CN104964972A - Method and apparatus for determining titration end point and realizing automatic titration analysis by means of vision sensor - Google Patents
Method and apparatus for determining titration end point and realizing automatic titration analysis by means of vision sensor Download PDFInfo
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Abstract
The invention discloses a method and apparatus for determining a titration end point and realizing automatic titration analysis by means of a vision sensor. The method comprises the following steps: preprocessing a sample, facilitating dosing reaction before titration of the sample, charging a titration indicator agent, charging a standard titration solution, performing the titration, suddenly changing the titration indicator agent and reporting and utilizing a titration result. The apparatus comprises a sample automatic preprocessing system, a preprocessed sample container, a peristaltic pump A, a peristaltic pump B, a peristaltic pump C, a stirrer A, a reagent bottle, a titration indicator agent bottle, a standard titration solution bottle, a vision sensor and a PLC electric control system. The titration end point is detected by virtue of the vision sensor rather than the manual observation, the automatic titration analysis is realized, and the labor cost is zero; moreover, the application range is wide, the detection efficiency is high, the original record information of the detection process is richer, the immediate titration analysis can be realized, the demand for storing the sample can be reduced, and the probability of the error caused by the sample storage can be reduced to zero.
Description
Technical field
The invention belongs to chemical analysis technology field, particularly relate to one and realize titrimetry automated method and device by vision sensor determination titration end-point.
Background technology
In production and life process, usually need to carry out qualitative and quantitative detection to many materials, include but not limited to environment measuring, on-line checkingi, content of material detection etc.Conventional detection method has chemical analysis, instrumental analysis, bioanalysis etc.Detection analysis carries out productive life for people and social management has important effect.And chemical analysis is these conventional most basic the most frequently used methods of detection method.Analysis based on the chemical reaction utilizing material, is called chemical analysis.Chemical analysis is absolute quantitation, amount per sample, the amount of reaction product or consume the amount of reagent and the stoichiometric relationship of reaction, by calculating the amount of component to be measured.
Titration assay method is ingredient important in chemical analysis, and titration assay method conventional at present has three kinds.The first is manual titrimetry, namely utilize the sudden change of indicator to determine the arrival of titration end-point, need to stop titration by during manual observation indicator discoloration, and be titration end-point with this point, utilize the consumption of buret vs to go out the content of measured matter by formulae discovery.The second is full-automatic Potential Titration Analysis, is by potential electrode potential change, measures ion concentration.First select suitable indicator electrode and contrast electrode, form a working battery with detected solution, then add titrant.In titration process, owing to there is chemical reaction, constantly changed by the concentration of measured ion, thus the current potential of indicator electrode changes thereupon.Near titration end-point, undergone mutation by the concentration of measured ion, cause the hop of electrode potential, therefore can determine titration end-point according to the hop of electrode potential, and provide measurement result.The third is micro-coulometric titration, one " zero balancing " closed loop negative feedback system be made up of coulomb amplifier, titration cell and suitable electrolysis system.The collection of its bias voltage data, the control of pyrolysis furnace temperature are performed by single-chip microcomputer, and are connected with computing machine in the mode of serial communication, thus realize whole system and automatically control.The titration that micro-coulometric titration is used for sulphur and chlorine detects, (1) sulphur titration testing principle: when system is in equilibrium state, constant I3-concentration is kept in titration cell, when there being SO2 to enter titration cell, just react with I3-ion: the I3-concentration in I3-+SO2+H2O → SO3+2H++3I-electrolytic cell reduces, potential electrode to experiencing this change, and by the signal of change input coulomb amplifier, then exports a corresponding electric current by coulomb amplifier and is added to electrolysis electrode to upper.Electrolytic anode electricity bear the I3-that consumes by SO2, until recover original I3-ion concentration: the electricity consumed when 3I-→ I3-+2e measures electrolysis, just can try to achieve the content of total sulfur in sample according to Faraday's laws of electrolysis.(2) chlorine titration testing principle: when system is in equilibrium state, constant Ag+ concentration is kept in titration cell. sample is after cracking, organochlorine is converted into chlorion, bring titration cell into by carrier gas again to react with silver ion: in Ag++Cl-→ AgCl titration cell, concentration of silver ions reduces, indicator electrode is to the change namely indicating this signal, and by the signal of this change input coulomb amplifier, then export a corresponding electric current by coulomb amplifier and be added to electrolysis electrode to upper.Electrolytic anode electricity bear the Ag+ that consumes by Cl-, until recover original Ag+ ion concentration, the electricity consumed when measuring the raw Ag+ of electricity, just can try to achieve the content of total chlorine in sample according to Faraday's laws of electrolysis.Electrolytic cell is safeguarded: should preserve without air pollution place shady and cool, chlorine electrolytic cell must strictly keep in Dark Place; A certain amount of electrolytic solution to be maintained the moment in electrolytic cell, and make platinized platinum below liquid level; Can't reference electrode be stirred, and protect its reference electrode arm and answer bubble-free; Electrolytic solution will often be prepared, and keeps fresh; Do not allow washing lotion or acetone infiltrate with reference to side arm during cleaning, otherwise whole electrolytic cell will be reinstalled.
