CN1982887B - Anionic surfactant electrochemical sensor and its manufacture method - Google Patents
Anionic surfactant electrochemical sensor and its manufacture method Download PDFInfo
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- CN1982887B CN1982887B CN2005101284919A CN200510128491A CN1982887B CN 1982887 B CN1982887 B CN 1982887B CN 2005101284919 A CN2005101284919 A CN 2005101284919A CN 200510128491 A CN200510128491 A CN 200510128491A CN 1982887 B CN1982887 B CN 1982887B
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- insulation tube
- tinsel
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Abstract
A surface active anionic electrochemical sensor and a method for manufacturing the same are provided. In an insulation tube, a core wire of a coaxial cable is connected to a metal wire. The metal wire is sealingly and fixedly connected to a lower end of the insulation tube. The metal wire exposes the insulation tube by 10-15mm. The core wire of the coaxial cable at the other end of the insulation tube is connected to a universal BNC joint. An upper segment of the metal wire which exposes the insulation tube is covered by an insulation film, and a lower end is covered by an active dodecyl ammonia polyvinylchloride film. The surface active anionic electrochemical sensor is used for content measurement of various anionic surface active matters in samples. The use temperature is DEG C- DEG C. The detection concentration range is wide and within 10<-7>mol/L-0.10mol/L. The sensitivity is high up to 10<-7>mol/L and is improved by 100-1000 times than that of a conventional anionic surface active sensor. The use effect is notable. The measurement error mainly takes a slope of a standard curve and general is +0.01% to 0.05%.
Description
Technical field
The invention belongs to the organic anion electrode permeable membrane sensor of electrochemical sensor, particularly a kind of surface active anion electrochemical sensor and manufacturing approach thereof.
Background technology
Present organic ion electrochemical sensor generally adopts membrane structure.But present existing thin film electrochemistry sensor, the serviceability temperature narrow range, the detectable concentration narrow range, sensitivity is not high, and error at measurment is big.
Summary of the invention
The purpose of this invention is to provide a kind of organic anion permeable membrane surface active anion electrochemical sensor and manufacturing approach thereof, the temperature range that overcomes the current thin film electrode is narrow, the detectable concentration narrow range, and sensitivity is not high, the big problem of error at measurment.
Scheme of the present invention is: a kind of PVC anion penetrant film surface active anion electrochemical sensor; It is characterized in that: concentric cable is arranged in insulation tube; The heart yearn of its concentric cable connects tinsel; Tinsel is sealedly and fixedly connected in the lower end of insulation tube, and tinsel exposes the outer 10～15mm of insulation tube; The heart yearn of the concentric cable of the insulation tube other end is connected on the general BNC connector, exposes the outer tinsel epimere of insulation tube and is surrounded by dielectric film, and the lower end is active dodecane ammonia polychloroethylene film.
PVC anion-permeable membrane membrane preparation method is characterized in that: at first a kind of PVC 100～200mg of ammonification is dissolved in the organic solvent tetrahydrofuran of 20～30ml, under agitation dissolves 1～2h; With redistilled water preparation 300～500ml anion surface active thing (straight chained alkyl that contains 8～14 carbon atoms) solution to be detected, concentration is 2 times of anion surface active thing (straight chained alkyl that contains 8～14 carbon atoms) critical micelle concentration (CMC); Then consoluet PVC liquid is dropwise dripped the anion surface active thing solution to be detected in the 300ml for preparing, continuous stirring 48h under the condition of no dust; Sediment is filtered with glass sand hourglass, clean three times with redistilled water after and dry.
Secondly a kind of polymeric plasticizer Elvaloy742 0.5～1.0g is dissolved in the organic solvent tetrahydrofuran of 10～15ml; And stir 1-2h with magnetic stirrer; The dried activation PVC of 2/3～1/2 times of amount that adds polymeric plasticizer Elvaloy742 then continues to stir 1h again; After treating that it dissolves fully, filter, and keep filtrating and use when to be coated with millipore filter (aperture is 10 μ m).
