A waste liquid treatment device of a liquid chromatograph-mass spectrometer

Abstract

This utility model discloses a waste liquid treatment device for a liquid chromatography-mass spectrometry (LC-MS) instrument, relating to the field of LC-MS instruments. It includes an outlet pipe connected to the waste liquid port of the LC-MS instrument, with the other end of the outlet pipe connected to a converter head. The converter head has three outlets connected to a chromatographic waste liquid tank, a mass spectrometry waste liquid tank, and a clear waste liquid tank, respectively. A cross-shaped converter head separates the mobile phase waste liquid generated by the liquid chromatography unit, the high-salt matrix waste liquid generated at the mass spectrometer interface, and the waste liquid generated during instrument cleaning into independent collection tanks. This avoids the risks of chemical reactions, heat generation, gas generation, and even explosions that may occur when waste liquids of different properties are mixed. Furthermore, it lays the foundation for subsequent professional and low-cost treatment. The classified waste liquid can be treated according to its specific properties, with treatment costs far lower than mixed hazardous waste, while also facilitating the recovery and purification of valuable solvents.

Description

Technical Field

[0001] This utility model relates to the field of chromatography-mass spectrometry devices, specifically to a waste liquid treatment device for a liquid chromatography-mass spectrometry instrument. Background Technology

[0002] Liquid chromatography-mass spectrometry (LC-MS) generates various waste liquids with complex compositions and varying hazards during operation, mainly including:

[0003] Chromatographic waste liquid: originates from the liquid chromatography unit and contains a large amount of organic solvents, buffer salts, and separated analytes.

[0004] Mass spectrometry waste liquid: mainly comes from the vacuum system interface of the mass spectrometer. It is a mixture of unseparated sample and mobile phase, usually containing high concentrations of matrix and salt, which is prone to crystallization and precipitation that can clog the pipeline.

[0005] Cleaning waste liquid: from the instrument's automatic cleaning system, containing a high concentration of organic solvents.

[0006] Currently, the common practice in laboratories is to pipe all waste liquids into a single waste container. This method has serious drawbacks:

[0007] Significant safety hazards: When waste liquids of different properties (such as acids, alkalis, and organic solvents) are mixed in a single container, chemical reactions may occur, generating heat, pressure, or toxic gases, posing risks of combustion, explosion, or poisoning.

[0008] High subsequent treatment costs: Mixed waste liquid is considered the most hazardous waste, and the treatment cost is extremely expensive. If the waste liquid contains high concentrations of salt and organic solvents, the treatment is even more difficult. Summary of the Invention

[0009] The technical problem to be solved by this utility model is to provide a waste liquid treatment device for a liquid chromatography-mass spectrometry instrument, which is highly safe and has low subsequent treatment costs, in order to address the shortcomings of the existing technology.

[0010] To solve the above-mentioned technical problems, the technical solution of this utility model is as follows:

[0011] A waste liquid treatment device for a liquid chromatography-mass spectrometry (LC-MS) instrument includes an outlet pipe connected to the waste liquid port of the LC-MS instrument, the other end of the outlet pipe being connected to the inlet of a cross-shaped converter head, and the three outlets of the converter head being respectively connected to a chromatographic waste liquid tank, a mass spectrometry waste liquid tank, and a clear liquid waste liquid tank via pipes.

[0012] As an improved technical solution, it also includes a central control unit that is connected to the liquid chromatography-mass spectrometry instrument. The inlet pipes of the chromatographic waste tank, the mass spectrometry waste tank and the clear liquid waste tank are respectively equipped with a first solenoid valve, a second solenoid valve and a third solenoid valve, which are electrically connected to the central control unit.

[0013] As an improved technical solution, the outlet pipe is equipped with a conductivity sensor, and the outlet pipe is connected to a pretreatment agent storage tank via a metering pump at the lower end of the conductivity sensor. The conductivity sensor and the metering pump are respectively electrically connected to the central control unit.

[0014] As an improved technical solution, the chromatographic waste liquid tank is provided with two parallel tanks, and the inlets of the two chromatographic waste liquid tanks are respectively provided with a fourth solenoid valve and a fifth solenoid valve. The two chromatographic waste liquid tanks are respectively provided with a first liquid level sensor and a second liquid level sensor. The fourth solenoid valve, the fifth solenoid valve, the first liquid level sensor and the second liquid level sensor are respectively electrically connected to the central control unit.

