CN105510518A - Automatic continuous micro-flow titration system and method - Google Patents
Automatic continuous micro-flow titration system and method Download PDFInfo
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- CN105510518A CN105510518A CN201511010214.8A CN201511010214A CN105510518A CN 105510518 A CN105510518 A CN 105510518A CN 201511010214 A CN201511010214 A CN 201511010214A CN 105510518 A CN105510518 A CN 105510518A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/166—Continuous titration of flowing liquids
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Abstract
The invention discloses an automatic continuous micro-flow titration system and method. The automatic continuous micro-flow titration system comprises a bracket, a stepping motor, a transmission shaft, a stirring paddle, a titration cell, an opaque titration cell shell, a precise injection pump, a three-way valve, a connection thin tube and a titration tube, wherein the titration cell is positioned in the titration cell shell; the bottom of the titration cell is provided with a liquid inlet/outlet tube; the liquid inlet/outlet tube passes through the bottom of the titration cell shell; the bracket is provided with an opaque bracket base; the bracket base covers the upper part of the titration cell shell to form an opaque cavity; the bracket base is provided with a titration hole; the stepping motor is arranged on the bracket; an output shaft of the stepping motor is connected with the stirring paddle through the transmission shaft; the stirring paddle passes through the bracket base in order that a stirring head is suspended in the titration cell; the precise injection pump is connected with a public end of the three-way valve; one of other two ports of the three-way valve is communicated with the connection thin tube introduced into a titrating solution, and the other is communicated with the upper end of the titration tube through the connection thin tube; the titration tube is inserted into the titration cell. The system and the method have high sensitivity, and titration data are accurate and reliable.
Description
Technical field
The present invention relates to titrimetry equipment and method, be specifically related to a kind of Automatic continuous miniflow titration system and method.
Background technology
Titration is that standard solution adds in analyzed solution by amount by one, and the color caused in titration process with component to be measured, vs, reaction product, precipitation or conductivity variations etc. determine reaction end, the method for analytical solution composition.The principle judged by titration end-point is different, and titration can be divided into photometric titration, potentiometric titration, coulometric titration etc.; By the difference of reaction principle, soda acid, redox, precipitation or complexometry etc. can be divided into.
Drop reaction is analytical approach conventional in lab analysis, has a lot of index can measure with drop reaction.But drop reaction is very high to manually-operated requirement in laboratory, and the amount of reagent consumed is very large.
Existing titration apparatus many employings electromagnetic agitation, but the mixed effect of electromagnetic agitation is not fine, particularly when vs is darker.Existing titration apparatus adopts dropwise titration, and due to the about 0.25ml of every drop of liquid, this will affect data resolution, and when the small volume of solution undetermined time, the sensitivity of the method obviously reduces.
Due to these reasons, prior art is unsuitable for miniaturization, the robotization of drop reaction especially.
Summary of the invention
In order to solve the problem, the invention provides a kind of Automatic continuous miniflow titration system and method, this system and method mix and blend is effective, and work efficiency is high, can realize the continuous microflow titration of vs, improves titration resolution.
Above-mentioned purpose is achieved by the following technical solution:
A kind of Automatic continuous miniflow titration system, comprises as lower part:
Mechanical raking system: comprise support, stepper motor, transmission shaft, paddle, titration cell and lighttight titration cell shell; Described titration cell is positioned at titration cell shell, is provided with into discharging tube bottom described titration cell, enters discharging tube through titration cell outer casing bottom; Described support has lighttight carrier base, and carrier base is sealed on titration cell shell upper and forms lighttight cavity, and carrier base is provided with titration hole; Described stepper motor is located on support, and the output shaft of stepper motor is connected with paddle by transmission shaft, and paddle makes stirring-head be suspended from titration cell through carrier base;
Continuous microflow titration system: comprise precise injection pump, T-valve, connection tubule and buret; Described precise injection pump is connected with the common port of T-valve, an interface in two other interface of T-valve is communicated with the connection tubule passed in titrant, another interface is communicated with buret upper end by connecting tubule, and buret is inserted in titration cell by titration hole.
Further, described titration cell shell is also provided with the path channels that light can be allowed to pass titration cell bottom, and described titration cell is colorimetric pool.
Further, be also provided with potential electrode, potential electrode is suspended from titration cell through carrier base.
Further, the internal diameter≤1mm of buret.
