Intelligent chromatograph with concentration judgment function

Abstract

The utility model discloses an intelligent chromatograph with a concentration judgment function. The intelligent chromatograph comprises: a concentration detection module, wherein the concentration detection module comprises a first switching valve, a first quantitative loop, a first detector and a first driving pump; the concentration adjusting module comprises a second switching valve, a third switching valve, a fourth switching valve, a mixer, a second quantitative loop, a second driving pump and a third driving pump, the second switching valve is at least provided with a second sample injection valve port and a second dilution valve port, and the mixer and the second driving pump are connected to the third switching valve; the second quantitative loop is connected to the fourth switching valve, the second switching valve is connected with the third switching valve, and the third switching valve and the third driving pump are connected with the fourth switching valve. The dilution ratio is automatically adjusted according to the sample concentration, and the sample and the diluent are fully mixed, so that the detection accuracy of the intelligent chromatograph with the concentration judgment function is improved.

Description

Technical Field

[0001] The utility model relates to the technical field of intelligent measuring instrument analyzers, in particular to an intelligent chromatograph with a concentration judgment function. Background Art

[0002] For accurate qualitative and quantitative detection and analysis of trace substances, chromatographic technology is used for processing. Taking an ion chromatograph as an example, before detection and analysis, the samples to be detected need to be pre-treated (filtered, water-soluble to remove organic matter, etc.), and then diluted so that the concentration of the sample is within the measurement range of the ion chromatograph before the sample can be input into the ion chromatograph for analysis. In the laboratory, operators are generally required to make an initial judgment on the concentration of unknown samples to be detected, and then manually dilute them and inject them into the ion chromatograph to analyze and observe the results. If the dilution factor is too large, there will be no peak or the peak area of ​​the peak is small, and it cannot be accurately judged and calculated; if the dilution factor is too small, the chromatographic column is overloaded and a flat peak appears, and the data is also invalid. For this reason, Chinese Patent Publication No. CN 108267356 A discloses a sample automatic dilution device, which uses a conductivity detector to check the concentration of the sample, and then dilutes the sample in a quantitative loop as needed.

[0003] However, in actual use, after the concentration to be tested is determined by the dilution multiple, the sample and diluent input into the quantitative loop according to the dilution multiple are mixed unevenly. This will also lead to inaccurate test data in the later stage. In view of this, how to design a technology that automatically adjusts the dilution multiple according to the sample concentration and achieves full mixing of the sample and the diluent to improve the detection accuracy is the technical problem to be solved by the utility model. Utility Model Content

[0004] The utility model provides an intelligent chromatograph with a concentration judgment function, which can automatically adjust the dilution multiple according to the sample concentration and fully mix the sample with the diluent, so as to improve the detection accuracy of the intelligent chromatograph with the concentration judgment function.

[0005] In order to achieve the above purpose, the utility model adopts the following technical solutions:

[0006] The utility model provides an intelligent chromatograph with a concentration judgment function, comprising:

[0007] A concentration detection module, the concentration detection module comprising a first switching valve, a first quantitative loop, a first detector and a first driving pump; the first switching valve has at least a first injection valve port and a first dilution valve port, the first quantitative loop is connected to the first switching valve, the first switching valve is also connected to the first detector or the first driving pump, and the first driving pump is connected to the first detector;

[0008] A concentration adjustment module, the concentration adjustment module comprising a second switching valve, a third switching valve, a fourth switching valve, a mixer, a second quantitative loop, a second driving pump and a third driving pump, the second switching valve having at least a second injection valve port and a second dilution valve port, the mixer and the second driving pump being connected to the third switching valve, the second quantitative loop being connected to the fourth switching valve, the second switching valve being connected to the third switching valve, and the third switching valve and the third driving pump being connected to the fourth switching valve respectively;

[0009] Wherein, the second dilution valve port is connected to the first switching valve;

[0010] The first switching valve is configured to switch the first quantitative loop to connect between the first injection valve port and the first detector, and to switch the first quantitative loop to connect between the first dilution valve port and the second dilution valve port;

[0011] The second switching valve is configured to switch the second injection valve port or the second dilution valve port to connect to the third switching valve;

[0012] The third switching valve is configured to switch the second driving pump to selectively connect to the second switching valve, the mixer or the fourth switching valve;

[0013] The fourth switching valve is configured to switch the second quantitative loop to connect to the third switching valve or the third driving pump.

