CN110734583A - Induction film of calcium ion selective electrodes and preparation method thereof - Google Patents
Induction film of calcium ion selective electrodes and preparation method thereof Download PDFInfo
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- CN110734583A CN110734583A CN201910836645.1A CN201910836645A CN110734583A CN 110734583 A CN110734583 A CN 110734583A CN 201910836645 A CN201910836645 A CN 201910836645A CN 110734583 A CN110734583 A CN 110734583A
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- calcium ion
- selective electrodes
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- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 229910001424 calcium ion Inorganic materials 0.000 title claims abstract description 50
- 230000006698 induction Effects 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000012528 membrane Substances 0.000 claims abstract description 30
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 239000004014 plasticizer Substances 0.000 claims abstract description 12
- 239000013543 active substance Substances 0.000 claims abstract description 10
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 10
- 239000002861 polymer material Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 6
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 claims description 10
- FLKPEMZONWLCSK-UHFFFAOYSA-N diethyl phthalate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC FLKPEMZONWLCSK-UHFFFAOYSA-N 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000001506 calcium phosphate Substances 0.000 claims description 5
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 5
- 235000011010 calcium phosphates Nutrition 0.000 claims description 5
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Natural products CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 claims description 5
- 229960001826 dimethylphthalate Drugs 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 5
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 5
- 229920002301 cellulose acetate Polymers 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 3
- 239000013504 Triton X-100 Substances 0.000 claims description 3
- 229920004890 Triton X-100 Polymers 0.000 claims description 3
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000012258 stirred mixture Substances 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- CJAONIOAQZUHPN-KKLWWLSJSA-N ethyl 12-[[2-[(2r,3r)-3-[2-[(12-ethoxy-12-oxododecyl)-methylamino]-2-oxoethoxy]butan-2-yl]oxyacetyl]-methylamino]dodecanoate Chemical compound CCOC(=O)CCCCCCCCCCCN(C)C(=O)CO[C@H](C)[C@@H](C)OCC(=O)N(C)CCCCCCCCCCCC(=O)OCC CJAONIOAQZUHPN-KKLWWLSJSA-N 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- URAUKAJXWWFQSU-UHFFFAOYSA-N n,n-dicyclohexyl-2-[2-(dicyclohexylamino)-2-oxoethoxy]acetamide Chemical compound C1CCCCC1N(C1CCCCC1)C(=O)COCC(=O)N(C1CCCCC1)C1CCCCC1 URAUKAJXWWFQSU-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- 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
- G01N27/333—Ion-selective electrodes or membranes
- G01N27/3335—Ion-selective electrodes or membranes the membrane containing at least one organic component
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/10—Esters of organic acids
- C08J2301/12—Cellulose acetate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/325—Calcium, strontium or barium phosphate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Medicinal Chemistry (AREA)
- Materials Engineering (AREA)
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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
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Abstract
The invention provides an induction membrane of calcium ion selective electrodes and a preparation method thereof, wherein the induction membrane is formed by uniformly mixing a solute and a volatile solvent after the volatile solvent volatilizes, and the mass ratio of the components in the solute is 5-15% of a calcium ion active agent, 0.5-3% of a non-ionic surfactant, 30-50% of a polymer material and 40-60% of a plasticizer.
Description
Technical Field
The invention belongs to the technical field of sensors and ion detection, and particularly relates to an induction membrane of calcium ion selective electrodes and a preparation method thereof.
Background
The calcium ion selective electrode can measure the concentration of calcium ions in a solution, and the principle is that the calcium ion selective sensing membrane responds to the calcium ions, when the membrane is contacted with the solution, movable ions in a membrane phase selectively interact with the calcium ions in the solution, the mandatory and selective effects cause uneven charge distribution of two phase interfaces, double electric layers are generated, potential difference is formed, the potential is called interface potential, the solution concentration is different, the interface potential strength is different, the relationship between the potential and the concentration follows the Nernst equation, namely the potential is in direct proportion to the negative logarithm of the concentration, the calcium ions are divalent ions, and the theoretical slope is 29.58 mV/pCa.
The calcium ion selective induction membrane is used as the core part of the calcium ion selective electrode and plays a decisive role in various performances of the electrode. In the prior art, PVC is mostly adopted as a polymer matrix, and the problems of change of the detection lower limit of an induction membrane and short service life caused by plasticizer leakage can occur; in addition, ETH1001, ETH129 and the like which are often used as calcium ion neutral carriers are basically imported medicines, and the purchase period is long and the price is high.
