CN114280224A - Device for sample tube digestion and titration - Google Patents
Device for sample tube digestion and titration Download PDFInfo
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- CN114280224A CN114280224A CN202111615100.1A CN202111615100A CN114280224A CN 114280224 A CN114280224 A CN 114280224A CN 202111615100 A CN202111615100 A CN 202111615100A CN 114280224 A CN114280224 A CN 114280224A
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Abstract
The invention provides a device for sample tube digestion and titration, which comprises a condensation module, a heating module, a sample tube module, a linear module and a stepping motor, wherein the condensation module comprises a condensation tube disc and a condensation water pipeline; the sample tube module comprises a sample tube turntable, the surface of the sample tube turntable is provided with two or more circles of sample tube jacks, and each sample tube jack is vertically corresponding to the jack of the condensing tube disk; the surface of the heating module is provided with two or more circles of hole-shaped heating holes, and each heating hole is internally provided with a heating block, wherein each heating hole vertically corresponds to each sample tube insertion hole so as to accommodate a sample tube. Because sample tube or sample cup are fixed in the vertical direction for the condensation module cools the condensation tube according to the instruction, the heating module carries out cold heating to sample tube or sample cup, and realize that condensation tube and heating module break away from the sample tube respectively through sharp module, thereby realize the high throughput processing to titrating the sample simultaneously or differentiation.
Description
Technical Field
The invention relates to a device used in a Chemical Oxygen Demand (COD) tester, in particular to a device capable of realizing digestion and titration of a high-flux sample tube, belonging to the field of analytical chemical detection.
Background
Chemical-Oxygen-Demand (COD), which is abbreviated as COD, refers to the mass concentration of Oxygen in mg/L corresponding to the dissolved substances in water and the potassium dichromate which is a strong oxidant consumed by suspended substances under certain conditions. It is a comprehensive index for representing the reductive substances in the water body. The COD in the water body is too high, which indicates that the organic pollution is serious, and the balance of the environment and the biological community is damaged, so that the water body is deteriorated. Therefore, COD is an important parameter of sewage treatment plants and an important index for environmental monitoring.
The traditional chemical oxygen demand is divided into a permanganate method (also called permanganate index) and a potassium dichromate method according to different oxidation reagents, corresponding national standards are correspondingly established, the current national standard corresponding to the permanganate index is GB11892-1989 determination of water quality permanganate index, the current national standard for determining the chemical oxygen demand by the potassium dichromate method is HJ828-2017 determination of water quality chemical oxygen demand (hereinafter referred to as HJ828-2017 standard), the whole process of the existing determination scheme of the standard method is manually determined, manual operation equipment such as a user reflux device, a heating device, an acid burette and the like (detailed in 3-4 pages of the standard) is required, and the steps such as manual reagent addition, high-temperature reflux digestion, manual color end point titration and the like are carried out according to the standard requirements (detailed in 4-5 pages of the standard), the method can be widely applied to the determination of the chemical oxygen demand in surface water, domestic sewage and industrial wastewater, has the advantages of wide test range, good reproducibility, strong interference elimination, high accuracy and precision and the like, but still has the following problems in use:
(1) the method strictly stipulates the testing steps, such as heating digestion time, solution acidity, dosage of oxidant and catalyst and other condition indexes, and different testers inevitably produce testing errors in manual testing.
(2) The method has long time consumption, more required reagents and tools, high labor intensity and low efficiency when measuring a large number of samples.
(3) Reagents contacted in the experiment process have certain harm to human bodies, and gas released due to high-temperature digestion also has certain negative effects on the health of testers in the experiment.
(4) The method strictly stipulates that a digestion bottle (i.e. a conical bottle) should be added for heavy metal reagents (such as mercury sulfate and potassium dichromate standard solution) while anti-explosion boiling glass beads are prevented from shaking up. For low boiling point reagents (such as silver sulfate-sulfuric acid solution) should be added slowly from the upper end of the condenser tube to prevent the escape of low boiling point organics. This determines different reagents and different adding methods, so that different adding devices are needed.
According to the requirements of the above standards, semi-automatic instruments and equipment for solving part of the work of users appear on the market, for example, a COD automatic titration device is designed and developed according to the rain (research on chemical oxygen demand automatic titration device, current chemical research, 3 rd of 2019). The device utilizes the color sensor to simulate human eyes to recognize the color of the solution, and intelligently regulates and controls the titration speed according to the color, thereby accurately and quickly determining the titration end point. The titration apparatus consists of titration cell, injector, color sensor and electromagnetic stirring motor, and is connected via capillary of PTFE material and three-way solenoid valve. The titration cell is arranged on an alternating current stirring motor, and a stirrer is arranged in the titration cell. The injector is positioned above the titration cell and is connected with the three-way electromagnetic valve through a capillary tube, the three-way electromagnetic valve is connected with the ammonium ferrous sulfate standard solution through the capillary tube in the opening state, and the three-way electromagnetic valve is inserted into the titration cell through the capillary tube in the opening state. The color sensor is fixed at the position which is 10cm away from the plane under the titration cell. In use, the three-way valve is switched to the port a, and the standard solution of ferrous ammonium sulfate is pumped by the injection pump; adding an indicator into the cooled solution to be detected after digestion, and transferring the solution to a titration cell; turning on an electromagnetic stirring motor; switching the three-way valve to the port b, starting titration by the injection pump at a certain speed, outputting a signal when the color sensor senses the target color, and stopping the operation of the injection pump; and outputting the consumption of the ferrous ammonium sulfate to computer software, and calculating and displaying the measurement result by the software. However, the device only realizes the automatic titration of a limited number of sample tubes mainly by modifying the pipelines for sample feeding, liquid adding and titration and the electromagnetic valves thereof, and cannot realize the condensation and titration of high-throughput or large-batch sample tubes.
