Carbon isotope test sample preparation device and preparation method thereof

Abstract

The present application provides a carbon isotope test sample preparation device and a preparation method thereof, which are used to extract target components from original samples for preparation of test samples, including at least one sample preparation reaction structure; a liquid adding structure for introducing reaction reagents into the sample preparation reaction structure; a gas stirring structure for introducing gas into the sample preparation reaction structure to stir the reaction reagents; a control unit for driving the sample preparation reaction structure, the liquid adding structure and the gas stirring structure respectively; the liquid adding structure and the gas stirring structure are respectively connected to the sample preparation reaction structure; the control unit is electrically connected to the sample preparation reaction structure, the liquid adding structure and the gas stirring structure respectively. The integration of the device enables the extraction of effective components from various types of original samples to be completed on one set of devices, saving instrument costs; the mechanical automation control of the preparation device solves the problems of low efficiency, high cost, exposure to chemical reagents and poor repeatability caused by manual operation.

Description

Technical Field

[0001] The present application relates to the field of isotope detection, and in particular to a carbon isotope test sample preparation device and a preparation method thereof. Background Art

[0002] Carbon in nature 12 C. 13 C. 14 C exists in various isotopic forms, among which 12 C and 13 C is a stable isotope. 14 C is a radioactive isotope. Carbon, as the skeleton of organic and inorganic carbon molecules, is widely distributed in all spheres of the earth system and participates in most processes at all stages of the earth system evolution. Using carbon isotope ratios as the main indicator for process tracing and chronological research has expanded from the traditional field of geology to cover many natural science disciplines such as ecology, environmental science, groundwater science, archaeology, marine science, criminal investigation science, and biomedicine.

[0003] However, the original samples collected from the natural environment often contain complex chemical compositions of carbon-containing substances and various forms of carbon. If the original samples are used for carbon isotope composition analysis without distinction, the experimental test results will represent mixed information of the samples, which will directly lead to the serious consequence that the results cannot be interpreted. Therefore, how to extract effective components from the original samples for isotope analysis is a basic scientific issue that cannot be avoided in carbon isotope tracing and chronology research.

[0004] Sample pretreatment is a key component of isotope sample preparation technology, which uses physical and chemical methods to remove harmful components and extract effective components from the original sample. However, at present, the sample pretreatment methods in the industry vary from laboratory to laboratory, the experimental equipment is scattered and diverse, the experimental operation is manually performed, and the experimental operators are required to have high skills. With the advancement of carbon isotope analysis technology and the continuous expansion of its application fields, the experimental methods are constantly developing in depth and refinement, and the sample volume is also growing rapidly. The existing equipment and methods have low working efficiency and cannot avoid various difficult problems that arise in manual experimental operations. Summary of the invention

[0005] In view of the above problems, the present application is proposed to provide a carbon isotope test sample preparation device and a preparation method thereof that overcome the above problems or at least partially solve the above problems, comprising:

[0006] A carbon isotope test sample preparation device, the device is used to extract target components in an original sample to prepare a test sample, comprising at least one sample preparation reaction structure; a liquid adding structure for introducing a reaction reagent into the sample preparation reaction structure; a gas stirring structure for introducing a gas into the sample preparation reaction structure to stir the reaction reagent; a control unit for driving the sample preparation reaction structure, the liquid adding structure and the gas stirring structure respectively; and also comprising a recovery structure for collecting reaction waste liquid of the sample preparation reaction structure;

[0007] The sample preparation reaction structure is mainly composed of a liquid level probe, a stirring gas pipe, a liquid inlet pipe, a waste liquid pipe, a cavity plug, a clamp and a reaction chamber;

[0008] The recovery structure includes a first collector, a first peristaltic pump, a first multi-channel control valve and a plurality of waste liquid barrels; the liquid adding structure is mainly composed of a second collector, a second peristaltic pump, a second multi-channel control valve, a hose and a reagent storage structure; the gas stirring structure is mainly composed of a third multi-channel control valve, an air inlet pipe, a gas washing chamber and a dispersion head;

[0009] The liquid adding structure and the gas stirring structure are respectively connected to the sample preparation reaction structure; the control unit is electrically connected to the sample preparation reaction structure, the liquid adding structure and the gas stirring structure, respectively. Specifically, the control unit drives the liquid adding structure to introduce the reaction reagent into the sample preparation reaction structure; the control unit drives the gas stirring structure to introduce the gas used for stirring the reaction reagent in the sample preparation reaction structure into the sample preparation reaction structure; the control unit drives the start and stop of the sample preparation reaction structure.

[0010] Furthermore, the recovery structure is used to collect the reaction waste liquid of the sample preparation reaction structure, and the recovery structure is connected to the sample preparation reaction structure and is electrically connected to the control unit; specifically, the control unit drives the recovery structure to suck out and recycle the reaction waste liquid in the sample preparation reaction structure.

[0011] Furthermore, the liquid outlet of the first multi-channel control valve corresponds to and is connected to the waste liquid barrel; the liquid inlet of the first collector corresponds to and is connected to the sample preparation reaction structure; the liquid inlet of the first multi-channel control valve is connected to the liquid outlet of the first collector through the first peristaltic pump; the control unit drives the on and off of the first multi-channel control valve and the switch of the first peristaltic pump. Specifically, the control unit drives the first peristaltic pump to suck out the reaction waste liquid in each of the sample preparation reaction structures, and diverts the reaction waste liquid to the corresponding waste liquid barrel by driving the on and off of the first multi-channel control valve.

[0012] Further, the sample preparation reaction structure further comprises: a sample preparation reactor, a heating component for heating the sample preparation reactor;

[0013] The sample preparation reactor is arranged in the heating chamber of the heating assembly; the sample preparation reactor is connected to the liquid adding structure through a liquid inlet pipe; the sample preparation reactor is connected to the gas stirring structure through a stirring gas pipe; the sample preparation reactor is connected to the liquid inlet of the first collector in the recovery structure through a reaction waste liquid pipe;

[0014] The control unit is electrically connected to the heating component. Specifically, the control unit heats the sample preparation reactor by driving a switch of the heating component.

[0015] Furthermore, it also includes a two-dimensional moving device for moving the sample preparation reaction structure, the two-dimensional moving device includes a first Z-axis lifting platform, a second Z-axis lifting platform, an X-axis moving platform, a Z-axis lifting guide rail, an X-axis moving guide rail and a chassis;

[0016] The Z-axis lifting guide rail is vertically fixed on the surface of the chassis, and the X-axis moving guide rail is horizontally fixed on the surface of the chassis;

[0017] The first Z-axis lifting platform and the second Z-axis lifting platform are respectively movably connected to the Z-axis lifting guide rail, and move up and down along the direction of the Z-axis lifting guide rail through the corresponding Z-axis stepper motor, wherein the first Z-axis lifting platform is located above the second Z-axis lifting platform; the X-axis moving platform is movably connected to the X-axis moving guide rail, and moves forward and backward along the direction of the X-axis moving guide rail through the X-axis stepper motor;

[0018] The control unit is electrically connected to the Z-axis stepper motor and the X-axis stepper motor respectively, and drives the switches of the Z-axis stepper motor and the X-axis stepper motor;

[0019] The reaction waste liquid pipe is fixed to the first Z-axis lifting platform of the two-dimensional moving device, and the reaction waste liquid pipe passes through the cavity plug of the sample preparation reactor to insert the pipe body into the reaction chamber of the sample preparation reactor. The reaction waste liquid pipe moves up and down along the Z-axis direction with the first Z-axis lifting platform to adjust the length of the pipe body inserted into the reaction chamber;

[0020] The cavity plug is fixed to the second Z-axis lifting platform of the two-dimensional moving device, and the cavity plug is tightly connected to the reaction chamber, and the cavity plug drives the reaction chamber to move up and down along the Z-axis direction along with the second Z-axis lifting platform;

[0021] The heating component is fixed to the X-axis moving platform of the two-dimensional moving device, and moves forward and backward along the X-axis direction along with the X-axis moving platform.

