CN107101850B - Online sampling method - Google Patents
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- CN107101850B CN107101850B CN201710221910.6A CN201710221910A CN107101850B CN 107101850 B CN107101850 B CN 107101850B CN 201710221910 A CN201710221910 A CN 201710221910A CN 107101850 B CN107101850 B CN 107101850B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/20—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials
- G01N1/2035—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials by deviating part of a fluid stream, e.g. by drawing-off or tapping
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2247—Sampling from a flowing stream of gas
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/20—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials
- G01N1/2035—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials by deviating part of a fluid stream, e.g. by drawing-off or tapping
- G01N2001/205—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials by deviating part of a fluid stream, e.g. by drawing-off or tapping using a valve
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N2001/2282—Devices for withdrawing samples in the gaseous state with cooling means
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Abstract
The invention provides an online sampling method, which carries out online sampling through an online sampling device, wherein the online sampling device comprises: the online sampling method comprises the following steps of purging a pipeline, a sample introduction pipeline, a sampling pipeline, a tail gas pipeline, a protective container and a sampling container, wherein the online sampling method comprises the following steps: sequentially communicating a purging pipeline, a sampling pipeline, a protective container and a tail gas pipeline, and purging the sampling pipeline, the protective container and the tail gas pipeline by using the purging pipeline; and communicating the sample introduction pipeline, the sampling container and the tail gas pipeline in sequence, and performing online sampling by utilizing the blown sampling pipeline and the sampling container. Purging away through impurity or aqueous vapor etc. in sampling pipeline and the sampling container, for follow-up utilize sample introduction pipeline, sampling pipeline and sampling container to treat the sample article and take a sample under the sample state, got rid of danger factors such as impurity pollution and aqueous vapor, and then realized taking a sample safely, accurately.
Description
Technical Field
The invention relates to the field of online sampling equipment, in particular to an online sampling method.
Background
Hexachlorodisilane (Si)2Cl6) Is a high-efficiency deoxidizer, is used as an amorphous silicon film, a photochemical fiber raw material, a siloxane and other excellent raw materials, and has wide application prospect and practical value in the fields of semiconductors, photoelectric materials and the like. The most important use of hexachlorodisilane is in the production of silicon nitride films,compared with the traditional method for preparing the silicon nitride film by dichlorosilane and silane vapor deposition, the method for preparing the silicon nitride film by hexachlorodisilane vapor deposition has the advantages of low deposition temperature, low deposition pressure, high efficiency and better density, insulation property, corrosion resistance and compatibility of the obtained film.
The hexachlorodisilane is easy to generate hydrolysis reaction when meeting water, the produced hydrolysate is extremely easy to burn, and meanwhile, the purity requirement of the hexachlorodisilane for semiconductors and photoelectric materials is relatively high (the total amount of metal impurities is below 100 ng/g), so that the safety of the sampling process can be ensured and the quality level of the hexachlorodisilane can be accurately reflected by the sampled product only by sampling in a fully-closed system.
In addition, the sealed sampling system has potential pollution sources such as chemical micro-pollution and particle impurity pollution inside the pipeline, so a new online sampling device is needed to be provided to improve the safety and accuracy of sampling samples such as hexachlorodisilane.
Disclosure of Invention
The invention mainly aims to provide an online sampling method, which ensures that a sample is high in purity and is not polluted, and the sampling is safe and environment-friendly.
In order to achieve the above object, according to one aspect of the present invention, there is provided an online sampling method for online sampling by an online sampling device, the online sampling device comprising: the online sampling method comprises the following steps of purging a pipeline, a sample introduction pipeline, a sampling pipeline, a tail gas pipeline, a protective container and a sampling container, wherein the online sampling method comprises the following steps: sequentially communicating a purging pipeline, a sampling pipeline, a protective container and a tail gas pipeline, and purging the sampling pipeline, the protective container and the tail gas pipeline by using the purging pipeline; and communicating the sample introduction pipeline, the sampling container and the tail gas pipeline in sequence, and performing online sampling by utilizing the blown sampling pipeline and the sampling container.
