CN111044596A - Printed electrode, preparation method and detection method for heavy metal ions in water - Google Patents
Printed electrode, preparation method and detection method for heavy metal ions in water Download PDFInfo
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- CN111044596A CN111044596A CN201911196576.9A CN201911196576A CN111044596A CN 111044596 A CN111044596 A CN 111044596A CN 201911196576 A CN201911196576 A CN 201911196576A CN 111044596 A CN111044596 A CN 111044596A
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- 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
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
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- 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
- G01N27/301—Reference electrodes
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- 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
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
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- 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
- G01N27/38—Cleaning of electrodes
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Abstract
A method of making a printed electrode comprising the steps of: s10, inserting the disposable printing electrode into the reference electrode electroplating solution, applying a first positive voltage for a preset first time length by taking the reference electrode of the printing electrode as an anode and the counter electrode of the printing electrode as a cathode; s11, connecting the printed electrode to a heavy metal measuring unit, simultaneously inserting the printed electrode into an acidic solution, and applying a second positive voltage for a predetermined second time; s12, washing the printing electrode with deionized water, transferring the printing electrode into a gold plating solution, and applying a third voltage for a predetermined third time; and S13, washing the printed electrode with deionized water, airing, and placing the printed electrode in a black container for a fourth time period for stabilization.
Description
Technical Field
The invention belongs to the technical field of heavy metal ion detection, and particularly relates to a reusable gold-plated screen-printed electrode, a preparation method and a method for detecting heavy metal ions in water by using the reusable gold-plated screen-printed electrode.
Background
At present, most of portable heavy metal instruments for rapidly detecting trace heavy metal ions in the market adopt an electrochemical stripping voltammetry. The instrument has the characteristics of small volume and simple and convenient operation, and meets the requirements of field detection on portability and simple and convenient operation of the instrument.
Such instrumentation and detection systems fall into two main categories: one type is a three-electrode system with a glassy carbon electrode as a working electrode, the detection precision of the system is high, but the analysis time is greatly prolonged in actual detection and analysis due to polishing of the glassy carbon electrode and maintenance of a reference electrode, and the requirements of rapidness and convenience in field detection are difficult to achieve. The other type is a printed electrode system, the printed electrode is also called a thick film electrode, a working electrode, a reference electrode and a counter electrode are directly integrated on a substrate, and the electrochemical sensor is prepared by a thick film integrated circuit process.
Compared with a glassy carbon electrode and a gold electrode, the screen printing electrode does not need an additional reference electrode and an additional counter electrode, so that the cost is greatly reduced, and importantly, the electrode almost does not need to be processed, i.e. thrown immediately and used at one time. However, because of the disposable use, the difference between the electrodes causes the measurement result to be too large to be qualitative or semi-quantitative. The three-electrode system using the glassy carbon electrode as the working electrode has high measurement accuracy mainly as follows: the same glassy carbon electrode can ensure the consistency of the working surface, and the solid reference electrode can provide stable electrode potential because the reference solution and the solution to be measured are separated by the salt bridge.
The screen printing electrode is convenient to use, and mainly has the advantages that the working electrode, the reference electrode and the counter electrode are integrated on one substrate, plug and play are realized, and maintenance is not needed. However, the reference electrode of the printed electrode is a mixed material of silver and silver chloride which is overprinted on the substrate, the solid reference electrode is formed by plating a layer of compact silver chloride on a silver wire, the screen-printed electrode is directly inserted into a solution to be measured, the reference electrode is difficult to provide stable electrode potential, and the difference of measurement results among different electrodes is large.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a reusable gold-plated screen printing electrode, a preparation method and a method for detecting heavy metal ions in water by using the reusable gold-plated screen printing electrode, and realizes rapid and quantitative detection on site.
