CN107101850A - On-line period method - Google Patents
On-line period method Download PDFInfo
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- CN107101850A CN107101850A CN201710221910.6A CN201710221910A CN107101850A CN 107101850 A CN107101850 A CN 107101850A CN 201710221910 A CN201710221910 A CN 201710221910A CN 107101850 A CN107101850 A CN 107101850A
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- line period
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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
-
- 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
-
- 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
-
- 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
Abstract
The invention provides a kind of on-line period method, the on-line period method carries out on-line period by on-line period device, and on-line period device includes：Scavenging pipeline, sample introduction pipeline, sampling line, tail gas pipeline, protective container and sampling container, on-line period method include：Scavenging pipeline, sampling line, protective container and tail gas pipeline are sequentially communicated, sampling line, protective container and tail gas pipeline purged using scavenging pipeline；And be sequentially communicated sample introduction pipeline, sampling line, sampling container and tail gas pipeline, and carry out on-line period using purged sampling line and sampling container.By the way that impurity or aqueous vapor in sampling pipe and sampling container etc. is purged away, to be subsequently sampled under sampling state using sample introduction pipeline, sampling line and sampling container to product to be sampled, the hazards such as impurity pollution and aqueous vapor are eliminated, and then realize the safe and accurate sampling to sample.
Description
Technical field
The present invention relates to on-line period apparatus field, in particular to a kind of on-line period method.
Background technology
Hexachloro-silane (Si2Cl6) be a kind of efficient deoxidier, as amorphous si film, photochemistry fibrous raw material with
And the good raw material of siloxanes etc., had a wide range of applications and real value in fields such as semiconductor, photoelectric materials.Chlordene
The most important purposes of disilane is manufacture N-Si film, thin compared to traditional dichlorosilane, silane gas deposition legal system nitrogen silicon
Film, depositing temperature, the deposition pressure of hexachloro-silane vapour deposition process are low, efficiency high and obtain the density of film, it is insulating properties, anti-
Corrosivity, compatibility are all more excellent.
Hexachloro-silane meets water and easily occurs hydrolysis, and the hydrolysate of production easily burns, while semiconductor, photoelectric material
It is relatively high (below metal impurities total amount 100ng/g) with the purity requirement of hexachloro-silane, it is therefore necessary in totally enclosed system
In be sampled, just can guarantee that the safety of sampling process and samples taken is accurately reflected the quality level of hexachloro-silane.
In addition, there is the potential pollution sources such as the micro- pollution of chemistry and granule foreign pollution inside enclosed sampling system pipeline,
Therefore need to provide a kind of new on-line period device, with the security of the sampling that improves the sample such as hexachloro-silane etc and
Accuracy.
The content of the invention
It is a primary object of the present invention to provide a kind of on-line period method, it is ensured that sample is high-purity not to be stain and sampled
It is safe and environment-friendly.
To achieve these goals, according to an aspect of the invention, there is provided a kind of on-line period method, this takes online
Quadrat method carries out on-line period by on-line period device, and on-line period device includes：Scavenging pipeline, sample introduction pipeline, probe tube
Road, tail gas pipeline, protective container and sampling container, on-line period method include：Scavenging pipeline, sampling line, protection are held
Device and tail gas pipeline are sequentially communicated, and sampling line, protective container and tail gas pipeline are purged using scavenging pipeline；With
And be sequentially communicated sample introduction pipeline, sampling line, sampling container and tail gas pipeline, and using purged sampling line and take
Sample container carries out on-line period.
Further, after the step of purging, and before progress on-line period, on-line period method also includes：It will blow
Sweep pipeline, sampling line, sampling container and tail gas pipeline to be sequentially communicated, sampling container is purged using scavenging pipeline
Step.
Further, after on-line period is carried out, on-line period method also includes：Scavenging pipeline and sample introduction pipeline are connected
The step of leading to, and blowback carried out to the residual sample in sample introduction pipeline.
