CN111257396A - Miniature electrochemical system based on near field communication technology and detection method - Google Patents
Miniature electrochemical system based on near field communication technology and detection method Download PDFInfo
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Abstract
The invention discloses a micro electrochemical system based on an NFC technology and a detection method. The system comprises a first substrate, an NFC antenna, an NFC chip and a peripheral circuit thereof, a single chip microcomputer chip and a peripheral circuit thereof, an electrochemical potentiostat circuit, an electrode connecting pad and a heavy metal detection electrode array, wherein the NFC antenna, the NFC chip and the peripheral circuit thereof are processed on the first substrate and are sequentially connected. The invention integrates a miniature electrochemical system on the wireless passive flexible NFC label, realizes the miniaturization, flexibility and integration of the electrochemical detection device, can be attached to the inner walls of various containers, realizes the detection of heavy metals in solution, and has wide application prospect in the fields of food safety, environmental monitoring and the like. The method can be used for quantitative detection of trace heavy metal ions such as lead, cadmium and the like.
Description
Technical Field
The embodiment of the invention relates to an electrochemical detection technology, in particular to a micro electrochemical system and a detection method based on a Near Field Communication (NFC) technology.
Background
Heavy metals such as lead, cadmium, mercury, and copper pose serious threats to health, such as cancer, cardiovascular diseases, brain damage, and kidney diseases. Some containers commonly used by people, such as ceramic, enamel or glazed glass containers, can slowly transfer heavy metals such as lead and cadmium into food during long-time food or beverage containing processes, and indirectly harm the health of people. Therefore, a miniaturized label-type heavy metal detection system is constructed, and the heavy metal detection system can be placed in a container to monitor the content of heavy metals in food or drink, which is particularly urgent.
At present, the technical means for detecting heavy metals are very mature in the research field. The traditional detection method mainly uses large instruments to carry out heavy metal analysis on a target sample, such as X-ray fluorescence spectroscopy, Atomic Absorption Spectroscopy (AAS), inductively coupled plasma mass spectrometry (ICP-MS) and the like, but the large instruments are expensive, time-consuming and labor-consuming in detection, need professional operation and complex pretreatment process, and are not suitable for detection anytime and anywhere in daily life.
Disclosure of Invention
In view of this, embodiments of the present invention provide a Near Field Communication (NFC) -technology-based micro electrochemical system and a detection method, which solve the problems in the related art that a detection system is not integrated enough, is not miniaturized enough, is not flexible enough, and has a high price of an instrument, and detection is time-consuming and labor-consuming.
The purpose of the embodiment of the invention is realized by the following technical scheme:
the embodiment of the invention provides a micro electrochemical system based on a near field communication technology, which is characterized by comprising a first substrate, an NFC antenna, an NFC chip and a peripheral circuit thereof, a singlechip chip and a peripheral circuit thereof, an electrochemical potentiostat circuit, an electrode connecting pad and a heavy metal detection electrode array, wherein the NFC antenna, the NFC chip and the peripheral circuit thereof, the singlechip chip and the peripheral circuit thereof, the electrochemical potentiostat circuit, the electrode connecting pad and the heavy metal detection electrode array are processed on the first substrate and.
Furthermore, the mobile terminal with the NFC function wirelessly supplies power to the NFC chip and a peripheral circuit thereof, the singlechip chip and a peripheral circuit thereof, and the electrochemical potentiostat circuit through electromagnetic induction between the mobile terminal and the NFC antenna; the electrochemical potentiostat circuit applies corresponding potential excitation to the heavy metal detection electrode array through the electrode connecting pad under the control of the singlechip and the peripheral circuit thereof, heavy metal ions in the solution are firstly reduced and deposited on the electrode array and then oxidized, the generated response current is transmitted to the electrochemical potentiostat circuit through the electrode connecting pad, the response current is transmitted to the singlechip chip and the peripheral circuit thereof for analog-to-digital conversion after signal processing, and the converted data is transmitted to the NFC chip and the peripheral circuit thereof; the mobile terminal with the NFC function acquires concentration information of heavy metal ion detection in real time through electromagnetic induction between the mobile terminal and the NFC antenna.
Further, the heavy metal detection electrode array comprises a second substrate, and a working electrode, a common reference electrode and a common counter electrode which are processed on the second substrate.
Further, the working electrode comprises a lead ion working electrode and a cadmium ion working electrode.
Furthermore, a layer of gold nanoparticles is modified on the carbon substrate of the lead ion working electrode, and a layer of Nafion film is covered on the gold nanoparticles.
