CN109900852A - Boron element based on chemical titration analysis technology automatically analyzes test device and method - Google Patents
Boron element based on chemical titration analysis technology automatically analyzes test device and method Download PDFInfo
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Abstract
The present invention relates to the boron elements based on chemical titration analysis technology to automatically analyze test device and method, device includes: computer used in Specimen eliminating beaker or crucible, program controlled heater device, mechanical linkage, sliding rail and transmission transmission device, Vltrasonic device, peristaltic pump and its control motor, liquid storage device, catheter, outlet tube, pH meter, sand core funnel, potentiometric titrimeter and system control；Control system includes corresponding control module: executing the melting control module of sample melting, the wash-off control module to complete the dissolution of sample frit, adjusting control module, impurity absorption to the pH value that sample solution pH value is adjusted and being separated by filtration module, solution concentration control module, chemistry titration control module and computing module.The present invention can be operated by instrumentation, realize the visualization of the ordered of process control, function modoularization and standardization and operation automation and process.
Description
Technical field
The present invention relates to a kind of boron elements based on classical chemical analysis technology to automatically analyze test device and method.
Background technique
Boron element is widely present in nature, is the important component in the materials such as steel, alloy, glass, semiconductor.Add
Add the pyrex formed after boron element that there is excellent chemical stability, thermal stability, optical property and mechanical performance.
And boron carbide can largely absorb neutron and not will form radioactive isotope, be ideal control nuclear fission in nuclear plant
The neutron-absorbing material of rate.In addition boron is also human body and animal skeleton growth, improves necessary to brain function and plant growth
Microelement.The presence of boron element often has decisive influence to the quality of formed compound, therefore, Accurate Determining boron and
The content of boride has vital meaning.
According to the difference of boron content in sample, the detection of boron is divided into microanalysis and gram method.It is micro and
The measurement of trace boron element mainly has ion selective electrode method, inductively coupled plasma body method, fluorescence method, liquid chromatography, heat
Electric mass spectrography, nuclear reaction analysis method etc..And the measurement of constant boron element mainly using classical chemical titration and divides in material
Light photometry.Spectrophotometry is usually to use curcumin and azomethine-H spectrophotometry, but it is easy by a variety of chemicals
The interference of matter can reduce the sensitivity of spectrophotometry although can eliminate interfering substance with screening agent, so it is general
It is not used in the sample of measurement complicated component.Mannitol acid-base titration is the classics chemistry point for being used to measure boron content earliest
Analysis method, B in borosilicate2O3National standard method (GB/T 1549-2008, the fibrous glass chemical analysis side of assay
Method) use mannitol acid-base titration.Meanwhile mannitol acid-base titration be also in the borides such as boron carbide boron element contain
Boron content in fixed industry standard methods (JB/T 7993-2012, boron carbide chemical analysis method) or ferro-boron is measured to measure
National standard method (GB/T 3653.1-1988, ferro-boron chemical analysis method alkalim-etry measure boron amount).Currently, often
The analysis for measuring boric acid in boric acid and drug also still uses mannitol acid-base titration.
The basic principle of mannitol acid-base titration is that the boron in sample is changed into boric acid form, by alkali titration
The content of boron is calculated in consumed standard solution amount and titer.Since boric acid is weak acid, cannot directly be carried out with alkali
And titration, ethylene glycol, glycerine, mannitol and carbohydrate can be used and acid reaction generates the hydroxo complexes such as alcohol boric acid, this network
It closes object to be easier to dissociate hydrogen ion, with standard base (SB) direct titration, to measure boron content indirectly.In mannitol acid-base titration,
The metal ion that hydroxide precipitating can be formed in titration process can have interference to measuring method, therefore need after sample dissolution
It to be handled and be excluded by precipitation and separation.This separation process can precipitate the non-meltability being mingled in sample solution simultaneously
Discharge, so that certain sample frits have color and have the material of turbid phenomenon to be still suitble to using mannitol soda acid after washing out
Titration measuring boron content.
Using classical chemical titration constant boron content accuracy with higher.But traditional classical is chemical
The overall process of titration is usually completed by manual operation, and there is complex steps, chemical contamination is serious, detection speed is slow, unfavorable
In the fast read result the disadvantages of.
The bibliography of above content includes: [1] R. N. Sah and P. H. Brown, Boron
determination—A review of analytical methods, Microchemical journal. 56,
285-304 (1997) [2] Yin Xianwu, Zhang Jun, boron content in mannitol determination of acid-basetitration ferro-boron, Tianjin smelting
Gold, 6,53-55 (2015) [3] Liang Yali, Jiang Hui carry out Effective Boron of Soil survey using azomethine reagent spectrophotometry
Fixed analysis of Influential Factors, Shanxi science and technology, 33,25-28 (2018).
