CN112525896A - Hydrogen peroxide test paper and quantitative detection H thereof2O2Method (2) - Google Patents

Hydrogen peroxide test paper and quantitative detection H thereof2O2Method (2) Download PDF

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CN112525896A
CN112525896A CN202011308343.6A CN202011308343A CN112525896A CN 112525896 A CN112525896 A CN 112525896A CN 202011308343 A CN202011308343 A CN 202011308343A CN 112525896 A CN112525896 A CN 112525896A
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hydrogen peroxide
test paper
test
value
standard
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廖丹葵
李纯枝
孙建华
江宇威
孙丽霞
周利琴
童张法
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Guangxi University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour

Abstract

The invention discloses a hydrogen peroxide test paper and a quantitative detection method thereof2O2The method of (1) using 3,3',5,5' -tetramethylbenzidine as a color-developing agent in Fe3O4/Ti3C2When the material is used for catalyzing and decomposing hydrogen peroxide, the hydrogen peroxide detection test paper prepared by the principle that 3,3',5,5' -tetramethylbenzidine is oxidized to display blue can not only qualitatively judge the approximate content range of hydrogen peroxide by observing the color change condition of the detection test paper by naked eyes, but also be combined with a smart phone, and quantitatively determine H by reading a chromatic value through a mobile phone scanning test paper2O2And (4) content. The color test paper disclosed by the invention is simple to prepare, small and portable, convenient to use, wide in test range, free of professional personnel and professional equipment, and suitable for rapidly detecting hydrogen peroxide in a water body in various environments.