[0022] Furthermore, the liquid level probe is used to detect the liquid level of the reaction reagent in the reaction chamber;

[0023] The liquid level probe penetrates through the cavity plug and enters the reaction cavity;

[0024] The control unit is electrically connected to the liquid level probe and receives an electrical signal fed back by the liquid level probe.

[0025] Furthermore, the liquid adding structure includes a plurality of reagent storage structures, a second multi-channel control valve respectively connected to the plurality of reagent storage structures, a second peristaltic pump, and a second distributor for equally distributing the derived reaction reagents;

[0026] The liquid inlet of the second multi-channel control valve corresponds to the reagent storage structure; the liquid outlet of the second manifold corresponds to the sample preparation reaction structure; the second multi-channel control valve is connected to the second manifold through the second peristaltic pump;

[0027] The control unit controls the on-off of the second multi-channel control valve, and guides the reaction reagents in each of the reagent storage structures to each of the sample preparation reaction structures through the second manifold and distributor by means of the second peristaltic pump.

[0028] Further, the gas stirring structure includes a third multi-channel control valve respectively connected to the plurality of sample preparation reaction structures, a gas washing chamber for removing impurities from the gas source gas, and an air inlet pipe for directing the gas source gas into the gas washing chamber;

[0029] The gas outlet of the third multi-channel control valve corresponds to the sample preparation reaction structure; the gas inlet pipe and the gas inlet of the third multi-channel control valve are respectively connected to the gas washing chamber;

[0030] The control unit is electrically connected to the third multi-channel control valve, and drives the switch of the third multi-channel control valve to introduce the gas used for stirring the reaction reagents in the sample preparation reaction structure after the impurities are removed in the gas washing chamber into the sample preparation reaction structure.

[0031] A method for preparing a carbon isotope test sample, the method being applied to the carbon isotope test sample preparation device as described above, comprising:

[0032] Obtain basic sample information and set relevant preparation parameters;

[0033] Determine the sampling process parameters, the liquid feeding process parameters, the recovery process parameters, the elution process parameters, the drying process parameters, and the number of execution times of the recovery process according to the basic information of the sample and the relevant preparation parameters;

[0034] The carbon isotope test sample is prepared according to the sampling process parameters, the liquid feeding process parameters, the recovery process parameters, the elution process parameters, the drying process parameters, and the number of execution times of the recovery process.

[0035] Furthermore, the step of preparing the carbon isotope test sample according to the sampling process parameters, the liquid feeding process parameters, the recovery process parameters, and the number of execution times of the recovery process includes:

[0036] Adding the original sample into the reaction chamber according to the sampling process parameters;

[0037] Adding the reaction reagent into the reaction chamber according to the liquid inlet process parameters;

[0038] Performing elution treatment on the reaction chamber according to the elution process parameters;

[0039] Performing reaction waste liquid recovery processing according to the recovery process parameters, and determining whether the current recovery process number reaches the execution number;

[0040] If yes, the substance in the reaction chamber is dried according to the drying process parameters; if no, the process returns to execute adding the reaction reagent to the reaction chamber according to the liquid inlet process parameters, and recovering the reaction waste liquid according to the recovery process parameters, until the number of recovery processes reaches the execution number;

[0041] The prepared test sample is taken out according to the sampling process parameters.

[0042] Furthermore, the sampling process includes:

[0043] Controlling the first Z-axis lifting platform and the second Z-axis lifting platform to lift to a specified height, and controlling the X-axis moving platform to move forward a specified distance;

[0044] Adding the original sample into the reaction chamber; or taking out the test sample from the reaction chamber;

[0045] Control the first Z-axis lifting platform, the second Z-axis lifting platform, and the X-axis moving platform to reset.

[0046] Furthermore, the liquid feeding process includes:

[0047] Determining the number of open channels of the second multi-channel control valve, the pumping speed of the second peristaltic pump, the preset working time, and the delayed start time of the second multi-channel control valve and the third multi-channel control valve according to the relevant preparation parameters;

[0048] respectively starting the peristaltic pump, the second multi-channel control valve and the third multi-channel control valve; and detecting the liquid level in the reaction chamber;

[0049] If the liquid level is greater than the warning value, the second multi-channel control valve and the second peristaltic pump are closed; if the liquid level is less than the warning value, it is determined whether the current working time of the second peristaltic pump reaches the preset working time;

[0050] If the second peristaltic pump reaches the preset working time, the second multi-channel control valve and the third multi-channel control valve are closed, and the second peristaltic pump is set to be closed after reaching the first delayed closing time.

[0051] Furthermore, the recycling process comprises:

[0052] Wait for the preset waiting time;

[0053] Detecting the liquid level and determining a value based on the liquid level;

[0054] Controlling the first Z-axis lifting platform to descend to the position corresponding to the assigned value;

[0055] Starting the first multi-channel control valve, and starting the first peristaltic pump at a preset pump speed;

[0056] When the pump speed of the first peristaltic pump is greater than zero, detecting the current liquid level, and determining whether the high liquid level and the low liquid level are equal;

[0057] If so, the first peristaltic pump and the first multi-channel control valve are set to close after reaching a second delayed closing time.

[0058] Furthermore, the elution process includes:

[0059] Determining the elution time and elution temperature of the heating component according to the elution process parameters;

[0060] The heating group is started according to the elution time and the elution temperature.

[0061] Furthermore, the drying process comprises:

[0062] Determining the drying time and drying temperature of the heating component according to the drying process parameters;

[0063] The heating component is activated according to the drying time and the drying temperature.

[0064] A device comprises a processor, a memory and a computer program stored in the memory and capable of running on the processor, wherein the computer program implements the steps of the carbon isotope test sample preparation method as described above when executed by the processor.

[0065] A computer-readable storage medium stores a computer program, and when the computer program is executed by a processor, the steps of the carbon isotope test sample preparation method as described above are implemented.

[0066] This application has the following advantages:

[0067] In an embodiment of the present application, it includes at least one sample preparation reaction structure; a liquid adding structure for introducing a reaction reagent into the sample preparation reaction structure; a gas stirring structure for introducing a gas into the sample preparation reaction structure to stir the reaction reagent; a control unit for driving the sample preparation reaction structure, the liquid adding structure and the gas stirring structure respectively; the liquid adding structure and the gas stirring structure are respectively connected to the sample preparation reaction structure; the control unit is electrically connected to the sample preparation reaction structure, the liquid adding structure and the gas stirring structure respectively, specifically, the control unit drives the liquid adding structure to introduce the reaction reagent into the sample preparation reaction structure; the control unit drives the gas stirring structure to introduce the gas used for stirring the reaction reagent in the sample preparation reaction structure into the sample preparation reaction structure; the control unit drives the start and stop of the sample preparation reaction structure. The integration of the device enables the extraction of effective components from various types of original samples on one set of equipment, saving instrument costs; the mechanical automation control of the preparation device solves the problems of low efficiency, high cost, exposure to chemical reagents and poor repeatability caused by manual operation; by adding a disturbance-free automatic recovery device, it can ensure that the reaction waste liquid is recovered to the maximum extent without disturbance and there is no sediment pollution; a sample preparation reaction structure is added, and under automated control, this structure can realize the traditional high-temperature Soxhlet extraction experimental steps under room temperature conditions (i.e., no need for electric heating jacket heating), getting rid of the problem of flammable and explosive hazards of the device; a bubble stirring structure is added, and under automated control, this structure can make the original sample and the reaction reagent fully contact, improve the reaction efficiency, shorten the reaction time, and make the chemical reaction more sufficient and thorough within the effective reaction time. BRIEF DESCRIPTION OF THE DRAWINGS

[0068] In order to more clearly illustrate the technical solution of the present application, the drawings required for use in the description of the present application will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative labor.