Further, after on-line period is carried out, on-line period method also includes：By scavenging pipeline, sampling line, guarantor
Shield container and tail gas pipeline are sequentially communicated, and the residual sample in sampling line is purged to the step into protective container
Suddenly.
Further, after the step of being purged, and before the step of progress on-line period, on-line period method
Also include：Sample introduction pipeline, sampling line and counter sample pipeline are sequentially communicated, and the step of sample displacement is carried out to sampling line
Suddenly.
Further, after on-line period is carried out, on-line period method also includes：By scavenging pipeline, sampling line with
And counter sample pipeline is sequentially communicated, and in sampling line and counter sample pipeline residual material carry out blowback the step of.
Further, on-line period device also includes cooling device, and cooling device is arranged on sampling line, and along material
Flow direction is arranged on the upstream of sampling container, during on-line period, and on-line period method also includes：Utilize cooling device
The step of being cooled down to the sample that sample introduction pipeline is delivered to sampling line.
Further, scavenging pipeline also includes purging check-valves, after purge step, and before on-line period step,
On-line period method also includes closing the step of purging check-valves is to terminate purging.
Further, the blowing medium in purge step is the high pure nitrogen or inert gas that water content is less than 3ppm.
Further, after tail gas pipeline is above-mentioned the step of be additionally provided with tail gas check-valves, on-line period, on-line period method
Also include closing tail gas check-valves preventing the step of tail gas enters sampling container.
Apply the technical scheme of the present invention, by setting scavenging pipeline, sample introduction pipeline, sampling line, tail gas pipeline, protection
Container and sampling container, and scavenging pipeline, sampling line, protective container and tail gas pipeline are utilized to probe tube in the state of purging
Road is purged, and protective container is replaced with into sampling container after the completion of blowing pipeline, and further sampling container is blown
Sweep, impurity or aqueous vapor in sampling pipe and sampling container etc. is purged away, be that sample introduction is utilized subsequently under sampling state
Pipeline, sampling line and sampling container are sampled to product to be sampled, are eliminated the hazards such as impurity pollution and aqueous vapor, are entered
And realize the safe and accurate sampling to sample.
Brief description of the drawings
The Figure of description for constituting the part of the application is used for providing a further understanding of the present invention, and of the invention shows
Meaning property embodiment and its illustrate be used for explain the present invention, do not constitute inappropriate limitation of the present invention.In the accompanying drawings：
Fig. 1 shows the structural representation of the on-line period device in a kind of preferred embodiment of the invention.
Wherein, above-mentioned accompanying drawing is marked including the following drawings：
10th, scavenging pipeline；20th, sample introduction pipeline；30th, sampling line；40th, tail gas pipeline；50th, counter sample pipeline；60th, cooling is set
It is standby；100th, panel is sampled；
11st, the first purging valve；12nd, the second purging valve；13rd, the 3rd purging valve；14th, check-valves is purged；15th, pressure measurement
Device；
21st, the first sample introduction valve；22nd, the second sample introduction valve；23rd, the 3rd sample introduction valve；
31st, sampling container；32nd, sample cock；33rd, protective container；
41st, the first tail gas valve；42nd, the second tail gas valve；43 the 3rd tail gas valves；44th, tail gas check-valves；
51st, the first counter sample valve；52nd, the second counter sample valve；53rd, the 3rd counter sample valve.
Embodiment
It should be noted that in the case where not conflicting, the feature in embodiment and embodiment in the application can phase
Mutually combination.The present invention is described in detail below in conjunction with embodiment.
As background technology is previously mentioned, it is this kind of to hexachloro-silane chance the environmental factor such as water or oxygen and decompose generation it is inflammable
Or explosive material, or easily sample contaminated by the impurity in sampling equipment, there is sampling when being sampled dangerous
And it is inaccurate the problem of.In order to improve the sampling accuracy and security of this kind of sample, in a kind of typical implementation of the invention
There is provided a kind of on-line period device in mode, as shown in figure 1, the on-line period device includes：Scavenging pipeline 10, sample feeding pipe
Road 20, sampling line 30, tail gas pipeline 40, protective container 33 and sampling container 31, on-line period device include purging state
With sampling state, in the state of purging, scavenging pipeline 10 passes through the sampling line 30 and protective container 33 and tail gas that are sequentially connected
Pipeline 40 is connected；In the state of sampling, sample introduction pipeline 20 passes through the sampling line 30 and sampling container 31 and tail that are sequentially connected
Air pipe 40 is connected.
