CN106872232A - Full-automatic microwave device - Google Patents
Full-automatic microwave device Download PDFInfo
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- CN106872232A CN106872232A CN201710074426.5A CN201710074426A CN106872232A CN 106872232 A CN106872232 A CN 106872232A CN 201710074426 A CN201710074426 A CN 201710074426A CN 106872232 A CN106872232 A CN 106872232A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
Abstract
Full-automatic microwave device, including raw material add module and catch up with least one, the microwave reaction module in acid cut molar block, and respectively with raw material add module, microwave reaction module, catch up with the control system that acid cut molar block is connected；Raw material add module controls the addition of response sample and reaction reagent；Microwave reaction module is used for the microwave reaction of response sample and reaction reagent；Catch up with acid cut molar block carries out catching up with acid cut appearance to process to product；Control system to raw material add module, microwave reaction module, catches up with acid cut molar block to be controlled according to parameter preset.Full-automatic microwave apparatus structure of the invention is reasonable in design, it is simple to operate, avoid the personal injury of various acid and reagent to operating personnel in pretreatment process, the industrial accident that digestion process high-temperature high-voltage reaction brings is prevented, ensure the standardization of pretreatment process, prevent from, because artificial uncertain factor causes pre-treatment result inaccurate, improving operating efficiency, lift the reactivity of sample.
Description
Technical field
The present invention relates to technical field of microwave application, more particularly to a kind of automatic processing device for sample pre-treatments and
Method.
Background technology
Sample pre-treatments, i.e. sample are being loaded to AAS (AtomicAbsorptionSpectrometry, atomic absorption light
Spectrum) or the detecting instrument such as HPLC (HighPerformanceLiquidChromatography, high performance liquid chromatography) on examined
The every pretreatment mode used before surveying, comprising the pretreatment mode such as organic and inorganic, for inorganic samples pre-treatment, microwave
Sample-pretreating method with its it is efficiently quick the characteristics of, be currently most commonly used, comprising sampling, acid adding, airtight digestion
It is canned match somebody with somebody, clear up, sample transfer, catch up with acid cut hold etc. step.In actual sample detection process, these pre-treatment steps are all point
Operation is opened, and universal is all artificial operation.
Sampling is generally at present artificial balance by sample weighing it is good after be put into test tube.Acid adding, adds usually using liquid
Plus device or suction pipe carry out reagent addition, it is also possible to which buying automated reagent addition platform carries out reagent addition, but cost is too high, instrument
Device poor compatibility each other.Counteracting tank is assembled, and at present mainly by manual assembly, assembling process is cumbersome, and operating personnel
It is readily accessible reagent.Clear up, using Microwave Digestion, oxidation rate is fast.Sample is shifted, and the digestion solution that will have been cleared up is from disappearing
Poured out in solution tank, and tank skin remaining sample is cleared up in cleaning, the process is easily operated with a large amount of acid gas in counteracting tank, misoperation
Person sucks, while the incomplete of transfer also easily brings sample loss.Acid cut is caught up with to hold, by modes such as heating or negative-pressure vacuums,
Residual acid inside digestion solution is caught up with and is removed, then adding pure water carries out constant volume.
Before one sample wants loading to analyze, it is necessary to could be completed by above-mentioned multiple working procedure, and step, except day to be purchased
Flat, liquid adder, microwave dissolver, catch up with outside the pre-processing devices such as acid cut looks, to be also manually sampled, tinning, transfer.
Not only equipment is more, cumbersome, and is readily incorporated human error, causes sample pre-treatments effect poor repeatability and influences follow-up
Analysis result.The food and drug safety Frequent Accidents such as melamine in recent years in addition, toxic capsule, plasticiser and occur in the recent period
Tsing-Hua University's laboratory explosion accident so that in the market to automation, high accuracy, the sample pre-treatments equipment of high stability need
Ask more urgent.
The content of the invention
The present invention is directed to these problems, designs a kind of full-automatic microwave device and method, and the device is utilized
Rational structure design, various high-precision sensors and executive component also have the Row control of specification, by sampling, acid adding, closed
Counteracting tank is assembled, cleared up, sample is shifted, catch up with acid cut to hold these cumbersome pre-treatment steps automations and system must combine,
Realize the automation mechanized operation of sample pre-treatments.
Concrete technical scheme is as follows：
Full-automatic microwave device, including raw material add module and/or acid cut molar block, microwave reaction module are caught up with,
And respectively with the raw material add module, microwave reaction module, catch up with the control system that acid cut molar block is connected；
The addition of the raw material add module control response sample and reaction reagent；
The microwave reaction module is used for the microwave reaction of the response sample and reaction reagent；
It is described to catch up with the acid cut molar block to product catch up with acid cut appearance to process；
The control system to the raw material add module, microwave reaction module, catches up with acid cut molar block according to parameter preset
It is controlled.
