CN102798694A - Method and device for automatic determination of lime activity by titration - Google Patents
Method and device for automatic determination of lime activity by titration Download PDFInfo
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- CN102798694A CN102798694A CN2012102942728A CN201210294272A CN102798694A CN 102798694 A CN102798694 A CN 102798694A CN 2012102942728 A CN2012102942728 A CN 2012102942728A CN 201210294272 A CN201210294272 A CN 201210294272A CN 102798694 A CN102798694 A CN 102798694A
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Abstract
The invention relates to a method and a device for automatic determination of lime activity by titration, and the device comprises a titration rack, a burette, a flowmeter, a titration cup, a stirrer, a PH electrode, a titration control device, a titration table, and a water-bath heater. The burette is connected with a titrant bottle, and is provided with a titration switch. The titration control device is respectively connected with the PH electrode, the flowmeter and the titration switch circuit. The determination comprises the following steps: (1) accurately weighing 50.0 g of samples with a particle size of 1-5 mm, adding 4 mol/L hydrochloric acid into the titrant bottle; (2) setting the titration control device; (3) measuring 2000 ml water into the titration cup, stirring and heating to 40 DEG C; (4) adding the sample into the titration cup for digestion, starting the device for automatic titration; (5) displaying the consumption amount of the hydrochloric acid consumed by the titration. According to the invention, the PH value is used for titration control; the digestion reaction and the neutralization reaction are completed synchronously; precision of the hydrochloric acid amount is realized; the accuracy for lime activity determination is improved; and multifunctional analysis of the test data is realized through the titration control device.
Description
Technical field
The invention belongs to the technical field of performance test of chemical materials, relate to the method for testing and the device of activity of lime, be specifically related to a kind of titrimetry and measure the active method and apparatus of lime automatically.
Background technology
The active important indicator of the water of lime for the check lime quality.Lime and water reaction generate calcium hydroxide, are commonly called as lime hydrate, and this reaction is called the digestion reaction of lime and water again.The digestion reaction that lime and water carry out is to characterize the active main method of lime.
The test of activity of lime is current in the world has two kinds of methods, hydrochloric titration and temperature method.Domestic employing hydrochloric titration is measured, and current now examination criteria is YB/T105-2005 " the metallurgy lime physical property method 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, through with the alkalescence in the method neutralization solution of salt acidometric titration, guarantees the equivalent point of solution simultaneously; The consumption of record hydrochloric acid, the i.e. activity degree of this lime of volume characterization of used hydrochloric acid.
Prior art is measured the lime activity and is adopted manually operated method fully, and weak point comprises: one, human factor is many in testing process, and error is big, and the activity degree precision of test result is low.Two, equivalence point of titration is judged with the phenolphthalein indicator change color; Phenolphthalein is a kind of weak organic acid, and the color change interval of phenolphthalein is 8.2～10.0, and promptly the colour developing pH value of phenolphthalein reagent is 8.2; Therefore to carry out back pH value be just chromogenic reaction can occur, equivalent point existence hysteresis at 8.2 o'clock to digestion reaction.Three, be not clearly during change color, because the effect of vision, error is very big in the control of equivalent point.
Summary of the invention
For overcoming the deficiency of prior art, the present invention provides a kind of titrimetry to measure the active method of lime automatically to reduce personal error, improves the accuracy of lime determination of activity, realizes the robotization of lime determination of activity.Another purpose of the present invention provides a kind of titrimetry and measures the active device of lime automatically.
Titrimetry of the present invention is measured the active method of lime automatically, and determination step is following:
⑴ accurately take by weighing the sample 50.0g that granularity is 1 ~ 5mm, places exsiccator subsequent use, and the hydrochloric acid of 4mol/L is packed in the titrant bottle that links to each other with buret.
⑵ set titration controller (4), and equivalent point is ph=7; When ph＞7, titration switch (5) is opened and is carried out titration, and the titration switch is closed in ph＜7 o'clock; Setting titration time is >=10min.
⑶ measure 2000ml water and place titration cup, opens water-bath heater (8), and turn on agitator stirs, and stirring rate is 300 ~ 400r/min, is heated to 40 ℃.
⑷ join sample in the titration cup and digest, and starts titration controller (4), carries out automatic titration with the hydrochloric acid of 4mol/L.
⑸ titration stops, and the titration controller shows the hydrochloric acid content that titration consumed.
Titrimetry of the present invention is tested the active device of lime automatically, comprises titration stand, buret, titration cup, titration platform and water-bath heater, and buret is connected with the titrant bottle.Device is provided with PH electrode and titration controller.Buret is provided with flowmeter and titration switch.The titration controller is connected with PH electrode, flowmeter and titration on-off circuit respectively.
