CN102706941B - Preparation method of ion-selective membrane electrode - Google Patents
Preparation method of ion-selective membrane electrode Download PDFInfo
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- CN102706941B CN102706941B CN201210027311.8A CN201210027311A CN102706941B CN 102706941 B CN102706941 B CN 102706941B CN 201210027311 A CN201210027311 A CN 201210027311A CN 102706941 B CN102706941 B CN 102706941B
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- 239000012528 membrane Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 38
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 17
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012088 reference solution Substances 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 7
- 229910021607 Silver chloride Inorganic materials 0.000 claims abstract description 6
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910052939 potassium sulfate Inorganic materials 0.000 claims abstract description 6
- 235000011151 potassium sulphates Nutrition 0.000 claims abstract description 6
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract 4
- 239000000203 mixture Substances 0.000 claims description 10
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 239000011263 electroactive material Substances 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 6
- 239000011159 matrix material Substances 0.000 abstract description 3
- 239000012744 reinforcing agent Substances 0.000 abstract description 3
- 229920000915 polyvinyl chloride Polymers 0.000 abstract 4
- 239000004800 polyvinyl chloride Substances 0.000 abstract 4
- -1 polytetrafluoroethylene Polymers 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 description 13
- 230000000694 effects Effects 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 238000011160 research Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000004313 potentiometry Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
The invention relates to a preparation method of a sulfate ion-selective membrane electrode. The preparation method comprises the following steps: dissolving 4.8g-6g of PTFE (polytetrafluoroethylene) into 95g of water to be as a matrix; then mixing 1-2ml of sulfuric acid solution with the concentration of 5mol/l, taken as an electroactive substance, with 5ml of the PTFE solution; further adding 0.2-0.5g of nano-aluminum oxide as a reinforcing agent, fully stirring, then uniformly distributing on a porous PVC (polyvinyl chloride) membrane, further covering another layer of PVC membrane on the porous PVC membrane, placing at the temperature of 75 DEG C-85 DEG C, heating for 15-16 hours to prepare a sensitive membrane, and then assembling the membrane electrode by taking Ag/AgCl as an internal reference electrode and 0.1mol/L of potassium sulfate solution as an internal reference solution. The membrane electrode prepared by the method disclosed by the invention has the advantages of excellent strength, good stability and low cost.
Description
Technical field
The present invention relates to a kind of preparation method of membrane electrode.
Background technology
Ion-selective electrode is one of the fastest analytical technology of development in recent years, has formed the potentiometry of system.It is simple that this analytic approach has equipment, easy to operate, be suitable for the features such as on-site measurement and automatic continuous analysis measurement, become commercial production control, environmental monitoring, theoretical research and with the novel important tool of the Relevant Analysis work such as ocean, geology, medical science, chemical industry, metallurgy, atomic energy industry, food processing, agricultural.
Ion-selective electrode is a class electrochemical sensor, mainly comprises three parts:
(1) sensitive membrane: be the part of ion-selective electrode most critical, the character of determining electrode, its effect is that specific ion activity in solution is transformed into film potential;
(2) internal reference electrode: its role is to film potential to draw;
(3) interior reference solution: contain the ion with film and internal reference electrode response.
As most important ingredient in ion-selective electrode, sensitive membrane can be carried out selective response to the ion in solution.In the situation that the ionic strength in solution is certain, the current potential of ion-selective electrode and the logarithm of given ion activity are linear, meet Nernst equation.
The Specifeca tion speeification of ion-selective electrode is intensity, stability, reappearance and life-span, and wherein the stability of ion-selective electrode refers to that a certain concentration of this electrode METHOD FOR CONTINUOUS DETERMINATION is when measured ion, the size of its potential fluctuation amplitude.When reappearance represents that electrode is repeatedly alternately measured in the solution of variable concentrations, the degree that its current potential reappears, hysteresis phenomenon and the memory effect of reflection electrode.Generally with the standard deviation (SD) of electrode potential reading, represent stability and the reappearance of electrode.The life-span of electrode refers to the time that keeps electrode performance parameter constant, and the life-span of electrode is longer, and use value is larger.
The development of membrane electrode all has practical significance for actual production and research.Therefore about for the preparation of membrane electrode also existing many achievements in research, yet although existing membrane electrode performance parameter is fine, as organic sulfonate polymeric membrane etc., its cost is very high, is not suitable for promoting on a large scale; Although and some existing sensitive membrane cost is more moderate, strength and stability is not enough.
Summary of the invention
The object of this invention is to provide a kind of method of preparing low cost and the reliable membrane electrode of strength and stability.