The Chinese invention application CN201810059775.4, a laboratory COD automatic analysis robot, discloses the automatic mechanical device, realizes the full process automatic analysis of sample addition to digestion reflux and color titration, and solves the full automatic application requirement. However, according to the mechanical anthropomorphic scheme adopted by the scheme, a plurality of mechanical control parts such as a plurality of mechanical clamping jaw groups and a plurality of sets of movable liquid adding arms are adopted, and in the actual production and application process, the defects of high mechanical structure design difficulty and complete machine fault rate, high production and assembly difficulty, low complete machine reliability and the like exist; and the glass magic mouth in the scheme is transferred and matched, so that data deviation caused by loose matching and component damage caused by collision in the matching process are easily caused.
Chinese patent application 202010197092.2, "a full-automatic chemical oxygen demand analyzer and its working process" discloses an analyzer including an automatic titration unit, wherein the automatic titration unit includes a lower liquid feeding assembly, a lower transmission mechanism, a detection unit, a light source bracket, a magnetic stirring mechanism, an optical sensor, etc., wherein the lower transmission mechanism includes a lower base sliding table; the lower base sliding table is slidably arranged on a guide rail of the lower liquid feeding transmission mechanism; a lower liquid adding arm is arranged on the lower base sliding table; a plurality of reagent channels can be arranged on the lower liquid adding arm; the magnetic stirring mechanism is also arranged on the lower base sliding table; when the lower liquid adding assembly moves to a certain digestion drop positioning position, the magnetic stirring mechanism is just positioned under the digestion drop positioning position, and the reagent passage outlet of the lower liquid adding arm is just positioned above the digestion drop positioning position. The lower base sliding table and the lower liquid adding arm of the device are complex in structure, and the titration positioning can only be moved in the horizontal direction, so that the titration speed is influenced.
Chinese patent application CN201110204582.1, entitled COD full-automatic on-line monitoring system and monitoring method thereof, discloses a monitoring device comprising an electric injector, an optical quantitative device, a multi-way adapter and a reaction tank. In the operation process, the electric injector is used for pumping air to enable the optical quantitative device to generate negative pressure, so that the measuring liquid and various reaction reagents are driven to enter the optical quantitative device through a sample introduction channel of the multi-way adapter, then gas is pressed in through the electric injector, and the liquid in the optical quantitative device enters the reaction cell one by one to carry out digestion reaction. In the reaction process, a detection electrode arranged in the reaction cell monitors the current change value of the solution in real time, so that the reaction end point is determined. After the reaction is finished, the electric injector is used for pumping air again, so that the waste liquid flows to the waste liquid pool through the multi-way adapter and the waste liquid flow path. Although the invention is simpler, the defects are as follows: an optical quantitative device similar to a buffer pool needs to be additionally arranged, and if all reaction solutions are contained at one time, digestion reaction is caused in advance, harmful gas and heat are generated, and the control is difficult; if the reaction solution is added and transferred one by one, excessive residue of the reaction solution is caused; the invention utilizes the change value of the monitoring current signal in the reaction tank, which is completely different from the prior titration tank device, thereby being not beneficial to the improvement and the application of the prior COD detector; in addition, the method adopts a potentiometric titration method for determination, and has substantial difference with the detection standard of the invention, wherein the high-pressure high-temperature rapid digestion is adopted, so that only the absorption, reagent addition, titration analysis and the like of a single sample can be completed, and the large-batch multichannel circulation rapid analysis in a laboratory cannot be realized.
The invention discloses a device capable of automatically fixing the volume of solution and reducing the accumulated error of liquid taking, and the invention is characterized in that the invention combines the laser triangulation distance measuring principle with the linear stepping motor positioning and horizontal moving rod technology to realize high-precision, flexible, random and continuous constant volume liquid taking, thereby ensuring the precision of the liquid volume measurement, changing the defect of the traditional mechanical fixed volume liquid taking and having higher effect. The Chinese patent application CN201521028392.9, the invention name "chemical oxygen demand detector" discloses a detector which comprises a sampling pump, a multi-way valve, a high-temperature high-pressure digestion chamber and a controller. Compared with the existing measuring instrument, the improved measuring instrument is characterized in that a high-pressure electromagnetic valve is arranged in the multi-way valve and the digestion chamber, and a liquid flow path can be opened and closed according to computer instructions so as to prevent high-pressure gas from impacting the multi-way valve. In addition, a high-pressure electromagnetic valve is also arranged at a waste liquid outlet at the bottom of the digestion chamber, so that the waste liquid can be automatically discharged conveniently.
