment, sampling is completed, the six-way valve is in a sample injection state, carrier gas helium enters from a number A, passes through a number B, drives sample gas in a quantitative pipe to enter a chromatographic column of a gas chromatograph through a number E and a number F, and after components of the sample gas are separated by the chromatographic column, the components enter a TCD detector to be detected; the gas from the TCD detector is absorbed by an alkali absorption tank and then is exhausted by a high-level blow-down pipe, and after sample injection is completed, the six-way valve is automatically switched to a sampling state;
step five, after the replacement of the pipeline rear section and the chromatographic six-way valve is completed, closing a fifth valve and a sixth valve and starting detection;
working condition II, pipeline purging flow:
and opening a seventh valve, a third valve, a fourth valve, a fifth valve and a sixth valve, closing the second valve, blowing nitrogen to the second recovery tank through the seventh valve, the third valve, the fourth valve and the sixth valve, and thoroughly blowing the sample in the pipeline through the seventh valve, the third valve, the fourth valve, the fifth valve and the sixth valve to the third recovery tank, and then closing the seventh valve.
Working condition three, standard gas correction: and opening the ninth valve, closing the fifth valve, and allowing standard gas to enter the gas chromatograph through the ninth valve for sampling, sample introduction and detection.
Specifically, the technical requirements of the embodiment are as follows:
1. the system introduces a PLC control system to automatically control all valves (electromagnetic valves) so as to complete sampling, sample introduction and detection according to a program. The gas chromatograph is connected with a remote computer through an optical fiber, and the gas chromatograph is controlled to run according to a program through control software installed on the computer.
The influence of the strong corrosiveness of the sample on the pipeline and the valve and the pollution of the pipeline and the valve to the materials are reduced, and in order to prolong the service life of the materials, the pipeline and the valve of the detection system are 316L in material and are treated on the appearance. The six-way valve (gas injection valve) of the gas chromatograph is made of hastelloy.
The chromatographic column is a 316L stainless steel packed column and is subjected to passivation treatment, and the stationary phase is OV-1. The detector of the detection system is TCD.
The chromatographic conditions are as follows: sample injection temperature is 80 ℃, column temperature is 40 ℃, detector temperature is 110 ℃, and carrier gas flow rate is 20mL/min.
And quantifying by adopting an area normalization method, namely after each component is subjected to color spectrum peak on TCD, the proportion of the peak area to the total peak area of each component is the content.
2. Because the on-line instrument installation site has inflammable and explosive dangers and strong corrosivity, the pretreatment system is provided with a positive pressure explosion-proof cabinet, air is filled in the cabinet, the explosion-proof grade is ExdII CT6 Gb, and the protection grade is as follows: IP65, material 316 and corrosion protection. The heat tracing, heating and vaporization, the PLC system, the lighting, the power distribution cabinet and the like are all placed in the explosion-proof cabinet.
3. In order to ensure the safety of detection instruments and production sites, the system adopts an explosion-proof cabinet meeting the explosion-proof protection requirements and performs anti-corrosion treatment. In order to keep the instrument at a proper environment temperature, the explosion-proof cabinet is provided with an explosion-proof cooling and heating air conditioner. For safety consideration and corrosion protection, the explosion-proof grade of the explosion-proof cooling and heating air conditioner is ExdII CT4 Gb, and the protection grade is as follows: IP65, material 316, and as a corrosion resistant treatment or galvanized plastic coated housing.
4. The working condition of the detection system is as follows: the pressure of the chlorosilane discharged from the tank is 1.0-1.3MPa, and the temperature is 10-40 ℃; the temperature of the pipeline heat tracing is about 50 ℃, the temperature is about 80 ℃ after the pipeline heat tracing passes through a heating and reducing valve, and the pressure is regulated to about 100 KPa; the flow rate is about 2L/min (the pressure and flow rate can be properly adjusted).
5. The detection system is connected with the gas chromatograph and the remote computer through the optical fiber, transmits detection result data to the remote computer, and simultaneously remotely controls the gas chromatograph through computer software.
6. Because the gas chromatograph installation place has inflammable and explosive danger and strong corrosiveness, this detecting system is equipped with the explosion-proof cabinet of malleation, fills air in, and explosion-proof grade is exdII CT6 Gb, protection level: IP65, material 316 and corrosion protection. The heat tracing, heating vaporization, the PLC system, lighting, the power distribution cabinet, the gas chromatograph and the like are all placed in the explosion-proof cabinet.