Summary of the invention
In order to solve the above technical problems, one aspect of the present invention provide a kind of boron element based on chemical titration analysis technology from
Dynamic analysis test apparatus, which is characterized in that be made of hardware system and corresponding control system, the device packet in hardware system
Include: Specimen eliminating beaker or crucible, program controlled heater device, mechanical linkage, sliding rail and transmission transmission device, Vltrasonic device,
Peristaltic pump and its control motor, liquid storage device, catheter, outlet tube, pH meter, sand core funnel, potentiometric titrimeter and system control
Computer used；
Test device structure is followed successively by sample heating zone, chemical treatment area, constant-current titration area and data processing area in order,
It is on the same operating platform, the sample heating zone is kept apart with other three areas by baffle；
Program controlled heater device is located at heat treatment area, carries out melting behaviour to the sample in crucible or beaker by process control
Make；
Mechanical linkage and sliding rail are located at chemical treatment area and constant-current titration area, to hang and fix catheter and buret,
Three-dimensional direction moving is carried out under motor driven or under manual, completes fixed, movement and liquid adding functions；
Liquid-adding device is located at chemical treatment area, including peristaltic pump, liquid storage device, catheter and buret, peristaltic pump are driven by motor,
To titrate or carry out acid-base neutralization；
PH meter includes reference electrode, working electrode and galvanometer, to monitor the pH value of solution；
Potentiometric titrimeter is located at constant-current titration area, is made of reference electrode and indicator electrode, including buret, magnetic stirrer and
The instrument for measuring electromotive force monitors solution acid alkalinity in conjunction with pH meter, pre- when reaching by the dripping quantity of computer control standard solution
After determining terminal current potential, it is automatically stopped titration, the content of institute's test elements is calculated by computer data acquisition；
The Vltrasonic device can carry out decentralized and dissolution to sample and operate；
Control system includes corresponding control module: to execute the melting control module of sample melting, melt to complete sample
The wash-offs control module of block dissolution, the module to the adjusting of sample solution pH value, impurity absorption, to be separated by filtration module, solution dense
Contracting control module, chemistry titration control module and computing module.
It by means of this, can be operated by instrumentation, realize the ordered of process control, function modoularization and standardization,
And the visualization of operation automation and process.The present apparatus can also carry out editor's setting to the various parameters of titrimetry, right
Titration curve automatically records, and calculates printing measurement result and saves as original record, reduces the operation and operation of analyst
Error improves the comparativity of laboratory monitoring analysis result, is conducive to laboratory room managing, is suitable for physics & chemistry lab and is used as substitution
Manually-operated boron analyzer device.
Preferably, the transmission transmission device contains the container of sample under motor driven according to program setting, into
Row is mobile and transmission, transmission device are moved in a linear fashion.
Preferably, the program controlled heater device executes alternating temperature speed by process control using electromagnetic heating mode
Rate, heating-up time and soaking time operation.
Preferably, the melting for melting control module and executing sample by controlling；The sample being placed on conveyer belt
It is transmitted to designated position, heating rate and the time of electromagnetic heater are set, after reaching a defined temperature, is kept the temperature into sample
Holding temperature and time is arranged in process；It is all melted to sample, reaches specified time, complete heating and cooling procedure, instrument is certainly
Turn enters in next step.
Preferably, the wash-off control module completes sample frit by controlling come the cleaning function of complete paired samples
It impregnates, dissolution, forms corresponding solution, and liquid feeding cleaning crucible inner wall and outer wall, instrument is transferred in next step automatically after the completion.
Preferably, the pH value adjusts control module and is acidified by controlling to the sample after wash-off resume module
Processing, in favor of impurity under the conditions of pH value appropriate in adsorption sample, after reaching specified parameter, instrument is transferred to next
Step.
Preferably, the adsorbent of predetermined quality is added by controlling for the separation of foreign elements control module, then plus
Heat arrives assigned temperature and time, for adsorbing the impurity in liquor sample；It is filtered after cooling using sand core funnel, using adding
Liquid device is rinsed precipitating and separating and filtering operation, is collected into conical flask using the deionized water of predetermined volume；The feature operation
After, instrument is transferred in next step.
Preferably, the pH value adjusts control module, and solution carries out acid again after being removed by controlling to impurity
Change processing guarantees that solution composition is stablized, and after which reaches specified parameter, instrument is transferred in next step.
Preferably, control module is concentrated in the solution, is added by the way that the container that solution is housed to be transferred on electromagnetic heating plate
Heat carries out solution concentration operation, and solution is made to reach predetermined volume, and after the feature operation, instrument is transferred in next step.
