CN112326647A - Phosphorus content detection reagent based on molybdenum trioxide and preparation method and detection method thereof - Google Patents
Phosphorus content detection reagent based on molybdenum trioxide and preparation method and detection method thereof Download PDFInfo
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- 239000011574 phosphorus Substances 0.000 title claims abstract description 110
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 110
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- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical class [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 4
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- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 229920006092 Strator® Polymers 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- DYJGATXRPZAVGS-UHFFFAOYSA-N [Sc].[Sb].[Mo] Chemical compound [Sc].[Sb].[Mo] DYJGATXRPZAVGS-UHFFFAOYSA-N 0.000 description 1
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- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 1
- 235000011180 diphosphates Nutrition 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 125000005341 metaphosphate group Chemical group 0.000 description 1
- VOGXWIXFACVZHK-UHFFFAOYSA-N molybdenum phosphoric acid vanadium Chemical compound [Mo][V].OP(O)(O)=O VOGXWIXFACVZHK-UHFFFAOYSA-N 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
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Images
Classifications
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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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems 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
- G01N21/78—Systems 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
-
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
-
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
Abstract
The invention discloses a phosphorus content detection reagent based on molybdenum trioxide and a preparation method and a detection method thereof. The detection reagent comprises molybdenum trioxide nanosheet dispersion liquid and ascorbic acid solution; the detection method comprises the following steps: mixing a detection reagent with a sample to be detected, and then comparing the mixture with a total phosphorus standard colorimetric card; or obtaining a standard curve through the total phosphorus standard solution; and finally, measuring the absorbance value of the solution obtained by mixing the detection reagent and the sample to be detected, and obtaining the corresponding phosphorus content through a standard curve. The detection method does not need complex pretreatment steps such as centrifugation, extraction, concentration and the like, is simple and convenient to operate, has high sensitivity, and has the lowest detection limit of 1.2 mug/L.
Description
Technical Field
The invention belongs to the technical field of water quality detection, and particularly relates to a molybdenum trioxide-based phosphorus content detection reagent capable of being visualized quickly, and a preparation method and a detection method thereof.
Background
The total phosphorus is the result of the determination after various forms of phosphorus are converted into orthophosphate by digestion of a water sample, and is measured by the mg of phosphorus contained in each liter of water sample. In water, phosphorus can exist in the forms of elemental phosphorus, orthophosphate, condensed phosphate, pyrophosphate, metaphosphate, organic group-bound phosphate and the like, and the main sources of the phosphorus are domestic sewage, chemical fertilizers, organic phosphorus pesticides, phosphate builders used in modern detergents and the like. Phosphates can interfere with the coagulation process in waterworks. Phosphorus in the water body is a key element required by the growth of algae, and excessive phosphorus is a main reason for causing the pollution and the foreign odor of the water body, causing the eutrophication of lakes and the red tide of gulf.
There are 3 common methods for assaying orthophosphate: firstly, a vanadium-molybdenum-phosphoric acid colorimetric method has lower sensitivity but less interfering substances; ② the molybdenum-stibium-scandium colorimetric method has high sensitivity, stable color and good repeatability. ③ stannous chloride method; the product is sensitive but has poor stability and is interfered by chloride ions, sulfate and the like. Therefore, the method for detecting total phosphorus, which is cheap in instrument price, simple and convenient in detection operation, sensitive and efficient, has important practical value.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a phosphorus content detection reagent based on molybdenum trioxide and a preparation method and a detection method thereof, which effectively solve the problems that the detection method in the prior art is complex and inconvenient to popularize; the method is simple and convenient to operate, sensitive and efficient.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows:
a phosphorus content detection reagent based on molybdenum trioxide comprises molybdenum trioxide nanosheet dispersion liquid and ascorbic acid solution in a volume ratio of 1.5-3: 0.5-1.