The control system also includes the locating module for interconnecting and moves module；
The locating module and the raw material add module, microwave reaction module, acid cut molar block is caught up with to be connected；
Module is moved according to the positioning of the locating module, described in the control device control to be added in the raw material
Module, microwave reaction module, catch up with mobile response container between acid cut molar block.
The raw material add module includes the meter, sample cavity, the adder that are sequentially connected；
The meter, adder are connected with the control system respectively；
After the response sample and reaction reagent are weighed by the meter, the addition is entered by the sample cavity
Device, the reaction vessel is added to by adder.
The raw material add module also includes the sample comminution device being connected with the meter and adder respectively；
When the response sample or reaction reagent are solid, crushed by the sample comminution device.
The raw material add module also includes the liquid level detection device being connected with the control system；
When the response sample or reaction reagent are liquid, liquid level is detected by the liquid level detection device, and will inspection
Survey result and feed back to the control system, the control system controls the raw material add module to institute according to the testing result
State reaction vessel addition sample or reagent.
It is described to catch up with the acid cut molar block to include the heater that is connected with the control system, and liquid appending apparatus；
The control system controls the heater to heat the reaction vessel with default temperature；
The liquid appending apparatus are used for adding liquid in the reaction vessel, protect the liquid in the reaction vessel
Hold in preset vol.
The microwave reaction module includes the pressure detecting assembly and the temperature detection group that are connected with the reaction vessel respectively
Part；
The pressure detecting assembly detects the pressure in the reaction vessel, and pressure value is fed back into the control system
System；
The temperature sensing assembly detects the temperature in the reaction vessel, and temperature value is fed back into the control system
System；
The control system is according to the pressure value and temperature value control microwave output.
The microwave reaction module and/or catch up with the exhaust sub-system that radiating is respectively provided with acid cut molar block.
The outlet of the exhaust sub-system is provided with device for recovering tail gas.
The microwave reaction module and/or catch up with is respectively equipped be connected with the control system some anti-in acid cut molar block
Answer room；
According to default parameter, the control system controls the reaction environment in each described reative cell respectively.
The control system includes main control unit and sub-control unit；
During the sub-control unit is respectively arranged on the raw material add module, microwave reaction module and/or catches up with acid cut molar block,
And corresponding module is controlled according to parameter preset respectively；
The main control unit is used to send control signal to the sub-control unit, and receives feedback letter from the sub-control unit
Number.
Described pretreating device, the also cleaning assemblies including being connected with the control system；The control system control
The cleaning assemblies is to sample cavity, adder, reaction vessel, sample comminution device, pressure detecting assembly and/or temperature sensing assembly
Cleaned.
Present invention also offers a kind of full-automatic microwave method, it is possible to use described in above-mentioned any one it is complete from
Dynamic microwave device, it would however also be possible to employ other microwave devices.Comprise the following steps：
S0, manually set control parameter on full-automatic microwave device；
S1, judge whether to need according to control parameter to add sample, if desired, then control Filtting device to remove reaction vessel
In moving to sample add module, and sample is added, otherwise into step S2；
S2, judge whether to need according to control parameter to add reagent, if desired, then control Filtting device to remove reaction vessel
In moving to reagent add module, and reagent is added, otherwise into step S3；
S3, judged whether to need microwave reaction according to control parameter, if desired, then control Filtting device to remove reaction vessel
In moving to microwave reaction module, otherwise into step S5；
S4, controlled microwave reaction module to change reaction environment according to control parameter, send microwave assisted reaction；
S5, judged whether to need to catch up with acid cut to hold according to control parameter, if desired, then control Filtting device to remove reaction vessel
Move in catching up with acid cut molar block, otherwise into step S7；
S6, according to control parameter control catch up with acid cut molar block change catch up with acid cut hold condition, promotion 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 preferred, in step sl, when reaction vessel is located at point of addition, solid adder is controlled to add sample
Add in reaction vessel, the detection of sample amount detecting device is added into the sample size in reaction vessel, when sample size reaches default sample
During product amount, stop addition sample.
Used as preferred, before addition solid sample, control system control sample comminution device crushes sample.
As preferred, during addition solid sample, realize that sample size is measured by the weight for measuring reaction vessel；Annex solution
During body sample, realize that sample size is measured by sample volume in the weight or metering liquid adder of measuring reaction vessel.
As preferred, in step s 2, if during addition reagent, reagent amount detecting device is in real time by the examination in reagent container
Dosage feeds back to control system, when the amount of reagent in reagent container be less than default minimum amount of reagent when, control system suspend to
Add reagent in reaction vessel, after candidate agent supplement addition, continue to adding reagent in reaction vessel.
Used as preferred, step S4 is specially：After control system confirms that reaction vessel moves to microwave cavity, according to default
Parameter, controls magnetron microwave, sample and reagent in heating response container, sample and reagent is heated and microwave shines
Penetrate, reacted in reaction tube, complete digestion process.