[0015] As an improved technical solution, the mass spectrometry waste liquid tank is provided with two parallel tanks, and the inlet of the two mass spectrometry waste liquid tanks is respectively provided with a sixth solenoid valve and a seventh solenoid valve. The two mass spectrometry waste liquid tanks are respectively provided with a third liquid level sensor and a fourth liquid level sensor. The sixth solenoid valve, the seventh solenoid valve, the third liquid level sensor and the fourth liquid level sensor are respectively electrically connected to the central control unit.

[0016] As an improved technical solution, the clear liquid waste tank is provided in two parallel configurations. The inlets of the two clear liquid waste tanks are respectively equipped with an eighth solenoid valve and a ninth solenoid valve. The two clear liquid waste tanks are respectively equipped with a fifth liquid level sensor and a sixth liquid level sensor. The eighth solenoid valve, the ninth solenoid valve, the fifth liquid level sensor, and the sixth liquid level sensor are respectively electrically connected to the central control unit.

[0017] As a preferred technical solution, the end of the outlet pipe is connected to a buffer tank, and the outlet of the buffer tank is connected to the converter head through a pipe.

[0018] Due to the adoption of the above technical solution, the beneficial effects of this utility model are:

[0019] This invention discloses a waste liquid treatment device for a liquid chromatography-mass spectrometry (LC-MS) instrument. The device includes an outlet pipe connected to the waste liquid port of the LC-MS instrument, and the other end of the outlet pipe connected to the inlet of a cross-shaped converter head. The three outlets of the converter head are respectively connected via pipes to a chromatographic waste liquid tank, a mass spectrometry waste liquid tank, and a clear waste liquid tank. Through a cross-shaped converter head, the mobile phase waste liquid (chromatographic waste liquid) generated by the liquid chromatography unit, the high-salt matrix waste liquid (mass spectrometry waste liquid) generated at the mass spectrometer interface, and the waste liquid (clear waste liquid) generated during instrument cleaning are separately introduced into independent collection tanks. This significantly reduces safety risks by avoiding the potential chemical reactions, heat generation, gas generation, or even explosion hazards that may occur when waste liquids of different properties (such as strong acids, strong organic solvents, and high-salt solutions) are mixed. Secondly, it lays the foundation for subsequent professional and low-cost treatment. The classified waste liquids can be treated according to their specific properties, resulting in treatment costs far lower than mixed hazardous waste. It also facilitates the recovery and purification of valuable solvents (such as acetonitrile and methanol).

[0020] This invention also includes a central control unit connected to the liquid chromatography-mass spectrometry (LC-MS) instrument. A first solenoid valve, a second solenoid valve, and a third solenoid valve are respectively installed on the inlet pipes of the chromatographic waste tank, the mass spectrometry waste tank, and the clear waste tank. These three solenoid valves are electrically connected to the central control unit. The central control unit receives operating status signals from the LC-MS instrument host (such as chromatography start / end, mass spectrometry ionization source switch, and cleaning program start / stop), and precisely controls the opening and closing of the corresponding solenoid valves accordingly. This ensures that the waste liquid separation action is completely synchronized with the instrument's operating status, achieving fully automatic and accurate classification without manual intervention, eliminating classification errors caused by human judgment mistakes or operational delays. This not only greatly reduces the burden on operators but also improves the reliability of classification and the automation level of the entire system, ensuring the traceability of experimental data.

[0021] The outlet pipe is equipped with a conductivity sensor. Below the conductivity sensor, the outlet pipe is connected to a pretreatment agent storage tank via a metering pump. Both the conductivity sensor and the metering pump are electrically connected to the central control unit. The conductivity sensor monitors the ion concentration (salt content) of the waste liquid in real time. When a high conductivity signal is detected (indicating that mass spectrometry waste liquid is being discharged and the salt content is extremely high), the central control unit immediately activates the metering pump to precisely inject a measured amount of diluent (such as pure water) into the waste liquid pipeline. This achieves instant online dilution of high-salt waste liquid, effectively preventing salt crystallization at the source, thus avoiding clogging of the expensive mass spectrometer vacuum pump discharge pipeline, protecting core equipment, and reducing costly maintenance costs and downtime. This is a proactive, preventative protective measure.

