CN112730351B - Method for rapidly detecting concentration of potassium permanganate solution - Google Patents
Method for rapidly detecting concentration of potassium permanganate solution Download PDFInfo
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- CN112730351B CN112730351B CN202011439722.9A CN202011439722A CN112730351B CN 112730351 B CN112730351 B CN 112730351B CN 202011439722 A CN202011439722 A CN 202011439722A CN 112730351 B CN112730351 B CN 112730351B
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6432—Quenching
Abstract
The invention discloses a method for rapidly detecting the concentration of a potassium permanganate solution, and relates to the technical field of chemical detection. The invention discloses a method for rapidly detecting the concentration of a potassium permanganate solution, which specifically comprises the following steps: preparing a composite fluorescent probe, wherein the composite fluorescent probe takes ferroferric oxide as a core, a compact titanium dioxide layer is wrapped outside the core, then sensitized graphene quantum dots are loaded, and the outermost layer is wrapped with a nano flower-shaped silicon dioxide shell layer; establishing a standard curve; and (5) detecting. The invention discloses a method for rapidly detecting the concentration of potassium permanganate solution, which uses a composite fluorescent probe to detect the concentration of potassium permanganate, wherein the sensitivity of the composite fluorescent probe is high, the detection limit is low, and the composite fluorescent probe can be separated and recovered through a magnet after the use is finished, so that the cost is saved, and the method is more environment-friendly.
Description
Technical Field
The invention relates to the technical field of chemical detection, in particular to a method for rapidly detecting the concentration of a potassium permanganate solution.
Background
Potassium permanganate is a strong oxidant, is black purple, slender prismatic crystals or particles, and has blue metallic luster. In modern medicine, potassium permanganate hip bath is a commonly used auxiliary treatment method after perianal operation, because potassium permanganate can play a role in sterilization by oxidizing protein active genes in bacteria and interfering with the enzyme function, and the solution is used for hip bath fumigation, so that anus Zhou Chuangmian can be cleaned, and the effects of preventing infection, astringing, relieving itching and diminishing inflammation are achieved. However, when potassium permanganate is used to prepare the hip bath, the concentration needs to be strictly controlled, marks on the skin if the concentration is too high, even burns the skin, and the disinfection effect is not obvious if the concentration is too low.
In clinical care, research has shown that when nursing staff prepares the potassium permanganate hip bath liquid, partial people judge the concentration of the potassium permanganate hip bath liquid according to the color, and the other partial people prepare the potassium permanganate hip bath liquid according to the habit, so that the risk of over-high or over-low concentration of the potassium permanganate hip bath liquid is high; the existing detection methods of the concentration of the potassium permanganate solution mainly comprise a redox method, biological detection and the like, and the pretreatment process of the detection methods is complex, the analysis time is long, and more instruments are needed. Therefore, it is necessary to establish a simple, rapid and highly sensitive method for detecting potassium permanganate.
In recent years, detection of substance concentration by quenching of quantum dots has attracted attention in various fields of research as a rapid and effective detection means, but many quantum dots are difficult to recycle, and not only affect the environment but also waste resources.
Disclosure of Invention
Aiming at the problems, the invention aims to disclose a method for rapidly detecting the concentration of potassium permanganate solution, which uses a composite fluorescent probe to detect the concentration of potassium permanganate, wherein the sensitivity of the composite fluorescent probe is high, the detection limit is low, and the composite fluorescent probe can be separated and recovered through a magnet after the use is completed, so that the cost is saved, and the method is more environment-friendly.
