Background technology
The sample that many online gcs that are used for the liquid phase medium constituent analysis often run into sampling process stops up and band gas problem, so that the work that influence chromatographic operate as normal, particularly on-line chromatograph are analyzed.
Common former because: pipeline is thin, and resistance is big, and flow is little, and factor such as medium thickness often causes sampling to be interrupted in addition; Dissolved gases is separated out in the liquid, especially from the higher sampling spot sampling of pressure, (also is not difficult to fully) not fully when implementing gas-liquid separation, cause to be mingled with a large amount of bubbles in the sample by the back of reducing pressure.So produce a series of problems: the maintenance workload of chromatograph sample pretreatment is big, has increased operating cost; Because of being subjected to the influence that sample introduction is not ideal enough and pretreatment unit comparatively frequently keeps in repair, chromatographic effective run time obviously reduces, and the promptness of on-line analysis is poor; The chromatograph errors of analytical results is big, meeting in the sampling period that bubble enters, tested component displayed value in the circulation (being generally 10-15 minute) is obvious on the low side even be zero than actual value, and this kind situation even can in few cycles subsequently, continuously take place, cause on-line analysis that compositional data accurately can't be provided, can not satisfy the needs of explained hereafter and operation.
Above-mentioned sample stops up and band gas problem in order to solve, some measures have roughly the same been taked in different system supply commercial city, as strengthen pipeline path, add filtrator, adopt one-level or two-stage decompression, gas-liquid separation device and (see figure 1)s such as loop fast are set, but actually show that their effects are not good enough, particularly the gas enclosure problem is difficult to resolve especially and determines.
The utility model content
Technical problem to be solved in the utility model is to provide a kind of on-line chromatograph to analyze liquid phase medium preprocess device, to solve liquid phase medium gas enclosure problem in the on-line chromatograph analysis.
Technical problem to be solved in the utility model can be achieved through the following technical solutions:
The utility model discloses a kind of on-line chromatograph and analyze liquid phase medium preprocess device, comprise sampling pipe, connect the chromatograph pipeline, go discharge, pipeline to cut valve, it is characterized in that, comprise a standing separation jar, the top connects removes discharge, the upper end connects sampling pipe, and the lower end connects chromatograph by pipeline.
The utility model saves decompressor commonly used at present or relevant decompression member, gas-liquid separator and attached regulating device thereof.
In an embodiment, on-line chromatograph analysis liquid phase medium preprocess device disclosed in the utility model also connects the nitrogen pressure pipeline.
In one embodiment, on-line chromatograph disclosed in the utility model is analyzed liquid phase medium preprocess device, and the standing separation jar also has overflow vent, is connected to liquid return trough by pipeline.
In one embodiment, on-line chromatograph disclosed in the utility model is analyzed liquid phase medium preprocess device, and the standing separation pot bottom liquid evacuation port of also having a surplus is connected to liquid return trough by pipeline.
Embodiment
Below in conjunction with the specific embodiments and the drawings explanation, further illustrate the utility model.Should be understood that these embodiment only to be used to the utility model is described and be not used in the restriction scope of the present utility model.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.
A kind of stratographic analysis liquid phase medium preprocess device referring to Fig. 2, has 5 import and export on the standing separation jar, be equipped with six of A-F and cut valve, does switch motion by certain procedure, to reach big, the anti-blocking and basic purpose of eliminating bubble of flow.
Workflow of the present utility model: in a chromatographic cycle period, on the standing separation jar, successively finish sample and advance jar, leave standstill multiple working procedures such as the sample introduction of cooling down, pressurize, surplus liquid emptying, the switch situation according to the form below (table 1) of each valve is carried out during the per pass operation.
The switch situation of each valve of table 1.
|
Operation |
The A valve |
The B valve |
The C valve |
The D valve |
The E valve |
The F valve |
1 |
Sample advances jar |
√ |
× |
√ |
× |
√ |
× |
2 |
Leave standstill and cool down |
× |
× |
√ |
× |
√ |
× |
3 |
The pressurization sample introduction |
× |
√ |
× |
√ |
× |
× |
4 |
Surplus liquid emptying |
× |
× |
× |
√ |
× |
√ |
Annotate: " √ " expression valve is opened; " * " expression valve closes.