Preferably, be also equipped with preneutralization module, the module by control in the case where pH meter monitors, using charger by standard
Lye instills in above-mentioned solution, and by solution acid alkalinity adjusting to predetermined pH value, which terminates, and instrument is transferred to next automatically
Step.
Preferably, chemistry titration control module and computing module pass through monitoring solution system pH value and potentiometric titrimeter
Electrode potential, automatic dripping standard solution stop after reaching predesigned end point current potential automatically according to obtained potentiometric titration curve
It only titrates, the content of institute's test elements is calculated by computer data acquisition.
Another aspect of the present invention provide it is a kind of test device automatically analyzed using boron element carry out boron element automatically analyze
Method, which is characterized in that system program executes and control process includes:
System boot and self-test check the hardware effort state in corresponding each area, including transmission device, peristaltic pump and corresponding control electricity
The working condition on road, including required heater, charger, potentiometric titrimeter, pH meter and deionized water and corresponding acid
Alkali titer.After System self-test passes through, into sample analysis test operation program；According to program setting, transmission device executes should
Functions of modules will be equipped with the crucible or beaker of sample, be transmitted to designated position, after completing heating, liquid feeding or titration function, according to
Parameter setting and respective feedback data carry out parameter discriminatory analysis, after test parameter meets the predetermined set parameter of the step,
The operating process is completed, sample specimens are then transferred to next specified region by transmission device, it is default to carry out next module
The operation of process.Until terminating to titration process, complete to calculate.
Detailed description of the invention
Fig. 1 shows a kind of boron element acid base titration test device basic operation process of an implementation form according to the present invention
With control sequence schematic diagram；
Fig. 2 shows a kind of semi-open structural representation of boron element acid base titration test device of an implementation form according to the present invention
Figure；
The sample that Fig. 3 shows an implementation form according to the present invention melts the process control process of module；
Fig. 4 shows sample frit and washes out process control process；
Fig. 5 shows sample pH value and adjusts control module process control process；
Fig. 6 shows sample adsorbing contaminant block process；
Fig. 7 shows sample concentration block process；
Fig. 8 shows sample preneutralization block process control flow；
Fig. 9 shows sample drop cover half block flow control procedure.
Specific embodiment
The present invention is further illustrated below in conjunction with attached drawing and following embodiments, it should be appreciated that attached drawing and following embodiments
It is merely to illustrate the present invention, is not intended to limit the present invention.
The object of the present invention is to provide a kind of boron element test device and method based on titration chemical analysis technology, operations
Basic process and control sequence are as shown in Figure 1.Instrumentation and sample treatment and detection process fundamental order are as follows: booting detection is logical
Later, solid sample to be melted is placed in sample heating zone and executes heating, followed by frit washes out process, is followed successively by thereafter molten
In liquid acidification, liquor sample absorption deposition, filtering and the solution concentration of impurity start current potential after completing preneutralization
Titration, obtains test curve, the content of boron element is calculated automatically by computer program.
In an implementation form of the invention, the semi-open structure of test device is as shown in Fig. 2, be from left to right followed successively by heating zone
A, area B, constant-current titration area C and data processing area D are chemically treated.Heating zone and chemical treatment area and constant-current titration area pass through insulation
Baffle 3 keep apart.Have several sliding rails 2 above sample chemical treatment region and constant-current titration area, to fixed suspension buret and
Liquid-adding devices such as soda acid etc., sliding rail can be controlled and be moved up and down for being aligned.Wherein control circuit and titration monitoring circuit are placed in phase
Region rear is answered to be connected to a computer.There is transmission device in heating zone, chemical treatment area, constant-current titration area, under program
Container is moved to corresponding position, may be moved in and out to corresponding station, the functions such as heating and titration are completed under process control.Its
Middle control circuit and titration monitoring circuit, exhaust system do not illustrate and, and are placed in above whole equipment.
The hardware system includes: program controlled heater device, Vltrasonic device, peristaltic pump and its control motor and liquid feeding dress
It sets, liquid-adding device is made of liquid storage device, inlet tube, catheter, outlet tube etc., and system further includes pH meter, sand core funnel 5, current potential
Titrator, mechanical linkage, sliding rail and transmission transmission device and system control, data acquisition, calculating and display computer.
The program controlled heater device, is electromagnetic heater, be used to monitor by temperature sensor and control circuit and
Control temperature.
The liquid-adding device, including peristaltic pump, inlet tube, liquid storage device, catheter, outlet tube, for complete to go from
Sub- water, dilute hydrochloric acid, weak aqua ammonia and standard lye are added in corresponding crucible or beaker, are carried out for dilute sample or with sample
Reaction.
The Vltrasonic device is to carry out decentralized and dissolution effect to sample for realizing.