Used as preferred, step S6 is specially：First control heater is heated within the scope of default temperature, control system
The liquid level of digestion solution in reaction vessel is monitored by liquid level detection device, when digestion solution height reduction is to catching up with sour preset value
Afterwards, control system controls sampling pump to distilled water is added in reaction vessel, the reaction solution in reaction vessel is maintained at setting liquid
Position, realizes constant volume.
Used as preferred, in step S4 and step S6, control system also controls exhaust system to discharge microwave reaction module
Catch up with acid cut molar block acid or steam.
Used as preferred, after step S7, control system also controls cleaning module cleaning sample add module and/or reagent
The sample and/or reagent of residual in add module.
The technical scheme of present invention use middle compared to existing technology, with advantages below：
1st, system utilizes rational structure design, using various sensors and executive component, by the Row control of specification,
Sampling, acid adding, closed digestion tank are assembled, is cleared up, sample is shifted, catch up with acid cut to hold these cumbersome pre-treatment steps automations simultaneously
Systematically combine, realize the automation mechanized operation of sample pre-treatments.
2nd, it is simple to operate.User is only needed to preset and automatically controls parameter, and sample is put into the pretreating device, and system is just
All flows that parameter completes pre-treatment can be automatically controlled according to default.
3rd, in all of flow, sample, reagent are all added in same reaction vessel so that in whole course of reaction
In, it is not necessary to migrate sample and reagent, it is to avoid sample and reagent are remained in relaying container, influence sample and reagent it is dense
Degree, while being also avoided that sample, reagent contamination or loss in transfer process, is greatly improved subsequent detection precision.
4th, this full-automatic microwave device, the sample add module required for microwave reaction, reagent are added
Plus module, microwave reaction module, catch up with acid cut molar block to be integrated in one, and the number of devices of Experimental Area is reduced, make test block
Domain is more succinct.
5th, in whole experiment process, it is not necessary to which the personage for possessing relevant professional knowledge carries out experimental implementation, it is only necessary to train
Instruction operating instrument.When needing to carry out microwave, it is only necessary to the specific arrange parameter of teaching process personnel, you can realize
Full automatic microwave, professional is freed from complicated work load, it is to avoid various in pretreatment process
The personal injury of acid and reagent to operating personnel, while preventing the industrial accident that this high-temperature high-voltage reaction of digestion process brings.
6th, whole course of reaction is relative in an environment more closed, and prevents from catching up with the acid come out during acid
It is directly sucked in lung by people, improves experimental situation.
7th, by Automatic Control, being capable of specification pre-treatment flow, it is ensured that the standardization of pretreatment process, prevent because people
For uncertain factor causes pre-treatment result inaccurate.
8th, the pre-treatment under the same conditions of various different samples can be simultaneously carried out, the microwave time is saved, is carried
High workload efficiency.
9th, in sample add module, it is provided with the sample comminution device for comminuted solids sample, it might even be possible to set many
Level sample comminution device, solid sample is crushed to and meets the size that reaction is required, solid sample is fully reacted, and lifts sample
The reactivity of product.
10th, after whole full-automatic microwave process is completed, control system can also control cleaning device to connecing
Touched sample, the container of reagent is cleaned comprehensively, and prevented from being residued in container or in adder, after influence because of sample, reagent
Continuous experiment effect.
11st, for the exhausting problem caught up with acid cut molar block and microwave reaction module, in the present invention, acid cut molar is being caught up with
One group of exhaust sub-system is respectively provided with block and microwave reaction module so that the steam and sour gas energy produced in course of reaction
It is enough to be discharged by the exhaust sub-system in time.At the same time it can also set tail gas recycle dress at the air outlet of the exhaust sub-system
Put, the steam and sour gas that will be produced in course of reaction absorb, and prevent sour gas to be directly discharged in air, cause air
Pollution.
12nd, full-automatic microwave device provided by the present invention, is provided with a main control unit and multiple sub-control lists
Unit, wherein, multiple sub-control units are separately mounted to sample add module, reagent add module, microwave reaction module and catch up with acid
In constant volume module, in device operation, corresponding control information is sent to sub-control unit by main control unit, each sub-control list
Unit controls the process operation of corresponding module respectively, and feeds back corresponding control result to main control unit.By this kind of design, Neng Gouyou
Effect ground reduces the amount of calculation of main control unit, lifts the processing speed of full-automatic microwave device.
13rd, the system can set different samples, reagent to each reaction tube, heating condition, catch up with sour temperature, constant volume body
The parameters such as product, during the course of the reaction, main control module can control other modules reaction bar different for reaction tube is provided
The reagent of part and addition different volumes, final each reaction tube can possess the different reaction condition of oneself, meet different
The pre-treatment demand of sample.
