CN104792836A - Method for detecting electrically neutral gas by electric potential type sensor based on ion selective electrode and device thereof - Google Patents
Method for detecting electrically neutral gas by electric potential type sensor based on ion selective electrode and device thereof Download PDFInfo
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Abstract
The invention relates to detection of electrically neutral gas by an electric potential type sensor and specifically relates to a method for detecting electrically neutral gas by an electric potential type sensor based on an ion selective electrode and a device thereof. According to the method provided by the invention, a molecularly imprinted polymer is taken as an identifying material for selective electrically neutral gas molecules, the identifying material is dispersed in a sensitive film of the polymer film ion selective electrode, and after the polymer film ion selective electrode adsorbs the gas molecules in a gas phase, organic ions with a similar chemical structure with the electrically neutral gas are adopted as indicating ions to indicate a selective identification process between the imprinted polymer in a polymer film phase and the electrically neutral gas molecules to be detected so as to realize electric potential detection of the electrically neutral gas molecules. By using the detection method provided by the invention, direct molecular identification of the electrically neutral gas molecules by the polymer film ion selective electrode in the gas phase is realized, the electric potential detection of the electrically neutral gas is further realized, and the range of application of the ion selective electrode is expanded.
Description
Technical field
The present invention relates to Copper diethlydithiocarbamate and detect electric neutrality gas, specifically a kind of Copper diethlydithiocarbamate based on ion-selective electrode detects method and the device thereof of electric neutrality gas.
Background technology
Polymer film ion selective electrode is an important branch of chemical sensor, this type of electrode has become the new focus in chemical sensor field since late nineteen nineties in last century, has been widely used in the direct mensuration of various electrolyte ion in whole blood, serum, urine, tissue, intracellular fluid and dilution thereof.In gas detect, recent domestic researcher has developed the ion-selective electrode of multiple detection gas, and part realizes commercialization, as ammonia gas-sensing electrode, sulfuretted hydrogen gas sensing electrode, oxysulfide gas sensing electrode and oxides of nitrogen gas sensing electrode etc.The Cleaning Principle of these gas sensing electrodes utilizes gas on the impact of a certain chemical equilibrium, the activity of certain specific ion in balance is changed, again with ion-selective electrode measure solution mutually in the activity change of this specific ion, thus record the concentration of tested gas.It is pointed out that the gas sensing electrode based on ion-selective electrode researched and developed at present only can measure in the solution can the water-soluble and gas of hydrolysis (as ammonia NH
3→ NH
4 +), for the electric neutrality gas molecule being difficult to be hydrolyzed as toluene, formaldehyde and acetone equal solvent gas molecule are difficult to realize detecting.
Adopt ion-selective electrode potential method to detect electric neutrality molecule is for a long time a difficult problem always, because the condition precedent of electrode potential response is that determinand is necessary for charged ion.Recently, we adopt ion-selective electrode technology to achieve the potentiometric detection of electric neutrality organic molecule.The method that the potential method researched and developed detects electric neutrality organic molecule be only for solution mutually in the detection of electric neutrality molecule, the research of the potentiometric detection of electric neutrality gas molecule in gas phase is not yet carried out.Meanwhile, at present all Copper diethlydithiocarbamate based on ion-selective electrode to the Selective recognition process of determinand all solution mutually in carry out, the research adopting this type sensor to realize direct molecular recognition in gas phase there is not yet bibliographical information.
Summary of the invention
The object of the invention is to the deficiency overcoming existing analytical technology, a kind of method providing Copper diethlydithiocarbamate based on ion-selective electrode to detect electric neutrality gas and device thereof.
For achieving the above object, the technical solution used in the present invention is:
A kind of Copper diethlydithiocarbamate based on ion-selective electrode detects the method for electric neutrality gas, identification material using molecularly imprinted polymer as selectivity electric neutrality gas molecule, identify that dispersion of materials is in the sensitive membrane of polymer film ion selective electrode, polymer film ion selective electrode is in the gas phase after adsorption gas molecule, adopt and there is the organic ion of similar chemical structure as indication ion with electric neutrality gas molecule, instruction polymer film is middle Selective recognition process between imprinted polymer and electric neutrality gas molecule to be measured mutually, thus the potentiometric detection realized electric neutrality gas molecule.
