CN111912694A - Liquid analysis device and method based on online dilution - Google Patents
Liquid analysis device and method based on online dilution Download PDFInfo
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- 239000007788 liquid Substances 0.000 title claims abstract description 201
- 238000004458 analytical method Methods 0.000 title claims abstract description 41
- 238000010790 dilution Methods 0.000 title claims abstract description 36
- 239000012895 dilution Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title abstract description 9
- 239000003085 diluting agent Substances 0.000 claims abstract description 16
- 238000002347 injection Methods 0.000 claims abstract description 7
- 239000007924 injection Substances 0.000 claims abstract description 7
- 238000004891 communication Methods 0.000 claims description 15
- 230000001105 regulatory effect Effects 0.000 claims description 9
- 230000003139 buffering effect Effects 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 description 21
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
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- 238000013507 mapping Methods 0.000 description 1
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- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
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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
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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Abstract
The present invention provides an online dilution-based liquid analysis apparatus and method, the online dilution-based liquid analysis apparatus including: the first valve has a plurality of ports; when the first valve is switched to sample injection, liquid to be detected passes through the first valve and the first liquid storage unit under the suction of the first pump; when the first valve is switched to be diluted, the second pump pushes the carrier liquid and the liquid to be detected in the first liquid storage unit, and the third pump pushes the diluent to sequentially enter the first conveying pipeline, the second valve and the second liquid storage unit through the first valve; the second valve has a plurality of ports; when the second valve is switched to be diluted, the second liquid storage unit receives liquid; when the second valve is switched to be used for conveying, gas enters the second valve, the second liquid storage unit, the second conveying pipeline, the third valve and the third liquid storage unit; the gas pipeline is communicated with the second valve; a second delivery conduit is disposed between the second valve and the third valve; the third valve has a plurality of ports; when the third valve is switched to delivery, the third liquid storage unit receives liquid; the liquid sensor is located downstream of the third liquid storage unit. The invention has the advantages of accurate dilution and the like.
Description
Technical Field
The present invention relates to liquid detection, and more particularly, to a liquid analyzer and method based on online dilution.
Background
In various production processes, such as semiconductor wafer production, non-ferrous metal industry smelting, pharmaceutical production process, environmental monitoring and other industries, the analysis of trace elements in materials is involved, and currently, these factories mainly rely on artificial sampling, dilution and then analysis by an analysis instrument, and the required samples are basically several milliliters.
There are also on-line real-time analyzers in the field of environmental monitoring, but the common practice is to use a pump to deliver water to a sample cell near the analyzer, which uses a large volume of liquid, and the analyzer draws a few milliliters through a capillary tube for analysis. In addition, too far a distance directly results in an extension of the time of transmission, so that such devices are usually built in the vicinity of the monitoring point.
In addition, in the processes of semiconductor wafer production, non-ferrous metal industry smelting, pharmaceutical factories and the like, samples with relatively complex matrixes such as strong acid, strong alkali, organic reagent and the like are usually adopted, and the samples usually need to be diluted to meet the detection requirement of an analytical instrument.
In most of the factories of semiconductor wafer production, non-ferrous metal industry smelting and pharmaceutical production, the area of the production factory is large, different process nodes are far apart, the factories can not provide a large amount of liquid for detection, some reagents are high (semiconductor industry), and the emission of excessive harmful solution is not allowed in consideration of environmental friendliness.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the liquid analysis device based on online dilution, which is accurate in dilution, capable of conveying liquid in a long distance, short in analysis time and automatic.
The purpose of the invention is realized by the following technical scheme:
an online dilution-based liquid analysis device, comprising:
a first valve and a first reservoir unit, the first valve having a plurality of ports; when the first valve is switched to sample injection, liquid to be detected passes through the first valve and the first liquid storage unit under the suction of the first pump; when the first valve is switched to be diluted, the second pump pushes the carrier liquid and the liquid to be detected in the first liquid storage unit, and the third pump pushes the diluent to sequentially enter the first conveying pipeline, the second valve and the second liquid storage unit through the first valve;
the second pump and the third pump are used for pumping liquid and pushing the liquid to move;
a second valve and a second reservoir unit, the second valve having a plurality of ports; when the second valve is switched to be diluted, the second liquid storage unit receives liquid; when the second valve is switched to be used for conveying, gas enters the second valve, the second liquid storage unit, the second conveying pipeline, the third valve and the third liquid storage unit;
a gas conduit in communication with the second valve;
a second delivery conduit having a length in excess of 10 meters and disposed between the second valve and the third valve;
a third valve and a third reservoir unit, the third valve having a plurality of ports; when the third valve is switched to delivery, the third liquid storage unit receives liquid; when the third valve is switched to analysis, the liquid in the third liquid storage unit is pushed out;
a liquid sensor downstream of the third reservoir unit.