Further, after the step of purging, and before performing the online sampling, the online sampling method further comprises: and communicating the purging pipeline, the sampling container and the tail gas pipeline in sequence, and purging the sampling container by using the purging pipeline.
Further, after performing online sampling, the online sampling method further includes: and communicating the purging pipeline with the sample injection pipeline, and performing back flushing on the residual sample in the sample injection pipeline.
Further, after performing online sampling, the online sampling method further includes: and communicating the purging pipeline, the sampling pipeline, the protective container and the tail gas pipeline in sequence, and purging the residual sample in the sampling pipeline into the protective container.
Further, after the step of performing the purging, and before the step of performing the online sampling, the online sampling method further comprises: and communicating the sample introduction pipeline, the sampling pipeline and the sample return pipeline in sequence, and performing sample replacement on the sampling pipeline.
Further, after performing online sampling, the online sampling method further includes: and communicating the purging pipeline, the sampling pipeline and the sample returning pipeline in sequence, and performing back flushing on residual materials in the sampling pipeline and the sample returning pipeline.
Further, the online sampling device further comprises a cooling device, the cooling device is arranged on the sampling pipeline and is arranged at the upstream of the sampling container along the material flowing direction, and in the online sampling process, the online sampling method further comprises the following steps: and cooling the sample conveyed to the sampling pipeline by using cooling equipment.
Further, the purge line further comprises a purge check valve, and after the purging step and before the on-line sampling step, the on-line sampling method further comprises the step of closing the purge check valve to terminate the purging.
Further, the purging medium in the purging step is high purity nitrogen or inert gas having a water content of less than 3 ppm.
Further, the tail gas pipeline is further provided with a tail gas check valve, and after the online sampling step, the online sampling method further comprises the step of closing the tail gas check valve to prevent tail gas from entering the sampling container.
By applying the technical scheme of the invention, the purging pipeline, the sampling pipeline, the tail gas pipeline, the protective container and the sampling container are arranged, the purging pipeline, the sampling pipeline, the protective container and the tail gas pipeline are used for purging the sampling pipeline in the purging state, the protective container is replaced by the sampling container after the pipeline purging is finished, the sampling container is further purged, so that impurities or water vapor and the like in the sampling pipeline and the sampling container are purged, the sampling is carried out by utilizing the sampling pipeline, the sampling pipeline and the sampling container in the sampling state, the danger factors such as impurity pollution and water vapor are eliminated, and the safe and accurate sampling of the sample is realized.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 shows a schematic structure of an on-line sampling device according to a preferred embodiment of the present invention.
Wherein the figures include the following reference numerals:
10. purging the pipeline; 20. a sample introduction pipeline; 30. a sampling pipeline; 40. a tail gas pipeline; 50. a sample returning pipeline; 60. a cooling device; 100. a sampling panel;
11. a first purge valve; 12. a second purge valve; 13. a third purge valve; 14. a purge check valve; 15. a pressure measuring device;
21. a first sample injection valve; 22. a second sample injection valve; 23. a third sample inlet valve;
31. a sampling container; 32. a sampling valve; 33. a protective container;
41. a first tail gas valve; 42. a second tail gas valve; 43 a third exhaust valve; 44. an exhaust gas check valve;
51. a first sample return valve; 52. a second sample return valve; 53. and a third sample return valve.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
As mentioned in the background, the sample which is decomposed by the environmental factors such as water or oxygen and generates flammable or explosive substances or is easily polluted by impurities in sampling equipment has the problems of unsafe and inaccurate sampling. In order to improve the sampling accuracy and safety of such samples, in an exemplary embodiment of the present invention, an online sampling device is provided, as shown in fig. 1, comprising: the online sampling device comprises a purging pipeline 10, a sample introduction pipeline 20, a sampling pipeline 30, a tail gas pipeline 40, a protective container 33 and a sampling container 31, wherein the online sampling device comprises a purging state and a sampling state, and in the purging state, the purging pipeline 10 is communicated with the tail gas pipeline 40 through the sampling pipeline 30 and the protective container 33 which are sequentially connected; in the sampling state, the sample introduction pipeline 20 is communicated with the tail gas pipeline 40 through the sampling pipeline 30 and the sampling container 31 which are connected in sequence.