Further, the preparation method of the molybdenum trioxide nanosheet dispersion liquid comprises the following steps:
fully grinding commercially available molybdenum trioxide powder, further crushing and dispersing the powder by using ultrasound, centrifuging to remove solid precipitates, and obtaining supernatant which is a dispersion liquid containing a large amount of molybdenum trioxide nanosheets, wherein the grinding-ultrasonic method comprises the steps of grinding 0.1-10.0g of commercially available molybdenum trioxide powder in a mortar for 30-120 minutes, transferring all the ground powder into 30-1000mL of pure water, then performing ultrasound for 2 hours, and finally obtaining the molybdenum trioxide nanosheet dispersion liquid with a certain concentration by standing or centrifuging.
Further, the preparation of the molybdenum trioxide nanosheet dispersion preferably comprises grinding 4.0g of commercially available molybdenum trioxide powder for 1 hour, adding into 500mL of pure water, ultrasonically dispersing for 2 hours, and centrifuging at 6000 rpm for 10 minutes to obtain a supernatant, i.e., the molybdenum trioxide nanosheet dispersion.
Further, the ultrasonic temperature is 30 ℃, the power is 100W, and the ultrasonic time is 2 h.
Further, the grinding time was 1 h.
Further, the volume ratio of the molybdenum trioxide nanosheet dispersion to the ascorbic acid solution was 3: 1.
Further, the concentration of the ascorbic acid solution is 70-176 mg/mL; the concentration of the molybdenum trioxide nanosheet dispersion liquid is 1.5-8 mg/mL.
A preparation method of a standard colorimetric card for rapidly and visually monitoring total phosphorus comprises the following steps:
(1) preparing a total phosphorus standard solution, and then diluting the total phosphorus standard solution into total phosphorus to-be-detected solutions with different concentrations; the concentration of the diluted total phosphorus to be detected is 0.2mg/L, 0.6mg/L, 1mg/L, 2mg/L and 5mg/L respectively;
the total phosphorus can be selected from one or more of three orthophosphoric acid salts of sodium phosphate, disodium hydrogen phosphate and sodium dihydrogen phosphate to be prepared into a total phosphorus standard solution, and then the total phosphorus standard solution is diluted into a series of total phosphorus to-be-detected solutions with different concentrations;
(2) respectively mixing the detection reagent and the solution to be detected obtained in the step (1) according to the volume ratio of 1-2: 1.5-3, standing for 15-20 min in a room temperature environment, and recording the color of the mixed solution by using a mobile phone or a digital camera;
(3) and (3) extracting the RGB value of the image obtained in the step (2) through a mobile phone App or computer software, and establishing a total phosphorus standard colorimetric card according to the RGB value.
Further, the method also comprises the step (4): establishing a standard curve of total phosphorus;
and (4) measuring the absorbance of the reaction liquid obtained in the step (3) in the range of 600 nm-1000 nm by using an ultraviolet-visible spectrophotometer, and fitting a standard curve of the absorbance and the total phosphorus concentration.
Further, the picture is taken by a mobile phone or a digital camera and is obtained by utilizing software developed by the mobile phone App or Adobell μ strator, ImageJ, Adobe Photoshop and the like.
Further, the concentration of the total phosphorus standard solution is 1 mg/mL; the concentration of the total phosphorus solution to be tested is 0.1-5.0 mg/L.
Further, the volume ratio of the detection reagent to the liquid to be detected is 3: 2.
Further, in the step (2), the color is recorded in a picture form, the RGB value in the picture is extracted through the mobile terminal, and then the standard colorimetric card is established according to the extracted RGB value.
A method for detecting total phosphorus in water by using the detection reagent comprises the following steps:
uniformly mixing the detection reagent and a sample to be detected according to the volume ratio of 3:2, and then measuring by using an ultraviolet-visible spectrophotometer or a colorimeter, or comparing with a total phosphorus standard color card.
Rapid in-situ measurement of total phosphorus: taking 0.5mL of the molybdenum trioxide nanosheet dispersion liquid to a colorimetric tube, then dropwise adding 9 drops (about 0.17mL) of ascorbic acid solution and the molybdenum trioxide nanosheet dispersion liquid, uniformly mixing, sampling 0.45mL of the solution to be detected on site in the reaction tube, and performing control detection with a total phosphorus colorimetric card after 15 minutes.