The invention also aims to provide a liquid analysis method based on-line dilution by applying the liquid analysis device, and the aim of the invention is realized by the following technical scheme:
an online dilution-based liquid analysis method, comprising the steps of:
(A1) the first valve is switched to sample introduction, and liquid to be detected enters the first valve and the first liquid storage unit under the suction of the first pump;
(A2) the first valve and the second valve are switched to be diluted, the second pump pushes the carrier liquid to enter the first valve, the third pump pushes the diluent liquid to enter the first valve, the carrier liquid pushes the liquid to be detected and the diluent liquid in the first liquid storage unit to be mixed in the first conveying pipeline, and then the liquid enters the second valve and the second liquid storage unit; the second pump and the third pump work simultaneously;
(A3) the second valve and the third valve are switched to be used for conveying, the pressure-regulated gas enters the second valve, and liquid in the second liquid storage unit is pushed to enter the third valve and the third liquid storage unit through a second conveying pipeline, wherein the length of the second conveying pipeline exceeds 10 meters;
(A4) the third valve is switched to analysis, and the liquid in the third liquid storage unit is pushed out and analyzed.
Compared with the prior art, the invention has the beneficial effects that:
1. the injection pump is used for accurate control, so that accurate online dilution in the pipeline is realized, and the dilution problem of corrosive samples and volatile samples is solved;
the liquid is mixed in the transmission pipeline, so that online dilution is realized, a special mixing pool and a stirrer are not required, the volume of the device is reduced, and the cost is reduced;
2. the pressure of gas during transmission is accurately regulated, the relative uniform speed of the transmission speed is ensured not to be attenuated, liquid is not scattered due to instant pressure, the transmission of a milliliter-grade sample is realized, the rapid transmission of 1000m (less than 15 minutes) is realized, and the analysis time is shortened;
3. the functions of online dilution, remote transmission and the like are integrated, the automation of the pretreatment of the sample is realized, and the manual intervention is not needed.
Drawings
The disclosure of the present invention will become more readily understood with reference to the accompanying drawings. As is readily understood by those skilled in the art: these drawings are only for illustrating the technical solutions of the present invention and are not intended to limit the scope of the present invention. In the figure:
fig. 1 is a flowchart of a liquid analysis method based on online dilution according to example 1 of the present invention.
Detailed Description
Fig. 1 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and reproduce the invention. Some conventional aspects have been simplified or omitted for the purpose of teaching the present invention. Those skilled in the art will appreciate that variations or substitutions from these embodiments will be within the scope of the invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Thus, the present invention is not limited to the following alternative embodiments, but is only limited by the claims and their equivalents.
Example 1:
the online dilution-based liquid analysis device according to an embodiment of the present invention includes:
a first valve and a first reservoir unit, the first valve having a plurality of ports, such as a multi-way valve; when the first valve is switched to sample injection, the liquid to be detected passes through the first valve and the first liquid storage unit under the suction of a first pump such as a syringe pump; when the first valve is switched to be diluted, the second pump pushes the carrier liquid and the liquid to be detected in the first liquid storage unit, and the third pump pushes the diluent to sequentially enter the first conveying pipeline, the second valve and the second liquid storage unit through the first valve;
the second pump and the third pump are used for pumping liquid and pushing the liquid to move;
a second valve and a second reservoir unit, the second valve having a plurality of ports; when the second valve is switched to be diluted, the second liquid storage unit receives liquid; when the second valve is switched to be used for conveying, gas enters the second valve, the second liquid storage unit, the second conveying pipeline, the third valve and the third liquid storage unit;
a gas conduit in communication with the second valve;
a second delivery conduit having a length in excess of 10 meters and disposed between the second valve and the third valve;
a third valve and a third reservoir unit, the third valve having a plurality of ports; when the third valve is switched to delivery, the third liquid storage unit receives liquid; when the third valve is switched to analysis, the liquid in the third liquid storage unit is pushed out;
a liquid sensor, such as a liquid flow rate sensor, downstream of the third reservoir unit.
In order to improve the dilution accuracy and reduce the amount of liquid used, a syringe pump is further used as at least one of the first pump, the second pump, and the third pump.