The sand core funnel is the function for completing to filter sample solution.
The mechanical linkage and sliding rail 2 is to be existed for hanging and fixing inlet tube and buret etc. according to program setting
Under motor driven, can carry out up and down, it is horizontal and move left and right, execute corresponding movement, complete the functions such as movement, liquid feeding, titration.
The transmission device can make crucible 1 and beaker etc. between each operating procedure according to program setting,
It is moved and is transmitted between heating and liquid feeding and titration, transmission device can be carried out with the transmission mode that moves along a straight line.
The pH meter and potentiometric titrimeter, contacts with sample solution to be tested, feeds back by electricity by survey to display
Amount data are shown, and pass to computer, for carrying out instruction and the data display prison of solution acid-base neutralization titration end-point criterion
Control is used.
The control system includes: that sample melts control module, the wash-off module for controlling wash-off portion 6, control pH value tune
The pH value in section portion 7 adjusts control module, the solution concentration control module of separation of foreign elements concentrating part 8, controls titration portion 9
Chemistry titration module and computing module etc..
The melting control module of the control system, function and parameter setting are as follows: the functions of modules is mainly completed
The melting of sample forms corresponding compound.Load weighted sample is placed in designated position on equipment conveyer belt, electromagnetism is set
The heating rate of heating device and time, after reaching a defined temperature, into sample insulating process, be arranged holding temperature and when
Between.It is all melted to sample, reaches specified time, complete heating and cooling procedure, instrument is transferred in next step.
The wash-off control module, function are the samples after melting for silver crucible or platinum crucible, after cooling,
Crucible with sample frit is transferred out of heating furnace by mechanical driving device, carries out wash-off operation.The function and parameter of the module
It is provided that the immersion for completing sample frit, dissolution, aqueous borate solution, and cleaning crucible inner wall and outer wall is formed, by sample
Composition is transferred completely into beaker.Parameter setting are as follows: the deionized water, dilute of predetermined volumes is added in crucible using liquid feeding module
Hydrochloric acid, by the immersion of predetermined time and temperature, and the ultrasound 4 for being subject to predetermined time and intensity is vibrated to promote frit to melt,
Then liquid feeding outlet is controlled by liquid feeding module, rinses the inner and outer wall of crucible several times with the deionized water of predetermined volumes.
With the pH value of liquid in pH meter measurement crucible in flushing, if reaching predetermined value, instrument completes this operation, is transferred to next
Step.
The pH value adjusts control module, and function is to carry out acidification to the sample after wash-off resume module, from
It is dynamic that specified acid, aqueous slkali is added, reach specified pH setting parameter, in favor of under acidity adjustment appropriate in sample impurity suction
It is attached.Operation is automatically controlled including the use of the mobile control sample capacity bottle of mechanical moving device, using charger respectively into sample
Bronsted lowry acids and bases bronsted lowry liquid needed for addition carries out process monitoring using electronics pH meter, reaches predetermined pH value.Parameter setting mainly includes soda acid
The setting of degree.After the parameter reaches specified parameter, instrument is transferred in next step.
The separation of foreign elements control module, function are that predetermined quality is added in the solution that last action obtains
The reagents such as adsorbent such as barium carbonate/calcium carbonate, be then heated to assigned temperature and time, be used to adsorbing contaminant.Make after cooling
It is filtered with sand core funnel, precipitating and separating and filtering behaviour is rinsed using the deionized water of predetermined volume using charger
Make, is collected into conical flask.Thereafter, beaker is cleaned three times by charger, filtrate is all collected into conical flask.Parameter setting
It include: temperature, soaking time etc..After the feature operation, instrument is transferred in next step.
The pH value adjusts control module, and function is controlled using mechanical arm is mobile the solution after impurity removal
Sample beaker adds the HCl (1+1) of predetermined concentration using charger into sample respectively and ammonium hydroxide (1+1) utilizes electronics pH meter
Process monitoring is carried out, predetermined pH is reached.After the parameter reaches specified parameter, instrument is transferred in next step.
Control module is concentrated in the solution, which is that the conical flask equipped with solution is transferred on electric hot plate to heat
Processing carries out concentration operation to solution, solution is made to reach predetermined volume.Parameter setting includes: predetermined volume (ml).Function behaviour
After work, instrument is transferred in next step.
The preneutralization module, which is: under pH meter monitoring, being instilled standard lye NaOH using charger
In above-mentioned solution, pH meter is set to be shown as neutral solution acid alkalinity adjusting.Parameter setting is pH.After the feature operation, instrument
Device is transferred in next step.