As the closest prior art D2, chinese patent application 202010181373.9, "a COD analyzing apparatus" discloses a COD analyzing apparatus, which includes a box, a condensing and refluxing mechanism disposed above the box, a sample turntable disposed below the box and corresponding to the condensing and refluxing mechanism, a driving mechanism disposed below the sample turntable for driving the sample turntable to rotate, a heating module disposed below the sample turntable for heating the sample, a lifting mechanism for lifting the heating module, and a detecting apparatus for detecting the sample. The device embodies sample carousel and condenser pipe carousel about being equipped with two-layer, and wherein the heating module of sample carousel bottom can the lifting sample carousel rise, until with the condenser pipe butt joint. Then, be equipped with precession formula condenser pipe liquid feeding arm (first swinging boom) and buret liquid feeding arm (second swinging boom) respectively, wherein the liquid feeding arm can set up different rotation angle as required to reach the liquid feeding distance of different distances. In addition, a color sensor or a photoelectric sensor is arranged on the second liquid adding arm for monitoring. However, the device does not fully comply with the operating specification of the HJ828-2017 standard, namely: (1) in order to simplify the structure of the device, the device can only add liquid into heavy metal reagents and light boiling point reagents through a liquid adding arm of a condenser pipe; (2) because heating module fixed connection sample sabot to drive it and connect and break away from the condenser pipe, consequently after heating time, this heating module can not directly break away from sample sabot, can only wait that the inside heat of heating module disappears gradually, just can be shifted to titration position by heating module drive sample sabot. Otherwise, if the heating module drives the sample turntable to separate from the condensing tube, high-heat liquid in the digestion bottle is splashed, and the detection precision is influenced. Therefore, the design of this kind of heating module fixed connection sample sabot has prolonged the cooling time of digesting solution, is unfavorable for the demand of short-term test.
In addition, only one digestion solution adding hole is usually arranged in the current screw-in type liquid adding arm, if the liquid adding speed is too high, the liquid can be splashed due to rapid impact on sample liquid, if the liquid adding speed is too low, or manual sample adding is adopted according to the standard of the dichromate determination method for chemical oxygen demand of water quality of HJ828 and 2017, the liquid adding speed is too low, and the liquid adding efficiency is difficult to ensure. Meanwhile, the liquid adding arm is limited by the rotating shaft center, and only suitable for sample adding of a single-circle sample disc.
Therefore, a device which strictly meets the standard HJ828-2017 and can realize rapid cooling of digestion solution and high-flux liquid adding titration is needed at present.
Disclosure of Invention
The first principle of the invention is that a condensing module and a heating module are fixed on a pair of straight line modules which move vertically, the modules can move oppositely and move reversely to combine and separate, because a sample tube or a sample cup is fixed in the vertical direction, the condensing module cools the condensing tube according to an instruction, the heating module performs cold heating on the sample tube or the sample cup, and the condensing tube and the heating module are separated from the sample tube respectively, so that the sample tube digestion liquid can immediately separate the heating module, and the cooling speed is improved. Each condensing tube and each sample tube/sample cup can also correspond to one group of linear modules, and each heating module adopts an independent parallel heating structure, so that digestion, catalysis, cooling, separation of the condensing tubes and the sample tubes, and simultaneous or differential high-throughput processing of titrating the samples are realized.
The second principle of the invention is to arrange two disc structures to accommodate the condenser tube and the sample tube, wherein the disc insertion hole of the condenser tube vertically corresponds to the insertion hole of the sample tube turntable, and two or more circles of insertion holes can be arranged. Meanwhile, different from the existing design of only setting one liquid adding arm or liquid adding pipe, two liquid adding arms are creatively set, namely a first liquid adding arm for filling a low-boiling point reagent and a second liquid adding arm for filling a digestion liquid. The first liquid adding arm is fixed above the axis of the condensing tube disc, and two or more liquid adding ports are arranged on the first liquid adding arm, so that liquid can be added into the condensing tube/sample tube in two or more circles. The second liquid adding arm is not fixed on the axle center of the sample turntable but arranged outside the edge of the sample turntable in order to not prevent the heating module from contacting the sample turntable. Because the sample carousel and the jack of two circles or many circles of condenser pipe disc are the interval arrangement, consequently the corresponding relation of outer lane radius difference and liquid feeding arm rotation angle is utilized to the second liquid feeding arm to realize carrying out the liquid feeding for the sample cell on the jack of two circles or many circles.
The third principle of the invention is that on the basis of the above principle, the liquid adding head part of the second liquid adding arm is provided with 6 liquid adding thin tubes, and the 6 liquid adding thin tubes are uniformly distributed on the circumference and are separated from each other by a certain distance so as to avoid the mixing of reagents. Meanwhile, the head of each liquid adding tubule tube is subjected to inner diameter shrinkage treatment, so that when liquid is pumped out at a high speed, the influence on the adding amount of the reagent caused by the suspension of the residual liquid of the reagent on the head of the reagent tube is effectively avoided.
The fourth principle of the invention is that on the basis of the above principle, a vacancy recognition function is set for the sample tube installation position to prevent misoperation such as liquid adding, cooling or heating without placing the sample tube. Meanwhile, each heating block of the heating modules is automatically controlled in parallel connection, so that the test of a small amount of or full-scale samples can be flexibly arranged, and misoperation caused by sample tube vacancy is avoided.