[0014] Furthermore, it also includes a fifth switching valve, the fifth switching valve having at least a third injection valve port, the fifth switching valve being connected to the first injection valve port and the second injection valve port respectively;

[0015] The fifth switching valve is configured to switch the third injection valve port to connect to the first injection valve port or the second injection valve port.

[0016] Furthermore, it also includes a sixth switching valve, wherein the sixth switching valve is provided with at least a plurality of fourth injection valve ports, and the fourth injection valve ports are used to connect different sample containers;

[0017] The sixth switching valve is connected to the third injection valve port, and the sixth switching valve is configured to switch one of the fourth injection valve ports to be connected to the third injection valve port.

[0018] Furthermore, a sample pre-treatment device is provided between the sixth switching valve and the third injection valve port, and the sample pre-treatment device is configured to filter and / or remove organic matter from the sample flowing through.

[0019] Furthermore, it also includes a seventh switching valve, wherein the seventh switching valve is provided with at least a plurality of third dilution valve ports, and the third dilution valve ports are used to connect different dilution containers;

[0020] The seventh switching valve is connected to the first dilution valve port, and the seventh switching valve is configured to switch one of the third dilution valve ports to be connected to the first dilution valve port.

[0021] Furthermore, the second driving pump is a syringe pump.

[0022] Furthermore, the concentration adjustment module further includes a quantitative container, and the quantitative container is connected to the fourth switching valve;

[0023] The fourth switching valve is configured to switch the quantitative container to connect to the third switching valve or the third driving pump;

[0024] Wherein, the volume of the quantitative container is greater than the volume of the second quantitative ring.

[0025] Furthermore, it also includes a chromatographic analysis module, the chromatographic analysis module includes a separation column, a suppressor and a second detector connected in sequence, and the separation column is connected to the fourth switching valve;

[0026] The fourth switching valve is further configured to switch the second quantitative loop or the quantitative container to be connected between the third driving pump and the separation column.

[0027] Furthermore, the first detector and the second detector are conductivity detectors, and a suppressor is provided between the separation column and the second detector.

[0028] Furthermore, the first detector and the second detector are ultraviolet detectors.

[0029] The technical solution of the utility model has the following technical effects compared with the prior art: by detecting whether the concentration of the sample needs to be diluted in the concentration detection module, when the sample needs to be diluted, a quantitative diluent enters the first quantitative loop according to the dilution multiple and is connected to the sample to enter the third switching valve, and the second driving pump is used to make the diluent and the sample reciprocate between the second driving pump and the mixer to achieve sufficient mixing of the diluent and the sample, and the dilution multiple is automatically adjusted according to the sample concentration to achieve sufficient mixing of the sample and the diluent, so as to improve the detection accuracy of the intelligent chromatograph with concentration judgment function. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 This is one of the structural principle diagrams of an embodiment of the intelligent chromatograph with concentration judgment function of the utility model;

[0031] Figure 2This is the second structural principle diagram of an embodiment of the intelligent chromatograph with concentration judgment function of the utility model;

[0032] Figure 3 This is the third structural principle diagram of an embodiment of the intelligent chromatograph with concentration judgment function of the utility model;

[0033] Figure 4 This is the fourth structural principle diagram of an embodiment of the intelligent chromatograph with concentration judgment function of the utility model;

[0034] Figure 5 This is the fifth structural principle diagram of an embodiment of the intelligent chromatograph with concentration judgment function of the utility model.