Be specially:
The molecularly imprinted polymer a. will with specific recognition capability is used as the molecular recognition material of polymer film ion selective electrode, makes it form ion-selective electrode based on molecularly imprinted polymer sensitive membrane;
B. the ion-selective electrode that step a obtains being inserted containing having in the indication ion measuring cell of analog structure with gas molecule to be measured, producing contrast potential change signal;
C. the gas collector that the ion-selective electrode that step a obtains is placed in containing electric neutrality gas molecule is carried out enrichment, then the ion-selective electrode that step a obtains is proceeded in the measuring cell containing indication ion solution again, produce normal potential variable signal;
D. change with contrast and normal potential and electric neutrality gas concentration is drawn to obtain standard working curve;
E. the gaseous sample that the ion-selective electrode that step a obtains is placed in containing gas to be measured is carried out enrichment, then the ion-selective electrode that step a obtains is proceeded in the measuring cell containing indication ion again, produce sample potential change signal; Namely the concentration of electric neutrality gas to be measured is obtained by reference standard working curve.
Described electric neutrality gas molecule is the gaseous molecular of benzene,toluene,xylene, chlorobenzene, dichloro-benzenes, dinitrotoluene (DNT), acetonitrile, chloroform, normal heptane, cyclohexane, trichloroethanes, tetrahydrofuran, ethyl acetate, DMF, triclene, formaldehyde, acetone, methyl alcohol, ethanol, isopropyl alcohol, normal butyl alcohol or isobutyl alcohol.
Described indication ion is the organic ion with electric neutrality gas molecule to be measured with similar chemical structure, and the indication ion as toluene gas molecule is benzoate.
The preparation of the sensitive membrane of described polymer film ion selective electrode: polymeric matrix material, plastifier, molecularly imprinted polymer particle and ion exchanger are 20-40:40-80:0.2-20:0.1-10 mixing by ratio of weight and the number of copies, then be dissolved in tetrahydrofuran solution, stirring makes it to mix, at room temperature naturally volatilize evenly, namely obtain polymer sensitive membrane.
Described polymeric matrix material is Polyvinylchloride, poly-butyl propyleneglycol acid esters, butyl polyacrylate, polyetherimide, rubber, sol-gel film; Plastifier is o-nitrobenzene octyl ether (o-NPOE), two-2-ethylhexyl esters in the last of the ten Heavenly stems, dibutyl sebacate, di-n-octyl sebacate; Ion exchanger is cationite four (3,5-bis-(trifluoromethyl) phenyl) sodium borate or anionite dinonylnaphthalene sulfonic acid or three (dodecyl) ammonium chloride.
Described molecularly imprinted polymer particle is mixed than 1:1-10:1-100 by mole fraction electric neutrality gas template molecule, function monomer and crosslinking chemical, then add 5-100ml pore-foaming agent, ultrasonic 10min, under initiating agent exists, 50-100 DEG C of thermal-initiated polymerization 1-24h obtains white chunks polymkeric substance, resulting polymers adopts the continuous wash-out repeatedly of eluting solvent, each wash-out 2h, until eluent in ultra-violet absorption spectrum without absorption peak, obtain molecularly imprinted polymer.
Described function monomer is acrylic acid, methacrylic acid, acrylamide, DAP, 2-vinylpyridine, 4-vinylpridine or 4-vinylphenylboronic acid; Described crosslinking chemical is glycol methacrylate or divinylbenzene; Described pore-foaming agent is benzene, toluene, acetonitrile, chloroform, tetrahydrofuran or methyl alcohol; Described initiating agent is 2,2 '-azoisobutyronitrile, 2,2 '-azoisobutyronitrile or 2,2 '-azo-bis-(2,4-methyl pentane nitrile); Described eluant, eluent is methyl alcohol and acetic acid (v/v, 1/1 ~ 9/1).