The present invention above-mentioned on-line period device by set scavenging pipeline, sample introduction pipeline, sampling line, tail gas pipeline,
Protective container and sampling container, and purge state when using scavenging pipeline, sampling line, protective container and tail gas pipeline to taking
Sample pipeline is purged, and protective container is replaced with into sampling container after the completion of blowing pipeline, and further sampling container is entered
Row purging, impurity or aqueous vapor in sampling pipe and sampling container etc. is purged away, is later use sample introduction pipeline, sampling
Pipeline and sampling container are sampled to product to be sampled eliminates impurity pollution and the hazards such as aqueous vapor, and then realizes pair
The safe and accurate sampling of sample.
In above-mentioned on-line period device, the purpose for setting scavenging pipeline 10 is in order to the impurity and moisture in sampling line
Purged away etc. hazards, to improve the accuracy of the security in sampling process and sampling.Thus, to scavenging pipeline 10
Specific set-up mode has no particular/special requirement, as long as above-mentioned purpose can be realized.In order to control the unlatching of purging for greater flexibility
And closing, in an advantageous embodiment, as shown in figure 1, above-mentioned scavenging pipeline 10 is set gradually along flow of sweep gas direction
There is the first purging valve 11, second to purge the purging valve 13 of valve 12 and the 3rd.The pipeline of connection is integrated according to actual pipeline
Or the pipeline of segmentation connection, one or more valves can be set on pipeline, purge gas is opened to realize
Open or close.
One or more purging valves are set on the scavenging pipeline in above preferred embodiment, have been able to realize to purging
Step is turned on and off.In order to further prevent when that need not purge, purge gas in pipeline is along scavenging pipeline adverse current
Purge gas is polluted into purge gas storage device, in a kind of preferred embodiment, above-mentioned scavenging pipeline 10
Also include purging check-valves 14, purging check-valves 14 is arranged between the second purging valve 12 and the 3rd purging valve 13.Closing
In the case of closing purging valve 13, then a purging check-valves 14 is set to be more conducive to prevent purge gas from flowing back.
In order to more accurately control the amount or purging effort of purging, in another preferred embodiment, such as Fig. 1 institutes
Show, the scavenging pipeline 10 also includes the pressure tester 15 for being arranged on the 3rd purging valve 13 downstream.In the outlet of scavenging pipeline 10
End sets measurement apparatus, such as pressure gauge can monitor the pressure for the purge gas being passed through in sampling line 30 in real time, so that more
Beneficial to the operation stability for maintaining whole on-line period device.
In above-mentioned on-line period device, the setting of tail gas pipeline 40 is easy for the tail containing impurity or aqueous vapor to purging out
Gas is reclaimed, and when it is determined that not containing the gas or material for having pollution to air or environment in tail gas after purging, also may be used
To omit the tail gas pipeline 40.Tail gas pipeline is set herein, mainly prevents the gas stained to be discharged into air, thus it is right
Tail gas is reclaimed, to be discharged again after carrying out harmless processing.
In purging or sampling process, in order to prevent the tail gas in tail gas pipeline 40 to be back to protective container 33 or sampling
Container 31, or even be back in sampling line 30, and pollute.In a kind of preferred embodiment, as shown in figure 1, tail gas pipeline
40 are disposed with the first tail gas valve 41, the second tail gas valve 42 and the 3rd tail gas valve 43 along the flow direction of tail gas.Together
Sample, the quantity of valve according to offgas duct route integrally formed pipeline still by multistage be formed by connecting pipeline actual state and
It is fixed, set one or more valves effectively to prevent the backflow of tail gas.