Laboratory measurement of total phosphorus: taking 1.0mL of molybdenum trioxide nanosheet dispersion liquid to a colorimetric tube, then uniformly mixing 0.35mL of ascorbic acid solution and the molybdenum trioxide nanosheet dispersion liquid, taking 0.9mL of to-be-detected liquid to a reaction tube, measuring absorption intensity by using an ultraviolet-visible spectrophotometer after 15 minutes, and calculating the total phosphorus concentration.
The utility model provides a kit for detecting total phosphorus in environmental water sample, includes water sample receiving flask, above-mentioned detect reagent, colour comparison tube and above-mentioned total phosphorus standard colour comparison card that awaits measuring.
Wherein, the water sample collecting bottle to be detected is a bottle with a cover of 10-500mL, and the material of the bottle can be plastic, glass, metal and alloy.
The detection reagent consists of molybdenum trioxide nanosheet dispersion liquid and ascorbic acid solution;
the colorimetric cylinder is a 1.8mL plastic bottle with a screwed cover, and can also be a glass bottle.
The invention has the beneficial effects that:
the invention establishes a method for detecting the total phosphorus content in an environmental water sample, wherein the total phosphorus sample reacts in a light yellow color developing solution formed by ascorbic acid aqueous solution and molybdenum trioxide to generate a colored derivative, the absorption intensity of the derivative is directly measured by an ultraviolet-visible spectrophotometer, and the linear relation between the total phosphorus content and the absorption intensity of the corresponding derivative is established.
The detection method does not need complex pretreatment steps such as centrifugation, extraction, concentration and the like, and meanwhile, the derivative formed by the light yellow color developing solution formed by the total phosphorus, the ascorbic acid aqueous solution and the molybdenum trioxide can stably exist, and the derivative has good specificity, specific wavelength and strong anti-interference capability.
The detection method has higher sensitivity, and the detection limit is as low as 1.2 mug/L. In addition, the reaction is a color-changing reaction, the color is changed from light yellow to blue before and after the reaction, the color is obviously changed, whether phosphorus and content are contained or not can be judged by batch quick detection and coarse screening, the detection time is saved, meanwhile, the detection method is stable, the prices of related reaction raw materials are not high, and the detection requirements of governments, common enterprises and institutions can be met.
Drawings
FIG. 1 is a digital picture, a standard color and RGB values of a molybdenum trioxide nanosheet dispersion obtained in example 1 after mixing of a first reagent and a second reagent and development of different total phosphorus concentrations (0.2, 0.6, 1, 2, 5 mg/L);
FIG. 2 is a graph showing UV absorption spectra after color development at different total phosphorus concentrations (0 to 5mg/L) in example 1;
FIG. 3 is the standard curve obtained in example 1;
FIG. 4 is a digital picture, a standard color and RGB values of a molybdenum trioxide nanosheet dispersion obtained in example 2 after mixing of the first and second reagents and development of different total phosphorus concentrations (0.2, 0.6, 1, 2, 5 mg/L);
FIG. 5 is a graph showing UV absorption spectra after color development at different total phosphorus concentrations (0-5mg/L) in example 2;
FIG. 6 is the standard curve obtained in example 2;
FIG. 7 is a digital picture, a standard color and RGB values of a molybdenum trioxide nanosheet dispersion obtained in example 3 after mixing of the first and second reagents and development of different total phosphorus concentrations (0.2, 0.6, 1, 2, 5 mg/L);
FIG. 8 is a graph showing UV absorption spectra after color development at different total phosphorus concentrations (0-5mg/L) in example 3;
FIG. 9 is the standard curve obtained in example 3;
fig. 10 is a picture of verifying the accuracy of the color chart in example 4.
Detailed Description
The following description of the embodiments of the present invention is provided to facilitate the understanding of the present invention by those skilled in the art, but it should be understood that the present invention is not limited to the scope of the embodiments, and it will be apparent to those skilled in the art that various changes may be made without departing from the spirit and scope of the invention as defined and defined in the appended claims, and all matters produced by the invention using the inventive concept are protected.