Therefore, the first objective of the present invention is to provide a sample tube digestion and titration device for COD determination, comprising a condensation module, a heating module, a sample tube module, a linear module, and a stepping motor, wherein:
(1) the condensation module comprises a condensation pipe disc, a condensation water pipeline and a cold water container, wherein the surface of the condensation pipe disc is provided with two or more circles of condensation pipe jacks; the upper end of the condensation pipe is provided with a water inlet, the lower end of the condensation pipe is provided with a water outlet, and the condensation pipe is respectively communicated with a water chiller through a cold condensation water pipeline so as to form a cooling loop;
(2) the sample tube module comprises a sample tube turntable, the surface of the sample tube turntable is provided with two or more circles of sample tube jacks, and each sample tube jack is vertically corresponding to the jack of the condensing tube disk;
(3) the heating module is a disc with the diameter slightly larger than or equal to that of the sample tube turntable, two or more circles of porous heating holes are arranged on the surface of the disc, and a heating block is arranged in each heating hole, wherein each heating hole vertically corresponds to each sample tube insertion hole so as to accommodate a sample tube;
(4) the linear module comprises a coupler, an upper slide block, a lower slide block, an upper screw rod and a lower screw rod, wherein the upper slide block is fixed on the condensing module, the lower slide block is fixed on the heating module, the coupler is arranged at the middle position of the condensing tube disc and the sample tube turntable, the upper screw rod and the lower screw rod respectively pass through the upper slide block and the lower slide block and then are connected through the coupler, and due to different rotation directions of the upper screw rod and the lower screw rod, when a stepping motor connected with the shaft end at the upper end of the upper screw rod rotates, the upper screw rod and the lower screw rod respectively drive the upper slide block and the lower slide block to move in opposite directions or opposite directions, so that the condensing module and the heating module are driven to simultaneously and vertically approach or separate the sample tube;
(5) the fixed end of the first liquid adding arm is connected to the center of the condensing tube disc, two or more liquid adding holes are formed in the extending arm, and when the first liquid adding arm rotates around the center, the two or more liquid adding holes can pass through the positions right above the openings of the condensing tubes; a hollow pipeline is arranged in the first liquid adding arm and is communicated with the catalyst container;
(6) the fixed end of the second liquid adding arm is connected to the outer side of the edge of the sample turntable, and liquid is added to each sample tube on the jack with two or more circles by using different rotating angles at the rotating end of the second liquid adding arm.
In one embodiment, each of the heating modules is connected in parallel, and the heating of the received sample tubes by the single or multiple heating wells is controlled by the automatic controller. In one embodiment, a separate PCB platelet is provided under each heating block for control. In a preferred embodiment, the bottom of the heating module is divided into several zones, each provided with several monolithic PCB boards (e.g. circuit boards), so that each separate PCB lower board is integrated into a monolithic PCB board and a zone or integral heating of all heating blocks is achieved. In order to prevent the high temperature from affecting the operator and prevent the internal heat from radiating outwards to cause uneven heating, the outer side edge of the heating module is also provided with a heating area protection plate. In a more preferred embodiment, the heating block is a ceramic heating block or a ceramic heat generating sheet, and a temperature switch is provided to prevent the heating temperature from exceeding 300 ℃.
In another embodiment, the liquid adding hole heads of the first liquid adding arm and the second liquid adding arm are subjected to inner diameter shrinkage treatment, the inner diameter is only 0.5-1 mm, and the influence on the adding amount of the reagent due to the fact that the reagent residual liquid is hung on the liquid adding hole heads can be effectively avoided.
In another embodiment, the head part of the second liquid adding arm is provided with 6 liquid adding holes which are uniformly distributed on the circumference and are separated from each other by a certain distance to avoid reagent mixing.
In any of the above embodiments, the fixed end of the second liquid adding arm is provided with a color sensor and a light source which are adjacent to each other in a vertical direction, wherein the light source emits light to the sample tube to be detected along with the rotation of the liquid adding arm, and the color sensor receives the light reflected or scattered in the sample tube, i.e. the color detection is completed.
In one embodiment, when the color sensor detects no change in the light source, i.e., it is determined that no sample tube is placed in the receptacle, and a detection signal is fed back to the automatic controller, the software program instructs the sample tube turntable to rotate directly, skip the detection position, and stop the liquid feeding arm from titrating, wherein the software program is full-automatic Chemical Oxygen Demand (COD) analyzer analysis software system V1.0 software with copyright number 2020SR 0537238.
In a specific embodiment, the liquid feeding tip center of second liquid feeding arm is equipped with the camera, and the camera is rotatory along with the liquid feeding arm, can whole journey shoot the liquid feeding, the overall process of titrating, and the video can show on electronic screen or computer, can supply to observe or backtrack.
In any of the above embodiments, the sample tube turntable can horizontally rotate under the control of the automatic controller, and simultaneously, the rotation angle of the rotation end of the second liquid adding arm is matched to accelerate the sample adding process of the second liquid adding arm.
In any of the above embodiments, wherein the digestion tubes employ serpentine inner tubes to ensure adequate reflux of condensate during the heated digestion.
In any of the above embodiments, the automatic controller is a computer or a mobile phone, is connected to the device through wifi or bluetooth, and implements real-time monitoring or remote monitoring of digestion and titration processes according to preset program software.
In one embodiment, the program software is full-automatic Chemical Oxygen Demand (COD) analyzer analysis software system V1.0 software, with copyright number soft bibliographic registration No. 2020SR 0537238.
In any of the embodiments above, wherein the device is a device suitable for the HJ828-2017 standard.
