CN105301069A - Liquid analysis method and device adopting ion-selective-electrode method - Google Patents
Liquid analysis method and device adopting ion-selective-electrode method Download PDFInfo
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- CN105301069A CN105301069A CN201510642590.2A CN201510642590A CN105301069A CN 105301069 A CN105301069 A CN 105301069A CN 201510642590 A CN201510642590 A CN 201510642590A CN 105301069 A CN105301069 A CN 105301069A
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Abstract
The embodiment of the invention relates to a liquid analysis method and a liquid analysis device adopting an ion-selective-electrode method. The method comprises the following steps: adding a solution to be analyzed into an analysis cup; inserting an external reference electrode and an electrode tube into the solution to be analyzed, wherein the electrode tube comprises a sensitive film and an internal reference electrode, the sensitive film is fixed at the top end of the electrode tube, the electrode tube is filled with an internally filled solution, the internal reference electrode is inserted into the internally filled solution, potential is kept stabilized between the inner surface of the sensitive film and the internal reference electrode, the potential of the external reference electrode is constant, the outer surface of the sensitive film is in contact with the solution to be analyzed, and the potential difference between the sensitive film and the external reference electrode and the activity of ions to be measured in the solution to be analyzed are in a function relation; quantifying the solution to be analyzed, thus obtaining a set amount of solution to be analyzed; adding an ion strength adjusting agent into the solution to be analyzed, and stirring; measuring the potential difference between the sensitive film and the external reference electrode; determining the activity of the ions to be measured in the solution to be analyzed according to the potential difference.
Description
Technical field
The present invention relates to a kind of technical field of analytical chemistry, particularly relate to a kind of liquid analysis method and the device that adopt ion selective electrode method.
Background technology
Ion selective electrode method is the technology grown up the seventies, and international pure chemistry with applied chemistry association to its definition is: " ion-selective electrode is a class chemical sensor, and its logarithm of current potential to the activity of ion given in solution is linear.”
Ion-selective electrode is that one has optionally indicator electrode to certain specific ion.If glass electrode is exactly to H
+ion has optionally electrode, is to measure the most frequently used H of pH value
+the indicator electrode of ion concentration.Since glass electrode was come out in 1906, the history of existing last 100 years.In succession occur Na again afterwards
+, Cl
-, I
-, Ca
+the indicator electrode of plasma sensitivity.But developing rapidly or the thing after the sixties in 20th century of ion-selective electrode.
At present, existing tens kinds of ion-selective electrode come into operation, and this is a kind of novel measurement and detection instrument developed rapidly in recent years.Simple, easy to operate owing to measuring device therefor by ion-selective electrode, and energy rapid Continuous Determination, at industrial automatic analysis, be used widely in environmental monitoring aspect.
Summary of the invention
The object of this invention is to provide a kind of liquid analysis method and the device that adopt ion selective electrode method, simple to operate, measuring accuracy is high, can carry out qualitative and quantitative analysis accurately measure testing liquid.
For achieving the above object, in first aspect, the invention provides a kind of liquid analysis method adopting ion selective electrode method, comprising:
Solution to be analyzed is added in analyzer cup; An outer contrast electrode and an electrode tube is inserted with in described solution to be analyzed; Described electrode tube comprises sensitive membrane and internal reference electrode, described sensitive membrane is fixed on the top of described electrode tube, described electrode tube fills solution built with interior, internal reference electrode be inserted in described in fill in solution, keep the stable of electromotive force between the inside surface of described sensitive membrane and described internal reference electrode; The current potential of described outer contrast electrode is constant, and the outside surface of described sensitive membrane contacts with described solution to be analyzed, treats that the activity of measured ion is funtcional relationship in the electric potential difference between described sensitive membrane and described outer contrast electrode and described solution to be analyzed;
Carry out quantitatively to described solution to be analyzed, discharge redundance, the solution to be analyzed of residue set amount;
In described solution to be analyzed, add ionic strength adjustor according to setting titration speed, and stir;
After leaving standstill, measure the electric potential difference between described sensitive membrane and described outer contrast electrode;
According to described electric potential difference, described in determining, treat the activity of measured ion in described solution to be analyzed.