The online sampling device comprises a purging pipeline, a sample introduction pipeline, a sampling pipeline, a tail gas pipeline, a protective container and a sampling container, wherein the purging pipeline, the sampling pipeline, the protective container and the tail gas pipeline are used for purging the sampling pipeline in a purging state, the protective container is replaced by the sampling container after the pipeline purging is finished, the sampling container is further purged, so that impurities or water vapor and the like in the sampling pipeline and the sampling container are purged, dangerous factors such as impurity pollution and water vapor are eliminated for the subsequent sampling of a sample to be sampled by using the sample introduction pipeline, the sampling pipeline and the sampling container, and the safe and accurate sampling of the sample is further realized.
In the above-mentioned on-line sampling device, the purpose of setting up the pipeline 10 that sweeps away in order to the dangerous factor such as impurity and moisture in the pipeline of taking a sample to the security in the sample process and the accuracy of sample are improved. Thus, the specific arrangement of the purge line 10 is not particularly limited as long as the above-described object can be achieved. In order to more flexibly control the opening and closing of the purge, in a preferred embodiment, as shown in fig. 1, the purge line 10 is provided with a first purge valve 11, a second purge valve 12 and a third purge valve 13 in sequence along the flow direction of the purge gas. According to whether the actual pipeline is an integrally communicated pipeline or a pipeline formed by segmented communication, one or more valves can be arranged on the pipeline so as to realize the opening or closing of the purging gas.
The preferred embodiment described above has one or more purge valves in the purge line to enable the purge step to be opened or closed. To further prevent contamination of the purge gas by the backflow of the purge gas in the line along the purge line into the purge gas storage device when purging is not required, in a preferred embodiment, the purge line 10 further comprises a purge check valve 14, the purge check valve 14 being disposed between the second purge valve 12 and the third purge valve 13. The provision of a purge check valve 14 in the closed condition of the purge valve 13 further facilitates the prevention of the backflow of the purge gas.
In order to more accurately control the amount or strength of the purge, in another more preferred embodiment, the purge line 10 further comprises a pressure measurement device 15 disposed downstream of the third purge valve 13, as shown in fig. 1. The outlet end of the purging pipeline 10 is provided with a measuring device, such as a pressure gauge, so that the pressure of the purging gas introduced into the sampling pipeline 30 can be monitored in real time, and the operation stability of the whole online sampling device is maintained.
In the above online sampling device, the tail gas pipeline 40 is provided to facilitate recovery of the purged tail gas containing impurities or moisture, and when it is determined that the purged tail gas does not contain gas or substance polluting air or environment, the tail gas pipeline 40 may be omitted. The tail gas pipeline is arranged here, and mainly prevents polluted gas from being discharged into the air, so that the tail gas is recycled so as to be discharged after harmless treatment.
During purging or sampling, contamination is caused in order to prevent the off-gas in the off-gas line 40 from flowing back to the protective vessel 33 or the sampling vessel 31, or even to the sampling line 30. In a preferred embodiment, as shown in fig. 1, the exhaust pipeline 40 is provided with a first exhaust valve 41, a second exhaust valve 42 and a third exhaust valve 43 in sequence along the flow direction of the exhaust. Similarly, the number of the valves is determined according to the actual condition that the tail gas pipeline is formed by integrally forming the pipeline or connecting multiple sections, and one or more valves are arranged to effectively prevent the tail gas from flowing back.
In another preferred embodiment, as shown in fig. 1, the exhaust line 40 further comprises an exhaust check valve 44 arranged between the first exhaust valve 41 and the second exhaust valve 42. The provision of the exhaust check valve 44 downstream of the first exhaust valve 41 in the exhaust gas flow direction can more effectively prevent the backflow of the exhaust gas.