[0069] Figure 1 It is a structural schematic diagram of a carbon isotope test sample preparation device provided in one embodiment of the present application;

[0070] Figure 2 This is an internal structure diagram of a multi-channel control valve of a carbon isotope test sample preparation device provided in one embodiment of the present application;

[0071] Figure 3 This is a structural diagram of a two-dimensional moving device of a carbon isotope test sample preparation device provided in one embodiment of the present application;

[0072] Figure 4 It is a flow chart of the steps of a method for preparing a carbon isotope test sample provided in one embodiment of the present application;

[0073] Figure 5 It is a flow chart of the experimental steps of acid-base and acid-acid treatment of existing coal samples provided in a specific embodiment of the present application;

[0074] Figure 6 It is a logic diagram of a coal isotope sample preparation control program provided in a specific embodiment of the present application;

[0075] Figure 7 is a schematic diagram of a process for preparing α-cellulose from a tree ring sample provided in another specific embodiment of the present application;

[0076] Figure 8 is a flow chart of the steps for preparing α-cellulose from existing tree ring samples provided by another specific embodiment of the present application;

[0077] Fig. 9 is a logic diagram of a control program for preparing α-cellulose from a tree ring sample provided in another specific embodiment of the present application;

[0078] Fig.10 This is a flowchart of the steps of an existing peat sample humic acid extraction experiment provided by another specific embodiment of the present application;

[0079] Fig.11 This is a logic diagram of a control program for preparing humic acid from a peat sample provided in another specific embodiment of the present application.

[0080] The second collector 1, the second peristaltic pump 2, the second multi-channel control valve 3, the hose 4, the reagent storage structure 5, the third multi-channel control valve 6, the air inlet pipe 7, the air washing chamber 8, the dispersion head 9, the Z-axis lifting slide bar 10, the liquid level probe 11, the stirring air pipe 12, the liquid inlet pipe 13, the waste liquid pipe 14, the cavity plug 15, the clamp 16, the reaction chamber 17, the first Z-axis lifting platform 18, the second Z-axis lifting platform 19, the graphite furnace 20, the X-axis moving platform 21, the X-axis moving guide rail 22, the chassis 23, the first Z-axis lifting guide rail 24, the second Z-axis lifting guide rail 25, the first collector 26, the first peristaltic pump 27, the first multi-channel control valve 28, the waste liquid barrel 29, and the device housing 30. DETAILED DESCRIPTION

[0081] In order to make the objects, features and advantages of the present application more obvious and understandable, the present application is further described in detail below in conjunction with the accompanying drawings and specific implementation methods. Obviously, the described embodiments are part of the embodiments of the present application, rather than all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in the field without creative work are within the scope of protection of the present application.

[0082] Reference Figure 1 , shows a carbon isotope test sample preparation device provided by an embodiment of the present application, the device is used to extract the target component in the original sample to prepare the test sample,

[0083] The invention comprises at least one sample preparation reaction structure; a liquid adding structure for introducing a reaction reagent into the sample preparation reaction structure; a gas stirring structure for introducing a gas into the sample preparation reaction structure to stir the reaction reagent; and a control unit for driving the sample preparation reaction structure, the liquid adding structure and the gas stirring structure respectively.

[0084] The liquid adding structure and the gas stirring structure are respectively connected to the sample preparation reaction structure; the control unit is electrically connected to the sample preparation reaction structure, the liquid adding structure and the gas stirring structure, respectively. Specifically, the control unit drives the liquid adding structure to introduce the reaction reagent into the sample preparation reaction structure; the control unit drives the gas stirring structure to introduce the gas used for stirring the reaction reagent in the sample preparation reaction structure into the sample preparation reaction structure; the control unit drives the start and stop of the sample preparation reaction structure.

[0085] In an embodiment of the present application, it includes at least one sample preparation reaction structure; a liquid adding structure for introducing a reaction reagent into the sample preparation reaction structure; a gas stirring structure for introducing a gas into the sample preparation reaction structure to stir the reaction reagent; a control unit for driving the sample preparation reaction structure, the liquid adding structure and the gas stirring structure respectively; the liquid adding structure and the gas stirring structure are respectively connected to the sample preparation reaction structure; the control unit is electrically connected to the sample preparation reaction structure, the liquid adding structure and the gas stirring structure respectively, specifically, the control unit drives the liquid adding structure to introduce the reaction reagent into the sample preparation reaction structure; the control unit drives the gas stirring structure to introduce the gas used for stirring the reaction reagent in the sample preparation reaction structure into the sample preparation reaction structure; the control unit drives the start and stop of the sample preparation reaction structure. The integration of the device enables the extraction of effective components from various types of original samples on one set of equipment, saving instrument costs; the mechanical automation control of the preparation device solves the problems of low efficiency, high cost, exposure to chemical reagents and poor repeatability caused by manual operation; by adding a disturbance-free automatic recovery device, it can ensure that the reaction waste liquid is recovered to the maximum extent without disturbance and there is no sediment pollution; a sample preparation reaction structure is added, and under automated control, this structure can realize the traditional high-temperature Soxhlet extraction experimental steps under room temperature conditions (i.e., no need for electric heating jacket heating), getting rid of the problem of flammable and explosive hazards of the device; a bubble stirring structure is added, and under automated control, this structure can make the original sample and the reaction reagent fully contact, improve the reaction efficiency, shorten the reaction time, and make the chemical reaction more sufficient and thorough within the effective reaction time.

[0086] Reference Figure 1-3 , the carbon isotope test sample preparation device in this exemplary embodiment will be further described below.

[0087] As an example, Figure 1The control unit is shown in the e area, and the control unit is mainly composed of a computer, a controller and a two-way transmission connection communication cable. The controller contains a peristaltic pump control module, a multi-channel control valve control module, a stepper motor control module, a liquid level detection control module and a central processing unit coordination work module. The first peristaltic pump 27 and the second peristaltic pump 2 are electrically connected to the peristaltic pump control module through a communication cable to control the pump speed and start-stop time. The first multi-channel control valve 28, the second multi-channel control valve 3 and the third multi-channel control valve 6 are electrically connected to the multi-channel control valve control module through a communication cable to control the channel opening position and opening and closing time of each multi-channel control valve. The stepper motors in the first Z-axis lifting guide rail 24, the second Z-axis lifting guide rail 25 and the X-axis moving guide rail 22 are electrically connected to the stepper motor control module through a communication cable to control the rotation and start-stop time of the stepper motor. The liquid level probe 11 is electrically connected to the liquid level detection control module through a communication cable to control the liquid level probe 11 to collect low liquid level and high liquid level values ​​in real time with high density. The control modules are coordinated through the central processing unit coordination work module. The controller is electrically connected to the computer via R232 or other serial communication methods, and the computer operates the controller through software to complete the programmed automatic operation of the entire device.

[0088] In one embodiment, it further comprises a recovery structure for collecting the reaction waste liquid of the sample preparation reaction structure.

[0089] The recovery structure is communicated with the sample preparation reaction structure and is electrically connected to the control unit; specifically, the control unit drives the recovery structure to suck out and recover the reaction waste liquid in the sample preparation reaction structure.

[0090] In one embodiment, the recycling structure includes a first collector 26, a first peristaltic pump 27, a first multi-channel control valve 28 and a plurality of waste liquid barrels 29;

[0091] The liquid outlet of the first multi-channel control valve 28 corresponds to and is in communication with the waste liquid bucket 29; the liquid inlet of the first manifold 26 corresponds to and is in communication with the sample preparation reaction structure; the liquid inlet of the first multi-channel control valve 28 is in communication with the liquid outlet of the first manifold 26 through the first peristaltic pump 27;

[0092] The control unit drives the on and off of the first multi-channel control valve 28 and the switch of the first peristaltic pump 27. Specifically, the control unit drives the first peristaltic pump 27 to suck out the reaction waste liquid in each sample preparation reaction structure, and drives the on and off of the first multi-channel control valve 28 to divert the reaction waste liquid to the corresponding waste liquid barrel 29.