[0035] Reference numerals:

[0036] 1. Concentration detection module; 11. First switching valve; 12. First quantitative loop; 13. First detector; 14. First driving pump; 15. pH detector; 16. Sample pretreatment device; 17. Fifth switching valve; 18. Sixth switching valve; 19. Seventh switching valve;

[0037] 2. Concentration adjustment module; 21. Second switching valve; 22. Third switching valve; 23. Fourth switching valve; 24. Mixer; 25. Second quantitative ring; 26. Second driving pump; 27. Third driving pump; 28. Quantitative container;

[0038] 3. Chromatographic analysis module; 31. Separation column; 32. Suppressor; 33. Second detector. DETAILED DESCRIPTION

[0039] like Figure 1-Figure 5 As shown, the utility model provides an intelligent chromatograph with a concentration judgment function, comprising:

[0040] A concentration detection module 1, the concentration detection module 1 comprises a first switching valve 11, a first quantitative ring 12, a first detector 13 and a first driving pump 14; the first switching valve 11 has at least a first injection valve port and a first dilution valve port, the first quantitative ring 12 is connected to the first switching valve 11, the first switching valve 11 is also connected to the first detector 13 or the first driving pump 14, and the first driving pump 14 is connected to the first detector 13;

[0041] A concentration adjustment module 2, wherein the concentration adjustment module 2 comprises a second switching valve 21, a third switching valve 22, a fourth switching valve 23, a mixer 24, a second quantitative ring 25, a second driving pump 26 and a third driving pump 27, wherein the second switching valve 21 has at least a second injection valve port and a second dilution valve port, the mixer 24 and the second driving pump 26 are connected to the third switching valve 22, the second quantitative ring 25 is connected to the fourth switching valve 23, the second switching valve 21 is connected to the third switching valve 22, and the third switching valve 22 and the third driving pump 27 are respectively connected to the fourth switching valve 23;

[0042] Wherein, the second dilution valve port is connected to the first switching valve 11;

[0043] The first switching valve 11 is configured to switch the first quantitative loop 12 to connect between the first injection valve port and the first detector 13, and to switch the first quantitative loop 12 to connect between the first dilution valve port and the second dilution valve port;

[0044] The second switching valve 21 is configured to switch the second injection valve port or the second dilution valve port to connect to the third switching valve 22;

[0045] The third switching valve 22 is configured to switch the second driving pump 26 to selectively connect to the second switching valve 21, the mixer 24 or the fourth switching valve 23;

[0046] The fourth switching valve 23 is configured to switch the second quantitative ring 25 to be connected to the third switching valve 22 or the third driving pump 27 .

[0047] Specifically, under the action of the first driving pump 14 , the concentration detection module 1 inputs the sample through the first injection valve port of the first switching valve 11 . After the sample enters the first switching valve 11 , it is output through the first quantitative ring 12 and flows into the first detector 13 .

[0048] The first detector 13 may be a conductivity detector (e.g. Figure 1 , Figure 2 Neutralization Figure 4 The first detector 13 in the embodiment) or the ultraviolet detector (such as Figure 3 and Figure 5The first detector 13 in the embodiment of the present invention is a representative entity of the first detector 13); wherein the conductivity detector can be used for ion chromatography detection, and the ultraviolet detector is used for liquid chromatography detection. According to the detection value of the sample detected by the first detector 13, it can be inferred whether the concentration of the sample is within the detection range. The specific method of using the conductivity detector and the ultraviolet detector to detect the detection value of the sample to determine the sample concentration and calculate the dilution multiple can be referred to in conventional technology, such as the record of CN 108267356 A, and will not be limited or repeated here.

[0049] Taking the first detector 13 as an example, the conductivity value of the sample is detected by the first detector 13. According to the detected conductivity value, it can be determined whether the sample needs to be diluted and the required dilution factor, thereby judging whether the concentration of the sample is appropriate or too high.

[0050] When the sample does not need to be diluted and the concentration of the sample is within the detection range, under the action of the second driving pump 26, the sample will enter the second switching valve 21 through the second injection valve port and be transported to the third switching valve 22. After the third switching valve 22 switches the flow path, the second driving pump 26 transports the sample entering the third switching valve 22 to the fourth switching valve 23 and flows into the second quantitative loop 25, so as to obtain a quantitative sample through the second quantitative loop 25. Then, under the action of the third driving pump 27, the eluent is transported to the fourth switching valve 23 and enters the second quantitative loop 25, and the eluent outputs the sample in the second quantitative loop 25 to the outside of the fourth switching valve 23 for ion chromatography analysis.

