CN205719601U - Full-automatic microwave device - Google Patents

Full-automatic microwave device Download PDF

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CN205719601U
CN205719601U CN201620121841.2U CN201620121841U CN205719601U CN 205719601 U CN205719601 U CN 205719601U CN 201620121841 U CN201620121841 U CN 201620121841U CN 205719601 U CN205719601 U CN 205719601U
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sample
module
reagent
microwave
control system
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江成德
倪晨杰
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Shanghai Yiyao Instrument Technology Development Co Ltd
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Shanghai Yiyao Instrument Technology Development Co Ltd
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Abstract

This utility model provides a kind of full-automatic microwave device, at least one include that control system, Filtting device, microwave reaction module and sample add module, reagent adds module, catching up with acid cut molar block.Control system can control to move system carrying reaction vessel and add module, reagent interpolation module to microwave reaction module, sample, catch up with acid cut molar block or the placement location specified, and can control microwave reaction module, sample interpolation module, reagent interpolation module, catch up with acid cut molar block to realize respective function according to default running parameter.

Description

Full-automatic microwave device
Technical field
This utility model relates to technical field of microwave application, particularly to a kind of automatic for sample pre-treatments Processing means and method.
Background technology
Sample pre-treatments, i.e. sample be loaded to AAS (Atomic Absorption Spectrometry, former Sub-absorption spectrum) or HPLC (High Performance Liquid Chromatography, efficient liquid phase Chromatograph) etc. carry out on detecting instrument detecting before every pretreatment mode of employing, comprise organic and inorganic etc. before Processing mode, for inorganic samples pre-treatment, microwave sample pre-treating method with its efficient quickly feature, Be currently most commonly used, comprise sampling, acid adding, closed digestion tank assemble, clear up, sample transfer, Catch up with the steps such as acid cut appearance.During actual sample detects, these pre-treatment steps are all separate operation, and And be generally all manual operation.
Sampling, is generally artificial balance at present and puts in test tube after good for sample weighing.Acid adding, generally makes Reagent interpolation is carried out, it is also possible to buy automated reagent interpolation platform and carry out reagent with liquid adder or suction pipe Add, but cost is the highest, instrument poor compatibility each other.Counteracting tank assembles, the most manually Assembling, assembling process is loaded down with trivial details, and operator are readily accessible reagent.Clear up, use micro-wave digestion Method, oxidation rate is fast.Sample shifts, and is poured out by the digestion solution cleared up in counteracting tank, and cleaning is cleared up Tank skin remaining sample, this process is with acid gas a large amount of in counteracting tank, and misoperation is easily sucked by operator, with Time transfer not exclusively the most easily bring sample loss.Acid cut is caught up with to hold, by modes such as heating or negative-pressure vacuums, Residual acid within digestion solution is caught up with and removes, then add pure water and carry out constant volume.
Before one sample wants loading to analyze, it is necessary to through above-mentioned multiple working procedure, and step just can complete, except Balance to be purchased, liquid adder, microwave dissolver, catch up with outside the pre-processing devices such as acid cut looks, also very important person Work is sampled, tinning, transfer.Not only equipment is many, complex operation, and is readily incorporated personal error, Cause sample pre-treatments effect poor repeatability and affect subsequent analysis result.Tripolycyanamide the most in recent years, poison Capsule, the food and drug safety Frequent Accidents such as plasticiser and the Tsing-Hua University's laboratory blast thing occurred in the recent period Therefore so that on market to automatization, in high precision, the demand of the sample pre-treatments equipment of high stability more urgent Cut.
Utility model content
This utility model, for these problems, designs a kind of full-automatic microwave device and method, This device utilizes the design of rational structure, various high-precision sensor and executive component to also have the flow process control of specification System, assembles sampling, acid adding, closed digestion tank, clears up, sample shifts, it is loaded down with trivial details to catch up with acid cut to hold these Pre-treatment step automatization system must combine, it is achieved the automation mechanized operation of sample pre-treatments.
In order to realize object above, this utility model provides a kind of full-automatic microwave device, including Control system, microwave reaction module and sample add module, reagent adds module, catch up with acid cut molar block At least one;
Described control system controls described microwave reaction module according to parameter preset, sample adds module, reagent Add module, catch up with acid cut molar block, and control Filtting device at described microwave reaction module, sample interpolation mould Block, reagent add module, catch up with acid cut molar block and place mobile response container between region.