Furthermore, a layer of bismuth nano-particles is modified on the carbon substrate of the cadmium ion working electrode, and a layer of Nafion film is covered on the bismuth nano-particles.
Further, the material of the common reference electrode is a silver-silver chloride substrate.
Further, the material of the common counter electrode is a carbon substrate.
Further, the method for manufacturing the gold nanoparticle layer comprises the following steps:
dissolving 0.1 wt% of chloroauric acid in 0.5M sodium sulfate solution, taking a proper amount of mixed solution, dropwise adding the mixed solution on a carbon substrate of a lead ion working electrode, scanning for 5 circles by adopting a cyclic voltammetry, wherein the scanning voltage is-1.4V-1V, the scanning speed is 0.1V/s, and obtaining a gold nanoparticle layer after the scanning is finished.
Further, the method for manufacturing the bismuth nanoparticle layer comprises the following steps:
adding Bi (NO)3)3Dissolving in 1M HCl solution, adding appropriate amount of the mixture dropwise onto carbon substrate of cadmium ion working electrode, scanning with constant potential method for 120s at-0.5V for-0.5VAnd obtaining the bismuth nano particle layer after the reaction is finished.
The invention also aims to provide a method for detecting target heavy metal ions by using a miniature electrochemical system based on a near field communication technology, which comprises the following steps:
(1) heavy metal ion standard sample solution with different concentrations detected by using electronic patch
The mobile terminal with the NFC function is close to the NFC antenna, and power is wirelessly supplied to the NFC chip and a peripheral circuit thereof, the single chip microcomputer chip and a peripheral circuit thereof, and the electrochemical potentiostat circuit; sequentially dripping prepared target heavy metal ion standard sample solutions with different concentrations on the surface of the heavy metal detection electrode array; under the control of the singlechip and a peripheral circuit thereof, the electrochemical potentiostat circuit applies potential excitation of anodic stripping square wave pulse voltammetry (SWASV) to the heavy metal detection electrode array through the electrode connecting pad, heavy metal ions in the solution are firstly reduced and deposited on the working electrode and then oxidized, the generated response current is transmitted to the electrochemical potentiostat circuit through the electrode connecting pad, the electrochemical potentiostat circuit is subjected to signal processing and then transmitted to the singlechip chip and the peripheral circuit thereof for analog-to-digital conversion, and the converted data is transmitted to the NFC chip and the peripheral circuit thereof; the method comprises the following steps that a mobile terminal with an NFC function continuously receives current signals measured by a miniature electrochemical system through electromagnetic induction between the mobile terminal and an NFC antenna, peak current under each concentration is calculated, constant potential is applied to a working electrode to carry out electrode cleaning after each concentration is measured, and the surface of a heavy metal detection electrode array is washed and dried;
(2) establishing a standard curve of the concentration of the heavy metal ion standard sample solution and the peak current of the square wave pulse voltammetry curve:
aiming at each heavy metal ion, at least three heavy metal detection electrode arrays are respectively used, the measurement process in the step (1) is repeated, the peak current of each heavy metal detection electrode array under different heavy metal ion concentrations is obtained, and then a relation curve between the solution concentration and the peak current of each heavy metal ion standard sample is obtained, and the relation curve is used for calculating the target heavy metal concentration in a real sample through the measured peak current value of the square wave pulse voltammetry curve;
(3) and (3) detecting the concentration of the target heavy metal ions in the real sample:
connecting the heavy metal detection electrode array to be detected with an electrochemical potentiostat circuit through an electrode connecting pad; the mobile terminal with the NFC function is close to the NFC antenna, and power is wirelessly supplied to the NFC chip and a peripheral circuit thereof, the single chip microcomputer chip and a peripheral circuit thereof, and the electrochemical potentiostat circuit; dripping a real sample solution to be detected on the surface of the heavy metal detection electrode array, applying potential excitation of anodic stripping square wave pulse voltammetry (SWASV) to the heavy metal detection electrode array through an electrode connecting pad by an electrochemical potentiostat circuit under the control of a single chip microcomputer and a peripheral circuit thereof, reducing and depositing target heavy metal ions in the solution on a working electrode, oxidizing the target heavy metal ions, transmitting a generated response current to the electrochemical potentiostat circuit through the electrode connecting pad, transmitting the response current to the single chip microcomputer chip and the peripheral circuit thereof for analog-to-digital conversion after signal processing, and transmitting converted data to an NFC chip and the peripheral circuit thereof; the mobile terminal with the NFC function continuously receives a current signal measured by the miniature electrochemical system through electromagnetic induction between the mobile terminal and the NFC antenna, and calculates peak current. Calculating the concentration of the target heavy metal ions by using the relation curve between the concentration of the heavy metal ion standard sample solution and the peak current in the step (2), and displaying; after each heavy metal ion is detected, a constant potential is applied to the corresponding working electrode for cleaning.