[0022] The chromatographic waste liquid tanks are arranged side by side. The inlets of the two tanks are respectively equipped with a fourth solenoid valve and a fifth solenoid valve. The two tanks are each equipped with a first level sensor and a second level sensor. The fourth and fifth solenoid valves, the first and second level sensors are electrically connected to the central control unit. The two parallel tanks, each with its own solenoid valve and level sensor, allow for intelligent "one in use, one on standby" management. When the central control unit detects that tank A is nearly full via the level sensor, it automatically switches the solenoid valve to guide the waste liquid to the empty tank B for continued collection, while simultaneously issuing an alarm indicating that tank A needs to be replaced. This achieves "hot switching" of waste liquid collection, ensuring that during long-term sequence analysis or large-volume sample testing, the waste liquid tank can be replaced without interrupting the liquid chromatography-mass spectrometry (LC-MS) instrument, greatly improving the overall work efficiency of the laboratory and the continuous operation capability of the equipment.

[0023] The mass spectrometry waste liquid tanks are arranged side by side. The inlets of the two tanks are respectively equipped with a sixth and a seventh solenoid valve. The tanks are also equipped with a third and a fourth level sensor, respectively. These six solenoid valves, the seventh solenoid valve, the third level sensor, and the fourth level sensor are electrically connected to the central control unit. Mass spectrometry waste liquid typically contains high concentrations of matrix and salt, requiring more frequent replacement. The dual-tank design ensures continuous collection. More importantly, this design provides redundancy for the safe management of high-risk waste liquids. When one tank is full and sealed for disposal, the other tank can be immediately put into use, reducing the time a full tank remains in the laboratory and lowering safety risks. Simultaneously, it facilitates the separate storage of high-risk waste liquids from different projects or with different characteristics, enabling more refined management.

[0024] The cleaning waste liquid tanks are arranged side-by-side. The inlets of the two tanks are respectively equipped with an eighth and a ninth solenoid valve. The tanks are also equipped with a fifth and a sixth level sensor, respectively. The eighth and ninth solenoid valves, the fifth and sixth level sensors, are electrically connected to the central control unit. The cleaning waste liquid typically contains a high concentration of organic solvents and has high recycling value. The dual-tank design enables continuous collection, ensuring that the instrument's automatic cleaning program will not be interrupted or trigger an alarm due to a full waste liquid tank, thus guaranteeing proper instrument maintenance and standby status.

[0025] The outlet pipe is connected to a buffer tank, and the outlet of the buffer tank is connected to the switching head via a pipe. Waste liquid outflow is not always stable and continuous; there may be pulses or instantaneous large-flow discharges (especially at the end of a gradient or when switching valves). The buffer tank, as a small intermediate container, can smooth out these fluctuations in flow and pressure, providing a more stable detection environment for the downstream conductivity sensor and improving measurement accuracy. Simultaneously, it also prevents the liquid flow from directly impacting the liquid path switching within the switching head, making fluid switching smoother, reducing potential splashing or mixing, further ensuring the purity of the classification, and extending the service life of components such as solenoid valves. Attached Figure Description

[0026] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0027] Figure 1 This is a structural schematic diagram of an embodiment of the present utility model;

[0028] Figure 2 yes Figure 1 Schematic diagram of the intermediate converter head;

[0029] The system includes: 1. Liquid Chromatography-Mass Spectrometry (LC-MS) instrument; 2. Discharge tube; 3. Converter head; 4. Chromatographic waste tank; 5. Mass spectrometry waste tank; 6. Clear liquid waste tank; 7. Central control unit; 8. First solenoid valve; 9. Second solenoid valve; 10. Third solenoid valve; 11. Conductivity sensor; 12. Metering pump; 13. Pretreatment agent storage tank; 14. Fourth solenoid valve; 15. Fifth solenoid valve; 16. First level sensor; 17. Second level sensor; 18. Sixth solenoid valve; 19. Seventh solenoid valve; 20. Third level sensor; 21. Fourth level sensor; 22. Eighth solenoid valve; 23. Ninth solenoid valve; 24. Fifth level sensor; 25. Sixth level sensor; 26. Buffer tank. Detailed Implementation

[0030] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0031] like Figure 1-2As shown, a waste liquid treatment device for a liquid chromatography-mass spectrometry (LC-MS) instrument includes an outlet pipe 2 connected to the waste liquid port of the LC-MS 1 instrument. The other end of the outlet pipe 2 is connected to the inlet of a cross-shaped converter head 3. The three outlets of the converter head 3 are respectively connected to a chromatographic waste liquid tank 4, a mass spectrometry waste liquid tank 5, and a clear waste liquid tank 6 via pipes. The mobile phase waste liquid (chromatographic waste liquid) generated by the liquid chromatography unit, the high-salt matrix waste liquid (mass spectrometry waste liquid) generated at the mass spectrometer interface, and the waste liquid (clear waste liquid) generated during instrument cleaning are respectively introduced into independent collection tanks through a cross-shaped converter head 3. This significantly reduces safety risks by avoiding the chemical reactions, heat generation, gas generation, and even explosion hazards that may occur when waste liquids of different properties (such as strong acids, strong organic solvents, and high-salt solutions) are mixed. Secondly, it lays the foundation for subsequent professional and low-cost treatment. The classified waste liquids can be treated according to their specific properties, with treatment costs far lower than mixed hazardous waste, and it also facilitates the recovery and purification of valuable solvents (such as acetonitrile and methanol).