As preferably, described sample adds module and includes sample feeding chamber, solid adder, quantifier;
After sample adds described sample feeding chamber, and described reaction vessel is positioned at described sample and adds adding of module During sample position, described control system controls described solid adder and is added in reaction vessel, described quantifier Metering is added into the amount of sample in described reaction vessel, and metric results feeds back to described control system.
As preferably, described sample feeding chamber includes solid sampling chamber and Liquid sample introduction chamber, and described sample adds Add device and include solid adder and liquid adder;
Fluid sample adds from described Liquid sample introduction chamber, is added into described reaction by described liquid adder and holds In device, solid sample adds from described solid sampling chamber, adds described reaction by described solid adder and holds In device.
As preferably, also including sample comminution device in described sample interpolation module, solid sample is from described solid After body sample cavity adds, enter described sample comminution device, after sample pulverized by described sample comminution device, by institute State solid adder to add in described reaction vessel.
As preferably, described reagent adds module and includes reagent container, reagent sampling device and Level Detection Device;
Described liquid level detection device detects the amount of reagent in described reagent container, and testing result feeds back to institute State control system, described control system according to described testing result control described reagent sampling device to described instead Answer interpolation reagent in container.
As preferably, described in catch up with acid cut molar block to include heater, liquid appending apparatus;
Described control system controls described heater and heats described reaction vessel, described liquid with default temperature Body adding set, for adding liquid in described reaction vessel, makes the liquid in described reaction vessel be maintained at Preset vol.
As preferably, described microwave reaction module includes pressure detecting assembly and temperature sensing assembly;
Described pressure detecting assembly detects the pressure of reactant in described reaction vessel, and feeds back to described control System;Described temperature sensing assembly detects the temperature of reactant in described reaction vessel, and feeds back to described control System processed;Described control system controls microwave output according to force value and the temperature value of feedback.
As preferably, described microwave reaction module and/or catch up with in acid cut molar block and be respectively equipped with exhaust sub-system; Described exhaust sub-system is respectively used to microwave reaction module and/or catches up with the heat radiation in acid cut molar block.
As preferably, microwave reaction module and/or catch up with in acid cut molar block and be respectively equipped with several reative cells;
Control system can control the reaction environment in each reative cell respectively according to default parameter.
As preferably, the outlet of described exhaust sub-system is provided with device for recovering tail gas.
As preferably, described control system includes main control unit and sub-control unit;
Described sub-control unit is respectively arranged on described sample and adds module, reagent interpolation module, microwave reaction module And/or catch up with in acid cut molar block, and controlling corresponding module according to parameter preset, described main control unit is for institute State sub-control unit and send control signal, and receive feedback signal from described sub-control unit.
As preferably, also include cleaning assemblies;
Described control system controls described cleaning assemblies and cleans described sample feeding chamber, solid adder, sample Destructor, reagent container, reagent sampling device, liquid appending apparatus, pressure detecting assembly and/or temperature inspection Survey assembly.
This utility model additionally provides a kind of full-automatic microwave method, it is possible to use above-mentioned any one Described full-automatic microwave device, it would however also be possible to employ other microwave device.Including following Step:
S0, artificial setup control parameter on full-automatic microwave device;
S1, judge whether to need to add sample according to controlling parameter, if desired, then controlling Filtting device will be anti- Answer container to move to sample interpolation module, and add sample, otherwise enter step S2;
S2, judge whether to need to add reagent according to controlling parameter, if desired, then controlling Filtting device will be anti- Answer container to move to reagent interpolation module, and add reagent, otherwise enter step S3;
S3, judge whether to need microwave reaction according to controlling parameter, if desired, then controlling Filtting device will be anti- Answer container to move to microwave reaction module, otherwise enter step S5;
S4, according to control state modulator microwave reaction module change reaction environment, send microwave assisted reaction;
S5, judge whether to need to catch up with acid cut to hold according to controlling parameter, if desired, then controlling Filtting device will instead Answer container to move to catching up with in acid cut molar block, otherwise enter step S7;
S6, according to control state modulator catch up with acid cut molar block change catch up with acid cut hold condition, promote catch up with acid cut to hold;
S7, catch up with acid cut hold terminate after, control Filtting device reaction vessel is moved to placement location.
As preferably, in step sl, when reaction vessel is positioned at point of addition, control solid adder Being added in reaction vessel by sample, sample amount detecting device detects the sample size being added in reaction vessel, When sample size reaches to preset sample size, stop adding sample.