One embodiment of the invention, 1, a method for preparing a printed electrode, which is characterized by comprising the following steps:
s10, inserting the disposable printing electrode into the reference electrode electroplating solution, applying a first positive voltage for a preset first time length by taking the reference electrode of the printing electrode as an anode and the counter electrode of the printing electrode as a cathode;
s11, inserting the printed electrode into a measuring unit of the portable heavy metal instrument, and applying a second positive voltage in the acidic solution for a predetermined second time;
s12, washing the printing electrode with deionized water, transferring the printing electrode into a gold plating solution, and applying a third voltage for a predetermined third time;
and S13, washing the printed electrode with deionized water, airing, and placing the printed electrode in a black container for a fourth time period for stabilization.
The embodiment of the invention provides a method for preparing a reusable gold-plated screen-printed electrode and detecting heavy metal ions in water by using the same, wherein the method for preparing the reusable gold-plated screen-printed electrode comprises the following steps: (1) modification of a reference electrode; (2) applying voltage to the working electrode for pickling; (3) the surface of the working electrode is pre-plated with gold. The method for detecting the heavy metal ions in the water by adopting the printed electrode adopts the voltammetry detection of the heavy metal ions.
The beneficial effects of the invention include:
(1) the provided electrode is a reusable printed electrode, namely the same electrode is repeatedly used for multiple times, the repeatability is good, and the maintenance is not needed. The problems that the traditional printed electrode can only be used once and the repeatability between electrodes is poor are solved, and the defects that a glassy carbon electrode needs to be polished and a reference electrode needs to be maintained in a three-electrode system are overcome.
(2) The pre-plated gold-plated printed electrode can be stored for a long time, does not need additional treatment before use, can be repeatedly used by the same electrode, and is used for detecting heavy metal ions such as mercury, arsenic, copper and the like in water which can be detected only by the gold electrode.
The invention combines the advantages of the two electrode systems, combines the measurement accuracy of the three-electrode system with the advantages of no need of processing and maintenance of the printed electrode, overcomes the inherent defects of the three electrode systems, really realizes the on-site rapid accurate reminding and accurate detection and analysis of the heavy metal ions in the water pollution accident, and has important significance in the aspect of rapid detection of the heavy metal ions.
Drawings
The above and other objects, features and advantages of exemplary embodiments of the present invention will become readily apparent from the following detailed description read in conjunction with the accompanying drawings. Several embodiments of the invention are illustrated by way of example, and not by way of limitation, in the figures of the accompanying drawings and in which:
FIG. 1 is a diagram of a reusable gold-plated screen-printed electrode according to one embodiment of the present invention.
1-working electrode (carbon substrate plated with gold), 2-counter electrode (carbon), 3-silver/silver chloride reference electrode, 4-conductive silver wire, 5-insulating substrate.
Fig. 2 is a superposition graph of stripping voltammetry of 2 times of adding standard mercury ions in water by the reusable gold-plated screen-printed electrode in the embodiment 4.
Fig. 3 is a superposition graph of stripping voltammetry of mercury ions in water with the same concentration in 3 times of repeated measurement of the reusable gold-plated screen-printed electrode in the embodiment 4.
Detailed Description
Example 1
A method for preparing a reusable gold-plated screen printing electrode comprises the following steps:
and S101, modifying the reference electrode of the disposable printing electrode. Inserting a disposable printing electrode into the electroplating solution containing chloride ions, taking a reference electrode of the printing electrode as an anode and a counter electrode of the printing electrode as a cathode, and applying a positive voltage of 2.2V for 60 s;
s102, acid cleaning is carried out on the surface of the working electrode of the printing electrode. Connecting the printed electrode processed in the step S101 into a measuring device of a portable heavy metal instrument, inserting the printed electrode into a nitric acid solution with the pH value of 2.0, and applying a voltage of 1.2v for 300S;
s103, washing the printed electrode washed by the acid in the step S102 by deionized water, transferring the washed printed electrode into a mixed solution of 0.042g/L chloroauric acid and 0.1mol/L hydrochloric acid, and applying a voltage of-0.3 v for 150S;
and S104, washing the printed electrode processed in the step by using deionized water, airing, and placing in a black packaging bag for stabilization (12-24) hours.