The constant-current titration and constituent content computing module, which is: sweet dew required for predetermined quality is added
The alcohols chemical substance such as alcohol, is chemically reacted accordingly, carries out acid base neutralization titration operation followed by potentiometric titrimeter.Electricity
Position titration is that a kind of titrimetry side of titration end-point is determined according to the variation of indicator electrode current potential during acid base titration
Method.In titration, it is inserted into an indicator electrode and a reference electrode in detected solution, forms working battery.With titrant
Addition, ion concentration is tested in solution and is constantly changed, thus the current potential of indicator electrode also accordingly changes.In chemistry
It near stoichiometric point, is tested ion concentration and jumping occurs, indicator electrode current potential also produces jumping, as long as therefore measuring work electricity
The variation of pond electromotive force, so that it may determine the position of titration end-point.Parameter setting includes: during constant-current titration, using referring to
The E-V curve (titration curve) for showing relationship between electrode potential E and titrated lye standard solution volume V is titrated further according to E-V
Single order inverse Δ E/ Δ V-V curve is calculated in curve, and titration volumes corresponding to extreme point are to chemically react terminal
(equivalent point).Finally, element to be tested is calculated according to consumed standard base (SB) liquid product and predetermined titer
Content.
The system program executes and control process is: system boot and self-test check corresponding hardware state, including machine
The motion state of tool transmission device, required heater, charger, potentiometric titrimeter, pH meter and deionized water and corresponding
Soda acid titer etc., after System self-test passes through, analyze test program into sample titration operating process.According to program setting,
Mechanical moving device executes the functions of modules, the crucible or beaker of sample will be housed, is transmitted to designated position, completes heating or adds
After the functions such as liquid, parameter discriminatory analysis is carried out according to parameter setting and respective feedback data, meets the step in test parameter
After predetermined set parameter, the operating process is completed, sample specimens are then transferred to next specified area by mechanical moving device
Domain carries out the operation that next module presets process.Until terminating to titration process, complete to calculate.
The basic step and sequence of operation include: that (1) sample melts；(2) sample washes out after melting；(3) solution ph tune
Section；(4) impurity separates in solution；(5) solution ph is adjusted and is concentrated；(6) constant-current titration；(7) boron content calculates；The base of operation
This step is not limited to said sequence, and adjusts and delete as needed, increases, or even modification process and sequence.
Specifically, the process control process that sample melts module is as shown in Figure 3.A certain amount of sample is put by hand and is added
In thermal crucible, crucible is automatically transferred in heating equipment by mechanical driving device.Program operation first checks for heated
Journey parameter setting, including temperature and time check after terminating correctly, pass through computer and issue instruction execution heating operation, complete
Cooling down removes after sample melts.Heating process can be interrupted or restarted as needed among operating process.This control
Process equally can be clamped and be moved to containers such as crucibles using mechanical arm.
Specifically, sample frit wash-off process control process is as shown in Figure 4.Program operation first checks for cleaning process parameter
Setting, including ultrasonic time and pH value, then going for predetermined volumes is added by peristaltic-type pump arrangement system in procedure auto-control
Ionized water, dilute hydrochloric acid by the immersion of predetermined time and temperature, and are subject to the sonic oscillation of predetermined time and intensity to promote to melt
Block dissolution.Liquid feeding outlet is controlled by liquid feeding module again, if rinsing the inner and outer wall of crucible with the deionized water of predetermined volumes
Dry time.With the pH value of liquid in pH meter measurement crucible in flushing, stops if pH reaches 7, complete to cool down after sample melts
It is cooling to remove.It can interrupt and restart as needed among operating process.After the parameter reaches specified parameter, instrument is automatic
It is transferred in next step.
Specifically, sample pH value adjusting control module process control process is as shown in Figure 5.The functions of modules is to wash-off
Sample after resume module carries out acidification, is automatically added to specified acid, aqueous slkali, reaches specified pH setting parameter, in favor of
Under acidity adjustment appropriate in sample impurity absorption.Program operation first checks for pH value parameter setting, automatically controls behaviour
Make to add HCl (+1) and ammonia into sample respectively using charger including the use of the mobile control sample container of mechanical slip device
Water (1+1) carries out process monitoring using electronics pH meter, reaches predetermined pH.Parameter setting mainly includes the setting of pH value.The ginseng
After number reaches specified parameter, instrument is transferred in next step automatically.
Specifically, sample impurity absorption block process is as shown in Figure 6.Program operation first checks for heating, cleaning process ginseng
Number setting, the function of the module is, in the solution that last action obtains, the examination such as barium carbonate/calcium carbonate of predetermined quality is added
Agent is then heated to assigned temperature and time, is used to adsorbing contaminant.It is filtered after cooling using sand core funnel, using adding
Liquid device is rinsed precipitating and separating and filtering operation, is collected into conical flask using the deionized water of predetermined volume.Thereafter, by adding
Liquid device cleans beaker three times, and filtrate is all collected into conical flask.Parameter setting includes: temperature, soaking time, cleaning.The function
After capable of operating, instrument is transferred in next step automatically.