Compared with the existing electrochemical heavy metal ion detection system, the invention has the following beneficial effects: according to the embodiment of the invention, the complete heavy metal detection function can be realized by using the mobile terminal with the NFC function without depending on any external instrument. The system is constructed based on the Near Field Communication (NFC) technology, does not need to be powered by a battery, does not need to be connected with a mobile terminal in a wired mode for data transmission, and achieves wireless data transmission and wireless power supply through an NFC antenna. The design greatly improves the miniaturization, integration and flexibility of the system. Based on the design, a potentiostat system for electrochemical sensing analysis is integrated on the ultrathin flexible NFC label for quantitative detection of trace heavy metal ions. After the system is well packaged, the system can be attached to the inner walls of various containers, such as mineral water buckets, wine jars and vegetable jars, so that long-time heavy metal ion detection is realized. The system can be widely applied to the fields of food safety, water pollution monitoring and the like in the future, and has wide application prospect.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 is a block diagram illustrating an overall structure of a micro electrochemical system based on Near Field Communication (NFC) technology according to an embodiment of the present invention;
FIG. 2 is an external view of an electrode array for heavy metal ion detection according to an embodiment of the present invention;
FIG. 3 is a detail view of the electrode array for heavy metal ion detection in the embodiment of the present invention;
FIG. 4 is a block diagram of the overall workflow of the system in an embodiment of the invention;
FIG. 5 is a schematic diagram of anodic stripping square wave pulse voltammetry (SWASV) potential excitation in an example of the invention;
FIG. 6 is a diagram showing the detection mechanism of the target heavy metal on the electrode surface in the embodiment of the present invention;
FIG. 7 is a diagram of a mobile terminal APP interface in an embodiment of the present invention;
FIG. 8 is a graph comparing system test results with electrochemical workstation test results in an embodiment of the present invention;
FIG. 9 is a square wave pulse voltammogram of lead ions of different concentrations tested by an embodiment of the present invention;
FIG. 10 is a standard curve of lead ion concentration versus peak current obtained from tests conducted in accordance with an embodiment of the present invention;
FIG. 11 is a square wave pulse voltammogram of cadmium ions of different concentrations tested according to an embodiment of the present invention;
FIG. 12 is a standard curve of cadmium ion concentration versus peak current obtained from the testing of an embodiment of the present invention;
fig. 13 is a view of a practical application scenario of the micro electrochemical system in an embodiment of the present invention.
In the figure: the device comprises a first substrate 1, an NFC antenna 2, an NFC chip and a peripheral circuit 3 thereof, a single chip microcomputer chip and a peripheral circuit 4 thereof, an electrochemical potentiostat circuit 5, an electrode connecting pad 6, a heavy metal detection electrode array 7, a second substrate 71, a lead ion working electrode 72, a cadmium ion working electrode 73, a common reference electrode 74, a common counter electrode 75, a carbon substrate 721 on the lead ion working electrode, gold nanoparticles 722, a Nafion film 723 on the lead ion working electrode, a carbon substrate 731 on the cadmium ion working electrode, bismuth nanoparticles 732, a Nafion film 733 on the cadmium ion working electrode, a silver-silver chloride substrate 741 on the common reference electrode, and a carbon substrate 751 on the common counter electrode.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the following will clearly and completely describe the technical solutions of the embodiments of the present invention with reference to specific embodiments of the present invention and corresponding drawings. It is to be understood that the described embodiments are only some, and not all, embodiments of the invention. All other embodiments obtained by persons of ordinary skill in the art based on the embodiments of the present invention without any creative efforts shall fall within the protection scope of the embodiments of the present invention.
As shown in figure 1, the invention provides a micro electrochemical system based on near field communication technology, which comprises a first substrate 1, an NFC antenna 2, an NFC chip and a peripheral circuit 3 thereof, a singlechip chip and a peripheral circuit 4 thereof, an electrochemical potentiostat circuit 5, an electrode connecting pad 6 and a heavy metal detection electrode array 7, wherein the NFC antenna 2, the NFC chip and the peripheral circuit 3 thereof are processed on the first substrate 1 and are sequentially connected.