Specifically, the invention relates to a method for rapidly detecting the concentration of a potassium permanganate solution, which specifically comprises the following steps:
s1: preparing a composite fluorescent probe, wherein the composite fluorescent probe takes ferroferric oxide as a core, a compact titanium dioxide layer is wrapped outside the core, then sensitized graphene quantum dots are loaded, and the outermost layer is wrapped with a nano flower-shaped silicon dioxide shell layer;
s2: standard curve establishment: preparing equal volumes of potassium permanganate solutions with different concentrations, respectively adding water solutions of composite fluorescent probes with the volume of V into each part of potassium permanganate solution, measuring an emission spectrum by using a fluorescence spectrophotometer, recording fluorescence intensity, taking equal volumes of water, adding the water solutions of the composite fluorescent probes with the volume of V, measuring the emission spectrum by using the fluorescence spectrophotometer, recording the fluorescence intensity, drawing a standard curve by taking the change value of the fluorescence intensity as an ordinate and the concentration of the potassium permanganate solution as an abscissa;
s2: and (3) detection: and adding the water solution of the V-volume composite fluorescent probe into the potassium permanganate solution to be measured with the same volume of the potassium permanganate standard solution, measuring the fluorescence intensity of the solution, and calculating the concentration of the potassium permanganate solution to be measured by combining the drawn standard curve.
According to the detection method disclosed by the invention, the concentration of potassium permanganate is detected by using the composite fluorescent probe, the sensitivity of the composite fluorescent probe is high, the detection limit is low, the composite fluorescent probe takes ferric oxide as a core, and the composite fluorescent probe can be separated and recovered through the magnet after the use is finished, so that the cost is saved, and the environment is protected. In addition, the compact titanium dioxide layer outside the core of the composite fluorescent probe can protect the internal ferroferric oxide on one hand, on the other hand, the titanium dioxide has an enhanced effect on the sensitized graphene quantum dots loaded on the titanium dioxide layer by utilizing the excellent optical performance of the titanium dioxide, and the nano flower-shaped silicon dioxide shell layer wrapped outside the titanium dioxide layer can protect the internal sensitized graphene quantum dots, prevent aggregation and loss of the sensitized graphene quantum dots, and the flower-shaped structure of the titanium dioxide layer also increases the contact area of the composite fluorescent probe and the potassium permanganate solution, so that the potassium permanganate can conveniently enter and exit.
Further, the sensitized graphene quantum dot is prepared from arachidonic acid grafted and modified graphene quantum dots.
The graphene quantum dots are grafted and modified by arachidonic acid, and the arachidonic acid contains a large number of double bonds in the molecules, so that the reducibility of the graphene quantum dots is improved, and the sensitivity of the graphene quantum dots to potassium permanganate is also improved.
Further, the concentration of the potassium permanganate standard solution ranges from 1X 10 -5 ～1×10 -2 mol/L。
Further, the excitation wavelength of the fluorescence spectrophotometer at the time of test is 350-365nm.
Further, in the aqueous solution of the composite fluorescent probe, the mass concentration of the composite fluorescent probe is 0.1-0.25 mg/ml.
Further, the preparation method of the composite fluorescent probe comprises the following steps:
a1: dispersing nano ferroferric oxide particles in ethanol solution by ultrasonic, adding deionized water and titanium tetraisopropoxide, continuously stirring for 20-30min, adding 25% ammonia water solution, and continuously stirring for 12h to obtain a core carrier;
a2: performing low-temperature plasma treatment on the prepared core carrier, stirring and dispersing the core carrier in deionized water, adding 3-aminopropyl triethoxysilane, heating to 45 ℃, continuously stirring and preserving heat for 2 hours, adding a sensitized graphene quantum dot solution, and continuously stirring and reacting for 5-8 hours to obtain an intermediate reaction solution;
a3: adding sodium citrate and ethyl orthosilicate into the intermediate reaction liquid, heating to 40 ℃ and stirring for reaction for 1h, adding hexamethylenetetramine, continuously stirring uniformly, immediately adding into a reaction kettle, reacting at a constant temperature of 100-105 ℃ for 7-8h, aging at a constant temperature of 80 ℃ for 4h, cooling to room temperature, filtering, washing the solid to neutrality by deionized water, and drying to obtain the composite fluorescent probe.