Example 1
A method for detecting total phosphorus in an environmental water sample by adopting a phosphorus content detection reagent based on molybdenum trioxide comprises the following steps:
(1) preparing a normal phosphate standard stock solution: accurately weighing 10.0mg of sodium phosphate, disodium hydrogen phosphate or sodium dihydrogen phosphate, dissolving with ultrapure water, adding into a 10mL glass bottle, adding water to a constant volume, and preparing into 1mg/mL normal phosphate standard stock solution; diluting the total phosphorus standard stock solution by ultrapure water step by step into total phosphorus solution to be detected with the concentration of 0mg/L, 0.2mg/L, 0.4mg/L, 0.6mg/L, 0.8mg/L, 1.0mg/L, 1.2mg/L, 1.6mg/L, 2.0mg/L, 5.0mg/L and 10.0mg/L respectively for later use;
(2) grinding 4g of molybdenum trioxide (CAS: 1313-27-5) for 30-60 min, dissolving in 500mL of water, centrifuging at 6000 rpm, collecting supernatant obtained by centrifugation, and obtaining molybdenum trioxide nanosheet dispersion liquid with the concentration of 8 mg/mL; dissolving 8.8g of L-ascorbic acid in 50mL of water to obtain a solution with the concentration of 176mg/mL, and adding 0.3mL of L-ascorbic acid solution into 1mL of molybdenum trioxide nanosheet dispersion to form a light yellow total phosphorus detection reagent;
taking 1.5mL of the solution to be tested (0mg/L, 0.2mg/L, 0.4mg/L, 0.6mg/L, 0.8mg/L, 1.0mg/L, 1.2mg/L, 1.6mg/L, 2.0mg/L, 5.0mg/L and 10.0mg/L) of the orthophosphate with different concentrations in the step (1), respectively adding 1.5mL of light yellow color development solution into the solution to perform reaction, and reacting for 15min to 30min at the temperature of between 25 and 30 ℃.
The reaction solution is blue, after the reaction is finished, ultraviolet-visible spectrophotometry detection is respectively carried out on the generated derivatives, the initial wavelength is set to be 600nm, the final wavelength is set to be 1000nm, and a series of corresponding absorption intensities are measured;
(3) a series of different concentrations (0mg/L, 0.1mg/L, 0.2mg/L, 0.3mg/L, 0.4mg/L, 0.5mg/L, 0.6mg/L, 0.8mg/L, 1.0mg/L, 2.5mg/L and 5.0mg/L) of the orthophosphate solution to be tested are used as abscissa, and the corresponding obtained absorption intensity is used as ordinate to draw a standard curve, wherein the standard curve is shown in figure 3. As can be seen from fig. 3, the linear relation between the total phosphorus concentration and the absorption intensity obtained is represented by y, 0.5799x +0.2825, and the square R of the correlation coefficient of the linear relation2Is 0.9975.
(4) And (3) taking an environmental water sample (the environmental water sample is from a pond, a lake and a river) for detection, repeating the step (2), replacing the solution to be detected of the orthophosphoric acid salt in the step (2) with the environmental water sample for reaction, detecting by using an ultraviolet-visible light photometer after the reaction is finished to obtain the absorption intensity of the environmental water sample, substituting the numerical value of the absorption intensity of the environmental water sample into the linear relation obtained in the step (3), calculating the content of total phosphorus in the environmental water sample, measuring two parts in parallel, and averaging.
The derivative is detected by stepwise dilution, the detection limit and the quantitative limit of the method are determined by a standard deviation method, and the result shows that the detection limit of the method is 1.2 mug/L; the total phosphorus concentration is in the range of 0.1mg/L to 5.0mg/LGood linearity of inside of the enclosure (R)20.9975); the method has high sensitivity, and the detection limit is as low as 1.2 mug/L.
The low, medium and high levels of total phosphorus content were added to the blank water sample for precision experiments-standard recovery tests, which were performed in parallel 6 times, and the average recovery and RSD data are shown in Table 1.