The feature of above-mentioned three kinds of detection modes determines titration end-point respectively by the hop of indicator colour developing sudden change, electrode potential, electrode potential change, its common trait for be all detect involved by chemical reaction termination and obtain the content that a numerical value can count out measured matter.
Manual titrimetry advantage is applied widely, is the titration assay method being suitable for detection material most species, and limitation is that sample can only manual titration one by one, and titration efficiency is low, and requires high to analyst's technological literacy, and cost of labor is high.
Full-automatic Potential Titration Analysis advantage is robotization titration, and limitation is narrow application range, is only applicable to acid base titration, redox titration, complexometry and precipitation titration, and can only single index successively detect.
Micro-coulometric titration is analyzed advantage and is the Aulomatizeted Detect achieving sulphur and chlorine, and limitation is that the scope of application only detects for the titration of sulphur and chlorine, and can only single index successively detect.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides one and realizing titrimetry automated method and device by vision sensor determination titration end-point.
Of the present inventionly realize technical scheme that titrimetry automated method adopts mainly by vision sensor determination titration end-point:
Realize titrimetry automated method by vision sensor determination titration end-point, comprise the following steps:
1) sample pretreatment, realizes sample pretreatment by the automatic pretreatment system of sample, and after the automatic pretreatment system pre-service of sample, sample splendid attire is in pretreatment sample container;
2) dosing reaction before sample titration, is drawn the reagent stored in reagent bottle in instillation pretreatment sample container by peristaltic pump A, is then stirred the sample of pretreatment sample container by stirrer A;
3) add titrate indicator, the titrate indicator of titrate indicator bottle quantitatively pipettes to pretreatment sample container by peristaltic pump B, and under stirrer A stirs, sample and titrate indicator complete chemical reaction, thus achieve and add titrate indicator;
4) standard titration solution titration is added, the standard titration solution of standard titration solution bottle quantitatively pipettes to pretreatment sample container by peristaltic pump C, under stirrer A stirs, sample and standard titration solution carry out drop reaction, thus achieve and add standard titration solution titration;
5) titrate indicator sudden change, by being provided with vision sensor, vision sensor comprises image acquisition units, graphics processing unit, image processing software, communications interface unit, pretreatment sample container is in one and is equipped with in the environment of image acquisition units, make titrate indicator suddenly change cause pretreatment sample container solution colour sudden change moment, immediately just identify by vision sensor thus determine titration end-point;
6) titration results report and utilization, the titer that when arriving titration end-point by being provided with PLC electric-control system record, peristaltic pump C provides to pretreatment sample container, and be supplied to image processing software by the communications interface unit of vision sensor, the image process and analysis program of image processing software utilizes peristaltic pump C to calculate titrimetric result to the titer that pretreatment sample container provides, and utilize the communications interface unit of vision sensor to carry out exporting printing device to, thus achieve data storing process and transmission, raw readings prints, the report of titration results and utilization.
As the improvement of technique scheme, the image acquisition units of described vision sensor comprises imageing sensor, optical system and illumination, graphics processing unit comprises image processor and video memory, and image processing software comprises image processing function storehouse and image process and analysis program.
As the further improvement of technique scheme, described step 2), 3), 4) in also include stirrer B, stirrer C and stirrer D respectively, described stirrer B, stirrer C and stirrer D stir the solution in reagent bottle, titrate indicator bottle and standard titration solution bottle respectively.
Further, described peristaltic pump A, peristaltic pump B, peristaltic pump C and stirrer A, stirrer B, stirrer C and stirrer D are subject to PLC electric control system controls and run by program of establishing in it.
Of the present inventionly realize technical scheme that titrimetry automation equipment adopts mainly by vision sensor determination titration end-point:
Titrimetry automation equipment is realized by vision sensor determination titration end-point, comprise the automatic pretreatment system of sample, pretreatment sample container, peristaltic pump A, peristaltic pump B, peristaltic pump C, stirrer A, reagent bottle, titrate indicator bottle, standard titration solution bottle, the vision sensor described in technique scheme, and PLC electric-control system.