Advance a jar stage at sample, the A valve is opened, processing medium can through stopple coupon (41) through sample tap (12) directly to the standing separation jar (1) that has emptied in bigger flow injection liquid phase sample to be analyzed fast, do not handle and need not make expenditure and pressure, this can play good effect to preventing that pipeline from stopping up.Cause the canful phenomenon for fear of injecting excess liquid, ad hoc have overflow vent (13), in case when liquid level was higher than overflow vent (13), sample can overflow through E valve, run-down pipe (51), flows in the liquid return trough.
After enough samples are injected in separating tank (1) lining, shut the A valve, arrived and left standstill the stage of cooling down.At this moment contained gas is constantly separated out under the situation that leaves standstill near normal pressure in the sample, as long as give time enough, the gas that almost all is mingled with is all arranged to discharge (31) from gas port (11), gas main (2) the C valve through opening.
After leaving standstill the stage end of cooling down, C, E, F valve are all closed, and D, B valve are opened, and enter the pressurization sample introduction stage.After the D valve is opened, N
2Gas is through N
2Tracheae (21), gas main (2) enter separating tank (1) by gas port (11).After the B valve is opened, at N
2Under the pressure of gas, gas-liquid has been separated sufficient pure liquid phase sample and has been injected into chromatograph through outlet (14), feed tube (61).This needs (generally should suitably shift to an earlier date the several seconds so that the surplus liquid in the pipeline is got rid of) synchronously with the sample injection time point of chromatogram stream constantly.Select coupling reasonable continuous sample injection time, after guaranteeing that sample can enough satisfy stream analysis needs, can close the B valve and stop feed liquor.
The time length coupling in pressurization sample introduction stage rationally except for the assurance sample size satisfies the needs of analyzing stream, will guarantee that also the liquid in the standing separation jar is not cleared before next sample introduction, in order to avoid gas enters the chromatogram stream.Last procedure then is exactly surplus liquid emptying, promptly shuts the B valve, opens the F valve, at N
2Under the pressure of gas, remaining medium is cleared through surplus liquid evacuation port (15), discharging tube (71) in jar, flows in the liquid return trough, with the sample absolute " fresh " that guarantees that next circulation enters, overcomes the hysteresis and the error of analysis.But the debugging of the duration reference table 2 of each step, the size of the volume of each time period length and standing separation jar and associated line, valve etc. are relevant, can do concrete adjustment according to actual conditions.
The duration of each step of table 2.
|
Operation | Duration |
Remarks | |
1 |
Sample advances jar |
Recommend 3-10s
* |
Selected according to standing separation tank volume, sample size, sample introduction speed etc. |
2 |
Leave standstill and cool down |
Recommendation>60s
* |
Be provided with according to gas parsing situation under normal conditions in the liquid phase. |
3 |
The pressurization sample introduction |
Recommend 10-30s
* |
With the sample injection time is that benchmark suitably increases, can be by regulating N
2Air pressure is controlled.
|
4 |
Surplus liquid emptying |
Recommend 30-60s
* |
With clear jar is purpose, looks N
2Air pressure bottom discharge speed and deciding.
|
* |
Slack tank |
The chromatogram loop cycle time deducts the summation of above four times in step |
This moment all valve closings.If the purpose in this step is under the time prerequisite is cooled down in enough the leaving standstill of assurance, the thing sample advances jar and pressurizes the sample introduction stage around as far as possible, reduces analysis and lags behind, and this step can not establish yet.Leave standstill the time of cooling down by prolongation, realize with the chromatograph whole circulation time synchronously. |
*: do not limit herein, refer to exceed the recommendation time, but each step must there be a lower limit limit time and regular hour scope.
*: slack tank can not established, and sees its remarks for details.
Stratographic analysis liquid phase medium preprocess device of the present utility model can reach big, the anti-blocking and basic purpose of eliminating bubble of flow, and can also reduce investment outlay.Adopt the common decompression and the preprocess method of gas-liquid separation, input cost is higher, can save many expense relatively (annotate: some chromatograph has the logic programmable function concurrently, just can conveniently realize the logical relation of each valve shown in the table 1 by the configuration in the chromatograph and be equipped with this solution that the PLC program controller forms again with a standing separation jar and several transfer valve.Transfer valve adopt electronic, pneumatic all can, the concrete condition design when looking requirement of explosion proof and actual enforcement is selected for use).For convenience of description, the A-F valve in the present embodiment explanation is all listed by the through swtich valve, can adopt two-bit triplet merger some of them valve when implementing.
Should be understood that in addition those skilled in the art can make various changes or modifications the utility model after having read above-mentioned teachings of the present utility model, these equivalent form of values fall within the application's appended claims institute restricted portion equally.