6. In order to keep the instrument at a proper environment temperature, the explosion-proof cabinet is provided with an explosion-proof cooling and heating air conditioner. For safety consideration and corrosion protection, the explosion-proof grade of the explosion-proof cooling and heating air conditioner is ExdII CT4 Gb, and the protection grade is as follows: IP65, material 316, and as a corrosion resistant treatment or galvanized plastic coated housing.
7. The detection system is provided with standard gas for correcting the instrument, and the content of each component in the standard gas is equivalent to the content of a sample to be detected. Helium is chosen for the background (balance gas) of the standard gas for safety. And standard gas is placed in an explosion-proof gas cylinder cabinet. The explosion-proof level of the gas cylinder cabinet is ExdII CT6 Gb, and the protection level is as follows: IP65, material 316 and corrosion protection. For safety reasons, the present detection system uses high purity helium instead of high purity hydrogen as a carrier gas.
8. The detection system discharges gas after passing through a detector: the tail gas is absorbed by alkali liquor, discharged by a high-altitude emptying pipe which is higher than a platform above the instrument by more than 3.5 meters, and the outlet of the emptying pipe is provided with a flame arrester and is subjected to rainproof treatment.
The running examples are as follows:
the computer software is set with instrument parameters and various power supplies and air valves of the equipment are opened.
The chlorosilane liquid is discharged from a storage tank, the pressure is 1.1MPa, the temperature is 20 ℃, the chlorosilane liquid is conveyed to a recovery tank through a first valve and an eighth valve to replace pipelines (other valves are closed at the moment), after 2 minutes, the eighth valve is closed, a second valve, a third valve, a fourth valve, a fifth valve and a sixth valve are opened, a liquid sample is filtered by the first valve and a filter to obtain large particles with the particle diameter of more than 0.4 micrometers, the heat is carried to 50 ℃, the liquid sample is vaporized by the second valve and the third valve at the fourth valve, the temperature is 80 ℃, the pressure is reduced to 0.1MPa, the temperature is kept at 80 ℃, the flow is 2L/min, and the liquid sample is divided into two paths: one path is connected to the recovery tank through a sixth valve to replace the pipeline, the other path is connected to the chromatograph six-way valve (sampling state) through a fifth valve to replace the pipeline, the six-way valve and the quantitative pipe, after 3 minutes of replacement, the six-way valve is automatically switched from the sampling state to the sample injection state, and carrier gas carries sample gas to enter the chromatographic column for separation, TCD detection is carried out, and the result is remotely transmitted to a computer. The TCD outlet gas of the chromatograph is discharged through a high-altitude emptying pipe after being absorbed by alkali liquor. And after the sampling is finished, the fifth valve, the sixth valve and the first valve are closed before detection. After the sample injection is completed, the six-way valve is automatically switched to a sampling state.
After the detection is completed, the second valve is closed, the seventh valve is opened, nitrogen is emptied into the pipeline and the six-way valve through the seventh valve, the third valve, the fourth valve, the fifth valve and the sixth valve, and the sample in the pipe is quantified, and then all valves are closed to wait for the next detection.
Standard gas correction (standard gas sample injection detection): and the ninth valve is opened, the fifth valve is closed, and the standard gas enters the gas chromatograph through the ninth valve for sampling, sample introduction and detection. Two different sample maps are shown in fig. 4 and 5.
The above embodiments are only preferred embodiments of the present invention, and should not be construed as limiting the present invention, and the scope of the present invention should be defined by the claims, including the equivalents of the technical features in the claims. I.e., equivalent replacement modifications within the scope of this invention are also within the scope of the invention.
Claims (7)
1. The utility model provides a chlorosilane component on-line measuring system, includes chlorosilane storage tank (14), its characterized in that: the chlorosilane storage tank (14) is sequentially connected with a first valve (1), a filter (15), a second valve (2), a third valve (3), a fourth valve (4), a fifth valve (5) and a gas chromatograph (10) through pipelines; the pipeline between the first valve (1) and the filter (15) is connected with an eighth valve (8), and the eighth valve (8) is connected with the first recovery tank (11) through the pipeline; the pipeline between the fourth valve (4) and the fifth valve (5) is connected with a sixth valve (6), and the sixth valve (6) is connected with a second recovery tank (12) through the pipeline; the pipeline between the second valve (2) and the third valve (3) is connected with a purging pipe, and a seventh valve (7) is arranged on the purging pipe; the gas chromatograph (10) is connected with a carrier gas pipeline, a driving gas pipeline and a tail gas absorption pipeline, and the tail gas absorption pipeline is sequentially provided with an alkali absorption tank and a flame arrester.
