CN113671012A - Electrochemical analysis sensitivity self-adjusting method suitable for on-site rapid detection - Google Patents
Electrochemical analysis sensitivity self-adjusting method suitable for on-site rapid detection Download PDFInfo
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Abstract
The invention provides an electrochemical analysis sensitivity self-adjusting method suitable for on-site rapid detection, which comprises a constant potential circuit and a mobile terminal for analyzing current data obtained by detection; during electrochemical detection, a constant potential circuit applies voltage waveform excitation to a substance to be detected, and response current of the substance to be detected is sampled by an analog-to-digital conversion module for analysis; the constant potential circuit comprises a programmable control digital potentiometer chip; the digital potentiometer chip is used for adjusting the resistance of a feedback loop when the electrochemical analysis sensitivity is automatically adjusted; when the mobile terminal judges that the current data measured in the detection process is not matched with the current sensitivity of the constant potential circuit, the digital potentiometer chip automatically adjusts the resistance value of the potentiometer to change the resistance value of the response current feedback circuit, so that the current analysis sensitivity of the constant potential circuit is matched with the current electrochemical detection.
Description
Technical Field
The invention relates to the technical field of electrochemical detection, in particular to an electrochemical analysis sensitivity self-adjusting method suitable for on-site rapid detection.
Background
The analysis sensitivity of the response current of the existing portable electrochemical detection device and method is usually manually selected when electrochemical detection is carried out, and some devices and methods also adopt fixed and unchangeable single current analysis sensitivity. The manual selection of amperometric sensitivity can lead to electrochemical detection that is too cumbersome and inefficient, making detection less convenient, and a single amperometric sensitivity that is fixed and not the same will necessarily bring about a lack in the accuracy of response amperometric detection.
Disclosure of Invention
The invention provides an electrochemical analysis sensitivity self-adjusting method suitable for on-site rapid detection, which can realize automatic adjustment of current analysis sensitivity during electrochemical detection.
The invention adopts the following technical scheme.
An electrochemical analysis sensitivity self-adjusting method suitable for on-site rapid detection comprises a constant potential circuit and a mobile terminal for analyzing current data obtained by detection;
the circuit composition of the constant potential circuit comprises an MCU (microprogrammed control unit) module for controlling a digital potentiometer chip, and further comprises a voltage follower module, an analog-digital conversion module, a digital-analog conversion module, an electrode interface module, a low-pass filter module, a TIA (three-dimensional interactive application) transimpedance amplifier module, an internal zero module, a reference voltage source module, a Bluetooth module and a digital potentiometer module; during electrochemical detection, a constant potential circuit applies voltage waveform excitation to a substance to be detected, and response current of the substance to be detected is sampled by an analog-to-digital conversion module for analysis; the constant potential circuit comprises a programmable control digital potentiometer chip;
the digital potentiometer chip is used for adjusting the resistance of a feedback loop when the electrochemical analysis sensitivity is automatically adjusted; when the mobile terminal judges that the current data measured in the detection process is not matched with the current sensitivity of the constant potential circuit, the digital potentiometer chip automatically adjusts the resistance value of the potentiometer to change the resistance value of the response current feedback circuit, so that the current analysis sensitivity of the constant potential circuit is matched with the current electrochemical detection.
The mobile terminal is provided with an electrochemical detection APP; when the constant potential circuit carries out electrochemical detection, the constant potential circuit sends real-time current data obtained by detection to an electrochemical detection APP, and the real-time current data are stored in a current data list mode in the mobile terminal.
In the self-adjusting method, the method for judging the overhigh sensitivity of current analysis and automatically adjusting the current analysis specifically comprises the following steps: an integer variable A is designed in a current analysis sensitivity abnormity capture code of an electrochemical detection APP, in the electrochemical detection process, the integer variable A is the sum of the number of current data with the absolute value of the current data in a current data list being more than or equal to the upper limit value of the current detection range, when the numerical value of the integer variable A is more than or equal to a preset threshold B, the electrochemical detection APP judges that an abnormal behavior with overhigh current analysis sensitivity occurs in the detection process, a constant potential circuit automatically reduces the resistance value of a response current return circuit and restarts the detection, so that the current analysis sensitivity of the constant potential circuit is matched with the current electrochemical detection.