Therefore, it is necessary to provide new sensing membranes of ion selective electrodes and methods for preparing the same to solve the above problems.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide induction films for calcium ion selective electrodes and a preparation method thereof, and the induction films are low in cost, high in measurement accuracy and good in stability.
The technical scheme includes that the induction membrane of calcium ion selective electrodes is formed by uniformly mixing a solute and a volatile solvent, and forming a membrane after the volatile solvent is volatilized, wherein the mass ratio of the components in the solute is 5% -15% of a calcium ion active agent, 0.5% -3% of a nonionic surfactant, 30% -50% of a polymer material and 40% -60% of a plasticizer.
, the calcium ion activator is basic calcium phosphate.
, the non-ionic surfactant is triton X-100.
Further to step , the polymer material is cellulose acetate.
Further , the plasticizer is at least of tributyl phosphate (TBP), dimethyl phthalate (DMP) and diethyl phthalate (DEP).
Further , the volatile solvent is at least of acetone and methyl acetate.
In order to achieve the above purposes, the invention adopts the technical scheme that the preparation method of the induction membrane of the calcium ion selective electrodes comprises the following steps:
5 to 15 percent of calcium ion active agent, 0.5 to 3 percent of nonionic surfactant, 30 to 50 percent of polymer material and 40 to 60 percent of plasticizer are used as solute and are mixed and stirred uniformly with a volatile solvent, the ratio of the solute to the solvent is 25 to 100mg/mL, the mixture is stirred hermetically at normal temperature for more than 4 hours, and the uniformly stirred mixture is stood and volatilized to form a film at normal temperature.
The preparation method of the calcium ion selective induction membrane has the advantages that the preparation method is simple in process, can be completed by using common laboratory equipment, is low in cost of used materials, and is environment-friendly; the prepared induction film has high flatness, good uniformity and good toughness; the calcium ion selective electrode prepared by the induction membrane has good selectivity, high measurement precision and good stability.
Drawings
FIG. 1 shows that the calcium ion concentration is 10-5～10-2mol·L-1Slope plots for examples 1-4, within the range;
FIG. 2 shows that the calcium ion concentration is 10-3mol·L-1Stability profiles in examples 1-4.
Detailed Description
In order to make the technical problems solved, technical solutions adopted and technical effects achieved by the present invention clearer, the following detailed description is given in steps with reference to the accompanying drawings, where it is obvious that the described embodiments are only some embodiments, but not all embodiments, of the present invention .
The invention provides an induction membrane of calcium ion selective electrodes, which is formed by uniformly mixing a solute and a volatile solvent, wherein the mass ratio of the solute to the volatile solvent is 5-15% of calcium ion active agent, 0.5-3% of nonionic surfactant, 30-50% of polymer material and 40-60% of plasticizer.
The calcium ion active agent is basic calcium phosphate. Basic calcium phosphate (Ca)5(PO4)3(OH)) has excellent biocompatibility and bioactivity, and calcium ions in the calcium ion can be replaced by cations through ion exchange, so that the calcium ion selective electrode can be used as an ion active agent of the calcium ion selective electrode. The basic calcium phosphate is easy to synthesize and purify, easy to purchase and low in price.
The nonionic surfactant is triton X-100.
The polymer material is Cellulose Acetate (CA) is environment-friendly materials, is cellulose derived from plant bodies, has good transparency and mechanical properties, is cellulose derivatives which are most widely applied in fields at present, selects a proper plasticizer and can be used as a matrix material of the ion selective electrode.
The plasticizer is at least of tributyl phosphate (TBP), dimethyl phthalate (DMP) and diethyl phthalate (DEP).
The volatile solvent is at least of acetone and methyl acetate.
The invention also provides a preparation method of the induction membrane of calcium ion selective electrodes, which comprises the following steps of mixing and stirring uniformly 5-15% of calcium ion active agent, 0.5-3% of nonionic surfactant, 30-50% of polymer material and 40-60% of plasticizer as solute with volatile solvent, wherein the ratio of the solute to the solvent is 25-100mg/mL, sealing, mixing and stirring for more than 4 hours at normal temperature, and volatilizing and standing the uniformly stirred mixed solution at normal temperature to form a membrane.