The sample introduction pipeline 20 in the online sampling device of the present invention can be communicated with the sampling pipeline 30 only when sampling, and the specific arrangement form can be determined according to the pipeline condition of the sample introduction pipeline 20 in the actual production. In a preferred embodiment of the present invention, the sample inlet line 20 comprises: a first sample injection valve 21, a second sample injection valve 22 and a third sample injection valve 23 which are arranged in sequence along the flow direction of the sample.
In the above preferred embodiment, a valve may be provided according to the communication status of the actual sample introduction pipeline, and the sample introduction pipeline 20 and the sampling pipeline 30 may be connected for sampling only by opening the valve when sample introduction is required. When the sampling is finished or the sampling is not needed, the valve is closed, and the sample is stopped from flowing to the sampling pipeline 30. Similarly, when the three valves are arranged on the sample inlet pipeline, the three valves can be closed in time at a position close to the sample storage device, so that unnecessary sample waste is prevented. And a second sample injection valve 22 is provided in the middle to prevent the sample missing from the first sample injection valve 21 from flowing further downward. And the third sample inlet valve 23 disposed near the end of the sampling line 30 further prevents further downward flow of the unnecessary sample.
In the above online sampling device, after the purging pipeline 10 purges the sampling pipeline 30 and the sampling container 31, the sampling pipeline 30 and the sampling container 31 can be sampled by using the sampling pipeline 20, and the sample in the sampling pipeline gradually drives the purging gas in the sampling pipeline 30 and the sampling container 31 to enter the sampling container 31, thereby completing the online sampling operation. In order to replace and remove the purge gas in the sampling line 30 before sampling, so as to facilitate sampling, in a preferred embodiment of the present invention, the online sampling device further comprises: the sample return pipeline 50 is provided with a sampling valve 32 on the sampling pipeline 30, and the sample return pipeline 50 is communicated with the sampling pipeline 30 through the sampling valve 32.
The arrangement of the sample return pipeline 50 and the sampling valve 32 is convenient for utilizing the sample introduction pipeline 20, the sampling pipeline 30 and the sample return pipeline 50 to be communicated after purging is finished, and the purging gas in the sampling pipeline 30 is replaced by utilizing the sample, so that the sampling pipeline is filled with the sample to be sampled in advance. In the case of hexachlorodisilane, since the purge gas (e.g., high purity nitrogen) does not react with the sample, the purge gas in the sampling line 30 entering the sample storage device through the return line 50 will not pollute the sample or cause unsafe risks. In addition, the setting of returning the appearance pipeline 50 and sampling valve 32 still is favorable to after the sample, retrieves the remaining sample in the sampling pipe. The specific recovery process comprises the following steps: the purging pipeline 10, the sampling pipeline 30 and the sample returning pipeline 50 are communicated, and the sampling valve is opened, so that the purging gas purges the sample remained in the sampling pipeline 30 to the sample storage device, and the waste of the sample is reduced.
Similarly, in order to prevent the sample in the sample return line 50 from flowing back into the sampling line 30 or the sampling container 31, in a preferred embodiment of the present invention, as shown in fig. 1, the sample return line 50 is provided with a first sample return valve 51, a second sample return valve 52 and a third sample return valve 53 in sequence along the material flow direction. The valve can effectively prevent the backflow of the backflow sample.
In the above-mentioned on-line sampling device, according to waiting to take a sample the nature of the article is different, can also set up corresponding device on the pipeline before the sampling container 31 to convert the sample into suitable form, conveniently take a sample. In a preferred embodiment, as shown in fig. 1, the on-line sampling apparatus further comprises a cooling device 60, wherein the cooling device 60 is disposed on the sampling pipe 30 and is located upstream of the sampling valve 32. A cooling device is provided before the sampling valve 32 of the sampling pipe 30 to cool the sample in a gas form into a liquid form, thereby performing online sampling more conveniently, safely and accurately. Of course, when the sample to be sampled has a high boiling point and is itself in liquid form, the cooling device may be omitted.