In the self-adjusting method, the automatic adjusting method with too low sensitivity to current analysis comprises the following steps: when single electrochemical detection is finished, subtracting the current maximum value and the current minimum value in the current data list to obtain a maximum and minimum current difference value; comparing the maximum and minimum current difference with the current detection range limit value, if the difference between the maximum current and the minimum current is less than or equal to half of the current detection range limit value, judging that an abnormal phenomenon that the current analysis sensitivity is too low occurs in the detection process by the electrochemical detection APP, automatically increasing the resistance value of the response current return circuit by the constant potential circuit, and restarting the detection to enable the current analysis sensitivity of the constant potential circuit to be matched with the current electrochemical detection.
When the resistance value of the response current return circuit is automatically adjusted through the digital potentiometer chip, the adjustment range of the resistance value is 100 omega-100 k omega, and the adjustment range of the resistance value is 10% of the current digital potentiometer resistance output value each time.
The mobile terminal is provided with an electrochemical detection APP; the functions of the electrochemical detection APP comprise detection parameter setting, detection state control and real-time detection voltammogram drawing of cyclic voltammetry.
The digital potentiometer chip is connected with the mobile terminal in a Bluetooth mode; the constant potential circuit comprises an MCU (microprogrammed control unit) module used for a digital potentiometer chip, and further comprises a voltage follower module, an analog-to-digital conversion module, a digital-to-analog conversion module, an electrode interface module, a low-pass filter module, a TIA (three-dimensional interactive application) transimpedance amplifier module, an internal zero module, a reference voltage source module, a Bluetooth module and a digital potentiometer module.
The MCU microcontroller module is STM32F103RCT 6; the voltage follower module is AD 8608; the analog-to-digital conversion module is AD 7694; the digital-to-analog conversion module is AD 5541; the internal zero module is ADR 4520; the reference voltage source module is ADR 4540; the Bluetooth module is HC-05; the digital potentiometer module is AD 5270.
The electrochemical detection is based on the oxidation-reduction reaction of substances, in the detection, a specific voltage excitation waveform is applied to an aqueous solution containing the substances to be detected through an electrochemical three-electrode system, so that the substances to be detected generate a response current through the oxidation-reduction reaction of electrons obtained and lost on the surface of an electrode, the generated response current flows through a response current return circuit formed by a counter electrode and a working electrode, the response current return circuit is connected with a current feedback resistor of a digital potentiometer, the digital potentiometer can change the resistance value of the response current return circuit through adjusting an output resistance value, the current analysis sensitivity of a constant potential circuit is automatically matched with the current electrochemical detection, and the constant potential circuit can quantitatively judge the concentration of the substances to be detected through analyzing the response current value.
According to the scheme, the current analysis sensitivity can be automatically adjusted aiming at abnormal detection behaviors of over-high current analysis sensitivity and over-low current analysis sensitivity in the electrochemical detection process, whether the current analysis sensitivity state is normal or not is judged in real time in the electrochemical detection process, and the scheme has the corresponding code and function of capturing current analysis sensitivity abnormality. After the current analysis sensitivity is captured to be abnormal, the scheme automatically adjusts the resistance value of the current feedback resistor of the digital potentiometer correspondingly, automatically matches the optimal current analysis sensitivity for electrochemical detection, and improves the accuracy of the electrochemical detection.
Compared with the traditional technology, the digital potentiometer module on the constant potential circuit can automatically realize the self-adjustment of the current analysis sensitivity through an automatic scheme (such as programmable firmware), and improves the precision of current detection and the accuracy of electrochemical detection. Compared with an electrochemical detection device which needs manual current analysis sensitivity adjustment, the device avoids the complex flow of manual operation and improves the automation degree during electrochemical detection; compared with an electrochemical detection device with only single current analysis sensitivity, the device has the advantage of self-adjustment of the current analysis sensitivity, and the current detection precision and the current detection sensitivity are greatly improved. The device and the method are extremely suitable for the electrochemical analysis requirement in the field of on-site rapid detection (such as various POCT (Point-of-care testing) devices based on electrochemical methods).
Drawings
The invention is described in further detail below with reference to the following figures and detailed description:
FIG. 1 is a schematic flow chart of the operation of the present invention;
FIG. 2 is a schematic diagram of the working principle of the present invention;
FIG. 3 is a schematic diagram of the sensitivity auto-adjustment of the present invention;
fig. 4 is a schematic diagram of a portion of the circuit of the present invention.