Sodium citrate is added into the intermediate reaction liquid and serves as a structure inducer, so that nano silicon dioxide generated by tetraethoxysilane is coated to form the outermost layer of the composite fluorescent probe, and a nano flower-shaped structure is formed.
Further, the low-temperature plasma treatment uses ammonia gas as working gas, the working pressure is 15-20pa, the discharge power is 50-65w, and the treatment time is 100-120s.
The method comprises the steps of performing low-temperature plasma treatment on a core carrier by taking ammonia gas as working gas, introducing amino groups on the surface of the core carrier, so that the core carrier presents electronegativity, and combining the effect of 3-aminopropyl triethoxysilane, so that positively sensitized graphene quantum dots can be better combined on the core carrier.
Further, the preparation method of the sensitized graphene quantum dot comprises the following steps: dissolving maleic acid and citric acid in deionized water, heating to 45 ℃, preserving heat and stirring for 10min, then placing in a reaction kettle, heating and preserving heat for 3h at 180 ℃, cooling to room temperature after the reaction is completed, adding arachidonic acid into the reaction solution, preserving heat and reacting for 1h at 65 ℃, decompressing and evaporating to dryness, dissolving the solid in deionized water, regulating the pH value to 7 by using sodium hydroxide, dialyzing for 5d by using deionized water, and freeze-drying the reactant to obtain the sensitized graphene quantum dot.
The graphene quantum dot prepared by taking maleic acid and citric acid as raw materials has good hydrophilicity and lipophilicity, and the citric acid is used as the raw materials, so that the edges of the graphene sheet contain abundant hydrophilic hydroxyl groups, and the groups can react with carboxyl groups on arachidonic acid, so that arachidonic acid is grafted on the graphene quantum dot, and a large number of double bonds are also formed on the arachidonic acid, the reducibility of the graphene quantum dot is improved, and the sensitivity of the graphene quantum dot to potassium permanganate is also improved.
The invention has the beneficial effects that:
1. the invention discloses a method for rapidly detecting the concentration of potassium permanganate solution, which uses a composite fluorescent probe to detect the concentration of potassium permanganate, wherein the sensitivity of the composite fluorescent probe is high, the detection limit is low, and the composite fluorescent probe can be separated and recovered through a magnet after the use is finished, so that the cost is saved, and the method is more environment-friendly.
2. The composite fluorescent probe is structurally designed, so that the contact area between the composite fluorescent probe and a potassium permanganate solution is increased, conventional graphene quantum dots are modified, the sensitivity of the composite fluorescent probe to potassium permanganate is improved, and the detection effect is better.
Detailed Description
The present invention will be described in detail with reference to the following specific examples:
according to the method for rapidly detecting the concentration of the potassium permanganate solution, in the detection process, the concentration of the potassium permanganate solution is detected by using a composite fluorescent probe, wherein the composite fluorescent probe takes ferroferric oxide as a core, a compact titanium dioxide layer is wrapped outside the core, sensitized graphene quantum dots are loaded, the outermost layer is wrapped with a nano flower-shaped silicon dioxide shell layer structure, and the sensitized graphene quantum dots are prepared from arachidonic acid grafted modified graphene quantum dots. The method comprises the following steps:
example 1 preparation of a Complex fluorescent Probe
Preparing sensitized graphene quantum dots: dissolving 1g of maleic acid and 0.5g of citric acid in 10ml of deionized water, heating to 45 ℃, preserving heat and stirring for 10min, placing in a reaction kettle, heating and preserving heat for 3h at 180 ℃, cooling to room temperature after the reaction is completed, adding 0.1g of arachidonic acid into the reaction liquid, heating to 65 ℃ for preserving heat and reacting for 1h, decompressing and evaporating to dryness, dissolving the solid in the deionized water, adjusting the pH to 7 with 0.5mol/L sodium hydroxide solution, dialyzing with the deionized water for 5d, replacing the deionized water every 6h, and freeze-drying the reactant after the dialysis is completed to obtain the sensitized graphene quantum dots.
