Multi-channel soil and sediment sulfide automatic measuring device
By designing a multi-channel soil and sediment sulfide automatic measurement device and automated processing of sample measurement processes, the problem of cumbersome manual operation and low efficiency in the prior art is solved, and efficient and safe multi-sample measurement is achieved.
Patent Information
- Application Number
- CN202411523737.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-29
- Publication Date
- 2025-02-07
AI Technical Summary
The prior art has cumbersome manual operations in soil and sediment sulfide measurement, which is inefficient and difficult to measure multiple samples at the same time, resulting in detection efficiency and safety problems.
A multi-channel soil and sediment sulfide automatic measurement device is designed, including acid reagent bottles, inert gas generators, absorbent bottles, reaction bottles, automatic quantitative liquid addition devices, absorbance measurement devices, etc., to realize the sample through automated processes Acidification, heating, absorption, color development and absorbance determination.
It greatly reduces manual operation steps and can measure multiple samples at the same time, improving detection efficiency and reducing operational risks.
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Figure CN119394940A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of ocean monitoring, and in particular to a multi-channel soil and sediment sulfide automatic determination device. Background Art
[0002] After the sulfide in the soil and sediment samples is acidified to generate hydrogen sulfide gas, the hydrogen sulfide is blown out by heating and blowing or distillation equipment, and absorbed by an absorbing liquid (sodium hydroxide or zinc acetate solution, etc.). The generated sulfide ions react with N,N-dimethyl-p-phenylenediamine in an acidic solution in the presence of ferric ions to generate methylene blue. Its absorbance is measured at a certain wavelength. The sulfide content is proportional to the absorbance value.
[0003] At present, there are sulfide pretreatment devices on the market, which only solve the process of acidifying the sulfide in the sample to generate hydrogen sulfide and absorbing it with absorption liquid. It still requires cumbersome manual operations, including but not limited to manual addition of absorption liquid, manual addition of reagents for color development, and manual measurement of absorbance on the machine.
[0004] Disadvantages of manual measurement:
[0005] (1) Only a single sample can be measured at a time, which is inefficient and not suitable for the measurement of large quantities of samples; (2) Manual acid addition requires opening the container during the acid addition process, resulting in hydrogen sulfide leakage; (3) The color development process requires opening the container to add reagents. Since the reagents are acidic media, their addition causes local reactions to generate hydrogen sulfide leakage; (4) Manual shaking requires opening the container again during the volume determination process, resulting in losses; (5) The pretreatment process is separated from the absorbance measurement process, which is cumbersome to operate; (6) Manual operation under high temperature conditions is highly risky.
[0006] In summary, providing a multi-channel soil and sediment sulfide automatic determination device is a technical problem that technical personnel in this field urgently need to solve. Summary of the invention
[0007] The purpose of the present invention is to provide a multi-channel soil and sediment sulfide automatic determination device to solve the problems existing in the above-mentioned prior art, which can greatly reduce the manual operation steps and can determine multiple samples at the same time, greatly improving the detection efficiency.
[0008] To achieve the above object, the present invention provides the following solutions:
[0009] The present invention provides a multi-channel soil and sediment sulfide automatic determination device, comprising an acid reagent bottle, an inert gas generating device, a pure water bottle, an absorption liquid bottle, a reagent bottle, a peristaltic pump, a plurality of absorption bottles, a plurality of reaction bottles, an automatic quantitative liquid adding device, an absorbance determination device, a heating device and a waste liquid collecting device;
[0010] Among them, the acid reagent bottle is used to hold acid solution, the inert gas generator is used to generate the required inert gas, the pure water bottle is used to hold pure water, the absorption liquid bottle is used to hold absorption liquid, the reagent bottle is used to hold reaction reagents, and the reaction bottle is used to hold samples;
[0011] The plurality of absorption bottles are arranged in sequence, and the plurality of reaction bottles correspond to the plurality of absorption bottles one by one and are arranged in sequence; each of the reaction bottles is connected with a liquid inlet and air inlet pipe and an air outlet pipe, and each of the reaction bottles is connected to the corresponding absorption bottle through the air outlet pipe;
[0012] The acid reagent bottle is connected with an acid outlet pipe, and the acid outlet pipe is provided with the automatic quantitative liquid adding device, the three-way solenoid valve for waste liquid discharge, the three-way solenoid valve for acid separation and the solenoid valve for acid separation in sequence from the head end to the tail end, wherein the three-way solenoid valve for waste liquid discharge is connected to the waste liquid collecting device through the waste liquid pipe 1, the acid separation solenoid valve is connected to the liquid and air inlet pipe on the reaction bottle at the end, and the liquid and air inlet pipes on the other reaction bottles are respectively connected to each of the three-way solenoid valves for acid separation;
[0013] The inert gas generating device is connected to a gas outlet main pipe, the ends of which are respectively connected to gas outlet pipe 1 and gas outlet pipe 2 through a gas outlet three-way solenoid valve, the gas outlet pipe 1 is connected to the acid outlet pipe at the rear end of the waste liquid three-way solenoid valve, the gas outlet pipe 2 is connected to the gas outlet pipe 3, and the gas outlet pipe 3 is respectively connected to the liquid and gas inlet pipes on each of the reaction bottles through a gas flow meter;
[0014] The bottom of each absorption bottle is provided with an inlet and outlet pipe, each inlet and outlet pipe is connected to the inlet and outlet pipe of the absorption bottle through an inlet and outlet three-way solenoid valve, one end of the inlet and outlet pipe of the absorption bottle is connected to the waste liquid collecting device, and a liquid detector is installed on the inlet and outlet pipe of the absorption bottle between the waste liquid collecting device and the absorption bottle, and the other end of the inlet and outlet pipe of the absorption bottle converges with the end of the reagent bottle outlet pipe on the reagent bottle and is connected to the absorbance measuring device through an absorbance measuring tube; the same peristaltic pump is installed on the inlet and outlet pipe of the absorption bottle and the outlet pipe of the reagent bottle, and the inlet and outlet pipe of the absorption bottle between the peristaltic pump and the absorbance measuring device are respectively connected to the absorption liquid outlet pipe and the pure water outlet pipe through the absorption liquid three-way solenoid valve and the pure water three-way solenoid valve, the absorption liquid outlet pipe is connected to the absorption liquid bottle, and the pure water outlet pipe is connected to the pure water bottle; a reagent solenoid valve is installed on the outlet pipe of the reagent bottle between the peristaltic pump and the absorbance measuring device;
[0015] The heating device is used to heat the reaction bottle.