2. The chlorosilane component online detection system of claim 1, wherein: the gas chromatograph (10) is provided with a six-way valve, the six-way valve comprises a number A, a number B, a number C, a number D, a number E and a number F, a communicating pipe is arranged between the number B and the number E, a metering pipe is arranged on the communicating pipe, the number C is a sample inlet, the number D is a sample outlet, the number A is a carrier gas inlet, and the number F is a carrier gas outlet; in the sampling state, the A bit is conducted with the F bit, the B bit is conducted with the C bit, and the D bit is conducted with the E bit; under the sample injection state, the A bit is conducted with the B bit, the C bit is conducted with the D bit, and the E bit is conducted with the F bit.
3. The chlorosilane component online detection system of claim 1, wherein: the fourth valve (4) is an electric heating pressure reducing valve.
4. The chlorosilane component online detection system of claim 1, wherein: the output end of the fifth valve (5) is provided with a flowmeter (13), and the output end of the sixth valve (6) is provided with the flowmeter (13).
5. The chlorosilane component online detection system of claim 1, wherein: electric tracing pipes are arranged on the pipelines between the chlorosilane storage tank (14) and the gas chromatograph (10).
6. The method for collecting chlorosilane components in-line detection system as in any one of claims 1-5, characterized by comprising the following working conditions:
working condition one, sampling and detecting process:
step one, a first valve, an eighth valve are opened, a second valve is closed, chlorosilane passes through the first valve and the eighth valve from a chlorosilane storage tank to a first recovery tank, replacement of the front section of a pipeline is completed, and then the eighth valve is closed;
step two, the first valve, the second valve, the third valve, the fourth valve, the fifth valve and the sixth valve are opened, the seventh valve is closed, chlorosilane is led out from a chlorosilane storage tank through the first valve and a filter and then is led out from a pipeline, a heat tracing pipe is attached to the pipeline to heat a chlorosilane sample, the chlorosilane sample is heated through the second valve and the third valve, and is decompressed after the fourth valve is heated and gasified into gas, and the pressure is regulated and then is divided into two paths, and the two paths are heated and kept warm; one path of the gas flow is regulated by a sixth valve and a flowmeter to a second recovery tank, the other path of the gas flow is regulated by a fifth valve and a flowmeter to a six-way valve of the gas chromatograph,
step three, the gaseous sample starts to the C position of a six-way valve of the chromatograph, and the six-way valve is in a sampling state and is discharged to a third recovery tank through the B position, the metering tube, the E position and the D position of the six-way valve, wherein the third recovery tank is used for being arranged at a sample outlet;
step four, a sample replacement system is used for ensuring that the system is cleaned for a period of time, after the sample at the moment can represent a tested sample, a gas is driven to drive a six-way valve to shift, at the moment, sampling is completed, the six-way valve is in a sample injection state, carrier gas helium enters from a number A, passes through a number B, drives sample gas in a quantitative pipe to enter a chromatographic column of a gas chromatograph through a number E and a number F, and after components of the sample gas are separated by the chromatographic column, the components enter a TCD detector to be detected; the gas from the TCD detector is absorbed by an alkali absorption tank and then is exhausted by a high-level blow-down pipe, and after sample injection is completed, the six-way valve is automatically switched to a sampling state;
step five, after the replacement of the pipeline rear section and the chromatographic six-way valve is completed, closing a fifth valve and a sixth valve and starting detection;
working condition II, pipeline purging flow:
the seventh valve, the third valve, the fourth valve, the fifth valve and the sixth valve are opened, the second valve is closed, the purging nitrogen flows through the seventh valve, the third valve, the fourth valve and the sixth valve to the second recovery tank, and flows through the seventh valve, the third valve, the fourth valve and the fifth valve to the sixth valve to the third recovery tank, so that the sample in the pipeline is thoroughly blown away, and then the seventh valve is closed;
working condition three, standard gas correction: and opening the ninth valve, closing the fifth valve, and allowing standard gas to enter the gas chromatograph through the ninth valve for sampling, sample introduction and detection.
7. The method for collecting chlorosilane components in-line detection system as in claim 6, wherein: the chromatographic column is a 316L stainless steel packed column and is subjected to passivation treatment, and the stationary phase is OV-1; the chromatographic conditions are as follows: sample injection temperature is 80 ℃, column temperature is 40 ℃, detector temperature is 110 ℃, and carrier gas flow rate is 20mL/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211595294.8A CN116148408A (en) | 2022-12-13 | 2022-12-13 | On-line detection system and method for chlorosilane component |
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| CN116973524A (en) * | 2023-09-25 | 2023-10-31 | 上海良薇机电工程有限公司 | Purity analysis device and method and semiconductor process system |
| CN116973524B (en) * | 2023-09-25 | 2024-05-28 | 上海良薇机电工程有限公司 | Purity analysis device and method and semiconductor process system |
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