TABLE 1 precision experimental data
Example 2
A method for detecting total phosphorus in an environmental water sample by adopting a phosphorus content detection reagent based on molybdenum trioxide comprises the following steps:
(1) preparing a normal phosphate standard stock solution: accurately weighing 10.0mg of sodium phosphate, disodium hydrogen phosphate or sodium dihydrogen phosphate, dissolving with ultrapure water, adding into a 10mL glass bottle, adding water to a constant volume, and preparing into 1mg/mL normal phosphate standard stock solution; diluting the total phosphorus standard stock solution by ultrapure water step by step into total phosphorus solution to be detected with the concentration of 0mg/L, 0.2mg/L, 0.4mg/L, 0.6mg/L, 0.8mg/L, 1.0mg/L, 1.2mg/L, 1.6mg/L, 2.0mg/L, 5.0mg/L and 10.0mg/L respectively for later use;
(2) grinding 4g of molybdenum trioxide (CAS: 1313-27-5) by using a mortar for 30-60 min, dissolving the molybdenum trioxide in 500mL of water, centrifuging at the speed of 6000 rpm, collecting supernatant obtained by centrifuging, and obtaining molybdenum trioxide nanosheet dispersion liquid with the concentration of 8 mg/mL; dissolving 3.5g of L-ascorbic acid in 50mL of water to obtain a solution with the concentration of 70mg/mL, and adding 0.3mL of L-ascorbic acid solution into 1mL of molybdenum trioxide nanosheet dispersion to form a light yellow total phosphorus detection reagent;
respectively taking 1.5mL of the solution to be detected of the orthophosphate with different concentrations in the step (1) (0mg/L, 0.2mg/L, 0.4mg/L, 0.6mg/L, 0.8mg/L, 1.0mg/L, 1.2mg/L, 1.6mg/L, 2.0mg/L, 5.0mg/L and 10.0mg/L), respectively adding 1.5mL of light yellow color development solution into the solution to perform reaction, and reacting for 15min at the temperature of between 25 and 30 ℃;
the reaction solution is blue, after the reaction is finished, ultraviolet-visible spectrophotometry detection is respectively carried out on the generated derivatives, the initial wavelength is set to be 600nm, the final wavelength is set to be 1000nm, and a series of corresponding absorption intensities are measured;
(3) a series of different concentrations (0mg/L, 0.1mg/L, 0.2mg/L, 0.3mg/L, 0.4mg/L, 0.5mg/L, 0.6mg/L, 0.8mg/L, 1.0mg/L, 2.5mg/L and 5.0mg/L) of the orthophosphate solution to be tested are used as abscissa, and the corresponding obtained absorption intensity is used as ordinate to draw a standard curve, wherein the standard curve is shown in figure 6. As can be seen from fig. 6, the linear relation between the total phosphorus concentration and the absorption intensity obtained is y-0.4046 x +0.2089, and the square R of the correlation coefficient of the linear relation is2Is 0.9987.
(4) And (3) taking an environmental water sample (the environmental water sample is from a pond, a lake and a river) for detection, repeating the step (2), respectively replacing the solution to be detected of the orthophosphate in the step (2) with the environmental water sample for derivatization reaction, detecting by using an ultraviolet-visible light photometer after the reaction is finished to obtain the absorption intensity of the environmental water sample, substituting the numerical value of the absorption intensity of the environmental water sample into the linear relation formula obtained in the step (3), calculating the content of total phosphorus in the environmental water sample, measuring two parts in parallel, and averaging.
The derivative is detected by stepwise dilution, the detection limit and the quantitative limit of the method are determined by a standard deviation method, and the result shows that the detection limit of the method is 1.7 mug/L; the total phosphorus concentration is in the range of 0.1 mg/L-5.0 mg/L with good linearity (R2＝0.9987)。
The low, medium and high levels of total phosphorus content were added to the blank water sample for precision experiments-standard recovery tests, which were performed in parallel 6 times, and the average recovery and RSD data are shown in Table 2.
