CN112255299B - Method and device for measuring ethylene concentration in fruit sample - Google Patents
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Abstract
The invention relates to the technical field of biological sampling analysis, in particular to a method for determining ethylene concentration in a fruit sample, which comprises the steps of converting an ethylene concentration signal in gas released by a fruit into a current signal, adjusting and amplifying the current signal, changing the color of an electrochromic material, and judging the maturity of the fruit through the color change of a detection device; the invention also relates to an ethylene concentration detector, which consists of a gas transmission system, a detection system and a display system which are arranged in the shell, and has simple and reliable structure and easy maintenance; the innovation point of the invention lies in that the defect that the high-temperature environment is needed for detecting the ethylene by using the mode of combining the electrochromic material and the electrochemical sensor and bypassing the catalytic luminescence technology is provided, the gas sensor based on the luminescence phenomenon can be used at normal temperature, and the alkene concentration detection method and the instrument do not need to be combined with a large-scale analytical instrument, are slightly influenced by the environment and have loose use conditions.
Description
Technical Field
The invention relates to the technical field of biological sampling analysis, in particular to a method and a device for measuring ethylene concentration in a fruit sample.
Background
Organisms release various Volatile Organic Compounds (BVCOs) during metabolism in the New City, which are terminal metabolites of biological metabolism and important biological pheromones. Analysis of BVCOs can provide reference for the study of biological metabolic processes and the change of biological information of metabolic processes. For example, during ripening of fruit, the odor characteristics of the fruit change. The maturity of the fruit not only has direct influence on the flavor, hardness, color and luster of the fruit, but also affects multiple links of picking, storing, processing, transporting and the like of the fruit. Therefore, the detection of the maturity of the fruits plays an important role in fruit grading, the optimal picking time of the fruits can be determined according to the grading of the fruits, a basis is provided for subsequent processing, the selling period of the fruits is prolonged, and the color deterioration, the hardness reduction and the nutrient loss of the fruits are prevented.
At present, methods for judging the ripeness of fruits based on the electrical characteristics of the fruits mainly comprise a coaxial probe technology, a parallel polar plate technology and a transmission line technology, but the fruit electrical characteristic detection technology is greatly influenced by temperature and humidity, and the integration level is not high, so that the method is inconvenient in practical application.
The method for judging the fruit maturity based on the optical characteristics of the fruit mainly comprises a near infrared spectrum detection technology and a spectrum imaging detection technology, but the method has the advantages of easy light scattering, complex instruments and poor anti-interference capability during testing, and limits the wide application of the method in the aspect of fruit quality detection.
Based on the color and the shape of the fruit, the ripeness of the fruit is judged by utilizing a visual detection technology of a computer, so that the method is an effective computer visual classification method. However, the computer vision system is difficult to be widely applied due to the defects of high cost, complex system structure, accuracy intersection and the like.
The method for judging the maturity of the fruit based on the acoustic characteristics of the fruit is an economic and nondestructive detection technology and is a method for analyzing and processing sound wave signals scattered and reflected. However, the technology is easily interfered by the surrounding environment, has higher requirement on the testing environment, and is difficult to be widely popularized and applied.
For the above reasons, a technology for judging the ripeness of fruit based on ethylene gas released from the fruit has attracted much attention in recent years, and among them, an intelligent electronic nose detection system, which mainly consists of signal processing, pattern recognition and a plurality of sets of gas sensors, is excellent. However, the system has complex composition, numerous integrated elements and expensive selling price of each detection instrument, so the system is not really popularized and applied in a front-line working site for fruit quality detection.
Therefore, aiming at the current situation in the field of fruit detection at present, the invention provides a mature fruit detection method which is not required to be used with a large-scale analytical instrument, is slightly influenced by the environment, has stable and reliable detection results, and simultaneously provides a detection device which is low in price and simple and reliable in structure.
Disclosure of Invention
The invention aims to provide a mature fruit detection method which is not required to be used with a large-scale analytical instrument, is slightly influenced by the environment, has stable and reliable detection results and can meet the use requirements of common related personnel.
The second purpose of the present invention is to provide a detection device which is inexpensive, simple and reliable in structure, inexpensive, and easy to maintain.