The surface of the printed electrode contains a reference electrode, a working electrode and a counter electrode. The middle circle part is the working electrode and is connected with a lead. After the reference electrode of the printed electrode prepared by the method is modified, the same printed electrode can measure dozens of times or even hundreds of times of data from the original condition that only one datum can be measured, and the printed electrode can be used repeatedly; after the surface of the working electrode is pickled by applying voltage, a layer of gold film is plated on the surface of the working electrode by optimizing enrichment voltage and enrichment time and selecting gold plating solution, and the gold film greatly improves the sensitivity of measuring heavy metal ions such as copper, arsenic, mercury and the like. And the gold film can be stored for a long time after being plated. Compared with a three-electrode system, the glassy carbon electrode needs to be polished and pre-plated with a gold film before each measurement, and the operation is complicated. The printed electrode prepared by the method is applied to a portable heavy metal instrument, can be directly used in field or field test, and does not need additional treatment.
Example 2
A method for detecting heavy metal copper ions in water by adopting a reusable gold-plated screen printing electrode. The method comprises the following steps:
s201, the gold-plated screen-printed electrode prepared in the embodiment 1 is directly connected to a portable heavy metal instrument measuring device, inserted into 20ml of 10 mug/L heavy metal copper ion standard solution, added with 2ml of copper electrolyte, applied with a certain time of voltage, stood for 20S, scanned, dissolved out, and applied with a certain positive voltage to clean the surface of the working electrode. In this step, the applied enrichment potential is-0.80 v; the applied concentration potential was for 60 s; the scanning dissolution range is-0.3 v-0.5 v; the applied cleaning potential was 0.6 v; the applied cleaning potential was applied for 30 s.
And S202, after the step S201 is finished, continuously adding marks in the same measuring cup for 2 times, and repeatedly using the electrode in the step S201. And after the two times of labeling, directly reading the concentration of the heavy metal copper ions in the water sample to be detected, wherein the reading of the instrument is 9.15 mug/L, after the labeling is finished, storing the calibration result, and repeatedly measuring 10 mug/L of heavy metal copper ion standard solution, wherein the reading is respectively 9.76 mug/L and 8.97 mug/L.
Example 3
A method for detecting heavy metal arsenic ions in water by adopting a reusable gold-plated screen printing electrode comprises the following steps:
s301, the gold-plated screen-printed electrode prepared in the embodiment 1 is connected to a measuring device of a portable heavy metal instrument, and is inserted into 10ml of 10 mug/L heavy metal arsenic ion standard solution, 10ml of arsenic electrolyte and 0.2ml of reducing agent solution are added, voltage is applied for a certain time, the gold-plated screen-printed electrode is scanned and dissolved out after standing for 20S, and then a certain positive voltage is applied to clean the surface of the working electrode. In this step, the applied enrichment potential is-0.5 v; the applied concentration potential was for 60 s; the scanning dissolution range is-0.3 v; the applied cleaning potential was 0.6 v; the applied cleaning potential was applied for 30 s.
S302, after the step S301 is finished, continuously adding marks in the same measuring cup for 2 times, and repeatedly using the electrode in the step S301. And after the two times of labeling, directly reading the concentration of the heavy metal arsenic ions in the water sample to be detected, wherein the reading of the instrument is 8.62 mu g/L, after the labeling is finished, storing the calibration result, and repeatedly measuring the readings of the 10 mu g/L heavy metal arsenic ion standard solution to be 8.76 mu g/L and 8.57 mu g/L respectively.