[0051] If the concentration of the sample is too high and exceeds the measured concentration range, the sample needs to be diluted. Under the action of the second driving pump 26, for the sample in the first quantitative ring 12, a diluent corresponding to the dilution multiple is transported to the first switching valve 11, and the diluent outputs the sample in the first quantitative ring 12 from the first switching valve 11 and flows into the second dilution valve port of the second switching valve 21, and the sample and the diluent are output from the second switching valve 21 and flow into the third switching valve 22. The third switching valve 22 switches the flow path so that the sample and the diluent flow back and forth between the second driving pump 26 and the mixer 24, thereby fully mixing the sample and the diluent. After uniform mixing, the diluted sample is output from the third switching valve 22 and transported to the fourth switching valve 23 under the action of the second driving pump 26, and the diluted sample flows into the second quantitative ring 25 connected to the fourth switching valve 23 to obtain a quantitative diluted sample through the second quantitative ring 25. Then, under the action of the third driving pump 27, the eluent is delivered to the fourth switching valve 23 and enters the second quantitative loop 25, and the eluent outputs the diluted sample in the second quantitative loop 25 to the outside of the fourth switching valve 23 for ion chromatography analysis.

[0052] The second driving pump 26 may be a syringe pump, which can be used to inject the diluent and the sample into the mixer 24 and then extract them from the mixer 24, and repeat this process for multiple times to achieve uniform mixing.

[0053] In order to realize automatic control, a controller (not shown) can also be configured, and the controller is electrically connected to the first switching valve 11, the second switching valve 21, the third switching valve 22, the fourth switching valve 23, the first detector 13, the first driving pump 14, the second driving pump 26 and the third driving pump 27 respectively.

[0054] Specifically, the controller may be a conventional device with communication control function, such as a single chip microcomputer, a CPU, or a PLC or other control module. The specific entity of the controller and its specific control process are not limited or elaborated here.

[0055] Furthermore, it also includes a fifth switching valve 17, which has at least a third injection valve port, and the fifth switching valve 17 is connected to the first injection valve port and the second injection valve port respectively; the fifth switching valve 17 is configured to switch the third injection valve port to connect to the first injection valve port or the second injection valve port.

[0056] Specifically, the third injection valve port of the fifth switching valve 17 is used to directly or indirectly connect to an external container for holding samples, and the sample enters the fifth switching valve 17 through the third injection valve port, so as to control the sample to enter the first switching valve 11 or the second switching valve 21 through the fifth switching valve 17.

[0057] Furthermore, it further comprises a sixth switching valve 18, wherein the sixth switching valve 18 is provided with at least a plurality of fourth injection valve ports, and the fourth injection valve ports are used to connect different sample containers;

[0058] The sixth switching valve 18 is connected to the third injection valve port, and the sixth switching valve 18 is configured to switch one of the fourth injection valve ports to be connected to the third injection valve port.

[0059] Specifically, when multiple samples need to be automatically analyzed, multiple containers containing samples can be first connected to the sixth switching valve 18 , and then the corresponding sample containers can be selectively connected to the fifth switching valve 17 through the sixth switching valve 18 .

[0060] Furthermore, a sample pre-treatment device 16 is provided between the sixth switching valve 18 and the third injection valve port, and the sample pre-treatment device is configured to filter and / or remove organic matter from the sample flowing through.

[0061] Specifically, the sample may be pre-treated by a sample pre-treatment device, and the pre-treatment method may include at least filtering and / or removing organic matter. As for the specific entity of the sample pre-treatment device, the pre-treatment device 16 used in the ion chromatography analysis process in the prior art may be adopted, and the specific entity of the sample pre-treatment device is not limited here.

[0062] Furthermore, it further comprises a seventh switching valve 19, wherein the seventh switching valve 19 is provided with at least a plurality of third dilution valve ports, and the third dilution valve ports are used to connect different dilution containers;

[0063] The seventh switching valve 19 is connected to the first dilution valve port, and the seventh switching valve 19 is configured to switch one of the third dilution valve ports to be connected to the first dilution valve port.

[0064] Specifically, the seventh switching valve 19 can be connected to a plurality of containers containing diluents to meet the dilution requirements of different samples.