In order to meet the technical requirements, the technical scheme of the invention needs to be clarified by combining theories and experiments, and the technical content of the invention is summarized.
The detection principle of the electrochemical sensor is that a material with a specific recognition function is fixed on the surface of a substrate to form a sensitive element, and the recognition component mainly has two functions:
(1) The sensitive element and the target substance are subjected to specific reaction, and the obtained reaction parameters are converted into a conduction system to generate a sensing signal;
(2) The sensing signal is received by a transducer of the conversion system. The regulating and switching system also has two main functions: firstly, the induction signal is converted into an electric signal which can be measured, and then the obtained electric signal is output after secondary amplification processing by an electronic system and recorded by an instrument. Under a certain condition, the signal change and the concentration of the detected object form a linear relation, so that the aim of qualitatively or quantitatively analyzing the detected object is fulfilled.
The development of new gas sensors based on luminescence phenomena has been a research focus in recent years in analytical chemistry, particularly in the fields related to gas detection. The catalytic luminescence (CTL) is a luminescence phenomenon generated when an excited state product generated in the catalytic oxidation reaction process returns to a ground state, and a sensor based on the catalytic luminescence on the surface of a solid material can be constructed on the basis of the luminescence phenomenon. Although the catalytic luminescence sensor has many unique advantages, such as reversible response, good thermodynamic stability, etc., in the detection process, a better response signal is usually obtained at a higher temperature, and a high detection working temperature causes high-energy radiation in the matrix to generate background radiation, which is not beneficial for detection.
Therefore, in order to achieve the two objects of the present invention, the present invention provides a gas sensor based on luminescence phenomenon, which can be used at normal temperature, by combining an electrochromic material with an electrochemical sensor to bypass the defect of high temperature environment in the catalytic luminescence technology, and the specific technical scheme is as follows:
1. preparation of electrochemical sensor
1. Preparing a modified working electrode:
preparation of SnO 2 Matrix: with SnCl 4 ·5H 2 Adding acetic acid as a dispersing agent into the raw material O, titrating the mixture by using ammonia water until the pH value of the system is 3, and obtaining sol after oxalic acid is removed; drying and aging the sol to obtain gel, and roasting the gel at 550 ℃ for 2.5h to obtain SnO 2 A substrate.
At SnO 2 Base addition 5wt% of PdCl 2 Then coating the mixture on the surface of a gold sheet, and roasting the gold sheet at 550 ℃ for 3.5 hours to obtain the modified working electrode.
2. The counter electrode and the reference electrode were prepared from platinum sheets.
3. Phosphoric acid which has good stability and is not easy to crystallize is used as electrolyte.
2. Preparation of electrochromic materials
S1: preparing chemical bath deposition liquid: the volume percentage ratio is 5:5:1 in a ratio of 05mol of NiSO 4 ·6H 2 O、0.15molK 2 S 2 O 8 And ammonia water to prepare chemical bath deposition liquid;
s2: preparing electrophoretic deposition liquid: 1 percent of graphene oxide and 1 percent of Mg (NO) by mass 3 ) 2 ·6H 2 0, adding the mixture into isopropanol, and stirring by ultrasound and magnetic force to form stable sol as electrolyte;
s3: preparing a graphene/ITO glass substrate: taking the cleaned ITO glass plate as a working electrode, electrolyzing a platinum sheet as a counter electrode, adding an electrophoretic deposition solution, depositing for 15s under the conditions of a distance of 1cm, a voltage of 100V and a temperature of 25 ℃, and then processing for 1.5h at 280 ℃ in an argon atmosphere to obtain a graphene/ITO glass substrate;
s4: placing the graphene/ITO glass substrate in chemical bath deposition liquid, stirring for 15min at 60 ℃, and then treating for 1.5h at 280 ℃ in an argon atmosphere to obtain TiO 2 The/graphene composite electrochromic material.
3. Selection of hardware equipment of fruit ethylene detection device
The power supply of the system is a 4.2V lithium battery, and the charging interface of the system is a USB interface.
The microprocessor is MSP430 series single-chip microcomputer.