The mobile terminal with the NFC function wirelessly supplies power to the NFC chip and a peripheral circuit 3 thereof, the singlechip chip and a peripheral circuit 4 thereof and the electrochemical potentiostat circuit 5 through electromagnetic induction between the mobile terminal and the NFC antenna 2; the electrochemical potentiostat circuit 5 applies corresponding potential excitation to the heavy metal detection electrode array 7 through the electrode connecting pad 6 under the control of the singlechip and the peripheral circuit 4 thereof, heavy metal ions in the solution are firstly reduced and deposited on the electrode array 7 and then oxidized, the generated response current is transmitted to the electrochemical potentiostat circuit 5 through the electrode connecting pad 6, the response current is transmitted to the singlechip chip and the peripheral circuit 4 thereof for analog-to-digital conversion after signal processing, and the converted data is transmitted to the NFC chip and the peripheral circuit 3 thereof; the mobile terminal with the NFC function acquires concentration information of heavy metal ion detection in real time through electromagnetic induction between the mobile terminal and the NFC antenna 2.
In one possible implementation, as shown in fig. 2, the heavy metal detection electrode array 7 includes a second substrate 71, and a working electrode, a common reference electrode 74 and a common counter electrode 75 processed on the second substrate 71.
In one possible implementation, the working electrodes include a lead ion working electrode 72, a cadmium ion working electrode 73, and the like.
The two working electrodes, the common reference electrode and the common counter electrode are all subjected to multilayer modification, as shown in FIG. 3.
In one possible implementation, the carbon substrate 721 of the lead ion working electrode 72 is modified with a layer of gold nanoparticles 722 covered with a layer of Nafion film 723.
Further, the gold nanoparticle layer 722 is prepared by the following method:
dissolving 0.1 wt% of chloroauric acid in 0.5M sodium sulfate solution, taking a proper amount of mixed solution, dropwise adding the mixed solution on a carbon substrate of a lead ion working electrode, scanning for 5 circles by adopting a cyclic voltammetry, wherein the scanning voltage is-1.4V-1V, the scanning speed is 0.1V/s, and obtaining a gold nanoparticle layer after the scanning is finished.
In one possible implementation, the carbon substrate 731 of the cadmium ion working electrode 73 is modified with a layer of bismuth nanoparticles 732, and covered with a layer of Nafion film 733.
Further, the method for manufacturing the bismuth nanoparticle layer 732 is as follows:
adding Bi (NO)3)3Dissolving in 1M HCl solution, adding appropriate amount of the mixture dropwise onto carbon substrate of cadmium ion working electrode, and sweeping by constant potential methodAnd (4) scanning for 120s, scanning the voltage to be-0.5V, and obtaining the bismuth nanoparticle layer after scanning is finished.
In one possible implementation, the material of the common reference electrode 74 is a silver-silver chloride substrate 741.
In one possible implementation, the material of the common counter electrode 75 is a carbon substrate 751.
Another object of the present invention is to provide a method for detecting heavy metals by using the above-mentioned micro electrochemical system based on Near Field Communication (NFC) technology, comprising the following steps:
(1) heavy metal ion standard sample solution with different concentrations detected by using electronic patch
Fig. 4 shows a flow diagram of a micro electrochemical system. A mobile terminal with an NFC function is close to an NFC antenna 2 to wirelessly supply power to an NFC chip and a peripheral circuit 3 thereof, a single chip microcomputer chip and a peripheral circuit 4 thereof, and an electrochemical potentiostat circuit 5; sequentially dripping prepared target heavy metal ion standard sample solutions with different concentrations on the surface of the heavy metal detection electrode array 7; under the control of the singlechip and the peripheral circuit 4 thereof, the electrochemical potentiostat circuit 5 applies potential excitation of anodic stripping square wave pulse voltammetry (SWASV) to the heavy metal detection electrode array 7 through the electrode connecting pad 6, heavy metal ions in the solution are firstly reduced, deposited and oxidized on the working electrode, the generated response current is transmitted to the electrochemical potentiostat circuit 5 through the electrode connecting pad 6, is transmitted to the singlechip chip and the peripheral circuit 4 thereof for analog-to-digital conversion after signal processing, and the converted data is transmitted to the NFC chip and the peripheral circuit 3 thereof; the mobile terminal with the NFC function continuously receives current signals measured by the micro electrochemical system through electromagnetic induction between the mobile terminal and the NFC antenna 2, the peak current of each concentration is calculated, constant potential is applied to a working electrode to clean the electrode after each concentration is measured, and the surface of the heavy metal detection electrode array 7 is washed and dried;