In another exemplary embodiment of the present invention, there is provided an online sampling method for online sampling by an online sampling device, the online sampling device including: the online sampling method comprises the following steps of (1) purging a pipeline 10, sampling a pipeline 20, sampling a pipeline 30, a tail gas pipeline 40, a protective container 33 and a sampling container 31, wherein the online sampling method comprises the following steps: the purging pipeline 10, the sampling pipeline 30, the sampling container 31 and the tail gas pipeline 40 are communicated in sequence, and the sampling pipeline 30, the sampling container 31 and the tail gas pipeline 40 are purged by the purging pipeline 10; and the sample introduction pipeline 20, the sampling pipeline 30, the sampling container 31 and the tail gas pipeline 40 are sequentially communicated, and the blown sampling pipeline 30 and the sampling container 31 are used for online sampling.
The application discloses online sampling method, through will sweeping the pipeline, the sample pipeline, protective container and tail gas pipeline communicate in proper order, and utilize the pipeline that sweeps to sweep the sample pipeline, sweep away impurity or aqueous vapor etc. in with the sample pipeline, then will advance the appearance pipeline, the sample pipeline, sample container and tail gas pipeline communicate in proper order, and utilize the sample pipeline that sweeps to sweep to carry out online sampling, dangerous factors such as impurity pollution and aqueous vapor have been got rid of, and then realized the safety to the sample, accurate sample.
In order to further improve the accuracy and safety of sampling based on the above-mentioned safe and accurate sampling, in a preferred embodiment of the present application, after the step of purging, and before performing online sampling, the online sampling method further includes: and a step of sequentially communicating the purge line 10, the sampling line 30, the sampling vessel 31, and the tail gas line 40, and purging the sampling vessel 31 by using the purge line 10.
In the above preferred embodiment, the protective container is replaced with the sampling container after the sampling pipeline is purged, and the sampling container is further purged to purge out impurities or moisture and the like in the sampling container. The on-line sampling is carried out by utilizing the blown sampling pipeline and the sampling container, so that the accuracy and the safety of the on-line sampling are further improved.
In order to reduce the sample waste in the sampling step based on the realization of the safe and high-purity sampling, in a preferred embodiment of the present application, after the online sampling, the online sampling method further comprises: and communicating the purging pipeline 10 with the sample injection pipeline 20, and performing back flushing on the residual sample in the sample injection pipeline 20. The back flushing step is added to back flush the residual sample in the sample inlet pipeline 20 to the sample storage device, thereby reducing the waste of the sample.
Similarly, in order to reduce the sample waste in the sampling step based on the accurate and safe sampling, in another preferred embodiment of the present application, after the online sampling, the online sampling method further comprises: and communicating the purging pipeline 10, the sampling pipeline 30, the protective container 33 and the tail gas pipeline 40 in sequence, and purging the residual sample in the sampling pipeline 30 into the protective container 33. The step of back flushing the sampling pipeline is added, so that residual samples in the sampling pipeline can be cleaned up, and the continuity and effectiveness of online sampling are improved.
In order to further improve the purity of the sampled product based on the accurate and safe sampling, in a preferred embodiment of the present application, after the step of purging and before the step of online sampling, the online sampling method further comprises: and communicating the sample introduction pipeline 20, the sampling pipeline 30 and the sample return pipeline 50 in sequence, and performing sample replacement on the sampling pipeline 30.
The step of carrying out sample replacement on the sampling pipeline is added after purging and before online sampling, and the purging gas in the sampling pipeline after purging is replaced by the sample to be sampled, so that the gas content in the sample to be sampled is reduced, and the purity of the sample is improved.
In view of reducing sample waste during online sampling and improving the continuity of online sampling, in a preferred embodiment of the present application, after online sampling is performed, the online sampling method further includes: and communicating the purging pipeline 10, the sampling pipeline 30 and the sample returning pipeline 50 in sequence, and performing back flushing on residual materials in the sampling pipeline 30 and the sample returning pipeline 50.