14th, control is scheduled to all modules of system by control system unification, realizes whole samples pre-processing data
Tracking, backup and management, meet U.S. EPA (US Gov Env Protection Agency) for data management requirement, to promoting laboratory
Automation, data management standardization, offer operating efficiency etc. are respectively provided with very big meaning.EPA data managements mentioned here,
Refer to what U.S. EPA was proposed for office automation and management information system, laboratory equipment and its service data are unified
Management is formatted, all operational factors of equipment test relevant parameter including operating personnel's information, time, method, service data etc.
It is both needed to be preserved according to specific format, facilitates inquiry and management of the related personnel to experimentation information and experimental result.
Brief description of the drawings
Fig. 1 is the system structural framework schematic diagram of the pretreating device of embodiment 1；
Fig. 2 is the Electronic Control block diagram of the pretreating device of embodiment 1；
Fig. 3 is the working-flow figure of the pretreating device of embodiment 1；
Fig. 4 is the system structural framework schematic diagram of each module of pretreating device of embodiment 2；
Fig. 5 is the system structural framework schematic diagram of the pretreating device of embodiment 3；
Fig. 6 is the Electronic Control block diagram of the pretreating device of embodiment 3；
Fig. 7 is the working-flow figure of the pretreating device of embodiment 3.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing to each reality of the invention
The mode of applying is explained in detail.The elaboration is not construed as any limitation to the scope of the present invention.
Embodiment 1
As shown in figure 1, the full-automatic microwave device of the present embodiment includes sample add module, reagent addition mould
Block, microwave reaction module, the mechanical arm caught up with acid cut molar block, reaction tube is moved in each intermodule, and distinguish with each module
The main control module of connection.
The sample add module includes sample cavity, adder, weighing apparatus.Form according to sample is different, the sample introduction
Chamber can be solid sampling chamber or Liquid sample introduction chamber；Fluid sample enters reaction tube after entering Liquid sample introduction chamber by charger,
Solid sample enters solid sampling chamber and enters reaction tube by sample adder after sample comminution device is crushed.Reaction tube with weigh
Device is connected, and the metric results of reaction tube are fed back to main control module by weighing apparatus.
The reagent add module includes liquid level sensor, sampling pump, the sample introduction needle on sampling pump, level sensing
Device will need the signal for adding reagent to feed back to main control module, and main control module control sampling pump is added reagent by sample introduction needle
Add to reaction tube.
The microwave reaction module includes magnetron, pressure sensor, temperature sensor and air draft cooling system, pressure
Reaction is in control pressure and temperature and feeds back to main control module by sensor, temperature sensor respectively, and main control module is according to pressure
Force value and temperature value control magnetron launch the microwave of appropriate power to the reaction tube in microwave cavity.
It is described catch up with acid cut molar block include electric hot plate, temperature sensor, sampling pump, liquid level sensor, exhaust system, temperature
Sensor and liquid level sensor are respectively by the liquid level feedback of the temperature of electric hot plate and reaction tube to main control module, main control module
Control sampling pump is heated to reaction tube sample introduction, control electric hot plate to reaction tube, and reaction tube is connected with exhaust system.
The Electronic Control block diagram of above-mentioned each unit or module is as shown in Fig. 2 working-flow figure is as shown in Figure 3.
In the present embodiment, microwave reaction module is based primarily upon microwave cavity, magnetron, and impressed pressure sensor, temperature are passed
The peripheral functionality parts such as sensor, air draft cooling system are constituted.Microwave cavity sends out microwave in magnetron as the coupled chamber of microwave
After injecting microwave cavity, the microwave field of some strength can be coupled into cavity, the reaction tube equipped with sample and reagent (hold by reaction
Device) it is heated up under the irradiation of microwave, complete microwave reaction process.In this process, pressure sensor and TEMP
Device plays monitoring reaction tube internal temperature and pressure effect, and pressure and temperature signal is fed back into control after amplifier amplifies
System MCU (micro-control unit) processed, MCU can be according to the temperature, pressure setting value for setting in advance, by D/A conversion and control magnetic controls
The microwave output of pipe, reaches the purpose of control reaction tube internal temperature and pressure.Because microwave reaction belongs to high-temperature high-voltage reaction,
And reaction reagent used is basic based on strong acid, so air draft cooling system is also very necessary, the air draft cooling system
The ventilation velocity of (exhaust sub-system) settable multiple gear, the acid during module can be excluded in time in whole course of reaction
Gas, while in cooling stage according to the cooling velocity for accelerating reaction tube by increasing ventilation velocity, shortening whole course of reaction
Time, improve microwave reaction efficiency.Further, it is also possible to be returned by setting a tail gas in the port of export of air draft cooling system
Receiving apparatus.The device for recovering tail gas can be equipped with the container of alkaline solution, for by acid gas and, or fill other
Container of acid gas etc. can be absorbed, prevents acid gas to be directly discharged in air, influence the health of experimenter.