[0016] Preferably, the inert gas generating device is a nitrogen generator.
[0017] Preferably, there are four absorption bottles, including absorption bottle 1, absorption bottle 2, absorption bottle 3 and absorption bottle 4. The inlet and outlet three-way solenoid valve 1, inlet and outlet three-way solenoid valve 2, inlet and outlet three-way solenoid valve 3 and inlet and outlet three-way solenoid valve 4 are respectively installed on the inlet and outlet liquid pipes at the bottom of absorption bottle 1, absorption bottle 2, absorption bottle 3 and absorption bottle 4.
[0018] Preferably, there are four reaction bottles, including reaction bottle one, reaction bottle two, reaction bottle three and reaction bottle four. The liquid and air inlet pipes of reaction bottle one, reaction bottle two, reaction bottle three and reaction bottle four are connected to the acid outlet pipe through acid separation three-way solenoid valve one, acid separation three-way solenoid valve two, acid separation three-way solenoid valve three and acid separation solenoid valve respectively. Gas flowmeter one, gas flowmeter two, gas flowmeter three and gas flowmeter four are respectively arranged on the liquid and air inlet pipes of reaction bottle one, reaction bottle two, reaction bottle three and reaction bottle four.
[0019] Preferably, there are two reagent bottles, including reagent bottle one and reagent bottle two, both of which are connected to the reagent bottle liquid outlet pipe, and the reagent solenoid valve includes reagent solenoid valve one and reagent solenoid valve two, and the reagent solenoid valve one and reagent solenoid valve two are respectively installed on the reagent bottle liquid outlet pipes on the reagent bottle one and the reagent bottle two.
[0020] Preferably, the automatic quantitative liquid adding device includes a motor, a threaded rod, a push-pull plate, a piston and a sleeve, the power output end of the motor is connected to the top of the threaded rod, the bottom end of the threaded rod is threadedly connected to one end of the push-pull plate, the other end of the push-pull plate is connected to the piston rod at the top of the piston, the piston is movably connected in the sleeve, the sleeve is connected to the acid outlet pipe between the waste liquid three-way solenoid valve and the acid reagent bottle, and the inner cavity of the sleeve is connected to the pipe channel of the acid outlet pipe.
[0021] Preferably, a one-way valve 1 is provided on the acid outlet pipe between the sleeve and the acid reagent bottle, and the one-way valve can prevent the acid liquid from flowing back into the acid reagent bottle; a one-way valve 2 is provided on the waste liquid pipe 1, and the one-way valve 2 can prevent the discharge liquid from flowing back into the acid outlet pipe.
[0022] Preferably, it also includes a liquid level detector, which is installed on a guide rail through a mobile device, and is used to detect the liquid level in the absorption bottle.
[0023] Preferably, the absorbance measuring device is arranged on the top of the waste liquid collecting device, and a quartz flow cell is arranged inside the absorbance measuring device, the inlet of the quartz flow cell is connected to the absorbance measuring tube, an outlet is arranged on the top of the quartz flow cell and connected to the overflow pipe of the waste liquid collecting device, and an outlet is arranged on the bottom of the quartz flow cell and connected to the waste liquid pipe 2 of the waste liquid collecting device, and a waste liquid discharge solenoid valve is arranged on the waste liquid pipe 2.
[0024] Preferably, the waste liquid collecting device is a waste liquid collecting barrel.
[0025] Compared with the prior art, the present invention has achieved the following technical effects:
[0026] The multi-channel soil and sediment sulfide automatic determination device of the present invention can automatically complete the processes of absorption liquid filling, sample acidification, heating and blowing, absorption, constant volume mixing, reagent addition and color development, absorbance determination, pipeline cleaning, etc., which greatly reduces the manual operation steps and can determine multiple samples at the same time, greatly improving the detection efficiency. BRIEF DESCRIPTION OF THE DRAWINGS
[0027] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.