In an additional preferred embodiment, as shown in figure 1, tail gas pipeline 40 also includes being arranged on the He of the first tail gas valve 41
Tail gas check-valves 44 between second tail gas valve 42.In the downstream of the first tail gas valve 41 along exhaust gas flow direction, tail gas is set
Check-valves 44 can more efficiently prevent from the backflow of tail gas.
As long as sample introduction pipeline 20 can be connected in sampling with sampling line 30 in the above-mentioned on-line period device of the present invention
Logical, it specifically sets form can be depending on the pipeline situation according to sample introduction pipeline 20 in actual production.Of the invention a kind of
In preferred embodiment, sample introduction pipeline 20 includes：The first sample introduction valve 21, the second sampling valve set gradually along sample flow direction
The sample introduction valve 23 of door 22 and the 3rd.
In above preferred embodiment, according to the connection situation of actual sample introduction pipeline, a valve can be set, only needed
The valve is opened during sample introduction sample introduction pipeline 20 can be connected with sampling line 30 and is sampled.And when sampling terminates or need not
During sampling, then the valve is closed, stop sample and circulated to sampling line 30.Equally, when setting above three on sample introduction pipeline
During valve, it can in time be closed close to the position of sample storage device, prevent unnecessary sample waste.And in centre setting
One the second sample introduction valve 22 can prevent from further flowing downward from the sample that the first sample introduction valve 21 is omitted.And taken close
The 3rd sample introduction valve 23 that the one end of sample pipeline 30 is set further avoid further flowing downward for unnecessary sample.
In above-mentioned on-line period device, after scavenging pipeline 10 to sampling line 30, sampling container 31 purge totally,
Just sampling line 30 and sampling container 31 are sampled using sample introduction pipeline 20, the sample in sample introduction pipeline is gradually driven
Sampling line 30 and purge gas in sampling container 31 and enter in sampling container 31, so as to complete on-line period work.And
Removed to before sampling, enter line replacement to the purge gas in sampling line 30, to be more easily sampled, at this
Invent in a kind of preferred embodiment, above-mentioned on-line period device also includes：It is provided with and takes on counter sample pipeline 50, sampling line 30
Sample valve 32, counter sample pipeline 50 is connected by sample cock 32 with sampling line 30.
The setting of above-mentioned counter sample pipeline 50 and sample cock 32, is easy to after purging terminates, and utilizes sample introduction pipeline 20, sampling
Pipeline 30 is connected with counter sample pipeline 50, enters line replacement to the purge gas in sampling line 30 using sample, so as to sampling pipe
In in advance be full of product to be sampled.By taking hexachloro-silane as an example, because purge gas (such as high pure nitrogen) is not reacted with sample,
Thus, the purge gas in sampling line 30 enters through counter sample pipeline 50 can't pollute in sample storage device to sample
Or cause hidden danger.In addition, the setting of counter sample pipeline 50 and sample cock 32, is also helped after sampling terminates, to taking
The sample remained in sample pipeline is reclaimed.Specifically recovery process is：By scavenging pipeline 10, sampling line 30 and counter sample pipeline 50
Connection, sample cock is opened so that purge gas is by the sample purge remained in sampling line 30 to sample storage device
In, to reduce the waste of sample.
Similarly, in order to avoid the sample in counter sample pipeline 50 enters sampling line 30 or sampling container 31 along pipeline adverse current
In, in a kind of preferred embodiment of the invention, as shown in figure 1, counter sample pipeline 50 is disposed with along Flow of Goods and Materials direction
One counter sample valve 51, the second counter sample valve 52 and the 3rd counter sample valve 53.The setting of valve being capable of effectively anti-backflow sample
Adverse current.