[0065] Furthermore, the concentration adjustment module 2 further includes a quantitative container 28, and the quantitative container 28 is connected to the fourth switching valve 23;

[0066] The fourth switching valve 23 is configured to switch the quantitative container to connect to the third switching valve 22 or the third driving pump 27;

[0067] The volume of the quantitative container 28 is greater than the volume of the second quantitative ring 25 .

[0068] Specifically, in actual use, there is a situation where the concentration of the sample is too low and exceeds the sample concentration detection range. Since the sample concentration is too low to be concentrated, in order to meet the detection requirements of samples with too low concentration, a larger quantitative container 28 (such as a longer quantitative ring or concentration column, etc.) can be configured on the fourth switching valve 23.

[0069] In this way, when the concentration of the sample detected by the concentration detection module 1 is lower than the set concentration detection range, the fourth switching valve 23 switches the quantitative container 28 to participate in the work, which is similar to the process where the sample does not need to be diluted.

[0070] That is, when the concentration of the sample is lower than the detection range, under the action of the second driving pump 26, the sample will enter the second switching valve 21 through the second injection valve port and be transported to the third switching valve 22. After the third switching valve 22 performs the reversal of the flow path, the second driving pump 26 will transport the sample entering the third switching valve 22 to the fourth switching valve 23 and flow into the quantitative container 28, so as to obtain a sufficient amount of sample through the quantitative container 28. Due to the large total amount of the sample, when a large amount of the sample is output from the fourth switching valve 23 under the action of the third driving pump 27 for ion chromatography analysis, although the concentration of the sample is low, the sufficient amount of the sample makes the total amount of the substance to be detected meet the detection requirements, thereby meeting the detection requirements of the sample with too low concentration, and more effectively broadening the scope of application of the intelligent chromatograph, and the degree of intelligence is higher.

[0071] Figure 1-Figure 3 The third switching valve in the embodiment may be composed of two valves, namely, a two-position three-way valve 221 and a multi-way reversing valve 222; or, Figure 4-Figure 5 The third switching valve in is a multi-way reversing valve.

[0072] Figure 1-Figure 5 The first switching valve is a two-position six-way valve, the sixth switching valve and the seventh switching valve are multi-turn one-way valves, the second reversing valve and the fifth reversing valve are two-position three-way valves, and the fourth switching valve is a two-position ten-way valve. Here, there is no restriction on the specific manifestation entities of the above switching valves.

[0073] Based on the above technical solution, optionally, the intelligent chromatograph further includes a chromatographic analysis module 3, wherein the chromatographic analysis module 3 includes a separation column 31 and a second detector 33 connected together, and the separation column 31 is connected to the fourth switching valve 23;

[0074] The fourth switching valve 23 is further configured to switch the second quantitative ring 25 or the quantitative container to be connected between the third driving pump 27 and the separation column 31 .

[0075] Specifically, the sample output from the fourth switching valve 23 or the diluted sample is input into the separation column 31 and then enters into the second detector 33, and then conventional chromatographic analysis is performed.

[0076] Among them, the first detector 13 and the second detector 33 are the same detector type, for example: the first detector 13 and the second detector 33 are conductivity detectors, then ion chromatography analysis can be performed; or the first detector 13 and the second detector 33 are ultraviolet detectors, then liquid chromatography analysis can be performed.

[0077] In addition, when using a conductivity detector, Figure 2 and 4As shown, a pH detector 15 may also be included, and the pH detector 15 is connected between the first detector 13 and the first driving pump 14. Similarly, a suppressor 32 may be provided between the separation column 31 and the second detector 33.

[0078] The technical solution of the utility model has the following technical effects compared with the prior art: by detecting whether the concentration of the sample needs to be diluted in the concentration detection module, when the sample needs to be diluted, a quantitative diluent enters the first quantitative loop according to the dilution multiple and is connected to the sample to enter the third switching valve, and the second driving pump is used to make the diluent and the sample reciprocate between the second driving pump and the mixer to achieve sufficient mixing of the diluent and the sample, and the dilution multiple is automatically adjusted according to the sample concentration to achieve sufficient mixing of the sample and the diluent, so as to improve the detection accuracy of the intelligent chromatograph with concentration judgment function.

