CN102798694B - The method and apparatus of automatic determination of lime activity by titration - Google Patents
The method and apparatus of automatic determination of lime activity by titration Download PDFInfo
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- CN102798694B CN102798694B CN201210294272.8A CN201210294272A CN102798694B CN 102798694 B CN102798694 B CN 102798694B CN 201210294272 A CN201210294272 A CN 201210294272A CN 102798694 B CN102798694 B CN 102798694B
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Abstract
The present invention relates to the method and apparatus that a kind of titrimetry tests Activity of Lime automatically, comprise titration stand, buret, flowmeter, titration cup, stirrer, PH electrode, titration control device, titration platform and water-bath heater.Buret is connected with titrant bottle, and buret is provided with titration switch.Titration control device is connected with PH electrode, flowmeter and titration switch circuit respectively.Determination step is: (1) accurately take the sample 50.0g that granularity is 1 ~ 5mm, is loaded by the hydrochloric acid of 4mol/L in titrant bottle; (2) set titration control device; (3) measure 2000ml water and be placed in titration cup, be heated with stirring to 40 DEG C; (4) sample is joined in titration cup and digest, start and carry out automatic Titration; (5) show the consumption of the hydrochloric acid that titration consumes.The present invention utilizes pH value to control titration, and digestion reaction and neutralization reaction synchronously complete, and realize hydrochloric acid consumption precision, improve the accuracy of Activity of Lime mensuration, carry out multifunctional analysis by titration control device to test figure.
Description
Technical field
The invention belongs to the technical field of performance test of chemical materials, relate to method of testing and the device of activity of lime, be specifically related to a kind of method and apparatus of automatic determination of lime activity by titration.
Background technology
The water activity of lime is the important indicator of inspection lime quality.Lime and water react and generate calcium hydroxide, are commonly called as lime hydrate, and this reaction is also called the digestion reaction of lime and water.The digestion reaction that lime and water carry out is the main method characterizing Activity of Lime.
The test of activity of lime is current in the world has two kinds of methods, hydrochloric titration and temperature rise method.Domestic employing hydrochloric titration is measured, and now current examination criteria is YB/T105-2005 " the metallurgy lime physical property methods of inspection ".Its basic test principle and course of reaction are: after active lime and water react, generate calcium hydroxide, the pH value of solution presents alkalescence, by by the alkalescence in the method neutralization solution of HCI, ensure the equivalent point of solution simultaneously, the consumption of record hydrochloric acid, i.e. the activity degree of this lime of volume characterization of hydrochloric acid used.
Prior art measures Activity of Lime and adopts manually operated method completely, and weak point comprises: one, in testing process, human factor is many, and error is large, and the accuracy of activity degree test result is low.Two, equivalence point of titration judges with the change of phenolphthalein indicator color, phenolphthalein is a kind of weak organic acid, and the color change interval of phenolphthalein is 8.2 ~ 10.0, and namely the colour developing pH value of phenolphthalein reagent is 8.2, therefore digestion reaction carries out just there will be chromogenic reaction when rear pH value is 8.2, and equivalent point exists delayed.Three, be not that clearly due to the effect of vision, in the control of equivalent point, error is very large during color change.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides a kind of method of automatic determination of lime activity by titration to reduce personal error, improving the accuracy that Activity of Lime measures, realize the robotization that Activity of Lime measures.Another object of the present invention is to provide a kind of device of automatic determination of lime activity by titration.
The method of automatic determination of lime activity by titration of the present invention, determination step is as follows:
(1) accurately take the sample 50.0g that granularity is 1 ~ 5mm, be placed in exsiccator for subsequent use, the hydrochloric acid of 4mol/L is loaded in the titrant bottle be connected with buret.
(2) set titration control device (4), equivalent point is ph=7; As ph > 7, titration switch (5) is opened and is carried out titration, during ph < 7, closes titration switch; Set titration time as >=10min.
(3) measure 2000ml water and be placed in titration cup, open water-bath heater (8), turn on agitator stirs, and stirring rate is 300 ~ 400r/min, is heated to 40 DEG C.
(4) sample is joined in titration cup and digest, start titration control device (4), carry out automatic Titration with the hydrochloric acid of 4mol/L.
(5) titration stops, the hydrochloric acid content that titration control device display titration consumes.
Titrimetry of the present invention tests the device of Activity of Lime automatically, comprises titration stand, buret, titration cup, titration platform and water-bath heater, and buret is connected with titrant bottle.Device is provided with PH electrode and titration control device.Buret is provided with flowmeter and titration switch.Titration control device is connected with PH electrode, flowmeter and titration switch circuit respectively.
