A pretreatment device for adding liquid, extracting and concentrating organic matter for environmental analysis.

Abstract

This invention discloses a pretreatment device for adding, extracting, and concentrating environmental organic matter for analysis, relating to the field of organic matter analysis technology. It includes a sample tray, a compressed air source, several reagent bottles, a vacuum pump, and a nitrogen blowing structure. The sample tray is equipped with several sets of tubular structures, each set including several concentration bottles and several sample bottles. The vacuum pump is connected to each concentration bottle, the compressed air source is connected to each reagent bottle, each reagent bottle is connected to each sample bottle and each concentration bottle, and each sample bottle is connected to each concentration bottle. The nitrogen blowing structure is used to blow nitrogen gas into the concentration bottles. This invention enables the addition, extraction, nitrogen blowing concentration, and reconstitution of reagents, replacing the manual operations involved in multiple reagent additions in current processes, standardizing the sample pretreatment process, and reducing testing errors introduced by human operation.

Description

Technical Field

[0001] This invention relates to the field of organic matter analysis technology, and in particular to a pretreatment device for adding liquid, extracting and concentrating environmental organic matter for analysis. Background Technology

[0002] Currently, advanced instrumental analytical methods such as gas chromatography-mass spectrometry (GC-MS), high-performance liquid chromatography-mass spectrometry (HPLC-MS), and nuclear magnetic resonance (NMR) are used for the detection of stable isotopes of organic compounds. However, the analysis and determination of organic compounds still hinges on sample pretreatment, which is a crucial process affecting the precision of analytical results. Ultrasonic-microwave synergistic extraction technology has been widely used in the pretreatment of environmental organic compounds, involving multiple repeated liquid additions, nitrogen blowing concentration, and reconstitution, requiring significant manpower and time costs. Commercially available pretreatment equipment is mostly designed for small sample volumes and single functions, with limited sample capacity and high equipment purchase costs.

[0003] Existing technologies mainly rely on manual processes for adding liquids, extraction, and concentration pretreatment, which are prone to errors. Summary of the Invention

[0004] The purpose of this invention is to provide a pretreatment device for adding, extracting, and concentrating environmental organic matter for analysis, in order to solve the problems existing in the prior art. It can process a large number of samples, save costs, replace the manual operations such as multiple reagent additions involved in the current operation, standardize the sample pretreatment process, and reduce the test errors introduced by human operation.

[0005] To achieve the above objectives, the present invention provides the following solution:

[0006] This invention provides a pretreatment device for adding, extracting, and concentrating environmental organic matter for analysis, comprising a sample tray, a compressed air source, several reagent bottles, a vacuum pump, and a nitrogen blowing structure. The sample tray is provided with several sets of tube structures, each set of tube structures including several concentration bottles and several sample bottles. The vacuum pump is connected to each of the concentration bottles, the compressed air source is connected to each of the reagent bottles, each of the reagent bottles is connected to each of the sample bottles and each of the concentration bottles, and each of the sample bottles is connected to each of the concentration bottles. The nitrogen blowing structure is used to blow nitrogen gas into the concentration bottles.

[0007] Preferably, the system further includes a cylinder, the cylinder body of which is connected to the compressed air source. A pneumatic valve is installed on the pipeline between the cylinder and the compressed air source. A sealing base is installed on the movable end of the cylinder. A concentration cap corresponding to the concentration bottle and a sample cap corresponding to the sample bottle are installed on the sealing base. Each concentration cap and the sample cap are made of polytetrafluoroethylene. Each concentration cap is provided with a main pipeline and several bypass pipelines. One end of the main pipeline is connected to the vacuum pump, and the other end of the main pipeline is connected to one end of each bypass pipeline. The other end of each bypass pipeline extends into each concentration bottle and is above the liquid surface. Each sample cap is provided with a liquid addition and aspiration needle. One end of each liquid addition and aspiration needle is connected to each reagent bottle and each concentration bottle, and the other end of each liquid addition and aspiration needle extends into each sample bottle and is below the liquid surface.

[0008] Preferably, the device also includes a motor, the power output end of which is provided with a lead screw, and a slider threadedly connected to the lead screw is provided on the lead screw. The slider is connected to the cylinder body of the cylinder. The motor drives the lead screw to rotate, and the slider moves along the axis of the lead screw, so that the cylinder drives the concentration cap and the sample cap to move in translation.

