CN109187706B - Method for detecting refined illegal cooking oil by using polyaniline chip - Google Patents
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Abstract
The invention discloses a method for detecting refined illegal cooking oil by utilizing a polyaniline chip. According to the invention, the polyaniline chip is selected, sodium ions are doped in the polyaniline chip which is not conductive originally, a current-concentration curve of different sodium ion concentrations under a certain voltage can be made by measuring the conductivity of the polyaniline chip under different sodium ion concentrations for multiple times, and illegal cooking oil and edible oil with different degrees can be distinguished by utilizing the curve, so that the aim of quickly, efficiently and widely detecting illegal cooking oil is fulfilled.
Description
Technical Field
The invention relates to the technical field of illegal cooking oil detection, in particular to a method for detecting refined illegal cooking oil by utilizing a polyaniline chip.
Background
With the development of the times and the progress of science and technology, people pay more and more attention to the taste and health of food. However, when people eat food, the difference between normal oil and edible oil is difficult to judge, and a precise and acknowledged method for identifying and identifying illegal cooking oil has not been provided so far, so that the illegal cooking oil has great harm to the health of people.
The illegal cooking oil is mostly extracted and refined from used edible oil, wherein salt used for overeating is necessarily used, and sodium ions which are necessary in the salt cannot be removed in the illegal cooking oil along with the sodium ions; on the other hand, since the illegal cooking oil is significantly acidic due to a large amount of substances present therein, sodium carbonate or ammonium hydrogen carbonate or the like is used for removing the acidity in the illegal cooking oil, and a large amount of sodium ions are also present therein. The presence of these sodium ions is not normally found in uneaten cooking oils, and one such identification of illegal cooking oils is based on the detection of the conductivity of the illegal cooking oil due to the sodium ions.
Polyaniline is a polymer synthetic material, commonly called conductive plastic. It is a kind of special functional material, has the density of plastics, conductivity of metal and machinability of plastics, and chemical and electrochemical properties which are deficient in metal and plastics, and can be used as stealth material and anticorrosion material in national defense industry, and can be used as metal anticorrosion material, antistatic material and electronic chemicals for civil use.
At present, a reasonable, effective and rapid method detection method cannot be researched for the illegal cooking oil at home and abroad, and the main reason is that a specific convincing illegal cooking oil marker cannot be determined to identify the illegal cooking oil. The method is characterized in that the method takes sodium ions in the illegal cooking oil as a root element to identify the illegal cooking oil, selects a polyaniline chip, dopes the sodium ions in the polyaniline chip which is not conductive originally, and detects the conductivity of the polyaniline chip by using an electrochemical workstation. By the method, a current-concentration curve of different sodium ion concentrations under a certain voltage can be made by measuring the conductivity of the polyaniline chip under different sodium ion concentrations for multiple times, and illegal cooking oil and edible oil with different degrees can be distinguished by utilizing the curve.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a method for detecting and refining illegal cooking oil by utilizing a polyaniline chip, wherein the polyaniline chip is selected, sodium ions are doped in the polyaniline chip which is not conductive originally, a current-concentration curve of different sodium ion concentrations under a certain voltage can be made by measuring the conductivity of the polyaniline chip under different sodium ion concentrations for multiple times, and illegal cooking oil and edible oil with different degrees can be distinguished by utilizing the curve, so that the aim of quickly, efficiently and widely detecting the illegal cooking oil is fulfilled.
The invention provides a method for detecting refined illegal cooking oil by utilizing a polyaniline chip.
Preferably, the method comprises the steps of:
(1) preparing a concentration-current standard curve: firstly, three probe electrodes of an electrochemical workstation are utilized and are added on a polyaniline interdigital electrode chip, a working electrode and a reference electrode are arranged on one side, a counter electrode is arranged on the other corresponding side, and a soap solution is used as a solution to be detected; then selecting CV-Cyclic volt-amperometry, performing scanning test on different soap solution concentrations by using Cyclic Voltammetry, and collating data to obtain a concentration-current standard curve;
(2) and (3) testing the illegal cooking oil: firstly, 100ml of deionized water is taken, 1-5mg of aniline and 1-2 drops of illegal cooking oil samples are added into the deionized water, and the mixture is fully stirred and mixed; dripping mixed swill-cooked dirty oil on a polyaniline electrode chip, drying, and repeatedly operating for 2-3 times; and finally, testing a corresponding current-time map at a voltage of-0.15V by using an electrochemical station, and analyzing an experimental result according to the concentration-current standard curve.
