CN108802131A - Acetic acid electrode and preparation method thereof - Google Patents
Acetic acid electrode and preparation method thereof Download PDFInfo
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- CN108802131A CN108802131A CN201810401416.2A CN201810401416A CN108802131A CN 108802131 A CN108802131 A CN 108802131A CN 201810401416 A CN201810401416 A CN 201810401416A CN 108802131 A CN108802131 A CN 108802131A
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- acetic acid
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title claims abstract description 367
- 238000002360 preparation method Methods 0.000 title description 4
- 239000011521 glass Substances 0.000 claims abstract description 66
- 238000011049 filling Methods 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 28
- 239000007853 buffer solution Substances 0.000 claims abstract description 25
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 20
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- 238000004519 manufacturing process Methods 0.000 claims description 15
- -1 polytetrafluoroethylene Polymers 0.000 claims description 14
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 10
- 235000011187 glycerol Nutrition 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000001139 pH measurement Methods 0.000 claims description 10
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 10
- 239000011780 sodium chloride Substances 0.000 claims description 8
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 239000004743 Polypropylene Substances 0.000 claims description 4
- 229920001155 polypropylene Polymers 0.000 claims description 4
- 239000007987 MES buffer Substances 0.000 claims description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- BUCIWTBCUUHRHZ-UHFFFAOYSA-K potassium;disodium;dihydrogen phosphate;hydrogen phosphate Chemical compound [Na+].[Na+].[K+].OP(O)([O-])=O.OP([O-])([O-])=O BUCIWTBCUUHRHZ-UHFFFAOYSA-K 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 230000002093 peripheral effect Effects 0.000 claims description 2
- 239000008057 potassium phosphate buffer Substances 0.000 claims description 2
- 238000010025 steaming Methods 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 239000002033 PVDF binder Substances 0.000 claims 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims 1
- 239000001913 cellulose Substances 0.000 claims 1
- 229920002678 cellulose Polymers 0.000 claims 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 13
- 230000035945 sensitivity Effects 0.000 abstract description 4
- 239000000523 sample Substances 0.000 description 11
- 238000012360 testing method Methods 0.000 description 10
- RAHZWNYVWXNFOC-UHFFFAOYSA-N sulfur dioxide Inorganic materials O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 229940058401 polytetrafluoroethylene Drugs 0.000 description 5
- 239000004800 polyvinyl chloride Substances 0.000 description 5
- 241000894006 Bacteria Species 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000005515 coenzyme Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000004128 high performance liquid chromatography Methods 0.000 description 4
- 230000002209 hydrophobic effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000000855 fermentation Methods 0.000 description 3
- 230000004151 fermentation Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XPFJYKARVSSRHE-UHFFFAOYSA-K trisodium;2-hydroxypropane-1,2,3-tricarboxylate;2-hydroxypropane-1,2,3-tricarboxylic acid Chemical compound [Na+].[Na+].[Na+].OC(=O)CC(O)(C(O)=O)CC(O)=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O XPFJYKARVSSRHE-UHFFFAOYSA-K 0.000 description 3
- 102000005369 Aldehyde Dehydrogenase Human genes 0.000 description 2
- 108020002663 Aldehyde Dehydrogenase Proteins 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 2
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 2
- 235000003140 Panax quinquefolius Nutrition 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229920003020 cross-linked polyethylene Polymers 0.000 description 2
- 239000004703 cross-linked polyethylene Substances 0.000 description 2
- 238000010494 dissociation reaction Methods 0.000 description 2
- 230000005593 dissociations Effects 0.000 description 2
- 229920002313 fluoropolymer Polymers 0.000 description 2
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 description 2
- 235000008434 ginseng Nutrition 0.000 description 2
- 230000002452 interceptive effect Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 230000000813 microbial effect Effects 0.000 description 2
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- KOPBYBDAPCDYFK-UHFFFAOYSA-N Cs2O Inorganic materials [O-2].[Cs+].[Cs+] KOPBYBDAPCDYFK-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- AKUNKIJLSDQFLS-UHFFFAOYSA-M dicesium;hydroxide Chemical compound [OH-].[Cs+].[Cs+] AKUNKIJLSDQFLS-UHFFFAOYSA-M 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- CCIVGXIOQKPBKL-UHFFFAOYSA-M ethanesulfonate Chemical compound CCS([O-])(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-M 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 1