In order to make the liquid transport at a uniform speed and prevent the transport speed from fluctuating, further, a pressure regulating unit and a pressure buffering unit are arranged on the gas pipeline.
In order to obtain the mapping relationship between the pressure and the flow rate in the second transmission pipeline, further, a plurality of liquid sensors, such as liquid flow rate sensors, are additionally arranged on the transmission pipeline.
Fig. 1 schematically shows a flow chart of an online dilution-based liquid analysis method according to an embodiment of the present invention, which includes the following steps, as shown in fig. 1:
(A1) the first valve is switched to sample introduction, and liquid to be detected enters the first valve and the first liquid storage unit under the suction of the first pump;
(A2) the first valve and the second valve are switched to be diluted, the second pump pushes the carrier liquid to enter the first valve, the third pump pushes the diluent liquid to enter the first valve, the carrier liquid pushes the liquid to be detected and the diluent liquid in the first liquid storage unit to be mixed in the first conveying pipeline, and then the liquid enters the second valve and the second liquid storage unit; the second pump and the third pump work simultaneously;
(A3) the second valve and the third valve are switched to be used for conveying, the pressure-regulated gas enters the second valve, and liquid in the second liquid storage unit is pushed to enter the third valve and the third liquid storage unit through a second conveying pipeline, wherein the length of the second conveying pipeline exceeds 10 meters;
(A4) the third valve is switched to analysis, and the liquid in the third liquid storage unit is pushed out and analyzed.
To achieve accurate in-line dilution, further, the second and third pumps simultaneously begin to push liquid into the first valve and end at the same time, with the ratio of the flow of diluent pushed by the third pump to the flow of carrier liquid pushed by the second pump being equal to the dilution ratio.
To switch the third valve accurately, further, when a liquid is detected downstream of the third reservoir unit, indicating that the third reservoir unit already has liquid, the third valve is switched to analyze.
In order to increase the liquid transport speed to shorten the overall analysis time, further, the pressure of the gas pipeline is adjusted so that the liquid in the second transport pipeline flows at a constant speed.
Example 2:
an application example of the liquid analysis apparatus and method based on online dilution according to embodiment 1 of the present invention.
In the application example, the first pump, the second pump and the third pump are all injection pumps, through switching, the first pump is selectively communicated with the first valve and the waste liquid pool, the second pump is selectively communicated with the first valve and the carrier liquid, and the third pump is selectively connected with the first valve and the diluent;
the first valve adopts two-position seven-way valve, and a plurality of ports are: the first port selectively communicates with the second port and the sixth port, the third port selectively communicates with the second port and the fourth port, the fifth port selectively communicates with the fourth port and the sixth port, and the common port selectively communicates with the second port and the third port; the first port is communicated with liquid to be detected, and two ends of the first liquid storage unit are communicated with the second port and the fifth port; the first pump is communicated with the sixth port, the second pump is communicated with the fourth port, the third pump is communicated with the third port, and the first conveying pipeline is communicated with the public port and the second valve;
the fourth valve adopts a two-position three-way valve and is used for enabling the first port to be selectively communicated with the liquid to be detected and the clean liquid;
the automatic pressure regulating valve, the pressure sensor and the pressure buffer ring are sequentially arranged on the gas pipeline;
the second valve adopts two-position six-way valve, and a plurality of ports are: the seventh port is in selective communication with the eighth port and the twelfth port, the ninth port is in selective communication with the eighth port and the tenth port, and the eleventh port is in selective communication with the tenth port and the twelfth port; the first conveying pipeline is communicated with the twelfth port, and two ends of the second liquid storage unit are communicated with the eighth port and the eleventh port;
the third valve adopts two-position six-way valve, and a plurality of ports are: the thirteenth port is in selective communication with the fourteenth port and the eighteenth port, the fifteenth port is in selective communication with the fourteenth port and the sixteenth port, and the seventeenth port is in selective communication with the sixteenth port and the eighteenth port; two ends of the third liquid storage unit are communicated with the fourteenth port and the seventeenth port;
the length of the second conveying pipeline is 1000 meters, and 1/16 inert PTFE pipes are adopted;
the liquid flow rate sensors are respectively arranged at the downstream of the third liquid storage unit and on the second transmission pipeline in sequence, and the fifteenth port is communicated with the liquid flow rate sensors.