Technical effects
1. According to the requirements of HJ828-2017, in order to realize that a low-boiling point reagent (silver sulfate-sulfuric acid solution) is slowly added from the upper end of a condenser tube and a digesting agent is slowly added from the upper end of a burette (namely a sample tube or a sample bottle), the linear module is used for folding and separating three modules (the condenser module, the adding module and the sample tube module), so that the heating module can be separated from a sample cup/the sample bottle/the sample tube as soon as possible to stop heating, the upper end of the sample tube is ensured not to be too far away from the condenser tube, and the defect that the sample splashes due to the fact that the heating module and the sample tube module are directly separated from the condenser tube is overcome.
2. The invention improves the fixing mode of the second liquid adding arm, namely the second liquid adding arm is arranged outside the edge of the sample tube turntable, so that the downward butt joint of the condensing tube turntable is not hindered.
3. The invention improves the liquid adding opening of the first liquid adding arm, adopts the arrangement of a plurality of liquid adding openings and is matched with the two or more circles of arranged condenser tubes, thereby realizing the simultaneous sample adding of the two or more circles of condenser tubes and improving the sample adding efficiency.
4. In order to simultaneously add samples to two or more circles of sample cups/sample bottles/sample tubes/burettes/titration bottles, the invention improves the liquid adding mode of the second liquid adding arm, namely, the liquid adding process of titrating two or more circles of sample tubes/sample bottles by one liquid adding hole is realized by matching with the rotation of the sample tube rotating disc through the swing arm angle of the second liquid adding arm and the radius difference between the inner circle and the outer circle of the sample tubes.
5. The sample tube can rotate but can not vertically lift, the condensing tube disc and the heating module can not rotate but can vertically lift, and the moving positions of the sample tube are controlled by the automatic controller to vertically correspond to the condensing tube and the heating hole, so that the condensing tube, the sample tube and the accelerating hole in each group can be ensured to be positioned in the same linear direction, and the condensing tube and the heating module are only moved at the same time, thereby avoiding the defects of liquid splashing or omission and the like caused by the movement of the sample tube, meeting the operating specification of the HJ828 standard and being beneficial to the rapid cooling of the liquid in the sample tube.
6. According to the invention, 6 liquid adding holes are formed in the liquid adding head of the second liquid adding arm, and the 6 liquid adding holes are internally provided with thin tubes which are uniformly distributed on the circumference and are separated from each other by a certain distance so as to avoid the mixing of reagents. The design avoids overlarge caliber of the liquid adding hole, and the high-temperature liquid is easily splashed by the thick-caliber liquid fluid when the titrant is added. Meanwhile, the design of the dispersed tubules can fill high-speed liquid, so that the sample filling speed is ensured.
7. According to the single heating hole and the heating block in the heating module, the heating speed is far higher than that of the whole heating block due to the small size of the heating block.
8. According to the invention, the independent PCB small plate is arranged at the bottom of each heating block to control the heating block, and the heating block can be independently heated under the action of the automatic controller.
9. The bottom of the whole heating module can be divided into a plurality of areas, and the independent small PCB plates under the large PCBs can be connected with the large PCBs to control different areas of the heating module, so that the heating module can be independently heated, or the heating module can be heated in the divided areas, or even heated integrally. This is advantageous in cases where the sample size is small and not all sample grades need to be heated.
10. According to the invention, the camera is arranged at the head part of the second liquid adding arm, the camera rotates along with the liquid adding arm, the whole process of liquid adding and titration can be shot in the whole process, and a video can be displayed on an electronic screen or a computer for observation or backtracking.
11. The fixed end of the second liquid adding arm is provided with a color sensor and a light source, and is matched with self-developed analysis software system V1.0 software (copyright number is soft registration number 2020SR0537238), so that the monitoring of the vacant position or the vacant liquid of the sample tube and the burette, namely the vacant position identification and vacant cup identification functions can be realized, and the misoperation of adding the sample reagent can be prevented when the sample cup is not placed or the reagent to be tested and the catalyst are not placed in the sample cup.
12. In the COD determinator of the invention, the reagent container is provided with the waste liquid overflow sensor and the pure water liquid level sensor, thereby having the liquid level detection function and preventing the liquid level from being too low or overflowing.
13. The COD tester of the invention does not need to transfer the sample in the testing process and is always in a sample cup. The valve and the pipeline are also avoided to be shared, and the different channels adopt independent pipelines and valves.
14. The invention adopts the design of two or more circles of sample grade, and can measure a large amount of samples in a limited space with high flux by matching with the corresponding condenser tube and the heating hole.
15. The COD tester is a closed box body, the upper part of the COD tester is provided with an exhaust pipe and a top exhaust fan, the COD tester can be conveniently connected with an exhaust system of a client, a side cooling fan is adopted to blow air from outside to inside on the design of an air channel, and the harmful gas generated in an experiment is collected as much as possible in a mode of exhausting air from the top, enters the exhaust system from the top and is exhausted out of a laboratory along with the exhaust system.
16. In order to ensure that the condensation reflux is sufficient in the heating digestion process, the digestion pipe adopts a snake-shaped inner pipe.
17. The COD tester is designed in a floor mode, does not occupy a laboratory table, and can be moved easily only by pushing the COD tester in the carrying process.
18. The panel of the outer box body of the COD tester is embedded with the electronic screen, so that the experiment progress can be displayed, and other information which needs to be known, such as an image displayed by a titration arm camera, can also be displayed. The box body is provided with a large-area organic glass observation window, and the experimental process can be directly observed. And has a video storage reference function.