Preferably, in step (1), the cyclic voltammetry is set to a voltage range of-0.8V to 0.8V at a scan rate of 0.05V/s.
Preferably, the preparation process of the polyaniline chip comprises the following steps:
s1, weighing 0.0010g of soap solid by using an electronic balance, dissolving the soap solid in 100ml of deionized water, and stirring the soap solid by using a glass rod until the soap solid is completely dissolved, wherein the soap solid is marked as a solution A;
s2, taking 10ml of soap solution from the solution A by using a 10ml measuring cylinder, adding the soap solution into 90ml of deionized water, and slightly stirring by using a glass rod to obtain a solution B;
s3, taking 10ml of soap solution from the solution B by using a 10ml measuring cylinder, adding the soap solution into 90ml of deionized water, and slightly stirring by using a glass rod to obtain a solution C;
s4, preparing a solution D, a solution E, a solution F, a solution G, a solution H, a solution I and a solution J respectively by analogy;
s5, respectively taking 5ml of solution from the solutions A to J, adding 1-5mg of polyaniline powder, vibrating and stirring uniformly, and then carrying out ultrasonic treatment for 10-15 minutes to obtain solutions, namely solution a, solution b, solution c, solution d, solution e, solution f, solution g, solution h, solution i and solution J;
and S6, respectively dripping the solutions a to j on the interdigital electrodes to enable the solutions to be paved on the interdigital electrodes, drying the interdigital electrodes in an oven for 3-5 minutes, taking out the dried interdigital electrodes, dripping the solutions a to j one by one, drying the interdigital electrodes in the oven for 3-5 minutes, and repeating the steps for 2-3 times to obtain the polyaniline interdigital electrode chips doped with sodium ions with different concentrations.
Preferably, the preparation method of the polyaniline comprises the following steps: A. weighing aniline monomers, adding the aniline monomers into a beaker of deionized water, and stirring with a glass rod until the solution is clear to obtain an aniline solution with the concentration of 16-17 g/L; weighing ammonium persulfate, dissolving in a beaker of deionized water, and slightly stirring by using a glass rod to obtain an ammonium persulfate solution with the concentration of 4.1-4.2 g/L; B. dropwise adding the ammonium persulfate solution with the same volume into the aniline solution, and stirring for reaction for 5-6 hours; C. and washing the reaction product with ethanol and deionized water, and drying to obtain the polyaniline.
The invention respectively manufactures polyaniline chips a to j from the solutions a to j, and correspondingly, 10 polyaniline is doped in the polyaniline-3g/100ml、10-4g/100ml、10-5g/100ml、10-6g/100ml、10-7g/100ml、 10-8g/100ml、10-9g/100ml、10-10g/100ml、10-11g/100ml and 10-12The soap solution with the concentration of g/100ml forms a stably reduced sodium ion concentration, the doping under different ion concentrations has different influences on the conductivity of the doped polyaniline, so that different C-V curves appear, and finally the C-V curves of the polyaniline doped with sodium ions with various concentrations are compared, synthesized and analyzed. The technical scheme of the invention can realize effective and rapid detection of the illegal cooking oil and the content thereof, and the method is simple and easy to realize.
Drawings
FIG. 1 is a graph of polyaniline chips i-c prepared from soap solutions of different concentrations at-0.15V in accordance with the present invention.
FIG. 2 is an i-t curve of a sample of the drainage oil of the present invention.
FIG. 3 is a di-i-t curve of a sample of the drainage oil of the present invention.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples. The reagents used in the examples were all routinely tested or commercially available.
Example 1:
a method for detecting refined illegal cooking oil by utilizing a polyaniline chip comprises the following steps:
1.1 preparation of acid-free polyaniline
(1) Taking a 100ml beaker, weighing 0.5000g of aniline monomer by using an electronic balance, adding the aniline monomer into the beaker filled with 30ml of deionized water, and stirring by using a glass rod until the solution is clear;
(2) weighing 1.2500g of ammonium persulfate in another 100ml beaker by using an electronic balance, dissolving the ammonium persulfate in the beaker filled with 30ml of deionized water, and slightly stirring the mixture by using a glass rod;
stirring aniline solution with an electric stirrer, sucking the prepared ammonium persulfate solution with a rubber head dropper, slowly dripping the ammonium persulfate solution into the aniline solution (controlling the temperature at about zero centigrade by using an ice bag),
(3) after the dropwise addition is finished, reacting the solution for 5-6 hours;
(4) carrying out suction filtration on the polyaniline solution after the reaction by using ethanol and deionized water, and alternately repeating for three times;
(5) drying the polyaniline solution after suction filtration; and (5) obtaining the polyaniline nano-rod after drying.