- ZDGGJQMSELMHLK-UHFFFAOYSA-N m-Trifluoromethylhippuric acid Chemical compound OC(=O)CNC(=O)C1=CC=CC(C(F)(F)F)=C1 ZDGGJQMSELMHLK-UHFFFAOYSA-N 0.000 description 1
- 238000012269 metabolic engineering Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000000825 ultraviolet detection Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
Abstract
The present invention provides a kind of acetic acid electrode.The acetic acid electrode includes insulating cover, and extends outward to form insulated cavity, glass tube chamber and internal reference electrode from one surface of the insulating cover, and the insulated cavity, glass tube chamber are coaxial with internal reference electrode；It is folded in the glass tube cavity outer wall circumferential direction and is equipped with outer reference electrode；The internal reference electrode and the glass segment dislocation first chamber, the first chamber is interior to be filled with buffer solution；The insulated cavity and the glass segment dislocation second chamber, the second chamber is interior to be filled with acetic acid electrode internal-filling liquid；PH sensing glass films are formed on the end of the glass tube chamber far from the insulating cover；It is socketed with acetic acid air-sensitive film on end of the insulated cavity far from the insulating cover；The conducting wire for connecting the internal reference electrode extends to outside another surface of the insulating cover.The acetic acid electrode of the invention has the characteristics that detection sensitivity is high, accuracy is good and may be reused, is at low cost, is easy to detect.
Description
Technical field
The invention belongs to acetic acid detection technique fields, and in particular to a kind of acetic acid electrode and preparation method thereof.
Background technology
Acetic acid is a kind of important flavouring and industrial chemicals, in traditional acetic acid production process, substantially with fermentation
Mode obtains.In addition, acetic acid is also a kind of common tunning in microbial cultivation process.In the incubation of Escherichia coli
In, often there is the organic acid by-product generation largely based on acetic acid, it is inhibited to the growth of Escherichia coli.In work
In the fermentation of journey bacterium, the key constraints of acetic acid accumulated not in still engineering bacteria High Density Cultivation, and influence external source base
One obstacle of the expression of cause.Acetic acid content is that engineering bacterium fermentation needs control important parameter in the process.And in engineering
In the metabolic engineering research of bacterium, acetic acid analysis is even more an indispensable research contents, it is therefore necessary to be examined to acetic acid
It surveys.
Acetic acid detection method common at present has high performance liquid chromatography, enzymic colorimetric.Wherein, high performance liquid chromatography is
Using the mixed solution of methanol and the PBS (pH=2.0) of 0.01mol/L as mobile phase, flow velocity 0.5mL/min, ultraviolet detection wave
A length of 210nm, column temperature are 35 DEG C.With each 10 μ L of sample introduction of the acetic acid titer of 7 various concentrations, peak area is measured, draws peak face
Working curve of the product to acetic acid concentration.Into the peak area after sample sample acetic acid concentration is relatively obtained with working curve.
Enzymic colorimetric is to be digested acetic acid in the presence of reducibility coenzyme (having absorption peak under 340nm) using aldehyde dehydrogenase
For acetaldehyde, and reproducibility auxiliary enzymes are oxidized to coenzyme (without absorption peak under 340nm).By measuring reducibility coenzyme in 340nm
The decrease speed of absorbance measures the concentration of acetic acid at wavelength.
In above two method, high performance liquid chromatography has degree of detection height, stability good a little, and still, instrument is set
It is standby expensive, and personage's operation, the analysis of profession are needed, test process takes longer.Enzymic colorimetric has detection speed fast, special
It is anisotropic high, not by characteristics such as allogenic material interference, still, the reducibility coenzyme and aldehyde dehydrogenase in kit are expensive, inspection
It is excessively high to survey cost, it is often more important that easily by oxygenolysis in storing process, influence to detect stability and accuracy.It is therefore desirable to
Seek a kind of new acetic acid detection method.