Description

Hydrogen peroxide test paper and quantitative detection H thereof2O2Method (2)
Technical Field
The invention relates to the technical field of hydrogen peroxide content detection, in particular to hydrogen peroxide detection test paper and quantitative detection H thereof2O2The method of (1).
Background
Hydrogen peroxide (H)2O2) An important raw material in chemical industry, often used as an oxidant. The pharmaceutical industry is used as a bactericide and a disinfectant. Bleaches for the printing and dyeing industry, color development after dyeing with vat dyes. Also used for electroplating liquid, can remove inorganic impurities and improve the quality of plated parts. It is also used for bleaching wool, silk, ivory, pulp, fat, etc. Industrial waste water in chemical industry, medicine, printing and dyeing, electroplating, bleaching and the like contains hydrogen peroxide, even hydrogen peroxide is added in waste water treatment to treat various pollutants, however, hydrogen peroxide may be remained in different treatment methods, the remained hydrogen peroxide can affect Biological Oxygen Demand (BOD) and Chemical Oxygen Demand (COD), waste water which fails to reach the standard is directly discharged to the natural environment, hydrogen peroxide and other pollutants can easily cause water source pollution and damage soil structures, further growth of crops is influenced, aquatic organisms are damaged, and the natural environment is seriously threatened, and a rat orally takes LD50 (mg/kg): at a concentration of 90%, 376mg/kg showed acute toxicity. Excessive hydrogen peroxide also poses a threat to human health, namely 10 and 27 in 2017, and the list of carcinogens published by the international cancer research institution of the world health organization is preliminarily collated for reference, and the hydrogen peroxide is in the list of 3 types of carcinogens.
Therefore, the establishment of the detection of hydrogen peroxide has important significance for the sustainable development of industry and agriculture and the human health, and the traditional methods for measuring the concentration of hydrogen peroxide can be divided into chemical analysis methods and instrumental analysis methods. For samples with higher concentration, chemical titration analysis methods such as a potassium permanganate method, an iodometry method, a cerium sulfate method and the like are adopted. The low-concentration sample is generally analyzed by instruments such as high performance liquid chromatography, an electrochemical sensor, an ultraviolet spectrophotometer, a flow injection-spectrophotometry and the like.
TABLE 1 comparison of different detection methods
Figure BDA0002789415940000011
Figure BDA0002789415940000021
However, in the actual operation process, these measurement methods not only require laboratory conditions, but also are complex and time-consuming to operate, require a certain professional knowledge, have high precious metal cost, and cannot meet the requirements of rapid real-time measurement.
Disclosure of Invention
In order to solve the problems, the invention provides a hydrogen peroxide detection test paper and a quantitative detection method H thereof2O2The method has the advantages of low test cost, simple and convenient operation and capability of quickly detecting the concentration of the hydrogen peroxide in real time.
The invention adopts the following technical scheme:
the preparation method of the hydrogen peroxide detection test paper comprises the following steps:
step 1, titanium aluminum carbon (Ti)3AlC2) Placing the titanium carbide substrate into hydrofluoric acid (HF) water solution at room temperature for corrosion reaction to obtain titanium carbide (Ti)3AlC2 MXene);
Step 2, putting iron (III) acetylacetonate and the titanium carbide obtained in the step 1 into benzyl alcohol together for mixing to obtain a mixed solution; putting the obtained mixed solution into a hydrothermal reaction kettle for reaction for 1-3 hours, then carrying out magnet separation on the reacted mixed solution, and drying to obtain Fe3O4/Ti3C2A material;
step 3, mixing the Fe obtained in the step 23O4/Ti3C2Dissolving the material in deionized water to obtain a solution I; dissolving 3,3',5,5' -tetramethyl benzidine in absolute ethyl alcohol to obtain a solution II;
step 4, sucking the solution I obtained in the step 3, uniformly dripping the solution I on filter paper, and heating and drying the filter paper;
and 5, after the filter paper in the step 4 is dried and cooled to room temperature, dripping the solution II obtained in the step 3 on the filter paper, heating, drying and cooling again to obtain the hydrogen peroxide detection test paper, and finally cutting the hydrogen peroxide detection test paper and putting the hydrogen peroxide detection test paper into a light-resistant and moisture-proof packaging bag for storage.
As a preferred technical scheme of the invention, the reaction temperature of the hydrothermal reaction kettle in the step 2 is 150-250 ℃.
As a preferable technical scheme of the present invention, in the step 3, the ratio of 3,3',5,5' -tetramethylbenzidine to absolute ethyl alcohol is (20-50) mg: (10-50) ml.
As a preferred technical solution of the present invention, the filter paper used in the step 4 is a quantitative filter paper or a qualitative filter paper.
Quantitative determination H of hydrogen peroxide test paper2O2The method comprises the following steps:
standard card and preparation of standard concentration curve
