CN110133089B - Automatic internal calibration system and calibration method for electrochemical sensor - Google Patents
Automatic internal calibration system and calibration method for electrochemical sensor Download PDFInfo
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- CN110133089B CN110133089B CN201910471915.3A CN201910471915A CN110133089B CN 110133089 B CN110133089 B CN 110133089B CN 201910471915 A CN201910471915 A CN 201910471915A CN 110133089 B CN110133089 B CN 110133089B
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Abstract
The invention provides an automatic internal calibration system of an electrochemical sensor, which comprises: the device comprises a microprocessor, a sensor module, a reference module, a voltage excitation circuit, an amplifying circuit, a digital-to-analog converter and an analog-to-digital converter, wherein the microprocessor is connected with the digital-to-analog converter and the analog-to-digital converter; the reference module is used as a built-in calibration module and is consistent with the sensor module connecting circuit; the invention also relates to an automatic internal calibration method of the electrochemical sensor. The automatic internal calibration system of the electrochemical sensor realizes automatic judgment and intelligent automatic internal calibration of the automatic judgment; the calibration can be carried out while working, the sensor does not need to be placed in an external standard detected substance, the calibration range is wide, and the calibration accuracy is higher.
Description
Technical Field
The invention relates to an automatic internal calibration system of an electrochemical sensor and also relates to an automatic internal calibration method of the electrochemical sensor.
Background
An electrochemical sensor is a sensor commonly used in research work and daily life, and is generally used for measuring the electrical and electrochemical properties of a target molecule or substance so as to perform qualitative and quantitative analysis and measurement.
The basic elements of a typical electrochemical sensor are: a working (or sensing) electrode, a counter electrode, and typically a reference electrode. The electrodes are attached within the sensor, lined with an electrolyte. The electrode is located on the inner face of a diffusion membrane and has a plurality of pores through which the detection substance passes but is impermeable to the electrolyte. After the substance to be measured diffuses into the sensor and passes through the membrane to the electrodes, an electrochemical reaction takes place-either oxidation or reduction, depending on the type of substance. The oxidation reaction causes electrons to flow from the working electrode to the counter electrode through an external circuit; in contrast, the reduction reaction causes electrons to flow from the counter electrode to the working electrode. The electron flow constitutes an electric current and is proportional to the gas concentration. The sensor module and the circuit in the instrument detect and amplify the current, and finally realize the measurement of the category and the concentration of the object to be measured and output the result.
The electrochemical sensor has small volume, high detection speed and low cost, is suitable for the application scenes of direct field detection and continuous detection, and is widely applied to the fields of gas detection, water quality detection, biological detection and the like. However, since the electrochemical sensor detects by directly contacting with the substance to be detected, the sensor often absorbs the pollutants and remains on the diffusion film during the use of the sensor, even on the electrode, the pollutants can reduce the area of the electrode and affect the diffusion channel of the substance to be detected; on the other hand, evaporation and contamination of the electrode material also affect the sensor performance. In practical applications, the detection result of the electrochemical sensor is accurate and stable in the initial stage of use, but after the use period, the data becomes uncontrollable, and the detection data can be greatly deviated and even fail.
In response to this electrochemical sensor limitation, current general technical solutions include: replacing the sensor; manually setting an offset for correction according to empirical data; and (4) manually calibrating, namely setting the sensor in a standard detected substance environment and correcting the output value of the sensor. However, the above technical solutions have the following limitations: replacing the sensor increases the cost and causes inconvenience; the method needs manual intervention, and can not accurately judge the data deviation in time and even fail, so that misjudgment and misjudgment are caused, and even irreparable loss is caused.
Patent CN201 cite 0291057.7 discloses an automatic calibration system for gas sensor and a calibration method for gas sensor thereof, in which the sensor is disposed in an environment of a measured substance with specific external concentration, and the sensor is calibrated only by referring to the collected characteristic values of a single point or a limited number of points, which is inefficient, has limited calibration effect, and cannot be used as a precise and simple calibration method.