As preferably, before adding solid sample, control system controls sample comminution device and pulverizes sample.
As preferably, when adding solid sample, realize sample size by the weight of metering reaction vessel and measure; During adding liquid sample, realized by sample volume in the metering weight of reaction vessel or metering liquid adder Sample size is measured.
As preferably, in step s 2, if add reagent, reagent is held by reagent amount detecting device in real time Amount of reagent in device feeds back to control system, when the amount of reagent in reagent container is less than the minimum amount of reagent preset Time, control system is suspended and is added reagent in reaction vessel, after candidate agent supplements interpolation, continues to hold to reaction Device adds reagent.
As preferably, step S4 particularly as follows: after control system confirms that reaction vessel moves to microwave cavity, root According to default parameter, control magnetron microwave, the sample in reacting by heating container and reagent, sample and Reagent is heated and microwave irradiation, reacts, complete digestion process in reaction tube.
As preferably, step S6 particularly as follows: first control heater and heat within the scope of default temperature, Control system is by the liquid level of digestion solution in liquid level detection device monitoring reaction vessel, when digestion solution height After being reduced to catch up with acid preset value, control system controls sampling pump and adds distilled water in reaction vessel, makes reaction Reactant liquor in container is maintained at setting liquid level, it is achieved constant volume.
As preferably, in step S4 and step S6, control system also controls exhaust system and discharges microwave Reaction module or the acid in catching up with acid cut molar block or steam.
As preferably, after step S7, control system also control cleaning module clean sample add module and / or reagent add sample and/or the reagent of residual in module.
This utility model middle technical scheme used compared to existing technology, has the advantage that
1, system utilizes rational structure to design, and uses various sensor and executive component, by the stream of specification Process control, assembles sampling, acid adding, closed digestion tank, clears up, sample transfer, to catch up with acid cut to hold these numerous Trivial pre-treatment step automatization system must combine, it is achieved the automation mechanized operation of sample pre-treatments.
2, simple to operate.User has only to preset and automatically controls parameter, and sample is put into this pretreating device, System just can complete all flow processs of pre-treatment according to the default parameter that automatically controls.
3, in all of flow process, sample, reagent are all added in same reaction vessel so that whole In course of reaction, it is not necessary to migrate sample and reagent, it is to avoid sample and reagent remain in relaying container, Affect the concentration of sample and reagent, be the most also avoided that sample in transfer process, reagent contamination or loss, pole Big raising subsequent detection precision.
4, this full-automatic microwave device, microwave is reacted required for sample add module, Reagent adds module, microwave reaction module, catches up with acid cut molar block to be integrated in one, and decreases Experimental Area Number of devices, makes Experimental Area more succinct.
5, in whole experimentation, it is not necessary to the people possessing relevant professional knowledge carries out experimental implementation, only need Operating instrument to be trained.When needs carry out microwave, it is only necessary to teaching process personnel specifically set Put parameter, full automatic microwave can be realized, professional is liberated from complicated work load Out, it is to avoid various acid and the reagent personal injury to operator in pretreatment process, stop to clear up simultaneously The industrial accident that this high-temperature high-voltage reaction of process brings.
6, during whole course of reaction is in an environment more closed relatively, give out during preventing from catching up with acid The acid come is directly sucked in lung by people, improves experimental situation.
7, Automatic Control is passed through, it is possible to specification pre-treatment flow process, it is ensured that the standardization of pretreatment process, anti- Only because artificial uncertain factor causes pre-treatment result inaccuracy.
8, multiple different sample pre-treatment under the same conditions can be carried out, when saving microwave simultaneously Between, improve work efficiency.
9, in sample adds module, it is provided with the sample comminution device for comminuted solids sample, it might even be possible to Multistage sample comminution device is set, is crushed to solid sample meet the size that reaction requires, makes solid sample energy Enough fully reactions, promote the response rate of sample.
10, after completing whole full-automatic microwave process, control system can also control cleaning device To have contacted sample, the container of reagent cleans comprehensively, prevent because sample, reagent residue in container Or in adder, affect subsequent experimental.
11, for the exhausting problem caught up with in acid cut molar block and microwave reaction module, in this utility model, One group of exhaust sub-system it is provided with in acid cut molar block and microwave reaction module so that course of reaction produces catching up with Steam and sour gas can be discharged by this exhaust sub-system in time.At the same time it can also be in this air draft At the air outlet of subsystem, device for recovering tail gas is set, the steam produced in course of reaction and sour gas are inhaled Receive, prevent sour gas to be directly discharged in air, cause air pollution.