Step A, preparing a plurality of standard hydrogen peroxide solutions with different concentrations, marking the hydrogen oxide detection test paper obtained in the step 5 and the hydrogen peroxide solutions with different concentrations in a one-to-one correspondence manner, then putting the marked hydrogen oxide detection test paper into the hydrogen peroxide solution with the corresponding concentration for 1-5 seconds for color development test, and taking out the hydrogen oxide detection test paper after the test is finished to obtain test standard cards of the standard hydrogen peroxide solutions with different concentrations;
b, shooting the pictures of the test standard cards of the hydrogen peroxide solutions with different concentrations obtained in the step A through a mobile phone, and introducing the shot pictures into a color recognition APP to recognize the RGB values of the test standard cards of the hydrogen peroxide solutions with different concentrations;
and C, processing the RGB values of the test standard cards of the hydrogen peroxide solutions with different concentrations obtained in the step B, and calculating the percentage ratio of the B value in the RGB values, wherein the calculation formula is as follows: (B value/(R value + G value + B value)). times.100%;
step D, corresponding the percentage of the value B obtained in the step C to the corresponding concentration of the perhydrogenated oxygen, so as to draw a standard concentration curve and obtain a linear regression equation;
process for quantitatively testing hydrogen peroxide concentration of liquid to be tested
Step E, putting the hydrogen oxide detection test paper obtained in the step 5 into the collected liquid sample to be detected for 1-5 seconds for color development test, taking out the hydrogen oxide detection test paper after the test is finished, taking a picture of the hydrogen oxide detection test paper by a mobile phone, introducing the picture into a color recognition APP for picture RGB value recognition, and then calculating the percentage of the B value of the detection picture of the liquid sample to be detected by the calculation formula in the step C;
and F, substituting the percentage of the B value of the detection picture of the liquid sample to be detected obtained in the step E into a linear regression equation of a standard concentration curve to correspondingly calculate the concentration of the perhydrogenated oxygen in the liquid sample to be detected.
The invention has the beneficial effects that:
the invention adopts 3,3',5,5' -tetramethyl benzidine as color developing agent, and uses Fe3O4/Ti3C2The hydrogen peroxide detection test paper prepared by the principle that 3,3',5,5' -tetramethyl benzidine is oxidized to show blue when the material is used for catalytically decomposing hydrogen peroxide is low in price and high in relative stability of test; meanwhile, the color development of the test paper is blue during detection, and the color development depth of the test paper is in direct proportion to the concentration of the perhydrogenated oxygen in the sample, so that a linear regression equation is prepared by adopting a standard solution for testing before testing and matching with mobile phone photographing to calculate the percentage of the B value of a test paper color development photo, and the concentration of the perhydrogenated oxygen in the detected sample can be quickly and conveniently detected during use; the whole testing process is convenient and quick, the testing range is wide, no professional personnel or professional equipment is needed, and the method is particularly suitable for quickly measuring the content of the hydrogen peroxide on site in real time.
Drawings
FIG. 1 is a graph of a standard concentration profile according to the present invention;
Detailed Description
The invention will now be described in further detail with reference to the drawings and examples.
First, it is worth mentioning that, in the embodiments,the titanium aluminum carbon (Ti)3AlC2) The mass content is 99%; hydrofluoric acid (HF) was analytically pure; the mass content of the 3,3',5,5' -tetramethyl benzidine is 99%; the mass content of the iron (III) acetylacetonate is 98 percent;
the preparation method of the hydrogen peroxide detection test paper comprises the following steps:
step 1, putting titanium aluminum carbon into hydrofluoric acid aqueous solution at room temperature for corrosion reaction to obtain titanium carbide (Ti)3AlC2 MXene);
Step 2, putting ferric acetylacetonate and the titanium carbide obtained in the step 1 into benzyl alcohol together for mixing to obtain a mixed solution; putting the obtained mixed solution into a hydrothermal reaction kettle for reaction for 2 hours, then carrying out magnet separation on the mixed solution after the reaction, and drying to obtain Fe3O4/Ti3C2A material;
wherein the mass ratio of the ferric acetylacetonate to the titanium carbide is 5: 1; in this example, the mass of the iron acetylacetonate was 0.5g, and the mass of the titanium carbide was 0.1 g; the reaction temperature of the hydrothermal reaction kettle is 180 ℃; in the practical application process, a person skilled in the art can determine the reaction temperature of the hydrothermal reaction kettle according to actual needs, for example, the reaction temperature can be any temperature value from 150 ℃ to 250 ℃;
step 3, mixing the Fe obtained in the step 23O4/Ti3C2Dissolving the material in deionized water to obtain a solution I; dissolving 3,3',5,5' -tetramethyl benzidine in absolute ethyl alcohol to obtain a solution II;