[0032] The system also includes a central control unit 7 connected to the liquid chromatography-mass spectrometry (LC-MS) instrument 1. A first solenoid valve 8, a second solenoid valve 9, and a third solenoid valve 10 are respectively installed on the inlet pipes of the chromatographic waste tank 4, the mass spectrometry waste tank 5, and the clear waste tank 6. These three solenoid valves are electrically connected to the central control unit 7. The central control unit 7 includes a main control MCU and a power module. In this invention, the main control MCU is an STM32 microcontroller. The power module supplies power to the main control MCU and each solenoid valve and sensor. The main control MCU receives operating status signals from the LC-MS instrument 1 (such as chromatography start / end, mass spectrometry ionization source switch, and cleaning program start / stop) and precisely controls the opening and closing of the corresponding solenoid valves accordingly. This ensures that the waste liquid separation action is completely synchronized with the instrument's operating status, achieving fully automatic and accurate classification without manual intervention, eliminating classification errors caused by human judgment mistakes or operational delays. This not only greatly reduces the burden on operators but also improves the reliability of classification and the automation level of the entire system, ensuring the traceability of experimental data.

[0033] The outlet pipe 2 is equipped with a conductivity sensor 11. The lower end of the outlet pipe 2, via a metering pump 12, is connected to a pretreatment agent storage tank 13. The conductivity sensor 11 and the metering pump 12 are electrically connected to the central control unit 7. The conductivity sensor 11 can monitor the ion concentration (salt content) of the waste liquid in real time. When a high conductivity signal is detected (indicating that the mass spectrometry waste liquid is being discharged and the salt content is extremely high), the central control unit 7 immediately starts the metering pump 12 to precisely inject a quantitative amount of diluent (such as pure water) into the waste liquid pipeline. This achieves instant online dilution of high-salt waste liquid, effectively preventing salt crystallization at the source, thus avoiding clogging of the expensive mass spectrometer vacuum pump discharge pipeline, protecting core equipment, and reducing costly maintenance costs and downtime. This is a proactive, preventative protective measure.

[0034] The chromatographic waste liquid tank 4 is provided in two parallel configurations. The inlets of the two tanks are respectively equipped with a fourth solenoid valve 14 and a fifth solenoid valve 15. The two tanks are respectively equipped with a first level sensor 16 and a second level sensor 17. The fourth solenoid valve 14, the fifth solenoid valve 15, the first level sensor 16, and the second level sensor 17 are electrically connected to the central control unit 7. The two parallel chromatographic waste liquid tanks 4 are equipped with independent solenoid valves and level sensors, allowing for intelligent "one in use, one on standby" management. When the central control unit 7 detects that tank A is about to be full via the level sensor, it can automatically switch the solenoid valve to guide the waste liquid to the empty tank B for continued collection, while simultaneously issuing an alarm indicating that tank A needs to be replaced. This achieves "hot switching" of waste liquid collection, ensuring that during long-term sequence analysis or large-volume sample detection, the waste liquid tank can be replaced without interrupting the liquid chromatography-mass spectrometry instrument 1, greatly improving the overall work efficiency of the laboratory and the continuous operation capability of the equipment.

[0035] The mass spectrometry waste liquid tank 5 has two parallel tanks. The inlets of the two tanks are respectively equipped with a sixth solenoid valve 18 and a seventh solenoid valve 19. The tanks are also equipped with a third level sensor 20 and a fourth level sensor 21. These sensors are electrically connected to the central control unit 7. Mass spectrometry waste liquid typically contains high concentrations of matrix and salt, requiring more frequent replacement. The dual-tank design ensures continuous collection. More importantly, this design provides redundancy for the safe management of high-risk waste liquids. When one tank is full and sealed for disposal, the other tank can be immediately put into use, reducing the time a full tank remains in the laboratory and lowering safety risks. It also facilitates the separate storage of high-risk waste liquids from different projects or with different characteristics, enabling more refined management.