[0009] Preferably, a pressure relief valve, a negative pressure controller, and an air extraction valve assembly are installed on the pipeline between the vacuum pump and each of the main pipelines.

[0010] Preferably, each of the reagent bottles is provided with a first connecting tube and a second connecting tube; one end of each first connecting tube is above the liquid surface of each reagent bottle, and the other end of each first connecting tube is connected to the compressed air source, and a pressure valve assembly is provided on the pipeline between each first connecting tube and the compressed air source; one end of each second connecting tube is below the liquid surface of each reagent bottle, and the other end of each second connecting tube is connected to a liquid dispenser, and a liquid flow control valve assembly is provided on the pipeline between each second connecting tube and the liquid dispenser, and the liquid dispenser is connected to each sample bottle.

[0011] Preferably, the nitrogen blowing structure includes a nitrogen source, a lifting structure, and a plurality of nitrogen blowing liquid adding composite needles. The plurality of nitrogen blowing liquid adding composite needles are disposed on a nitrogen blowing support. The lifting structure drives the nitrogen blowing support to move up and down. One end of each nitrogen blowing liquid adding composite needle is connected to the nitrogen source, and the other end of each nitrogen blowing liquid adding composite needle is used to extend into the concentration bottle. The other end of each nitrogen blowing liquid adding composite needle is provided with a plurality of air holes.

[0012] Preferably, it further includes a three-way solenoid valve, the first end of which is connected to the nitrogen source through a first gas pipe, the first gas pipe being equipped with a pressure controller and a flow valve, the second end of which is connected to each of the nitrogen blowing and liquid adding composite needles through a second gas pipe, and the third end of which is connected to the first gas pipe between the pressure controller and the flow valve through a third gas pipe.

[0013] Preferably, the sample tray is mounted on the base, and the sample tray is equipped with a first liquid level sensor and a second liquid level sensor. The first liquid level sensor is used to detect the liquid level in the concentration bottle, and the second liquid level sensor is used to detect the liquid level in the sample bottle.

[0014] Preferably, a magnetic stirrer is provided on the sample tray at a position corresponding to each of the concentration bottles and each of the sample bottles, and a magnetic stir bar is provided in each of the concentration bottles and each of the sample bottles.

[0015] Preferably, a pressure controller is installed on the pipeline between the compressed air and the pressurization valve assembly.

[0016] The present invention achieves the following technical effects compared to the prior art:

[0017] This invention utilizes a sample tray with several sets of tubes to process large quantities of samples. Reagents are forced into sample vials using compressed air for liquid addition. A vacuum pump then sequentially evacuates the corresponding concentration vials, transferring the liquid from the sample vials to the concentration vials for transfer and collection. Nitrogen blowing is then used to concentrate the liquid in the concentration vials. This invention is suitable for scientific research and environmental monitoring departments for pretreatment processes involving the extraction and concentration of environmental samples such as environmental organic pollutants (e.g., phthalates, polychlorinated biphenyls) and microbial metabolites (e.g., phospholipids and fatty acids). It can be used in conjunction with a gas chromatography-quadrupole mass spectrometry-combustion-stability isotope mass spectrometer (GC-MS-C-IRMS) for qualitative, quantitative, and carbon isotope ratio analysis of organic monomers, achieving high-throughput sample pretreatment. Attached Figure Description

[0018] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0019] Figure 1 This is a schematic diagram of the pretreatment apparatus for adding liquid, extracting and concentrating environmental organic matter for analysis according to the present invention.

[0020] The components are as follows: 1-Controller, 2-Base, 3-Magnetic stirrer, 4-Sample tray, 5.1-First liquid level sensor, 5.2-Second liquid level sensor, 6-Vacuum pump, 7-Concentration bottle, 8-Sample bottle, 9-Support column, 10.1-Concentration cap, 10.2-Sample cap, 11-Liquid addition and aspiration combined needle, 12-Sealed base, 13-Motor, 14-Cylinder, 15-Pneumatic valve assembly, 16-Nitrogen blowing liquid addition combined needle, 17-Flow path control valve assembly, 18-Fixed bracket, 19-Reagent bottle, 20-Nitrogen blowing bracket, 21-Pressure valve assembly, 22-Pressure controller, 23-Compressed air source, 24-Flow valve, 25-Nitrogen source, 26-Three-way solenoid valve, 27-Lifting controller, 28-Negative pressure controller, 29-Pressure relief valve, 30-Aeration valve assembly, 31-Liquid dispenser. Detailed Implementation

[0021] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0022] The purpose of this invention is to provide a pretreatment device for adding, extracting, and concentrating environmental organic matter for analysis, in order to solve the problems existing in the prior art. It can process a large number of samples, save costs, replace the manual operations such as multiple reagent additions involved in the current operation, standardize the sample pretreatment process, and reduce the test errors introduced by human operation.