wherein the ratio of the 3,3',5,5' -tetramethylbenzidine to the absolute ethyl alcohol is (20-50) mg: (10-50) ml, specifically, in this embodiment, the mass of the 3,3',5,5' -tetramethylbenzidine is 48mg, and the amount of the absolute ethanol is 20ml, and in an actual application process, a person skilled in the art may also determine the amounts of the 3,3',5,5' -tetramethylbenzidine and the absolute ethanol according to the above ratio according to actual needs;
step 4, sucking the solution I obtained in the step 3, uniformly dripping the solution I on filter paper, and heating and drying the filter paper;
wherein the filter paper is any one of quantitative filter paper or qualitative filter paper;
and 5, after the filter paper in the step 4 is dried and cooled to room temperature, dripping the solution II obtained in the step 3 on the filter paper, heating, drying and cooling again to obtain the hydrogen peroxide detection test paper, and finally cutting the hydrogen peroxide detection test paper and putting the hydrogen peroxide detection test paper into a light-resistant and moisture-proof packaging bag for storage.
Quantitative determination H of hydrogen peroxide test paper2O2The method comprises the following steps:
standard card and preparation of standard concentration curve
Step A, preparing a plurality of standard hydrogen peroxide solutions with different concentrations, marking the hydrogen oxide detection test paper obtained in the step 5 and the hydrogen peroxide solutions with different concentrations in a one-to-one correspondence manner, then putting the marked hydrogen oxide detection test paper into the hydrogen peroxide solution with the corresponding concentration for 1-5 seconds for color development test, and taking out the hydrogen oxide detection test paper after the test is finished to obtain test standard cards of the standard hydrogen peroxide solutions with different concentrations;
b, shooting the pictures of the test standard cards of the hydrogen peroxide solutions with different concentrations obtained in the step A through a mobile phone, and introducing the shot pictures into a color recognition APP to recognize the RGB values of the test standard cards of the hydrogen peroxide solutions with different concentrations;
and C, processing the RGB values of the test standard cards of the hydrogen peroxide solutions with different concentrations obtained in the step B, and calculating the percentage ratio of the B value in the RGB values, wherein the calculation formula is as follows: (B value/(R value + G value + B value)). times.100%;
step D, corresponding the percentage of the value B obtained in the step C to the corresponding concentration of the perhydrogenated oxygen, so as to draw a standard concentration curve and obtain a linear regression equation;
more specifically, in this embodiment, the number of the standard hydrogen peroxide solution is 10 (in the actual application process, a person skilled in the art can determine the number of the standard hydrogen peroxide solution according to actual needs), the specific concentration thereof and the percentage of the corresponding B value measured by the above method are as follows:
TABLE 1
Figure BDA0002789415940000061
Meanwhile, as shown in fig. 1, a standard concentration curve graph plotted according to the above data and a linear regression equation obtained correspondingly are shown in this embodiment.
Application process for quantitatively testing hydrogen peroxide concentration of liquid to be tested
Step E, putting the hydrogen oxide detection test paper obtained in the step 5 into the collected liquid sample to be detected for 1-5 seconds for color development test, taking out the hydrogen oxide detection test paper after the test is finished, taking a picture of the hydrogen oxide detection test paper by a mobile phone, introducing the picture into a color recognition APP for picture RGB value recognition, and then calculating the percentage of the B value of the detection picture of the liquid sample to be detected by the calculation formula in the step C;
and F, substituting the percentage of the B value of the detection picture of the liquid sample to be detected obtained in the step E into a linear regression equation of a standard concentration curve to correspondingly calculate the concentration of the perhydrogenated oxygen in the liquid sample to be detected.
More specifically, in the application process, eight groups of known concentrations are prepared: group 1: 0.2mmol/L, set 2: 0.7mmol/L, set 3: 1mmol/L, set 4: 2mmol/L, set 5: 4.5mmol/L, set 6: 8mmol/L, 7 groups: 13mmol/L, set 8: 19mmol/L of hydrogen peroxide solution, which was then tested in the above test manner, wherein the concentration of the test results versus the actual hydrogen peroxide solution concentration is given in table 2 below:
TABLE 2
Figure BDA0002789415940000062
According to the data, the hydrogen peroxide concentration tested by the method is high in accuracy and wide in concentration test range; meanwhile, the operation is convenient and fast, and the industrial popularization and application are facilitated.
Finally, it should be noted that: these embodiments are merely illustrative of the present invention and do not limit the scope of the present invention. In addition, other variations and modifications will be apparent to persons skilled in the art based on the foregoing description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the scope of the invention.