Disclosure of Invention
Aiming at the problems, the invention provides an automatic internal calibration system of an electrochemical sensor and also relates to an automatic internal calibration method of the electrochemical sensor.
The invention provides an automatic internal calibration system of an electrochemical sensor, which comprises:
the microprocessor: the device is provided with an AD interface and a DA interface, wherein the DA interface outputs an analog signal, and the AD interface acquires data;
the microprocessor is connected with the digital-to-analog converter and the analog-to-digital converter, the digital-to-analog converter is connected with the voltage exciting circuit, the voltage exciting circuit is connected with a counter electrode of the sensor module, the analog-to-digital converter is connected with the amplifying circuit, and the amplifying circuit is connected with a working electrode of the sensor module;
the microprocessor is connected with the digital-to-analog converter and the analog-to-digital converter, the digital-to-analog converter is connected with the voltage exciting circuit, the voltage exciting circuit is connected with the reference module counter electrode, the analog-to-digital converter is connected with the amplifying circuit, and the amplifying circuit is connected with the reference module working electrode.
Further, the reference module is one of redundant electrodes, equivalent circuits and a module form with unchanged intrinsic parameters.
Further, the reference module is stored in a closed mode and is not in contact with the outside, and the electrochemical properties are kept stable and unchanged.
Further, the reference module and the sensing module have consistent performance or have errors within an acceptable range in the initial state.
Furthermore, the parameters and the models of the amplifying circuit, the digital-to-analog converter and the analog-to-digital converter are consistent, and the circuit connection modes are consistent.
Furthermore, the microprocessor is internally provided with a calibration algorithm which is used for comparing the data difference between the sensor module and the reference module and the corresponding excitation waveform data, calculating a calibration factor, and correcting the data output by the sensor module by using the calibration factor to enable the data output by the sensor module to approach the data output by the reference module until the data difference between the two is controlled within a specific acceptable range.
The invention provides an automatic internal calibration method of an electrochemical sensor, which comprises the following steps:
(1) the microprocessor outputs a quantized data sequence of a specific voltage waveform, the quantized data sequence is converted into the specific voltage waveform through the digital-to-analog converter, the voltage waveform is applied to the counter electrode of the sensor module through the voltage excitation circuit to form voltage excitation on the sensor module, the waveform of the voltage excitation is generated by programming control of the microprocessor, signals are output by the working electrode of the sensor module, and output data are acquired by the microprocessor through the amplifying circuit and the analog-to-digital converter;
(2) the microprocessor outputs a quantized data sequence of a specific voltage waveform, the quantized data sequence is converted into the specific voltage waveform through the digital-to-analog converter, the voltage waveform is applied to the reference module counter electrode through the voltage excitation circuit, voltage excitation on the reference module is formed, and the waveform of the voltage excitation is generated by programming control of the microprocessor. The working electrode of the reference module outputs signals, and the microprocessor acquires output data through the amplifying circuit and the analog-to-digital converter;
(3) and calculating and processing a calibration factor according to different excitation voltage waveforms and comparing the output data difference between the sensor module and the reference module by an analysis algorithm preset in the microprocessor, correcting according to the data of the reference module, circulating the steps, and applying different voltage waveform modes until the deviation between the data acquired by the sensor module and the data acquired by the reference module is controlled within a certain range, thereby realizing automatic calibration.
In the initial state, the same voltage waveform excitation is applied to the sensor and the calibration module, and the output data of the sensor is the same as that of the calibration module due to the consistent characteristics of the sensor and the calibration module in the initial state. When the sensor characteristics are changed, the reference module maintains the inherent characteristics in the sensor, and the characteristics of the two modules are different. When the calibration process is started, the microprocessor controls the sensors and the calibration module to be respectively excited by the same voltage waveform, and the output data of the sensors and the calibration module form a certain difference. The invention utilizes the difference value between the sensor and the calibration module to correct, thereby realizing automatic calibration.