Copper diethlydithiocarbamate based on ion-selective electrode detects a special purpose device for the method for electric neutrality gas, and special purpose device comprises gas generator 1, gas collector 5, detection cell 6, ion-selective electrode 7, contrast electrode 8 and PXSJ-216L ionometer 10; Gas generator 1 comprises carrier gas device 2 and liquid memory 4, wherein be connected by pipeline A between carrier gas device 2 with liquid memory 4, be connected by pipeline B between liquid memory 4 with gas collector 5, a pipeline C in parallel on the pipeline A between carrier gas device 2 with the liquid memory 4 and pipeline B between liquid memory 4 with gas collector 5; Ion-selective electrode 7 is connected with PXSJ-216L ionometer 10 respectively by wire with contrast electrode 8; Ion-selective electrode 7 is inserted in detection cell 6 after first inserting gas collector 5 adsorbed gas again; Polymer sensitive membrane 9 is provided with bottom ion-selective electrode 7.
Flowmeter 3 is respectively equipped with on pipeline A between described carrier gas device 2 and liquid memory 4 and on described pipeline C.
Under pipeline A between described carrier gas device 2 and liquid memory 4 is inserted into the liquid level of liquid memory 4; Pipeline B between liquid memory 4 and gas collector 5 is inserted on the liquid level of liquid memory 4.
Cleaning Principle: molecularly imprinted polymer has the features such as structure effect precordainment, specific recognition and extensive practicality, is widely used in analytical chemistry field.Molecular imprinting integrates the feature of separation and consentration, can improve selectivity and the sensitivity of analysis; Molecularly imprinted polymer has very strong stability, can resist the rugged surroundings of detection, and therefore molecularly imprinted polymer is that polymer film ion selective electrode detects the perfect ion carrier in application at complicated substrate.In addition, molecularly imprinted polymer not only can solution mutually in realize the selective separation enrichment of determinand, but also the high-selectivity adsorption of gas molecule in gas phase can be realized as adsorbent.Given this, first the present invention synthesizes electric neutrality gas molecule imprinted polymer, and be that ionophore is scattered in polymer film ion selective electrode sensitive membrane, then the electrode obtained is placed in gas phase gas sample and adsorbs electric neutrality gas molecule, finally the electrode after absorption is inserted containing having in the indication ion solution of similar chemical structure with gas to be measured, instruction gas molecule and film be middle imprinted polymer Selective recognition effect mutually, thus realizes measuring electric neutrality gas molecule.
The invention has the advantages that:
1. the potentiometric sensor of detection electric neutrality gas molecule of the present invention, efficiently solve the difficult problem that traditional electrode potential method is difficult to detect electric neutrality gas molecule, widen the application of ion-selective electrode, will effectively promote the development of chemical sensor in environmental monitoring field.
2. the present invention achieves polymer film ion selective electrode Direct Recognition gas molecule in the gas phase first, for ion-selective electrode technology analytical applications in the gas phase provides certain theoretical reference.
3. the present invention adopts the molecularly imprinted polymer of high selectivity as the Selective recognition carrier of electric neutrality organic gas molecule to be measured, select the organic ion with electric neutrality gas molecule with similar structure to conduct electric potential signal as indication ion, and then obtain the Copper diethlydithiocarbamate for detecting electric neutrality gas molecule.The present invention adopts ion-selective electrode to detect electric neutrality gas molecule, avoid and use large-scale chromatography instrument, testing cost is reduced greatly, and make the quantitative field monitoring of gas pollutant become possibility, thus the present invention plays huge effect by fields such as atmospheric surveillance, environmental analysis, pollutant catabolic gene.
Accompanying drawing explanation
The schematic diagram of the pick-up unit of the detection of the Copper diethlydithiocarbamate based on the ion-selective electrode electric neutrality gas that Fig. 1 provides for the embodiment of the present invention.Wherein, 1. gas generator, 2. carrier gas, 3. flowmeter, 4. liquid memory, 5. gas collector, 6. detection cell, 7. ion-selective electrode, 8. contrast electrode, 9. polymer sensitive membrane, 10.PXSJ-216L ionometer.