(2) establishing a standard curve of the concentration of the heavy metal ion standard sample solution and the peak current of the square wave pulse voltammetry curve:
aiming at each heavy metal ion, at least three heavy metal detection electrode arrays 7 are respectively used, the measurement process in the step (1) is repeated, the peak current of each heavy metal detection electrode array 7 under different heavy metal ion concentrations is obtained, and then a relation curve between the solution concentration and the peak current of each heavy metal ion standard sample is obtained, and the relation curve is used for calculating the target heavy metal concentration in a real sample through the measured peak current value of the square wave pulse voltammetry curve;
(3) and (3) detecting the concentration of the target heavy metal ions in the real sample:
connecting a heavy metal detection electrode array 7 to be detected with an electrochemical potentiostat circuit 5 through an electrode connecting pad 6; a mobile terminal with an NFC function is close to an NFC antenna 2 to wirelessly supply power to an NFC chip and a peripheral circuit 3 thereof, a single chip microcomputer chip and a peripheral circuit 4 thereof, and an electrochemical potentiostat circuit 5; dripping a real sample solution to be detected on the surface of a heavy metal detection electrode array 7, applying potential excitation of anodic stripping square wave pulse voltammetry (SWASV) to the heavy metal detection electrode array 7 through an electrode connecting pad 6 by an electrochemical potentiostat circuit 5 under the control of a single chip microcomputer and a peripheral circuit 4 thereof, reducing and depositing target heavy metal ions in the solution on a working electrode, oxidizing the target heavy metal ions, transmitting the generated response current to the electrochemical potentiostat circuit 5 through the electrode connecting pad 6, performing signal processing, transmitting the response current to the single chip microcomputer chip and the peripheral circuit 4 thereof for analog-to-digital conversion, and transmitting the converted data to an NFC chip and the peripheral circuit 3 thereof; the mobile terminal with the NFC function continuously receives the current signal measured by the micro electrochemical system through electromagnetic induction between the mobile terminal and the NFC antenna 2, and calculates peak current. Calculating the concentration of the target heavy metal ions by using the relation curve between the concentration of the heavy metal ion standard sample solution and the peak current in the step (2), and displaying; after each heavy metal ion is detected, a constant potential is applied to the corresponding working electrode for cleaning.
The electrochemical heavy metal ion detection system comprises modules such as a sensing electrode, an electrochemical sensing circuit, data transmission, energy collection and the like, and can realize a complete heavy metal detection function by using a mobile terminal with an NFC function without depending on any external instrument. The system is constructed based on the Near Field Communication (NFC) technology, does not need to be powered by a battery, does not need to be connected with a mobile terminal in a wired mode for data transmission, and achieves wireless data transmission and wireless power supply through an NFC antenna. The design greatly improves the miniaturization, integration and flexibility of the system. Based on the design, a potentiostat system for electrochemical sensing analysis is integrated on the ultrathin flexible NFC label, so that several classical electrochemical sensing methods in electrochemical sensing, such as an anodic stripping square wave pulse voltammetry, can be realized, and the method can be used for quantitative detection of trace heavy metal ions such as lead and cadmium. After the system is well packaged, the system can be attached to the inner walls of various containers, such as mineral water buckets, wine jars and vegetable jars, so that long-time heavy metal ion detection is realized. The system can be widely applied to the fields of food safety, water pollution monitoring and the like in the future, and has wide application prospect.
The present invention is described in further detail below by way of examples.
Example (b):
1. design of a miniature electrochemical system based on Near Field Communication (NFC) technology:
as shown in fig. 1, a substrate of the flexible circuit board adopts flexible Polyimide (PI) as a first substrate 1, a resonant frequency of the NFC antenna is 13.56MHz, an NFC chip adopts NT3H2111 of enginepu, and a mobile terminal with an NFC function in an experiment selects samsung Galaxy S5. The wireless power supply and the bidirectional data transmission of the system are realized between the smart phone and the NFC antenna through electromagnetic induction. The single chip and its peripheral circuit 4 adopt MSP430FR2632 of Texas instruments and 16 bit AD conversion chip ADS1115 of Texas instruments. The electrochemical potentiostat circuit 5 employs 4 operational amplifiers AD8605, a sixteen-bit DA converter DAC8562, and a multiplexing check chip SN74LVC1G3157 for selecting different working electrodes.