[0023] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0024] like Figure 1As shown: This embodiment provides a pretreatment device for adding liquid, extracting, and concentrating environmental organic matter for analysis. It includes a sample tray 4, a compressed air source 23, several reagent bottles 19, a vacuum pump 6, and a nitrogen blowing structure. This embodiment includes four reagent bottles 19, numbered from left to right as the first, second, third, and fourth reagent bottles. The sample tray 4 is equipped with several sets of tube structures, each set including several concentration bottles 7 and several sample bottles 8. The concentration bottles 7 and sample bottles 8 are glass screw-top bottles with a volume of 12 mL. This embodiment includes four concentration bottles 7 and four sample bottles 8, numbered from left to right as the first, second, third, and fourth concentration bottles. From left to right, the four sample bottles are: the first sample bottle, the second sample bottle, the third sample bottle, and the fourth sample bottle. The vacuum pump 6 is connected to each of the concentration bottles 7. The compressed air source 23 is connected to each of the reagent bottles 19. The first reagent bottle is connected to the first sample bottle and the first concentration bottle. The second reagent bottle is connected to the second sample bottle and the second concentration bottle. The third reagent bottle is connected to the third sample bottle and the third concentration bottle. The fourth reagent bottle is connected to the fourth sample bottle and the fourth concentration bottle. The first sample bottle is connected to the first concentration bottle. The second sample bottle is connected to the second concentration bottle. The third sample bottle is connected to the third concentration bottle. The fourth sample bottle is connected to the fourth concentration bottle. The nitrogen blowing structure is used to blow nitrogen into the concentration bottle 7.

[0025] Specifically, in this embodiment, the first reagent bottle is used to hold sample extraction reagent I, the second reagent bottle is used to hold sample extraction reagent II, the third reagent bottle is used to hold sample concentration and reconstitution reagent I, and the fourth reagent bottle is used to hold sample concentration and reconstitution reagent II.

[0026] In this embodiment, the sample tray 4 is mounted on the base 2. A first liquid level sensor 5.1 and a second liquid level sensor 5.2 are mounted on the sample tray 4. The first liquid level sensor 5.1 detects the liquid level in the concentration bottle 7, and the second liquid level sensor 5.2 detects the liquid level in the sample bottle 8. The first liquid level sensor 5.1 and the second liquid level sensor 5.2 are activated by a red light when there is liquid in the corresponding concentration bottle 7 and sample bottle 8, and deactivated when the liquid level drops. The first liquid level sensor 5.1 is linked to the control valve of the vacuum pump 6, and the second liquid level sensor 5.2 is linked to the control valve of the three-way solenoid valve 26 for nitrogen blowing. The first liquid level sensor 5.1 and the second liquid level sensor 5.2 respectively control the operation of the vacuum pump 6 and the opening and closing of the three-way solenoid valve 26.

[0027] In this embodiment, the sample tray 4 has 64 positions, including 32 sample positions and 32 concentrated liquid positions. Magnetic stirrers 3 are installed on the sample tray 4 at positions corresponding to each concentrated flask 7 and each sample flask 8. Each concentrated flask 7 and each sample flask 8 contains a magnetic stir bar. The sample tray 4 also incorporates a temperature controller, thermocouples, a heating structure, an ultrasonic generator, a transducer, and an ultrasonic controller. This embodiment may also include a microwave generator, which can be used simultaneously with the ultrasonic generator. The heating structure and thermocouples correspond to each concentrated flask 7 and each sample flask 8, and are used to heat the liquids in each concentrated flask 7 and each sample flask 8. The thermocouples detect the temperature of the liquids in each concentrated flask 7 and each sample flask 8 and transmit the signal to the temperature controller. The temperature controller controls the heating structure based on the temperature detected by the thermocouples. The ultrasonic generator is connected to the transducer, and the ultrasonic power (1~100%) of the ultrasonic generator (20kHz) is controlled by adjusting the transducer's operating frequency to achieve ultrasonic extraction of the sample. When the controlled temperature decreases, the heating structure is opened wider under the action of the reset device to increase the output temperature, so that the controlled temperature reaches and is maintained within the set temperature range. The reset device consists of multiple independent solid-state relays connected to the heating structure and simultaneously connected to the temperature controller, which controls the temperature.