In insulation tube,, and tinsel is bonded in an end of insulation tube, lets tinsel expose the outer 10～15mm of insulation tube with epoxy resin with the heart yearn and the welded wire of concentric cable; The heart yearn of concentric cable is connected on the general BNC connector and bonds to together at the other end of insulation tube, after one section tinsel that will expose is done deoxidize and surface finish and handled, clean up and dry; Tinsel after will handling again is with the tetrahydrofuran solution of 2%～5% pure (unionization) PVC coating film treatment that insulate; After treating the dielectric film bone dry, peel off the long dielectric film of 3～5mm on top wiry so that plate active dodecane ammonia polychloroethylene film; The method that the active dodecane ammonia polychloroethylene film plating bath that on exposed tinsel, will prepare is at last dipped with gradation is plated active dodecane ammonia polychloroethylene film and is handled; When treating the about 0.1～0.2mm of the thickness of active dodecane ammonia polychloroethylene film, place it in dry ventilation 3～4d.
Characteristics of the present invention are: this product is applicable to the assay of various anion surface active things in sample; For example in cosmetics and washing industry, measure the Cf of anionic surfactant; Soil; The ion concentration of the anionic surface active substances in river and other water sample also can be developed the mensuration that is used for the relevant active anion concentration with pharmacy industry of medicine.The anionic surface active substances of being measured is the straight chained alkyl that contains 8～14 carbon atoms.Serviceability temperature is :+10 ℃～+ 50 ℃; The detectable concentration scope is wide by 10
-7Mol/L～0.10mol/L, sensitivity is up to 10
-7Mol/L, more conventional anion surface active sensor 10
-5Mol/L～10
-4The sensitivity of mol/L improves 100～1000 times, and its result of use is remarkable, and error at measurment is a benchmark by the slope of typical curve mainly, generally ± 0.01%～0.05%.
Description of drawings
The structural representation of Fig. 1, PVC anion-permeable membrane membrane electrode
Fig. 2, PVC anion-permeable membrane membrane electrode use the structural representation of coupling arrangement
Among the figure: 1 electric signal receiving trap, 2 is contained sampling receptacle, 3 automatic samplers, 4 ion-type contrast electrodes, 5 surface active anion electrochemical sensors, 6 electrochemical cells, 7 welding nodes, 8 shell bodies, 9 concentric cable, the heart yearn of 10 concentric cable, 11 tinsels, 12BNC joint, 13 dielectric films, 14 active plated films
Specific embodiment
Production technology: the production technology of this product mainly contains three parts: use the amino PVC pressed powder of (by the PVC of dodecane ammonia activation) dodecane; The plated film tinsel; Process electrochemical sensor, advantage is the surface that tested negative ion can be adsorbed on sensor securely by PVC.(others directly uses PVC, and shortcoming is that tested negative ion can not be adsorbed by PVC securely).
At first (100～200mg) are dissolved in that a certain amount of (20～30ml) organic solvent tetrahydrofuran under agitation dissolves 1-2h with a kind of PVC of ammonification.With redistilled water preparation 300-500ml anion surface active thing (containing 8 straight chained alkyls to 14 carbon atoms) solution to be detected, concentration is 2 times of anion surface active thing (containing 8 straight chained alkyls to 14 carbon atoms) critical micelle concentration (CMC).Then consoluet PVC liquid is dropwise dripped the anion surface active thing solution to be detected in the 300ml for preparing, continuous stirring 48h under the condition of no dust.Sediment is filtered with glass sand hourglass, clean three times with redistilled water after and dry.
Secondly (0.5～1.0g) is dissolved in a certain amount of (10～15ml) tetrahydrofuran with a kind of polymeric plasticizer Elvaloy742; And with magnetic stirrer stirring 1～2h; The dried activation PVC that adds 2/3～1/2 times of amount of polymeric plasticizer Elvaloy742 then continues to stir 1h again.After treating that it dissolves fully, filter and keep filtrating with millipore filter (aperture is 10 μ m) and use when to be coated.