In the present embodiment, sample add module is to complete the functional module that sample is added automatically, mainly comprising weighing apparatus
The accessory such as (meter), liquid adder, these three core components of solid adder and sample comminution device.Weighing apparatus are used
In the weight of metering reaction tube, the weight metering equipment such as balance, pressure ceramic sensor are can select；Liquid adder is used to add
The flowable samples such as liquid, paste class, can select the equipment such as syringe pump, peristaltic pump；Solid adder is similar to determining on the market
Amount packing machine or proportional sampling device, for adding solid sample, if sample is not by pretreatment, volume ratio is larger, can be by
Sample comminution device, pulverization process is carried out by big solid sample, and sample addition is carried out by solid adder again after the completion of crushing.
If it is necessary, two groups of sample comminution devices can be set, wherein first group is used to carry out big solid sample to smash treatment, afterwards
Crushed sample is carried out by pulverization process by second group of sample comminution device again.By this kind of design so that in comminuted solids
During sample, the size for crushing sample particle can not only be reduced, additionally it is possible to lift the use longevity of Disintegrating knife in Sample Grinder
Life.During work, main control module can control weighing apparatus to remove the peel zero.Peeling zero is referred to and is placed on empty reaction vessel
After on weighing apparatus, weighing apparatus can weigh to the reaction vessel, and now control system will be adjusted to weight parameter, putting
Measured weight is defined as 0 when being equipped with reaction vessel.After the completion of weighing apparatus peeling, main control module sets according to advance sample
Be added to sample in reaction tube by species and volume or weight, control liquid adder or solid adder.In sample addition
During, main control module can monitor in real time liquid adder and weighing apparatus volume and weight parameter, when the two values wherein
One or two reaches the preset value in system, and main control module is that can determine whether that sample-adding is completed.
In the present embodiment, reagent add module is automated fluid adder, is mainly made up of sampling pump, while in order to
The volume of reagent bottle (reagent container) interior reagent is monitored, liquid level sensor can be added, monitor the volume of reagent bottle interior reagent,
When reagent solution bit comparison is low, liquid level information is fed back into control system, control system prompting user adds reagent in time.Work
When, main control module adds volume according to default reagent, controls sampling pump, reagent quantitative is added in reaction tube, reagent
In adding procedure, liquid level sensor can liquid level signal is fed back into control system in real time, when reagent very little, influence the normal work of module
When making, main control module can suspend reagent to be added and points out user to supplement reagent, and after liquid level recovers normal, module can continue
Work.The sampling pump that this module is used can select the pumps with function of measuring such as syringe pump, peristaltic pump or measuring pump, as long as the pump energy
Meet the accurate addition of reagent.
In the present embodiment, catch up with acid cut molar block main by heater, temperature sensor, sampling pump, liquid level sensor
And exhaust system composition.Reaction tube is positioned on heater, and main control module control controls electric hot plate by drive circuit
(one kind of heater) generates heat, so that heating response pipe, after reaction tube heats up, accelerates the evaporation of the digestion solution inside reaction tube
Speed, during this, temperature sensor is used for controlling the temperature of electric hot plate, and liquid level sensor (liquid level detection device) is then prison
The volume of control reaction tube inside digestion solution, the liquid level signal of main control module real-time reception liquid level sensor feedback works as reaction tube
After the volume of interior digestion solution reaches setting value, main control module control sampling pump, toward the solution of the interior addition certain volume of reaction tube,
Ensure that the cumulative volume of digestion solution in test tube meets setting value.Electric hot plate mentioned here can be metal material, it is also possible to
It is graphite material or other materials, module demand for heat can be met.Sampling pump then can select syringe pump, peristaltic pump or meter
The pumps with function of measuring such as amount pump.Similarly, during catching up with acid cut to hold, acid gas can be equally produced, therefore, catching up with acid cut molar block
On an air draft cooling system and device for absorbing tail gas can also be set.
In the present embodiment, microwave reaction module and/or to catch up with and be respectively equipped with several reative cells in acid cut molar block；Control
System can respectively control the reaction environment in each reative cell according to default parameter.The system can be to each reaction
Pipe sets different samples, reagent, heating condition, catches up with the parameters such as sour temperature, constant volume, during the course of the reaction, master control molding
Block can control the reagent of other modules reaction condition different for reaction tube is provided and addition different volumes, it is final each
Reaction tube can possess the different reaction condition of oneself, meet the pre-treatment demand of different samples.
In the present embodiment, Filtting device selects mechanical arm.Mechanical arm as reaction tube in whole system mobile instrument,
Its movement is by control system control.Can select the conventional shaft mechanical arms of X/Y/Z tri- or rotating mechanical arm, it is only necessary to which can meet will be anti-
Should pipe accurately picked and placeed in each module, remaining parameter etc. is not restricted.