The invention has the beneficial effects that:
(1) the automatic internal calibration method of the electrochemical sensor disclosed by the invention autonomously judges the data accuracy and effectiveness of the sensor and autonomously triggers the sensor to realize intelligent and automatic calibration without manual intervention;
(2) the automatic internal calibration method of the electrochemical sensor disclosed by the invention has the advantages that the calibration mode is inserted at intervals of sensor data detection, the operation is carried out while the calibration is carried out, and the operation of the sensor is not required to be interrupted;
(3) the automatic internal calibration system of the electrochemical sensor disclosed by the invention is internally provided with the calibration reference module in the sensor, and internal self-calibration can be completed without placing the sensor in an external standard detected substance;
(4) the automatic internal calibration method of the electrochemical sensor disclosed by the invention has the advantages of wide calibration range and higher calibration accuracy, and is not limited by the numerical correction calibration of a plurality of characteristic points.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, 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 of an automatic internal calibration system for an electrochemical sensor in an embodiment of the present invention;
FIG. 2 is a schematic diagram of a gas sensor electrode structure with redundant electrodes as calibration reference modules according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of an electrode structure of a sensor module according to an embodiment of the present invention;
FIG. 4 is a schematic diagram of an automatic internal calibration system for a standard electrode of a sensor and a redundant electrode of a reference module according to an embodiment of the present invention;
FIG. 5 is a flow chart of a process for calibrating a gas sensor system having redundant electrodes as calibration reference modules in an embodiment of the present invention;
FIG. 6 is a schematic diagram of an electrode structure of a gas sensor with an equivalent circuit as a calibration reference module according to an embodiment of the present invention;
FIG. 7 is a schematic structural diagram of an automatic internal calibration system of an equivalent circuit of a sensor standard electrode and a reference module according to an embodiment of the present invention.
Detailed Description
The technical solution of the present invention is further described in detail by the following embodiments.
Example 1:
the formaldehyde gas sensor with the redundant electrode as a calibration standard module and the automatic internal calibration system are as follows:
as shown in fig. 3, the gas sensor includes a substrate, an electrolyte, an electrode plate, a diffusion membrane, a case, and a gas permeable hole.
As shown in fig. 2, the gas sensor electrode plate includes a standard electrode and a redundant electrode. The electrode patterns, the electrode manufacturing process and the electrode catalyst modification process of the two are completely the same. The electrolyte and the diffusion membrane of the standard electrode and the redundant electrode are made of the same materials and processes. The difference between the standard electrode and the redundant electrode is that the shell above the standard electrode is provided with air holes, the shell above the redundant electrode part is not provided with air holes, and the redundant electrode part can be considered to be completely sealed and isolated from the outside.
Since the standard electrode and the redundant electrode are made of the same material and are processed in parallel, the characteristics of the standard electrode and the redundant electrode are basically consistent or within a certain acceptable range in the initial state. And the performance of the sensor at the middle and later stages can be maintained stably and unchanged due to the sealing state of the redundant electrode.
As shown in fig. 4, the standard electrode and the redundant electrode are respectively provided with an independent set of voltage input excitation and output amplification data acquisition circuit, and the two sets of circuits are designed and have consistent parameters. A microprocessor with AD and DA interfaces, such as STM32F051K6U6, with high integration level at the same time can be selected. The DA outputs an analog signal, and the analog signal applies voltage excitation to a reference electrode and a counter electrode of the sensor through an operational amplifier. And after the output of the working electrode is subjected to precise operational amplification and secondary amplification, AD sampling is carried out, and the output numerical value of the working electrode of the sensor is collected.
The voltage excitation signal is generated into a waveform quantization sequence by a microprocessor program, and the generated waveform can be a waveform sequence of various frequencies, such as sine waveform, triangular waveform, square waveform, pulse and the like.