12, full-automatic microwave device provided by the utility model, be provided with a main control unit and Multiple sub-control unit, wherein, multiple sub-control unit are separately mounted to sample interpolation module, reagent adds module, Microwave reaction module and catch up with in acid cut molar block, in device operation, main control unit will be controlled accordingly Information processed is sent to sub-control unit, and each sub-control unit controls the process operation of corresponding module respectively, and feeds back The corresponding result that controls is to main control unit.By this kind of design, it is possible to efficiently reduce the amount of calculation of main control unit, Promote the processing speed of full-automatic microwave device.
13, native system can arrange different sample, reagent, heating condition, catch up with acid temperature each reaction tube The parameters such as degree, constant volume, in course of reaction, it is anti-that main control module can control other modules Should provide different reaction conditions and add the reagent of different volumes by pipe, final each reaction tube can have The different reaction condition of oneself, meets the pre-treatment demand of different sample.
14, it is scheduling controlling by control system unification module all to system, it is achieved all sample pre-treatments Datumization is followed the tracks of, and backs up and manages, meets U.S. EPA (US Gov Env Protection Agency) for data management Requirement is the biggest to promoting laboratory automation, data management standardization, offer work efficiency etc. to be respectively provided with Meaning.EPA data management mentioned here, refers to that U.S. EPA is for office automation and agrment information system System proposes, and laboratory equlpment and service data thereof are carried out consolidation form management, and equipment is all runs ginseng Number, tests relevant parameter including operator's information, time, method, service data etc. and is both needed to according to specific Form preserves, and facilitates related personnel to experimentation information and the inquiry of experimental result and management.
Accompanying drawing explanation
Fig. 1 is the system general diagram of this utility model one embodiment.
Fig. 2 is the Electronic Control block diagram of this utility model one embodiment.
Fig. 3 is the working-flow figure of this utility model one embodiment.
Detailed description of the invention
For making the purpose of this utility model, technical scheme and advantage clearer, below in conjunction with accompanying drawing to this Each embodiment of utility model is explained in detail.
For solving above-mentioned technical problem, the first embodiment of the present utility model provides a kind of full-automatic microwave Pretreating device, at least includes that control system, sample add module and microwave reaction module, it is also possible to include Reagent adds module and/or catches up with acid cut molar block.
In the present embodiment, on the basis of microwave reaction module is based primarily upon microwave cavity, magnetron, additional The peripheral functionality parts such as pressure transducer, temperature sensor, air draft cooling system.Microwave cavity is as microwave Coupled chamber, after Microwave emission is entered microwave cavity by magnetron, can be coupled into the micro-of some strength in cavity Wave field, the reaction tube (reaction vessel) equipped with sample and reagent is heated up under the irradiation of microwave, complete Become microwave reaction process.In this process, pressure transducer and temperature sensor are played inside monitoring reaction tube Temperature and pressure effect, and feed back to control system MCU after being amplified by amplifier by pressure and temperature signal (micro-control unit), MCU can according to set in advance temperature, pressure setting value, by D/A conversion and control The microwave output of magnetron, reaches to control reaction tube internal temperature and the purpose of pressure.Owing to microwave reaction belongs to In high-temperature high-voltage reaction, and the reagent used by reaction is substantially based on strong acid, so air draft cooling system is also The most necessary, this air draft cooling system (exhaust sub-system) can arrange the ventilation velocity of multiple gear, can To get rid of the acid gas in module in whole course of reaction in time, arrange according to by increase at cooling stage simultaneously Wind velocity accelerates the rate of cooling of reaction tube, shortens the time of whole course of reaction, improves microwave reaction Efficiency.Further, it is also possible to by arranging a device for recovering tail gas at the port of export of air draft cooling system.Should Device for recovering tail gas can be equipped with the container of alkaline solution, for being neutralized by acid gas, it is also possible to be to fill it He can absorb the container etc. of acid gas, prevents acid gas to be directly discharged in air, affects the health of experimenter.