When an ethylene concentration sensor senses ethylene gas, a tiny current signal is output, the tiny current signal is amplified by an INA123 amplifier and then is sampled by a 12-bit A/D converter integrated in a single-chip microcomputer MSP430, a sampled digital signal is processed and compared by the single-chip microcomputer, a stable concentration value is found out, and the stable concentration value is stored in a data storage device to serve as a maturity contrast value.
After the maturity contrast value is collected, a current signal is transmitted, and the maturity contrast color is presented on a display system after the maturity contrast value is converted by an I/V conversion circuit and amplified by an amplifier.
4. Preparation of fruit ethylene detection device
The detection device designed by the invention consists of a gas transmission system, a detection system, a display system and a control panel which are arranged in a shell.
Furthermore, the gas transmission system comprises a gas transmission channel, the gas transmission channel comprises a gas inlet and a gas outlet and is communicated with the gas chamber, and a vacuum pump is arranged on the gas transmission channel and close to the gas outlet.
Furthermore, the detection system consists of an ethylene sensor and a control circuit; the ethylene sensor comprises a waterproof shell, a filter is arranged on the contact surface of the waterproof shell and the air chamber, a hydrophobic membrane is arranged on the surface of the filter, which is far away from the air chamber, and a modified working electrode, a reference electrode and a counter electrode are arranged in an electrolyte chamber in the waterproof shell; the control circuit is formed by electrically connecting an I/V conversion circuit, an amplifier and a microprocessor power supply.
Furthermore, the display system is formed by superposing a first glass layer, a first transparent conducting layer, a TiO/graphene composite electrochromic layer, an ion conducting layer, an ion storage layer, a second transparent conducting layer and a second glass layer in the sequence; the first transparent conducting layer and the second transparent conducting layer are connected with the amplifier through a circuit.
5. Detection of fruit ripeness
The fruit maturity detection method adopted by the invention specifically comprises the following steps:
s1: taking a single variety of fruits as an object to be detected, and placing the object in a non-ventilated environment;
s2: opening a fruit ethylene concentration detector to preheat a system after the ambient atmosphere of the fruit to be detected is stable;
s3: after selecting the type of the fruit to be detected, aligning an air inlet of a fruit ethylene concentration detector to the fruit to be detected, and extracting the air around the fruit to be detected;
s4: the ethylene concentration signal in the gas released by the fruit to be detected is converted into a current signal by an electrochemical sensor in a fruit ethylene detection concentration meter, the current signal is input into a display system after being regulated and amplified, and the maturity of the fruit can be judged through the color change of a detection device; the mathematical expression for predicting fruit ripening is:
wherein y is the fruit maturity grade, U is the voltage value corresponding to the ethylene gas concentration of the fruit to be detected, and k 1 Voltage regulation factor, k, for different fruit types 1 U is the corresponding input voltage value of different fruit ethylene gas concentrations in the detection device;
setting a and b as the color changing node voltage of the detection device, when the input voltage value k 1 When U is less than node voltage a, the display color of the detection device 1 Indicating that the fruit is not ripe; when the input voltage value k 1 When U is greater than or equal to the node voltage a and less than the node voltage b, the display color of the detection device 2 Indicating fruit ripening; when the input voltage value k 1 When U is greater than node voltage b, the detection device displays color 3 Indicating over ripening of the fruit.
By combining the above expressions, the specific structure and the measurement method of the ethylene concentration detector designed by the invention can be determined.
Compared with the prior ethylene detection device, the invention has the beneficial effects that:
(1) The detection method based on the ethylene concentration detector provided by the invention has the characteristics of convenience, wide application range, quick and stable detection result and low detection cost.
(2) The invention provides a gas sensor based on luminescence phenomenon, which can be used at normal temperature, and is free from being used with a large-scale analytical instrument, little influenced by environment and loose in use condition.
Drawings
FIG. 1 is a schematic structural diagram of a fruit ethylene concentration detection device according to the present invention;
FIG. 2 is an external view of the fruit ethylene concentration detecting device of the present invention;
FIG. 3 is a graph showing the placement of materials in a comparison window and a display window according to the present invention.