1.2 preparation of polyaniline chip
(1) Weighing 0.0010g of soap solid by using an electronic balance, dissolving the soap solid in 100ml of deionized water, and stirring the soap solid by using a glass rod until the soap solid is completely dissolved, and marking the soap solid as a solution A;
(2) taking 10ml of soap solution from the solution A by using a 10ml measuring cylinder, adding the soap solution into 90ml of deionized water, and slightly stirring by using a glass rod to obtain a solution B;
(3) taking 10ml of soap solution from the solution B by using a 10ml measuring cylinder, adding the soap solution into 90ml of deionized water, and slightly stirring by using a glass rod to obtain a solution C;
(4) repeating the two steps to respectively prepare a solution D, a solution E, a solution F, a solution G, a solution H, a solution I and a solution J;
(5) respectively taking 5ml of solution from the solutions A to J, adding 2mg of polyaniline powder, shaking and uniformly stirring, and then carrying out ultrasonic treatment for 10-15 minutes to obtain solutions a, b, c, d, e, f, g, h, i and J
(6) And taking out the micro-solution from the solution a by using a dropper, dripping the micro-solution on the interdigital electrode, and putting the interdigital electrode into an oven to dry for 3-5 minutes. Taking out, dripping the solution a again, putting into an oven for 3-5 minutes, and repeating the steps for 2-3 times;
(7) repeating the sixth step until 15-20 identical polyaniline chips are prepared;
(8) and repeating the sixth step and the seventh step, and manufacturing the same polyaniline chip by using the solutions b-j for standby. Marking the prepared polyaniline interdigital electrode chips as chips a-j respectively;
(9) and (4) arranging the experimental instrument, marking the polyaniline chip, and then applying the polyaniline chip in the next step.
1.3 preparation of concentration-Current Standard Curve
(1) Three probe electrodes of an electrochemical workstation are utilized and are added on the prepared polyaniline interdigital electrode chip, a working electrode and a reference electrode are arranged on one side, and a counter electrode is arranged on the other side;
(2) selecting CV-Cyclic volt-metric, setting the voltage range to be-0.8V by using Cyclic volt-ampere, setting the number of scanning cycles to be one circle and the scanning rate to be 0.05V/s, and scanning;
(3) repeating the steps, and carrying out scanning test on the polyaniline chip prepared previously;
(4) arranging instruments, summarizing, arranging and analyzing data;
(5) current curves were synthesized at different soap solution concentrations using OriginPro plots.
1.4 illegal cooking oil test
(1) Taking 100ml of deionized water, adding 4mg of synthesized polyaniline nano-rods and 1-2 drops of illegal cooking oil sample I, and fully stirring and mixing;
(2) dripping the mixed swill-cooked dirty oil on an electrode plate, drying for 3-5 min, and repeatedly operating for 2-3 times;
(3) testing an i-t image of the prepared illegal cooking oil chip under a voltage of-0.15V by using an electrochemical station;
(4) and repeating the three steps on the second sample of the illegal cooking oil, and finishing the data image for later use.
Based on the above test results, to be more efficient and accurateIn this example, the concentration is plotted on the abscissa and the current value at-0.15V is plotted on the ordinate to form a current curve (working curve) corresponding to different concentrations at-0.15V, as shown in FIG. 1, at a constant voltage of-0.15V, the current value increases with the increase of the soap solution concentration, and at 10V-5g/100ml～10-3In the process of g/100ml, the curve has a trend of approaching a flat state, and is 10-12g/100ml～10-11The trend is nearly gentle in the process of g/100ml, because when the soap solution is 0, the corresponding current value is 0, the trend is a reasonable phenomenon, and the reason that the upper right corner of the curve tends to be gentle is probably that when the concentration is increased to a certain value, the degree of doping of sodium ions is not large, so that the conductivity difference tends to be obvious without middle.