According to the different properties of the sample to be sampled, a corresponding device can be arranged on the pipeline in front of the sampling container 31, so that the sample can be converted into a proper form and can be sampled conveniently. In a preferred embodiment of the present application, the online sampling apparatus further comprises a cooling device 60, the cooling device 60 is disposed on the sampling pipeline 30 and upstream of the sampling container 31 in the material flow direction, and during the online sampling, the online sampling method further comprises: and cooling the sample conveyed from the sample inlet pipeline 20 to the sampling pipeline 30 by using the cooling device 60. The addition of the cooling device to the sampling line facilitates the conversion of relatively low boiling point samples, such as hexachlorodisilane, from a gaseous state to a liquid state, thereby facilitating more convenient, safer, and more accurate on-line sampling.
In the above-mentioned on-line sampling method, the cooling medium for cooling the sample by the cooling device 60 may be any medium that can be used for cooling, and is preferably cooling water in the present application.
In the online sampling method, after the sampling pipeline and the sampling container are purged, online sampling is carried out, so that the purity and the accuracy of a sampled product can be improved. In order to reduce the contamination of the purge gas source by the backflow of the purge gas from the purge step into the purge gas source along the purge line, in a preferred embodiment of the present application, the purge line 10 further comprises a purge check valve 14, and the online sampling method further comprises the step of closing the purge check valve 14 to terminate the purge after the purge step and before the online sampling step.
In the above-mentioned on-line sampling method, the purging medium in the purging step may be any gas that does not react with the sample to be sampled. In the present application, it is preferred that the purging medium is high purity nitrogen or an inert gas having a water content of less than 3 ppm.
In a preferred embodiment of the present application, the off-gas line 40 is further provided with an off-gas check valve 44, and after the on-line sampling step, the on-line sampling method further comprises the step of closing the off-gas check valve 44 to prevent off-gas from entering the sampling vessel 31. The check valve 44 more effectively prevents back flow of the exhaust gas, reducing the chance of contamination of the sample being taken.
In a most preferred embodiment of the present invention, as shown in FIG. 1, an on-line sampling apparatus for hexachlorodisilane is provided, which includes a piping system, a sample bottle, high purity nitrogen, and a vent gas system. Wherein the pipeline and the valve that relate to among the pipe-line system are the EP grade, and the sample bottle is the PFA material, and trace hexachlorodisilane in the tail gas system processing system, nitrogen system provide the high-purity nitrogen gas that the water content is less than 3ppm for entire system. The piping and valves within the dashed box are shown mounted on the sampling panel 100 of the enclosure.
In the above preferred embodiment, the method for sampling hexachlorodisilane specifically comprises the following steps:
1) and (5) purging with high-purity nitrogen. And opening the first purge valve 11 and the second purge valve 12 of the purge pipeline 10, and the third tail gas valve 43 and the second tail gas valve 42 of the tail gas pipeline 40, then opening the third purge valve 13, and sequentially opening the first tail gas valve 41 and the sampling valve 32 to perform high-purity nitrogen purging. After purging, the sampling valve 32 is closed. The protective container 33 (protective bottle) was replaced with the sampling container 31 (sample bottle), and then the sample valve 32 was opened slowly, and after purging and replacement with high-purity nitrogen gas again, the third purge valve 13, the sampling valve 32, and the first off-gas valve 41 were closed.
2) Replacement with hexachlorodisilane. The first sample injection valve 21, the second sample injection valve 22, the third sample return valve 53 and the second sample return valve 52 are opened, then the third sample injection valve 23, the sampling valve 32 and the first sample return valve 51 are opened slowly in sequence, and the sampling pipeline 30 is replaced by hexachlorodisilane. The first sample return valve 51 is opened during the displacement process to ensure the flow displacement of the sample in the pipeline.