[0093] As an example, Figure 1The recycling structure is shown in the d area. The recycling structure is mainly composed of a first manifold 26, a first peristaltic pump 27, a first multi-channel control valve 28, and a plurality of waste liquid barrels 29. The first manifold 26 is made of glass or Teflon material, and the number of branch pipes can be increased or decreased according to design requirements. In the example shown in the figure, there are 8 branches, one of which is a liquid outlet branch, and the other branches are liquid inlet branches. Each liquid inlet branch corresponds to a group Figure 1 The sample preparation reaction structure shown in region c is used to Figure 1 The reaction waste liquid is collected in the reaction waste liquid pipe 14 in the c area. The speed and start and stop time of the first peristaltic pump 27 can be controlled by the control unit. The first multi-channel control valve 28 has multiple channels, the number of which can be increased or decreased according to design requirements, and the start and close time of each channel can be controlled separately by the control unit. In the example shown in the figure, it is a 6-channel structure, and its internal detailed structure is as follows Figure 2 As shown, there are 6 liquid outlets (i.e. 6 channels) and 1 liquid inlet, which are used to collect the reaction waste liquid into the corresponding waste liquid barrel 29. The material of the waste liquid barrel 29 depends on the chemical reagent, which can be glass or Teflon. The capacity depends on the amount of chemical reagent used. The number can be increased or decreased according to the preparation needs. In the example shown in the figure, there are 5 reagent bottles. In the example shown in the figure, the first collector 26, the first peristaltic pump 27, the first multi-channel control valve 28, and the waste liquid barrel 29 are connected by a hose. Figure 1 Connect as shown in area d.

[0094] In one embodiment, the sample preparation reaction structure includes: a sample preparation reactor, a heating component for heating the sample preparation reactor;

[0095] The sample preparation reactor is arranged in the heating chamber of the heating assembly; the sample preparation reactor is connected to the liquid adding structure through the liquid inlet pipe 13; the sample preparation reactor is connected to the gas stirring structure through the stirring gas pipe 12; the sample preparation reactor is connected to the liquid inlet of the first collector 26 in the recovery structure through the reaction waste liquid pipe 14;

[0096] The control unit is electrically connected to the heating component. Specifically, the control unit heats the sample preparation reactor by driving a switch of the heating component.

[0097] In one embodiment, it further comprises a two-dimensional moving device for moving the sample preparation reaction structure.

[0098] The two-dimensional moving device includes a first Z-axis lifting platform 18, a second Z-axis lifting platform 19, an X-axis moving platform 21, a Z-axis lifting guide rail, an X-axis moving guide rail 22 and a chassis 23;

[0099] The Z-axis lifting guide rail is vertically fixed on the surface of the chassis 23, and the X-axis moving guide rail 22 is horizontally fixed on the surface of the chassis 23;

[0100] The first Z-axis lifting platform 18 and the second Z-axis lifting platform 19 are respectively movably connected to the Z-axis lifting guide rail, and move up and down along the direction of the Z-axis lifting guide rail through the corresponding Z-axis stepper motor, wherein the first Z-axis lifting platform 18 is located above the second Z-axis lifting platform 19; the X-axis moving platform 21 is movably connected to the X-axis moving guide rail 22, and moves forward and backward along the direction of the X-axis moving guide rail 22 through the X-axis stepper motor;

[0101] The control unit is electrically connected to the Z-axis stepper motor and the X-axis stepper motor respectively, and drives the switches of the Z-axis stepper motor and the X-axis stepper motor;

[0102] The reaction waste liquid pipe 14 is fixed to the first Z-axis lifting platform 18 of the two-dimensional moving device. The reaction waste liquid pipe 14 passes through the cavity plug 15 of the sample preparation reactor to insert the pipe body into the reaction chamber 17 of the sample preparation reactor. The reaction waste liquid pipe 14 moves up and down along the Z-axis direction with the first Z-axis lifting platform 18 to adjust the length of the pipe body inserted into the reaction chamber 17.

[0103] The cavity plug 15 is fixed to the second Z-axis lifting platform 19 of the two-dimensional moving device, and the cavity plug 15 is tightly connected to the reaction chamber 17. The cavity plug 15 drives the reaction chamber 17 to move up and down along the Z-axis direction along with the second Z-axis lifting platform 19.

[0104] The heating structure is fixed to the X-axis moving platform 21 of the two-dimensional moving device, and moves forward and backward along the X-axis direction along with the X-axis moving platform 21 .

[0105] In one embodiment, the sample preparation reaction structure includes a liquid level probe 11 for detecting the level of the reaction reagent in the reaction chamber 17;

[0106] The liquid level probe 11 penetrates through the cavity plug 15 and enters the reaction cavity 17;

[0107] The control unit is electrically connected to the liquid level probe 11 and receives an electrical signal fed back by the liquid level probe 11 .

[0108] As an example, Figure 1 Region c shows the combined structure of the sample preparation reaction structure and the two-dimensional moving device.

[0109] In this example, the sample preparation reaction structure is mainly composed of a liquid level probe 11, a stirring gas pipe 12, a liquid inlet pipe 13, a waste liquid pipe 14, a cavity plug 15, a clamp 16 and a reaction chamber 17. The connection between the liquid level probe 11, the stirring gas pipe 12, the liquid inlet pipe 13, the waste liquid pipe 14, the cavity plug 15, the clamp 16 and the reaction chamber 17 is as follows: Figure 1 c. It should be noted that the reaction chamber 17 is a test tube in this example, and the cavity plug 15 is a tube plug with four through holes corresponding to the size of the test tube; the liquid level probe 11 is a non-contact probe to avoid contamination of the sample by materials, etc., and is specifically a laser ranging probe or a microwave ranging probe.

[0110] The liquid level probe 11 can be set to high-density sampling to detect high and low liquid level values ​​in real time and feed back to the control unit.

[0111] The stirring air pipe 12 is fixed on the cavity plug 15 and can move along the Z axis with the cavity plug 15. After passing through the cavity plug 15 and inserting 15 cm, Figure 1 The state shown in area c is when it just reaches the bottom of the reaction chamber 17, which is used to bubblingly disturb the original sample to achieve the purpose of stirring.

[0112] The liquid inlet tube 13 is fixed on the cavity plug 15 and can also move in the Z-axis direction with the cavity plug 15. After passing through the cavity plug 15 and inserted 5cm, it is used to add reaction reagents.

[0113] The waste liquid pipe 14 is fixed on the first Z-axis lifting platform 18 in the two-dimensional moving device, and can move along the Z-axis direction with the first Z-axis lifting platform 18. Its height is determined by the height of the first Z-axis lifting platform 18. It is movably connected to the cavity plug 15, is not fixed, and can freely pass through the cavity plug 15. Figure 1 In the state shown in area c, the waste liquid pipe 14 passes through the opening and penetrates the first Z-axis lifting platform 18 and the cavity plug 15, and is inserted 5 cm.

[0114] The cavity plug 15 is made of glass material, and has four through holes in the middle, which are used to insert the liquid level probe 11, the stirring gas pipe 12, the liquid inlet pipe 13 and the waste liquid pipe 14. The upper diameter of the tube plug is 2 cm larger than the lower diameter, and the upper part of the tube plug is fixed on the second Z-axis lifting platform 19 in the two-dimensional mobile device by the clamp 16; the lower part is a frosted surface with a height of 3 cm, which is used to connect with the frosted opening of the upper part of the reaction chamber 17. The lower diameter of the cavity plug 15 matches the opening diameter of the reaction chamber 17. It is completed in the reaction chamber 17 with a frosted opening, which effectively avoids the contamination of the sample by exogenous substances such as environmental dust.

[0115] The clamp 16 is a buckle clamp, which is fixed on the second Z-axis lifting platform 19 in the two-dimensional moving device, and is used to fix the cavity plug 15 and provide support force for the cavity plug 15 to rise and fall with the second Z-axis lifting platform 19.