Preferably, described in analyzer cup, add solution to be analyzed before, described method also comprises carries out prerinse to described analyzer cup.
Preferred further, described prerinse comprises:
Discharge opeing is carried out to described analyzer cup;
Use cleaning liquid to inject described analyzer cup, and stir;
Described cleaning liquid is discharged described analyzer cup;
Re-use cleaning liquid and inject described analyzer cup, and stir;
Again described cleaning liquid is discharged described analyzer cup.
In second aspect, embodiments provide a kind of liquid analysis device adopting ion selective electrode method, in order to realize the liquid analysis method described in above-mentioned first aspect, described device comprises:
Analyzer cup, has bulge loop structure at the rim of a cup of described analyzer cup; Magnet rotor is equipped with in described analyzer cup;
Porous plug is circular configuration; Center has electrode-inserting holes, for electrode insertion; Around described electrode-inserting holes, there is multiple circular hole, in order to insert different liquid lines; Internal diameter and the external diameter of described porous plug and described bulge loop structure match respectively;
Stirring motor, passes through external power source;
Magnet, is fixed in the rotating shaft of described stirring motor, by described stirring motor driven rotary, drives the magnet rotor in described analyzer cup to rotate, thus stir liquid accommodating in described analyzer cup by magnetic force;
Fixed support, comprises fixed support body, upper cover and base;
Described fixed support body comprises saucer and cup; One end of described saucer is connected by backboard with one end of described cup; The center of described saucer has circular hole, and described analyzer cup puts into described fixed support body through described circular hole, be arranged on described saucer, and the bottom of described analyzer cup is carried on described cup by described bulge loop structure;
Described upper cover, top has ring structure, is fastened on described porous plug by described ring structure, establishes be connected with the upper surface spiral shell of described fixed support body; Described electrode-inserting holes and described circular hole expose by the middle of described ring structure;
Described stirring motor and described magnet are fixed on the below of described fixed support body by described base.
Preferably, described electrode comprises: outer contrast electrode and electrode tube;
Described electrode tube comprises sensitive membrane and internal reference electrode, and described sensitive membrane is fixed on the top of described electrode tube, and described electrode tube fills solution built with interior, internal reference electrode be inserted in described in fill in solution.
Preferably, the basal diameter of described analyzer cup is less than the end face diameter of described analyzer cup.
Preferably, described liquid line at least comprises: titration liquid feed tube, liquid feed tube to be analyzed, cleaning liquid feed tube, quantity tube and discharging tube.
Preferably, described porous plug has gulde edge, coordinates be fixed described porous plug with described ring structure, rotates around axial direction to avoid described porous plug.
The liquid analysis method of the employing ion selective electrode method that the embodiment of the present invention provides, simple to operate, measuring accuracy is high, can carry out qualitative and quantitative analysis accurately measure testing liquid.
Accompanying drawing explanation
The process flow diagram of the liquid analysis method of the employing ion selective electrode method that Fig. 1 provides for the embodiment of the present invention;
The schematic diagram of the liquid analysis device that Fig. 2 provides for the embodiment of the present invention.
Embodiment
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
The process flow diagram of the liquid analysis method of the employing ion selective electrode method that Fig. 1 provides for the embodiment of the present invention.Below in conjunction with Fig. 1, the liquid analysis method of the employing ion selective electrode method that the present embodiment provides is described.
Described method comprises the steps:
Step 110, carries out prerinse to analyzer cup;
Concrete, before carrying out fluid analysis, first need to carry out emptying and cleaning to analyzer cup.Cleaning can adopt the cleaning liquids such as deionized water, and wash number is preferably twice.
Prewashed concrete steps can comprise:
Step 111, carries out discharge opeing to analyzer cup;
Step 112, uses cleaning liquid to inject analyzer cup, and stirs;
Step 113, discharges analyzer cup by cleaning liquid;
Step 114, re-uses cleaning liquid and injects analyzer cup, and stir;
Step 115, then cleaning liquid is discharged described analyzer cup.