3) A sample of hexachlorodisilane was taken. The first exhaust valve 41 is opened. And slowly opening the sampling valve 32, enabling the sample to enter the sample bottle, closing the sampling valve 32, the third sample inlet valve 23 and the first sample return valve 51 in sequence after sampling is finished, taking down the sample bottle, and screwing up the protection bottle.
4) Purging and replacing with high-purity nitrogen. The third purge valve 13 is opened. And slowly opening a third sample inlet valve 23 to perform high-purity nitrogen purging, performing back flushing on the materials in the feed pipeline to the system, and closing the first sample inlet valve 21, the second sample inlet valve 22 and the third sample inlet valve 23 in sequence. And slowly opening the first sample return valve 51 to perform high-purity nitrogen purging, reversely purging the materials in the pipeline back to the system, and closing the third sample return valve 53, the second sample return valve 52 and the first sample return valve 51 in sequence. The sampling valve 32 is slowly opened to allow the high purity nitrogen to purge the contents of the sampling line 30. And the sampling valve 32 and the first tail gas valve 41 are kept normally open, so that the high-purity nitrogen is continuously blown and protected to the sampling device.
In the preferred embodiment, the sample pipeline system and the sample bottle are fully purged and replaced by high-purity nitrogen, then the nitrogen is closed, and the inlet and outlet valves of the hexachlorodisilane product are opened. And (3) after the pipeline system is fully replaced by the hexachlorodisilane, opening a sampling valve for sampling. And after sampling, closing the sampling valve. And finally, opening a nitrogen valve, and closing an inlet valve and an outlet valve of the hexachlorodisilane product after the liquid product in the pipeline system is back blown to the system. The sampling method has the advantages that: the system is closed, high-purity and pollution-free, and the sampling is safe and environment-friendly.
The following examples are provided to further illustrate the beneficial effects of the present invention.
Example 1:
the hexachlorodisilane produced by a certain Luoyang polysilicon factory is subjected to closed online sampling and then sent to a laboratory for detection. Compared with the standard of AIR liquid company (see tables 1 and 2), the result basically meets the production requirement.
Table 1: results of impurity detection in example 1
Table 2: results of component detection in example 1
| Components | AIR liquid Standard | Example 1 |
| Si2Cl6 | ＞99.7％ | 99.99％ |
| SiHCl3+SiCl4 | ＜0.2％ | 0.01％ |
Example 2:
comparative analysis with dao kaning: the raw material is hexachlorodisilane produced by a certain Luoyang polysilicon factory, the content of the hexachlorodisilane is more than 99 percent, after the stable operation is carried out for 15 days, A, B samples are simultaneously sampled by the online sampling device, wherein, A sample is sent to the Corning test, B sample is sent to the laboratory test of the certain Luoyang polysilicon factory for test. The analytical results are shown in Table 3.
Table 3: comparative analysis result with dao kangning
| Components | Sample A | Sample B |
| Si2Cl6 | 99.86％ | 99.88％ |
| SiHCl3 | 0.003％ | 0.005％ |
| SiCl4 | 0.019％ | 0.010％ |
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects: through will sweeping pipeline, sample pipeline, protective container and tail gas pipeline and communicate in proper order to utilize and sweep the pipeline and sweep the sample pipeline, sweep away impurity or aqueous vapor etc. in the sample pipeline, then will advance kind pipeline, sample container and tail gas pipeline and communicate in proper order, and utilize and sweep the sample pipeline that the sample pipeline carries out online sampling, get rid of dangerous factors such as impurity pollution and aqueous vapor, and then realized the safety to the sample, accurate sample.