[0116] The reaction chamber 17 is made of glass, and its height, diameter and capacity are determined according to the preparation requirements, and are usually 150-500 ml. Figure 1 As shown in area c, the reaction chamber 17 is usually placed in a corresponding heating groove in the heating structure.

[0117] The heating component is a graphite furnace 20, which is used to provide heating function for the original sample to undergo chemical reaction or drying in the reaction chamber 17. The heating temperature and start and stop time of the graphite furnace 20 are controlled by the control unit according to the preparation needs. The number of heating slots in the graphite furnace 20 can be increased or decreased according to design needs, such as Figure 3 The graphite furnace 20 is shown as having 6 heating slots. The graphite furnace 20 is fixed on an X-axis moving platform 21, and moves forward and backward in the X-axis direction, and the moving distance is determined by the moving amplitude of the X-axis moving platform 21.

[0118] The two-dimensional moving device is mainly composed of a Z-axis lifting slide bar 10, a first Z-axis lifting platform 18, a first Z-axis lifting guide rail 24, a second Z-axis lifting platform 19, a second Z-axis lifting guide rail 25, an X-axis moving platform 21, an X-axis moving guide rail 22, a chassis 23 and a device housing 30, and the above components are all made of stainless steel. Figure 1 c shows a cross-sectional view of the two-dimensional moving device in the X direction. Figure 3 a is a three-dimensional structural diagram of the two-dimensional mobile device, and the connection relationship between the components is as follows: Figure 3 As shown in a.

[0119] Four Z-axis lifting slide bars 10 are vertically fixed at the four corners of the chassis 23 to maintain the stability of the first Z-axis lifting platform 18 and the second Z-axis lifting platform 19 . Figure 3 As shown in a, at the center position of the left and right sides of the device housing 30, a first Z-axis lifting rail 24 and a second Z-axis lifting rail 25 are respectively vertically fixedly installed in a gantry-style symmetrical manner. Taking the first Z-axis lifting rail 24 on the left side as an example, they are parallel to the first Z-axis lifting rail 24 on the opposite side (right side) and the second Z-axis lifting rail 25 on this side (left side), and the relative position relationship of the remaining Z-axis rails is the same as the first Z-axis lifting rail 24 on the left side, wherein the first Z-axis lifting rails 24 on both sides are used to provide lifting power transmission for the first Z-axis lifting platform 18, and the second Z-axis lifting rails 25 on both sides are used to provide lifting power transmission for the second Z-axis lifting platform 19. The X-axis moving rail 22 is horizontally fixedly installed on the chassis 23 along the X-axis direction to provide power transmission for the X-axis moving platform 21 to move on the X-axis.

[0120] The first Z-axis lifting platform 18 is provided with an opening, the diameter of which is kept consistent with the waste liquid pipe 14, and the position of the opening is kept concentric with the position of the opening corresponding to the waste liquid pipe 14 on the cavity plug 15. The waste liquid pipe 14 is fixed on the first Z-axis lifting platform 18. The second Z-axis lifting platform 19 is also provided with an opening, the diameter of which is kept consistent with the diameter of the lower part of the cavity plug 15, and the position of the opening is kept concentric with the heating tank of the bottom graphite furnace 20, and the fixture 16 is fixed at the opening. The number of openings of the first Z-axis lifting platform 18 and the second Z-axis lifting platform 19 is determined according to design requirements.

[0121] The first Z-axis lifting platform 18 and the second Z-axis lifting platform 19 are stacked up and down, wherein the first Z-axis lifting platform 18 is located above the second Z-axis lifting platform 19, and the four corners of the two lifting platforms are connected to four vertically installed Z-axis lifting slide bars 10 through sliders, and can be lifted and lowered under the action of external force. Figure 3 As shown in a, the left and right sides of the middle position of the first Z-axis lifting platform 18 and the second Z-axis lifting platform 19 are connected to the corresponding lifting rails through sliders, and the corresponding manner of the lifting rails and the lifting platforms is as described above. This connection method can ensure the stability of the first Z-axis lifting platform 18 and the second Z-axis lifting platform 19, while also ensuring the synchronous lifting of the left and right sides of the lifting platform. The height of the platform lifting is controlled by the control unit according to the preparation needs to control the stepper motor in the guide rail, and the control accuracy can reach the millimeter level.

[0122] The graphite furnace 20 is fixedly mounted on the X-axis moving platform 21 and can move in the X-axis direction. The X-axis moving platform 21 is connected to the X-axis moving guide rail 22 through a slider, and the X-axis moving guide rail 22 is horizontally fixedly mounted on the chassis 23 along the X-axis direction. The moving distance of the graphite furnace 20 is controlled by the control unit to control the stepping motor in the X-axis moving guide rail 22 according to the preparation needs, and the control accuracy can reach the millimeter level.

[0123] like Figure 3 b shows the internal structure of the X-axis moving guide rail 22, the first Z-axis lifting guide rail 24 and the second Z-axis lifting guide rail 25. Each guide rail is composed of a stepper motor, a ball screw and a slider. Among them, each guide rail corresponds to a stepper motor, and the stepper motor is connected to the ball screw, and the stepper motor rotates to drive the ball screw to rotate. The slider is connected to the ball screw through a threaded port, and the ball screw rotates to drive the slider to move along the ball screw. The control unit drives the stepper motor to rotate, and the slider moves to the corresponding position accordingly.

[0124] In one embodiment, the liquid adding structure includes a plurality of reagent storage structures 5, a second multi-channel control valve 3 respectively connected to the plurality of reagent storage structures 5, a second peristaltic pump 2, and a second distributor 1 for equally distributing the derived reaction reagents;

[0125] The liquid inlet of the second multi-channel control valve 3 corresponds to the reagent storage structure 5; the liquid outlet of the second manifold 1 corresponds to the sample preparation reaction structure; the second multi-channel control valve 3 is connected to the second manifold 1 through the second peristaltic pump 2;

[0126] The control unit controls the on and off of the second multi-channel control valve 3 , and guides the reaction reagents in each of the reagent storage structures 5 to each of the sample preparation reaction structures through the second collector 1 by means of the second peristaltic pump 2 .

[0127] As an example, Figure 1 The liquid adding structure is shown in the a area. The liquid adding structure is mainly composed of the second manifold 1, the second peristaltic pump 2, the second multi-channel control valve 3, the hose 4 and the reagent storage structure 5. The second manifold 1, the second peristaltic pump 2, the second multi-channel control valve 3 and the reagent storage structure 5 are connected by the hose 4. Figure 1 In this example, the reagent storage structure 5 is a reagent bottle.

[0128] The second collector 1 is made of glass or Teflon material, and the number of its branch pipes can be increased or decreased according to design requirements. The figure shows an 8-branch structure, one of which is the liquid inlet branch, and the other branches are liquid outlet branches. Its function is to distribute the reagents in equal parts to Figure 1 Area c shows the reaction structures for preparing each sample.

[0129] The speed and start and stop time of the second peristaltic pump 2 can be controlled by a control unit.

[0130] The second multi-channel control valve 3 has multiple channels, the number of which can be increased or decreased according to design requirements, and each channel can be independently controlled by a controller to control its opening and closing time. The figure shows a 6-channel structure, and its internal detailed structure is as follows Figure 2 As shown, 6 liquid inlets (ie 6 channels) and 1 liquid outlet are provided, and their function is to pump various reagents into the collector and distributor through a pipeline by a peristaltic pump 1, thereby avoiding the use of multiple peristaltic pumps and complicated pipeline connections.

[0131] The material of the reagent storage structure 5 depends on the chemical reagent, and can be glass or Teflon. The capacity depends on the amount of chemical reagent used, and the number can be increased or decreased according to preparation needs. In this example, there are 5 reagents.