Specifically, the control of pre-sample concentration block process is as shown in Figure 7.Program operation first checks for concentration parameter setting,
The module is that the conical flask equipped with solution is transferred in electromagnetic heating area to heat, and carries out concentration operation to solution,
Solution is set to reach predetermined volume.Parameter setting includes: predetermined volume.After the feature operation, instrument is transferred in next step automatically.
Specifically, sample preneutralization block process control flow is as shown in Figure 8.Program operation first checks for preneutralization parameter
Setting, e.g., parameter setting is pH=7.Under pH meter monitoring, standard lye NaOH is instilled in above-mentioned solution using charger, it will
Solution acid alkalinity adjusting makes pH meter be shown as neutrality 7.After the feature operation, instrument is transferred in next step automatically.
Specifically, sample drop cover half block flow control procedure is as shown in Figure 9.Program operation first checks for solution acid alkalinity ginseng
The module operational process: number setting carries out chemistry titration operation using potentiometric titrimeter.With the addition of titrant, in solution
Tested ion concentration constantly changes, thus the current potential of indicator electrode also accordingly changes.Near stoichiometric point, quilt
Jumping occurs for measured ion concentration, and indicator electrode current potential also produces jumping, as long as therefore measuring the change of working battery electromotive force
Change, so that it may determine the position of titration end-point.Parameter setting include: during constant-current titration, using indicator electrode current potential E with
The E-V curve (titration curve) of relationship, is calculated further according to E-V titration curve between titrated NaOH standard solution volume V
Single order inverse Δ E/ Δ V-V curve, titration volumes corresponding to extreme point are to chemically react terminal (equivalent point).Most
Afterwards, according to consumed standard base (SB) liquid product and predetermined titer, the content of element to be tested is calculated.
Illustrate substantive distinguishing features and significant progress of the invention combined with specific embodiments below.It should be understood that these realities
Example is applied to be only used for limiting the scope of the invention.In the following examples, the experimental methods for specific conditions are not specified, usually according to routine
Condition.
Embodiment: the main test process and implementation method of the boron element instrument analysis based on chemical analysis technology
Titration test chemical method based on boron element, generally relate to following key step and process: solid sample melts
Solution, frit wash-off, acidification, impurity absorption with separate, solution concentration, preneutralization, acid base titration and calculating.For
Above-mentioned instrument and function, the main example for illustrating following three main process and operation, including, melt the journey of control module operation
Sequence is implemented, and sample washes out process and function (wherein, the work such as pH value adjusting, filtering and preneutralization module are similar), with
And constant-current titration step and implement.
1, the program for melting control module operation is implemented
The functions of modules is mainly to complete the melting of sample, forms borate.Load weighted sample is placed in setting for heating zone
In crucible 1 on standby conveyer belt, the heating rate of control module setting heating device is melted using computer and time, setting are protected
Warm temperature and time.Program operation starts, and the crucible for filling sample is sent into electromagnetic heating furnace by mechanical driving device, according to
The program of setting is heated, after reaching a defined temperature, into insulating process.It is all melted to sample, reaches specified time,
It completes heating and cooling procedure, mechanical driving device automatically moves out crucible according to program, process control instrument is transferred in next step.
In the process in case of contingency procedure, such as need to continue heating to melt, can first terminator, then rerun.
2, sample washes out process and function
Program operation first checks for cleaning process parameter setting.According to program, mechanical moving device sets the crucible for filling sample
In the beaker of cleaning parts (the wash-off portion 6 in Fig. 2).Liquid feeding is controlled by peristaltic pump in a reservoir according to program, (in Fig. 2
In acid-base accommodation portion 7) be added predetermined volumes deionized water and dilute hydrochloric acid.By the immersion of predetermined time and temperature, and add
With the sonic oscillation of predetermined time and intensity to promote frit to melt, then the inner wall of the deionized water flushing crucible with predetermined volumes
Several times with outer wall.Stop rinsing if feedback parameter reaches 7 with the pH value of liquid in pH meter measurement beaker in flushing, by
Mechanical moving device moves the containers out.Pilot process can be taking human as interrupting and continue to execute.PH value adjusting, filtering and preneutralization
The work such as module are similar.