Titration switch is electromagnetic switch.The material of titration cup is glass or PVC material.
Titration control device is provided with analog-to-digital conversion device, microprocessor, storage hard disk, touch screen interaction control module and control unit of electromagnetic valve.Analog-to-digital conversion device, storage hard disk are connected with microcontroller circuit respectively with control unit of electromagnetic valve.Analog-to-digital conversion device is connected with flowmeter and PH telegraph circuit.Touch screen interaction control module is connected with the mutual circuit of microprocessor.Storage hard disk is connected with the mutual circuit of touch screen interaction control module.Storage hard disk is connected with USB flash disk and printer.
Titration control device take microprocessor as core, realize ph signals collecting, built-in time signals collecting, hydrochloric acid volumetric flow rate signals collecting, realize the display of LCD process, touch screen interaction controls, electromagnetic valve switch controlling functions, analog to digital converter is for realizing the conversion of electric signal and digital signal.
The present invention adopts full automatic mode, utilize the design concept of industrial automation, by computer chip and programme controlled method, in digestion reaction process, there is alkalescence in solution, pH value changes, soda acid electrode produces different electric signal, meanwhile time signal and potential of hydrogen signal export to signal processor, time signal in course of reaction, potential of hydrogen signal are carried out analyzing and processing, and the effect through software provides judgement, and processing instruction is passed to titration control device, control the titration work of hydrochloric acid, realize the instant control of neutralization reaction.By time signal, potential of hydrogen signal, hydrochloric acid volume instant recording while test, store on computers, and form test curve and show over the display, be i.e. the relation curve of time variations and hydrochloric acid volume change.After having tested, by USB port, test figure and analytic curve are downloaded out, carry out filing and exchanging, realize omnidistance digital manipulation.Realize the automation mechanized operation of activity of lime test and the digitizing of test figure.
The present invention is connected with titration switch, PH electrode and flowmeter the automation mechanized operation achieving titration measuring Activity of Lime by titration control.Compared with prior art, beneficial effect of the present invention is: the degree of accuracy 1. improving activity degree measurement result, and error can be controlled within 1% (national standard YB/T105-2005 can permissible error be 4%).2. by titration control device, multifunctional analysis is carried out to test figure.3. reduce personal error factor, reduce experimenter's labour intensity.4. utilize pH value to control titration, digestion reaction and neutralization reaction synchronously complete, and realize the precision of hydrochloric acid consumption, improve the accuracy of Activity of Lime mensuration.
Accompanying drawing explanation
Fig. 1 is the device schematic diagram that titrimetry of the present invention tests Activity of Lime automatically;
Fig. 2 is titration control device schematic diagram.
Wherein:
1-titration stand, 2-PH electrode, 3-stirrer, 4-titration control device, 5-titration switch, 6-buret, 7-titration cup, 8-water-bath heater, 9-titration platform, 10-flowmeter, 11-titrant bottle.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described further.
Titrimetry of the present invention tests the device of Activity of Lime as shown in Figure 1 automatically, comprise titration stand 1, buret 6, flowmeter 10, titration cup 7, stirrer 3, PH electrode 2, titration control device 4, titration platform 9 and water-bath heater 8, buret is connected with titrant bottle 11, buret is provided with titration switch 5, and titration switch is electromagnetic switch.Titration control device is connected with PH electrode, flowmeter and titration switch circuit respectively.The material of titration cup is glass.Titration control device schematic diagram as shown in Figure 2, is provided with analog-to-digital conversion device, microprocessor, storage hard disk, touch screen interaction control module and control unit of electromagnetic valve.Analog-to-digital conversion device, storage hard disk are connected with microcontroller circuit respectively with control unit of electromagnetic valve.Touch screen interaction control module is connected with the mutual circuit of microprocessor.Storage hard disk is connected with the mutual circuit of touch screen interaction control module.Analog-to-digital conversion device is connected with flowmeter and PH telegraph circuit, and storage hard disk is connected with USB flash disk and printer.
The determination step of automatic determination of lime activity by titration of the present invention is:
(1) accurately take the sample 50.0g that granularity is 1 ~ 5mm, be placed in exsiccator for subsequent use, the hydrochloric acid of 4mol/L is loaded in the titrant bottle 11 be connected with buret 6.
(2) set titration control device 4, equivalent point is ph=7; As ph > 7, titration switch (5) is opened and is carried out titration, during ph=7, closes titration switch 5; Setting titration time is 10min.
(3) measure 2000ml water and be placed in titration cup 7, open water-bath heater 8, turn on agitator 3 stirs simultaneously, and stirring rate is 300 ~ 400r/min, is heated to 40 DEG C.