Invention content
For testing cost present in current high performance liquid chromatography acetic acid detection process the high, testing time at and enzyme
The problems such as storage stability existing for colorimetric method is poor, detection stability and accuracy be not high, the present invention provides a kind of acetic acid electrode
And preparation method thereof.
For achieving the above object, technical scheme is as follows：
A kind of acetic acid electrode, including insulating cover, and extend outward to form insulated cavity, glass from one surface of the insulating cover
Tube chamber and internal reference electrode, the insulated cavity, glass tube chamber are coaxial with internal reference electrode；The glass tube cavity outer wall circumferential direction
It is upper folded equipped with outer reference electrode；The internal reference electrode and the glass segment dislocation first chamber are filled out in the first chamber
Filled with buffer solution；The insulated cavity and the glass segment dislocation second chamber, the second chamber is interior to be filled with acetic acid electrode
Internal-filling liquid；PH sensing glass films are formed on the end of the glass tube chamber far from the insulating cover；It is separate in the insulated cavity
Acetic acid air-sensitive film is socketed on the end of the insulating cover；Connecting the conducting wire of the internal reference electrode, to extend to the insulating cover another
Outside one surface.
Correspondingly, a kind of production method of acetic acid electrode, at least includes the following steps：
Step S01. is attached with outer ginseng to one end open in other end formation pH sensing glass film and outer wall peripheral direction
Glass tube chamber than electrode is filled with buffer solution, and the buffer solution is made to riddle the glass tube intracavitary；
The step S02. insulating covers for being plugged with internal reference electrode cover the open end of the glass tube chamber, and make in described
Reference electrode is placed in the glass tube intracavitary；
Step S03., which is socketed with to the one end open other end in the insulated cavity of acetic acid air-sensitive film, is full of acetic acid internal-filling liquid；
Step S04. covers the open end of the insulated cavity with the obtained insulating covers of step S02, and the glass tube chamber is made to set
In in the insulated cavity, acetic acid electrode is obtained.
The present invention technique effect be：Compared with the existing technology, acetic acid electrode provided by the invention to acetic acid to have choosing
The film layer that the acetic acid air-sensitive film of permeability is detected as acetic acid is selected, and is filled with acetic acid electrode internal-filling liquid in acetic acid electrode, into
Enter the acetic acid of the acetic acid electrode interior release hydrogen ions in acetic acid electrode internal-filling liquid, changes the pH of internal-filling liquid, incuded by electrode
And detect, to realize the quick detection to acetic acid.This acetic acid electrode is high with detection sensitivity, accuracy is good and can repeat
Use, feature at low cost, easy to detect.
The above-mentioned production method of the present invention, manufacture craft simple possible, and the acetic acid electrode obtained have high sensitivity, steady
It is qualitative good, the characteristics of long lifespan.
Description of the drawings
It to describe the technical solutions in the embodiments of the present invention more clearly, below will be to needed in the embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for ability
For the those of ordinary skill of domain, without creative efforts, it can also be obtained according to these attached drawings other attached
Figure.
Fig. 1 is that acetic acid electrode solid is intended in the embodiment of the present invention；
Fig. 2 is acetic acid electrode schematic elevation view in the embodiment of the present invention；
Fig. 3 is schematic cross-sectional view of Fig. 2 acetic acid electrode along cavity central axes direction；
Wherein, 1- insulating covers；2- insulated cavities；3- glass tube chambers；4- internal reference electrodes；The outer reference electrodes of 5-；6- buffer solutions；
7- acetic acid electrode internal-filling liquids；8-pH sensing glass films；9- acetic acid air-sensitive films；10- fasteners；11- conducting wires.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, not
For limiting the present invention.