[0028] Figure 1 It is a schematic diagram of the three-dimensional structure of the multi-channel soil and sediment sulfide automatic determination device from the first viewing angle of the present invention;
[0029] Figure 2 It is a schematic diagram of the three-dimensional structure of the multi-channel soil and sediment sulfide automatic determination device of the present invention from a second viewing angle;
[0030] Figure 3 It is a schematic diagram of the three-dimensional structure of the multi-channel soil and sediment sulfide automatic determination device of the present invention from a third viewing angle;
[0031] In the figure: 1, acid reagent bottle; 2, inert gas generating device; 3, pure water bottle; 4, absorption liquid bottle; 5, reagent bottle 1; 6, reagent bottle 2; 7, peristaltic pump; 8, absorption bottle 1; 9, absorption bottle 2; 10, absorption bottle 3; 11, absorption bottle 4; 12, reaction bottle 1; 13, reaction bottle 2; 14, reaction bottle 3; 15, reaction bottle 4; 16, automatic quantitative liquid adding device; 17, absorbance measuring device; 1 8. Heating device; 19. Waste liquid collection device; 20. Liquid and air inlet pipes; 21. Air outlet pipe; 22. Acid outlet pipe; 23. Three-way solenoid valve for waste liquid discharge; 24. Three-way solenoid valve for acid separation 1; 25. Three-way solenoid valve for acid separation 2; 26. Three-way solenoid valve for acid separation 3; 27. Solenoid valve for acid separation; 28. Waste liquid pipe 1; 29. Air outlet main pipe; 30. Three-way solenoid valve for air separation; 31. Air separation pipe 1; 32. Air separation pipe 2; 3 3. Gas distribution pipe 3; 34. Gas flow meter 1; 35. Gas flow meter 2; 36. Gas flow meter 3; 37. Gas flow meter 4; 38. Three-way solenoid valve 1 for inlet and outlet liquid; 39. Three-way solenoid valve 2 for inlet and outlet liquid; 40. Three-way solenoid valve 3 for inlet and outlet liquid; 41. Three-way solenoid valve 4 for inlet and outlet liquid; 42. Inlet and outlet pipes for absorption bottle; 43. Liquid detector; 44. Liquid outlet pipe for reagent bottle; 45. One solenoid valve for reagent; 46 , reagent solenoid valve 2; 47, absorption liquid three-way solenoid valve; 48, pure water three-way solenoid valve; 49, absorption liquid outlet pipe; 50, pure water outlet pipe; 51, liquid level detector; 52, guide rail; 53, absorbance measurement tube; 54, quartz circulation pool; 55, overflow pipe; 56, waste liquid pipe 2; 57, waste liquid discharge solenoid valve; 58, motor; 59, threaded rod; 60, push-pull plate; 61, piston; 62, sleeve. DETAILED DESCRIPTION
[0032] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0033] The purpose of the present invention is to provide a multi-channel soil and sediment sulfide automatic determination device to solve the problems existing in the prior art.
[0034] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.
[0035] The multi-channel soil and sediment sulfide automatic determination device in this embodiment is as follows: Figure 1-Figure 3As shown, it includes an acid reagent bottle 1, an inert gas generating device 2, a pure water bottle 3, an absorption liquid bottle 4, a reagent bottle, a peristaltic pump 7, a plurality of absorption bottles, a plurality of reaction bottles, an automatic quantitative liquid adding device 16, an absorbance measuring device 17, a heating device 18 and a waste liquid collecting device 19;
[0036] Among them, the acid reagent bottle 1 is used to hold acid solution, the inert gas generator 2 is used to generate the required inert gas, the pure water bottle 3 is used to hold pure water, the absorption liquid bottle 4 is used to hold absorption liquid, the reagent bottle is used to hold reaction reagents, and the reaction bottle is used to hold samples;
[0037] A plurality of absorption bottles are arranged in sequence, and a plurality of reaction bottles correspond to the plurality of absorption bottles one by one and are arranged in sequence; each reaction bottle is connected with a liquid inlet and air inlet pipe 20 and an air outlet pipe 21, and each reaction bottle is connected to the corresponding absorption bottle through the air outlet pipe 21;
[0038] The acid reagent bottle 1 is connected with an acid outlet pipe 22, and the acid outlet pipe 22 is provided with an automatic quantitative liquid adding device 16, a three-way solenoid valve 23 for discharging waste liquid, a three-way solenoid valve for acid separation, and an acid separation solenoid valve 27 in sequence from the head end to the tail end, wherein the three-way solenoid valve 23 for discharging waste liquid is connected to the waste liquid collecting device 19 through a waste liquid pipe 28, the acid separation solenoid valve 27 is connected to the liquid and air inlet pipe 20 on the reaction bottle at the end, and the liquid and air inlet pipes 20 on other reaction bottles are respectively connected to each three-way solenoid valve for acid separation;
[0039] The inert gas generating device 2 is connected to a gas outlet main pipe 29, the ends of which are connected to a gas outlet pipe 1 31 and a gas outlet pipe 2 32 respectively through a gas outlet three-way solenoid valve 30, the gas outlet pipe 1 31 is connected to the acid outlet pipe 22 at the rear end of the waste liquid three-way solenoid valve 23, the gas outlet pipe 2 32 is connected to a gas outlet pipe 3 33, and the gas outlet pipe 3 33 is connected to the liquid inlet and gas inlet pipes 20 on each reaction bottle through a gas flow meter;