The titration switch is an electromagnetic switch.The material of titration cup is glass or PVC material.
The titration controller is provided with analog-to-digital conversion device, microprocessor, storage hard disk, touch screen interaction control module and solenoid control unit.Analog-to-digital conversion device, storage hard disk are connected with microcontroller circuit respectively with the solenoid control unit.The analog-to-digital conversion device is connected with the PH telegraph circuit with flowmeter.The touch screen interaction control module is connected with the mutual circuit of microprocessor.The storage hard disk is connected with the mutual circuit of touch screen interaction control module.The storage hard disk is connected with printer with USB flash disk.
The titration controller is core with the microprocessor; Realize ph signals collecting, built-in time signal collection, hydrochloric acid volumetric flow rate signals collecting, realize that the LCD process shows, touch screen interaction is controlled, the electromagnetic valve switch control function, analog to digital converter is used to realize the conversion of electric signal and digital signal.
The present invention adopts full automatic mode, utilizes the design concept of industrial automation, through computer chip and programme controlled method; In the digestion reaction process, alkalescence appears in solution, and the pH value changes; The soda acid electrode produces different electric signal, and meanwhile time signal and potential of hydrogen signal are exported to signal processor, and the time signal in the course of reaction, potential of hydrogen signal are carried out analyzing and processing; Effect through software provides judgement; And processing instruction passed to the titration controller, the titration work of control hydrochloric acid realizes the instant control of neutralization reaction.With time signal, potential of hydrogen signal, hydrochloric acid volume instant recording, storage and forms test curve and on display, shows on computers in test, and promptly the time changes and the relation curve of hydrochloric acid volume change.After test is accomplished, test figure and analytic curve are downloaded out, file and exchange, realize that omnidistance digitizing operates through the USB mouth.Realize the automation mechanized operation of activity of lime test and the digitizing of test figure.
The present invention is connected the automation mechanized operation that has realized titration measuring lime activity with flowmeter through titration control and titration switch, PH electrode.Compared with prior art, beneficial effect of the present invention is: 1. improve the degree of accuracy that activity degree is measured the result, error can be controlled in 1% with interior (but the permissible error of national standard YB/T105-2005 is 4%).2. through the titration controller test figure is carried out multifunctional analysis.3. reduce the personal error factor, reduce experimenter's labour intensity.4. utilize pH value control titration, digestion reaction and neutralization reaction are accomplished synchronously, realize the precision of hydrochloric acid consumption, improve the accuracy of lime determination of activity.
Description of drawings
Fig. 1 tests the active device synoptic diagram of lime automatically for titrimetry of the present invention;
Fig. 2 is a titration controller schematic diagram.
Wherein:
1-titration stand, 2-PH electrode, 3-stirrer, 4-titration controller, 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 done further explanation.
It is as shown in Figure 1 that titrimetry of the present invention is tested the active device of lime automatically; Comprise titration stand 1, buret 6, flowmeter 10, titration cup 7, stirrer 3, PH electrode 2, titration controller 4, titration platform 9 and water-bath heater 8; Buret is connected with titrant bottle 11; Buret is provided with titration switch 5, and the titration switch is an electromagnetic switch.The titration controller is connected with PH electrode, flowmeter and titration on-off circuit respectively.The material of titration cup is a glass.Titration controller schematic diagram is as shown in Figure 2, is provided with analog-to-digital conversion device, microprocessor, storage hard disk, touch screen interaction control module and solenoid control unit.Analog-to-digital conversion device, storage hard disk are connected with microcontroller circuit respectively with the solenoid control unit.The touch screen interaction control module is connected with the mutual circuit of microprocessor.The storage hard disk is connected with the mutual circuit of touch screen interaction control module.The analog-to-digital conversion device is connected with the PH telegraph circuit with flowmeter, and the storage hard disk is connected with printer with USB flash disk.
Titrimetry of the present invention is measured the active determination step of lime automatically:
⑴ accurately take by weighing the sample 50.0g that granularity is 1 ~ 5mm, places exsiccator subsequent use, in the titrant bottle 11 that the hydrochloric acid of 4mol/L is packed into buret 6 links to each other.
⑵ set titration controller 4, and equivalent point is ph=7; When ph＞7, titration switch (5) is opened and is carried out titration, during ph=7, closes titration switch 5; The setting titration time is 10min.
⑶ measure 2000ml water and place titration cup 7, opens water-bath heater 8, and turn on agitator 3 stirs simultaneously, and stirring rate is 300 ~ 400r/min, is heated to 40 ℃.