Preparation of composite fluorescent probe
A1: 1.2g of nano ferroferric oxide particles are dispersed in 100ml of ethanol solution by ultrasonic, 20ml of deionized water and 100ml of 1.6mmol/L tetraisopropoxide titanium are added, stirring is continued for 25min, 18ml of 25% ammonia water solution is added, stirring is continued for 12h, and a core carrier is obtained;
a2: carrying out low-temperature plasma treatment for 120s by taking ammonia gas as working gas under the conditions that the working pressure is 15pa and the discharge power is 60w, stirring and dispersing the core carrier in 100ml of deionized water, adding 2ml of 3-aminopropyl triethoxysilane, heating to 45 ℃, continuously stirring and preserving heat for 2h, adding sensitized graphene quantum dot solution, and continuously stirring and reacting for 7h to obtain intermediate reaction liquid;
a3: adding 2.3g of sodium citrate and 3g of ethyl orthosilicate into the intermediate reaction liquid, heating to 40 ℃, stirring and reacting for 1h, adding 8g of hexamethylenetetramine, continuously stirring uniformly, immediately adding into a reaction kettle, reacting for 8h at a constant temperature of 105 ℃, aging for 4h at a temperature of 80 ℃, cooling to room temperature, filtering, washing the solid to be neutral by deionized water, and drying to obtain the composite fluorescent probe.
Example two preparation of composite fluorescent Probe 2
Preparing sensitized graphene quantum dots: dissolving 1.5g of maleic acid and 0.5g of citric acid in 12ml of deionized water, heating to 45 ℃, preserving heat and stirring for 10min, placing in a reaction kettle, heating and preserving heat for 3h at 180 ℃, cooling to room temperature after the reaction is completed, adding 0.12g of arachidonic acid into the reaction solution, heating to 65 ℃ and preserving heat for 1h, evaporating under reduced pressure to dryness, dissolving the solid in the deionized water, regulating the pH to 7 with 0.5mol/L sodium hydroxide solution, dialyzing with deionized water for 5d, replacing deionized water every 6h, and freeze-drying the reactant after the dialysis is completed to obtain the sensitized graphene quantum dots.
Preparation of composite fluorescent probe
A1: 1.2g of nano ferroferric oxide particles are dispersed in 100ml of ethanol solution by ultrasonic, 20ml of deionized water and 100ml of 1.6mmol/L tetraisopropoxide titanium are added, stirring is continued for 30min, 20ml of 25% ammonia water solution is added, and stirring is continued for 12h, so as to obtain a core carrier;
a2: performing low-temperature plasma treatment for 110s by taking ammonia gas as working gas under the conditions of working pressure of 20pa and discharge power of 50w, stirring and dispersing the core carrier in 100ml of deionized water, adding 2ml of 3-aminopropyl triethoxysilane, heating to 45 ℃, continuously stirring and preserving heat for 2h, adding sensitized graphene quantum dot solution, and continuously stirring and reacting for 8h to obtain intermediate reaction liquid;
a3: adding 2.0g of sodium citrate and 2.5g of ethyl orthosilicate into the intermediate reaction liquid, heating to 40 ℃ and stirring for reaction for 1h, adding 10g of hexamethylenetetramine, continuously stirring uniformly, immediately adding into a reaction kettle, reacting at a constant temperature of 105 ℃ for 8h, aging at a temperature of 80 ℃ for 4h, cooling to room temperature, filtering, washing the solid to neutrality by deionized water, and drying to obtain the composite fluorescent probe.