[0132] In one embodiment, the gas stirring structure includes a third multi-channel control valve 6 respectively connected to the plurality of sample preparation reaction structures, a gas washing chamber 8 for removing impurities from the gas source gas, and an air inlet pipe 7 for guiding the gas source gas into the gas washing chamber 8;

[0133] The gas outlet of the third multi-channel control valve 6 corresponds to the sample preparation reaction structure; the gas inlet pipe 7 and the gas inlet of the third multi-channel control valve 6 are respectively connected to the gas washing chamber 8;

[0134] The control unit is electrically connected to the third multi-channel control valve 6, and drives the switch of the third multi-channel control valve 6 to introduce the gas used for stirring the reaction reagents in the sample preparation reaction structure after the impurities are removed in the washing chamber 8 into the sample preparation reaction structure.

[0135] As an example, Figure 1 b shows a gas stirring structure. The gas stirring structure is mainly composed of a third multi-channel control valve 6, an air inlet pipe 7, a gas washing chamber 8 and a dispersion head 9. Among them, the third multi-channel control valve 6, the air inlet pipe 7, the gas washing chamber 8 and the dispersion head 9 are connected by a hose 4. Figure 1 Connect as shown in b.

[0136] The third multi-channel control valve 6 has multiple channels, the number of which can be increased or decreased according to design requirements, and the opening and closing time of each channel can be controlled independently by the control unit. This example is a 6-channel structure, with 6 outlets (i.e. 6 channels) and 1 inlet. Its function is to distribute the gas from the gas source to the Figure 1 c each stirring air pipe 12, and realize automatic control of air intake time and air intake channel.

[0137] The air inlet pipe 7 is used to connect the gas source, which can be compressed air, liquid argon or other inert gases. In order to avoid the contamination of the sample by acidic gases such as CO2 and particulate matter, a gas washing chamber 8 is designed, and the gas washing reagent is 1 mol·l -1 NaOH solution. The gas washing chamber 8 is made of Teflon, and its capacity is determined according to the preparation requirements.

[0138] In order to make the gas fully contact with the NaOH solution, a dispersion head 9 is provided at the tail end of the air inlet pipe 7. The dispersion head 9 is a shower-like structure with a plurality of air outlet holes.

[0139] Reference Figure 4 , shows a method for preparing a carbon isotope test sample provided by an embodiment of the present application, the method being applied to a carbon isotope test sample preparation device as described in any of the above embodiments, comprising:

[0140] S410, obtaining basic information of the sample and setting relevant preparation parameters;

[0141] S420, determining the sampling process parameters, the liquid feeding process parameters, the recovery process parameters, the elution process parameters, the drying process parameters, and the number of execution times of the recovery process according to the basic information of the sample and the relevant preparation parameters;

[0142] S430. Prepare the carbon isotope test sample according to the sampling process parameters, the liquid inlet process parameters, the recovery process parameters, the elution process parameters, the drying process parameters, and the number of execution times of the recovery process.

[0143] The carbon isotope test sample preparation method in this exemplary embodiment will be further described below.

[0144] In one embodiment, the step of preparing the carbon isotope test sample according to the sampling process parameters, the liquid feeding process parameters, the recovery process parameters, and the number of execution times of the recovery process includes:

[0145] Adding the original sample into the reaction chamber 17 according to the sampling process parameters;

[0146] Adding the reaction reagent into the reaction chamber 17 according to the liquid feeding process parameters;

[0147] Performing elution treatment on the reaction chamber 17 according to the elution process parameters;

[0148] Performing reaction waste liquid recovery processing according to the recovery process parameters, and determining whether the current recovery process number reaches the execution number;

[0149] If yes, the substance in the reaction chamber 17 is dried according to the drying process parameters; if no, the process returns to the step of adding the reaction reagent to the reaction chamber according to the liquid inlet process parameters, and recovering the reaction waste liquid according to the recovery process parameters, until the number of recovery processes reaches the execution number;

[0150] The prepared test sample is taken out according to the sampling process parameters.

[0151] In one embodiment, the sampling process includes:

[0152] Control the first Z-axis lifting platform 18 and the second Z-axis lifting platform 19 to lift to a specified height, and control the X-axis moving platform 21 to move forward a specified distance;

[0153] Adding the original sample into the reaction chamber 17; or taking out the test sample from the reaction chamber 17;

[0154] The first Z-axis lifting platform 18, the second Z-axis lifting platform 19, and the X-axis moving platform 21 are controlled to reset.

[0155] In one embodiment, the liquid feeding process includes:

[0156] Determine the number of open channels of the second multi-channel control valve 3, the pumping speed of the second peristaltic pump 2, the preset working time, and the delayed start time of the second multi-channel control valve 3 and the third multi-channel control valve 6 according to the relevant preparation parameters;

[0157] respectively start the peristaltic pump, the second multi-channel control valve 3 and the third multi-channel control valve 6;

[0158] Detecting the liquid level in the reaction chamber 17;

[0159] If the liquid level is greater than the warning value, the second multi-channel control valve 3 and the second peristaltic pump 2 are closed; if the liquid level is less than the warning value, it is determined whether the current working time of the second peristaltic pump 2 reaches the preset working time;

[0160] If the second peristaltic pump 2 reaches the preset working time, the second multi-channel control valve 3 and the third multi-channel control valve 6 are closed, and the second peristaltic pump 2 is set to be closed after reaching the first delayed closing time.

[0161] In one embodiment, the recycling process includes:

[0162] Wait for the preset waiting time;

[0163] Detecting the liquid level, and determining an assigned value according to the liquid level; wherein the assigned value = low liquid level value + preset safety value b;

[0164] Controlling the first Z-axis lifting platform 18 to descend to the position corresponding to the assigned value;

[0165] Starting the first multi-channel control valve 28, and starting the first peristaltic pump 27 at a preset pump speed;

[0166] When the pump speed of the first peristaltic pump 27 is greater than zero, the current liquid level is detected, and it is determined whether the high liquid level and the low liquid level are equal;

[0167] If so, the first peristaltic pump 27 and the first multi-channel control valve 28 are set to close after reaching the second delayed closing time.

[0168] In one embodiment, the rinsing process comprises:

[0169] Determining the elution time and elution temperature of the heating component according to the elution process parameters;

[0170] The heating group is started according to the elution time and the elution temperature.

[0171] In one embodiment, the drying process comprises:

[0172] Determining the drying time and drying temperature of the heating component according to the drying process parameters;

[0173] The heating component is activated according to the drying time and the drying temperature.

[0174] Reference Figure 5 and 6 In a specific embodiment, a coal isotope sample preparation experiment is performed. The existing extraction steps and requirements are as follows: Figure 5 shown.

[0175] According to the overall design of the control program, the program parameters H, L, X, t, t1-t6, T1-T2, S1-S2, a, b and n need to be specified in the experimental method file. Since the size of the two-dimensional mobile device determines H, L, a and b, Figure 1 The second Z-axis lifting platform 19 in the state shown in c is used as the reference surface of Z=0, and H=20cm, L=50cm, a=-5cm, b=2cm are set according to experience. According to experimental calculation, when the peristaltic pump speed is 1rps, the flow rate is 3.3ml·min -1 According to the preparation steps of the method of the present invention, the program parameters are designed as shown in Table 1. Figure 6 Shown is the logic diagram of the coal isotope sample preparation control program.

[0176] The existing coal sample preparation is mainly a simple acid-base pickling process. The devices used in the experiment are mainly hot plates and beakers, and the reagents used are 0.5M HCl and NaOH solutions. Figure 5 Although the experimental device is simple, the experimental steps are complicated.

[0177]

[0178] Table 1

[0179] Reference Figure 7 and 8 In another specific embodiment, the tree ring sample α-cellulose sample preparation is performed, and the existing extraction steps and requirements are as follows Figure 7 shown.