(4) sample is joined in titration cup 7 and digest, start titration control device 4, carry out automatic Titration with the hydrochloric acid of 4mol/L;
(5) titration stops, and titration control device 4 shows the hydrochloric acid content that titration consumes.
The consumption of hydrochloric acid is the activity degree of lime.
Lime and water generation digestion reaction in titration process, solution ph raises, PH electrode detection is to potential of hydrogen signal, pass to analog-to-digital conversion device and be converted into digital signal, then export to microprocessor and carry out analysis judgement, when pH value is greater than 7, the electromagnetic switch to buret exports opening signal, in reactor, instill hydrochloric acid.Period, hydrochloric acid solution flows through flowmeter, and the signal realizing fluid flow exports, and is input to microprocessor, then outputs to the control module of storage unit and touch-screen, indicate the curve of volumetric flow rate on the touchscreen intuitively by analog-to-digital conversion device.When the solution pH value in reactor is less than 7, microprocessor exports shutdown signal to solenoid valve, stops the titration of hydrochloric acid.Touch-screen realizes two functions: display and analysis.In test process, show test curve on a display screen, horizontal ordinate is the time, and ordinate is hydrochloric acid volume used.After having tested, store Test Information by storage hard disk, carried out the setting of parameter by the interactive interface of touch-screen and carried out data analysis, parameter comprises time, volume and the time interval, by printer print result.
Claims (1)
1. a titrimetry tests the device of Activity of Lime automatically, comprise titration stand (1), buret (6), titration cup (7), titration platform (9) and water-bath heater (8), buret is connected with titrant bottle, it is characterized in that: described device is provided with PH electrode and titration control device (4), described buret is provided with flowmeter (10) and titration switch (5); Described titration control device is connected with PH electrode, flowmeter and titration switch circuit respectively; Described titration switch is electromagnetic switch; Described titration control device is provided with analog-to-digital conversion device, microprocessor, storage hard disk, touch screen interaction control module and control unit of electromagnetic valve; Described analog-to-digital conversion device, storage hard disk are connected with microcontroller circuit respectively with control unit of electromagnetic valve; Described analog-to-digital conversion device is connected with flowmeter and PH telegraph circuit; Described touch screen interaction control module is connected with the mutual circuit of microprocessor; Described storage hard disk is connected with the mutual circuit of touch screen interaction control module; Described storage hard disk is connected with USB flash disk and printer; The material of described titration cup (7) is glass or PVC material.
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| CN103336087B (en) * | 2013-06-07 | 2015-04-22 | 中电投远达环保工程有限公司 | Testing device of desulphurization efficiency and testing method thereof |
| CN104250688B (en) * | 2013-06-26 | 2016-12-28 | 宝山钢铁股份有限公司 | The evaluation methodology that sintering quick lime is reactive |
| CN107238676A (en) * | 2017-05-08 | 2017-10-10 | 中山大学 | A kind of controllable temperature control constant-current titration system of environment and its application process |
| CN107957441B (en) * | 2017-11-22 | 2020-01-07 | 孙国明 | Detection device for electrochemical analysis |
| CN109856317A (en) * | 2019-01-21 | 2019-06-07 | 包头钢铁（集团）有限责任公司 | A kind of laboratory dolomite digestion effect real-time characterization method |
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| CN102012375A (en) * | 2010-11-24 | 2011-04-13 | 华中科技大学 | Automatic test method and instrument for modules of sodium silicate |
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| CN1104334A (en) * | 1994-04-29 | 1995-06-28 | 清华大学 | Automatic potentiometric titrimeter |
| EP1912741A1 (en) * | 2005-07-29 | 2008-04-23 | Mettler-Toledo AG | Titration system |
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| CN102012375A (en) * | 2010-11-24 | 2011-04-13 | 华中科技大学 | Automatic test method and instrument for modules of sodium silicate |
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| S7-200pH自动控制系统;李瑾等;《江苏石油化工学院学报》;19990331;第11卷(第1期);第46-49页 * |
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Address after: 051431 Hebei city of Shijiazhuang province Luancheng douyu town equipment manufacturing base of Xinhua Road No. 6 (douyu West Middle School) Applicant after: Shijiazhuang Xinhua Energy and Environmental Protection Technology Co., Ltd. Address before: 051431 Hebei city of Shijiazhuang province Luancheng douyu town equipment manufacturing base of Xinhua Road No. 6 (douyu West Middle School) Applicant before: Shijiazhuang Xinhua Industrial Furnace Co., Ltd. |
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