In the present embodiment, control system includes man-machine interface, main control module MCU, drive circuit, amplifier, level
Various chips, circuit and the programs such as conversion, D/A conversions.As shown in Figure 2.Control system mainly completes human-computer dialogue, receives operation
Person is instructed and controls back-end circuit by program, and the order of rear end modules follow procedure setting is controlled by controlling circuit
Operation, and the procedural information and final data of operation are fed back in man-machine interface, allow operator to get information about system current
The module of working condition and real time data.
Because in whole pretreatment process, the data processing amount being related to is larger, as preferred, can be by control
System is divided into two parts of master control system and sub-control system, wherein, master control system is used for user and sets working environment parameter and letter
Number treatment etc., while corresponding control parameter is sent into corresponding sub-control system.Sub-control system is respectively used to control sample
Add module, reagent add module, microwave reaction module, catch up with sample, the addition of reagent and course of reaction in acid cut molar block
Control, and corresponding result is fed back into master control system.
In the present embodiment, after in order to prevent reaction, sample and reagent remain in the containers such as reagent, solid adder
In, a cleaning device can be designed, after completion of reaction, these containers are cleaned by control system control cleaning device, prevent
During subsequent reactions, the result of the residue influence experiment of original reagent or sample.
Because the system is, based on the basis of microwave reaction module, to have increased sample add module, reagent add module newly
And acid cut molar block is caught up with, and by outside robotic arm automation function, under being uniformly controlled of main control module, be combined into whole
Cover full-automatic microwave system.So user can arbitrarily configure required module, if such as user's selection adds manually
Sample-adding product, it is only necessary to configure reagent add module, microwave reaction module, catch up with acid cut molar block and mechanical arm, it is possible to after realization
Continuous sample automation pre-treatment；If user is not high for sample and reagent addition requirement, microwave reaction can be only selected
Module, acid cut molar block and mechanical arm are caught up with, realize that sample automates pre-treatment.
Present invention also offers a kind of full-automatic microwave method, the method can utilize foregoing device reality
It is existing, it is also possible to be realized by other microwave devices.The specific workflow of the method is as shown in figure 3, including five masters
Want step：
Step one：
After user sets method and starts working, the main control module of system can judge whether certainly according to parameter preset
Dynamic sample-adding, if it is, control machinery arm moves in sample add module reaction tube, if it is not, then carrying out step 2.When
It is determined that when being, first be zeroed for weighing apparatus after confirming that reaction tube is moved into place by the main control module of system, is then set according to system
Be added to sample in reaction tube by fixed parameter, control liquid adder or solid adder, if default sample is needed
Pulverization process is done, main control module can control sample comminution device first to be crushed to sample, pass through solid after the completion of crushing again
Be added to sample in reaction tube by adder.In sample adding procedure, the weight of weighing apparatus meeting real-time monitoring sample addition is led to
The function of weighing and liquid adder for crossing weighing apparatus determine volume function, accurately according to default value can complete sample
Sample-adding.After sample addition is completed, control machinery arm takes out reaction tube to master control system from sample add module, carries out step
Two.
Step 2：
Whether the main control module of system is automatic reagent adding according to the setting of default parameter determination methods, if it is,
Control machinery arm moves in reagent add module reaction tube, if it is not, then carrying out step 3.When it is determined that being, system
Main control module, according to the volume parameter of default, controls sampling pump by reagent from examination after confirming that reaction tube is moved into place
It is added in reaction tube in agent bottle.In adding procedure, liquid level signal can be fed back to main control module by liquid level sensor in real time,
When reagent very little, influence module normal work when, main control module can suspend reagent adds and point out user supplement reagent, work as liquid
After bit recovery is normal, module can work on, and complete automatic reagent adding process.Master control system is controlled after reagent addition is completed
Mechanical arm processed takes out reaction tube from reagent add module, carries out step 3.
Step 3：
The main control module of system is to need microwave reaction according to the setting of default parameter determination methods, is if it is controlled
Mechanical arm moves in microwave reaction module reaction tube, if it is not, then carrying out step 4.When it is determined that being, the master control of system
After confirming that reaction tube moves to microwave cavity, the parameter such as temperature, pressure or time according to default controls magnetic control to molding block
Pipe launches microwave, sample and reagent in heating response pipe, sample and reagent be heated and microwave irradiation after, in reaction tube
React, complete digestion process.In digestion process, in temperature sensor and pressure sensor meeting monitor in real time reaction tube
Temperature and pressure parameter, and by main control module, by data display in man-machine interface, allow operator to understand the real-time of reaction
Process.In digestion process, air draft cooling system is controlled by main control module, can realize that different ventilation velocities are adjusted according to setting
Section, the quick cooling function of reaction tube after the completion of realizing during the microwave reaction acid discharge heat sinking function of module and clearing up.When
After system receives reaction tube cooling END instruction, meeting control machinery arm takes out reaction tube from microwave reaction module, carries out
Step 4.