[0040] The bottom of each absorption bottle is provided with an inlet and outlet pipe, each inlet and outlet pipe is connected to the absorption bottle inlet and outlet pipe 42 through an inlet and outlet three-way solenoid valve, one end of the absorption bottle inlet and outlet pipe 42 is connected to the waste liquid collecting device 19, and a liquid detector 43 is installed on the absorption bottle inlet and outlet pipe 42 between the waste liquid collecting device 19 and the absorption bottle, and the other end of the absorption bottle inlet and outlet pipe 42 is connected to the end of the reagent bottle outlet pipe 44 on the reagent bottle through the absorbance measuring tube 53 to the absorbance measuring device 17; The same peristaltic pump 7 is installed on the bottle inlet and outlet pipe 42 and the reagent bottle outlet pipe 44, and the absorption bottle inlet and outlet pipe 42 between the peristaltic pump 7 and the absorbance measuring device 17 is connected to the absorption liquid outlet pipe 49 and the pure water outlet pipe 50 respectively through the absorption liquid three-way solenoid valve 47 and the pure water three-way solenoid valve 48, the absorption liquid outlet pipe 49 is connected to the absorption liquid bottle 4, and the pure water outlet pipe 50 is connected to the pure water bottle 3; a reagent solenoid valve is installed on the reagent bottle outlet pipe 44 between the peristaltic pump 7 and the absorbance measuring device 17;
[0041] The heating device 18 is used to heat the reaction bottle.
[0042] In this specific embodiment, the inert gas generating device 2 is a nitrogen generator.
[0043] In this specific embodiment, four absorption bottles are provided, including absorption bottle 1 8, absorption bottle 2 9, absorption bottle 3 10 and absorption bottle 4 11. The inlet and outlet three-way solenoid valve 1 38, the inlet and outlet three-way solenoid valve 2 39, the inlet and outlet three-way solenoid valve 3 40 and the inlet and outlet three-way solenoid valve 4 41 are respectively installed on the inlet and outlet liquid pipes at the bottom of absorption bottle 1 8, absorption bottle 2 9, absorption bottle 3 10 and absorption bottle 4 11. There are four reaction bottles, including reaction bottle 1 12, reaction bottle 2 13, reaction bottle 3 14 and reaction bottle 4 15. The liquid and air inlet pipes 20 of reaction bottle 1 12, reaction bottle 2 13, reaction bottle 3 14 and reaction bottle 4 15 are connected to the acid outlet pipe 22 through acid separation three-way solenoid valve 1 24, acid separation three-way solenoid valve 25, acid separation three-way solenoid valve 26 and acid separation solenoid valve 27 respectively. Gas flowmeter 1 33, gas flowmeter 2 35, gas flowmeter 3 36 and gas flowmeter 4 37 are respectively arranged on the liquid and air inlet pipes 20 of reaction bottle 1 12, reaction bottle 2 13, reaction bottle 3 14 and reaction bottle 4 15.
[0044] In this specific embodiment, the automatic quantitative liquid adding device 16 includes a motor 58, a threaded rod 59, a push-pull plate 60, a piston 61 and a sleeve 62. The power output end of the motor 58 is connected to the top of the threaded rod 59, the bottom end of the threaded rod 59 is threadedly connected to one end of the push-pull plate 60, and the other end of the push-pull plate 60 is connected to the piston rod at the top of the piston 61. The piston 61 is movably connected in the sleeve 62, and the sleeve 62 is connected to the acid outlet pipe 22 between the waste liquid three-way solenoid valve 23 and the acid reagent bottle 1, and the inner cavity of the sleeve 62 is connected to the pipe channel of the acid outlet pipe 22.
[0045] In this specific embodiment, a one-way valve 1 is provided on the acid outlet pipe 22 between the sleeve 62 and the acid reagent bottle 1 , and the one-way valve can prevent the acid solution from flowing back into the acid reagent bottle 1 .
[0046] In this specific embodiment, a one-way valve 2 is provided on the waste liquid pipe 1 28 , and the one-way valve 2 can prevent the discharge liquid from flowing back into the acid outlet pipe 22 .
[0047] In this specific embodiment, a liquid level detector 51 is further included. The liquid level detector 51 is installed on a guide rail 52 through a mobile device. The liquid level detector 51 is used to detect the liquid level in the absorption bottle.
[0048] In this specific embodiment, the absorbance measuring device 17 is arranged on the top of the waste liquid collecting device 19, and a quartz flow cell 54 is arranged on the inner side of the absorbance measuring device 17. The inlet of the quartz flow cell 54 is connected to the absorbance measuring tube 53, and an overflow pipe 55 with an outlet connected to the waste liquid collecting device 19 is arranged on the top of the quartz flow cell 54. A waste liquid pipe 2 56 with an outlet connected to the waste liquid collecting device 19 is arranged at the bottom of the quartz flow cell 54, and a waste liquid discharge solenoid valve 57 is arranged on the waste liquid pipe 2 56.