It please refers to Fig.1, the schematic diagram of Fig. 2, Fig. 3, the present invention provides a kind of acetic acid electrode, including insulating cover 1, and alienates oneself
1 one surface of edge lid extends outward to form insulated cavity 2, glass tube chamber 3 and internal reference electrode 4.
Wherein, insulated cavity 2, glass tube chamber 3 are coaxial with internal reference electrode 4；And it folds and sets in 3 outer wall circumferential direction of glass tube chamber
There is outer reference electrode 5；Internal reference electrode 4 forms first chamber with glass tube chamber 3, and buffer solution 6 is filled in the first chamber；
Insulated cavity 2 and glass tube chamber 3 form second chamber, and acetic acid electrode internal-filling liquid 7 is filled in the second chamber；In glass tube chamber
PH sensing glass film 8 is formed on 3 ends far from insulating cover 1；It is socketed with acetic acid on end of the insulated cavity 2 far from insulating cover 1
Air-sensitive film 9；The conducting wire 11 of connection internal reference electrode 4 extends to outside 1 another surface of insulating cover.
Preferably, the material of insulating cover 1 is polyethylene, crosslinked polyethylene, polyvinyl chloride, polypropylene, polyolefin, fluoroplastics
Deng.
Insulated cavity 2 be both ends open cavity, at one end on be socketed with acetic acid air-sensitive film 9.
Preferably, the material of insulated cavity 2 is polyethylene, crosslinked polyethylene, polyvinyl chloride, polypropylene, polyolefin, fluoroplastics
Deng.Insulated cavity 2 primarily serves the purpose for preventing external interference acetic acid from measuring.
Preferably, acetic acid air-sensitive film 9 is polytetrafluoroethylene film, cellulose acetate film, polychloroethylene film, Kynoar
Any one of film, polypropylene screen, pellosil, these types of film have that hydrophobic, air-permeability is good, insulating properties is high, acid-fast alkali-proof and tension
The big characteristic of intensity.Since it is with good hydrophobic, air-permeability, only allow uncharged molecule, such as acetic acid, oxygen, nitrogen
Pass through, and the molecule such as H with charge+Cannot then it pass through, so as to significantly improve the accuracy of test.
It is further preferred that the membrane aperture of acetic acid air-sensitive film 9 is 0.01~0.8 μm, film thickness is 10~100 μm.
When acetic acid air-sensitive film 9 is polytetrafluoroethylene film, aperture is 0.1 μm, thickness is 25 μm, the aperture size and thickness
Degree can make molecular acid quickly establish diffusion balance in film both sides, to accelerate detection speed.Further, since polytetrafluoro
Ethylene has good acid-fast alkali-proof performance and stronger tensile resistance, and electrode film can be made to use the longevity with overlength
Life, may be implemented repeated measurement, to reduce testing cost.
In order to enable acetic acid air-sensitive film 9 is preferably attached at 2 outer wall of insulated cavity, the filling liquid in insulated cavity 2 is avoided to leak outside
Or other extraneous substances are entered in insulated cavity 2 by gap by cause measurement error, using fastener 10 by acetic acid air-sensitive film 9
It is anchored in the outside wall surface of insulated cavity 2.
Preferably, fastener 10 is O-ring seal.
Glass tube chamber 3 is the cavity of both ends open, one end and the fusion of pH sensing glass film 8 is formed one so that glass
It closes one end of glass tube chamber 3.
Preferably, the material composition of pH sensing glass film is, 25%Li according to mass percent2O:7%Cs2O:2%
La2O3:66%SiO2。
Preferably, internal reference electrode 4 and/or outer reference electrode 5 are Ag/AgCl reference electrodes, with Ag/AgCl reference electrodes
As internal reference electrode and/or outer reference electrode, there is potential to stablize, reproducibility is fine and is still shown in temperature change
Good stability.Certainly, internal reference electrode 4 and/or outer reference electrode 5 are not limited to Ag/AgCl reference electrodes, can also adopt
With Au, Pt, graphite etc..