TABLE 2 precision experimental data
Example 3
A method for detecting total phosphorus in an environmental water sample by adopting a phosphorus content detection reagent based on molybdenum trioxide comprises the following steps:
(1) preparing a normal phosphate standard stock solution: accurately weighing 10.0mg of sodium phosphate, disodium hydrogen phosphate or sodium dihydrogen phosphate, dissolving with ultrapure water, adding into a 10mL glass bottle, adding water to a constant volume, and preparing into 1mg/mL normal phosphate standard stock solution; diluting the total phosphorus standard stock solution by ultrapure water step by step into total phosphorus solution to be detected with the concentration of 0mg/L, 0.2mg/L, 0.4mg/L, 0.6mg/L, 0.8mg/L, 1.0mg/L, 1.2mg/L, 1.6mg/L, 2.0mg/L, 5.0mg/L and 10.0mg/L respectively for later use;
(2) grinding 4g of molybdenum trioxide (CAS: 1313-27-5) by using a mortar for 30-60 min, dissolving the molybdenum trioxide in 500mL of water, centrifuging at 6000 rpm, and collecting supernatant obtained by centrifuging to obtain molybdenum trioxide nanosheet dispersion liquid with the concentration of 8 mg/mL; dissolving 7.1g of L-ascorbic acid in 50mL of water to obtain a solution with the concentration of 142mg/mL, and adding 0.3mL of L-ascorbic acid solution into 1mL of molybdenum trioxide nanosheet dispersion to form a light yellow total phosphorus detection reagent;
taking 1.5mL of the solutions to be tested (0mg/L, 0.2mg/L, 0.4mg/L, 0.6mg/L, 0.8mg/L, 1.0mg/L, 1.2mg/L, 1.6mg/L, 2.0mg/L, 5.0mg/L and 10.0mg/L) of the orthophosphate with different concentrations in the step (1), respectively adding 1.5mL of light yellow color development solution into the solutions to carry out reaction, and carrying out reaction for 15min at the temperature of between 25 and 30 ℃.
The reaction solution is blue, after the reaction is finished, ultraviolet-visible spectrophotometry detection is respectively carried out on the generated derivatives, the initial wavelength is set to be 600nm, the final wavelength is set to be 1000nm, and a series of corresponding absorption intensities are measured;
(3) and drawing a standard curve by taking a series of different concentrations (0mg/L, 0.1mg/L, 0.2mg/L, 0.3mg/L, 0.4mg/L, 0.5mg/L, 0.6mg/L, 0.8mg/L, 1.0mg/L, 2.5mg/L and 5.0mg/L) of the solution to be detected of the orthophosphate as an abscissa and the absorption intensity obtained correspondingly as an ordinate, wherein the standard curve is shown in figure 9. As can be seen from FIG. 9, the total phosphorus obtainedThe linear relation between the concentration and the absorption intensity is that y is 0.4891x +0.2575, and the square R of the correlation coefficient of the linear relation is2Is 0.9990.
(4) And (3) taking an environmental water sample (the environmental water sample is from a pond, a lake and a river) for detection, repeating the step (2), replacing the solution to be detected of the orthophosphate in the step (2) with the environmental water sample for derivatization reaction, detecting by using an ultraviolet-visible light photometer after the reaction is finished to obtain the absorption intensity of the environmental water sample, substituting the numerical value of the absorption intensity of the environmental water sample into the linear relation formula obtained in the step (3), calculating the content of total phosphorus in the environmental water sample, measuring two parts in parallel, and averaging.
The derivative is detected by stepwise dilution, the detection limit and the quantitative limit of the method are determined by a standard deviation method, and the result shows that the detection limit of the method is 1.4 mug/L; the total phosphorus concentration is in the range of 0.1 mg/L-5.0 mg/L with good linearity (R2＝0.9990)。
The low, medium and high levels of total phosphorus content were added to the blank water sample for precision experiments-standard recovery tests, which were performed in parallel 6 times, and the average recovery and RSD data are shown in table 3.