The contrast electric potential signal response curve of the electrode pair indication ion without toluene gas molecular adsorption that Fig. 2 provides for the embodiment of the present invention and the electrode normal potential response signal after the enrichment of variable concentrations toluene gas molecule.
The standard working curve of the determination of electrode variable concentrations toluene gas molecule that Fig. 3 provides for the embodiment of the present invention.
Embodiment
Embodiment 1
To detect electric neutrality gas molecule toluene gas.Concrete detecting step is as follows:
A. the preparation of toluene molecule imprinted polymer:
Getting 4mmol methacrylic acid, 10mmol divinylbenzene and 30mg azoisobutyronitrile is dissolved in 30mL pore-foaming agent toluene, and sonic oscillation 5min, passes into nitrogen deoxygenation 15min.Reaction vessel is sealed under nitrogen atmosphere, after be transferred in oil bath, at 60 DEG C, react 12h, obtain white solid particle.Obtained white solid particulate polymers in 70 DEG C of vacuum drying, with the abundant wash-out of methanol-acetic acid (V/V=9/1) solution to remove template molecule.Adopt methyl alcohol cyclic washing white solid particulate polymers removing remaining acetic acid, at 70 DEG C, dry 24h obtains toluene MIP.
B. the preparation of electrode:
Accurately take 360mg 2.8wt% toluene molecule imprinted polymer, 31.9wt% polyvinyl chloride particles, the o-nitrobenzene octyl ether of 51.0wt%, 12.8wt% polyglycol and 1.5wt% tri-(dodecyl) ammonium chloride, add 3.5mL tetrahydrofuran, ultrasonic, stirring 2h makes it to be uniformly dispersed.Membrane component being poured into internal diameter is in the glass ring of 3.6cm, and 25 DEG C of volatilization 12h in thermostatic drier, after tetrahydrofuran volatilization completely, namely obtain molecularly imprinted polymer sensitive membrane, now the thickness of film is about 200 μm.Utilize card punch that the sensitive membrane obtained is cut into the circular slice that diameter is 6mm, sticked to polyvinyl chloride pipe top with tetrahydrofuran.Liquid and activated solution activation 24h is rushed in doing with 1/30M phosphate buffered solution (pH=8.0) before electrode uses.
C. electrode is inserted containing 2 × 10
-4in the measuring cell of mol/L as the phosphate buffered solution of the benzoate anion of indication ion, produce contrast electric potential signal;
Electrode is inserted enrichment 30 minutes (toluene gas concentration is respectively 10,50,75,100,125,150ppm) in the toluene gas of a series of variable concentrations, then again electrode is proceeded to containing 2 × 10
-4in the measuring cell of mol/L as the phosphate buffered solution of the benzoate anion of indication ion, produce normal potential signal (see Fig. 2); Described phosphate buffered solution concentration is 1/30mol/L, and pH value is 8.0;
D. with contrast and normal potential rate of change, standard working curve (as Fig. 3) is obtained to toluene gas plotted against concentration;
E. electrode is inserted and to fill in the gas collector of gaseous sample to be measured enrichment 30 minutes, then again electrode is proceeded to containing 2 × 10
-4in the measuring cell of mol/L as the phosphate buffered solution of the benzoate anion of indication ion, produce sample electric potential signal; By reference standard working curve, obtain the concentration of toluene gas to be measured.
Electrode performance: electrode of the present invention can in the concentration range of 10-125ppm, the initial potential rate of change of electrode and the concentration of toluene gas linear, detection limit is about 3.3ppm (3 σ).Herein, the initial potential rate of change of electrode is defined as: current potential initial change is in the scope being less than 5mV, and current potential is to the single order matching of time.