Buffer solution 6 is citric acid-sodium citrate buffer solution, disodium hydrogen phosphate-potassium phosphate buffer, MES (2- (N-
Any one of morpholine) ethanesulfonic acid) buffer solution.The pH value of buffer solution 6 is 5.2~5.6.It, both can be under the conditions of this pH
Make acetic acid there are enough vapour pressures to penetrate acetic acid air-sensitive film 9 and enters acetic acid electrode internal-filling liquid 7.It can inhibit deposit in sample again
Other interfering substances such as hydrofluoric acid, formic acid, carbon dioxide, the sour gas such as sulfur dioxide through acetic acid air-sensitive film 9 to survey
Test result generates interference, to substantially increase the anti-interference ability of acetic acid electrode.
Acetic acid electrode internal-filling liquid 7 is CH3A concentration of 90~105mmol/L of COONa, NaCl concentration are 135~150mmol/
L, the double steaming solution that glycerine mass content is 6%.Wherein, the mass content of glycerine can be extended to 0.5~23%, third
Triol can prevent bubble from entering electrode under the mass content, to improve the stability of electrode.
The operation principle of the present invention is that：
It uses buffer solution 6 to handle sample first, the acetate in sample is made to be converted into molecular acid by a certain percentage, and second
Acid molecule has the ability that can penetrate acetic acid air-sensitive film 9.After acetic acid penetrates acetic acid air-sensitive film 9, into acetic acid electrode internal-filling liquid 7,
Until reaching balance, shown in balanced reaction such as following formula (1)：
In formula (1), H+Release change H in acetic acid electrode internal-filling liquid 7+Concentration to make the pH value of solution have occurred
Variation, the side of pH sensing glass film 8 is to very sensitive, the other side H of pH sensing glass 8 of this change+Concentration gradient draw
The voltage difference across pH sensing glass film 7 is played, this variation is measured when voltage passes through pH sensing glass films 7 by potentiometer.
PH value and the relationship of the acetic acid concentration in sample are indicated by following formula (a)：
In formula：KαFor CH3The dissociation constant of COOH.
Due to CH3The dissociation constant of COOH is a definite value, it may be determined that it is K, and the c in acetic acid electrode internal-filling liquid 7
(CH3COO-) sufficiently large, it is also assumed that being a constant.Therefore formula (a) can be reduced to formula (b)：
PH=K-logc (CH3COOH)……(b)。
Then the CH in sample3COOH concentration (b) can be calculated according to formula above.
Acetic acid electrode provided by the present invention, on the one hand, the sample pretreatment buffer solution for using pH=5.4 or so,
Under the conditions of this pH, it can not only make acetic acid there are enough vapour pressures to penetrate acetic acid air-sensitive film and enter acetic acid electrode internal-filling liquid, but also can
To inhibit other interfering substances that may be present in sample to generate interference to test result through acetic acid air-sensitive film, to carry significantly
The high anti-interference ability of acetic acid electrode.
Second aspect, the present invention is good using hydrophobic, air-permeability, and insulating properties is high, acid and alkali-resistance and the big acetic acid gas of tensile strength
Quick film.Due to its good hydrophobic, air-permeability, uncharged molecule is only allowed to pass through, and the molecule such as H with charge+
Cannot then it pass through, to significantly enhance test accuracy.
6% or so glycerine is added in acetic acid electrode internal-filling liquid, can prevent bubble from entering electrode for the third aspect,
To improve the stability of electrode.
Correspondingly, under the premise of above-mentioned acetic acid electrode, production method that the present invention furthermore provides acetic acid electrode.
In one embodiment, the production method of the acetic acid electrode at least includes the following steps：
Step S01. is attached with outer ginseng to one end open in other end formation pH sensing glass film 8 and outer wall circumferential direction
Glass tube chamber 3 than electrode 5 is filled with buffer solution 6, and the buffer solution 6 is made to riddle in the glass tube chamber 3；
Step S02. covers the open end of 3 chamber of the glass tube with the insulating cover 1 for being plugged with internal reference electrode 4, and makes institute
Internal reference electrode 4 is stated to be placed in the glass tube chamber 3；
Step S03., which is socketed with to the one end open other end in the insulated cavity 2 of acetic acid air-sensitive film 9, is full of acetic acid internal-filling liquid 7；
The insulating cover 1 that step S04. is obtained with step S02 covers the open end of the insulated cavity 2, makes the glass tube chamber 3
It is placed in the insulated cavity 2, obtains acetic acid electrode.