For achieving the above object, technical scheme of the present invention is: a kind of preparation method of membrane electrode, comprises the following steps:
1) configuration polymkeric substance is supported body
By PTFE 4.8g ~ 6g, be dissolved in 95g water, be mixed with PTFE solution;
2) add electroactive material and prepare mixed solution
Get the sulfuric acid solution that 1 ~ 2ml concentration is 5mol/l, then get the PTFE solution that 5 ~ 7ml has configured, both mix and blends;
3) prepare sensitive membrane
Get nano aluminium oxide 0.2 ~ 0.5g, add above-mentioned mixed solution, fully stir the solution that becomes homogeneous transparent, this solution is slowly poured on one deck porous PVC film, and through coating and knifing, mentioned component is evenly distributed on porous PVC film, then cover again another layer of PVC film thereon, under vacuum condition, be placed in the temperature of 75 ° of C ~ 85 ° C, heat 13 ~ 16 hours, thus preparation sensitive membrane;
4) assembling of membrane electrode
Preparation internal diameter is the pvc pipe that 15 ~ 18mm, length are 10cm, cut-off footpath is the sensitive membrane having prepared of 15 ~ 18mm, with the tetrahydrofuran solution of 5wt % PVC, be bonded at the inside bottom of above-mentioned pvc pipe, the past potassium sulfate solution that is wherein filled with 0.1mol/L is as interior reference solution again, in this, in reference solution, insert Ag/AgCl internal reference electrode, component film electrode.
In addition,, as preferred technical scheme, in step 4), the diameter of pvc pipe internal diameter and sensitive membrane is 16mm.
In addition, as preferred technical scheme, in step 3), the vacuum heating conditions of preparation sensitive membrane is: keeping temperature is 80 ° of C, 15 hours heat times.
The present invention, by the prepared ion selective membrane of great many of experiments, leans on molecular force but not chemical bonds between matrix and ionic activity material; And by adding SiO 2 powder as reinforcing agent, increase further physical strength and reduce costs.
Beneficial effect of the present invention is, through METHOD FOR CONTINUOUS DETERMINATION, can obtain operating voltage more than 0.8V, and the film potential value variation of 10 measurement results is no more than 1mV, illustrates that the strength and stability of membrane electrode of the present invention is all better, and cheap.
Embodiment
The present invention is a kind of preferred technical scheme obtaining through experiment, specifically by PTFE 4.8g ~ 6g, is dissolved in 95g water, as matrix; Then will get 1 ~ 2ml concentration and be the sulfuric acid solution of 5mol/l as electroactive material, mix with the above-mentioned PTFE solution of 5ml; Add again 0.2 ~ 0.5g nano aluminium oxide as reinforcing agent, after fully stirring, be distributed on porous PVC film, then cover again another layer of PVC film thereon, in the temperature that is placed in 75 ° of C ~ 85 ° C, heat 15 ~ 16 hours, thereby preparation sensitive membrane, and then potassium sulfate solution that Ag/AgCl is internal reference electrode, the 0.1mol/L membrane electrode as interior reference solution is usingd in assembling.
Wherein, below in conjunction with embodiment and test effect, describe.
Embodiment 1:
A preparation method for membrane electrode, comprises the following steps:
1) configuration polymkeric substance is supported body
By PTFE 4.8g, be dissolved in 95g water, be mixed with PTFE solution;
2) add electroactive material and prepare mixed solution
Get the sulfuric acid solution that 1.5ml concentration is 5mol/l, then get the PTFE solution that 5 ~ 7ml has configured, both mix and blends; Between two kinds of compositions, lean on intermolecular force combination;
3) prepare sensitive membrane
Get nano aluminium oxide 0.3g, add above-mentioned mixed solution, fully stir the solution that becomes homogeneous transparent, this solution is slowly poured on one deck porous PVC film, and through coating and knifing, mentioned component is evenly distributed on porous PVC film, then cover again another layer of PVC film thereon, under vacuum condition, be placed in the temperature of 75 ° of C, heat 16 hours, thus preparation sensitive membrane;
4) assembling of membrane electrode
Preparation internal diameter is the pvc pipe that 15mm, length are 10cm, cut-off footpath is the sensitive membrane having prepared of 15mm, with the tetrahydrofuran solution of 5wt % PVC, be bonded at the inside bottom of above-mentioned pvc pipe, the past potassium sulfate solution that is wherein filled with 0.1mol/L is as interior reference solution again, in this, in reference solution, insert Ag/AgCl internal reference electrode, component film electrode.
The membrane electrode METHOD FOR CONTINUOUS DETERMINATION that this embodiment is made, can obtain operating voltage more than 0.8V, and the film potential value variation of 10 measurement results is no more than 1mV, illustrates that the strength and stability of this membrane electrode is all better.