[0049] In this specific embodiment, the waste liquid collecting device 19 is a waste liquid collecting barrel.
[0050] The multi-channel soil and sediment sulfide automatic determination device of the present invention has the following working process:
[0051] Preparation: Add the corresponding reagents to the acid reagent bottle 1, reagent bottle 1 5, reagent bottle 2 6, and absorption liquid bottle 4, and cover the bottle stoppers as shown. Add a quantitative sample to be tested (or a standard sample) and an appropriate amount of pure water (according to the experimental requirements) to the reaction bottle 1 12, reaction bottle 2 13, reaction bottle 3 14, and reaction bottle 4 15, and place each reaction bottle on the heating device 18 as shown, and cover the bottle stoppers. The following process is controlled by the built-in program and does not require manual operation.
[0052] (1) Filling with absorption liquid. The purpose is to draw the absorption liquid from the absorption liquid bottle 4 into the absorption bottle 1 8, the absorption bottle 2 9, the absorption bottle 3 10 and the absorption bottle 4 11. The reagent solenoid valve 1 45 and the reagent solenoid valve 2 46 are closed, the absorption liquid three-way solenoid valve 47 is opened in the direction from the absorption liquid bottle 4 to the peristaltic pump 7, the inlet and outlet three-way solenoid valve 1 38, the inlet and outlet three-way solenoid valve 2 39, the inlet and outlet three-way solenoid valve 3 40, and the inlet and outlet three-way solenoid valve 4 41 are opened in the direction from the peristaltic pump 7 to the liquid detector 43, the liquid detector 43 is turned on, the peristaltic pump 7 is turned on counterclockwise, and the absorption liquid in the absorption liquid bottle 4 flows toward the liquid detector 43. When the liquid detector 43 detects liquid, the peristaltic pump 7 is paused, and the inlet and outlet three-way solenoid valve 1 38 is opened in the direction from the peristaltic pump 7 to the absorption bottle 1 8. The peristaltic pump 7 is turned on and rotated counterclockwise to draw the absorption liquid into the absorption bottle 1 8, and the corresponding rotation time is set according to the program (the volume of the extracted liquid is calculated based on the rotation time of the peristaltic pump 7). After the set time is reached, the peristaltic pump 7 is paused, and the inlet and outlet three-way solenoid valve 1 38 is changed back to the direction leading to the liquid detector 43. The absorption bottle 1 8 is then filled with the set volume of absorption liquid. The opening direction of the inlet and outlet three-way solenoid valve 2 39 is changed to the peristaltic pump 7 leading to the absorption bottle 2 9. The peristaltic pump 7 continues to rotate counterclockwise, and fills the corresponding volume of absorption liquid into the absorption bottle 2 9 according to the set time. The inlet and outlet three-way solenoid valve 2 39 is changed back to the liquid detector 43. This process is repeated by analogy until the absorption liquid is filled into each absorption bottle, the peristaltic pump 7 is closed, the inlet and outlet three-way solenoid valve is changed back to the liquid detector 43, and the absorption liquid filling is completed. (At this time, there will be residual absorption liquid in the pipeline, which will be emptied according to the subsequent step 7).
[0053] (2) Emptying the acid reagent pipeline. Each time the machine is restarted before measuring the first sample, it automatically runs to exhaust the air in the acid reagent pipeline so that the acid reagent pipeline is filled with acid (no need to empty it during continuous measurement after starting the machine). The three-way electromagnetic valve 23 for discharging waste liquid opens from the acid outlet pipe 22 to the waste liquid pipe 28. The motor 58 is started and rotated counterclockwise, and the push-pull plate 60 is driven upward by the threaded rod 59 through the internal thread of the push-pull plate 60, thereby pulling the piston 61 upward, and then the acid in the acid reagent bottle 1 is pumped into the pipeline. After reaching the program setting time, the motor 58 rotates clockwise to exhaust the air in the sleeve 62 into the waste liquid collection device 19. The motor 58 reciprocates multiple times (the number of times is set by the program) until the sleeve 62 is filled with the set volume of acid.
[0054] (3) Heating: The heating device 18 is started to heat to a set temperature and maintain the set temperature.
[0055] (4) Acid is added to the reaction flask 12. The opening direction of the three-way solenoid valve 23 for discharging waste liquid is changed from the acid outlet pipe 22 to the three-way solenoid valve 24 for discharging acid. The opening direction of the three-way solenoid valve 24 for discharging acid is from the acid outlet pipe 22 to the reaction flask 12. The motor 58 is started to rotate clockwise to discharge the acid in the sleeve 62 to the reaction flask 12. The opening direction of the three-way solenoid valve 30 for discharging gas is from the gas outlet main pipe 29 to the three-way solenoid valve 24 for discharging acid. The inert gas generator 2 (nitrogen generator) is started. The nitrogen blows the acid remaining in the pipeline to the reaction flask 12, and at the same time discharges the air in the pipeline and the reaction flask 12 to avoid the loss caused by oxidation of sulfide. The nitrogen generator is paused. At the same time, the opening direction of the three-way solenoid valve 23 for discharging waste liquid is changed from the acid outlet pipe 22 to the waste liquid pipe 28. The automatic quantitative liquid adding device 16 is opened again to fill the sleeve 62 with the set volume of acid.