Further, described titration cell bottom centre is recessed, described in enter discharging tube and be located at bottom centre.
Further, described stirring-head is provided with the blade of four crossing distribution, and the angle of blade and surface level is 30 DEG C.
Based on an Automatic continuous miniflow titration method for above-mentioned Automatic continuous miniflow titration system, comprise following process:
Continuous microflow titration process: start stepper motor after adding liquid to be titrated in titration cell, rotating speed of agitator progressively reaches setting value; After liquid to be titrated stirs evenly, continuous microflow titration system starts titration; Precise injection pump continuously and smoothly injects titrant in titration cell, buret one end is positioned at liquid levels to be titrated with on lower stirring paddle, titrant continuously and smoothly is mixed in liquid to be titrated, rapid mixing reacting under stirring, analyzes the detection data of liquid to be titrated by path channels or potential electrode synchronous acquisition;
Automatic control process: the detection data according to liquid to be titrated judge titration end-point, after arriving titration end-point, titration stops titration in 1 ~ 20 second automatically again, then obtains titration end-point accurately by the detection data that analytical calculation gathers;
Cleaning process: after titration completes, first stops continuous microflow titration, then stops mechanical raking, discharge liquid in titration cell again, last continuous microflow titration system continues plug-flow titrant, plug-flow titrant column length >=1cm, suck afterwards, makes air column length >=5mm; Enter cleaning fluid to titration cell, cleaning fluid liquid level is higher than the height of liquid level in titration cell when dripping off into, and stirring and washing, discharges cleaning fluid, clean 1 ~ 3 time.
Further, before titration starts, in described continuous microflow titration system, be full of vs, only retain one section of air column, air column length >=5mm in one end of buret insertion titration cell.
Further, titrant injection rate≤0.01ml/s, detection data acquiring frequency >=5 of titration liquid/s.
The method of described continuous microflow titration refers to, titrant enters in liquid to be titrated by precise injection pump with very little flow velocity (miniflow) continuously, by stirring rapid mixing reaction continuously, dropwise entering liquid to be titrated from traditional titrant has significantly different, significantly can improve the performance of titration, reduce the demand of whole system water sample and medicine.
Beneficial effect of the present invention:
(1) Automatic continuous miniflow titration system mix and blend provided by the invention is effective, and work efficiency is high, and accuracy is high.
(2) Automatic continuous miniflow titration system provided by the invention can realize the continuous microflow titration of vs, and resolution is high.
(3) Automatic continuous miniflow titration system provided by the invention can realize miniaturization and the robotization of titration apparatus, improves titration efficiency, reduces reagent consumption.
(4) Automatic continuous miniflow titration method provided by the invention can realize the continuous microflow titration of vs, the mode changing the dropwise titration of traditional interruption is push away the mode that titrant enters liquid to be titrated continuously, and adopt and push away titrant technology slowly and realize miniflow, sensitivity and resolution high, the accuracy of titration method can be significantly improved.
Accompanying drawing explanation
Fig. 1 is Automatic continuous miniflow titration system structural representation;
Wherein, 1, support; 2, stepper motor; 3, transmission shaft; 4, paddle; 5, titration cell; 6, titration cell shell; 7, path channels; 8, discharging tube is entered; 9, outage is entered; 10, carrier base; 11, titration hole; 12, stirring-head.
Embodiment
Technical scheme of the present invention is described in detail below in conjunction with specific embodiment.
A kind of Automatic continuous miniflow titration system, comprises mechanical raking system and continuous microflow titration system:
Mechanical raking system as shown in Figure 1, comprises support 1, stepper motor 2, transmission shaft 3, paddle 4, titration cell 5 and lighttight titration cell shell 6.Described titration cell 5 is positioned at titration cell shell 6, is provided with into discharging tube 8 bottom described titration cell 5, enters discharging tube 8 through bottom titration cell shell 6.Described support 1 has lighttight carrier base 10, and carrier base 10 is sealed on titration cell shell 6 and forms lighttight cavity, and carrier base 10 is provided with titration hole 11.Described stepper motor 2 is located on support 1, and the output shaft of stepper motor 2 is connected with paddle 4 by transmission shaft 3, and paddle 4 makes stirring-head 12 be suspended from titration cell through carrier base 10.Described stirring-head 12 is provided with the blade of four crossing distribution, and blade and horizontal plane angle are 30 DEG C.