3, constant-current titration step and implementation
The constant-current titration and boron content computing module function, which is: predetermined quality mannitol is added, by borate
Conversion is alcohol boric acid, to carry out acid base neutralization titration (the titration portion 9 in Fig. 2), carries out chemistry using potentiometric titrimeter
Titration operation and monitoring.Program operation, mechanical moving device, which moves into the container for filling sample, to be added in mannitol station, according to journey
Sequence setting predetermined amount carries out addition mannitol, after mixing evenly, tests pH value.Then start to be titrated, NaOH mark is added
Quasi- solution.During constant-current titration, relationship between indicator electrode current potential E and titrated NaOH standard solution volume V, number are utilized
It is sampled according to computer is sent to, determines E-V titration curve.Titration terminates, and sample beaker is moved out to initial original by manipulator
Position, end of run.Thereafter, single order inverse Δ E/ Δ V-V curve, extreme point is calculated according to E-V titration curve in program
Corresponding titration volumes are to chemically react terminal (equivalent point).Finally, long-pending and preparatory according to consumed standard base (SB) liquid
The content of boron element is calculated in determining titer.
An of the invention implementation form provides a kind of boron element based on classical chemical analysis titration technique and automatically analyzes survey
Apparatus and method are tried, carry out automatic operation, including sample particular by the overall process to mannitol Acid and Alkali Titration Analysis technology
The meltings of product, impurity separation, titration.The test device is made of hardware system and corresponding control system, specifically by
Four parts form: sample heating zone, chemical treatment area, constant-current titration area and data processing area.Hardware system includes program
Control heater, Vltrasonic device, liquid-adding device, pH meter, mechanical linkage and transmission device, potentiometric titrimeter and system control
Computer used etc..Control system includes sample heating control module, washes out module, pH value adjustment module, impurity element point
From module, solution concentration control module, chemistry titration module etc..Control system issues instruction and controls each operation link, every
After one operation, according to sample in the setting requirements of the link endpoint parameter, by parameter extraction, computer pair is fed back to
Set parameter is compared and judges, with ensure this step sample treatment correctness and next operating procedure it is normal into
Row.Finally, providing the content of institute's test elements by calculating.The advantages of device is with instrument visualized operation characteristic, together
When have ordered and normalized characteristic, can reduce manual operation error, test analysis quickly, safety, and to each behaviour
Make step have can artificial direct intervention ability.
Under the objective for not departing from essential characteristic of the invention, the present invention can be presented as diversified forms, therefore in the present invention
Implementation form be to be illustrative rather than definitive thereof, limited since the scope of the present invention is defined by the claims rather than by specification,
And all changes fallen in the full scope of equivalents of the range that claim defines or the range that it is defined be understood to include
In detail in the claims.
Claims (12)
1. a kind of boron element based on chemical titration analysis technology automatically analyzes test device, which is characterized in that by hardware system
It is constituted with corresponding control system, the device in hardware system includes: Specimen eliminating beaker or crucible, program controlled heater
Device, mechanical linkage, sliding rail and transmission transmission device, Vltrasonic device, peristaltic pump and its control motor, catheter, go out liquid at liquid storage device
Computer used in pipe, pH meter, sand core funnel, potentiometric titrimeter and system control；
Test device structure is followed successively by sample heating zone, chemical treatment area, constant-current titration area and data processing area in order,
It is on the same operating platform, the sample heating zone is kept apart with other three areas by baffle；
Program controlled heater device is located at heat treatment area, carries out melting behaviour to the sample in crucible or beaker by process control
Make；
Mechanical linkage and sliding rail are located at chemical treatment area and constant-current titration area, to hang and fix inlet tube and buret,
Three-dimensional direction moving is carried out under motor driven or under manual, completes fixed, movement and liquid adding functions；
Liquid-adding device is located at chemical treatment area, including peristaltic pump, liquid storage device, catheter and buret, peristaltic pump are driven by motor,
To titrate or carry out acid-base neutralization；
PH meter includes reference electrode, working electrode and galvanometer, to monitor the pH value of solution；
Potentiometric titrimeter is located at constant-current titration area, is made of reference electrode and indicator electrode, including buret, magnetic stirrer and
The instrument for measuring electromotive force monitors solution acid alkalinity in conjunction with pH meter, pre- when reaching by the dripping quantity of computer control standard solution
After determining terminal current potential, it is automatically stopped titration, the content of institute's test elements is calculated by computer data acquisition；
The Vltrasonic device carries out decentralized and dissolution to sample and operates；
Control system includes corresponding control module: to execute the melting control module of sample melting, melt to complete sample
The wash-offs control module of block dissolution, the pH value adjusting control module that sample solution pH value is adjusted, impurity absorption and
It is separated by filtration module, solution concentration control module, chemistry titration control module and computing module.
2. boron element according to claim 1 automatically analyzes test device, which is characterized in that the transmission transmission device,
According to program setting, the container of sample being contained under motor driven, is moved and is transmitted, transmission transmission device is in a linear fashion
It is moved.