TABLE 3 precision experimental data
Example 4
A method for detecting total phosphorus in an environmental water sample by adopting a phosphorus content detection reagent based on molybdenum trioxide comprises the following steps:
(1) preparing a normal phosphate standard stock solution: accurately weighing 10.0mg of sodium phosphate, disodium hydrogen phosphate or sodium dihydrogen phosphate, dissolving with ultrapure water, adding into a 10mL glass bottle, adding water to a constant volume, and preparing into 1mg/mL normal phosphate standard stock solution; diluting the total phosphorus standard stock solution by ultrapure water step by step into total phosphorus solution to be detected with the concentration of 0mg/L, 0.2mg/L, 0.4mg/L, 0.6mg/L, 0.8mg/L, 1.0mg/L, 1.2mg/L, 1.6mg/L, 2.0mg/L, 5.0mg/L and 10.0mg/L respectively for later use;
(2) grinding 4g of molybdenum trioxide (CAS: 1313-27-5) for 30-60 min, dissolving in 500mL of water, centrifuging at 6000 rpm, collecting supernatant obtained by centrifugation, and obtaining molybdenum trioxide nanosheet dispersion liquid with the concentration of 8 mg/mL; dissolving 8.8g of L-ascorbic acid in 50mL of water to obtain a solution with the concentration of 176mg/mL, and adding 0.3mL of L-ascorbic acid solution into 1mL of molybdenum trioxide nanosheet dispersion to form a light yellow total phosphorus detection reagent;
(3) respectively mixing the standard total phosphorus solution to be detected with a detection reagent according to the volume ratio of 2:3, standing at room temperature for 15min, and recording the color of the mixed solution by using a mobile phone or a digital camera;
(4) extracting RGB values of the image obtained in the step (3) through a mobile phone App or computer software, setting color blocks corresponding to the RGB values in a conventional mode, and printing and cutting to obtain corresponding standard color comparison cards, wherein the color comparison cards with different colors represent phosphorus contents with different concentrations, and the color of each color comparison card is determined according to actual conditions;
(5) uniformly mixing the prepared total phosphorus detection reagent with an environmental water sample (the environmental water sample is from a pond, a lake and a river) according to a volume ratio of 3:2 to obtain a sample to be detected;
(6) and (4) comparing the sample obtained in the step (5) with a total phosphorus standard colorimetric card, and obtaining the total phosphorus in the water sample through color comparison.
Meanwhile, the accuracy verification of the colorimetric card rapid measurement method is performed by adding low, medium and high levels of total phosphorus content to a blank water sample, and the comparison result is shown in fig. 10. The color of the solution is close to that of a total phosphorus color comparison card with corresponding concentration, which shows that the color comparison card mode analysis has good accuracy, and the minimum analysis concentration of the color comparison card analysis method can be 0.2 mg/L.
Claims (9)
1. A phosphorus content detection reagent based on molybdenum trioxide is characterized by comprising a molybdenum trioxide nanosheet dispersion liquid and an ascorbic acid solution which are mixed in a volume ratio of 1.5-3: 0.5-1.
2. The molybdenum trioxide-based phosphorus content detection reagent according to claim 1, wherein the preparation method of the molybdenum trioxide nanosheet dispersion comprises:
grinding molybdenum trioxide powder for 1-2 h, adding a solvent for dissolving, carrying out ultrasonic grinding for 1-5 h at the temperature of 20-50 ℃ under the condition of 40-100W, separating, and collecting an upper layer separation solution.
3. The molybdenum trioxide-based phosphorus content detection reagent according to claim 2, wherein the ultrasonic temperature is 30 ℃, the power is 100W, and the ultrasonic time is 2 h.
4. The molybdenum trioxide-based phosphorus content detection reagent according to claim 1, wherein the volume ratio of the molybdenum trioxide nanosheet dispersion to the ascorbic acid solution is 3: 1.
5. The molybdenum trioxide-based phosphorus content detection reagent according to claim 1, wherein the concentration of the ascorbic acid solution is 70 to 176 mg/mL; the concentration of the molybdenum trioxide nanosheet dispersion liquid is 1.5-8 mg/mL.
6. A preparation method of a standard colorimetric card for rapidly and visually monitoring total phosphorus is characterized by comprising the following steps:
(1) preparing a total phosphorus standard solution, and then diluting the total phosphorus standard solution into total phosphorus to-be-detected solutions with different concentrations;
(2) mixing the detection reagent of the right 1 with the solution to be detected obtained in the step (1) according to a volume ratio of 1.5-3: 1-2, standing for 15-20 min in a room temperature environment, and recording the color respectively;
(3) and (3) establishing a total phosphorus standard colorimetric card according to the color obtained in the step (2).