[0079] The above is only a specific implementation of the utility model, but the protection scope of the utility model is not limited to this. Any changes or substitutions that can be easily thought of by technicians familiar with the technical field within the technical scope disclosed by the utility model should be included in the protection scope of the utility model. Therefore, the protection scope of the utility model should be based on the protection scope of the claims.

Claims

1. An intelligent chromatograph with concentration judgment function, characterized in that: include: A concentration detection module, the concentration detection module comprising a first switching valve, a first quantitative ring, a first detector and a first driving pump; The first switching valve has at least a first injection valve port and a first dilution valve port, the first quantitative loop is connected to the first switching valve, the first switching valve is also connected to the first detector or the first driving pump, and the first driving pump is connected to the first detector; A concentration adjustment module, the concentration adjustment module comprising a second switching valve, a third switching valve, a fourth switching valve, a mixer, a second quantitative loop, a second driving pump and a third driving pump, the second switching valve having at least a second injection valve port and a second dilution valve port, the mixer and the second driving pump being connected to the third switching valve, the second quantitative loop being connected to the fourth switching valve, the second switching valve being connected to the third switching valve, and the third switching valve and the third driving pump being connected to the fourth switching valve respectively; Wherein, the second dilution valve port is connected to the first switching valve; The first switching valve is configured to switch the first quantitative loop to connect between the first injection valve port and the first detector, and to switch the first quantitative loop to connect between the first dilution valve port and the second dilution valve port; The second switching valve is configured to switch the second injection valve port or the second dilution valve port to connect to the third switching valve; The third switching valve is configured to switch the second driving pump to selectively connect to the second switching valve, the mixer or the fourth switching valve; The fourth switching valve is configured to switch the second quantitative loop to connect to the third switching valve or the third driving pump.

2. The intelligent chromatograph with concentration judgment function according to claim 1, characterized in that: It also includes a fifth switching valve, the fifth switching valve having at least a third injection valve port, and the fifth switching valve is connected to the first injection valve port and the second injection valve port respectively; The fifth switching valve is configured to switch the third injection valve port to connect to the first injection valve port or the second injection valve port.

3. The intelligent chromatograph with concentration judgment function according to claim 2, characterized in that: It also includes a sixth switching valve, wherein the sixth switching valve is provided with at least a plurality of fourth injection valve ports, and the fourth injection valve ports are used to connect different sample containers; The sixth switching valve is connected to the third injection valve port, and the sixth switching valve is configured to switch one of the fourth injection valve ports to be connected to the third injection valve port.

4. The intelligent chromatograph with concentration judgment function according to claim 3, characterized in that: A sample pre-treatment device is also provided between the sixth switching valve and the third injection valve port, and the sample pre-treatment device is configured to filter and / or remove organic matter from the sample flowing through.

5. The intelligent chromatograph with concentration judgment function according to claim 1, characterized in that: It also includes a seventh switching valve, wherein the seventh switching valve is provided with at least a plurality of third dilution valve ports, and the third dilution valve ports are used to connect different dilution containers; The seventh switching valve is connected to the first dilution valve port, and the seventh switching valve is configured to switch one of the third dilution valve ports to be connected to the first dilution valve port.

6. The intelligent chromatograph with concentration judgment function according to claim 1, characterized in that: The second driving pump is a syringe pump.

7. The intelligent chromatograph with concentration judgment function according to any one of claims 1 to 6, characterized in that: The concentration adjustment module further includes a quantitative container, and the quantitative container is connected to the fourth switching valve; The fourth switching valve is configured to switch the quantitative container to connect to the third switching valve or the third driving pump; Wherein, the volume of the quantitative container is greater than the volume of the second quantitative ring.

8. The intelligent chromatograph with concentration judgment function according to claim 7, characterized in that: Also includes a chromatographic analysis module, the chromatographic analysis module includes a separation column and a second detector connected together, the separation column is connected to the fourth switching valve; The fourth switching valve is further configured to switch the second quantitative loop or the quantitative container to be connected between the third driving pump and the separation column.

9. The intelligent chromatograph with concentration judgment function according to claim 8, characterized in that: The first detector and the second detector are conductivity detectors, and a suppressor is arranged between the separation column and the second detector.

10. The intelligent chromatograph with concentration judgment function according to claim 8, characterized in that: The first detector and the second detector are ultraviolet detectors.

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