During for photometric titration, described titration cell shell 6 is also provided with the path channels 7 that light can be allowed to pass titration cell 5 bottom, and described titration cell 5 is colorimetric pool, and described stirring-head 12 is positioned at above path channels 7 level.Described lighttight titration cell shell 6 and lighttight carrier base 10 black nylon material are made.Paddle 4 and stirring-head 12 are quartzy material.Titration cell 5 bottom centre is recessed, enters discharging tube 8 and is located at bottom centre, thus is conducive to the emptying rate of liquid in colorimetric pool, is beneficial to and tests the cleaning after terminating, and avoids polluting.
During for electrometric titration, be also provided with potential electrode, potential electrode is suspended from titration cell through carrier base.
Continuous microflow titration system comprises precise injection pump, T-valve, connection tubule and buret; Described precise injection pump is connected with the common port of T-valve, an interface in two other interface of T-valve is communicated with the connection tubule passed in titrant, another interface is communicated with buret upper end by connecting tubule, and buret is inserted in titration cell by titration hole.Internal diameter≤the 1mm of buret.Buret inserts titration cell by titration hole, and buret titration end is positioned on below liquid level, paddle when titration.
During titration, T-valve first switches to common port and the orifice being communicated with titrant, and titrant drawn by precise injection pump; T-valve is switched to the orifice that common port is communicated with buret again, slowly promote precise injection pump, buret inserts in titration cell and realizes miniflow titration under liquid level.
Based on an Automatic continuous miniflow titration method for above-mentioned Automatic continuous miniflow titration system, comprise following process:
Continuous microflow titration process: start stepper motor after adding liquid to be titrated in titration cell, rotating speed of agitator progressively reaches setting value; After liquid to be titrated stirs evenly, continuous microflow titration system starts titration; Precise injection pump continuously and smoothly injects titrant in titration cell, buret one end is positioned at liquid levels to be titrated with on lower stirring paddle, titrant continuously and smoothly is mixed in liquid to be titrated, rapid mixing reacting under stirring, analyzes the detection data of liquid to be titrated by path channels or potential electrode synchronous acquisition;
Automatic control process: the detection data according to liquid to be titrated judge titration end-point, after arriving titration end-point, titration stops titration in 1 ~ 20 second automatically again, then obtains titration end-point accurately by the detection data that analytical calculation gathers;
Cleaning process: after titration completes, first stops continuous microflow titration, then stops mechanical raking, discharge liquid in titration cell again, last continuous microflow titration system continues plug-flow titrant, plug-flow titrant column length >=1cm, suck afterwards, makes air column length >=5mm; Enter cleaning fluid to titration cell, cleaning fluid liquid level is higher than the height of liquid level in titration cell when dripping off into, and stirring and washing, discharges cleaning fluid, clean 1 ~ 3 time.
Before titration starts, in described continuous microflow titration system, be full of vs, only retain one section of air column, air column length >=5mm in one end of buret insertion titration cell.
Titrant injection rate≤0.01ml/s, detection data acquiring frequency >=5 of titration liquid/s.
Described mechanical raking system, in whipping process, will be guaranteed when reaching maximum stirring rate that vs mixes with liquid to be titrated and complete very soon, and does not produce bubble in stirring liquid.
Paddle in described mechanical raking system has paddle, and paddle and surface level form acute angle, thus liquid can be impelled to move up and down, and acceleration vs mixes with liquid to be titrated.
The method of described continuous microflow titration refers to, titrant enters in liquid to be titrated by precise injection pump with very little flow velocity (miniflow) continuously, by stirring rapid mixing reaction continuously, dropwise entering liquid to be titrated from traditional titrant has significantly different, significantly can improve the performance of titration, reduce the demand of whole system water sample and medicine.
The effect of above-described embodiment is essentiality content of the present invention is described, but does not limit protection scope of the present invention with this.Those of ordinary skill in the art should be appreciated that and can modify to technical scheme of the present invention or equivalent replacement, and does not depart from essence and the protection domain of technical solution of the present invention.