Through above-mentioned pre-cleaning process, the remaining liq that in analyzer cup, possibility is remaining can be got rid of, avoid having an impact to current analytical test result.
Step 120, adds solution to be analyzed in analyzer cup;
Concrete, first, using solution to be analyzed to clean analyzer cup, make the environment facies of environment and solution to be analyzed in analyzer cup seemingly, getting rid of test interference further, subsequently, then with adding solution to be analyzed, with to be detected.
An outer contrast electrode and an electrode tube is inserted with in solution to be analyzed.Electrode tube comprises sensitive membrane and internal reference electrode, and sensitive membrane is fixed on the top of electrode tube, and electrode tube fills solution built with interior, fills in solution in internal reference electrode is inserted in, and keeps the stable of electromotive force between the inside surface of sensitive membrane and internal reference electrode; The current potential of outer contrast electrode is constant, and the outside surface of sensitive membrane contacts with solution to be analyzed, treats that the activity of measured ion is funtcional relationship in the electric potential difference between the film potential of sensitive membrane and the current potential of outer contrast electrode and solution to be analyzed.
Step 130, treats analytical solution and carries out quantitatively, discharges redundance, the solution to be analyzed of residue set amount;
Concrete, carry out quantitatively according to the capacity of setting to the solution to be analyzed in analyzer cup, the part exceeding set amount is discharged analyzer cup, all identical with the amount of the solution to be analyzed ensureing each test, make test result more accurately and reliably.
Step 140, adds ionic strength adjustor according to setting titration speed, and stirs in described solution to be analyzed;
The film potential of ion-selective electrode with had functional relation by the activity of measured ion, be that supposition solution is when being in perfect condition.But surveyed solution nonideal solution in actual applications, thus also exists various interference, interference first just shows as effective concentration (i.e. " activity ") that ion works in the chemical reaction situation lower than actual concentrations.Only have when effects of ion intensity reaches certain numerical value, this impact is just negligible, and film potential is just linear with ion concentration.When by selective Electrodes Method For The Determination effects of ion, usually will add a certain amount of indifferent electrolyte, regulate solution ion strength, this indifferent electrolyte is called " ionic strength adjustor ".
Step 150, after leaving standstill, measures the electric potential difference between sensitive membrane and outer contrast electrode;
Step 160, according to described electric potential difference, treats the activity of measured ion in described solution to be analyzed described in determining.
Concrete, because the current potential of outer contrast electrode is certain, therefore learn that electric potential difference can calculate the film potential of sensitive membrane.
The liquid analysis method of the employing ion selective electrode method that the embodiment of the present invention provides, simple to operate, measuring accuracy is high, can carry out qualitative and quantitative analysis accurately measure testing liquid.
Accordingly, the embodiment of the present invention additionally provides a kind of device in order to realize aforesaid liquid analytical approach, specifically can as shown in Figure 2,
As shown in the figure, analytical equipment comprises: analyzer cup 1, porous plug 2, electrode 3, stirring motor 4, magnet 5 and fixed support 6.
Analyzer cup 1, is made up of corrosion-resistant and high-temperature resistant glass, has bulge loop structure 11 at the rim of a cup of analyzer cup 1.The basal diameter of analyzer cup 1 is less than end face diameter.
Magnet rotor (not shown) is equipped with, for stirring the liquid in analyzer cup in analyzer cup 1.
Porous plug 2 is circular configuration; Center has electrode-inserting holes 21, for electrode insertion 3; Electrode 3 comprises outer contrast electrode and electrode tube; Electrode tube comprises sensitive membrane and internal reference electrode, and sensitive membrane is fixed on the top of electrode tube, and electrode tube fills solution built with interior, internal reference electrode be inserted in described in fill in solution.
Around electrode 3 patchhole 21, there is multiple circular hole 22, in order to insert different liquid lines.Liquid line at least comprises: these are several for titration liquid feed tube, liquid feed tube to be analyzed, cleaning liquid feed tube, quantity tube and discharging tube.