[0028] In this embodiment, a cylinder 14 is also included. The cylinder body of the cylinder 14 is connected to a compressed air source 23. A pneumatic valve is installed on the pipeline between the cylinder 14 and the compressed air source 23. The pneumatic valve is a two-position five-way valve. After opening, the cylinder 14 moves downward. A sealing base 12 is provided on the movable end of the cylinder 14. A concentration cap 10.1 corresponding to the concentration bottle 7 and a sample cap 10.2 corresponding to the sample bottle 8 are provided on the sealing base 12. Each concentration cap 10.1 and sample cap 10.2 is made of polytetrafluoroethylene (PTFE). The concentration cap 10.1 and sample cap 10.2 are sealed to the outside by a PTFE sealing gasket. Each sample cap 10.1 is equipped with a main pipeline and several bypass pipelines. One end of the main pipeline is connected to the vacuum pump 6, and the other end is connected to one end of each bypass pipeline. The other end of each bypass pipeline extends 5 mm into each concentration bottle 7 and is above the liquid surface. Each sample cap 10.2 is equipped with a liquid addition / absorption needle 11. One end of each liquid addition / absorption needle 11 is connected to each reagent bottle 19 and each concentration bottle 7, and the other end extends into each sample bottle 8 and is below the liquid surface. The bottom inlet of the liquid addition / absorption needle 11 is equipped with a polytetrafluoroethylene semi-permeable membrane, which allows solution to pass through but not solid, preventing environmental particles from entering the second connecting tube. After the liquid addition / absorption needle 11 descends to the bottom of the sample bottle 8, the vacuum pump 6 is turned on, and the reagent in the sample bottle 8 is transferred to the concentration bottle 7 through the liquid addition / absorption needle 11 by negative pressure, thus realizing the liquid transfer.

[0029] In this embodiment, a motor 13 is also included. The motor 13 is preferably a stepper motor. The body of the motor 13 is mounted on the support column 9. A lead screw is provided at the power output end of the motor 13. A slider is provided on the lead screw and threadedly connected to the lead screw. The slider is connected to the cylinder body of the cylinder 14. The motor 13 drives the lead screw to rotate, and then the slider moves along the axis of the lead screw, so that the cylinder 14 drives the concentration cap 10.1 and the sample cap 10.2 to move horizontally.

[0030] In this embodiment, a pressure relief valve 29, a negative pressure controller 28, and a vacuum valve group 30 are installed on the pipelines between the vacuum pump 6 and each main pipeline. The pressure relief valve 29 is a two-way solenoid valve used for depressurizing and venting the vacuum pump 6. The vacuum valve group 30 is a group of three-way solenoid valves 26. The negative pressure controller 28 precisely controls the liquid suction force, and the first liquid level sensor 5.1 and the second liquid level sensor 5.2 control the liquid transfer volume. A two-way solenoid valve is also installed between the vacuum valve group 30 and the vacuum pump 6 for depressurizing and venting the concentration bottle 7. When the two-way solenoid valve is opened, the concentration bottle 7 is connected to the outside air, realizing depressurization and venting.