Claims (9)
1. an Automatic continuous miniflow titration system, is characterized in that comprising as lower part:
Mechanical raking system: comprise support, stepper motor, transmission shaft, paddle, titration cell and lighttight titration cell shell; Described titration cell is positioned at titration cell shell, is provided with into discharging tube bottom described titration cell, enters discharging tube through titration cell outer casing bottom; Described support has lighttight carrier base, and carrier base is sealed on titration cell shell upper and forms lighttight cavity, and carrier base is provided with titration hole; Described stepper motor is located on support, and the output shaft of stepper motor is connected with paddle by transmission shaft, and this paddle makes stirring-head be suspended from titration cell by carrier base;
Continuous microflow titration system: comprise precise injection pump, T-valve, connection tubule and buret; Described precise injection pump is connected with the common port of T-valve, an interface in two other interface of T-valve is communicated with the connection tubule passed in titrant, another interface is communicated with buret upper end by connecting tubule, and buret is inserted in titration cell by described titration hole.
2. Automatic continuous miniflow titration system according to claim 1, it is characterized in that: described titration cell shell is also provided with the path channels that light can be allowed to pass titration cell bottom, described titration cell is colorimetric pool.
3. Automatic continuous miniflow titration system according to claim 1, is characterized in that: be also provided with potential electrode, and potential electrode is suspended from titration cell through carrier base.
4. Automatic continuous miniflow titration system according to claim 1, is characterized in that: the internal diameter≤1mm of buret.
5. Automatic continuous miniflow titration system according to claim 1, is characterized in that: described titration cell bottom centre is recessed, described in enter discharging tube and be located at bottom centre.
6. Automatic continuous miniflow titration system according to claim 1, is characterized in that: described stirring-head is provided with the blade of four crossing distribution, and the angle of blade and surface level is 30 DEG C.
7., based on an Automatic continuous miniflow titration method for the arbitrary described Automatic continuous miniflow titration system of claim 1 ~ 6, it is characterized in that, comprise following process:
Continuous microflow titration process: start stepper motor after adding liquid to be titrated in titration cell, rotating speed of agitator progressively reaches setting value; After liquid to be titrated stirs evenly, continuous microflow titration system prepares titration;
Buret lower end is inserted into liquid levels to be titrated with position on lower stirring paddle, precise injection pump continuously and smoothly injects titrant in titration cell, titrant continuously and smoothly is mixed in liquid to be titrated, rapid mixing reacting under stirring, analyzes the detection data of liquid to be titrated by path channels or potential electrode synchronous acquisition;
Automatic control process: the detection data according to liquid to be titrated judge titration end-point, after arriving titration end-point, titration stops titration in 1 ~ 20 second automatically again, then obtains titration end-point accurately by the detection data that analytical calculation gathers;
Cleaning process: after titration completes, first stops continuous microflow titration, then stops mechanical raking, discharge liquid in titration cell again, last continuous microflow titration system continues plug-flow titrant, plug-flow titrant column length >=1cm, suck afterwards, makes air column length >=5mm; Enter cleaning fluid to titration cell, cleaning fluid liquid level is higher than the height of liquid level in titration cell when dripping off into, and stirring and washing, discharges cleaning fluid, clean 1 ~ 3 time.
8. Automatic continuous miniflow titration method according to claim 7, is characterized in that: before titration starts, and is full of vs in described continuous microflow titration system, only retains one section of air column, air column length >=5mm in one end of buret insertion titration cell.
9. Automatic continuous miniflow titration method according to claim 7, is characterized in that: titrant injection rate≤0.01ml/s, detection data acquiring frequency >=5 of titration liquid/s.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106198532A (en) * | 2016-09-05 | 2016-12-07 | 江苏德林环保技术有限公司 | The dual wavelength autocontrol method of a kind of quick photometric titration and device |
CN109115762A (en) * | 2018-08-15 | 2019-01-01 | 南京财经大学 | A kind of oil iv analyzer and its application method |
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SU1330559A2 (en) * | 1986-02-13 | 1987-08-15 | Предприятие П/Я В-8644 | Device for titration |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN106198532A (en) * | 2016-09-05 | 2016-12-07 | 江苏德林环保技术有限公司 | The dual wavelength autocontrol method of a kind of quick photometric titration and device |
CN106198532B (en) * | 2016-09-05 | 2018-09-04 | 江苏德林环保技术有限公司 | A kind of the dual wavelength autocontrol method and device of quick photometric titration |
CN109115762A (en) * | 2018-08-15 | 2019-01-01 | 南京财经大学 | A kind of oil iv analyzer and its application method |
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