In the present embodiment, it has been the functional module that sample adds automatically that sample adds module, mainly wraps Containing weighing apparatus (quantifier), liquid adder, solid adder these three core component and sample comminution device Deng accessory.Weighing apparatus, for measuring the weight of reaction tube, can be selected for balance, pressure ceramic sensor etc. Weight metering equipment;Liquid adder is used for the flowable sample such as adding liquid, paste class, can be selected for injection The equipment such as pump, peristaltic pump;Solid adder is similar to quantitative package machine on the market or proportional sampling device, uses In adding solid sample, if sample is not through pretreatment, volume ratio relatively greatly, can by sample comminution device, Big solid sample is carried out pulverization process, after having pulverized, carries out sample interpolation by solid adder again. If it is necessary, two groups of sample comminution devices can be arranged, wherein first group is used for carrying out big solid sample beating Broken process, carries out pulverization process by second group of sample comminution device by crushed sample the most again.By this Plant design so that when comminuted solids sample, the size pulverizing sample particle can not only be reduced, additionally it is possible to Promote the service life of Disintegrating knife in Sample Grinder.During work, main control module can control weighing apparatus and go Skin makes zero.Peeling zero refers to after being placed on weighing apparatus by empty reaction vessel, and weighing apparatus can be to this Reaction vessel is weighed, and now weight parameter will be adjusted by control system, being placed with reaction vessel Time measured weight be defined as 0.After weighing apparatus has been removed the peel, main control module sets according to sample in advance and plants Class and volume or weight, control liquid adder or sample is added in reaction tube by solid adder.? In sample adding procedure, main control module can monitor liquid adder and the volume of weighing apparatus and weight ginseng in real time Number, when the two value, wherein one or two reaches the preset value in system, and main control module i.e. can determine whether to add Sample completes.
In the present embodiment, reagent adds module i.e. automated fluid adder, is mainly made up of sampling pump, Simultaneously in order to monitor the volume of reagent bottle (reagent container) interior reagent, can annex solution level sensor, monitoring examination The volume of agent bottle interior reagent, when reagent solution bit comparison is low, feeds back to control system by liquid level information, control System prompts user processed adds reagent in time.During work, main control module adds volume according to the reagent preset, Controlling sampling pump, added to by reagent quantitative in reaction tube, in reagent adding procedure, liquid level sensor can be real Time liquid level signal is fed back to control system, when reagent very little, affect module when normally working, master control molding Block can suspend reagent and adds and point out user to supplement reagent, and after liquid level is recovered normally, module can continue work Make.The sampling pump that this module uses can be selected for the pump of the band function of measuring such as syringe pump, peristaltic pump or dosing pump, As long as this pump can meet accurately adding of reagent.
In the present embodiment, catch up with acid cut molar block mainly by heater, temperature sensor, sampling pump, Liquid level sensor and exhaust system composition.Reaction tube is positioned on heater, and main control module controls to pass through Drive circuit, controls electric hot plate (one of heater) and generates heat, thus reacting by heating pipe, reaction tube liter Wen Hou, the evaporation rate of quickening digestion solution within reaction tube, during this, temperature sensor is used for controlling The temperature of electric hot plate processed, liquid level sensor (liquid level detection device) is then the internal digestion solution of monitoring reaction tube Volume, the liquid level signal of main control module real-time reception liquid level sensor feedback, when digestion solution in reaction tube After volume reaches setting value, main control module controls sampling pump, adds the solution of certain volume in reaction tube, In guarantee test tube, the cumulative volume of digestion solution meets setting value.Electric hot plate mentioned here can be metal material Matter, it is also possible to for graphite material or other materials, module demand for heat can be met.Sampling pump is the most optional Pump with band function of measuring such as syringe pump, peristaltic pump or dosing pumps.In like manner, during catching up with acid cut to hold, Acid gas can be produced equally, therefore, an air draft cooling system and tail can also be set on acid cut molar block catching up with Aspiration receiving apparatus.
In the present embodiment, microwave reaction module and/or catch up with is respectively equipped with several reactions in acid cut molar block Room;Control system can control the reaction environment in each reative cell respectively according to default parameter.This System can arrange different sample, reagent, heating condition, catch up with acid temperature, constant volume body each reaction tube The parameter such as long-pending, in course of reaction, main control module can control other modules to be provided not for reaction tube Same reaction condition and the reagent of interpolation different volumes, final each reaction tube can have the difference of oneself Reaction condition, meet the pre-treatment demand of different samples.
In the present embodiment, Filtting device selects mechanical arm.Mechanical arm is as reaction tube in whole system Mobile instrument, it moves by control system control.Can be selected for X/Y/Z tri-shaft mechanical arm or the whirler of routine Mechanical arm, it is only necessary to can meet and accurately be picked and placeed in each module by reaction tube, does not makees remaining parameter etc. Limit.