In the figure: the device comprises a shell 1, a gas transmission system 2, a gas transmission channel 21, a gas inlet 211, a gas outlet 212, a gas chamber 22, a vacuum pump 23, a detection system 3, an ethylene sensor 31, a waterproof shell 311, a filter 312, a hydrophobic membrane 313, an electrolyte chamber 314, a modified working electrode 315, a reference electrode 316, a counter electrode 317, a control circuit 32, an I/V conversion circuit 321, an amplifier 322, a microprocessor 323, a power supply 324, a display system 4, a contrast window 41, a display window 42, a first glass 421, a first transparent conductive layer 422, a first 423-TiO 2/graphene composite electrochromic layer 424, an ion conductive layer 427, an ion storage layer 425, a second transparent conductive layer 426, a second glass 427 and a control panel 5.
Detailed Description
To further illustrate the manner in which the present invention is made and the effects achieved, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings.
Example one
Measuring the concentration of ethylene gas released by the apple serving as a test object, and evaluating the maturity of the apple; with TiO as a carrier 2 If the/graphene composite electrochromic material is a color development material, the fruit detection method specifically comprises the following steps:
s1: taking apples as fruits to be detected, and placing the apples in a non-ventilated environment;
s2: opening a fruit ethylene concentration detector after the ambient atmosphere of the fruit to be detected is stable, and carrying out system preheating;
s3: after selecting the type of the fruit to be detected, aligning an air inlet of a fruit ethylene concentration detector to the fruit to be detected, and extracting the air around the fruit to be detected;
s4: the ethylene concentration signal in the gas released by the fruit to be detected is converted into a current signal by an electrochemical sensor in a fruit ethylene concentration detector, the current signal is input into a display system after being regulated and amplified, and the maturity of the fruit can be judged through the color change of a detection device; the mathematical expression for predicting fruit ripening is:
selecting apples with different maturity, cleaning, airing, placing in a non-ventilated environment, and then testing, wherein each apple is tested for 3 times. The results are shown in Table 1.
TABLE 1 detection results of the concentration of ethylene gas released from apples
As can be seen from the data in Table 1, the concentration of the unripe apples is lower than 1mg/L, and the fruit ethylene detection device is colorless; the concentration range of the ripe apples is 3-6mg/L, and the fruit ethylene detection device presents indigo; the concentration of the over-ripe apples is higher than 6mg/L, and the fruit ethylene detection device is dark blue.
Conclusion 1: when it is made of TiO 2 The/graphene composite electrochromic material is a color development material, and when the fruits are detected to be apples and the fruit ethylene concentration detection device is blue, the fruits are mature.
Example two
The second embodiment is the same as the first embodiment except that bananas are used as measuring objects, and the purpose is to detect the performance of the instrument on different fruit ripeness degrees.
Measuring the concentration of the released ethylene gas by taking bananas as a test object, and evaluating the maturity of the bananas; with TiO 2 If the/graphene composite electrochromic material is a color development material, the fruit detection method specifically comprises the following steps:
s1: taking bananas as fruits to be detected, and placing the bananas in a non-ventilated environment;
s2: opening a fruit ethylene concentration detector to preheat a system after the ambient atmosphere of the fruit to be detected is stable;
s3: after selecting the type of the fruit to be detected, aligning a gas inlet of a fruit ethylene concentration detector to the fruit to be detected, and extracting gas around the fruit to be detected;
s4: the ethylene concentration signal in the gas released by the fruit to be detected is converted into a current signal by an electrochemical sensor in a fruit ethylene detection concentration meter, the current signal is input into a display system after being regulated and amplified, and the maturity of the fruit can be judged through the color change of a detection device; the mathematical expression for predicting fruit ripening is:
selecting bananas with different ripeness degrees, cleaning, airing, placing in an unventilated environment, and then testing, wherein each banana is tested for 3 times. The results are shown in Table 2.
TABLE 2 detection results of gas concentration of banana released ethylene
As can be seen from the data in Table 2, the concentration of the unripe bananas is lower than 2mg/L, and the fruit ethylene detection device is colorless; the concentration range of the ripe bananas is 4-7mg/L, and the fruit ethylene detection device presents indigo; the concentration of the over-ripe bananas is higher than 8mg/L, and the fruit ethylene detection device is dark blue.