Embodiments also include calibration algorithms. The calibration algorithm is preset in a microprocessor operation program, the generation of the excitation waveform of the sensor is controlled, the data after the output amplification of the sensor is collected, the calibration algorithm compares the difference of the output data of the sensor module and the reference module with the corresponding excitation waveform data, a calibration factor is calculated, the output data of the sensor module is corrected by utilizing the calibration factor to be close to the output data of the reference module until the data difference between the two is controlled within a specific acceptable range.
The process of calibrating the sensor system for the parameter characteristics of the formaldehyde gas sensor of this embodiment is shown in fig. 5. And the calibration calls the data acquisition sub-process in sequence, and the acquisition excitation frequencies can be set to be 10khz, 9khz, 8khz to 1khz, 900hz, 800hz to 100hz, 10hz, 9hz to 0.1hz, 0.5hz and 0.1hz in sequence. After the data acquisition of each frequency point is completed, the calibration algorithm 1 analyzes the data acquired by the sensor module and the reference module respectively, and calculates and stores corresponding single acquisition parameters. After the data acquisition of all the frequency points is completed, the calibration algorithm 2 comprehensively analyzes the acquisition parameters of all the frequency points, compares the analysis result difference of the sensor module and the reference module to generate a calibration factor, substitutes the calibration factor into the data acquisition algorithm of the sensor module, and corrects the data acquisition algorithm. And repeating the processes to generate a final calibration factor, so that the difference of the analysis parameters of the acquired data of the sensor module and the reference module is within an acceptable range, and the calibration process is finished.
Example 2:
the electrochemical sensor automatic internal calibration system with the equivalent circuit as a calibration reference module comprises:
as shown in fig. 6, the present embodiment uses the equivalent circuit model as a reference module. The internal structure of the electrochemical sensor is unchanged, and when the sensor is in an initial state, a data acquisition process is started to acquire output data of each frequency point. The equivalent circuit algorithm calculates an equivalent circuit model according to the output data of each frequency point, and the equivalent circuit parameters are solidified into a reference module circuit through an adjustable resistor, a capacitor and an inductor and are fixed through physical means without changing.
After the sensor module is used for a period of time, parameters change, the reference module consisting of the equivalent circuit does not change, and the acquisition parameter difference of the sensor module and the reference module is compared through a calibration algorithm to generate a calibration factor. The specific calibration algorithm is as in example 1.
As a supplement to the embodiment 1, the analog-to-digital conversion or the digital-to-analog conversion may adopt a scheme of separating devices of an independent microprocessor, and is specially processed by an independent analog-to-digital conversion chip or a digital-to-analog conversion chip, and the microprocessor mainly completes the work of overall process control, data analysis, calibration, and the like, as shown in fig. 7.
Those skilled in the art will appreciate that the figures are merely schematic representations of one preferred implementation scenario and that the blocks or flow diagrams in the figures are not necessarily required to practice the present invention.
It should be understood that the above-mentioned embodiments are only examples of the present invention, and are not intended to limit the present invention, and any modifications, equivalent substitutions, improvements, etc. made within the spirit of the present invention should be included in the protection scope of the present invention, and the protection scope of the present invention should be subject to the protection scope defined by the claims.