In order to verify the feasibility of the experimental result, a first sample and a second sample of the illegal cooking oil are collected from a school canteen, the same experimental steps are adopted to replace the soap solution for carrying out experimental operation, a constant-0.15V voltage is finally applied to the chip, the current magnitude of the chip is observed, as shown in figures 2 and 3, when the given voltage is-0.15V, the first sample presents a stable current value, the value is compared with a previous working curve i-c diagram, and the concentration of sodium ions corresponding to the first sample and the second sample is about the concentration of the soap solution at 10-11g/100ml～10-12Sodium ion concentration in g/100 ml. Under this curve, we know that it is basically feasible to measure illegal cooking oil by this method.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (3)
1. A method for detecting refined illegal cooking oil by utilizing a polyaniline chip is characterized in that the method obtains a current-concentration standard curve by measuring the conductivity of the polyaniline interdigital electrode chip in a plurality of sodium ion concentration gradients, and then the illegal cooking oil is detected according to the standard curve;
characterized in that the method comprises the following steps:
(1) preparing a current-concentration standard curve: firstly, three probe electrodes of an electrochemical workstation are utilized and are added on a polyaniline interdigital electrode chip, a working electrode and a reference electrode are arranged on one side, a counter electrode is arranged on the other corresponding side, and a soap solution is used as a solution to be detected; then selecting CV-Cyclic volt-ametry, performing scanning test on different soap solution concentrations by using Cyclic Voltammetry, and collating data to obtain a current-concentration standard curve;
(2) and (3) testing the illegal cooking oil: firstly, 100ml of deionized water is taken, 1-5mg of polyaniline and 1-2 drops of illegal cooking oil samples are added into the deionized water, and the mixture is fully stirred and mixed; dripping mixed drainage oil on a polyaniline interdigital electrode chip, drying, and repeatedly operating for 2-3 times; finally, testing a corresponding current-time map at-0.15V voltage by using an electrochemical station, and analyzing an experimental result according to the current-concentration standard curve;
the preparation process of the polyaniline interdigital electrode chip comprises the following steps:
s1, weighing 0.0010g of soap solid by using an electronic balance, dissolving the soap solid in 100ml of deionized water, and stirring the soap solid by using a glass rod until the soap solid is completely dissolved, wherein the soap solid is marked as a solution A;
s2, taking 10ml of soap solution from the solution A by using a 10ml measuring cylinder, adding the soap solution into 90ml of deionized water, and slightly stirring by using a glass rod to obtain a solution B;
s3, taking 10ml of soap solution from the solution B by using a 10ml measuring cylinder, adding the soap solution into 90ml of deionized water, and slightly stirring by using a glass rod to obtain a solution C;
s4, preparing a solution D, a solution E, a solution F, a solution G, a solution H, a solution I and a solution J respectively by analogy;
s5, respectively taking 5ml of solution from the solutions A to J, adding 1-5mg of aniline powder, vibrating and uniformly stirring, and performing ultrasonic treatment for 10-15 minutes to obtain solutions, namely solution a, solution b, solution c, solution d, solution e, solution f, solution g, solution h, solution i and solution J;
and S6, respectively dripping the solutions a to j on the interdigital electrodes to enable the solutions to be paved on the interdigital electrodes, drying the interdigital electrodes in an oven for 3-5 minutes, taking out the dried interdigital electrodes, dripping the solutions a to j one by one, drying the interdigital electrodes in the oven for 3-5 minutes, and repeating the steps for 2-3 times to obtain the polyaniline interdigital electrode chips doped with sodium ions with different concentrations.
2. The method for detecting refined gutter oil by using polyaniline chip as claimed in claim 1, wherein in the step (1), the voltage range is set to-0.8V by cyclic voltammetry, and the scan rate is 0.05V/s.
3. The method for detecting refined illegal cooking oil by using polyaniline chip as claimed in claim 1, wherein the preparation method of polyaniline comprises the following steps: A. weighing aniline monomers, adding the aniline monomers into a beaker of deionized water, and stirring with a glass rod until the solution is clear to obtain an aniline solution with the concentration of 16-17 g/L; weighing ammonium persulfate, dissolving in a beaker of deionized water, and slightly stirring by using a glass rod to obtain an ammonium persulfate solution with the concentration of 4.1-4.2 g/L; B. dropwise adding the ammonium persulfate solution with the same volume into the aniline solution, and stirring for reaction for 5-6 hours; C. and washing the reaction product with ethanol and deionized water, and drying to obtain the polyaniline.
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2018
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