In an embodiment of the present invention, a liquid analysis method based on online dilution, that is, a working method of a liquid analysis apparatus according to the present embodiment, includes the following steps:
(A1) the first valve is switched to sample injection, namely the first port is communicated with the second port, the third port is communicated with the fourth port, and the fifth port is communicated with the sixth port; under the suction of the first pump, the liquid to be detected sequentially passes through the fourth valve, the first valve and the first liquid storage unit;
(A2) the first valve and the second valve are switched to be diluted, namely the first port is communicated with the sixth port, the third port is communicated with the second port, and the fifth port is communicated with the fourth port; the seventh port is communicated with the eighth port, the ninth port is communicated with the tenth port, and the eleventh port is communicated with the twelfth port; the first pump pushes away surplus samples to the waste liquid pool, the second pump is communicated with the third pump and sucks carrier liquid and diluent at the same time, the pushing speeds of the second pump and the third pump are adjusted, so that the ratio of the flow of the diluent pushed by the third pump to the flow of the carrier liquid pushed by the second pump is equal to the dilution ratio, the second pump and the third pump simultaneously start to push the liquid to enter the first valve, and the process is finished;
mixing the liquid to be measured and the diluent in the first transmission pipeline, allowing the mixed liquid to enter the second liquid storage unit, and discharging the redundant liquid to be measured from the seventh port;
(A3) the second valve and the third valve are switched to delivery, namely the seventh port is communicated with the twelfth port, the eighth port is communicated with the ninth port, and the tenth port is communicated with the eleventh port; the thirteenth port is communicated with the eighteenth port, the fifteenth port is communicated with the fourteenth port, and the seventeenth port is communicated with the sixteenth port;
the pressure-regulated and pressure-buffered gas enters the second valve: adjusting gas pressure by using a pressure adjusting valve according to parameters detected by a liquid flow velocity sensor on a second transmission pipeline, pushing liquid in a second liquid storage unit to pass through the second transmission pipeline at a constant speed, and then entering a third valve and a third liquid storage unit, wherein the length of the second transmission pipeline exceeds 10 meters, specifically 1000 meters;
respectively arranging liquid flow velocity sensors at 100m, 200m, 300m, 400m, 500m, 600m, 700m, 800m, 900m and 1000m, manually adjusting the pressure to make the transmission time of each 100m consistent, recording the pressure value (P), and establishing P-P0enL(P<0.4Mpa) model, where n is related to the material and inner diameter of the pipeline, and n, P, is obtained by experiment according to the required pipeline0Is the initial pressure of the gas, such as the pressure of the gas as it enters the second valve, or the pressure of the gas before pressure regulation and pressure buffering; and L is the length of the second conveying pipeline. Considering the pressure resistance of the valve, Pmax is 0.4MPa, and when 0.4MPa is reached, the pressure is maintained for transmission.
Through experiments and observation of the transmission effect, the transmission speed is controlled to be 0.9-1.5 m/s, the transmission speed is too high, liquid in the pipeline is easy to break up, the transmission fails, and the efficiency is influenced by too low speed.
In actual application, only P needs to be given0And the length L, and then the P value is automatically regulated and controlled through the model, so that the transmission speed is optimal;
(A4) when the liquid flow rate sensor detects liquid, the third valve is switched to analysis, namely the thirteenth port is communicated with the fourteenth port, the fifteenth port is communicated with the sixteenth port, and the seventeenth port is communicated with the eighteenth port; the gas emptying pipeline is used for pushing the liquid to be tested diluted by the third liquid storage unit out and sending the liquid to be tested to the analysis under the pushing action of the liquid or gas;
(A5) switching the fourth valve and the first valve, namely, the clean liquid is communicated with the first port, the first port is communicated with the second port, the third port is communicated with the fourth port, and the fifth port is communicated with the sixth port;
under the suction of the first pump, clean liquid sequentially passes through the fourth valve, the first valve and the first liquid storage unit; the line is cleaned by means of the steps (A2) - (A3).
Claims (10)
1. An online dilution-based liquid analysis device, comprising:
a first valve and a first reservoir unit, the first valve having a plurality of ports; when the first valve is switched to sample injection, liquid to be detected passes through the first valve and the first liquid storage unit under the suction of the first pump; when the first valve is switched to be diluted, the second pump pushes the carrier liquid and the liquid to be detected in the first liquid storage unit, and the third pump pushes the diluent to sequentially enter the first conveying pipeline, the second valve and the second liquid storage unit through the first valve;
the second pump and the third pump are used for pumping liquid and pushing the liquid to move;
a second valve and a second reservoir unit, the second valve having a plurality of ports; when the second valve is switched to be diluted, the second liquid storage unit receives liquid; when the second valve is switched to be used for conveying, gas enters the second valve, the second liquid storage unit, the second conveying pipeline, the third valve and the third liquid storage unit;
a gas conduit in communication with the second valve;
a second delivery conduit having a length in excess of 10 meters and disposed between the second valve and the third valve;
a third valve and a third reservoir unit, the third valve having a plurality of ports; when the third valve is switched to delivery, the third liquid storage unit receives liquid; when the third valve is switched to analysis, the liquid in the third liquid storage unit is pushed out;
a liquid sensor downstream of the third reservoir unit.