It is different according to the property of product to be sampled in above-mentioned on-line period device, can also be in the pipe before sampling container 31
Corresponding device is set on road, in order to which sample changeover, into suitable form, is conveniently sampled.In a kind of preferred embodiment
In, as shown in figure 1, above-mentioned on-line period device also includes cooling device 60, cooling device 60 is arranged on sampling line 30, and
Positioned at the upstream of sample cock 32.Cooling device is set before the sample cock 32 of sampling line 30, so as to by gas form
Sample be cooled to liquid form so that it is more convenient, safer, more accurately carry out on-line period.Certainly, when product to be sampled boil
Point it is higher, inherently with liquid form in the presence of, then the cooling device can be omitted.
There is provided a kind of on-line period method, the on-line period side in another typical embodiment of the present invention
Method carries out on-line period by on-line period device, and on-line period device includes：Scavenging pipeline 10, sample introduction pipeline 20, probe tube
Road 30, tail gas pipeline 40, protective container 33 and sampling container 31, the on-line period method include：By scavenging pipeline 10, sampling
Pipeline 30, sampling container 31 and tail gas pipeline 40 are sequentially communicated, using scavenging pipeline 10 to sampling line 30, sampling container 31
And tail gas pipeline 40 is purged；And by sample introduction pipeline 20, sampling line 30, sampling container 31 and tail gas pipeline 40 according to
Secondary connection, and carry out on-line period using purged sampling line 30 and sampling container 31.
The on-line period method of the application, by the way that scavenging pipeline, sampling line, protective container and tail gas pipeline are connected successively
It is logical, and sampling line is purged using scavenging pipeline, impurity or aqueous vapor in sampling line etc. is purged away, then
Sample introduction pipeline, sampling line, sampling container and tail gas pipeline are sequentially communicated, and carried out using purged sampling line
Line is sampled, and eliminates the hazards such as impurity pollution and aqueous vapor, and then realize the safe and accurate sampling to sample.
On the basis of the sampling of above-mentioned safety and precise, in order to further improve the accuracy and security of sampling, in this Shen
Please in a kind of preferred embodiment, the step of above-mentioned purging after, and before carrying out on-line period, the on-line period method is also
Including：Scavenging pipeline 10, sampling line 30, sampling container 31 and tail gas pipeline 40 are sequentially communicated, scavenging pipeline 10 is utilized
The step of being purged to sampling container 31.
In above-mentioned preferred embodiment, protective container is replaced with into sampling container after the completion of sampling pipe purging, enters one
Step is purged to sampling container, and impurity or aqueous vapor in sampling container etc. is purged away.Utilize purged probe tube
Road and sampling container carry out on-line period, further increase the accuracy and security of on-line period.
State in realization safety, high-purity sampling on the basis of, in order to down-sample the sample waste of step, in the application
In a kind of preferred embodiment, after on-line period is carried out, the on-line period method also includes：By scavenging pipeline 10 and sample introduction
Pipeline 20 is connected, and in sample introduction pipeline 20 residual sample carry out blowback the step of.The step of increasing the blowback will can enter
The sample blowback remained in sample pipeline 20 is into sample storage device, so as to reduce the waste of sample.
Similarly, state in realization it is accurate, safety sampling on the basis of, in order to down-sample the sample waste of sample step,
In another preferred embodiment of the application, after on-line period is carried out, the on-line period method also includes：By scavenging conduit
Road 10, sampling line 30, protective container 33 and tail gas pipeline 40 are sequentially communicated, and the residual sample in sampling line 30 is entered
Step of the row purging into protective container 33.The step of increase is to sampling line blowback, can be by the residual sample in sampling line
Product are cleaned out, so as to improve the continuity and validity of on-line period.
State in realization it is accurate, safety sampling on the basis of, in order to further improve the purity of samples taken, in the application
A kind of preferred embodiment in, after the step of being purged, and carry out on-line period the step of before, this takes online
Quadrat method also includes：Sample introduction pipeline 20, sampling line 30 and counter sample pipeline 50 are sequentially communicated, and sampling line 30 is carried out
The step of sample displacement.