The working flow diagram of the whole micro electrochemical system is shown in figure 4. Energy transmission starts from an NFC module of the smart phone, is transmitted to an NFC antenna 2 of the detection device through mutual inductance of the antenna, an NFC chip connected with the NFC antenna and a peripheral circuit 3 of the NFC chip obtain energy from the NFC antenna 2, the energy is continuously transmitted to a rear end circuit (about 2.72V) through an internal power management circuit, and a singlechip and the peripheral circuit 4 of the singlechip at the rear end work under the energy provided by the NFC chip and the peripheral circuit 3 of the NFC chip. Under the control of the smart phone, the singlechip and the peripheral circuit 4 thereof, the electrochemical potentiostat circuit 5 applies potential excitation of anodic stripping square wave pulse voltammetry to the heavy metal detection electrode array 7 (as shown in fig. 5). Heavy metal ions are reduced and deposited on the surface of a corresponding working electrode, and then oxidized and dissolved out (as shown in fig. 6), a generated current signal is captured by an electrochemical potentiostat circuit 5, the current signal is converted into a voltage signal through a single chip microcomputer and a peripheral circuit 4 thereof, the voltage signal is converted into a digital signal and transmitted to an internal storage space of an NFC chip, smart phone Application software reads internal storage data of the NFC chip by calling an internal NFC driving related Application Program Interface (API), and a result is displayed in a phone Interface (fig. 7).
The micro electrochemical system is compared with a standard electrochemical workstation, the electrode adopted in the comparison is a standard electrochemical three-electrode system, and the target solution is a redox couple containing 20mM potassium ferricyanide/potassium ferrocyanide of 0.1MKCl solution. Three different sets of parameters were selected for comparison: step,4mV or 10 mV; pulse,40mV or 80 mV; frequency,40 Hz; voltage range-0.4 to 0.8V vs standard Ag/AgCl reference electrode. As can be seen from fig. 8, in the three cases, the errors of the two are 0.48%, 0.39%, and 2.33%, respectively, and a higher consistency is achieved.
2. Design and construction and modification of electrode arrays:
as shown in fig. 2, the heavy metal detection electrode array 7 employs flexible polyethylene terephthalate (PET) as a second substrate 71 on which 4 electrodes including a lead ion working electrode 72, a cadmium ion working electrode 73, a common reference electrode 74, a common counter electrode 75, and the like are printed. The 4 electrodes are all designed in a layered manner (as shown in fig. 3), wherein the lead ion working electrode 72 and the cadmium ion working electrode 73 are ellipses with the size of 4mm × 2.5mm, and the substrates are all printed by carbon ink; the substrate of the common counter electrode 75 is also printed with carbon ink; the lead portion of the electrode array and the substrate of the common reference electrode 74 are printed with silver-silver chloride ink, and the printed electrode array needs to be dried at 80 ℃ for 15 minutes and stored at room temperature for later use.
The gold nanoparticle layer 722 on the lead ion working electrode 72 is fabricated as follows: dissolving 0.1 wt% of chloroauric acid in 0.5M sodium sulfate solution, dropwise adding a proper amount of mixed solution on a carbon substrate of a lead ion working electrode, and scanning for 5 circles by adopting a cyclic voltammetry method, wherein the scanning voltage is-1.4V-1V, and the scanning speed is 0.1V/s.
The method of making the bismuth nanoparticle layer 732 on the cadmium ion working electrode 73 is as follows: adding Bi (NO)3)3Dissolving in 1M HCl solution, dropwise adding a proper amount of mixed solution on a carbon substrate of a cadmium ion working electrode, scanning for 120s by a constant potential method, wherein the scanning voltage is-0.5V, and obtaining a bismuth nanoparticle layer after scanning.
The gold nanoparticle layer 722 and the bismuth nanoparticle layer 732 are both covered with a layer of Nafion film, and the manufacturing method is as follows: mu.l of 5 wt% Nafion solution was applied dropwise to the two working electrodes, respectively, covering the nanoparticle layer.
3. Sensitivity and linearity test of electrodes:
in all experiments, the target heavy metal ions were dissolved in 0.01M acetate buffered saline at pH 4.6 and containing 50mM NaCl. In the test of lead ions, the gradient distribution of lead ions was 0ppb, 50ppb, 100ppb, 150ppb, 200ppb, 250ppb, and 300ppb, the working electrode was a gold nanoparticle-modified lead ion working electrode 72, and the test employed was anodic stripping square wave pulse voltammetry (SWASV) including three stages. In the first stage, lead ions are deposited for 120s at a voltage of-0.7V; in the second stage, performing electrochemical scanning of square wave stripping voltammetry under the voltage range of-0.7V to 0.1V, wherein the scanning step is 4mV, the amplitude (pulse) is 40mV, and the frequency is 40 Hz; in the third stage, the electrode cleaning process was performed at a voltage of 0.1V for 120 s. In the test of cadmium ions, the gradient distribution of the cadmium ions is 0ppb, 100ppb, 150ppb, 200ppb, 250ppb and 300ppb, the working electrode is a bismuth nanoparticle modified cadmium ion working electrode 73, and the test adopts a method of anodic stripping square wave pulse voltammetry (SWASV) and comprises three stages. In the first stage, cadmium ions are deposited for 120s at a voltage of-1.5V; in the second stage, performing electrochemical scanning of square wave stripping voltammetry in a voltage range from-1.2V to-0.5V, wherein the scanning step is 4mV, the amplitude (pulse) is 40mV, and the frequency is 40 Hz; in the third stage, the electrode cleaning process is carried out for 180s under the voltage of-0.5V.