[0031] In this embodiment, reagent bottle 19 is a glass screw-top bottle equipped with a flat-bottomed threaded cap, the inside of which is sealed with a PTFE gasket. The flat-bottomed threaded cap has two holes, and two straight-through ferrule connectors are fitted with sealing gaskets. The first and second connecting pipes pass through the holes in the flat-bottomed threaded cap and are tightened inside the cap using matching nuts. The PTFE gaskets seal the plane of the ferrule connectors against the outer plane of the flat-bottomed threaded cap. One end of each first connecting pipe is above the liquid level in each reagent bottle 19. Each first connecting pipe is mounted on a fixed bracket 18, and the other end of each first connecting pipe is connected to a compressed air source 23. A pressure valve assembly 21 is installed on the pipeline between each first connecting pipe and the compressed air source 23. The pressure valve assembly 21 is a two-position three-way solenoid valve 26. After group 21 is opened, the reagent in reagent bottle 19 is forced into sample bottle 8. A pressure controller 22 is installed on the pipeline between compressed air and pressure valve group 21. After initial pressure reduction and secondary precision pressure reduction, the compressed air supplies a stable pressure to pressure valve group 21, with a pressure range of 6-8 PSI. One end of each second connecting pipe is below the liquid level of each reagent bottle 19, and the other end of each second connecting pipe is connected to the liquid dispenser 31. A liquid flow path control valve group 17 is installed on the pipeline between each second connecting pipe and the liquid dispenser 31. The liquid flow path control valve group 17 is a polytetrafluoroethylene two-way solenoid valve. The liquid dispenser 31 is connected to each sample bottle 8. Compressed air enters the reagent bottle 19 through the first connecting pipe, driving the chemical reagent in the reagent bottle 19 to be forced into the corresponding sample bottle 8 through the second connecting pipe, the corresponding liquid flow path control valve group 17, and the liquid dispenser 31. The delivery flow rate is controlled by precisely controlling the pressure of the compressed air, and the liquid volume is controlled by precisely controlling the liquid addition time.

[0032] In this embodiment, the nitrogen blowing structure is located above the sample tray 4. The nitrogen blowing structure includes a nitrogen source 25, a lifting structure, and several nitrogen blowing and liquid adding composite needles 16. Preferably, there are 32 nitrogen blowing and liquid adding composite needles 16. Several nitrogen blowing and liquid adding composite needles 16 are arranged on the nitrogen blowing support 20. The lifting controller 27 controls the lifting structure, which drives the nitrogen blowing support 20 to rise and fall. One end of each nitrogen blowing and liquid adding composite needle 16 is connected to the nitrogen source 25, and the other end of each nitrogen blowing and liquid adding composite needle 16 is used to extend into the concentration bottle 7. Each nitrogen blowing and liquid adding composite needle 16 is made of polytetrafluoroethylene, and the other end of each nitrogen blowing and liquid adding composite needle 16 is provided with several air holes to ensure uniform dispersion of liquid droplets. During nitrogen blowing, the lifting structure drives the nitrogen blowing support 20 to descend, and the other end of the nitrogen blowing and liquid adding composite needle 16 extends into the concentration bottle 7, maintaining a certain height between the other end of the nitrogen blowing and liquid adding composite needle 16 and the liquid surface to improve nitrogen blowing efficiency. The opening and closing of the three-way solenoid valve 26 is controlled by the first liquid level sensor 5.1 to ensure that the liquid enters the low flow rate nitrogen blowing sludge mode for timed purging after it is nearly dry. The low flow rate nitrogen blowing sludge mode is existing technology.

[0033] In this embodiment, a three-way solenoid valve 26 is also included. The first end of the three-way solenoid valve 26 is connected to the nitrogen source 25 through a first gas pipe. A pressure controller 22 and a flow valve 24 are installed on the first gas pipe, and the speed of the nitrogen is regulated by the pressure controller 22 and the flow valve 24. The second end of the three-way solenoid valve 26 is connected to each nitrogen blowing and liquid adding composite needle 16 through a second gas pipe. The third end of the three-way solenoid valve 26 is connected to the first gas pipe between the pressure controller 22 and the flow valve 24 through a third gas pipe. Every four nitrogen blowing and liquid adding composite needles 16, one three-way solenoid valve 26, one first gas pipe, one second gas pipe, and one third gas pipe constitute a group.

[0034] This embodiment also includes a controller 1. Each valve and vacuum pump 6 is connected to the controller 1 via wires, and the controller 1 controls their opening and closing. The negative pressure controller 28 is powered and controlled independently. After connecting all the pipelines, the corresponding functional programs are programmed through the control terminal. The corresponding functional programs are existing technologies.

[0035] The materials used in this embodiment are inexpensive, resulting in a relatively low cost. All valves are corrosion-resistant solenoid valves, and all pipelines are made of polytetrafluoroethylene (PTFE), reducing corrosion from organic reagents and ensuring durability.