By the way that after purging and before on-line period, the step of increase carries out sample displacement to sampling line will blow
The purge gas in sampling line after sweeping is replaced into product to be sampled, so as to reduce the gas content in samples taken, improves
Sample purity.
The continuity of sample waste and raising on-line period considers during on-line period is reduced, a kind of in the application
In preferred embodiment, after on-line period is carried out, on-line period method also includes：By scavenging pipeline 10, sampling line 30
And counter sample pipeline 50 is sequentially communicated, and in sampling line 30 and counter sample pipeline 50 residual material carry out blowback the step of.
According to the difference of moral character matter to be sampled, corresponding device can also be set on the pipeline before sampling container 31,
In order to which sample changeover, into suitable form, is conveniently sampled.In a kind of preferred embodiment of the application, on-line period device
Also include cooling device 60, the cooling device 60 is arranged on sampling line 30, and sampling appearance is arranged on along Flow of Goods and Materials direction
During the upstream of device 31, on-line period, the on-line period method also includes：Sample introduction pipeline 20 is conveyed using cooling device 60
The step of being cooled down to the sample of sampling line 30.Increasing the cooling device on sampling line contributes to such as silicon of chlordene two
The sample that the boiling point of alkane etc is relatively low is converted into liquid by gaseous state, consequently facilitating it is more convenient, safer, more accurately carry out
On-line period.
In above-mentioned on-line period method, the cooling medium that cooling device 60 is cooled down to sample can be existing any energy
The medium of cooling is enough in, the application is preferably cooling water.
In above-mentioned on-line period method, after being purged to sampling line and sampling container, then carry out online
Sampling, it is possible to increase the purity and accuracy of samples taken.In order to reduce the purge gas of purge step along scavenging pipeline adverse current
Polluted into source purge gas and to source purge gas, in a kind of preferred embodiment of the application, above-mentioned scavenging pipeline 10 is also
Including purging check-valves 14, after purge step, and before on-line period step, above-mentioned on-line period method also includes closing
Purge the step of check-valves 14 is to terminate purging.
In above-mentioned on-line period method, the blowing medium in purge step can not react to be any with product to be sampled
Gas.In this application, preferably blowing medium is the high pure nitrogen or inert gas that water content is less than 3ppm.
In a kind of preferred embodiment of the application, above-mentioned tail gas pipeline 40 is above-mentioned to be additionally provided with tail gas check-valves 44,
After the step of above-mentioned on-line period, the on-line period method also includes closing tail gas check-valves 44 preventing tail gas from entering sampling
The step of container 31.Check-valves 44 can more efficiently prevent from the backflow of tail gas, reduce the probability polluted to samples taken.
In a kind of most preferred embodiment of the invention, exist as shown in Figure 1 there is provided a kind of suitable for hexachloro-silane
Line sampler, it includes pipe-line system, sample bottle, high pure nitrogen and exhaust system.The pipe being wherein related in pipe-line system
Road and valve are EP grades, and sample bottle is hexachloro-silane micro in PFA materials, exhaust system processing system, nitrogen system
Unite and provide the high pure nitrogen that water content is less than 3ppm for whole system.Pipeline and valve in figure in dotted line frame are arranged on guard box
Sampling panel 100 on.
In above preferred embodiment, the sampling method of hexachloro-silane is specifically comprised the steps of：
1) high pure nitrogen is purged.Open the first purging purging valve 12 of valve 11, second of scavenging pipeline 10, and tail gas
The 3rd tail gas valve 43, the second tail gas valve 42 of pipeline 40, then open the 3rd and purge valve 13, the first tail gas is opened successively
Valve 41, sample cock 32, carry out high pure nitrogen purging.Purging is finished, and closes sample cock 32.By (the protection of protective container 33
Bottle) be replaced by sampling container 31 (sample bottle) after tighten, it is slow to open sample cock 32, carry out purging with high pure nitrogen again and put
After changing, close the 3rd and purge valve 13, the tail gas valve 41 of sample cock 32 and first.