Example 4
A method for detecting heavy metal mercury ions in water by adopting a reusable gold-plated screen printing electrode comprises the following steps:
s401, connecting the gold-plated screen-printed electrode prepared in the embodiment 1 into a measuring device of a portable heavy metal instrument, inserting the gold-plated screen-printed electrode into 20ml of 2 mug/L heavy metal mercury ion standard solution, adding 1ml of mercury electrolyte and 0.2ml of reducing agent solution, applying voltage for a certain time, standing for 20S, scanning and dissolving out, and applying a certain positive voltage to clean the surface of a working electrode. In this step, the applied enrichment potential was 0.01 v; the applied concentration potential was applied for 90 s; the scanning dissolution range is 0.1 v-0.55 v; the applied cleaning potential was 0.6 v; the applied cleaning potential was applied for 30 s.
S402, after the step S401 is finished, continuously adding marks in the same measuring cup for 2 times, and repeatedly using the electrode in the step S401. And after the two times of labeling, directly reading the concentration of the heavy metal mercury ions in the water sample to be detected, wherein the reading of the instrument is 1.97 mu g/L, after the labeling is finished, storing the calibration result, and repeatedly measuring the readings of the 2 mu g/L heavy metal mercury ion standard solution to be 1.84 mu g/L and 1.76 mu g/L respectively.
In examples 3 to 4, the same gold-plated printed electrode prepared in example 1 was used to detect low-concentration copper, mercury, and arsenic, and the results showed high measurement accuracy, high sensitivity, and good reproducibility.
The integrated unit, if implemented in the form of a software functional unit and sold or used as a stand-alone product, may be stored in a computer readable storage medium. Based on such understanding, the technical solution of the present invention essentially or partially contributes to the prior art, or all or part of the technical solution can be embodied in the form of a software product stored in a storage medium and including instructions for causing a computer device (which may be a personal computer, a server, or a network device) to execute all or part of the steps of the method according to the embodiments of the present invention. And the aforementioned storage medium includes: a U-disk, a removable hard disk, a Read-only Memory (ROM), a Random Access Memory (RAM), a magnetic disk or an optical disk, and other various media capable of storing program codes.
While the invention has been described with reference to specific embodiments, the invention is not limited thereto, and various equivalent modifications and substitutions can be easily made by those skilled in the art within the technical scope of the invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (12)
1. A method of making a printed electrode, the method comprising the steps of:
s10, inserting the disposable printing electrode into the reference electrode electroplating solution, applying a first positive voltage for a preset first time length by taking the reference electrode of the printing electrode as an anode and the counter electrode of the printing electrode as a cathode;
s11, connecting the printed electrode to a heavy metal measuring unit, simultaneously inserting the printed electrode into an acidic solution, and applying a second positive voltage for a predetermined second time;
s12, washing the printing electrode with deionized water, transferring the printing electrode into a gold plating solution, and applying a third voltage for a predetermined third time;
and S13, washing the printed electrode with deionized water, airing, and placing the printed electrode in a black container for a fourth time period for stabilization.
2. The method of claim 1, wherein in step S10, the electroplating solution is a chloride ion-containing solution.
3. The method of claim 2, wherein the first positive voltage range is (1.0-2.2) v, and the first duration is (5-60) s.
4. The method for preparing a printed electrode according to claim 1, wherein in step S11, the acidic solution is one of a hydrochloric acid solution, a nitric acid solution or a sulfuric acid solution, and the PH value is in a range of 1 to 4.
5. The method for preparing a printed electrode according to claim 4, wherein the second positive voltage is in a range of (1.0-1.5) v, and the second time period is in a range of (60-300) s.
6. The method for preparing a printed electrode according to claim 1, wherein the gold plating solution is a mixed solution of chloroauric acid and hydrochloric acid in step S12.
7. The method for preparing a printed electrode according to claim 6, wherein the gold plating solution is a mixed solution of (0.01-0.1) g/L chloroauric acid and 0.1mol/L hydrochloric acid.