7. The method for preparing the standard colorimetric card for rapid visual monitoring of total phosphorus according to claim 6, wherein the volume ratio of the detection reagent to the solution to be detected is 3: 2.
8. The method for preparing the standard colorimetric card for rapid visual monitoring of total phosphorus according to claim 6, wherein in the step (2), the color is recorded in a form of a picture, the RGB values in the picture are extracted through a mobile terminal, and then the standard colorimetric card is established according to the extracted RGB values.
9. A method for detecting total phosphorus in a body of water using the detection reagent of claim 1, comprising the steps of:
mixing a detection reagent and a sample to be detected in a volume ratio of 1-2: 1.5-3, and then comparing the mixture with the total phosphorus standard colorimetric card of claim 6; or
Preparing total phosphorus standard solution, and diluting the total phosphorus standard solution into total phosphorus solution to be tested with different concentrations; mixing the detection reagent of claim 1 with total phosphorus solution to be detected according to a volume ratio of 1.5-3: 1-2, and then measuring absorbance to obtain a corresponding standard curve;
and finally, measuring the absorbance value of the solution obtained by mixing the detection reagent and the sample to be detected in a volume ratio of 1-2: 1.5-3, and obtaining the corresponding phosphorus content through a standard curve.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113820305A (en) * | 2021-09-30 | 2021-12-21 | 盈奇科技（深圳）有限公司 | Total phosphorus detection equipment and method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106841188A (en) * | 2017-03-01 | 2017-06-13 | 福建医科大学 | A kind of paper micro-fluidic chip that intracellular hydrogen peroxide is detected for nanoscale molybdenum oxide analogue enztme |
| CN108003864A (en) * | 2017-12-04 | 2018-05-08 | 西南科技大学 | A kind of luminol lighting function nm-class boron nitride and preparation method thereof |
| CN108344731A (en) * | 2017-01-21 | 2018-07-31 | 王斌 | A kind of detection method for measuring quantity of cadmium release in domestic ceramics |
| CN109030440A (en) * | 2018-07-18 | 2018-12-18 | 西北农林科技大学 | A method of based on molybdenum trioxide quantum dots characterization tannin acid content |
| CN111690406A (en) * | 2020-07-09 | 2020-09-22 | 长江师范学院 | Preparation method and application of optical property-adjustable molybdenum oxide quantum dots |
-
2020
- 2020-11-05 CN CN202011223782.7A patent/CN112326647A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108344731A (en) * | 2017-01-21 | 2018-07-31 | 王斌 | A kind of detection method for measuring quantity of cadmium release in domestic ceramics |
| CN106841188A (en) * | 2017-03-01 | 2017-06-13 | 福建医科大学 | A kind of paper micro-fluidic chip that intracellular hydrogen peroxide is detected for nanoscale molybdenum oxide analogue enztme |
| CN108003864A (en) * | 2017-12-04 | 2018-05-08 | 西南科技大学 | A kind of luminol lighting function nm-class boron nitride and preparation method thereof |
| CN109030440A (en) * | 2018-07-18 | 2018-12-18 | 西北农林科技大学 | A method of based on molybdenum trioxide quantum dots characterization tannin acid content |
| CN111690406A (en) * | 2020-07-09 | 2020-09-22 | 长江师范学院 | Preparation method and application of optical property-adjustable molybdenum oxide quantum dots |
Non-Patent Citations (3)
| Title |
|---|
| 李银峰 等,: "《碳纳米材料制备及其应用研究》", 31 March 2019 * |
| 杜佳艳: "基于三氧化钼的比色传感体系构建及应用研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
| 柴波 等: "基于Android平台的母乳成分多指标试纸检测软件的设计", 《中国医学装备》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113820305A (en) * | 2021-09-30 | 2021-12-21 | 盈奇科技（深圳）有限公司 | Total phosphorus detection equipment and method |
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