See shown in the accompanying drawing 1: in the preparation or production of electrochemical sensor; The shell 8 of sensor can directly be selected simple glass tube or rigid pvc tube for use; The heart yearn of concentric cable 10 and tinsel 11 (for example Au, Pt, metals such as Ag and Cu) are welded; (welding node 7) also is bonded in an end of glass tube with epoxy resin with tinsel, lets tinsel expose the outer about 10～15mm of glass tube.The heart yearn of concentric cable is connected on general BNC (the Bayonet Neill Concelman) joint 12 and bonds to together at the other end of glass tube.One section tinsel that will expose cleans up and drying after doing deoxidize and surface finish processing.Tinsel after will handling again is with the tetrahydrofuran solution of 2%～5% pure (unionization) PVC coating film treatment that insulate; After treating dielectric film 13 bone dries, peel off the long dielectric film of 3～5mm on top wiry so that plate active PVC plated film 14.The active membrane plating bath that on exposed tinsel, will prepare at last plates active dodecane ammonia polychloroethylene film processing with the method that the libation at an ancient wedding ceremony is soaked in gradation.When treating the about 0.1～0.2mm of the thickness of active polychloroethylene film, re-use after placing it in dry ventilation 3～4d.
Technical parameter: when the drafting of making typical curve, slope of a curve is the important technological parameters of this anionic electrodeposition chemical sensor.The slope of typical curve is followed ability this spy (NERNST) equation,
Δ E is the mensuration magnitude of voltage (mV) of solution in the formula; Δ E
0Be standard voltage value (mV); N is the valence mumber of treating measured ion (as ± 1 etc., ± symbology sun, negative ion); F is Faraday constant (96485C); R is gas general constant (8.314J mol
-1K
-1); T is absolute temperature (K).A is that the activity of solution to be measured (equals concentration at this, mol/L).As making the mensuration of typical curve 25 ℃ the time, the slope of the typical curve of monovalence active anion, under the situation of every change one one magnitude of solution concentration, its value should be-59.2 (mV).In addition, also can use measured value and the literature value of the critical micelle concentration (CMC) of Anionic Active to oppose and recently judge the performance of this anionic electrodeposition chemical sensor.
1) use method of operating and rules: the experimental provision synoptic diagram: the use of surface active anion electrochemical sensor must be united use with electrochemical cell and electric signal receiving trap computer.Its method of attachment is shown in accompanying drawing 2 tables.
Among the figure: (1) expression electric signal receiving device, a computer that has the data acquisition plug-in unit, this plug-in unit can be bought from businessman, and computer is used to gather and handle the data of measuring.Also can adopt general millivoltmeter or acidity tester etc.(2) be the container of a Sheng sample; (3) be automatic sampler, the programmable operation.Also can adopt micro syringe to come sample introduction; (4) contrast electrode of a kind of ion-type of representative, mercurous chloride electrode for example, silver chloride electrode, nonmetallic ion electrode etc.; (5) be this product-surface active anion electrochemical sensor; (6) be electrochemical cell, constitute by the glassware of a jacketed.Wherein being placed with magnetic stirs seed and is driven by a pneumatic pump.
2) drafting of typical curve: in a steady temperature is 25 ℃ the glassware of jacketed, contain 20～50ml and contain 1.0 * 10
-4The sodium chloride solution of M, generally speaking contrast electrode can select for use bromine to repair ion or silver chloride electrode, and constitutes electrochemical cell with the electrochemical sensor for preparing, and forms complete experimental provision according to accompanying drawing 2 again.Must wait for before the experiment beginning that the reading of voltage/voltmeter tends towards stability, again according to adding certain ion surface active thing for preparing in advance to the order of high concentration by low concentration.Whenever add behind additive need wait 2～3min continue base this write down a secondary data when stablize, and then repeat to total concentration during above about 2～3 times of the critical micelle concentration (CMC) of this surface-active substance, stop to test collection with data.Then all data are made horizontal ordinate by the logarithm of concentration, voltage (millivolt value) is mapped as ordinate, and the curve of gained is typical curve.This mensuration altogether must the time be 1～2h.The slope of typical curve follow can this spy (NERNST) equation, as 25 ℃ the time to the mensuration of the anion surface active thing pure material of monovalence, like the concentration of every change one one magnitude, slope is generally-59.2 (mV), negative sign is represented active anion.