Detailed Description
As shown in the figure, the self-regulation method of the electrochemical analysis sensitivity suitable for the on-site rapid detection comprises a constant potential circuit and a mobile terminal for analyzing current data obtained by detection; the circuit composition of the constant potential circuit comprises an MCU (microprogrammed control unit) module for controlling a digital potentiometer chip, and further comprises a voltage follower module, an analog-digital conversion module, a digital-analog conversion module, an electrode interface module, a low-pass filter module, a TIA (three-dimensional interactive application) transimpedance amplifier module, an internal zero module, a reference voltage source module, a Bluetooth module and a digital potentiometer module; during electrochemical detection, a constant potential circuit applies voltage waveform excitation to a substance to be detected, and response current of the substance to be detected is sampled by an analog-to-digital conversion module for analysis; the constant potential circuit comprises a programmable control digital potentiometer chip; the digital potentiometer chip is used for adjusting the resistance of a feedback loop when the electrochemical analysis sensitivity is automatically adjusted; when the mobile terminal judges that the current data measured in the detection process is not matched with the current sensitivity of the constant potential circuit, the digital potentiometer chip automatically adjusts the resistance value of the potentiometer to change the resistance value of the response current feedback circuit, so that the current analysis sensitivity of the constant potential circuit is matched with the current electrochemical detection.
The mobile terminal is provided with an electrochemical detection APP; when the constant potential circuit carries out electrochemical detection, the constant potential circuit sends real-time current data obtained by detection to an electrochemical detection APP, and the real-time current data are stored in a current data list mode in the mobile terminal.
In the self-adjusting method, the method for judging the overhigh sensitivity of current analysis and automatically adjusting the current analysis specifically comprises the following steps: an integer variable A is designed in a current analysis sensitivity abnormity capture code of an electrochemical detection APP, in the electrochemical detection process, the integer variable A is the sum of the number of current data with the absolute value of the current data in a current data list being more than or equal to the upper limit value of the current detection range, when the numerical value of the integer variable A is more than or equal to a preset threshold B, the electrochemical detection APP judges that an abnormal behavior with overhigh current analysis sensitivity occurs in the detection process, a constant potential circuit automatically reduces the resistance value of a response current return circuit and restarts the detection, so that the current analysis sensitivity of the constant potential circuit is matched with the current electrochemical detection.
The preset threshold value B is an integer of 20,
in the self-adjusting method, the automatic adjusting method with too low sensitivity to current analysis comprises the following steps: when single electrochemical detection is finished, subtracting the current maximum value and the current minimum value in the current data list to obtain a maximum and minimum current difference value; comparing the maximum and minimum current difference with the current detection range limit value, if the difference between the maximum current and the minimum current is less than or equal to half of the current detection range limit value, judging that an abnormal phenomenon that the current analysis sensitivity is too low occurs in the detection process by the electrochemical detection APP, automatically increasing the resistance value of the response current return circuit by the constant potential circuit, and restarting the detection to enable the current analysis sensitivity of the constant potential circuit to be matched with the current electrochemical detection.
When the resistance value of the response current feedback circuit is automatically adjusted through the digital potentiometer chip, the adjustment range of the resistance value is 100-100 k omega, and the adjustment range of the resistance is 10% of the current digital potentiometer resistance output value each time;
when the total output resistance range of the potentiometer is within 100 kilohms and the resolution of the output resistance is 10 bits, a method of multiple self-adjustment is adopted when the resistance value of the current feedback resistor of the potentiometer is adjusted, and the method specifically comprises the following steps:
if the current output resistance value range of the potentiometer is 10-100K omega, the resistance adjustment value is 10K omega when the potentiometer is adjusted each time;
if the current output resistance value range of the potentiometer is between 1 and 10K omega, the resistance adjustment value is 1K omega when the potentiometer is adjusted each time;
and if the current output resistance value range of the potentiometer is between 100 and 1000 omega, the resistance adjustment value is 100 omega when the potentiometer is adjusted each time.
The mobile terminal is provided with an electrochemical detection APP; the functions of the electrochemical detection APP comprise detection parameter setting, detection state control and real-time detection voltammogram drawing of cyclic voltammetry.