Liquid feed tube to be analyzed is inserted into the bottom of analyzer cup 1, in analyzer cup 1, carry liquid to be analyzed;
Titration liquid feed tube is inserted into the top of analyzer cup 1, quantitatively instills the titration liquid carrying out with liquid to be analyzed reacting;
Quantity tube is inserted into the middle and upper part of analyzer cup 1 with fixed position, is discharged by the liquid exceeding this position, makes residual liquid quantity in analyzer cup 1 be fixed amount;
Cleaning liquid feed tube injects cleaning liquid in analyzer cup 1, as deionized water;
Discharging tube is inserted into the bottom of analyzer cup 1, is all discharged by the liquid in analyzer cup 1.
Internal diameter and the external diameter of porous plug 2 and bulge loop structure 11 match respectively.
In addition, porous plug 2 also has gulde edge, for fixing the angle position of porous plug 2 when mounted.
Fixed support 6, comprises fixed support body 61, upper cover 62 and base 63; Can be made up of plastic material.
Fixed support body 61 comprises saucer 611 and cup 612; One end of saucer 611 is connected by backboard 613 with one end of cup 612; The center of saucer 611 has circular hole 614, when mounted, analyzer cup 1 puts into fixed support body 61 through circular hole 614, the external diameter of bulge loop structure 11 is greater than the internal diameter of circular hole 614, therefore by bulge loop structure 11, analyzer cup 1 is arranged on saucer 611, and the bottom of analyzer cup 1 is carried on cup 612.
The top of upper cover 62 has ring structure 621, and the edge shape of ring structure 621 and the edge shape of porous plug 2 match, and makes upper cover 62 closely be fastened on porous plug 2 by ring structure 621, establishes be connected with the upper surface spiral shell of fixed support body 61; Electrode-inserting holes 21 and circular hole 22 expose by the middle of ring structure 621.
Stirring motor 4 and magnet 5 are fixed on the below of fixed support body 61 by base 63.
Concrete, stirring motor 4, by external power source, produces rotating force; Magnet 5, is fixed in the rotating shaft (not shown) of stirring motor 4, by stirring motor 4 driven rotary, drives the magnet rotor in analyzer cup 1 to rotate, thus stir liquid accommodating in analyzer cup 1 by magnetic force.
When analytical equipment works, stirring motor 4, by external power source, makes the rotating shaft (not shown) band moving magnet 5 of stirring motor 4 rotate, and drives the magnet rotor in analyzer cup 1 to rotate, stir the liquid in analyzer cup 1 by magnetic force.After stirring, tested by the liquid in electrode 3 pairs of analyzer cups 1, obtain test result.
The analytical equipment that the embodiment of the present invention provides, structure is simple, and working stability, is applicable to ion selective electrode method and carries out analysis to measure accurately to liquid accommodating in it.
Professional should recognize further, in conjunction with unit and the algorithm steps of each example of embodiment disclosed herein description, can realize with electronic hardware, computer software or the combination of the two, in order to the interchangeability of hardware and software is clearly described, generally describe composition and the step of each example in the above description according to function.These functions perform with hardware or software mode actually, depend on application-specific and the design constraint of technical scheme.Professional and technical personnel can use distinct methods to realize described function to each specifically should being used for, but this realization should not thought and exceeds scope of the present invention.
The software module that the method described in conjunction with embodiment disclosed herein or the step of algorithm can use hardware, processor to perform, or the combination of the two is implemented.Software module can be placed in the storage medium of other form any known in random access memory (RAM), internal memory, ROM (read-only memory) (ROM), electrically programmable ROM, electrically erasable ROM, register, hard disk, moveable magnetic disc, CD-ROM or technical field.