Example preparation of three Complex fluorescent probes 3
Preparing sensitized graphene quantum dots: dissolving 0.8g of maleic acid and 0.3g of citric acid in 10ml of deionized water, heating to 45 ℃, preserving heat and stirring for 10min, placing in a reaction kettle, heating and preserving heat for 3h at 180 ℃, cooling to room temperature after the reaction is completed, adding 0.1g of arachidonic acid into the reaction solution, heating to 65 ℃ and preserving heat for 1h, evaporating under reduced pressure to dryness, dissolving the solid in the deionized water, regulating the pH to 7 with 0.5mol/L sodium hydroxide solution, dialyzing with deionized water for 5d, replacing deionized water every 6h, and freeze-drying the reactant after the dialysis is completed to obtain the sensitized graphene quantum dots.
Preparation of composite fluorescent probe
A1: dispersing 1.0g of nano ferroferric oxide particles in 100ml of ethanol solution by ultrasonic, adding 15ml of deionized water and 100ml of 1.6mmol/L tetraisopropoxide titanium, continuously stirring for 20min, adding 25ml of 25% ammonia water solution, and continuously stirring for 12h to obtain a core carrier;
a2: performing low-temperature plasma treatment on the prepared core carrier for 100 seconds by taking ammonia gas as working gas under the conditions of working pressure of 18pa and discharge power of 65w, stirring and dispersing the core carrier in 100ml of deionized water, adding 2ml of 3-aminopropyl triethoxysilane, heating to 45 ℃, continuously stirring and preserving heat for 2 hours, adding sensitized graphene quantum dot solution, and continuously stirring and reacting for 5 hours to obtain intermediate reaction liquid;
a3: adding 2.1g of sodium citrate and 2.7g of ethyl orthosilicate into the intermediate reaction liquid, heating to 40 ℃ and stirring for reaction for 1h, adding 8g of hexamethylenetetramine, continuously stirring uniformly, immediately adding into a reaction kettle, reacting at a constant temperature of 100 ℃ for 7h, aging at 80 ℃ for 4h, cooling to room temperature, filtering, washing the solid to neutrality with deionized water, and drying to obtain the composite fluorescent probe.
Example Potassium permanganate solution concentration detection
S1: preparing a composite fluorescent probe, wherein the composite fluorescent probe prepared in the first embodiment is used in the present embodiment;
s2: standard curve establishment: respectively preparing the mixture with equal volume and concentration of 1 multiplied by 10 -5 mol/L、2.1×10 -4 mol/L、4.3×10 -3 mol/L、1×10 -2 Adding a volume of V aqueous solution of a compound fluorescent probe with the mass concentration of 0.1-0.25 mg/ml, preferably 0.14mg/ml, into each part of potassium permanganate solution, measuring an emission spectrum at an excitation wavelength of 350-365nm by using a fluorescence spectrophotometer, recording fluorescence intensity, adding an equal volume of water into the V aqueous solution of the compound fluorescent probe, measuring the emission spectrum by using the fluorescence spectrophotometer, recording fluorescence intensity, taking a change value of the fluorescence intensity as an ordinate, and drawing a standard curve by using the concentration of the potassium permanganate solution as an abscissa;
s2: and (3) detection: and adding the water solution of the V-volume composite fluorescent probe into the potassium permanganate solution to be measured with the same volume of the potassium permanganate standard solution, measuring the fluorescence intensity of the solution, and calculating the concentration of the potassium permanganate solution to be measured by combining the drawn standard curve.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered by the scope of the claims of the present invention. The technology, shape, and construction parts of the present invention, which are not described in detail, are known in the art.