[0036] In this embodiment, the pneumatic valve assembly 15 is opened, and the cylinder 14 drives the sealing base 12 to move the concentration cap 10.1 and sample cap 10.2 down to connect with the concentration bottle 7 and sample bottle 8. The liquid flow path control valve assembly 17 is opened, and compressed air forces the liquid from the corresponding reagent bottle 19 into the corresponding sample bottle 8. After the liquid addition is completed, the liquid addition and aspiration composite needle 11 is below the liquid surface, and the processing program of the sample tray 4 is started (microwave / ultrasound coordinated extraction processing program 30 min: 5 min interval), which is the existing technology; the first liquid level sensor 5.1 is started, the vacuum pump 6 is activated, and the corresponding valve of the suction valve assembly 30 is opened, drawing the liquid from each sample bottle 8 into the corresponding concentration bottle 7 through negative pressure, thereby realizing the transfer and collection of liquid. When the liquid level drops to the point where the first liquid level sensor 5.1 is turned off, the vacuum pump 6 automatically shuts off, and at the same time, the negative pressure in the concentration bottle 7 is released. The above procedure will be repeated three times. After the above steps are completed, the pneumatic valve is activated, and the cylinder 14 drives the sealing base 12 to move the concentration cap 10.1 and the sample cap 10.2 upwards to disconnect them from the concentration bottle 7 and the sample bottle 8, returning them to their initial positions, thus completing the extraction and collection of the sample.

[0037] The nitrogen blowing concentration program is initiated. The lifting controller 27 controls the nitrogen blowing support 20 to move downwards, positioning the nitrogen blowing liquid addition needle 16 directly above the concentration bottle 7. The nitrogen switch and corresponding solenoid valve are turned on, and nitrogen begins to blow dry and concentrate the sample. Based on the rate at which the sample liquid level drops due to the nitrogen blowing pressure, the lifting mechanism is activated periodically to keep the nitrogen blowing liquid addition needle 16 at a constant height above the liquid surface until the nitrogen blowing process is complete. Once the nitrogen blowing liquid addition needle 16 reaches the set height, the second liquid level sensor 5.2 controls the opening and closing of the three-way solenoid valve 26. Simultaneously, the liquid flow path control valve group 17 opens, and compressed air forces the liquid from the corresponding reagent bottle 19 into the corresponding concentration bottle 7. After the liquid addition is completed, a second nitrogen blowing concentration is performed until the programmed nitrogen blowing action is complete. The nitrogen blowing support 20 then moves upwards, lifting the nitrogen blowing liquid addition needle 16 to its initial uppermost position, completing the nitrogen blowing concentration process.

[0038] The above steps complete the sample pretreatment process of adding liquid, extraction, and concentration.

[0039] In this embodiment, the liquid addition is mainly achieved by positioning the sample bottle 8 by the motor 13, and then adding the liquid from the reagent bottle 19 to the corresponding sample bottle 8 by connecting the corresponding pipeline (gas pipeline or liquid pipeline). The liquid is added by adjusting the pressure and controlling the liquid addition time by the program. The addition of different liquids in different reagent bottles 19 can be achieved by switching the control valve.

[0040] Extraction involves mixing the reactants evenly in a metal bath using a temperature controller, combined with an ultrasonic controller and a magnetic stirrer 3, after the liquid has been added to the sample bottle 8. This ensures uniform temperature, accelerates the extraction speed, improves extraction efficiency, and shortens the extraction time. Subsequently, the extract is transferred using a liquid addition and aspiration needle 11, achieving solid-liquid separation.

[0041] The concentration pretreatment is achieved by using a metal bath with a temperature controller and simultaneously introducing nitrogen gas through a nitrogen blowing and liquid addition needle 16 to concentrate the extract. Liquid is added through the nitrogen blowing and liquid addition needle 16 for the reconstitution of the concentrated sample, thereby achieving the concentration pretreatment.

[0042] This embodiment enables the extraction and concentration of organic matter in environmental samples. Reagents are forced into sample vials 8 using compressed air, and then the corresponding concentration vials 7 are evacuated using a vacuum pump 6 to collect the extracted components. An electromagnetic induction sensor is positioned approximately 1 mm from the bottom of sample vials 8 to ensure complete liquid transfer by positioning the liquid level. The optimal operating time of the vacuum pump 6 is also set to guarantee complete transfer of liquid from sample vials 8 to concentration vials 7. A three-way solenoid valve 26, combined with electromagnetic induction positioning, ensures that the sample in concentration vials 7 is concentrated and dried under low-flow-rate nitrogen protection. Sample tray 4 provides a microwave / ultrasound and constant-temperature sample processing environment. Corrosion-resistant solenoid valves and PTFE tubing reduce the corrosion of organic reagents. This embodiment enables the complete liquid addition, extraction, and concentration process in the pretreatment of environmental organic matter, overcoming the testing errors that may be introduced by cumbersome manual operations. Furthermore, the device is simple to operate and provides accurate measurement results.