8. The method of claim 7, wherein the third voltage range is (-1.0-0) v, and the third time period is (30-300) s.
9. A printed electrode prepared by the method of claim 1.
10. A device for detecting heavy metal ions in water, characterized in that it comprises a printed electrode according to claim 9.
11. A method for detecting heavy metal ions in water, wherein the printed electrode of claim 9 is used as a measuring electrode, the method comprising the steps of:
the printing electrode is connected to a heavy metal measuring device, inserted into a heavy metal ion water sample to be measured, added with heavy metal electrolyte, applied with a fifth voltage for a fifth time, kept static for a sixth time, scanned and dissolved out, and then applied with a sixth positive voltage to clean the surface of the working electrode;
and (4) calibrating by adopting a 2-time labeling method, repeatedly using the printing electrode, and directly reading the concentration of the heavy metal ions in the water sample to be measured after the 2-time labeling is finished.
12. The method for detecting the heavy metal ions in the water as claimed in claim 11, wherein the heavy metal electrolyte is (1-10) ml of copper electrolyte, arsenic electrolyte or mercury electrolyte, a voltage (-1.0-0) v of (30-150) s is applied, the solution is scanned and dissolved after standing for 20s, and then a positive potential (0-0.8) v is applied for a long time of (10-60) s to clean the surface of the working electrode.
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| CN201911196576.9A CN111044596A (en) | 2019-11-29 | 2019-11-29 | Printed electrode, preparation method and detection method for heavy metal ions in water |
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| CN201911196576.9A CN111044596A (en) | 2019-11-29 | 2019-11-29 | Printed electrode, preparation method and detection method for heavy metal ions in water |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113702477A (en) * | 2021-04-30 | 2021-11-26 | 广州钰芯智能科技研究院有限公司 | Gold film modified electrode for heavy metal detection and preparation method thereof |
| CN115479984A (en) * | 2021-05-31 | 2022-12-16 | 武汉中科志康生物科技有限公司 | Detection method of inorganic arsenic |
Citations (2)
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| CN201060198Y (en) * | 2007-06-07 | 2008-05-14 | 复旦大学 | Integrated forming disposable electrochemical sensor for determining blood lead concentration |
| CN103207223A (en) * | 2012-11-23 | 2013-07-17 | 上海仪电科学仪器股份有限公司 | Manufacturing method of portable heavy metal meter printing electrode |
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2019
- 2019-11-29 CN CN201911196576.9A patent/CN111044596A/en active Pending
Patent Citations (2)
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| CN201060198Y (en) * | 2007-06-07 | 2008-05-14 | 复旦大学 | Integrated forming disposable electrochemical sensor for determining blood lead concentration |
| CN103207223A (en) * | 2012-11-23 | 2013-07-17 | 上海仪电科学仪器股份有限公司 | Manufacturing method of portable heavy metal meter printing electrode |
Non-Patent Citations (3)
| Title |
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| HAO WAN 等: "Screen-printed gold electrode with gold nanoparticles modification for simultaneous electrochemical determination of lead and copper", 《SENSORS AND ACTUATORS B: CHEMICAL》 * |
| PROSPER KANYONG 等: "Gold nanoparticle modified screen-printed carbon arrays for the simultaneous electrochemical analysis of lead and copper in tap water", 《MICROCHIM ACTA》 * |
| ZHIWEI LU 等: "A screen-printed carbon electrode modified with a bismuth film and gold nanoparticles for simultaneous stripping voltammetric determination of Zn(II), Pb(II) and Cu(II)", 《MICROCHIM ACTA》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113702477A (en) * | 2021-04-30 | 2021-11-26 | 广州钰芯智能科技研究院有限公司 | Gold film modified electrode for heavy metal detection and preparation method thereof |
| CN115479984A (en) * | 2021-05-31 | 2022-12-16 | 武汉中科志康生物科技有限公司 | Detection method of inorganic arsenic |
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Application publication date: 20200421 |