Step 4：
The main control module of system is to need to catch up with acid cut to hold according to the setting of default parameter determination methods, is if it is controlled
Mechanical arm moves to reaction tube to be caught up with acid cut molar block, if it is not, then carrying out step 5.When it is determined that being, the master control of system
After confirming that reaction tube is moved into place, the parameter such as temperature, time and constant volume according to default, first control adds molding block
Thermal is heated, and during heating devices heat, main control module is by temperature sensor, monitor in real time heater temperature
Degree, makes heater temperature stabilization in setting range.During heating devices heat, digestion solution inside reaction tube also by
Heat temperature raising, as digestion solution temperature is raised, its evaporation rate is also and then accelerated, and now main control module can be by level sensing
Device, the liquid level of digestion solution in monitoring reaction tube, after digestion solution volume is reached catches up with sour setting value, main control module can be controlled
Sampling pump, by sampling pump and the liquid adding functions or positioning function of liquid level sensor, finally ensures toward solution is added in reaction tube
The cumulative volume of solution reaches setting value in reaction tube, completes constant volume step.During digestion solution carries out catching up with acid cut to hold, main control
Module equally can quickly be arranged the steam evaporated from digestion solution by drive circuit, the exhaust system work in control module
Remove.After main control module completes the constant volume of digestion solution, meeting control machinery arm takes out reaction tube from acid cut molar block is caught up with, and enters
Row step 5.
Step 5：
After the completion of constant volume, user can be set the last placement location of reaction tube.If user is actually used, incited somebody to action
The system is combined with back-end analysis equipment and is mutually communicated by communication module, and that user can be set by mechanical arm, will be anti-
Should pipe direct injected on the testing equipment of rear end, carry out rear end detection.If system is not combined with rear end testing equipment, then when
After the completion of step 4, master control system control machinery arm moves on reaction pipe support reaction tube, and user will can react
Pipe support is taken away, carries out back end test analysis.Reaction pipe support said herein can be arranged on injector, it is also possible to be arranged on system
In operational blocks which partition system, or can individually set up, as long as mechanical arm can be picked and placeed to reaction tube on frame.
After step 5 terminates, control system can also control cleaning device to contacting sample, the container of reagent is carried out
Cleaning, it is to avoid sample, reagent residual in a device, influence the result tested in the future.
Embodiment 2
The present embodiment is essentially identical with the building block of embodiment 1, unlike, control system also includes mutual with mechanical arm
The locating module being connected, locating module is connected with the main control module of control system.As shown in figure 4, locating module with it is described
Raw material add module, microwave reaction module, acid cut molar block and external device is caught up with to connect；External device refers to atomic absorption spectrum
(AAS), icp mses (ICP-MS) and inductively coupled plasma atomic emission spectrometer (ICP-OES)
Deng testing equipment or the cleaning equipment that can be cleaned to parts such as test tube, closures.
Module is moved according to being accurately positioned for the locating module, described in the control device control to be added in the raw material
Add module, microwave reaction module, mobile response container between acid cut molar block is caught up with, can finally moved to external device.
Embodiment 3
When using acid-fast ability stronger detecting instrument, can not carry out catching up with acid treatment after some Specimen eliminatings and straight
Connect sample detection, this kind of user can just be unworthy of putting and catch up with acid cut molar block, system structural framework schematic diagram such as Fig. 5 of the present embodiment
Shown, Electronic Control block diagram as shown in Figure 6, working-flow figure as shown in fig. 7, other parts setting and embodiment 1 or
Embodiment 2 is similar to.
The full-automatic microwave device of the present embodiment includes sample add module, reagent add module, microwave reaction
Module, reaction tube is moved into module what each intermodule was moved, and the main control module being connected respectively with each module.Sample and
After reagent reacts in microwave reaction module, without catching up with acid cut appearance to process, directly moved module delivers to external device to product.
Generally speaking, the system can be, according to the actual sample pre-treatments demand of user, to select different functional modules,
It is combined into the preprocessing system of complete set.After user has selected module and has been combined into system, the master control molding of system
Block be can the type of modules that is currently configured of automatic identification, and given in man-machine interface and show, user can be directly man-machine
Corresponding workflow and method are set on interface, the microwave of sample is completed.Certainly, if system possesses whole moulds
The function of block, and user selects some functions or step not to process when method is set, system also can be according to the setting side of user
Method completes pre-treatment work.
The respective embodiments described above are to realize specific embodiment of the invention, and one of ordinary skill in the art can manage
Solution, and in actual applications, can to it, various changes can be made in the form and details, without departing from spirit of the invention and model
Enclose.
Claims (13)
1. full-automatic microwave device, it is characterised in that the pretreating device includes raw material add module and catches up with acid cut
At least one, microwave reaction module in molar block, and respectively with the raw material add module, microwave reaction module, catch up with acid
The control system of constant volume module connection；
The addition of the raw material add module control response sample and reaction reagent；
The microwave reaction module is used for the microwave reaction of the response sample and reaction reagent；
It is described to catch up with the acid cut molar block to product catch up with acid cut appearance to process；
The control system to the raw material add module, microwave reaction module, catches up with the acid cut molar block to carry out according to parameter preset
Control.