In the present embodiment, control system comprises man machine interface, main control module MCU, drive circuit, puts Various chips, circuit and the programs such as big device, level conversion, D/A conversion.As shown in Figure 2.Control system master Human computer conversation to be completed, accepts operator's instruction and controls back-end circuit by program, passing through control circuit Control the order operation that rear end modules follow procedure sets, and by the procedural information run and final data Feed back in man machine interface, allow operator get information about the module of system current operating state and real time data. Owing to, in whole pretreatment process, the data processing amount related to is relatively big, as preferably, can will control System processed is divided into master control system and two parts of sub-control system, and wherein, master control system works for user setup Ambient parameter and the process etc. of signal, be sent to corresponding sub-control system by controlling parameter accordingly simultaneously. Sub-control system is respectively used to control sample and adds module, reagent interpolation module, microwave reaction module, catches up with acid cut In molar block, sample, the interpolation of reagent and course of reaction control, and corresponding result is fed back to master control system System.
In the present embodiment, after preventing reaction, sample and reagent remain in reagent, solid adds In the containers such as device, one can be designed and clean device, after completion of reaction, control system control to clean dress Put these containers of cleaning, when preventing subsequent reactions, the knot of the residue impact experiment of original reagent or sample Really.
Due to native system be based on microwave reaction module on the basis of, increased sample newly and added module, reagent and add Add module and catch up with acid cut molar block, and by outside robotic arm automation function, in the unification of main control module Under control, it is combined into a whole set of full-automatic microwave system.So user can arbitrarily configure required Module, if such as user selects manually to add sample, it is only necessary to configuration reagent adds module, microwave reaction Module, catch up with acid cut molar block and mechanical arm, it is possible to realize follow-up sample automatization pre-treatment;If used It is the highest that requirement is added for sample and reagent in family, can only select microwave reaction module, catch up with acid cut molar block And mechanical arm, it is achieved the pre-treatment of sample automatization;Also have the detecting instrument acid-fast ability nowadays having stronger, So can not carry out catching up with acid treatment after some Specimen eliminatings and direct sample detection, this kind of user just may not be used Acid cut molar block is caught up with in configuration, it is only necessary to according to the needs of oneself, option and installment microwave reaction module, sample add Add module, reagent adds one or several block combiner in module and mechanical arm.Generally speaking, native system It is can to select different functional modules according to the sample pre-treatments demand of user's reality, be combined into a set of complete Whole preprocessing system.After user has selected module and has been combined into system, the main control module of system I.e. can automatically identify the type of modules being currently configured, and show in man machine interface, user can be straight It is connected in man machine interface and sets corresponding workflow and method, complete the microwave of sample.Certainly, If system has the function of whole modules, and user selects some function or step not when method is arranged Processing, system also can complete pre-treatment work according to the establishing method of user.
This utility model additionally provides a kind of full-automatic microwave method, and the method can utilize above institute The device stated realizes, it is also possible to realized by other microwave devices.The workflow that the method is concrete As it is shown on figure 3, include five key steps:
Step one:
After user sets method and starts working, the main control module of system can judge according to parameter preset Whether automatic sample, moves to reaction tube sample add in module if it is, controls mechanical arm, if No, then carry out step 2.When determine be time, the main control module of system after confirming that reaction tube moves into place, First weighing apparatus is made zero, then according to the parameter of default, control liquid adder or solid adder Being added in reaction tube by sample, if default sample needs to do pulverization process, main control module can be controlled Sample is first pulverized by sample preparation product destructor, is added to by sample by solid adder after having pulverized again In reaction tube.In sample adding procedure, weighing apparatus can monitor the weight that sample adds in real time, by weighing The function of weighing of device and liquid adder determine volume function, sample can be completed accurately according to default value The sample-adding of product.Master control system, after completing sample interpolation, controls mechanical arm and from sample, reaction tube is added module Middle taking-up, carries out step 2.
Step 2:
Whether the main control module of system sets according to the parameter determination methods preset is automatic reagent adding, if It is then to control mechanical arm and reaction tube is moved in reagent interpolation module, if it is not, then carry out step 3. When determine be time, the main control module of system is after confirming that reaction tube moves into place, according to the body of default Long-pending parameter, controls sampling pump and is added in reaction tube from reagent bottle by reagent.In adding procedure, liquid level Sensor can in real time liquid level signal is fed back to main control module, when reagent very little, affect module and normally work Time, main control module can suspend reagent and adds and point out user to supplement reagent, after liquid level is recovered normally, and mould Block can work on, and completes automatic reagent adding process.Master control system, after completing reagent interpolation, controls machine Reaction tube is added taking-up module from reagent by mechanical arm, carries out step 3.