With reference to table 1, the following description will be given in terms of 4 specific examples:
in examples 1-4, the solute is weighed according to the above ratio and put into a beaker, the solvent in the above ratio is added into a fume hood, clean magnetons are added, the beaker is sealed by a sealing film, and the beaker is placed on a magnetic stirrer to be stirred for more than 4 hours, so that the solute and the solvent are fully and uniformly stirred; and (3) transferring the uniformly stirred mixed solution into a clean and flat film-making container, slowly volatilizing the solvent at room temperature, and completely volatilizing the solvent to obtain the calcium ion selective induction film.
The obtained sensing membrane is placed in a calcium ion selective electrode, and connected with a calcium ion tester together with a reference electrode to test the slope and stability of the sensing membrane when the calcium ion concentration is 10-5～10-2mol·L-1The slope in the range is shown in figure 1, at a calcium ion concentration of 10-3mol·L-1The stability in solution of (a) is shown in figure 2. The test result shows that the slope is close to the Nernst theoretical slope 29.58mV/pCa, and the stability is good in 30 days.
TABLE 1
Compared with the prior art, the preparation method of the calcium ion selective induction membrane provided by the invention has the advantages that the process is simple, the preparation can be completed by using common laboratory equipment, the cost of the used materials is low, and the preparation method is environment-friendly; the prepared induction film has high flatness, good uniformity and good toughness; the calcium ion selective electrode prepared by the induction membrane has good selectivity, high measurement precision and good stability.
It will be understood by those skilled in the art that the sensing film and the manufacturing method of the present invention are not limited to the examples described in the detailed description, and the above detailed description is only for the purpose of explaining the present invention and is not intended to limit the present invention. Other embodiments will be apparent to those skilled in the art from the following detailed description, which is intended to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.
Claims (7)
- The induction membrane of calcium ion selective electrodes is characterized in that the induction membrane is formed by uniformly mixing a solute and a volatile solvent, wherein the volatile solvent is volatilized to form a membrane, and the mass ratio of the solute to the calcium ion active agent is 5-15%, the nonionic surfactant is 0.5-3%, the polymer material is 30-50%, and the plasticizer is 40-60%.
- 2. The sensing membrane of calcium ion-selective electrodes according to claim 1, wherein the calcium ion active agent is basic calcium phosphate.
- 3. The sensing membrane of calcium ion-selective electrodes, according to claim 1, wherein the non-ionic surfactant is Triton X-100.
- 4. The sensing membrane of calcium ion-selective electrodes according to claim 1, wherein the polymer material is cellulose acetate.
- 5. The sensing membrane of calcium ion-selective electrodes according to claim 1, wherein the plasticizer is at least of tributyl phosphate, dimethyl phthalate and diethyl phthalate.
- 6. The sensing membrane of calcium ion-selective electrodes according to claim 1, wherein the volatile solvent is at least of acetone and methyl acetate.
- 7. The method for preparing a sensing membrane of calcium ion selective electrodes according to claims 1-6, wherein the method comprises the following steps:5 to 15 percent of calcium ion active agent, 0.5 to 3 percent of nonionic surfactant, 30 to 50 percent of polymer material and 40 to 60 percent of plasticizer are used as solute and are mixed and stirred uniformly with a volatile solvent, the ratio of the solute to the solvent is 25 to 100mg/mL, the mixture is stirred hermetically at normal temperature for more than 4 hours, and the uniformly stirred mixture is stood and volatilized to form a film at normal temperature.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910836645.1A CN110734583A (en) | 2019-09-05 | 2019-09-05 | Induction film of calcium ion selective electrodes and preparation method thereof |
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| CN201910836645.1A CN110734583A (en) | 2019-09-05 | 2019-09-05 | Induction film of calcium ion selective electrodes and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116178860A (en) * | 2023-03-01 | 2023-05-30 | 北京华科仪科技股份有限公司 | Calcium ion selective response electrode sensitive film and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116178860A (en) * | 2023-03-01 | 2023-05-30 | 北京华科仪科技股份有限公司 | Calcium ion selective response electrode sensitive film and preparation method thereof |
| CN116178860B (en) * | 2023-03-01 | 2024-10-18 | 北京华科仪科技股份有限公司 | Calcium ion selective response electrode sensitive film and preparation method thereof |
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