The production method of the present invention is further explained in detail below.
In step S01, the buffer solution 6 is citric acid-sodium citrate buffer solution, disodium hydrogen phosphate-potassium dihydrogen phosphate is slow
Any one of fliud flushing, MES buffer solutions.And the pH value that should control the buffer solution 6 is 5.2~5.6.
In step S03, the production method of the acetic acid electrode internal-filling liquid 7 is：By CH3COONa, NaCl and glycerine dissolving
In distilled water, CH is obtained3A concentration of 90~105mmol/L of COONa, NaCl concentration are 135~150mmol/L, glycerine matter
Measure the acetic acid electrode internal-filling liquid that content is 0.5~23%.
Preferably, CH in the acetic acid electrode internal-filling liquid3A concentration of 100mmol/L of COONa, NaCl concentration 140mmol/
L, glycerine mass content is 6%.
The capping procedure of above-mentioned steps S02 and step S04, specifically may be used epoxy resin by insulating cover 1 respectively with glass
Glass official jargon 3 and insulated cavity 2 are sealed.
The production method of the acetic acid electrode of the above-mentioned offer of the present invention, manufacture craft simple possible, and the acetic acid electricity obtained
It is great to have the characteristics of high sensitivity, stability are good, long lifespan.
More effectively to illustrate technical scheme of the present invention, the technology of the present invention is illustrated below by multiple specific embodiments
Scheme.
Embodiment 1
A kind of acetic acid electrode, structure is as shown in Figures 1 to 3, including PVC insulating covers 1 and 1 one surface of self-insulating lid to
Extend to form PVC insulated cavities 2, glass tube chamber 3 and Ag/AgCl internal reference electrodes 4 outside.
Wherein, insulated cavity 2, glass tube chamber 3 are coaxial with Ag/AgCl internal reference electrodes 4；And 3 outer wall circumferential direction side of glass tube chamber
It is folded upwards to be equipped with reference electrode 5 outside Ag/AgCl；Ag/AgCl internal reference electrodes 4 and glass tube chamber 3 form first chamber, and described the
Buffer solution 6 is filled in one chamber, which is the citric acid-sodium citrate buffer solution of pH=5.4；Insulated cavity 2 and glass
Tube chamber 3 forms second chamber, and acetic acid electrode internal-filling liquid 7, the ingredient of the acetic acid electrode filling liquid 7 are filled in the second chamber
For CH3The distilled water that a concentration of 100mmol/L of COONa, NaCl concentration 140mmol/L, glycerine mass content are 6% is molten
Liquid；PH sensing glass film 8 is formed on end of the glass tube chamber 3 far from insulating cover 1；In end of the insulated cavity 2 far from insulating cover 1
On be socketed with polytetrafluoroethylene film 9, polytetrafluoroethylene film 9 is fastened using O-ring seal；Connect reference electricity in Ag/AgCl
The conducting wire 11 of pole 4 extends to outside 1 another surface of PVC insulating covers.
To verify the performance of 1 acetic acid electrode of embodiment, it is mounted on western Germania science and technology acetic acid analyzer, compound concentration
The respectively acetic acid sample solution of 2mM, 6mM, 10mM, 21mM, 30mM, 45mM is labeled as P1, P2, P3, P4, P5, P6；Then
It is tested, test result is as shown in table 1.