Fig. 9 shows a square wave pulse voltammogram of lead ion tests with different concentrations using the micro electrochemical system, and it can be seen that the peak current of lead ions is much higher at a position around-0.22V. FIG. 10 shows a lead ion concentration-peak current standard curve from which the sensitivity of lead ion detection was 0.1531 μ A/ppb, R20.997, exhibiting better linearity. FIG. 10 shows a square wave pulse voltammogram of cadmium ion tests of various concentrations using the miniaturized electrochemical system, and it can be seen that the peak of cadmium ions appears at approximately-0.96V. FIG. 12 shows a standard curve of cadmium ion concentration-peak current, from which it can be obtained that the sensitivity of cadmium ion detection is 0.18338 μ A/ppb, R20.976, also exhibits better detection linearity.
4. And testing the actual application scene.
Fig. 13 shows a practical application scenario of the micro electrochemical system in the present invention. In practical application, the miniaturized, integrated and flexible label system can be attached to the inner walls of various containers, such as wine jars, vegetable jars and the like, for a long time through proper packaging. When the heavy metal content in food or drink in the container needs to be known, people only need to open the APP of the smart phone, and the APP is separated from the shell of the container to wirelessly supply power to the system, and whether lead ions and cadmium ions in the container exceed standards or not is detected. Since the tag does not require a battery, there is no need to consider the safety problem of replacing the battery or leakage of the battery. The label has wide application prospect in the fields of food safety, environmental pollution and the like.
It should be noted that the heavy metal ions in the present invention are not limited to cadmium ions and lead ions in the above examples, and may include other various heavy metal ions such as copper, mercury, and zinc. With the above embodiments, those skilled in the art can unambiguously determine how other heavy metal ions, such as copper, mercury, zinc, etc., are detected. For the preparation of other heavy metal ion working electrodes, reference may also be made to the preparation methods of cadmium ion and lead ion working electrodes in this specification.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. The miniature electrochemical system based on the near field communication technology is characterized by comprising a first substrate (1), an NFC antenna (2), an NFC chip and a peripheral circuit (3), a singlechip chip and a peripheral circuit (4), an electrochemical potentiostat circuit (5), an electrode connecting pad (6) and a heavy metal detection electrode array (7), wherein the NFC antenna, the NFC chip and the peripheral circuit (3), the singlechip chip and the peripheral circuit (4) are processed on the first substrate (1) and are sequentially connected.
2. The micro electrochemical system based on the near field communication technology as claimed in claim 1, wherein the mobile terminal with the NFC function wirelessly supplies power to the NFC chip and its peripheral circuit (3), the one-chip and its peripheral circuit (4), and the electrochemical potentiostat circuit (5) by electromagnetic induction with the NFC antenna (2); under the control of the singlechip and a peripheral circuit (4) thereof, the electrochemical potentiostat circuit (5) applies corresponding potential excitation to the heavy metal detection electrode array (7) through the electrode connecting pad (6), heavy metal ions in the solution are firstly reduced and deposited on the electrode array (7) and then oxidized, the generated response current is transmitted to the electrochemical potentiostat circuit (5) through the electrode connecting pad (6), the response current is transmitted to the singlechip chip and the peripheral circuit (4) thereof for analog-to-digital conversion after signal processing, and the converted data is transmitted to the NFC chip and the peripheral circuit (3) thereof; the mobile terminal with the NFC function obtains the concentration information of heavy metal ion detection in real time through electromagnetic induction between the mobile terminal and the NFC antenna (2).
3. A near field communication technology-based micro electrochemical system according to claim 1, wherein the heavy metal detection electrode array (7) comprises a second substrate (71) and a working electrode, a common reference electrode (74) and a common counter electrode (75) processed on the second substrate (71).
4. The micro electrochemical system based on the near field communication technology as claimed in claim 3, wherein the working electrode comprises a lead ion working electrode (72) and a cadmium ion working electrode (73).