3) mensuration of actual sample: under the prerequisite of known anionic activated species, the mensuration of sample is just become very simple.If change the concentration of sample, the drafting of its experimentation and typical curve is just the same.If just the anionic active matter content in the working sample like river or other water sample, as long as can measure the millivolt value of its sample, again with the typical curve contrast, just can be learnt the content of anionic surface active substances wherein.If be soil or other solid sample, then need do pre-service to sample, as soaking, extraction extracting etc. are measured gained solution again.
Claims (2)
1. surface active anion electrochemical sensor is characterized in that: concentric cable is arranged in insulation tube, and the heart yearn of its concentric cable connects tinsel, and tinsel is sealedly and fixedly connected in the lower end of insulation tube, and tinsel exposes the outer 10～15mm of insulation tube; The heart yearn of the concentric cable of the insulation tube other end is connected on the general BNC connector, exposes the outer tinsel epimere of insulation tube and is surrounded by dielectric film, and the lower end is active dodecane ammonia polychloroethylene film.
2. a surface active anion electrochemical sensor manufacturing approach is characterized in that: at first a kind of PVC 100～200mg of ammonification is dissolved in the organic solvent tetrahydrofuran of 20～30ml, under agitation dissolved 1-2 hour; Contain 8 solution to the straight chained alkyl of 14 carbon atoms with redistilled water preparation 300-500 milliliter anion surface active thing to be detected, concentration contains 82 times to the critical micelle concentration CMC of the straight chained alkyl of 14 carbon atoms for the anion surface active thing; Then consoluet PVC liquid is dropwise dripped in 300 milliliters that prepare anion surface active thing solution to be detected, continuous stirring is 48 hours under the condition of no dust; Sediment is filtered with glass sand hourglass, clean three times with redistilled water after and dry;
Secondly a kind of polymeric plasticizer Elvaloy742 0.5-1.0g is dissolved in the tetrahydrofuran of 10-15ml; And with magnetic stirrer stirring 1～2h; The dried activation PVC that adds 2/3～1/2 times of amount of polymeric plasticizer Elvaloy742 then continues to stir 1h again; After treating that it dissolves fully, using the aperture is that the millipore filter of 10 μ m filters and keeps filtrating and uses when to be coated;
In insulation tube,, and tinsel is bonded in an end of insulation tube, lets tinsel expose the outer 10～15mm of insulation tube with epoxy resin with the heart yearn and the welded wire of concentric cable; The heart yearn of concentric cable is connected on the general BNC connector and bonds to together at the other end of insulation tube, after one section tinsel that will expose is done deoxidize and surface finish and handled, clean up and dry; Tinsel after will handling again is with the tetrahydrofuran solution of the PVC of 2%～5% pure unionization coating film treatment that insulate; After treating the dielectric film bone dry, peel off the long dielectric film of 3～5mm on top wiry so that plate active dodecane ammonia polychloroethylene film; The method that the active dodecane ammonia polychloroethylene film plating bath that on exposed tinsel, will prepare is at last dipped with gradation is plated active dodecane ammonia polychloroethylene film and is handled; When treating the about 0.1～0.2mm of the thickness of active dodecane ammonia polychloroethylene film, place it in dry ventilation 3～4d.
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| CN1384355A (en) * | 2002-06-10 | 2002-12-11 | 武汉大学 | Electrochemical sensor and its prepn and use |
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Patent Citations (6)
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|---|---|---|---|---|
| CN85106976A (en) * | 1985-09-16 | 1987-04-01 | 株式会社堀场制作所 | Measure the electrode of salt density |
| CN2388919Y (en) * | 1999-11-22 | 2000-07-26 | 大连轻工业学院 | Miniature glass electrode for medical use |
| CN1605026A (en) * | 2001-12-20 | 2005-04-06 | 武林敬 | Electrode for active oxygen species and sensor using the electrode |
| CN1384355A (en) * | 2002-06-10 | 2002-12-11 | 武汉大学 | Electrochemical sensor and its prepn and use |
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