Pick-up unit: electric neutrality gas-detecting device (see Fig. 1) comprises gas generator 1, gas collector 5, detection cell 6, ion-selective electrode 7, contrast electrode 8 and PXSJ-216L ionometer 10; Gas generator 1 comprises carrier gas device 2 and liquid memory 4, wherein be connected by pipeline A between carrier gas device 2 with liquid memory 4, be connected by pipeline B between liquid memory 4 with gas collector 5, a pipeline C in parallel on the pipeline A between carrier gas device 2 with the liquid memory 4 and pipeline B between liquid memory 4 with gas collector 5; Ion-selective electrode 7 is connected with PXSJ-216L ionometer 10 respectively by wire with contrast electrode 8; Ion-selective electrode 7 is inserted in detection cell 6 after first inserting gas collector 5 adsorbed gas again; Polymer sensitive membrane 9 is provided with bottom ion-selective electrode 7.Flowmeter 3 is respectively equipped with on pipeline A between described carrier gas device 2 and liquid memory 4 and on described pipeline C.Under pipeline A between described carrier gas device 2 and liquid memory 4 is inserted into the liquid level of liquid memory 4; Pipeline B between liquid memory 4 and gas collector 5 is inserted on the liquid level of liquid memory 4.
Ion-selective electrode 7 internal-filling liquid is 1/30M phosphate buffered solution.Contrast electrode 8 connects saturated calomel electrode for biliquid.
Embodiment 2
Electric neutrality disulfonic gas gas concentration in air is detected for the present invention.
Get air sample, measure potential change rate signal according to step c, d and e in embodiment 1, reference standard working curve, can obtain electric neutrality disulfonic gas gas concentration in air according to sample signal in air and standard working curve comparison.
Embodiment 3
Electric neutrality disulfonic gas gas concentration in industrial gaseous waste is detected for the present invention.
Get industrial gaseous waste sample, measure potential change rate signal according to step c, d and e in embodiment 1, reference standard working curve, can obtain electric neutrality disulfonic gas gas concentration in air according to sample signal in air and standard working curve comparison.
Embodiment 4
Electric neutrality gas formaldehyde gas concentration in air is detected for the present invention.
A. the preparation of formaldehyde molecule imprinted polymer:
Except pore-foaming agent is replaced by formalin, all the other implementation steps are carried out with reference to embodiment 1 step a;
B. the preparation of electrode:
Except indication ion is replaced by formic acid, all the other implementation steps are carried out with reference to embodiment 1 step b;
In air, electric neutrality gas formaldehyde gas concentration detects: according to embodiment 1 step c, d and e, reference standard working curve, can obtain formaldehyde gas concentration in air according to sample signal in air and standard working curve comparison.
Embodiment 5
Electric neutrality gas formaldehyde gas concentration in air is detected for the present invention.
A. the preparation of formaldehyde molecule imprinted polymer:
Except pore-foaming agent is replaced by formalin, all the other implementation steps are carried out with reference to embodiment 1 step a;
B. the preparation of electrode:
Except indication ion is replaced by formic acid, all the other implementation steps are carried out with reference to embodiment 1 step b;
In air, electric neutrality gas formaldehyde gas concentration detects: according to embodiment 1 step c, d and e, reference standard working curve, can obtain formaldehyde gas concentration in air according to sample signal in air and standard working curve comparison.
Embodiment 6
Electric neutrality gas dimethylbenzene gas concentration in air is detected for the present invention.
A. the preparation of dimethylbenzene molecularly imprinted polymer:
Except pore-foaming agent is replaced by xylene solution, all the other implementation steps are carried out with reference to embodiment 1 step a;
B. the preparation of electrode:
Except indication ion is replaced by p-methylbenzoic acid, all the other implementation steps are carried out with reference to embodiment 1 step b;
In air, electric neutrality gas dimethylbenzene gas concentration detects: according to embodiment 1 step b, c and d, reference standard working curve, can obtain dimethylbenzene gas concentration in air according to sample signal in air and standard working curve comparison.