Claims (9)
1. A method for automatic internal calibration of an automatic internal calibration system for an electrochemical sensor, wherein the automatic internal calibration system for an electrochemical sensor comprises:
the microprocessor: the device comprises an AD interface and a DA interface, wherein the DA interface outputs analog signals, and the AD interface acquires data;
treat calibration sensor module system: the microprocessor is connected with the digital-to-analog converter and the analog-to-digital converter, the digital-to-analog converter is connected with the voltage exciting circuit, the voltage exciting circuit is connected with a counter electrode of the sensor module, the analog-to-digital converter is connected with the amplifying circuit, and the amplifying circuit is connected with a working electrode of the sensor module;
a reference module system: the microprocessor is connected with the digital-to-analog converter and the analog-to-digital converter, the digital-to-analog converter is connected with the voltage exciting circuit, the voltage exciting circuit is connected with the counter electrode of the reference module, the analog-to-digital converter is connected with the amplifying circuit, and the amplifying circuit is connected with the working electrode of the reference module; the automatic internal calibration method of the automatic internal calibration system is characterized by comprising the following steps:
s1: the microprocessor outputs a quantized data sequence of a specific voltage waveform, the quantized data sequence is converted into the specific voltage waveform through the digital-to-analog converter, the voltage waveform is applied to the counter electrode of the sensor module through the voltage excitation circuit to form voltage excitation on the sensor module, the waveform of the voltage excitation is generated by programming control of the microprocessor, signals are output by the working electrode of the sensor module, and output data are acquired by the microprocessor through the amplifying circuit and the analog-to-digital converter;
s2: the microprocessor outputs a quantized data sequence of a specific voltage waveform, the quantized data sequence is converted into a specific voltage waveform through the digital-to-analog converter, the voltage waveform is applied to the reference module counter electrode through the voltage excitation circuit to form voltage excitation on the reference module, the waveform of the voltage excitation is generated by programming control of the microprocessor, signals are output by the reference module working electrode, and output data are acquired by the microprocessor through the amplifying circuit and the analog-to-digital converter;
s3: and calculating and processing a calibration factor according to different excitation voltage waveforms and comparing the output data difference between the sensor module and the reference module by an analysis algorithm preset in the microprocessor, correcting according to the data of the reference module, circulating the steps, and applying different voltage waveform modes until the deviation between the data acquired by the sensor module and the data acquired by the reference module is controlled within a certain range, thereby realizing automatic calibration.
2. The automatic internal calibration method of an automatic internal calibration system of an electrochemical sensor according to claim 1, wherein the reference module is one of a redundant electrode, an equivalent circuit, and a module configuration in which intrinsic parameters are not changed.
3. The automatic internal calibration method of an automatic internal calibration system of an electrochemical sensor according to claim 2, wherein the reference module is a redundant electrode, and the redundant electrode is identical to the sensor module electrode in electrode pattern, electrode manufacturing process and electrode catalyst modification process, and the material and process of electrolyte and diffusion film are identical.
4. The automatic internal calibration method of an automatic internal calibration system of an electrochemical sensor according to claim 2, wherein the reference module is an equivalent circuit, the initial state data of the sensor module is collected, an equivalent circuit model is calculated, and the equivalent circuit model is solidified into the reference module circuit recently through adjustable resistance, capacitance and inductance and is fixed through physical means.
5. The method for automatic internal calibration of an automatic internal calibration system of an electrochemical sensor according to claim 2, wherein the reference module is stored in a closed state without contact with the outside and the electrochemical characteristics are maintained.
6. The method for automatic internal calibration of an automatic internal calibration system of an electrochemical sensor according to any one of claims 1 to 5, wherein the reference module and the sensing module have the same performance or the error is within an acceptable range in the initial state.
7. The automatic internal calibration method of an automatic internal calibration system of an electrochemical sensor according to claim 1, wherein the parameters of the voltage excitation circuit, the amplifying circuit, the digital-to-analog converter and the analog-to-digital converter used by the sensor module system to be calibrated and the reference module system are consistent with the model and the circuit connection mode.
8. The method of claim 1, wherein the microprocessor is configured with a calibration algorithm for comparing the difference between the output data of the sensor module and the output data of the reference module and the corresponding excitation waveform data, calculating a calibration factor, and using the calibration factor to correct the output data of the sensor module to approach the output data of the reference module until the difference between the two data is controlled within a specific acceptable range.
9. The automatic internal calibration method of an automatic internal calibration system of an electrochemical sensor according to claim 1, wherein the microprocessor outputs a quantized data sequence of a specific voltage waveform, which may be at least one of a sine waveform, a triangle waveform, and a square waveform.
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| TWI502195B (en) * | 2009-03-10 | 2015-10-01 | Senova Systems Inc | Multi-phase analyte insensitive electrode for use in an electrochemical sensing device for measuring an analyte in a sample , electrochemical sensing device comprising the electrode and method of measuring an analyte in a sample using the electrochemical |
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