The digital potentiometer chip is connected with the mobile terminal in a Bluetooth mode; the constant potential circuit comprises an MCU (microprogrammed control unit) module used for a digital potentiometer chip, and further comprises a voltage follower module, an analog-to-digital conversion module, a digital-to-analog conversion module, an electrode interface module, a low-pass filter module, a TIA (three-dimensional interactive application) transimpedance amplifier module, an internal zero module, a reference voltage source module, a Bluetooth module and a digital potentiometer module.
The MCU microcontroller module is STM32F103RCT 6; the voltage follower module is AD 8608; the analog-to-digital conversion module is AD 7694; the digital-to-analog conversion module is AD 5541; the internal zero module is ADR 4520; the reference voltage source module is ADR 4540; the Bluetooth module is HC-05; the digital potentiometer module is AD 5270.
The electrochemical detection is based on the oxidation-reduction reaction of substances, in the detection, a specific voltage excitation waveform is applied to an aqueous solution containing the substances to be detected through an electrochemical three-electrode system, so that the substances to be detected generate a response current through the oxidation-reduction reaction of electrons obtained and lost on the surface of an electrode, the generated response current flows through a response current return circuit formed by a counter electrode and a working electrode, the response current return circuit is connected with a current feedback resistor of a digital potentiometer, the digital potentiometer can change the resistance value of the response current return circuit through adjusting an output resistance value, the current analysis sensitivity of a constant potential circuit is automatically matched with the current electrochemical detection, and the constant potential circuit can quantitatively judge the concentration of the substances to be detected through analyzing the response current value.
Example (b):
in the embodiment, a smart phone is used as a mobile terminal, when electrochemical detection and analysis are performed, a constant potential circuit part in the device is powered on first, and initialization operation is automatically performed after the constant potential circuit is powered on.
The method comprises the steps of opening an electrochemical detection APP installed on a mobile terminal, entering a parameter setting interface of a cyclic voltammetry method after the electrochemical detection APP is opened, and setting parameters such as an upper limit potential, a lower limit potential, a voltage scanning rate and a detection period number of the cyclic voltammetry method on the parameter setting interface.
Before the detection is opened to the official form, at first should accomplish the bluetooth connection of electrochemistry detection APP and constant potential circuit, the bluetooth is connected after successfully, click and begin to detect the button, electrochemistry APP just sends through the wireless mode of bluetooth and opens the detection instruction to the constant potential circuit, the constant potential circuit opens the detection this moment, the constant potential circuit applys specific voltage excitation waveform to the material that awaits measuring, and real-time sampling and conversion to response current, current data passes through the real-time transmission of bluetooth to electrochemistry APP, and real-time volt-ampere curve of drawing on electrochemistry APP's the detection interface, when electrochemistry APP draws volt-ampere curve, APP also monitors current analysis sensitivity state.
In the traditional technology, during electrochemical detection, if the sensitivity of current analysis is too high, the over-range problem of current detection is easy to occur in the electrochemical detection, which is represented as the peak clipping phenomenon of a detected volt-ampere result diagram; when the current analysis sensitivity is too low, the phenomenon that the voltammetry result graph is short and flat appears is shown, and the two voltammetry curve graphs are not beneficial to the observation of the detection result.
In the device of the embodiment, once the abnormal detection behavior of the response current analysis sensitivity is monitored, the APP automatically restarts the detection immediately, and the current analysis sensitivity is automatically adjusted by reconfiguring the resistance value of the current feedback resistor of the digital potential chip on the circuit through a program while restarting the detection, so that the optimal current analysis sensitivity is automatically matched for the electrochemical detection.
In this case, the purpose of the automatic adjustment of the sensitivity of the amperometric circuit is to adjust the magnitude of the response current of the substance to be measured received by the potentiostatic circuit analytical circuit so that it can be matched with the sensitivity of the analytical circuit.