19. The COD tester can be connected with wifi or connected with a computer or a mobile phone through Bluetooth, and can realize remote monitoring of the experimental state.
20. The COD tester disclosed by the invention realizes full automation and can work under the unattended condition.
Drawings
FIG. 1: a schematic perspective view of a COD analyzer comprising a sample tube digestion and titration apparatus.
FIG. 2: sample tube digestion and titration apparatus and first arm configuration, wherein the second arm is not shown.
FIG. 3: a second liquid adding arm in a perspective view.
FIG. 4: side view of sample tube module.
FIG. 5: a top view of the sample tube module.
FIG. 6: the internal structure of the heating module.
Legend:
1. a top exhaust fan, 2. an upper opening door, 3. an observation window, 4. a condensation pipe, 5. a condensation module, 6. a linear module, 7. a sample tube or a sample cup, 8. a sample tube rotating disc, 9. a heating zone protection plate, 10. a lower opening door, 11. a drawer, 12. a water cooler, 13. a water storage barrel, 14. a first liquid adding arm, 15. an electronic screen, 16. a second liquid adding arm, 17. a reagent connector, 18. a side cooling fan air inlet, 19. a reagent rack, 20. a coupler, 21. an upper screw rod, 22. a lower slide block, 23. an upper and lower fixed block (23.1 is an upper fixed block, 23.2 is a lower fixed block), 24. an upper slide block, 25. a lower screw rod, 26 heating module, 27. a camera (6 liquid adding holes are distributed around the camera), 28.1 a first liquid adding head of the first liquid adding arm, 28.2 a second liquid adding head of the first liquid adding arm, 29. a single PCB, 30. a whole PCB plate, 31. heating holes, 32. heating zone guard plate, 33 stepping motor.
Examples
The following examples are presented to enable one of ordinary skill in the art to more fully understand the present invention and are not intended to limit the scope of the embodiments described herein.
The device for sample tube digestion and titration for COD determination shown in FIGS. 1-2 comprises a condensation module (5), a heating module (26), a sample tube module, a stepping motor (33) and a linear module (6), wherein:
the condensation module (5) comprises a condensation pipe disc, a condensation water pipeline (not shown) and a cold water container (not shown), wherein the surface of the condensation pipe disc is provided with two or more circles of jacks of the condensation pipe (4); the upper end of the condensation pipe (4) is provided with a water inlet, the lower end of the condensation pipe is provided with a water outlet, and the condensation pipe is respectively communicated with the water cooler (12) through a condensation water pipeline, so that a cooling loop (not shown) is formed;
the sample tube module comprises a sample tube turntable (8), the surface of the sample tube turntable is provided with two or more circles of sample tube (7) jacks, and each sample tube (7) jack vertically corresponds to the jack of the condenser tube disk;
the heating module (26) is a disc with the diameter slightly larger than or equal to that of the sample tube turntable (8), and the surface of the heating module is provided with two or more circles of porous heating holes (31);
the linear module (6) comprises a coupler (20), an upper sliding block (24), a lower sliding block (22), an upper screw rod (21) and a lower screw rod (25), wherein the upper sliding block (24) is fixed on the condensing module (5), the lower sliding block (22) is fixed on the heating module (26), the coupler (20) is arranged at the middle position of the upper screw rod and the lower screw rod of the condensing tube disc and the sample tube rotary disc (8), the upper screw rod (21) and the lower screw rod (25) respectively penetrate through the upper sliding block (24) and the lower sliding block (22) and then are connected through the coupler (20), and due to different rotation directions of the upper screw rod and the lower screw rod, when a stepping motor (33) connected to the shaft end of the upper screw rod rotates, the upper screw rod and the lower screw rod respectively drive the upper sliding block and the lower sliding block to move in opposite directions or opposite directions, so as to drive the condensing module (5) and the heating module (26) to simultaneously and vertically approach or separate the sample tube (7);
the fixed end of the first liquid adding arm (14) is connected to the center of the condensing tube disc, two or more liquid adding holes are formed in the extending arm, and when the first liquid adding arm (14) rotates around the center, the two or more liquid adding holes can pass through the position right above the opening of each condensing tube (4); a hollow pipeline is arranged in the first liquid adding arm (14), and the pipeline is communicated with a catalyst container;
the fixed end of the second liquid adding arm (16) is connected with the outer side (not shown) of the edge of the sample tube rotating disc (8).
Fig. 1 shows that the linear module (6) starts to operate to drive the condensing module (5) to move downwards and the heating module (26) to move upwards until the condensing module (5) and the heating module (26) are close to the sample tube turntable (8) to reach the limit position; the linear module (6) shown in fig. 2 drives the heating module (26) and the condensing module (5) to be separated from the sample tube turntable (8) through a bidirectional screw rod structure.
As shown in fig. 3, the center of the head of the second liquid adding arm (16) is provided with a camera (27), the camera (27) rotates along with the liquid adding arm, the whole process of liquid adding and titration can be shot in the whole process, and the video can be displayed on an electronic screen (15) or a computer or a mobile phone and can be observed or traced back. Be equipped with 6 liquid feeding holes around camera (27), this liquid feeding hole evenly distributed in circumference, and all leave the mixture of certain distance avoiding reagent.