The invention has the beneficial effects as follows:
Of the present inventionly realize titrimetry automated method and device by vision sensor determination titration end-point, compared to manual titrimetry, the determination of titration end-point of the present invention is detected by vision sensor and replaces manual observation, key obstacle is removed for realizing automation titrimetric analysis, manual titrimetry can be replaced completely, cost of labor reduces to zero, applicability of the present invention covers the applicability of existing three kinds of titration assay method, compared to existing three kinds of titrimetric technique, the present invention is except achieving the automated analysis of the single index of single sample, also achieve different sample different index, the different indexs of same sample or the titrimetry simultaneously of the same index of different sample, substantially increase detection efficiency, compared to existing three kinds of titrimetric technique, testing process raw readings information of the present invention more horn of plenty, and the robotization achieving original detection record is preserved, include but not limited to that the vision achieving titrimetry process is preserved, compared to existing three kinds of titrimetric technique, the present invention can accomplish instant titrimetry, reduce the demand to Sample storage, probability because of the potential error of Sample storage is reduced to zero.
Accompanying drawing explanation
Fig. 1 is automation titrimetric analysis course of work block scheme of the present invention;
Fig. 2 is the composition schematic diagram of vision sensor of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
With reference to Fig. 1,2, of the present inventionly realize titrimetry automated method by vision sensor determination titration end-point, comprise the steps: 1) sample pretreatment 1, sample pretreatment 1 is realized by the automatic pretreatment system 1-1 of sample, the automatic pretreatment system 1-1 of sample obtains long-term ripe application and the equipment that can generally buy, for the Equipments Setting that different detection material (or index) is entered different.After sample automatic pretreatment system 1-1 pre-service, sample needs splendid attire in pretreatment sample container 1-2, the specification of pretreatment sample container 1-2 depending on measured matter (or index) titrimetry principle and standard need determine, material is including but not limited in glass spinner flask, the present invention illustrates for glass spinner flask, pretreatment sample container 1-2 quantity is determined one to one with measured matter index quantity, and following operating in the middle of it is reacted: dosing reaction 2 before sample titration, add titrate indicator 3, add standard titration solution titration 4, titrate indicator sudden change 5, pretreatment sample container 1-2 is in one and is equipped with in the environment of image acquisition units 100,
2) dosing reaction 2 before sample titration, by peristaltic pump A, the reagent stored in reagent bottle is drawn in instillation pretreatment sample container 1-2, then by stirrer A, the sample of pretreatment sample container 1-2 is stirred, stirrer A quantity is determined according to pretreatment sample container 1-2 quantity, it stirs object is sample after pre-service, according to pretreatment sample container 1-2 specification material and stirring object determination type selecting, reagent bottle, its material is determined with the physicochemical property of its corresponding reagent, includes but not limited to plastic bottle, vial; Its quantity measured matter titrimetry principle and the reagent type needed for standard are determined, a reagent bottle joined by normal a kind of reagent, and general total quantity can be more than or equal to 1.Reagent bottle specification volume is multiplied by titrimetric total access times in service time by the volume that the single of various reagent quantitatively pipettes and is multiplied by allowance coefficient to determine.Allowance coefficient is greater than 1, and during to reach last 1 time of total access times, peristaltic pump A hose inlet still can submerge in reagent solution and be as the criterion.Various reagent type and the concentration of its interior storage of each reagent bottle can meet measured matter titrimetry principle and standard, its conserving time limit and condition are restricted and different because of different reagent, quantity and the stirrer B of peristaltic pump A configure one to one according to reagent bottle quantity, and the type selecting of each peristaltic pump A is the demand that need quantitatively pipette with the reagent place of the reagent bottle splendid attire of its correspondence is foundation.The type selecting of stirrer B is type, specification according to reagent bottle and stirs object and determine.Stirrer B is arranged in reagent bottle, and its stirring object is the reagent in reagent bottle.Peristaltic pump A realizes reagent bottle by entrance one end of its flexible pipe and connects, even if its exit end perpendicular to pretreatment sample container 1-2 and titrimetry arrive titration end-point also can not with sample contacts, only can join 1 reagent bottle when following situation and include but not limited to reagent bottle to reduce, the quantity configuration of peristaltic pump A and stirrer B, for simplifying the operation and being conducive to reducing costs: when before sample titration, the reagent 2 kinds or two or more that quantitatively pipette needed for 2 are reacted in dosing, as it is determined testing result accuracy without under the prerequisite affected through experimental comparison checking (or other verification method) by the mixed mix reagent of respective titration volumes, only can configure 1 reagent bottle, stirrer A, stirrer B also stirs its respective stirring object prior to quantitatively pipetting reagent, peristaltic pump A quantitatively pipettes reagent operation again, the reagent quantitative of reagent bottle is moved to pretreatment sample container 1-2, under stirrer A stirs, sample and reagent complete chemical reaction, thus dosing reaction 2 before realizing sample titration, peristaltic pump A and stirrer A, stirrer B is subject to PLC electric control system controls and runs by program of establishing in it,