[0043] This embodiment can be used as a pretreatment device for the extraction and concentration pretreatment of organic matter in environmental samples, making it suitable for subsequent molecular structure identification, composition and content analysis and detection of stable isotopes such as 13C abundance.

[0044] This specification uses specific examples to illustrate the principles and implementation methods of the present invention. The descriptions of the above embodiments are only for the purpose of helping to understand the method and core ideas of the present invention. Furthermore, those skilled in the art will recognize that, based on the ideas of the present invention, there will be changes in the specific implementation methods and application scope. Therefore, the content of this specification should not be construed as a limitation of the present invention.

Claims

1. A pretreatment apparatus for adding liquid, extracting, and concentrating environmental organic matter for analysis, characterized in that: The sample disc, a compressed air source, a plurality of reagent bottles, a vacuum pump and a nitrogen blowing structure are provided, a plurality of groups of pipe structures are arranged on the sample disc, each group of the pipe structures comprises a plurality of concentrated bottles and a plurality of sample bottles, the vacuum pump is in communication with each of the concentrated bottles respectively, the compressed air source is in communication with each of the reagent bottles respectively, each of the reagent bottles is in communication with each of the sample bottles and each of the concentrated bottles respectively, each of the sample bottles is in communication with each of the concentrated bottles respectively, and the nitrogen blowing structure is used for blowing nitrogen into the concentrated bottles; A cylinder is further provided, a cylinder body of the cylinder is in communication with the compressed air source, a pneumatic valve group is arranged on a pipeline between the cylinder and the compressed air source, a movable end of the cylinder is provided with a sealing base, the sealing base is provided with concentrated gland corresponding to the concentrated bottles and sample gland corresponding to the sample bottles, a liquid adding and sucking composite needle is arranged on each of the sample glands respectively, one end of each of the liquid adding and sucking composite needles is in communication with each of the reagent bottles and each of the concentrated bottles, the other end of each of the liquid adding and sucking composite needles respectively extends into each of the sample bottles and is below the liquid level, and a polytetrafluoroethylene semi-permeable membrane is arranged at a bottom inlet of the liquid adding and sucking composite needle; The nitrogen blowing structure comprises a nitrogen source, a lifting structure and a plurality of nitrogen blowing liquid adding composite needles, the plurality of nitrogen blowing liquid adding composite needles are arranged on a nitrogen blowing support, the lifting structure drives the nitrogen blowing support to lift and lower, one end of each of the nitrogen blowing liquid adding composite needles is in communication with the nitrogen source, the other end of each of the nitrogen blowing liquid adding composite needles is used for extending into the concentrated bottles, and a plurality of air holes are arranged at the other end of each of the nitrogen blowing liquid adding composite needles; A three-way electromagnetic valve is further provided, a first end of the three-way electromagnetic valve is in communication with the nitrogen source through a first air pipe, and a second end of the three-way electromagnetic valve is in communication with each of the nitrogen blowing liquid adding composite needles through a second air pipe; A first liquid level sensor and a second liquid level sensor are arranged on the sample disc, the first liquid level sensor is used for detecting the liquid level of the liquid in the concentrated bottles, and the second liquid level sensor is used for detecting the liquid level of the liquid in the sample bottles; the first liquid level sensor is linked with a control valve of the vacuum pump, the second liquid level sensor is linked with a control valve of the three-way electromagnetic valve of the nitrogen blowing, and the first liquid level sensor and the second liquid level sensor respectively control the vacuum pump and the opening and closing of the three-way electromagnetic valve; An ultrasonic generator, a transducer and an ultrasonic controller are further arranged in the sample disc, the ultrasonic generator is connected with the transducer, the ultrasonic power of the ultrasonic generator is controlled by adjusting the working frequency of the transducer to achieve the purpose of controlling the ultrasonic intensity, and the ultrasonic extraction of the sample is realized. In use, the pneumatic valve group is opened, the cylinder drives the sealing base to move down the concentrated cover and the sample cover to communicate with the concentrated bottle and the sample bottle, compressed air pressurizes the liquid in the corresponding reagent bottle into the corresponding sample bottle, after the liquid addition is completed, the liquid addition and suction composite needle is below the liquid level, the processing program of the sample disc is started; the first liquid level sensor is started, the vacuum pump is linked, the liquid in each sample bottle is sucked into the corresponding concentrated bottle through negative pressure, realizing the transfer and collection of the liquid; when the liquid level drops to the first liquid level sensor, the vacuum pump is automatically closed, at the same time, the negative pressure in the concentrated bottle is released, after the above steps are completed, the pneumatic valve is started, the cylinder drives the sealing base to move up the concentrated cover and the sample cover to disconnect with the concentrated bottle and the sample bottle, and returns to the initial position, completing the extraction and collection of the sample; The nitrogen blowing concentration program is started, the nitrogen blowing support moves downward, the nitrogen blowing liquid addition composite needle is located directly above the concentrated bottle, and nitrogen starts to blow dry the concentrated sample; When the nitrogen blowing liquid addition composite needle drops to the set height, compressed air pressurizes the liquid in the corresponding reagent bottle into the corresponding concentrated bottle, liquid addition is carried out through the nitrogen blowing liquid addition composite needle, after the liquid addition is completed, the second nitrogen blowing concentration is carried out, until the programmed nitrogen blowing action is completed, the nitrogen blowing support moves upward to lift the nitrogen blowing liquid addition composite needle to the uppermost initial position, completing the nitrogen blowing concentration process.