Claims (7)
1. An electrochemical analysis sensitivity self-adjusting method suitable for on-site rapid detection is characterized in that: the self-adjusting method comprises a constant potential circuit and a mobile terminal for analyzing current data obtained by detection;
the circuit composition of the constant potential circuit comprises an MCU (microprogrammed control unit) module for controlling a digital potentiometer chip, and further comprises a voltage follower module, an analog-digital conversion module, a digital-analog conversion module, an electrode interface module, a low-pass filter module, a TIA (three-dimensional interactive application) transimpedance amplifier module, an internal zero module, a reference voltage source module, a Bluetooth module and a digital potentiometer module; during electrochemical detection, a constant potential circuit applies voltage waveform excitation to a substance to be detected, and response current of the substance to be detected is sampled by an analog-to-digital conversion module for analysis; the constant potential circuit comprises a programmable control digital potentiometer chip;
the digital potentiometer chip is used for adjusting the resistance of a feedback loop when the electrochemical analysis sensitivity is automatically adjusted; when the mobile terminal judges that the current data measured in the detection process is not matched with the current sensitivity of the constant potential circuit, the digital potentiometer chip automatically adjusts the resistance value of the potentiometer to change the resistance value of the response current feedback circuit, so that the current analysis sensitivity of the constant potential circuit is matched with the current electrochemical detection.
2. The self-regulating method of electrochemical analysis sensitivity suitable for rapid in-situ detection according to claim 1, wherein: the mobile terminal is provided with an electrochemical detection APP; when the constant potential circuit carries out electrochemical detection, the constant potential circuit sends real-time current data obtained by detection to an electrochemical detection APP, and the real-time current data are stored in a current data list mode in the mobile terminal.
3. The self-adjusting method for the sensitivity of electrochemical analysis suitable for rapid in situ detection according to claim 2, wherein: in the self-adjusting method, the method for judging the overhigh sensitivity of current analysis and automatically adjusting the current analysis specifically comprises the following steps: an integer variable A is designed in a current analysis sensitivity abnormity capture code of an electrochemical detection APP, in the electrochemical detection process, the integer variable A is the sum of the number of current data with the absolute value of the current data in a current data list being more than or equal to the upper limit value of the current detection range, when the numerical value of the integer variable A is more than or equal to a preset threshold B, the electrochemical detection APP judges that an abnormal behavior with overhigh current analysis sensitivity occurs in the detection process, a constant potential circuit automatically reduces the resistance value of a response current return circuit and restarts the detection, so that the current analysis sensitivity of the constant potential circuit is matched with the current electrochemical detection.
4. The self-adjusting method for the sensitivity of electrochemical analysis suitable for rapid in situ detection according to claim 2, wherein: in the self-adjusting method, the automatic adjusting method with too low sensitivity to current analysis comprises the following steps: when single electrochemical detection is finished, subtracting the current maximum value and the current minimum value in the current data list to obtain a maximum and minimum current difference value; comparing the maximum and minimum current difference with the current detection range limit value, if the difference between the maximum current and the minimum current is less than or equal to half of the current detection range limit value, judging that an abnormal phenomenon that the current analysis sensitivity is too low occurs in the detection process by the electrochemical detection APP, automatically increasing the resistance value of the response current return circuit by the constant potential circuit, and restarting the detection to enable the current analysis sensitivity of the constant potential circuit to be matched with the current electrochemical detection.
5. The self-regulating method of electrochemical analysis sensitivity suitable for rapid in-situ detection according to claim 3 or 4, wherein: when the resistance value of the response current return circuit is automatically adjusted through the digital potentiometer chip, the adjustment range of the resistance value is 100 omega-100 k omega, and the adjustment range of the resistance value is 10% of the current digital potentiometer resistance output value each time.
6. The self-regulating method of electrochemical analysis sensitivity suitable for rapid in-situ detection according to claim 1, wherein: the mobile terminal is provided with an electrochemical detection APP; the functions of the electrochemical detection APP comprise detection parameter setting, detection state control and real-time detection voltammogram drawing of cyclic voltammetry.
7. The self-regulating method of electrochemical analysis sensitivity suitable for rapid in-situ detection according to claim 1, wherein: the electrochemical detection is based on the oxidation-reduction reaction of substances, in the detection, a specific voltage excitation waveform is applied to an aqueous solution containing the substances to be detected through an electrochemical three-electrode system, so that the substances to be detected generate a response current through the oxidation-reduction reaction of electrons obtained and lost on the surface of an electrode, the generated response current flows through a response current return circuit formed by a counter electrode and a working electrode, the response current return circuit is connected with a current feedback resistor of a digital potentiometer, the digital potentiometer can change the resistance value of the response current return circuit through adjusting an output resistance value, the current analysis sensitivity of a constant potential circuit is automatically matched with the current electrochemical detection, and the constant potential circuit can quantitatively judge the concentration of the substances to be detected through analyzing the response current value.
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