Step 3:
It is to need microwave reaction that the main control module of system sets according to the parameter determination methods preset, if Then control mechanical arm to be moved in microwave reaction module by reaction tube, if it is not, then carry out step 4.When really When being surely, the main control module of system is after confirming that reaction tube moves to microwave cavity, according to the temperature of default The parameters such as degree, pressure or time, control magnetron microwave, the sample in reacting by heating pipe and reagent, Sample and reagent are being heated and after microwave irradiation, are reacting, complete digestion process in reaction tube.? In digestion process, temperature sensor and pressure transducer can monitor the temperature and pressure parameter in reaction tube in real time, And by main control module, data are shown in man machine interface, allow operator understand the real-time process of reaction. In digestion process, air draft cooling system, by main control module control, can realize different air draft according to setting Speed regulates, it is achieved the acid discharge heat sinking function of module and reaction tube after having cleared up during microwave reaction Quick cooling function.After system receives reaction tube cooling END instruction, mechanical arm can be controlled by reaction tube Take out from microwave reaction module, carry out step 4.
Step 4:
It is to need to catch up with acid cut to hold that the main control module of system sets according to the parameter determination methods preset, if In then reaction tube is moved to catch up with acid cut molar block by control mechanical arm, if it is not, then carry out step 5.When really When being surely, the main control module of system after confirming that reaction tube moves into place, according to the temperature of default, The parameter such as time and constant volume, first controls heating devices heat, during heating devices heat, master control Molding block passes through temperature sensor, in real time monitoring heater temperature, makes heater temperature stabilization set In the range of.During heating devices heat, the digestion solution within reaction tube is also heated up, along with disappearing Solution liquid temp raises, and its evaporation rate is also and then accelerated, and now main control module can pass through liquid level sensor, The liquid level of digestion solution in monitoring reaction tube, after digestion solution volume arrives and catches up with acid setting value, master control molding Block can control sampling pump toward adding solution in reaction tube, by sampling pump and the liquid adding functions of liquid level sensor or Positioning function, finally in guarantee reaction tube, the cumulative volume of solution reaches setting value, completes constant volume step.Disappearing During solution liquid carries out catching up with acid cut to hold, main control module can pass through drive circuit, the row in control module equally Wind system works, and is quickly got rid of by the steam of evaporation from digestion solution.When main control module completes digestion solution After constant volume, mechanical arm can be controlled by reaction tube from catching up with taking-up acid cut molar block, carry out step 5.
Step 5:
After constant volume completes, user can set placement location last for reaction tube.If user is actually used Time, this system and back-end analysis equipment are combined and pass through the mutual communication of communication module, that user can set Fixed by mechanical arm, by reaction tube direct injected to rear end detection equipment, carry out rear end detection.If being System is not combined with rear end detection equipment, then after step 4 completes, master control system controls mechanical arm will be anti- Should move to react on pipe support by pipe, reaction pipe support can be taken away by user, carries out back end test analysis. Reaction pipe support said herein can be arranged on injector, it is also possible to is arranged in system operational blocks which partition system, or Can individually set up, as long as reaction tube on frame can be picked and placeed by mechanical arm.
After step 5 terminates, control system can also control to clean the device appearance to contacting sample, reagent Device is carried out, it is to avoid sample, reagent remain in a device, the result that impact is tested in the future.
The respective embodiments described above are to realize detailed description of the invention of the present utility model, the ordinary skill people of this area Member be appreciated that and in actual applications, can to it, various changes can be made in the form and details, and not Deviate spirit and scope of the present utility model.