5. The near field communication technology-based micro electrochemical system as claimed in claim 4, wherein the carbon substrate (721) of the lead ion working electrode (72) is modified with a layer of gold nanoparticles (722) covered with a Nafion film (723).
6. The near field communication technology-based micro electrochemical system as claimed in claim 4, wherein the carbon substrate (731) of the cadmium ion working electrode (73) is modified with a layer of bismuth nanoparticles (732) covered with a Nafion film (733).
7. A near-field communication technology-based micro electrochemical system according to claim 4, characterized in that the material of the common reference electrode (74) is a silver-silver chloride substrate (741).
8. A near-field communication technology-based micro electrochemical system according to claim 4, characterized in that the material of the common counter electrode (75) is a carbon substrate (751).
9. The method for detecting the target heavy metal ions by using the micro electrochemical system based on the near field communication technology as claimed in any one of claims 1 to 8, wherein the method comprises the following steps:
(1) heavy metal ion standard sample solution with different concentrations detected by using electronic patch
A mobile terminal with an NFC function is close to an NFC antenna (2) to wirelessly supply power to an NFC chip and a peripheral circuit (3) thereof, a single chip microcomputer chip and a peripheral circuit (4) thereof and an electrochemical potentiostat circuit (5); sequentially dripping prepared target heavy metal ion standard sample solutions with different concentrations on the surface of the heavy metal detection electrode array (7); under the control of the singlechip and a peripheral circuit (4) thereof, an electrochemical potentiostat circuit (5) applies potential excitation of anodic stripping square wave pulse voltammetry (SWASV) to a heavy metal detection electrode array (7) through an electrode connecting pad (6), heavy metal ions in the solution are firstly reduced and deposited on a working electrode and then oxidized, the generated response current is transmitted to the electrochemical potentiostat circuit (5) through the electrode connecting pad (6), the response current is transmitted to the singlechip chip and the peripheral circuit (4) thereof for analog-to-digital conversion after signal processing, and the converted data is transmitted to an NFC chip and the peripheral circuit (3) thereof; the mobile terminal with the NFC function continuously receives current signals measured by the miniature electrochemical system through electromagnetic induction between the mobile terminal and the NFC antenna (2), the peak current of each concentration is calculated, constant potential is applied to a working electrode to clean the electrode after each concentration is measured, and the surface of the heavy metal detection electrode array (7) is washed and dried;
(2) establishing a standard curve of the concentration of the heavy metal ion standard sample solution and the peak current of the square wave pulse voltammetry curve:
aiming at each heavy metal ion, at least three heavy metal detection electrode arrays (7) are respectively used, the measurement process in the step (1) is repeated, the peak current of each heavy metal detection electrode array (7) under different heavy metal ion concentrations is obtained, and then a relation curve between the solution concentration and the peak current of each heavy metal ion standard sample is obtained, and the relation curve is used for calculating the target heavy metal concentration in a real sample through the measured peak current value of the square wave pulse voltammetry curve;
(3) and (3) detecting the concentration of the target heavy metal ions in the real sample:
connecting a heavy metal detection electrode array (7) to be detected with an electrochemical potentiostat circuit (5) through an electrode connection pad (6); a mobile terminal with an NFC function is close to an NFC antenna (2) to wirelessly supply power to an NFC chip and a peripheral circuit (3) thereof, a single chip microcomputer chip and a peripheral circuit (4) thereof and an electrochemical potentiostat circuit (5); dripping a real sample solution to be detected on the surface of a heavy metal detection electrode array (7), applying potential excitation of anodic stripping square wave pulse voltammetry (SWASV) to the heavy metal detection electrode array (7) by an electrochemical potentiostat circuit (5) through an electrode connecting pad (6) under the control of a single chip microcomputer and a peripheral circuit (4) thereof, reducing and depositing target heavy metal ions in the solution on a working electrode, oxidizing the target heavy metal ions, transmitting the generated response current to the electrochemical potentiostat circuit (5) through the electrode connecting pad (6), transmitting the response current to the single chip microcomputer and the peripheral circuit (4) thereof after signal processing for analog-to-digital conversion, and transmitting the converted data to an NFC chip and the peripheral circuit (3) thereof; the mobile terminal with the NFC function continuously receives a current signal measured by the miniature electrochemical system through electromagnetic induction between the mobile terminal and the NFC antenna (2), and the peak current is calculated. Calculating the concentration of the target heavy metal ions by using the relation curve between the concentration of the heavy metal ion standard sample solution and the peak current in the step (2), and displaying; after each heavy metal ion is detected, a constant potential is applied to the corresponding working electrode for cleaning.
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