Claims (6)
1. the method for the detection of the Copper diethlydithiocarbamate based on an ion-selective electrode electric neutrality gas, it is characterized in that: the identification material using molecularly imprinted polymer as selectivity electric neutrality gas molecule, identify that dispersion of materials is in the sensitive membrane of polymer film ion selective electrode, polymer film ion selective electrode is in the gas phase after adsorption gas molecule, adopt and there is the organic ion of similar chemical structure as indication ion with electric neutrality gas molecule, instruction polymer film is middle Selective recognition process between imprinted polymer and electric neutrality gas molecule to be measured mutually, thus the potentiometric detection realized electric neutrality gas molecule.
2. detect the method for electric neutrality gas by the Copper diethlydithiocarbamate based on ion-selective electrode according to claim 1, it is characterized in that:
The molecularly imprinted polymer a. will with specific recognition capability is used as the molecular recognition material of polymer film ion selective electrode, makes it form ion-selective electrode based on molecularly imprinted polymer sensitive membrane;
B. the ion-selective electrode that step a obtains being inserted containing having in the indication ion measuring cell of analog structure with gas molecule to be measured, producing contrast potential change signal;
C. the gas collector that the ion-selective electrode that step a obtains is placed in containing electric neutrality gas molecule is carried out enrichment, then the ion-selective electrode that step a obtains is proceeded in the measuring cell containing indication ion solution again, produce normal potential variable signal;
D. change with contrast and normal potential and electric neutrality gas concentration is drawn to obtain standard working curve;
E. the gaseous sample that the ion-selective electrode that step a obtains is placed in containing gas to be measured is carried out enrichment, then the ion-selective electrode that step a obtains is proceeded in the measuring cell containing indication ion again, produce sample potential change signal; Namely the concentration of electric neutrality gas to be measured is obtained by reference standard working curve.
3. the method for electric neutrality gas is detected by the Copper diethlydithiocarbamate based on ion-selective electrode described in claim 1 or 2, it is characterized in that: described electric neutrality gas molecule is the gaseous molecular of benzene,toluene,xylene, chlorobenzene, dichloro-benzenes, dinitrotoluene (DNT), acetonitrile, chloroform, normal heptane, cyclohexane, trichloroethanes, tetrahydrofuran, ethyl acetate, DMF, triclene, formaldehyde, acetone, methyl alcohol, ethanol, isopropyl alcohol, normal butyl alcohol or isobutyl alcohol.
4. the special purpose device of the method for the detection of the Copper diethlydithiocarbamate based on an ion-selective electrode electric neutrality gas according to claim 1, it is characterized in that: special purpose device comprises gas generator (1), gas collector (5), detection cell (6), ion-selective electrode (7), contrast electrode (8) and PXSJ-216L ionometer (10); Gas generator (1) comprises carrier gas device (2) and liquid memory (4), wherein be connected by pipeline A between carrier gas device (2) with liquid memory (4), be connected by pipeline B between liquid memory (4) with gas collector (5), a pipeline C in parallel on the pipeline A between carrier gas device (2) with liquid memory (4) and the pipeline B between liquid memory (4) with gas collector (5); Ion-selective electrode (7) is connected with PXSJ-216L ionometer (10) respectively by wire with contrast electrode (8); Ion-selective electrode (7) is inserted after first inserting gas collector (5) adsorbed gas in detection cell (6) again; Ion-selective electrode (7) bottom is provided with polymer sensitive membrane (9).
5. detect the special purpose device of the method for electric neutrality gas by the Copper diethlydithiocarbamate based on ion-selective electrode according to claim 4, it is characterized in that: on the pipeline A between described carrier gas device (2) and liquid memory (4) and on described pipeline C, be respectively equipped with flowmeter (3).
6. detect the special purpose device of the method for electric neutrality gas by the Copper diethlydithiocarbamate based on ion-selective electrode according to claim 4, it is characterized in that: under the pipeline A between described carrier gas device (2) and liquid memory (4) is inserted into the liquid level of liquid memory (4); Pipeline B between liquid memory (4) and gas collector (5) is inserted on the liquid level of liquid memory (4).
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