[0056] (5) Acid is added to other reaction bottles. After step (4) is completed, the direction of opening of the three-way electromagnetic valve 23 for discharging waste liquid is changed from the acid outlet pipe 22 to the three-way electromagnetic valve 1 for acid separation 24, the direction of opening of the three-way electromagnetic valve 1 for acid separation 24 is from the acid outlet pipe 22 to the three-way electromagnetic valve 2 for acid separation 25, and the direction of opening of the three-way electromagnetic valve 2 for acid separation 25 is from the three-way electromagnetic valve 1 for acid separation 24 to the reaction bottle 2 13. The motor 58 is started to rotate clockwise to discharge the acid in the sleeve 62 to the reaction bottle 2 13. The inert gas generator 2 (nitrogen generator) is started, and the nitrogen blows the acid remaining in the pipeline to the reaction bottle 2 13 and exhausts the air, and the nitrogen generator is paused. At the same time, the direction of opening of the three-way electromagnetic valve 23 for discharging waste liquid is changed from the acid outlet pipe 22 to the waste liquid pipe 1 28, and the automatic quantitative liquid adding device 16 is opened again to fill the sleeve 62 with the set volume of acid. And so on, until the set volume of acid is added to the four reaction bottles.
[0057] (6) Acidification, nitrogen blowing, and absorption. The purpose is to convert the sulfide in the sample into hydrogen sulfide gas through acidification, blow out the hydrogen sulfide with nitrogen, absorb it with absorption liquid, and use it for the next step of color development and determination. The heating device 18 maintains the set temperature, and the gas distribution three-way solenoid valve 30 opens in the direction of the gas outlet main pipe 29 to the gas distribution pipe 2 32, and then reaches the gas flowmeter 1 34, gas flowmeter 2 35, gas flowmeter 3 36 and gas flowmeter 4 37 (gas flowmeter with solenoid valve) on each gas distribution pipe 3 33 through the gas distribution pipe 2 32. The nitrogen generator is turned on, and the nitrogen enters each reaction bottle through the gas flowmeter. The nitrogen flow is controlled near the set value by the gas flowmeter 1 34, gas flowmeter 2 35, gas flowmeter 3 36 and gas flowmeter 4 37. After the reaction of the set time, the hydrogen sulfide gas generated by the reaction is blown to the absorption bottle 1 8, absorption bottle 2 9, absorption bottle 3 10 and absorption bottle 4 11. The heating device 18 is turned off.
[0058] (7) Volume adjustment. The purpose is to dilute the absorption liquid to the set volume after the reaction is completed and mix it for subsequent quantitative calculation. After step (6) is completed, the nitrogen generator is turned off, and the absorption liquid three-way solenoid valve 47 opens in the direction from the peristaltic pump 7 to the pure water three-way solenoid valve 48, and the pure water three-way solenoid valve 48 opens in the direction from the peristaltic pump 7 to the pure water bottle 3. Start the peristaltic pump 7 and rotate it counterclockwise to draw the pure water in the pure water bottle 3 into the pure water outlet pipe 50, and then flow into the waste liquid collection device 19 after passing through the peristaltic pump 7 to the inlet and outlet three-way solenoid valve four 41, the inlet and outlet three-way solenoid valve three 40, the inlet and outlet three-way solenoid valve two 39 and the inlet and outlet three-way solenoid valve one 38. This process, on the one hand, discharges the absorption liquid remaining in the pipeline after step (1) is completed to the waste liquid collection device 19, and on the other hand, cleans the pipeline. After the above steps are completed according to the set time, the peristaltic pump 7 is paused, the opening direction of the three-way electromagnetic valve 138 of the inlet and outlet liquid is changed to the peristaltic pump 7 leading to the absorption bottle 18, the liquid level detector 51 moves to the position opposite to the absorption bottle 18 through the guide rail 52 and starts the liquid level detection, the peristaltic pump 7 is turned on and rotates counterclockwise, the pure water enters the absorption bottle 18, and the peristaltic pump 7 is paused after the liquid level in the bottle reaches the detection interface of the liquid level detector 51, and the opening direction of the three-way electromagnetic valve 138 of the inlet and outlet liquid is changed to the peristaltic pump 7 leading to the waste liquid collection device 19, and the absorption bottle 18 is fixed in volume. The opening direction of the three-way electromagnetic valve 239 of the inlet and outlet liquid is changed to the peristaltic pump 7 leading to the absorption bottle 29, and the liquid level detector 51 moves to the position opposite to the absorption bottle 29 to start the liquid level detection, and the absorption bottle 29 is also fixed in volume. According to the above steps, the four absorption bottles are volume-fixed, the peristaltic pump 7 is turned off, the inlet and outlet three-way solenoid valve is changed back to the peristaltic pump 7 leading to the liquid detector 43, and the pure water three-way solenoid valve 48 is changed from the peristaltic pump 7 to the absorbance measuring device 17, and the volume fixing is completed. The nitrogen generator is turned on, and the nitrogen enters the absorption bottle after passing through the reaction bottle. The pure water and the absorption liquid in the absorption bottle are quickly mixed by gas agitation. After a certain period of time, the nitrogen generator can be turned off. An exhaust pipe for exhausting nitrogen is provided on each absorption bottle.