[0180] According to the overall design of the control program, the program parameters H, L, X, t, t1-t6, T1-T2, S1-S2, a, b and n need to be specified in the experimental method file. Since the size of the two-dimensional mobile device determines H, L, a and b, Figure 1 The second Z-axis lifting platform 19 in the state shown in c is used as the reference surface of Z=0, and H=20cm, L=50cm, a=-5cm, b=2cm are set according to experience. According to experimental calculation, when the peristaltic pump speed is 1rps, the flow rate is 3.3ml·min -1According to the preparation steps of the method of the present invention, the program parameters are designed as shown in Table 2. Fig. 9 Shown is the logic diagram of the control program for preparing α-cellulose from tree ring samples.

[0181] The prior art of preparing α-cellulose from tree ring samples mainly includes organic reagent elution, bleaching and acid-base pickling processes. The experimental equipment used for organic reagent elution is mainly electric heating mantle and Soxhlet extractor, and the reagents used vary from laboratory to laboratory, such as a mixture of CH3CH2OH and CHCl3 with a volume ratio of 1:1 and anhydrous CH3CH2OH solution; the experimental equipment used for the bleaching process is electric heating plate and beaker, and the reagents used vary from laboratory to laboratory, such as acidified NaClO2 solution or H2O2 solution; the experimental equipment used for acid-base pickling is mainly electric heating plate and beaker, and the reagents used are 1M concentration HCl and NaOH solutions. Existing experimental equipment such as Figure 7 The existing experimental steps are as follows Figure 8 ,There are many kinds of experimental devices, which are used separately and the experimental steps are complicated.

[0182]

[0183]

[0184] Table 2

[0185] Reference Fig.10 and 11 In another specific embodiment, the coal isotope sample preparation is performed, and the existing extraction steps and requirements are as follows Fig.10 shown.

[0186] According to the overall design of the control program, the program parameters H, L, X, t, t1-t6, T1-T2, S1-S2, a, b and n need to be specified in the experimental method file. Since the size of the two-dimensional mobile device determines H, L, a and b, Figure 1 The second Z-axis lifting platform 19 in the state shown in c is used as the reference surface of Z=0, and H=20cm, L=50cm, a=-5cm, b=2cm are set according to experience. According to experimental calculation, when the peristaltic pump speed is 1rps, the flow rate is 3.3ml·min -1 However, steps D4 and D8 in the experimental process cannot be integrated into this design and need to be completed manually. In addition, multiple samples cannot be prepared simultaneously and only one sample can be prepared at a time. According to the preparation steps of the method of the present invention, the design program parameters are shown in Table 3. Fig.11The figure shows the logic diagram of the control program for the preparation of humic acid from peat samples. It should be noted that steps D4 and D8 in the process cannot be integrated into this design and need to be completed manually. From the design of the program parameters, it can be seen that the supernatant of D3 should be extracted from the waste liquid barrel 29 of the third channel, 100 ml of concentrated HCl should be added, and the D4 humic acid should be precipitated at 80°C for 1 hour. The supernatant should be removed after centrifugation, and the residue (i.e. humic acid) should be freeze-dried for later use. The precipitate in the reaction chamber 17 after completing step D7 should be centrifuged to remove the supernatant, and the residue (i.e. humin) should be freeze-dried for later use. At this point, steps D4 and D8 are completed through the above-mentioned manual coordination, and the preparation process of humic acid from peat samples is completed.

[0187] The prior art peat sample humic acid extraction step is modified from the acid-base pickling experimental step. Its essence is the experimental process of obtaining humic acid by acid precipitation of the alkaline supernatant on the basis of the acid-base pickling experimental step ( Fig.10 ). Therefore, the main devices used in the experiment include hot plates, centrifuges, freeze dryers, beakers and other utensils, and the chemical reagents used are concentrated HCl, 0.5M HCl and NaOH solutions. There are many experimental devices, and they are used separately, and the experimental steps are complicated.

[0188]

[0189]

[0190] Table 3

[0191] A device comprises a processor, a memory and a computer program stored in the memory and capable of running on the processor, wherein the computer program implements the steps of the carbon isotope test sample preparation method as described above when executed by the processor.

[0192] A computer-readable storage medium stores a computer program, and when the computer program is executed by a processor, the steps of the carbon isotope test sample preparation method as described above are implemented.

[0193] Although the preferred embodiments of the present application have been described, those skilled in the art may make additional changes and modifications to these embodiments once they have learned the basic creative concept. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments and all changes and modifications that fall within the scope of the embodiments of the present application.

[0194] Finally, it should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or terminal device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or terminal device. In the absence of further restrictions, the elements defined by the sentence "comprise a ..." do not exclude the existence of other identical elements in the process, method, article or terminal device including the elements.

[0195] The carbon isotope test sample preparation device and preparation method provided by the present application are introduced in detail above. Specific examples are used in this article to illustrate the principles and implementation methods of the present application. The description of the above embodiments is only used to help understand the method of the present application and its core idea. At the same time, for general technicians in this field, according to the idea of ​​the present application, there will be changes in the specific implementation method and application scope. In summary, the content of this specification should not be understood as a limitation on the present application.

Claims

1. A carbon isotope test sample preparation device, the device is used to extract target components from an original sample to prepare a test sample, characterized in that: The invention comprises at least one sample preparation reaction structure, a liquid adding structure for introducing a reaction reagent into the sample preparation reaction structure, a gas stirring structure for introducing a gas into the sample preparation reaction structure to stir the reaction reagent, a control unit for driving the sample preparation reaction structure, the liquid adding structure and the gas stirring structure respectively, and a recovery structure for collecting the reaction waste liquid of the sample preparation reaction structure; The sample preparation reaction structure is mainly composed of a liquid level probe, a stirring gas pipe, a liquid inlet pipe, a waste liquid pipe, a cavity plug, a clamp and a reaction chamber; The recovery structure includes a first collector, a first peristaltic pump, a first multi-channel control valve and a plurality of waste liquid barrels; the liquid adding structure is mainly composed of a second collector, a second peristaltic pump, a second multi-channel control valve, a hose and a reagent storage structure; the gas stirring structure is mainly composed of a third multi-channel control valve, an air inlet pipe, a gas washing chamber and a dispersion head; The liquid adding structure and the gas stirring structure are respectively connected to the sample preparation reaction structure; the control unit is electrically connected to the sample preparation reaction structure, the liquid adding structure and the gas stirring structure, respectively. Specifically, the control unit drives the liquid adding structure to introduce the reaction reagent into the sample preparation reaction structure; the control unit drives the gas stirring structure to introduce the gas used for stirring the reaction reagent in the sample preparation reaction structure into the sample preparation reaction structure; the control unit drives the start and stop of the sample preparation reaction structure.

2. The device according to claim 1, characterized in that The recovery structure is used to collect the reaction waste liquid of the sample preparation reaction structure, The recovery structure is communicated with the sample preparation reaction structure and is electrically connected to the control unit; specifically, the control unit drives the recovery structure to suck out and recover the reaction waste liquid in the sample preparation reaction structure.

3. The device according to claim 2, characterized in that The liquid outlet of the first multi-channel control valve corresponds to and is connected to the waste liquid bucket; the liquid inlet of the first manifold corresponds to and is connected to the sample preparation reaction structure; the liquid inlet of the first multi-channel control valve is connected to the liquid outlet of the first manifold through the first peristaltic pump; The control unit drives the on and off of the first multi-channel control valve and the switch of the first peristaltic pump. Specifically, the control unit drives the first peristaltic pump to suck out the reaction waste liquid in each sample preparation reaction structure, and drives the on and off of the first multi-channel control valve to divert the reaction waste liquid to the corresponding waste liquid barrel.