3) titrate indicator 3 is added, the titrate indicator of titrate indicator bottle quantitatively pipettes to pretreatment sample container 1-2 by peristaltic pump B, under stirrer A stirs, sample and titrate indicator complete chemical reaction, thus achieve and add titrate indicator, the relation that peristaltic pump B is corresponding with titrate indicator bottle is the same with the peristaltic pump A relation corresponding with reagent bottle, the relation that stirrer C is corresponding with titrate indicator bottle is the same with the stirrer B relation corresponding with reagent bottle, and peristaltic pump B and stirrer C is by PLC electric control system controls and run by program of establishing in it;
4) standard titration solution titration 4 is added, the standard titration solution of standard titration solution bottle quantitatively pipettes to pretreatment sample container 1-2 by peristaltic pump C, under stirrer A stirs, sample and standard titration solution carry out drop reaction, thus achieve and add standard titration solution titration 4, the relation that peristaltic pump C is corresponding with standard titration solution bottle is the same with the peristaltic pump A relation corresponding with reagent bottle, the relation that stirrer D is corresponding with standard titration solution bottle is the same with the stirrer B relation corresponding with reagent bottle, peristaltic pump C and stirrer D is subject to PLC electric control system controls and runs by program of establishing in it,
5) titrate indicator sudden change 5, by being provided with vision sensor 5-1, vision sensor 5-1 comprises image acquisition units 100, graphics processing unit 200, image processing software 300, communications interface unit 400, pretreatment sample container 1-2 is in one and is equipped with in the environment of image acquisition units 100, the sudden change moment of the pretreatment sample container 1-2 solution colour that titrate indicator sudden change is caused, instant just identify by vision sensor 5-1 thus determine titration end-point, vision sensor 5-1 is by image acquisition units 100, graphics processing unit 200, image processing software 300, communications interface unit 400 forms, image acquisition units 100 is by imageing sensor 101, optical system 102, illumination 103 composition, under the environment that optical system 102, illumination 103 are built, when titrimetry is carried out adding standard titration solution titration 4 under stirrer A stirs, when the amount of the standard titration solution being titrated to pretreatment sample container 1-2 reaches the moment of titration end-point, titrate indicator suddenlys change, and the solution colour in pretreatment sample container 1-2 becomes another kind of significantly color completely.Optical imagery is converted to digital picture by imageing sensor 101 by this process, then exports graphics processing unit 200 to, and graphics processing unit 200 is made up of image processor 201, video memory 202; Graphics processing unit carries out pre-service, compression to collecting all image/video data in titrimetry process and selectively stores, combining image process software processes image and analyzes, and image processing software 300 is made up of image processing function storehouse 301, image process and analysis program 302.Image processing software comprises the image process and analysis program that the image processing function storehouse of bottom and upper strata are developed for titrimetry.Utilize the powerful image processing function storehouse of band in vision sensor 5-1, digital picture during titration end-point to graphics processing unit 200 pre-service and storage is analyzed, and confirms currently be titration end-point and stop dropping point;
6) titration results is reported and is utilized 6, the titer that when arriving titration end-point by being provided with PLC electric-control system record, peristaltic pump C provides to pretreatment sample container 1-2, and be supplied to image processing software 300 by the communications interface unit 400 of vision sensor 5-1, the titer that the image process and analysis program of image processing software 300 utilizes peristaltic pump C to provide to pretreatment sample container 1-2 calculates titrimetric result, and utilize the communications interface unit of vision sensor 5-1 (400) to carry out exporting printing device to, thus achieve data storing process and transmission, raw readings prints, the report of titration results and utilize 6.Communications interface unit 400 is made up of network interface 401, I/O interface 402, be another important component part of vision sensor 5-1, it mainly completes vision sensor 5-1 and computing machine or other calculate view data transmission between opertaing device and control information exchanges task.By communication interface, optimum configurations is carried out to vision sensor 5-1, complete uploading of data and program; Or transmitted the result of image or analysis chart picture to other equipment by communication interface.The input and output of control signal can also be used as by digital I/O interface, facilitate the connection of vision sensor 5-1 and other automation equipments.