Above-described embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only the specific embodiment of the present invention; the protection domain be not intended to limit the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. adopt a liquid analysis method for ion selective electrode method, it is characterized in that, described liquid analysis method comprises:
Solution to be analyzed is added in analyzer cup; An outer contrast electrode and an electrode tube is inserted with in described solution to be analyzed; Described electrode tube comprises sensitive membrane and internal reference electrode, described sensitive membrane is fixed on the top of described electrode tube, described electrode tube fills solution built with interior, internal reference electrode be inserted in described in fill in solution, keep the stable of electromotive force between the inside surface of described sensitive membrane and described internal reference electrode; The current potential of described outer contrast electrode is constant, and the outside surface of described sensitive membrane contacts with described solution to be analyzed, treats that the activity of measured ion is funtcional relationship in the electric potential difference between described sensitive membrane and described outer contrast electrode and described solution to be analyzed;
Carry out quantitatively to described solution to be analyzed, discharge redundance, the solution to be analyzed of residue set amount;
In described solution to be analyzed, add ionic strength adjustor according to setting titration speed, and stir;
After leaving standstill, measure the electric potential difference between described sensitive membrane and described outer contrast electrode;
According to described electric potential difference, described in determining, treat the activity of measured ion in described solution to be analyzed.
2. liquid analysis method according to claim 1, is characterized in that, described in analyzer cup, add solution to be analyzed before, described method also comprises carries out prerinse to described analyzer cup.
3. liquid analysis method according to claim 2, is characterized in that, described prerinse comprises:
Discharge opeing is carried out to described analyzer cup;
Use cleaning liquid to inject described analyzer cup, and stir;
Described cleaning liquid is discharged described analyzer cup;
Re-use cleaning liquid and inject described analyzer cup, and stir;
Again described cleaning liquid is discharged described analyzer cup.
4. adopt a liquid analysis device for ion selective electrode method, in order to realize the liquid analysis method described in the claims 1, it is characterized in that, described device comprises:
Analyzer cup, has bulge loop structure at the rim of a cup of described analyzer cup; Magnet rotor is equipped with in described analyzer cup;
Porous plug is circular configuration; Center has electrode-inserting holes, for electrode insertion; Around described electrode-inserting holes, there is multiple circular hole, in order to insert different liquid lines; Internal diameter and the external diameter of described porous plug and described bulge loop structure match respectively;
Stirring motor, passes through external power source;
Magnet, is fixed in the rotating shaft of described stirring motor, by described stirring motor driven rotary, drives the magnet rotor in described analyzer cup to rotate, thus stir liquid accommodating in described analyzer cup by magnetic force;
Fixed support, comprises fixed support body, upper cover and base;
Described fixed support body comprises saucer and cup; One end of described saucer is connected by backboard with one end of described cup; The center of described saucer has circular hole, and described analyzer cup puts into described fixed support body through described circular hole, be arranged on described saucer, and the bottom of described analyzer cup is carried on described cup by described bulge loop structure;
Described upper cover, top has ring structure, is fastened on described porous plug by described ring structure, establishes be connected with the upper surface spiral shell of described fixed support body; Described electrode-inserting holes and described circular hole expose by the middle of described ring structure;
Described stirring motor and described magnet are fixed on the below of described fixed support body by described base.
5. liquid analysis device according to claim 4, is characterized in that, described electrode comprises: outer contrast electrode and electrode tube;
Described electrode tube comprises sensitive membrane and internal reference electrode, and described sensitive membrane is fixed on the top of described electrode tube, and described electrode tube fills solution built with interior, internal reference electrode be inserted in described in fill in solution.
6. liquid analysis device according to claim 4, is characterized in that, the basal diameter of described analyzer cup is less than the end face diameter of described analyzer cup.
7. liquid analysis device according to claim 4, its feature exists, and described liquid line at least comprises: titration liquid feed tube, liquid feed tube to be analyzed, cleaning liquid feed tube, quantity tube and discharging tube.
8. liquid analysis device according to claim 4, is characterized in that, described porous plug has gulde edge, coordinates be fixed described porous plug with described ring structure, rotates around axial direction to avoid described porous plug.
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Cited By (2)
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CN107202830A (en) * | 2017-06-15 | 2017-09-26 | 南京工业大学 | Prussian blue membrane bioelectrode detection-based device |
CN107271514A (en) * | 2017-06-15 | 2017-10-20 | 南京工业大学 | Method for detecting glucose based on Prussian blue membrane bioelectrode |
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