2. pretreating device according to claim 1, it is characterised in that the control system also includes that what is interconnected determining
Module and move module in position；
The locating module and the raw material add module, microwave reaction module, acid cut molar block is caught up with to be connected；
According to the positioning of the locating module, module is moved described in the control device control in raw material addition addition mould
Block, microwave reaction module, catch up with mobile response container between acid cut molar block.
3. pretreating device according to claim 1, it is characterised in that the raw material add module includes what is be sequentially connected
Meter, sample cavity, adder；
The meter, adder are connected with the control system；
After the response sample and reaction reagent are weighed by the meter, the adder is entered by the sample cavity, by
The adder is added to reaction vessel.
4. pretreating device according to claim 3, it is characterised in that the raw material add module also include respectively with institute
State the sample comminution device of meter and adder connection；
When the response sample or reaction reagent are solid, crushed by the sample comminution device.
5. pretreating device according to claim 3, it is characterised in that the raw material add module also includes and the control
The liquid level detection device of system connection processed；
When the response sample or reaction reagent are liquid, liquid level is detected by the liquid level detection device, and detection is tied
Fruit feeds back to the control system, and the control system controls the raw material add module to described anti-according to the testing result
Container is answered to add sample or reagent.
6. pretreating device according to claim 2, it is characterised in that described to catch up with the acid cut molar block to include and the control
The heater of system connection, and liquid appending apparatus；
The control system controls the heater to heat the reaction vessel with default temperature；
The liquid appending apparatus are used for adding liquid in the reaction vessel, are maintained at the liquid in the reaction vessel
Preset vol.
7. pretreating device according to claim 2, it is characterised in that the microwave reaction module include respectively with it is described
The pressure detecting assembly and temperature sensing assembly of reaction vessel connection；
The pressure detecting assembly detects the pressure in the reaction vessel, and pressure value is fed back into the control system；
The temperature sensing assembly detects the temperature in the reaction vessel, and temperature value is fed back into the control system；
The control system is according to the pressure value and temperature value control microwave output.
8. the pretreating device according to claim 6 or 7, it is characterised in that the microwave reaction module and/or catch up with acid cut
The exhaust sub-system of radiating is respectively provided with molar block.
9. pretreating device according to claim 8, it is characterised in that the outlet of the exhaust sub-system is provided with tail gas and returns
Receiving apparatus.
10. the pretreating device according to claim 6 or 7, it is characterised in that the microwave reaction module and/or catch up with acid
The some reative cells being connected with the control system are respectively equipped with constant volume module；
The control system controls the reaction environment in each described reative cell respectively according to default parameter.
11. according to any described pretreating device of claim 1 to 7, it is characterised in that the control system includes master control list
Unit and sub-control unit；
During the sub-control unit is respectively arranged on the raw material add module, microwave reaction module and/or catches up with acid cut molar block, and root
Corresponding module is controlled respectively according to parameter preset；
The main control unit is used to send control signal to the sub-control unit, and receives feedback signal from the sub-control unit.
12. according to any described pretreating device of claim 1 to 7, it is characterised in that also including connecting with the control system
The external device for connecing；The external device is testing equipment or cleaning equipment.
13. pretreating devices according to claim 12, it is characterised in that the control system controls the cleaning equipment
Sample cavity, adder, reaction vessel, sample comminution device, pressure detecting assembly and/or temperature sensing assembly are cleaned.
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| CN2016100867167 | 2016-02-16 | ||
| CN201610086716.7A CN105628429A (en) | 2016-02-16 | 2016-02-16 | Full-automatic microwave pretreatment device |
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| CN201710074426.5A Pending CN106872232A (en) | 2016-02-16 | 2017-02-10 | Full-automatic microwave device |
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Cited By (5)
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| CN107478499A (en) * | 2017-08-08 | 2017-12-15 | 宋林涛 | Intelligent digestion detecting system |
| CN107607373A (en) * | 2017-09-01 | 2018-01-19 | 上海华之光谱仪器有限公司 | Acid cut looks is caught up with a kind of full-automatic inorganic samples pre-treatment |
| CN108732007A (en) * | 2018-08-06 | 2018-11-02 | 沈阳兴高网络科技有限公司 | A kind of full-automatic digestion system with mechanical arm |
| 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 |
| CN116448698A (en) * | 2023-06-14 | 2023-07-18 | 北京市计量检测科学研究院 | High-flux integrated solid sample detection device |
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| CN110560196A (en) * | 2019-09-06 | 2019-12-13 | 中国计量大学 | Heavy metal detection sample pretreatment workbench |
| CN110631890B (en) * | 2019-10-31 | 2022-06-17 | 上海屹尧仪器科技发展有限公司 | Full-automatic sample pretreatment platform taking microwave digestion as core |
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