Table 1
| Sample | P1 | P2 | P3 | P4 | P5 | P6 |
| Theoretical concentration (mM) | 2.00 | 6.00 | 10.00 | 21.00 | 30.00 | 45.00 |
| Measured concentration (mM) | 1.98 | 6.02 | 9.97 | 21.11 | 29.91 | 46.03 |
As can be seen from Table 1, acetic acid electrode detection accuracy of the present invention is high, and detection range is wide, is fully able to meet acetic acid
To the test request of acetic acid concentration in production and microbial cultivation process.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc. made by within refreshing and principle should all include within protection scope of the present invention.
Claims (10)
1. a kind of acetic acid electrode, which is characterized in that extended outward to form absolutely including insulating cover, and from one surface of the insulating cover
Edge chamber, glass tube chamber and internal reference electrode, the insulated cavity, glass tube chamber are coaxial with internal reference electrode；Outside the glass tube chamber
It is folded in wall circumferential direction and is equipped with outer reference electrode；The internal reference electrode and the glass segment dislocation first chamber, described the
Buffer solution is filled in one chamber；The insulated cavity and the glass segment dislocation second chamber, the interior filling of the second chamber
There is acetic acid electrode internal-filling liquid；PH sensing glass films are formed on the end of the glass tube chamber far from the insulating cover；Described
Insulated cavity is socketed with acetic acid air-sensitive film on the end far from the insulating cover；The conducting wire for connecting the internal reference electrode extends to institute
It states outside another surface of insulating cover.
2. acetic acid electrode as described in claim 1, which is characterized in that the acetic acid air-sensitive film is polytetrafluoroethylene film, acetic acid
Any one of cellulose membrane, polychloroethylene film, polyvinylidene fluoride film, polypropylene screen, pellosil.
3. acetic acid electrode as claimed in claim 1 or 2, which is characterized in that the membrane aperture of the acetic acid air-sensitive film be 0.01~
0.8 μm, film thickness is 10~100 μm.
4. acetic acid electrode as described in claim 1, which is characterized in that the internal reference electrode is Ag/AgCl reference electrodes；
And/or the outer reference electrode is Ag/AgCl reference electrodes.
5. acetic acid electrode as described in claim 1, which is characterized in that the acetic acid electrode internal-filling liquid is CH3COONa is a concentration of
The double steaming solution that 90~105mmol/L, NaCl concentration are 135~150mmol/L, glycerine mass content is 6%.
6. acetic acid electrode as described in claim 1, which is characterized in that the acetic acid air-sensitive film is anchored on described by fastener
The end of insulated cavity.
7. a kind of production method such as claim 1~6 any one of them acetic acid electrode, which is characterized in that include at least with
Lower step：
Step S01. is attached with outer reference electricity to one end open in other end formation pH sensing glass film and outer wall peripheral direction
The glass tube chamber of pole is filled with buffer solution, and the buffer solution is made to riddle the glass tube intracavitary；
The step S02. insulating covers for being plugged with internal reference electrode cover the open end of the glass tube chamber, and make the interior reference
Electrode is placed in the glass tube intracavitary；
Step S03., which is socketed with to the one end open other end in the insulated cavity of acetic acid air-sensitive film, is full of acetic acid internal-filling liquid；
Step S04. covers the open end of the insulated cavity with the obtained insulating covers of step S02, and the glass tube chamber is made to be placed in institute
It states in insulated cavity, obtains acetic acid electrode.
8. the production method of acetic acid electrode as claimed in claim 7, which is characterized in that the buffer solution is citric acid-lemon
Any one of sour sodium buffer solution, disodium hydrogen phosphate-potassium phosphate buffer, MES buffer solutions.
9. the production method of acetic acid electrode as claimed in claim 7 or 8, which is characterized in that the pH value of the buffer solution is 5.2
~5.6.
10. the production method of acetic acid electrode as claimed in claim 7, which is characterized in that the system of the acetic acid electrode internal-filling liquid
It is as method：By CH3COONa, NaCl and glycerine are dissolved in distilled water, obtain CH3A concentration of 100mmol/L of COONa,
The acetic acid electrode internal-filling liquid that NaCl concentration is 140mmol/L, glycerine mass content is 6%.
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