Embodiment 2
A preparation method for membrane electrode, comprises the following steps:
1) configuration polymkeric substance is supported body
By PTFE 6g, be dissolved in 95g water, be mixed with PTFE solution;
2) add electroactive material and prepare mixed solution
Get the sulfuric acid solution that 2ml concentration is 5mol/l, then get the PTFE solution that 7ml has configured, both mix and blends;
3) prepare sensitive membrane
Get nano aluminium oxide 0.5g, add above-mentioned mixed solution, fully stir the solution that becomes homogeneous transparent, this solution is slowly poured on one deck porous PVC film, and through coating and knifing, mentioned component is evenly distributed on porous PVC film, then cover again another layer of PVC film thereon, under vacuum condition, be placed in the temperature of 80 ° of C, heat 15 hours, thus preparation sensitive membrane;
4) assembling of membrane electrode
Preparation internal diameter is the pvc pipe that 16mm, length are 10cm, cut-off footpath is the sensitive membrane having prepared of 16mm, with the tetrahydrofuran solution of 5wt % PVC, be bonded at the inside bottom of above-mentioned pvc pipe, the past potassium sulfate solution that is wherein filled with 0.1mol/L is as interior reference solution again, in this, in reference solution, insert Ag/AgCl internal reference electrode, component film electrode.
The membrane electrode METHOD FOR CONTINUOUS DETERMINATION that this embodiment is made, can obtain operating voltage more than 0.8V, and the film potential value variation of 10 measurement results is no more than 1mV, illustrates that the strength and stability of this membrane electrode is all better.
The technical scope of this invention is not limited to the content on instructions, must determine its technical scope according to claim scope.
Claims (3)
1. a preparation method for sulfate ion selective membrane electrode, is characterized in that, this preparation method comprises the following steps:
1) configuration polymkeric substance is supported body
By PTFE 4.8g ~ 6g, be dissolved in 95g water, be mixed with PTFE solution;
2) add electroactive material and prepare mixed solution
Get the sulfuric acid solution that 1 ~ 2ml concentration is 5mol/l, then get the PTFE solution that 5 ~ 7ml has configured, both mix and blends;
3) prepare sensitive membrane
Get nano aluminium oxide 0.2 ~ 0.5g, add above-mentioned mixed solution, fully stir the solution that becomes homogeneous transparent, this solution is slowly poured on one deck porous PVC film, and through coating and knifing, mentioned component is evenly distributed on porous PVC film, then cover again another layer of PVC film thereon, under vacuum condition, be placed in 75
oc ~ 85
othe temperature of C, heats 13 ~ 16 hours, thus preparation sensitive membrane;
4) assembling of membrane electrode
Preparation internal diameter is the pvc pipe that 15 ~ 18mm, length are 10cm, cut-off footpath is the sensitive membrane having prepared of 15 ~ 18mm, with the tetrahydrofuran solution of 5wt % PVC, be bonded at the inside bottom of above-mentioned pvc pipe, the past potassium sulfate solution that is wherein filled with 0.1mol/L, as interior reference solution, inserts Ag/AgCl internal reference electrode in this in reference solution again.
2. the preparation method of sulfate ion selective membrane electrode according to claim 1, is characterized in that, in step 4), the diameter of pvc pipe internal diameter and sensitive membrane is 16mm.
3. the preparation method of sulfate ion selective membrane electrode according to claim 1, is characterized in that, in step 3), the vacuum heating conditions of preparation sensitive membrane is: keeping temperature is 80
oc, 15 hours heat times.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1515899A (en) * | 2003-08-25 | 2004-07-28 | 浙江大学 | Electrode for detecting dissolveld sulfate radical content in water body, its preparation and application method |
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- 2012-02-08 CN CN201210027311.8A patent/CN102706941B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1515899A (en) * | 2003-08-25 | 2004-07-28 | 浙江大学 | Electrode for detecting dissolveld sulfate radical content in water body, its preparation and application method |
Non-Patent Citations (4)
| Title |
|---|
| "一种新的硫酸根离子敏感电极";肖丹等;《高等学校化学学报》;19980131;第19卷(第1期);第51-52页 * |
| 段友构."高灵敏度的硫酸根离子选择性电极".《吉首大学学报（自然科学版）》.2002,第23卷(第2期),第31-33页. * |
| 段友构."高灵敏度的硫酸根离子选择性电极".《吉首大学学报(自然科学版)》.2002,第23卷(第2期),第31-33页. * |
| 肖丹等."一种新的硫酸根离子敏感电极".《高等学校化学学报》.1998,第19卷(第1期),第51-52页. * |
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