Conclusion 2: when it is made of TiO 2 The graphene composite electrochromic material is a color development material, and when the fruit is detected to be banana and the fruit ethylene concentration detection device is blue, the fruit is mature.
EXAMPLE III
Example three and example one except with TiO 2 The PANI electrochromic material is a color developing material, the rest contents are the same, and the purpose is to detect different display materialsNext, the instrument shows the ripeness of the fruit.
Measuring the concentration of ethylene gas released by the apple serving as a test object, and evaluating the maturity of the apple; with TiO 2 The fruit detection method comprises the following specific steps of:
s1: taking apples as fruits to be detected, and placing the apples in a non-ventilated environment;
s2: opening a fruit ethylene concentration detector to preheat a system after the ambient atmosphere of the fruit to be detected is stable;
s3: after selecting the type of the fruit to be detected, aligning a gas inlet of a fruit ethylene concentration detector to the fruit to be detected, and extracting gas around the fruit to be detected;
s4: the ethylene concentration signal in the gas released by the fruit to be detected is converted into a current signal by an electrochemical sensor in a fruit ethylene detection concentration meter, the current signal is input into a display system after being regulated and amplified, and the maturity of the fruit can be judged through the color change of a detection device; the mathematical expression for predicting fruit ripening is:
selecting apples with different ripeness degrees, cleaning, airing, placing in an unventilated environment, and then testing, wherein each apple is tested for 3 times. The results are shown in Table 3.
TABLE 3 detection results of the concentration of ethylene gas released from apples
As can be seen from the data in Table 3, the concentration of the unripe apples is lower than 1mg/L, and the fruit ethylene detection device is light green; the concentration range of the ripe apples is 3-6mg/L, and the fruit ethylene detection device is greenish; the concentration of the over-ripe apples is higher than 6mg/L, and the fruit ethylene detection device is dark green.
Conclusion 1: when being made of TiO 2 the/PANI electrochromic material is a color development material, and when the fruits are detected to be apples and the fruit ethylene concentration detection device is in a green color, the fruits are mature.
Finally, it should be noted that: the above examples are only for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (2)
1. A device for determining the ethylene concentration in a fruit sample, characterized in that it is composed of a gas transmission system (2), a detection system (3), a display system (4) group and a control panel (5) mounted in a housing (1);
the gas transmission system (2) comprises a gas transmission channel (21), the gas transmission channel (21) comprises a gas inlet (211) and a gas outlet (212) and penetrates through the gas chamber (22), and a vacuum pump (23) is arranged on the gas transmission channel (21) close to the gas outlet (212);
the detection system (3) consists of an ethylene sensor (31) and a control circuit (32); the ethylene sensor (31) comprises a waterproof shell (311), a filter (312) is arranged on the contact surface of the waterproof shell (311) and the air chamber (22), a hydrophobic film (313) is arranged on one surface, far away from the air chamber (22), of the filter (312), and a modified working electrode (315), a reference electrode (316) and a counter electrode (317) are arranged in an electrolyte chamber (314) in the waterproof shell (311); the control circuit (32) is formed by electrically connecting an I/V conversion circuit (321), an amplifier (322) and a microprocessor (323) power supply (324);
the display system (4) is divided into a comparison window (41) and a display window (42); the contrast window (41) and the display window (42) are respectively formed by sequentially laminating a first glass (421), a first transparent conducting layer (422), a TiO 2/graphene composite electrochromic layer (423), an ion conducting layer (424), an ion storage layer (425), a second transparent conducting layer (426) and a second glass (427); the first transparent conducting layer (422) and the second transparent conducting layer (426) are connected with the amplifier (322) through a circuit;
the preparation method of the modified working electrode (315) specifically comprises the following steps:
s1: preparation of SnO 2 Matrix: with SnCl 4 ·5H 2 Adding acetic acid as a dispersing agent into the raw material O, titrating the mixture by using ammonia water until the pH value of the system is 3, and obtaining sol after oxalic acid is removed; drying and aging the sol to obtain gel, and roasting the gel at 550 ℃ for 2.5h to obtain SnO 2 A substrate;