Claims (8)

1. a full-automatic microwave device, it is characterised in that at least one include that control system, microwave reaction module and sample add module, reagent adds module, catching up with acid cut molar block;
Described control system controls described microwave reaction module according to parameter preset, sample adds module, reagent adds module, catch up with acid cut molar block, and control Filtting device in described microwave reaction module, sample adds module, reagent adds module, catch up with acid cut molar block and place mobile response container between region;
Described sample adds module and includes sample feeding chamber, solid adder, quantifier;
After sample adds described sample feeding chamber, and described reaction vessel is when being positioned at the load position that described sample adds module, described control system controls described solid adder and is added in reaction vessel, the metering of described quantifier is added into the amount of sample in described reaction vessel, and metric results feeds back to described control system;
Described reagent adds module and includes reagent container, reagent sampling device and liquid level detection device;
Described liquid level detection device detects the amount of reagent in described reagent container, and testing result feeds back to described control system, and described control system controls described reagent sampling device according to described testing result and adds reagent in described reaction vessel;
Described acid cut molar block is caught up with to include heater, liquid appending apparatus;
Described control system controls described heater and heats described reaction vessel with default temperature, and described liquid appending apparatus, for adding liquid in described reaction vessel, makes the liquid in described reaction vessel be maintained at preset vol;
Described microwave reaction module includes pressure detecting assembly and temperature sensing assembly;
Described pressure detecting assembly detects the pressure of reactant in described reaction vessel, and feeds back to described control system;Described temperature sensing assembly detects the temperature of reactant in described reaction vessel, and feeds back to described control system;Described control system controls microwave output according to force value and the temperature value of feedback.
Full-automatic microwave device the most according to claim 1, it is characterised in that described sample feeding chamber includes that solid sampling chamber and Liquid sample introduction chamber, described sample adder include solid adder and liquid adder;
Fluid sample adds from described Liquid sample introduction chamber, is added in described reaction vessel by described liquid adder, and solid sample adds from described solid sampling chamber, is added in described reaction vessel by described solid adder.
Full-automatic microwave device the most according to claim 2, it is characterized in that, described sample interpolation module also includes sample comminution device, solid sample is after described solid sampling chamber adds, enter described sample comminution device, after sample pulverized by described sample comminution device, added in described reaction vessel by described solid adder.
Full-automatic microwave device the most according to claim 1, it is characterised in that described microwave reaction module and/or catch up with in acid cut molar block and be respectively equipped with exhaust sub-system;Described exhaust sub-system is respectively used to microwave reaction module and/or catches up with the heat radiation in acid cut molar block.
Full-automatic microwave device the most according to claim 4, it is characterised in that the outlet of described exhaust sub-system is provided with device for recovering tail gas.
Full-automatic microwave device the most according to claim 1, it is characterised in that described microwave reaction module and/or catch up with in acid cut molar block and be respectively equipped with several reative cells;
Described control system can control the reaction environment in each described reative cell respectively according to default parameter.
Full-automatic microwave device the most as claimed in any of claims 1 to 6, it is characterised in that described control system includes main control unit and sub-control unit;
Described sub-control unit is respectively arranged on described sample to be added module, reagent interpolation module, microwave reaction module and/or catches up with in acid cut molar block, and control corresponding module according to parameter preset, described main control unit is for sending control signal to described sub-control unit, and receives feedback signal from described sub-control unit.
Full-automatic microwave device the most as claimed in any of claims 1 to 6, it is characterised in that also include cleaning assemblies;
Described control system controls described cleaning assemblies and cleans described sample feeding chamber, solid adder, sample comminution device, reagent container, reagent sampling device, liquid appending apparatus, pressure detecting assembly and/or temperature sensing assembly.
CN201620121841.2U 2016-02-16 2016-02-16 Full-automatic microwave device Active CN205719601U (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106872232A (en) * 2016-02-16 2017-06-20 上海屹尧仪器科技发展有限公司 Full-automatic microwave pretreatment device
CN109030612A (en) * 2018-08-01 2018-12-18 深圳市华星光电技术有限公司 Sampling device
CN110146583A (en) * 2019-04-26 2019-08-20 中国科学院地质与地球物理研究所 The method that Carius pipe decomposes the method and Re-Os isotope analysis of sample
CN111879863A (en) * 2020-06-09 2020-11-03 广东省广袤科技有限公司 Method and device for detecting organic pesticide residue in food

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106872232A (en) * 2016-02-16 2017-06-20 上海屹尧仪器科技发展有限公司 Full-automatic microwave pretreatment device
CN109030612A (en) * 2018-08-01 2018-12-18 深圳市华星光电技术有限公司 Sampling device
CN110146583A (en) * 2019-04-26 2019-08-20 中国科学院地质与地球物理研究所 The method that Carius pipe decomposes the method and Re-Os isotope analysis of sample
CN111879863A (en) * 2020-06-09 2020-11-03 广东省广袤科技有限公司 Method and device for detecting organic pesticide residue in food

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