2. The liquid addition, extraction and concentration pretreatment device for environmental organic matter analysis according to claim 1, characterized in that: Each of the concentrated cover and the sample cover is made of polytetrafluoroethylene; each of the concentrated cover is provided with a main pipeline and a plurality of bypass pipelines, one end of the main pipeline is communicated with the vacuum pump, the other end of the main pipeline is connected with one end of each of the bypass pipelines, the other end of each of the bypass pipelines extends into each of the concentrated bottles and is located above the liquid level.

3. The liquid addition, extraction and concentration pretreatment apparatus for environmental organic matter analysis according to claim 2, characterized in that: Further comprising a motor, a screw rod is arranged at the power output end of the motor, a sliding block is arranged on the screw rod and threadedly connected with the screw rod, the sliding block is connected with the cylinder body of the cylinder, the motor drives the screw rod to rotate, and then the sliding block moves along the axis of the screw rod, so that the cylinder drives the concentrated cover and the sample cover to realize translation.

4. The liquid addition, extraction and concentration pretreatment apparatus for environmental organic matter analysis according to claim 2, characterized in that: A pressure relief valve, a negative pressure controller and an air suction valve group are arranged on the pipeline between the vacuum pump and each of the main pipelines.

5. The liquid addition, extraction and concentration pretreatment apparatus for environmental organic matter analysis according to claim 1, characterized in that: Each of the reagent bottles is provided with a first connecting pipe and a second connecting pipe; one end of each of the first connecting pipes is located above the liquid level of each of the reagent bottles, the other end of each of the first connecting pipes is communicated with the compressed air source, a pressure valve group is arranged on the pipeline between each of the first connecting pipes and the compressed air source; one end of each of the second connecting pipes is located below the liquid level of each of the reagent bottles, the other end of each of the second connecting pipes is communicated with a liquid addition device, a liquid flow path control valve group is arranged on the pipeline between each of the second connecting pipes and the liquid addition device, and the liquid addition device is communicated with each of the sample bottles.

6. The liquid addition, extraction, and concentration pretreatment apparatus for environmental organic analysis according to claim 1, characterized by: A pressure controller and a flow valve are arranged on the first gas pipe, and the third end of the three-way electromagnetic valve is communicated with the first gas pipe between the pressure controller and the flow valve through a third gas pipe.

7. The liquid addition, extraction, and concentration pretreatment apparatus for environmental organic analysis according to claim 1, characterized by: The sample disc is arranged on the base.

8. The liquid addition, extraction, and concentration pretreatment apparatus for environmental organic analysis according to claim 1, characterized by: The sample disc is provided with a magnetic stirrer corresponding to each of the concentrate bottles and sample bottles, and each of the concentrate bottles and sample bottles is provided with a magnetic stirrer.

9. The liquid addition, extraction and concentration pretreatment apparatus for environmental organic matter analysis according to claim 5, characterized in that: A pressure controller is arranged on the pipeline between the compressed air and the pressure valve group.

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