[0059] (8) Color development. This process is to react the absorption liquid with the reagent one in the reagent bottle one 5 first, and then react with the reagent two in the reagent bottle two 6. The solution after the reaction is used for the subsequent absorbance value determination. The opening direction of the three-way electromagnetic valve 38 of the inlet and outlet liquid is changed to be from the peristaltic pump 7 to the absorption bottle one 8. The peristaltic pump 7 is turned on and rotated clockwise to pump the absorption liquid out of the absorption bottle one 8 and flow along the three-way electromagnetic valve 38 of the inlet and outlet liquid and the peristaltic pump 7. After the set time, the reagent electromagnetic valve 45 is opened, and the reagent one is drawn out of the reagent bottle one 5 by the peristaltic pump 7 and mixed with the absorption liquid flow to react. Then the reagent electromagnetic valve two 46 is opened, and the reagent two in the reagent bottle two 6 is mixed with the above-mentioned mixed reaction liquid again after the peristaltic pump 7, and finally flows to the absorbance measurement device 17.
[0060] (9) Absorbance measurement. This step is to measure the absorbance value of the solution after the final reaction to calculate the sulfide content in the sample. The waste liquid discharge solenoid valve 57 is closed, and the peristaltic pump 7 is kept rotating clockwise. The solution after color development in step (8) enters the quartz circulation cell 54, and flows out from the overflow pipe 55 at the top after filling the circulation cell. The absorbance measurement device 17 is turned on to continuously measure the absorbance of the solution in the quartz circulation cell 54. After the absorbance value is stable (that is, the solution is evenly mixed and the reaction is sufficient), the data is automatically read and recorded. The waste liquid discharge solenoid valve 57 is opened, the reagent solenoid valve 1 45 and the reagent solenoid valve 2 46 are closed, and the peristaltic pump 7 continues to rotate clockwise to discharge all the absorption liquid in the absorption bottle 1 8 to the waste liquid collection device 19, and the peristaltic pump 7 is turned off. The waste liquid discharge solenoid valve 57 is closed, and the measurement of the sample in the sample bottle 1 is completed.
[0061] (10) Determination of samples 2, 3, and 4 in other sample bottles. The opening direction of the three-way solenoid valve 1 38 of the inlet and outlet liquid is changed to the absorption bottle 2 9. According to steps (8) and (9), the color development and determination of sample 2 are performed. Similarly, the determination of 4 samples is completed and all the absorption liquids are discharged into the waste liquid collection device 19.
[0062] The present invention uses specific examples to illustrate the principles and implementation methods of the present invention. The above examples are only used to help understand the method and core ideas of the present invention. At the same time, for those skilled in the art, according to the ideas of the present invention, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be understood as limiting the present invention.
Claims
1. A multi-channel soil and sediment sulfide automatic determination device, characterized in that: It includes an acid reagent bottle, an inert gas generating device, a pure water bottle, an absorption liquid bottle, a reagent bottle, a peristaltic pump, a plurality of absorption bottles, a plurality of reaction bottles, an automatic quantitative liquid adding device, an absorbance measuring device, a heating device and a waste liquid collecting device; Among them, the acid reagent bottle is used to hold acid solution, the inert gas generator is used to generate the required inert gas, the pure water bottle is used to hold pure water, the absorption liquid bottle is used to hold absorption liquid, the reagent bottle is used to hold reaction reagents, and the reaction bottle is used to hold samples; The plurality of absorption bottles are arranged in sequence, and the plurality of reaction bottles correspond to the plurality of absorption bottles one by one and are arranged in sequence; each of the reaction bottles is connected with a liquid inlet and air inlet pipe and an air outlet pipe, and each of the reaction bottles is connected to the corresponding absorption bottle through the air outlet pipe; The acid reagent bottle is connected with an acid outlet pipe, and the acid outlet pipe is provided with the automatic quantitative liquid adding device, the three-way solenoid valve for waste liquid discharge, the three-way solenoid valve for acid separation and the solenoid valve for acid separation in sequence from the head end to the tail end, wherein the three-way solenoid valve for waste liquid discharge is connected to the waste liquid collecting device through the waste liquid pipe 1, the acid separation solenoid valve is connected to the liquid and air inlet pipe on the reaction bottle at the end, and the liquid and air inlet pipes on the other reaction bottles are respectively connected to each of the three-way solenoid valves for acid separation; The inert gas generating device is connected to a gas outlet main pipe, the ends of which are respectively connected to gas outlet pipe 1 and gas outlet pipe 2 through a gas outlet three-way solenoid valve, the gas outlet pipe 1 is connected to the acid outlet pipe at the rear end of the waste liquid three-way solenoid valve, the gas outlet pipe 2 is connected to the gas outlet pipe 3, and the gas outlet pipe 3 is respectively connected to the liquid and gas inlet pipes on each of the reaction bottles through a gas flow meter; The bottom of each absorption bottle is provided with an inlet and outlet pipe, each inlet and outlet pipe is connected to the inlet and outlet pipe of the absorption bottle through an inlet and outlet three-way solenoid valve, one end of the inlet and outlet pipe of the absorption bottle is connected to the waste liquid collecting device, and a liquid detector is installed on the inlet and outlet pipe of the absorption bottle between the waste liquid collecting device and the absorption bottle, and the other end of the inlet and outlet pipe of the absorption bottle converges with the end of the reagent bottle outlet pipe on the reagent bottle and is connected to the absorbance measuring device through an absorbance measuring tube; the same peristaltic pump is installed on the inlet and outlet pipe of the absorption bottle and the outlet pipe of the reagent bottle, and the inlet and outlet pipe of the absorption bottle between the peristaltic pump and the absorbance measuring device are respectively connected to the absorption liquid outlet pipe and the pure water outlet pipe through the absorption liquid three-way solenoid valve and the pure water three-way solenoid valve, the absorption liquid outlet pipe is connected to the absorption liquid bottle, and the pure water outlet pipe is connected to the pure water bottle; a reagent solenoid valve is installed on the outlet pipe of the reagent bottle between the peristaltic pump and the absorbance measuring device; The heating device is used to heat the reaction bottle.