Claims (5)

1. The preparation method of the hydrogen peroxide detection test paper comprises the following steps:
step 1, putting titanium-aluminum-carbon into hydrofluoric acid aqueous solution at room temperature for corrosion reaction to obtain titanium carbide;
step 2, putting ferric acetylacetonate and the titanium carbide obtained in the step 1 into benzyl alcohol together for mixing to obtain a mixed solution; putting the obtained mixed solution into a hydrothermal reaction kettle for reaction for 1-3 hours, then carrying out magnet separation on the reacted mixed solution, and drying to obtain Fe3O4/Ti3C2A material;
step 3, mixing the Fe obtained in the step 23O4/Ti3C2Dissolving the material in deionized water to obtain a solution I; dissolving 3,3',5,5' -tetramethyl benzidine in absolute ethyl alcohol to obtain a solution II;
step 4, sucking the solution I obtained in the step 3, uniformly dripping the solution I on filter paper, and heating and drying the filter paper;
and 5, after the filter paper in the step 4 is dried and cooled to room temperature, dripping the solution II obtained in the step 3 on the filter paper, heating, drying and cooling again to obtain the hydrogen peroxide detection test paper, and finally cutting the hydrogen peroxide detection test paper and putting the hydrogen peroxide detection test paper into a light-resistant and moisture-proof packaging bag for storage.
2. The hydrogen peroxide test strip of claim 1, wherein: the reaction temperature of the hydrothermal reaction kettle in the step 2 is 150-250 ℃.
3. The hydrogen peroxide test strip of claim 1, wherein: in the step 3, the ratio of 3,3',5,5' -tetramethylbenzidine to absolute ethyl alcohol is (20-50) mg: (10-50) ml.
4. The hydrogen peroxide test strip of claim 1, wherein: the filter paper adopted in the step 4 is quantitative filter paper or qualitative filter paper.
5. The quantitative determination method H of hydrogen peroxide test paper according to claim 12O2The method of (2), characterized by: the method comprises the following steps:
standard card and preparation of standard concentration curve
Step A, preparing a plurality of standard hydrogen peroxide solutions with different concentrations, marking the hydrogen oxide detection test paper obtained in the step 5 and the hydrogen peroxide solutions with different concentrations in a one-to-one correspondence manner, then putting the marked hydrogen oxide detection test paper into the hydrogen peroxide solution with the corresponding concentration for 1-5 seconds for color development test, and taking out the hydrogen oxide detection test paper after the test is finished to obtain test standard cards of the standard hydrogen peroxide solutions with different concentrations;
b, shooting the pictures of the test standard cards of the hydrogen peroxide solutions with different concentrations obtained in the step A through a mobile phone, and introducing the shot pictures into a color recognition APP to recognize the RGB values of the test standard cards of the hydrogen peroxide solutions with different concentrations;
and C, processing the RGB values of the test standard cards of the hydrogen peroxide solutions with different concentrations obtained in the step B, and calculating the percentage ratio of the B value in the RGB values, wherein the calculation formula is as follows: (B value/(R value + G value + B value)). times.100%;
step D, corresponding the percentage of the value B obtained in the step C to the corresponding concentration of the perhydrogenated oxygen, so as to draw a standard concentration curve and obtain a linear regression equation;
process for quantitatively testing hydrogen peroxide concentration of liquid to be tested
Step E, putting the hydrogen oxide detection test paper obtained in the step 5 into the collected liquid sample to be detected for 1-5 seconds for color development test, taking out the hydrogen oxide detection test paper after the test is finished, taking a picture of the hydrogen oxide detection test paper by a mobile phone, introducing the picture into a color recognition APP for picture RGB value recognition, and then calculating the percentage of the B value of the detection picture of the liquid sample to be detected by the calculation formula in the step C;
and F, substituting the percentage of the B value of the detection picture of the liquid sample to be detected obtained in the step E into a linear regression equation of a standard concentration curve to correspondingly calculate the concentration of the perhydrogenated oxygen in the liquid sample to be detected.
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Publication number Priority date Publication date Assignee Title
CN107694510A (en) * 2017-11-14 2018-02-16 南昌大学 A kind of two-dimensional magnetic MXene is to dyeing waste water Methylene Blue minimizing technology
CN108251054A (en) * 2018-03-23 2018-07-06 中国工程物理研究院材料研究所 A kind of composite wave-suction material and preparation method thereof
CN108630920A (en) * 2018-04-17 2018-10-09 北京化工大学 A kind of nano-metal-oxide/MXene heterojunction structure composite material and preparation methods

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Title
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