[0036] The cleaning waste liquid tank 6 is provided in two parallel configurations. The inlets of the two tanks are respectively equipped with an eighth solenoid valve 22 and a ninth solenoid valve 23. The tanks are also equipped with a fifth level sensor 24 and a sixth level sensor 25. These sensors are electrically connected to the central control unit 7. The cleaning waste liquid typically contains a high concentration of organic solvents and has high recycling value. The dual-tank design enables continuous collection, ensuring that the instrument's automatic cleaning program will not be interrupted or trigger an alarm due to a full waste liquid tank, thus guaranteeing proper instrument maintenance and standby status.

[0037] The outlet pipe 2 is connected to a buffer tank 26 at its end, and the outlet of the buffer tank 26 is connected to the switching head 3 via a pipe. Waste liquid outflow is not always stable and continuous; there may be pulses or instantaneous large-flow discharges (especially at the end of a gradient or when switching valves). The buffer tank 26, as a small intermediate container, can smooth out these fluctuations in flow and pressure, providing a more stable detection environment for the downstream conductivity sensor 11 and improving measurement accuracy. Simultaneously, it also prevents the liquid flow from directly impacting the liquid path switching within the switching head 3, making fluid switching smoother, reducing potential splashing or mixing, further ensuring the purity of the classification, and extending the service life of components such as solenoid valves.

[0038] It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that after reading the teachings of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined by the appended claims.

Claims

1. A waste liquid treatment device for a liquid chromatography-mass spectrometry (LC-MS) instrument, comprising an outlet pipe connected to the waste liquid port of the LC-MS instrument, characterized in that: The other end of the outlet pipe is connected to the inlet of the cross-shaped converter head, and the three outlets of the converter head are respectively connected to the chromatographic waste liquid tank, the mass spectrometry waste liquid tank and the clear liquid waste liquid tank through pipes.

2. The waste liquid treatment device for a liquid chromatography-mass spectrometry system as described in claim 1, characterized in that: It also includes a central control unit that is connected to the liquid chromatography-mass spectrometry instrument. The inlet pipes of the chromatographic waste tank, the mass spectrometry waste tank and the clear liquid waste tank are respectively equipped with a first solenoid valve, a second solenoid valve and a third solenoid valve, which are electrically connected to the central control unit.

3. The waste liquid treatment device for a liquid chromatography-mass spectrometry system as described in claim 1, characterized in that: The outlet pipe is equipped with a conductivity sensor, and the outlet pipe is connected to a pretreatment agent storage tank via a metering pump at the lower end of the conductivity sensor. The conductivity sensor and the metering pump are electrically connected to the central control unit.

4. The waste liquid treatment device for a liquid chromatography-mass spectrometry system as described in claim 1, characterized in that: The chromatographic waste liquid tank is provided in two parallel configurations. The inlet of each chromatographic waste liquid tank is provided with a fourth solenoid valve and a fifth solenoid valve, respectively. The two chromatographic waste liquid tanks are respectively provided with a first liquid level sensor and a second liquid level sensor. The fourth solenoid valve, the fifth solenoid valve, the first liquid level sensor and the second liquid level sensor are electrically connected to the central control unit.

5. The waste liquid treatment device for a liquid chromatography-mass spectrometry instrument as described in claim 1, characterized in that: The mass spectrometer waste liquid tank is provided in two parallel configurations. The inlet of each mass spectrometer waste liquid tank is provided with a sixth solenoid valve and a seventh solenoid valve, respectively. The two mass spectrometer waste liquid tanks are respectively provided with a third liquid level sensor and a fourth liquid level sensor. The sixth solenoid valve, the seventh solenoid valve, the third liquid level sensor and the fourth liquid level sensor are electrically connected to the central control unit.

6. The waste liquid treatment device for a liquid chromatography-mass spectrometry system as described in claim 1, characterized in that: The clear liquid waste tank is provided in two parallel configurations. The inlet of each clear liquid waste tank is provided with an eighth solenoid valve and a ninth solenoid valve, respectively. The clear liquid waste tank is provided with a fifth liquid level sensor and a sixth liquid level sensor, respectively. The eighth solenoid valve, the ninth solenoid valve, the fifth liquid level sensor, and the sixth liquid level sensor are electrically connected to the central control unit.

7. The waste liquid treatment device for a liquid chromatography-mass spectrometry instrument as described in claim 1, characterized in that: The end of the outlet pipe is connected to a buffer tank, and the outlet of the buffer tank is connected to the converter head through a pipe.

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