Fig. 4 shows that the fixed end of the first liquid adding arm (14) is connected to the center of the circular disc of the condenser tube, and the extending arm is provided with two liquid adding holes, namely a first liquid adding hole (28.1) and a second liquid adding hole (28.2), wherein when the first liquid adding arm (14) rotates around the center, the two liquid adding holes can pass through the upper part of each condenser tube opening; the first arm (14) is internally provided with a hollow pipe which communicates with a catalyst container (not shown).
The fixed end of the second liquid adding arm (16) shown in fig. 5 is connected to the outer side of the edge of the sample turntable, and the rotating end of the second liquid adding arm utilizes different rotating angles to add liquid to each sample tube (7) on the jack with two or more circles. The sample tube turntable (8) can horizontally rotate under the control of the automatic controller, and is matched with the rotation angle of the rotation end of the second liquid adding arm (16) to accelerate the sample adding process of the second liquid adding arm (16).
Fig. 6 shows the heating module (26) with the upper cover opened. Wherein each heating block (not shown) in the heating modules (26) is connected in parallel, and the heating blocks of the single or multiple heating holes (31) are controlled by the automatic controller to heat the accommodated sample tubes (7). In one embodiment, a separate PCB panel (29) is provided beneath each heating block for control. The bottom of the heating module (26) is divided into a plurality of areas, and a plurality of whole PCB boards (30) are respectively arranged, so that each independent PCB small board (29) is integrated to the whole PCB board (30), and the area or the whole heating of all the heating blocks is realized. In order to prevent the high temperature from affecting the operator and prevent the internal heat from radiating outwards to cause uneven heating, the outer side edge of the heating module is also provided with a heating area protection plate (32). Wherein, the heating block is a ceramic heating block or a ceramic heating sheet and is provided with a temperature switch to prevent the heating temperature from exceeding 300 ℃.
The use method of the device comprises the following steps:
in the determination of chemical oxygen demand, the tester prepares reagents and pure water for the experiment, and sets corresponding parameters through a computer connected with the instrument. Before the experiment is started, pure water can be extracted to wash the condensation pipe (4) by the first liquid adding arm (14).
As shown in fig. 1, a tester places a sample to be tested on the sample grade of a sample tube turntable (8), clicks to start testing, and a second liquid adding arm (16) rotates to a fixed liquid adding level, wherein the liquid adding levels of the inner ring and the outer ring of the sample tube (7) are two different fixed positions respectively; the sample tube turntable (8) rotates to sequentially rotate the sample tubes (7) to the fixed liquid adding level, the second liquid adding arm (16) sequentially adds digesting agents (such as potassium dichromate and mercury sulfate) into the sample cups, and a magnetic stirring device (not shown) continuously rotates during dripping. After all samples are added, the second liquid adding arm (16) resets, the linear module (6) starts to operate to drive the condensing module (5) to move downwards and the heating module (26) to move upwards until the condensing module (5) and the heating module (26) are drawn close to the sample tube turntable (8) to reach a limit position, the condensing tube (4) is embedded with the upper part of the sample tube (7) one by one, the positions of the heating holes (31) on the heating module are embedded with the bottom of the sample tube (7) one by one, and the first liquid adding arm (14) rotates to each sample position in sequence to add a catalyst (such as silver sulfate-silver sulfate). After all the sample cups are added, the instrument starts to heat and digest, and in the whole process, the outer pipe of the condensation pipe (4) is communicated with the water chiller (12) to carry out condensation and reflux so as to ensure that the liquid gasified due to heating is condensed and refluxed to the sample cups.
As shown in fig. 1-2, after the heating digestion is finished for a specified time, the heating block stops heating, the linear module (6) drives the condensing module (5) to move upwards and the heating module (26) to move downwards for a short stroke, the bottom of the sample cup is separated from the heating block, the sample cup and the condensing pipe (4) are not tightly embedded, at the moment, the side cooling fan (18) starts to work, the first liquid adding arm (14) rotates again, and pure water is added to each sample position. After the pure water is added, the linear module (6) continues to work until the condensation module (5) rises to the upper limit position, and the heating module (26) falls to the lower limit position. The sample tube turntable (8) starts to rotate, and meanwhile, the magnetic stirring device continuously rotates, so that the sample is promoted to be cooled as soon as possible.
The second liquid adding arm (16) rotates to a fixed liquid adding level again, wherein the liquid adding levels of the inner ring and the outer ring are respectively two different fixed positions, and the sample tube turntable (8) sequentially rotates the sample to the fixed liquid adding levels for titration.
After the test is finished, the sample tube turntable (8) resets, the linear module (6) works again, the condenser tube (4) and the sample cup are embedded again, and the first liquid adding arm (14) sequentially adds pure water to each sample grade for cleaning the condenser tube (4) and diluting the sample.
The linear module (6) works again, the condenser pipe (4) rises to the upper limit, and the sample cup can be taken out for cleaning.
Specific embodiments of the invention have been described above. It is to be understood that the invention is not limited to the particular embodiments described above, and that equipment and structures not described in detail are to be understood as being practiced in a manner common in the art; various changes or modifications may be made by one skilled in the art within the scope of the claims without departing from the spirit of the invention, and without affecting the spirit of the invention.