s2: in said SnO 2 Base addition 5wt% of PdCl 2 Then coating the mixture on the surface of a gold sheet, and roasting the gold sheet at 550 ℃ for 3.5 hours to obtain a modified working electrode (315);
the preparation method of the NiO/graphene composite electrochromic layer (43) specifically comprises the following steps:
s1: preparing a chemical bath deposition solution: the volume percentage ratio is 5:5:1 to 0.5mol of NiSO 4 ·6H 2 O、0.15molK 2 S 2 O 8 And ammonia water to obtain chemical bath deposition liquid;
s2: preparing electrophoretic deposition liquid: 1 percent of graphene oxide and 1 percent of Mg (NO) by mass 3 ) 2 ·6H 2 Adding O into isopropanol, and stirring by ultrasound and magnetic force to form stable sol as electrolyte;
s3: preparing a graphene/ITO glass substrate: taking the cleaned ITO glass plate as a working electrode, electrolyzing a platinum sheet as a counter electrode, adding electrophoretic deposition liquid, depositing for 15s under the conditions of a distance of 1cm, a voltage of 100V and a temperature of 25 ℃, and then processing for 1.5h at 280 ℃ in an argon atmosphere to obtain a graphene/ITO glass substrate;
s4: and (2) placing the graphene/ITO glass substrate in a chemical bath deposition solution, stirring for 15min at 60 ℃, and then treating for 1.5h at 280 ℃ in an argon atmosphere to obtain the NiO/graphene composite electrochromic material.
2. The method of claim 1, comprising the steps of:
s1: taking a single variety of fruits as fruits to be detected, and placing the fruits in a non-ventilated environment;
s2: opening a fruit ethylene concentration detector to preheat a system after the ambient atmosphere of the fruit to be detected is stable;
s3: after selecting the type of the fruit to be detected, aligning an air inlet of a fruit ethylene concentration detector to the fruit to be detected, and extracting the air around the fruit to be detected;
s4: the ethylene concentration signal in the gas released by the fruit to be detected is converted into a current signal by an electrochemical sensor in a fruit ethylene detection concentration meter, the current signal is input into a display system after being regulated and amplified, and the maturity of the fruit can be judged through the color change of a detection device;
the mathematical expression of the maturity degree of the fruit is as follows:
wherein y is the fruit ripening grade, U is the voltage value corresponding to the ethylene gas concentration of the fruit to be detected, and k 1 Voltage regulation factor, k, for different fruit types 1 U is the corresponding input voltage value of different fruit ethylene gas concentrations in the detection device;
setting a and b as the color changing node voltage of the detection device, when the input voltage value k 1 When U is less than node voltage a, the detection device displays color 1 Indicating that the fruit is not ripe; when the input voltage value k 1 When U is greater than or equal to the node voltage a and less than the node voltage b, the display color of the detection device 2 Indicating fruit ripening; when the input voltage value k 1 When U is greater than node voltage b, the display color of the detection device 3 Indicating over ripening of the fruit;
the mathematical expression of the voltage value U corresponding to the ethylene gas concentration of the fruit to be detected and the ethylene concentration c of the fruit is as follows:
wherein i is the current value during the detection of the ethylene concentration c, U 1 The voltage value corresponding to the converted current value i, coefficient k 2 Is a voltage amplification factor, coefficient k 3 In relation to the structural parameters of the detecting device itself, when the structure of the detecting device is determined, k 3 Is a constant.
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| US4414839A (en) * | 1979-04-12 | 1983-11-15 | Board Of Trustees, A Constitutional Corporation Operating Michigan State University | Gas sensing apparatus and method |
| US4410632A (en) * | 1979-04-12 | 1983-10-18 | Board Of Trustees Operating Michigan State University | Gas sensing apparatus and method |
| KR20040043132A (en) * | 2001-11-14 | 2004-05-22 | 마츠시타 덴끼 산교 가부시키가이샤 | Gas sensor, and production method for gas sensor |
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| CN106970189B (en) * | 2017-03-23 | 2019-09-13 | 中北大学 | A kind of testing and analysis system and method for fruit freshness |
| CN109470824A (en) * | 2018-12-18 | 2019-03-15 | 华南农业大学 | A kind of ethylene concentration measurement monitoring device and its measuring and monitoring method |
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