Claims (7)
1. The method for rapidly detecting the concentration of the potassium permanganate solution is characterized by comprising the following steps of:
s1: preparing a composite fluorescent probe, wherein the composite fluorescent probe takes ferroferric oxide as a core, a compact titanium dioxide layer is wrapped outside the core, then sensitized graphene quantum dots are loaded, and the outermost layer is wrapped with a nano flower-shaped silicon dioxide shell layer;
s2: standard curve establishment: preparing equal volumes of potassium permanganate solutions with different concentrations, respectively adding water solutions of composite fluorescent probes with the volume of V into each part of potassium permanganate solution, measuring an emission spectrum by using a fluorescence spectrophotometer, recording fluorescence intensity, taking equal volumes of water, adding the water solutions of the composite fluorescent probes with the volume of V, measuring the emission spectrum by using the fluorescence spectrophotometer, recording the fluorescence intensity, drawing a standard curve by taking the change value of the fluorescence intensity as an ordinate and the concentration of the potassium permanganate solution as an abscissa;
s2: and (3) detection: taking a potassium permanganate solution to be measured, which is the same in volume as a potassium permanganate standard solution, adding a V-volume aqueous solution of a composite fluorescent probe, measuring the fluorescence intensity of the aqueous solution, and calculating the concentration of the potassium permanganate solution to be measured by combining the obtained standard curve;
the preparation method of the composite fluorescent probe comprises the following steps:
a1: dispersing nano ferroferric oxide particles in ethanol solution by ultrasonic, adding deionized water and titanium tetraisopropoxide, continuously stirring for 20-30min, adding 25% ammonia water solution, and continuously stirring for 12h to obtain a core carrier;
a2: performing low-temperature plasma treatment on the prepared core carrier, stirring and dispersing the core carrier in deionized water, adding 3-aminopropyl triethoxysilane, heating to 45 ℃, continuously stirring and preserving heat for 2 hours, adding a sensitized graphene quantum dot solution, and continuously stirring and reacting for 5-8 hours to obtain an intermediate reaction solution;
a3: adding sodium citrate and ethyl orthosilicate into the intermediate reaction liquid, heating to 40 ℃ and stirring for reaction for 1h, adding hexamethylenetetramine, continuously stirring uniformly, immediately adding into a reaction kettle, reacting at a constant temperature of 100-105 ℃ for 7-8h, aging at a constant temperature of 80 ℃ for 4h, cooling to room temperature, filtering, washing the solid to neutrality by deionized water, and drying to obtain the composite fluorescent probe.
2. The method for rapidly detecting the concentration of the potassium permanganate solution according to claim 1, wherein the sensitized graphene quantum dots are prepared from arachidonic acid grafted modified graphene quantum dots.
3. The method for rapidly detecting the concentration of the potassium permanganate solution as claimed in claim 2, wherein the concentration of the potassium permanganate standard solution is in the range of 1 x 10 -5 ～1×10 -2 mol/L。
4. A method for rapid detection of potassium permanganate solution concentration as claimed in claim 3, wherein the excitation wavelength of the fluorescence spectrophotometer at the time of test is 350-365nm.
5. The method for rapidly detecting the concentration of the potassium permanganate solution according to claim 4, wherein the mass concentration of the composite fluorescent probe in the aqueous solution of the composite fluorescent probe is 0.1-0.25 mg/ml.
6. The method for rapidly detecting the concentration of the potassium permanganate solution according to claim 5, wherein the low temperature plasma treatment uses ammonia gas as the working gas, the working pressure is 15-20pa, the discharge power is 50-65w, and the treatment time is 100-120s.
7. The method for rapidly detecting the concentration of the potassium permanganate solution according to claim 6, wherein the preparation method of the sensitized graphene quantum dots is as follows: dissolving maleic acid and citric acid in deionized water, heating to 45 ℃, preserving heat and stirring for 10min, then placing in a reaction kettle, heating and preserving heat for 3h at 180 ℃, cooling to room temperature after the reaction is completed, adding arachidonic acid into the reaction solution, preserving heat and reacting for 1h at 65 ℃, decompressing and evaporating to dryness, dissolving the solid in deionized water, regulating the pH value to 7 by using sodium hydroxide, dialyzing for 5d by using deionized water, and freeze-drying the reactant to obtain the sensitized graphene quantum dot.
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