Of the present inventionly realize titrimetry automation equipment by vision sensor determination titration end-point, comprise the automatic pretreatment system 1-1 of sample, pretreatment sample container 1-2, peristaltic pump A, peristaltic pump B, peristaltic pump C, stirrer A, reagent bottle, titrate indicator bottle, standard titration solution bottle, vision sensor 5-1 and PLC electric-control system, the present invention is determined the titration end-point of the titrimetry reaction in 1 pretreatment sample container 1-2 by 1 vision sensor 5-1, then can realize the automation titrimetric analysis of the single index of single sample, due to the graphics processing unit 200 of vision sensor 5-1 and image processing software 300 powerful, Iamge Segmentation can be carried out and levy extraction and object identification parameter estimation.The present invention can utilize the titration end-point of 1 vision sensor 5-1 to the titrimetry reaction in 2 or more pretreatment sample container 1-2 to determine, then can realize the different index of different sample, the different indexs of same sample or the titrimetry simultaneously of the same index of different sample, substantially increase detection efficiency.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, as long as the technical scheme realizing the object of the invention with basic same approach all belongs within protection scope of the present invention.
Claims (5)
1. realize titrimetry automated method by vision sensor determination titration end-point, it is characterized in that, comprise the following steps:
Sample pretreatment (1), realizes sample pretreatment (1) by the automatic pretreatment system of sample (1-1), and after the automatic pretreatment system of sample (1-1) pre-service, sample splendid attire is in pretreatment sample container (1-2);
Dosing reaction (2) before sample titration, is drawn the reagent stored in reagent bottle in instillation pretreatment sample container (1-2) by peristaltic pump A, is then stirred the sample of pretreatment sample container (1-2) by stirrer A;
Add titrate indicator (3), the titrate indicator of titrate indicator bottle quantitatively pipettes to pretreatment sample container (1-2) by peristaltic pump B, under stirrer A stirs, sample and titrate indicator complete chemical reaction, thus achieve and add titrate indicator (3);
Add standard titration solution titration (4), the standard titration solution of standard titration solution bottle quantitatively pipettes to pretreatment sample container (1-2) by peristaltic pump C, under stirrer A stirs, sample and standard titration solution carry out drop reaction, thus achieve and add standard titration solution titration (4);
Titrate indicator sudden change (5), by being provided with vision sensor (5-1), vision sensor (5-1) comprises image acquisition units (100), graphics processing unit (200), image processing software (300), communications interface unit (400), pretreatment sample container (1-2) is in one and is equipped with in the environment of image acquisition units (100), make titrate indicator suddenly change cause pretreatment sample container (1-2) solution colour sudden change moment, immediately just identify by vision sensor (5-1) thus determine titration end-point;
Titration results report and utilization (6), the titer that when arriving titration end-point by being provided with PLC electric-control system record, peristaltic pump C provides to pretreatment sample container (1-2), and be supplied to image processing software (300) by the communications interface unit (400) of vision sensor (5-1), the titer that the image process and analysis program of image processing software (300) utilizes peristaltic pump C to provide to pretreatment sample container (1-2) calculates titrimetric result, and utilize the communications interface unit of vision sensor (5-1) (400) to carry out exporting printing device to, thus achieve data storing process and transmission, raw readings prints, the report of titration results and utilization (6).
2. according to claim 1ly realize titrimetry automated method by vision sensor determination titration end-point, it is characterized in that: the image acquisition units (100) of described vision sensor (5-1) comprises imageing sensor (101), optical system (102) and illumination (103), graphics processing unit (200) comprises image processor (201) and video memory (202), and image processing software (300) comprises image processing function storehouse (301) and image process and analysis program (302).
3. according to claim 1ly realize titrimetry automated method by vision sensor determination titration end-point, it is characterized in that: described step 2), 3), 4) in also include stirrer B, stirrer C and stirrer D respectively, described stirrer B, stirrer C and stirrer D stir the solution in reagent bottle, titrate indicator bottle and standard titration solution bottle respectively.
4. according to claim 3ly realize titrimetry automated method by vision sensor determination titration end-point, it is characterized in that: described peristaltic pump A, peristaltic pump B, peristaltic pump C and stirrer A, stirrer B, stirrer C and stirrer D are by PLC electric control system controls and run by program of establishing in it.
5. realize titrimetry automation equipment by vision sensor determination titration end-point, it is characterized in that: it comprises the automatic pretreatment system of sample (1-1) described in the claims 1, pretreatment sample container (1-2), peristaltic pump A, peristaltic pump B, peristaltic pump C, stirrer A, reagent bottle, titrate indicator bottle, standard titration solution bottle, vision sensor (5-1) and PLC electric-control system.
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