2. The multi-channel soil and sediment sulfide automatic determination device according to claim 1 is characterized in that: The inert gas generating device is a nitrogen generator.
3. The multi-channel soil and sediment sulfide automatic determination device according to claim 1 is characterized in that: There are four absorption bottles, including absorption bottle 1, absorption bottle 2, absorption bottle 3 and absorption bottle 4. The inlet and outlet three-way solenoid valve 1, inlet and outlet three-way solenoid valve 2, inlet and outlet three-way solenoid valve 3 and inlet and outlet three-way solenoid valve 4 are respectively installed on the inlet and outlet liquid pipes at the bottom of the absorption bottle 1, absorption bottle 2, absorption bottle 3 and absorption bottle 4.
4. The multi-channel soil and sediment sulfide automatic determination device according to claim 3 is characterized in that: There are four reaction bottles, including reaction bottle 1, reaction bottle 2, reaction bottle 3 and reaction bottle 4. The liquid and air inlet pipes of reaction bottle 1, reaction bottle 2, reaction bottle 3 and reaction bottle 4 are connected to the acid outlet pipe through acid-dividing three-way solenoid valve 1, acid-dividing three-way solenoid valve 2, acid-dividing three-way solenoid valve 3 and acid-dividing solenoid valve respectively. Gas flowmeter 1, gas flowmeter 2, gas flowmeter 3 and gas flowmeter 4 are respectively arranged on the liquid and air inlet pipes of reaction bottle 1, reaction bottle 2, reaction bottle 3 and reaction bottle 4.
5. The multi-channel soil and sediment sulfide automatic determination device according to claim 1 is characterized in that: The reagent bottles are provided with two, including reagent bottle 1 and reagent bottle 2, both of which are connected to the reagent bottle liquid outlet pipe, and the reagent solenoid valve includes reagent solenoid valve 1 and reagent solenoid valve 2, and the reagent solenoid valve 1 and reagent solenoid valve 2 are respectively installed on the reagent bottle liquid outlet pipes on the reagent bottle 1 and the reagent bottle 2.
6. The multi-channel soil and sediment sulfide automatic determination device according to claim 1, characterized in that: The automatic quantitative liquid adding device includes a motor, a threaded rod, a push-pull plate, a piston and a sleeve, the power output end of the motor is connected to the top of the threaded rod, the bottom end of the threaded rod is threadedly connected to one end of the push-pull plate, the other end of the push-pull plate is connected to the piston rod at the top of the piston, the piston is movably connected in the sleeve, the sleeve is connected to the acid outlet pipe between the waste liquid three-way solenoid valve and the acid reagent bottle, and the inner cavity of the sleeve is connected to the pipe channel of the acid outlet pipe.
7. The multi-channel soil and sediment sulfide automatic determination device according to claim 6, characterized in that: A one-way valve 1 is arranged on the acid outlet pipe between the sleeve and the acid reagent bottle, and the one-way valve can prevent the acid liquid from flowing back into the acid reagent bottle; a one-way valve 2 is arranged on the waste liquid pipe 1, and the one-way valve 2 can prevent the discharge liquid from flowing back into the acid outlet pipe.
8. The multi-channel soil and sediment sulfide automatic determination device according to claim 1 is characterized by: It also includes a liquid level detector, which is installed on a guide rail through a mobile device and is used to detect the liquid level in the absorption bottle.
9. The multi-channel soil and sediment sulfide automatic determination device according to claim 1, characterized in that: The absorbance measuring device is arranged on the top of the waste liquid collecting device, and a quartz circulation cell is arranged inside the absorbance measuring device. The inlet of the quartz circulation cell is connected to the absorbance measuring tube, and an outlet is arranged on the top of the quartz circulation cell to connect to the overflow pipe of the waste liquid collecting device. The bottom of the quartz circulation cell is arranged to connect to the waste liquid pipe 2 of the waste liquid collecting device, and a waste liquid discharge solenoid valve is arranged on the waste liquid pipe 2.
10. The multi-channel soil and sediment sulfide automatic determination device according to claim 1, characterized in that: The waste liquid collecting device is a waste liquid collecting barrel.