⑷ join sample in the titration cup 7 and digest, and starts titration controller 4, carries out automatic titration with the hydrochloric acid of 4mol/L;
⑸ titration stops, and titration controller 4 shows the hydrochloric acid content that titration consumed.
The consumption of hydrochloric acid is the activity degree of lime.
Lime and water generation digestion reaction in the titration process; The pH value of solution value raises, and the PH electrode detection passes to the analog-to-digital conversion device and is converted into digital signal to the potential of hydrogen signal; Export to microprocessor then and carry out analysis and judgement; When the pH value greater than 7 the time, the electromagnetic switch output opening signal to buret splashes into hydrochloric acid in reactor.During this time, the hydrochloric acid solution flowmeter of flowing through is realized the signal output of fluid flow, is input to microprocessor through the analog-to-digital conversion device, outputs to the control module of storage unit and touch-screen again, on touch-screen, expresses the curve of volumetric flow rate intuitively.When the solution pH value in the reactor less than 7 the time, microprocessor is exported shutdown signal to solenoid valve, stops the titration of hydrochloric acid.Touch-screen is realized two functions: show and analysis.In the test process, on display screen, show test curve, horizontal ordinate is the time, and ordinate is used hydrochloric acid volume.After test was accomplished, through storage hard-disc storage Test Information, the interactive interface through touch-screen carried out the setting of parameter and carries out data analysis, and parameter comprises time, volume and the time interval, through the printer prints result.
Claims (6)
1. a titrimetry is measured the active method of lime automatically, and determination step is following:
⑴ accurately take by weighing the sample 50.0g that granularity is 1 ~ 5mm, places exsiccator subsequent use, in the titrant bottle (11) that the hydrochloric acid of 4mol/L is packed into buret (6) links to each other;
⑵ set titration controller (4), and equivalent point is ph=7; When ph＞7, titration switch (5) is opened and is carried out titration, during ph=7, closes the titration switch; The setting titration time is 10min;
⑶ measure 2000ml water and place titration cup (7), opens water-bath heater (8), and turn on agitator (3) stirs, and stirring rate is 300 ~ 400r/min, is heated to 40 ℃;
⑷ join sample in the titration cup and digest, and starts titration controller (4), carries out automatic titration with the hydrochloric acid of 4mol/L;
⑸ titration stops, and the titration controller shows the hydrochloric acid content that titration consumed.
2. a titrimetry is tested the active device of lime automatically; Comprise titration stand (1), buret (5), titration cup (7), titration platform (9) and water-bath heater (8); Buret is connected with the titrant bottle; It is characterized in that: said device is provided with PH electrode and titration controller (4), and said buret is provided with flowmeter (10) and titration switch (5); Said titration controller is connected with PH electrode, flowmeter and titration on-off circuit respectively.
3. titrimetry according to claim 2 is tested the active device of lime automatically, and it is characterized in that: said titration switch is an electromagnetic switch.
4. titrimetry according to claim 2 is tested the active device of lime automatically, and it is characterized in that: the material of said titration cup (7) is glass or PVC material.
5. titrimetry according to claim 2 is tested the active device of lime automatically, and it is characterized in that: said titration controller is provided with analog-to-digital conversion device, microprocessor, storage hard disk, touch screen interaction control module and solenoid control unit; Said analog-to-digital conversion device, storage hard disk are connected with microcontroller circuit respectively with the solenoid control unit; Said analog-to-digital conversion device is connected with the PH telegraph circuit with flowmeter; Said touch screen interaction control module is connected with the mutual circuit of microprocessor; Said storage hard disk is connected with the mutual circuit of touch screen interaction control module.
6. titrimetry according to claim 5 is tested the active device of lime automatically, and it is characterized in that: said storage hard disk is connected with printer with USB flash disk.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103336087A (en) * | 2013-06-07 | 2013-10-02 | 中电投远达环保工程有限公司 | Testing device of desulphurization efficiency and testing method thereof |
| CN104250688A (en) * | 2013-06-26 | 2014-12-31 | 宝山钢铁股份有限公司 | Evaluation method of reactivity of quicklime for sintering |
| 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 |
| CN107957441A (en) * | 2017-11-22 | 2018-04-24 | 孙国明 | A kind of 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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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103336087A (en) * | 2013-06-07 | 2013-10-02 | 中电投远达环保工程有限公司 | Testing device of desulphurization efficiency and testing method thereof |
| CN104250688A (en) * | 2013-06-26 | 2014-12-31 | 宝山钢铁股份有限公司 | Evaluation method of reactivity of quicklime for sintering |
| 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 |
| CN107957441A (en) * | 2017-11-22 | 2018-04-24 | 孙国明 | A kind of detection device for electrochemical analysis |
| 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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| CN102798694B (en) | 2016-02-10 |
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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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