Claims (10)
1. The utility model provides a device that is used for COD survey's sample tube to clear up and titrate, includes condensation module, heating module, sample tube module, straight line module, step motor, wherein:
(1) the condensation module comprises a condensation pipe disc, a condensation water pipeline and a cold water container, wherein the surface of the condensation pipe disc is provided with two or more circles of condensation pipe jacks; the upper end of the condensation pipe is provided with a water inlet, the lower end of the condensation pipe is provided with a water outlet, and the condensation pipe is respectively communicated with a water chiller through a cold condensation water pipeline so as to form a cooling loop;
(2) the sample tube module comprises a sample tube turntable, the surface of the sample tube turntable is provided with two or more circles of sample tube jacks, and each sample tube jack is vertically corresponding to the jack of the condensing tube disk;
(3) the heating module is a disc with the diameter slightly larger than or equal to that of the sample tube turntable, two or more circles of porous heating holes are arranged on the surface of the disc, and a heating block is arranged in each heating hole, wherein each heating hole vertically corresponds to each sample tube insertion hole so as to accommodate a sample tube;
(4) the linear module comprises a coupler, an upper slide block, a lower slide block, an upper screw rod and a lower screw rod, wherein the upper slide block is fixed on the condensing module, the lower slide block is fixed on the heating module, the coupler is arranged at the middle position of the condensing tube disc and the sample tube turntable, the upper screw rod and the lower screw rod respectively pass through the upper slide block and the lower slide block and then are connected through the coupler, and due to different rotation directions of the upper screw rod and the lower screw rod, when a stepping motor connected with the shaft end at the upper end of the upper screw rod rotates, the upper screw rod and the lower screw rod respectively drive the upper slide block and the lower slide block to move in opposite directions or opposite directions, so that the condensing module and the heating module are driven to simultaneously and vertically approach or separate the sample tube;
(5) the fixed end of the first liquid adding arm is connected to the center of the condensing tube disc, two or more liquid adding holes are formed in the extending arm, and when the first liquid adding arm rotates around the center, the two or more liquid adding holes can pass through the positions right above the openings of the condensing tubes; a hollow pipeline is arranged in the first liquid adding arm and is communicated with the catalyst container;
(6) the fixed end of the second liquid adding arm is connected to the outer side of the edge of the sample turntable, and liquid is added to each sample tube on the jack with two or more circles by using different rotating angles at the rotating end of the second liquid adding arm.
2. The apparatus of claim 1, wherein each of the heating blocks is connected in parallel and the heating of the sample tubes received by the heating holes is controlled by an automatic controller, for example, a separate PCB board is provided under each heating block.
3. The apparatus of claim 2, wherein the bottom of the heating module is divided into several zones, and several single PCB boards are provided, respectively, such that the respective separate PCB lower boards are integrated into the single PCB board and the zone or the whole heating of all the heating blocks is achieved, wherein preferably the heating blocks are ceramic heating blocks or ceramic heat generating sheets, and a temperature switch is provided to prevent the heating temperature from exceeding 300 ℃.
4. The device according to any one of claims 1 to 3, wherein the liquid adding hole heads of the first liquid adding arm and the second liquid adding arm are subjected to inner diameter shrinkage treatment, the inner diameter is only 0.5-1 mm, and the influence on the adding amount of the reagent caused by hanging of reagent residual liquid at the liquid adding hole heads can be effectively avoided.
5. The device according to any one of claims 1 to 3, wherein said second arm head is provided with 6 filling holes, which are uniformly distributed around the circumference and are all separated by a certain distance to avoid reagent contamination.
6. The device of claim 5, wherein the fixed end of the second liquid adding arm is provided with a color sensor and a light source which are adjacent in the vertical direction, the light source emits light to the sample tube to be detected along with the rotation of the liquid adding arm, the color sensor receives the light reflected or scattered in the sample tube, and the color detection is completed, and/or a camera is arranged at the center of the liquid adding end head of the second liquid adding arm, the camera rotates along with the liquid adding arm, the whole process of liquid adding and titration can be shot in the whole process, and the video can be displayed on an electronic screen or a computer and can be observed or traced back.
7. The apparatus of claim 6, wherein when the color sensor detects no change in the light source, it is predicted that no sample tube is placed in the well, and a detection signal is fed back to the automatic controller, the software program instructs the sample tube carousel to rotate directly, skip the detection position, and stop the addition arm from titrating, wherein the software program is full-automatic Chemical Oxygen Demand (COD) analyzer analysis software system V1.0 software having copyright number 2020SR 0537238.
8. The device of any one of claims 1-7, wherein the sample tube carousel can rotate horizontally under the control of an automatic controller, and simultaneously cooperates with the rotation angle of the rotating end of the second liquid adding arm to accelerate the sample adding process of the second liquid adding arm, wherein the automatic controller is a computer or a mobile phone, is connected to the device through wifi or bluetooth, and implements real-time monitoring or remote monitoring of digestion and titration processes according to preset program software.
9. The apparatus according to claim 8, wherein the digestion tube adopts a serpentine inner tube to ensure sufficient reflux of condensate during heating digestion.
10. The device of any one of claims 1-10, wherein the device is a device adapted to the HJ828-2017 standard.
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| CN116106113A (en) * | 2022-12-14 | 2023-05-12 | 武汉新烽光电股份有限公司 | Digestion mechanism of water quality detector |
| CN116754523A (en) * | 2023-04-13 | 2023-09-15 | 上海市第一人民医院 | Secretion light transmittance analysis device for ovarian cancer diagnosis |
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