3. boron element according to claim 1 or 2 automatically analyzes test device, which is characterized in that described program control adds
Hot device is executed Cooling rate, heating-up time and soaking time by process control and is operated using electromagnetic heating mode.
4. boron element as claimed in any of claims 1 to 3 automatically analyzes test device, which is characterized in that described
Melt the melting that control module executes sample by controlling；The sample being placed on conveyer belt is transmitted to designated position, setting
The heating rate of electromagnetic heater and time, after reaching a defined temperature, into sample insulating process, be arranged holding temperature and
Time；It is all melted to sample, reaches specified time, complete heating and cooling procedure.
5. boron element as claimed in any of claims 1 to 3 automatically analyzes test device, which is characterized in that described
Control module is washed out by controlling the immersion for completing sample frit come the cleaning function of complete paired samples, dissolution, is formed corresponding molten
Liquid, and liquid feeding cleaning crucible inner wall and outer wall.
6. boron element as claimed in any of claims 1 to 3 automatically analyzes test device, which is characterized in that described
PH value adjusts control module and carries out acidification to washing out control module treated sample by controlling, in favor of suitable
When pH value under the conditions of impurity in adsorption sample.
7. boron element as claimed in any of claims 1 to 3 automatically analyzes test device, which is characterized in that described
Impurity absorption and be separated by filtration module, the adsorbent of predetermined quality be added by controlling, be then heated to assigned temperature and when
Between, for adsorbing the impurity in liquor sample；It is filtered after cooling using sand core funnel, using charger, using predetermined body
Long-pending deionized water is rinsed precipitating and separating and filtering operation, is collected into conical flask.
8. boron element as claimed in any of claims 1 to 3 automatically analyzes test device, which is characterized in that described
PH value adjusts control module, and solution carries out acidification again after being removed by controlling to impurity, guarantees solution composition
Stablize.
9. boron element as claimed in any of claims 1 to 3 automatically analyzes test device, which is characterized in that described
Control module is concentrated in solution, carries out solution concentration operation by the way that the container that solution is housed is transferred to heating on electromagnetic heating plate,
Solution is set to reach predetermined volume.
10. boron element as claimed in any of claims 1 to 3 automatically analyzes test device, which is characterized in that also have
Standby preneutralization module, the module by control standard base (SB) drop to be entered in above-mentioned solution using charger in the case where pH meter monitors,
Solution acid alkalinity is adjusted to predetermined pH value.
11. boron element as claimed in any of claims 1 to 3 automatically analyzes test device, which is characterized in that described
Chemistry titration control module and computing module, by monitoring the electrode potential of solution system pH value and potentiometric titrimeter, automatic drip
Add standard solution, according to obtained potentiometric titration curve, after reaching predesigned end point current potential, titration is automatically stopped, by computer
The content of institute's test elements is calculated in acquisition data.
12. a kind of automatically analyze the method that test device progress boron element automatically analyzes using boron element, which is characterized in that system
Program executes and control process includes:
System boot and self-test check the hardware effort state in corresponding each area, including transmission device, peristaltic pump and corresponding control electricity
The working condition on road, including required heater, charger, potentiometric titrimeter, pH meter and deionized water and corresponding acid
Alkali titer；
After System self-test passes through, into sample analysis test operation program；According to program setting, transmission device executes the module function
Can, the crucible or beaker of sample will be housed, are transmitted to designated position, after completing heating, liquid feeding or titration function, is set according to parameter
It sets and carries out parameter discriminatory analysis with respective feedback data, after test parameter meets the predetermined set parameter of the step, completing should
Then sample specimens are transferred to next specified region by transmission device by operating process, carry out next module and preset process
Operation；
Until terminating to titration process, complete to calculate.
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| CN111474293A (en) * | 2020-04-27 | 2020-07-31 | 广东博创佳禾科技有限公司 | Ralstonia solanacearum solution determination method and determination system |
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| CN113740283A (en) * | 2021-08-29 | 2021-12-03 | 咸宁南玻光电玻璃有限公司 | Method for measuring low-content boron oxide in glass by photometric analysis method |
| CN114965861A (en) * | 2021-02-20 | 2022-08-30 | 宝山钢铁股份有限公司 | Method and device for jointly measuring concentration of sulfuric acid and zinc ions in electrogalvanizing solution |
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| CN114965861A (en) * | 2021-02-20 | 2022-08-30 | 宝山钢铁股份有限公司 | Method and device for jointly measuring concentration of sulfuric acid and zinc ions in electrogalvanizing solution |
| CN114965861B (en) * | 2021-02-20 | 2023-10-17 | 宝山钢铁股份有限公司 | Method and device for jointly measuring concentration of sulfuric acid and zinc ions in electrogalvanizing solution |
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