4. The device according to claim 3, characterized in that The sample preparation reaction structure further includes: a sample preparation reactor, a heating component for heating the sample preparation reactor; The sample preparation reactor is arranged in the heating chamber of the heating assembly; the sample preparation reactor is connected to the liquid adding structure through a liquid inlet pipe; the sample preparation reactor is connected to the gas stirring structure through a stirring gas pipe; the sample preparation reactor is connected to the liquid inlet of the first collector in the recovery structure through a reaction waste liquid pipe; The control unit is electrically connected to the heating component. Specifically, the control unit heats the sample preparation reactor by driving a switch of the heating component.

5. The device according to claim 4, characterized in that Also included is a two-dimensional moving device for moving the sample preparation reaction structure, The two-dimensional moving device includes a first Z-axis lifting platform, a second Z-axis lifting platform, an X-axis moving platform, a Z-axis lifting guide rail, an X-axis moving guide rail and a chassis; The Z-axis lifting guide rail is vertically fixed on the surface of the chassis, and the X-axis moving guide rail is horizontally fixed on the surface of the chassis; The first Z-axis lifting platform and the second Z-axis lifting platform are respectively movably connected to the Z-axis lifting guide rail, and move up and down along the direction of the Z-axis lifting guide rail through the corresponding Z-axis stepper motor, wherein the first Z-axis lifting platform is located above the second Z-axis lifting platform; the X-axis moving platform is movably connected to the X-axis moving guide rail, and moves forward and backward along the direction of the X-axis moving guide rail through the X-axis stepper motor; The control unit is electrically connected to the Z-axis stepper motor and the X-axis stepper motor respectively, and drives the switches of the Z-axis stepper motor and the X-axis stepper motor; The reaction waste liquid pipe is fixed to the first Z-axis lifting platform of the two-dimensional moving device, and the reaction waste liquid pipe passes through the cavity plug of the sample preparation reactor to insert the pipe body into the reaction chamber of the sample preparation reactor. The reaction waste liquid pipe moves up and down along the Z-axis direction with the first Z-axis lifting platform to adjust the length of the pipe body inserted into the reaction chamber; The cavity plug is fixed to the second Z-axis lifting platform of the two-dimensional moving device, and the cavity plug is tightly connected to the reaction chamber, and the cavity plug drives the reaction chamber to move up and down along the Z-axis direction along with the second Z-axis lifting platform; The heating component is fixed to the X-axis moving platform of the two-dimensional moving device, and moves forward and backward along the X-axis direction along with the X-axis moving platform.

6. The device according to claim 5, characterized in that The liquid level probe is used to detect the liquid level of the reaction reagent in the reaction chamber; The liquid level probe penetrates through the cavity plug and enters the reaction cavity; The control unit is electrically connected to the liquid level probe and receives an electrical signal fed back by the liquid level probe.

7. The device according to claim 6, characterized in that The liquid adding structure includes a plurality of reagent storage structures, a second multi-channel control valve respectively connected to the plurality of reagent storage structures, a second peristaltic pump, and a second distributor for equally distributing the derived reaction reagents; The liquid inlet of the second multi-channel control valve corresponds to the reagent storage structure; the liquid outlet of the second manifold corresponds to the sample preparation reaction structure; the second multi-channel control valve is connected to the second manifold through the second peristaltic pump; The control unit controls the on-off of the second multi-channel control valve, and guides the reaction reagents in each of the reagent storage structures to each of the sample preparation reaction structures through the second manifold and distributor by means of the second peristaltic pump.

8. The device according to claim 7, characterized in that The gas stirring structure comprises a third multi-channel control valve respectively connected to the plurality of sample preparation reaction structures, a gas washing chamber for removing impurities from the gas source gas, and an air inlet pipe for guiding the gas source gas into the gas washing chamber; The gas outlet of the third multi-channel control valve corresponds to the sample preparation reaction structure; the gas inlet pipe and the gas inlet of the third multi-channel control valve are respectively connected to the gas washing chamber; The control unit is electrically connected to the third multi-channel control valve, and drives the switch of the third multi-channel control valve to introduce the gas used for stirring the reaction reagents in the sample preparation reaction structure after the impurities are removed in the gas washing chamber into the sample preparation reaction structure.

9. A method for preparing a carbon isotope test sample, the method being applied to the carbon isotope test sample preparation device as claimed in claim 8, characterized in that: include: Obtain basic sample information and set relevant preparation parameters; Determine the sampling process parameters, the liquid feeding process parameters, the recovery process parameters, the elution process parameters, the drying process parameters, and the number of execution times of the recovery process according to the basic information of the sample and the relevant preparation parameters; The carbon isotope test sample is prepared according to the sampling process parameters, the liquid feeding process parameters, the recovery process parameters, the elution process parameters, the drying process parameters, and the number of execution times of the recovery process.

10. The method according to claim 9, characterized in that The step of preparing the carbon isotope test sample according to the sampling process parameters, the liquid feeding process parameters, the recovery process parameters, the elution process parameters, the drying process parameters, and the number of execution times of the recovery process includes: Adding the original sample into the reaction chamber according to the sampling process parameters; Adding the reaction reagent into the reaction chamber according to the liquid inlet process parameters; Performing elution treatment on the reaction chamber according to the elution process parameters; Performing reaction waste liquid recovery processing according to the recovery process parameters, and determining whether the current recovery process number reaches the execution number; If yes, the substance in the reaction chamber is dried according to the drying process parameters; if no, the process returns to execute adding the reaction reagent to the reaction chamber according to the liquid inlet process parameters, and recovering the reaction waste liquid according to the recovery process parameters, until the number of recovery processes reaches the execution number; The prepared test sample is taken out according to the sampling process parameters.

11. The method according to claim 9, characterized in that The sampling process comprises: Controlling the first Z-axis lifting platform and the second Z-axis lifting platform to lift to a specified height, and controlling the X-axis moving platform to move forward a specified distance; Adding the original sample into the reaction chamber; or taking out the test sample from the reaction chamber; Control the first Z-axis lifting platform, the second Z-axis lifting platform, and the X-axis moving platform to reset.

12. The method according to claim 9, characterized in that The liquid inlet process comprises: Determining the number of open channels of the second multi-channel control valve, the pumping speed of the second peristaltic pump, the preset working time, and the delayed start time of the second multi-channel control valve and the third multi-channel control valve according to the relevant preparation parameters; respectively starting the peristaltic pump, the second multi-channel control valve and the third multi-channel control valve; Detecting the liquid level in the reaction chamber; If the liquid level is greater than the warning value, the second multi-channel control valve and the second peristaltic pump are closed; if the liquid level is less than the warning value, it is determined whether the current working time of the second peristaltic pump reaches the preset working time; If the second peristaltic pump reaches the preset working time, the second multi-channel control valve and the third multi-channel control valve are closed, and the second peristaltic pump is set to be closed after reaching the first delayed closing time.

13. The method according to claim 9, characterized in that The recycling process includes: Wait for the preset waiting time; Detecting the liquid level and determining a value based on the liquid level; Controlling the first Z-axis lifting platform to descend to the position corresponding to the assigned value; Starting the first multi-channel control valve, and starting the first peristaltic pump at a preset pump speed; When the pump speed of the first peristaltic pump is greater than zero, detecting the current liquid level, and determining whether the high liquid level and the low liquid level are equal; If so, the first peristaltic pump and the first multi-channel control valve are set to close after reaching a second delayed closing time.

14. The method according to claim 9, characterized in that The elution process comprises: Determining the elution time and elution temperature of the heating component according to the elution process parameters; The heating group is started according to the elution time and the elution temperature.

15. The method according to claim 9, characterized in that The drying process comprises: Determining the drying time and drying temperature of the heating component according to the drying process parameters; The heating component is activated according to the drying time and the drying temperature.

16. A device comprising a processor, a memory and a computer program stored in the memory and capable of running on the processor, wherein the computer program implements the steps of the method according to any one of claims 9 to 15 when executed by the processor.

17. A computer-readable storage medium storing a computer program, wherein the computer-readable storage medium stores a computer program, and when the computer program is executed by a processor, the steps of the method according to any one of claims 9 to 15 are implemented.

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