2) hexachloro-silane is replaced.Open the first sample introduction valve 21, the second sample introduction valve 22, the 3rd counter sample valve 53 and
Second counter sample valve 52, it is then slow successively to open the 3rd sample introduction valve 23, the counter sample valve 51 of sample cock 32 and first, six
Chlorine disilane enters line replacement to sampling line 30.In replacement process the first counter sample valve 51 in opened condition, to ensure that sample exists
Circulation displacement in pipeline.
3) hexachloro-silane is sampled.Open the valve of the first tail gas valve 41.Slow to open sample cock 32, sample enters sample
In bottle, sampling is finished, and sample cock 32, the 3rd sample introduction valve 23 and the first counter sample valve 51 are closed successively, sample bottle is taken
Under, change protection bottle and tighten.
4) high pure nitrogen purging displacement.Open the 3rd purging valve 13.The 3rd sample introduction valve 23 of slow opening carries out high-purity
Nitrogen is purged, and material blowback in feeding pipe is returned into system, and the first sample introduction valve 21, the second sample introduction valve 22, the are closed successively
Three sample introduction valves 23.Slow first counter sample valve 51 of opening carries out high pure nitrogen purging, and material blowback in pipeline is returned into system, according to
The 3rd counter sample valve 53 of secondary closing, the second counter sample valve 52 and the first counter sample valve 51.Slow sample cock 32 of opening is carried out
Material in high pure nitrogen purging sampling line 30.Keep the tail gas valve 41 of sample cock 32 and first normally opened, it is ensured that High Purity Nitrogen
Gas persistently purges protection sampler.
In above preferred embodiment, sample inlet system and sample bottle are carried out fully purging and replaced by high pure nitrogen, then
Nitrogen is closed, the exits and entrances valve of hexachloro-silane product is opened.After pipe-line system is sufficiently displaced from by hexachloro-silane, beat
Open the sampling of sample cock row.Sampling is finished, and closes sample cock.Nitrogen valve is finally opened, the liquid in pipe-line system is produced
Product blowback is returned after system, closes hexachloro-silane product exits and entrances valve.The advantage of the sampling method is：System is closed, high-purity
Without contamination, sample safe and environment-friendly.
Beneficial effects of the present invention are further illustrated with reference to specific embodiment.
Embodiment 1：
The hexachloro-silane that Luoyang polysilicon factory produces is carried out after closed on-line period, send laboratory to be detected.
As a result (it is shown in Table 1, table 2) compared with AIR LIQUIDE company standards, basically reaches production requirement.
Table 1：Defects inspecting result in embodiment 1
Table 2：Component testing result in embodiment 1
| Component | AIR LIQUIDE company standards | Embodiment 1 |
| Si2Cl6 | ＞ 99.7% | 99.99% |
| SiHCl3+SiCl4 | ＜ 0.2% | 0.01% |
Embodiment 2：
With DOW CORNING comparative analysis：Raw material is the hexachloro-silane that Luoyang polysilicon factory produces, hexachloro-silane content
More than 99%, after stable operation 15 days, two samples of A, B are sampled by the on-line period device of the present invention simultaneously, wherein A samples are sent
DOW CORNING detects that B samples send Luoyang polysilicon factory test in laboratory.Analysis result is shown in Table 3.
Table 3：With DOW CORNING comparative analysis result
| Component | A samples | B samples |
| Si2Cl6 | 99.86% | 99.88% |
| SiHCl3 | 0.003% | 0.005% |
| SiCl4 | 0.019% | 0.010% |
As can be seen from the above description, the above embodiments of the present invention realize following technique effect：By that will blow
Sweep pipeline, sampling line, protective container and tail gas pipeline to be sequentially communicated, and sampling line purged using scavenging pipeline,
So that impurity or aqueous vapor in sampling line etc. to be purged away, then by sample introduction pipeline, sampling line, sampling container and tail gas
Pipeline is sequentially communicated, and carries out on-line period using purged sampling line, eliminate impurity pollution and aqueous vapor etc. it is dangerous because
Element, and then realize the safe and accurate sampling to sample.