2. The online dilution-based liquid analysis device according to claim 1, wherein: the plurality of ports of the first valve are: the first port selectively communicates with the second port and the sixth port, the third port selectively communicates with the second port and the fourth port, the fifth port selectively communicates with the fourth port and the sixth port, and the common port selectively communicates with the second port and the third port; the first port is communicated with liquid to be detected, and two ends of the first liquid storage unit are communicated with the second port and the fifth port; the first pump is communicated with the sixth port, the second pump is communicated with the fourth port, the third pump is communicated with the third port, and the first conveying pipeline is communicated with the public port and the second valve; alternatively, the first and second electrodes may be,
the plurality of ports of the second valve are: the seventh port is in selective communication with the eighth port and the twelfth port, the ninth port is in selective communication with the eighth port and the tenth port, and the eleventh port is in selective communication with the tenth port and the twelfth port; the first conveying pipeline is communicated with the twelfth port, and two ends of the second liquid storage unit are communicated with the eighth port and the eleventh port; alternatively, the first and second electrodes may be,
the plurality of ports of the third valve are: the thirteenth port is in selective communication with the fourteenth port and the eighteenth port, the fifteenth port is in selective communication with the fourteenth port and the sixteenth port, and the seventeenth port is in selective communication with the sixteenth port and the eighteenth port; and two ends of the third liquid storage unit are communicated with the fourteenth port and the seventeenth port.
3. The online dilution-based liquid analysis device according to claim 1, wherein: at least one of the first pump, the second pump, and the third pump uses a syringe pump.
4. The online dilution-based liquid analysis device according to claim 1, wherein: the pressure regulating unit and the pressure buffering unit are arranged on the gas pipeline.
5. The online dilution-based liquid analysis device according to claim 1, wherein: the conveying pipeline is additionally provided with a plurality of liquid sensors.
6. The online dilution-based liquid analysis device according to claim 1 or 5, wherein: the liquid sensor detects a liquid flow rate.
7. An online dilution-based liquid analysis method, comprising the steps of:
(A1) the first valve is switched to sample introduction, and liquid to be detected enters the first valve and the first liquid storage unit under the suction of the first pump;
(A2) the first valve and the second valve are switched to be diluted, the second pump pushes the carrier liquid to enter the first valve, the third pump pushes the diluent liquid to enter the first valve, the carrier liquid pushes the liquid to be detected and the diluent liquid in the first liquid storage unit to be mixed in the first conveying pipeline, and then the liquid enters the second valve and the second liquid storage unit; the second pump and the third pump work simultaneously;
(A3) the second valve and the third valve are switched to be used for conveying, the pressure-regulated gas enters the second valve, and liquid in the second liquid storage unit is pushed to enter the third valve and the third liquid storage unit through a second conveying pipeline, wherein the length of the second conveying pipeline exceeds 10 meters;
(A4) the third valve is switched to analysis, and the liquid in the third liquid storage unit is pushed out and analyzed.
8. The online dilution-based liquid analysis method according to claim 7, wherein: the second pump and the third pump simultaneously begin to push liquid into the first valve and end at the same time, and the ratio of the flow rate of the diluent pushed by the third pump to the flow rate of the carrier liquid pushed by the second pump is equal to the dilution ratio.
9. The online dilution-based liquid analysis method according to claim 7, wherein: when detecting liquid downstream of the third liquid storage unit, the third valve is switched to analysis.
10. The online dilution-based liquid analysis method according to claim 7, wherein: and adjusting the pressure of the gas pipeline to enable the liquid in the second conveying pipeline to flow at a constant speed.
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| CN202010682706.6A CN111912694A (en) | 2020-07-15 | 2020-07-15 | Liquid analysis device and method based on online dilution |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112834772A (en) * | 2020-12-31 | 2021-05-25 | 杭州谱育科技发展有限公司 | Trace element measuring device and method |
| CN117517696A (en) * | 2023-12-29 | 2024-02-06 | 杭州谱聚医疗科技有限公司 | System and sampling method for obtaining samples in situ on line |
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Application publication date: 20201110 |