Further, replace the protective container for the sampling container after the sampling pipeline sweeps and accomplish, further sweep the sampling container to impurity or aqueous vapor etc. in sweeping the sampling container away. The on-line sampling is carried out by utilizing the blown sampling pipeline and the sampling container, so that the accuracy and the safety of the on-line sampling are further improved.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. An online sampling method, wherein the online sampling method is used for online sampling through an online sampling device, and the online sampling device comprises: a purging pipeline (10), a sample introduction pipeline (20), a sampling pipeline (30), a tail gas pipeline (40), a protective container (33) and a sampling container (31),
the online sampling method comprises the following steps:
sequentially communicating the purging pipeline (10), the sampling pipeline (30), the protective container (33) and the tail gas pipeline (40), and purging the sampling pipeline (30), the protective container (33) and the tail gas pipeline (40) by using the purging pipeline (10); and
the sample introduction pipeline (20), the sampling pipeline (30), the sampling container (31) and the tail gas pipeline (40) are sequentially communicated, and the sampling pipeline (30) and the sampling container (31) which are blown away are utilized for online sampling;
after performing the purge, and before performing the online sampling, the online sampling method further comprises:
a step of sequentially communicating the purge line (10), the sampling line (30), the sampling vessel (31), and the tail gas line (40), and purging the sampling vessel (31) by using the purge line (10);
after the online sampling is performed, the online sampling method further comprises:
a step of sequentially communicating the purging pipeline (10), the sampling pipeline (30), the protective container (33) and the tail gas pipeline (40), and purging residual samples in the sampling pipeline (30) into the protective container (33);
after the online sampling is performed, the online sampling method further comprises:
communicating the purging pipeline (10) with the sample introduction pipeline (20), and performing back flushing on the residual sample in the sample introduction pipeline (20);
after performing the purge, and before performing the online sampling, the online sampling method further comprises:
sequentially communicating the sample introduction pipeline (20), the sampling pipeline (30) and the sample return pipeline (50), and performing sample replacement on the sampling pipeline (30);
after the online sampling is performed, the online sampling method further comprises:
and communicating the purging pipeline (10), the sampling pipeline (30) and the sample returning pipeline (50) in sequence, and performing back flushing on residual materials in the sampling pipeline (30) and the sample returning pipeline (50).
2. The on-line sampling method according to claim 1, wherein the on-line sampling apparatus further comprises a cooling device (60), the cooling device (60) being disposed on the sampling pipe (30) and upstream of the sampling vessel (31) in a material flow direction, the on-line sampling method further comprising, during the on-line sampling:
a step of cooling the sample conveyed to the sampling pipeline (30) by the sampling pipeline (20) by the cooling device (60).
3. The on-line sampling method according to claim 1, wherein the purge line (10) further comprises a purge check valve (14), and after the purging and before the on-line sampling, the on-line sampling method further comprises the step of closing the purge check valve (14) to terminate the purging.
4. The on-line sampling method of claim 1, wherein in the purging step, the purging medium is high purity nitrogen or an inert gas having a water content of less than 3 ppm.
5. The on-line sampling method according to claim 1, wherein an off-gas check valve (44) is further provided on the off-gas line (40), and after the on-line sampling, the on-line sampling method further comprises the step of closing the off-gas check valve (44) to prevent off-gas from entering the sampling vessel (31).
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| CN2426146Y (en) * | 1999-12-29 | 2001-04-04 | 师庆安 | Sealed sampler |
| CN201163246Y (en) * | 2008-01-23 | 2008-12-10 | 乐山市永晟仪表阀门制造有限公司 | Polysilicon chlorosilane sampling device |
| CN202013290U (en) * | 2010-11-26 | 2011-10-19 | 亚洲硅业（青海）有限公司 | Combined sealing sampler |
| CN102539197A (en) * | 2012-01-13 | 2012-07-04 | 武汉新硅科技有限公司 | Sampling method implemented during process of analyzing metal-element content of high-purity silicon tetrachloride product used for fibers |
| CN203405345U (en) * | 2012-11-30 | 2014-01-22 | 内蒙古神舟硅业有限责任公司 | Chlorosilane liquid sampling device |
| CN106226138B (en) * | 2016-08-23 | 2019-06-28 | 上海正帆科技股份有限公司 | The sampler and analysis method of trace metal impurity content in electron level arsine |
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