Further, protective container is replaced with into sampling container after the completion of sampling pipe purging, further sampling held
Device is purged, and impurity or aqueous vapor in sampling container etc. is purged away.Held using purged sampling line and sampling
Device carries out on-line period, further increases the accuracy and security of on-line period.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (10)
1. a kind of on-line period method, it is characterised in that the on-line period method is taken online by on-line period device
Sample, the on-line period device includes：Scavenging pipeline (10), sample introduction pipeline (20), sampling line (30), tail gas pipeline (40),
Protective container (33) and sampling container (31),
The on-line period method includes：
By the scavenging pipeline (10), the sampling line (30), the protective container (33) and the tail gas pipeline (40)
It is sequentially communicated, using the scavenging pipeline (10) to the sampling line (30), the protective container (33) and the tail gas
Pipeline (40) is purged；And
By the sample introduction pipeline (20), the sampling line (30), the sampling container (31) and the tail gas pipeline (40)
It is sequentially communicated, and on-line period is carried out using the purged sampling line (30) and the sampling container (31).
2. on-line period method according to claim 1, it is characterised in that after the purging is carried out, and carry out
Before the on-line period, the on-line period method also includes：
By the scavenging pipeline (10), the sampling line (30), the sampling container (31) and the tail gas pipeline (40)
It is sequentially communicated, the step of being purged using the scavenging pipeline (10) to the sampling container (31).
3. on-line period method according to claim 1, it is characterised in that described after the on-line period is carried out
On-line period method also includes：
The scavenging pipeline (10) is connected with the sample introduction pipeline (20), and to the residual sample in the sample introduction pipeline (20)
The step of carrying out blowback.
4. on-line period method according to claim 1, it is characterised in that described after the on-line period is carried out
On-line period method also includes：
By the scavenging pipeline (10), the sampling line (30), the protective container (33) and the tail gas pipeline (40)
It is sequentially communicated, and the residual sample in the sampling line (30) is purged into the step into the protective container (33).
5. on-line period method according to claim 1, it is characterised in that after the purging is carried out, and carry out
Before the on-line period, the on-line period method also includes：
The sample introduction pipeline (20), the sampling line (30) and counter sample pipeline (50) are sequentially communicated, and to the sampling
The step of pipeline (30) carries out sample displacement.
6. on-line period method according to claim 5, it is characterised in that described after the on-line period is carried out
On-line period method also includes：
The scavenging pipeline (10), the sampling line (30) and the counter sample pipeline (50) are sequentially communicated, and to described
The step of residual material in sampling line (30) and the counter sample pipeline (50) carries out blowback.
7. on-line period method according to claim 1, it is characterised in that the on-line period device is also set including cooling
Standby (60), the cooling device (60) is arranged on the sampling line (30), and is arranged on described take along Flow of Goods and Materials direction
The upstream of sample container (31), during the on-line period, the on-line period method also includes：
The sample that the sampling line (30) is delivered to the sample introduction pipeline (20) using the cooling device (60) carries out cold
But the step of.
8. on-line period method according to claim 1, it is characterised in that the scavenging pipeline (10) is also stopped including purging
Valve (14) is returned, after the purging is carried out, and before the progress on-line period, the on-line period method also includes closing
Close the step of purging check-valves (14) is to terminate purging.
9. on-line period method according to claim 1, it is characterised in that in the step of the purging, blowing medium
It is less than 3ppm high pure nitrogen or inert gas for water content.
10. on-line period method according to claim 1, it is characterised in that be additionally provided with the tail gas pipeline (40)
After tail gas check-valves (44), the on-line period, the on-line period method also includes closing the tail gas check-valves (44)
To prevent the step of tail gas enters the sampling container (31).
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| CN201710221910.6A CN107101850B (en) | 2017-04-06 | 2017-04-06 | Online sampling method |
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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 |
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| CN107101850B (en) | 2020-08-11 |
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