CN113125429B - Nano silver colorimetric sensor and preparation method and application thereof - Google Patents
Nano silver colorimetric sensor and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a nano silver colorimetric sensor and a preparation method and application thereof, belonging to the technical fields of environmental science, inspection chemistry and analytical chemistrySilver salt is used as a silver nanoparticle source, nitrilotriacetic acid trisodium salt is used as a ligand, other reducing agents are added, and the reaction is carried out under the condition of stirring at room temperature, so that the stable water-soluble nano silver colorimetric sensor is obtained. The sensor of the invention has a series of advantages of portability, high sensitivity, strong selectivity, good stability and the like, and can realize Cr 3+ The rapid detection of the trivalent chromium ion has the advantages of high detection speed, high sensitivity and the like, can effectively solve the problems of strict sample preservation condition, high analysis method cost, long analysis time and strong operation speciality existing in the existing trivalent chromium ion detection technology, and has wide application prospect and high market application value.
Description
Technical Field
The invention relates to the technical fields of environmental science, inspection chemistry and analytical chemistry, in particular to a nano silver colorimetric sensor and a preparation method and application thereof.
Background
In general, chromium is widely present in nature in two forms of Cr (III) and Cr (VI), and trivalent chromium and hexavalent chromium in the environment can be converted to each other. Wherein, trace Cr (III) is a trace element necessary for human body and plays an important role in the metabolism of sugar and lipid in the body. However, excessive intake of Cr (III) shows a cytotoxic reaction, and even causes mutation and cancer, and Cr (III) has a certain teratogenic effect. As trivalent chromium is increasingly applied to industrial production such as electroplating, leather production, metal processing and the like, the exceeding of the content causes harm to human bodies. Therefore, there is a great need for a rapid, convenient and sensitive method for detecting trivalent chromium ions in aqueous solutions.
Currently, the commonly used trivalent chromium ion detection and analysis instruments mainly comprise an electric coupling plasma emission spectrometer (ICP), atomic Absorption (AAS), atomic fluorescence Absorption (AFS) and the like. However, most of the detection methods have the defects of strict sample storage conditions, high cost of an analysis method, long analysis time, strong operation specialization and the like. In view of this, it would be of great interest to provide a sensor for rapid, sensitive, visual detection and analysis of trivalent chromium ions.
Disclosure of Invention
Aiming at the defects or shortcomings, the invention aims to provide a nano silver colorimetric sensor and a preparation method and application thereof, which can effectively solve the problems of strict sample preservation condition, high analysis method cost, long analysis time and strong operation speciality in the existing trivalent chromium ion detection technology.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a nano silver colorimetric sensor, which specifically comprises the following steps: and (3) sequentially adding the trisodium nitrilotriacetate solution and the reducing agent into the silver salt solution under the stirring state at room temperature, and continuously stirring to obtain a light yellow solution, thus obtaining the nano silver colorimetric sensor.
Further, the molar ratio of the silver salt, the trisodium nitrilotriacetate and the reducing agent in the silver salt solution is 1:1-8:10-30, preferably 1:1:26.
Further, the silver salt solution is one or more of silver nitrate solution, silver fluoride solution and silver ammonia solution.
Further, the reducing agent is one or more of sodium borohydride, ascorbic acid, citric acid, citrate, tannic acid, glucose and oxalic acid.
Further, the stirring is continued for 20 to 40 minutes, preferably 30 minutes, after sequentially adding the trisodium nitrilotriacetate solution and the reducing agent to the silver salt solution.
The invention also provides the nano silver colorimetric sensor prepared by the preparation method.
Further, the maximum absorption peak of the ultraviolet visible light of the nano silver colorimetric sensor is 380-420nm, and the particle size is 10-100 nm.
The invention also provides application of the nano silver colorimetric sensor in trivalent chromium ion detection.
Further, the specific process of the application of the nano silver colorimetric sensor in trivalent chromium ion detection is as follows: placing a certain amount of nano silver colorimetric sensor into a container, adding a sample to be detected with the same volume into the container, shaking uniformly, standing for 1-30 min, and observing the color change of the mixed solution or detecting the mixed solutionThe change of the ultraviolet visible absorption spectrum can realize the Cr 3+ And (5) performing qualitative and quantitative analysis.
Further, the macroscopic detection limit of the nano silver colorimetric sensor for trivalent chromium ions is 1.5 mu M, and the detection limit of an ultraviolet-visible spectrometer (Uv-Vis) is 0.4 mu M; when Cr 3+ When the concentration of (2) is 1.5 mu M-5 mu M, the color of the solution is changed from light yellow to blue-violet; when Cr 3+ At a concentration of greater than 5 μm, the color of the solution changes from pale yellow to orange-red; when Cr 3+ At a concentration of 0.4 μm or more, the characteristic absorption peak of the ultraviolet visible spectrum is red shifted.
The invention has the following advantages:
1. the invention provides a preparation method of a nano silver colorimetric sensor, which is characterized in that silver salt is used as a silver nanoparticle source, nitrilotriacetic acid trisodium salt is used as a ligand, and a reducing agent is added, so that the stable water-soluble nano silver colorimetric sensor is obtained under stirring at room temperature; the preparation method is different from the prior nano gold or nano silver prepared by a hydrothermal reduction method, does not need additional experimental conditions such as heating, is simpler and safer, and has more stable storage because the nano silver prepared by introducing other reducing agents has smaller particle size than the nano silver prepared by the hydrothermal reduction method;
2. the nano silver colorimetric sensor provided by the invention can realize Cr comparison 3+ The rapid detection of the method has a series of advantages of high sensitivity, strong selectivity, portability, good stability and the like, the detection limit which can be distinguished by naked eyes is 1.5 mu M, and the detection limit can reach 0.4 mu M by using an ultraviolet-visible spectrometer (Uv-Vis); and different from other nano gold colorimetric sensors or nano silver colorimetric sensors in the past, only single color change occurs, and the nano silver colorimetric sensor prepared by the invention is based on Cr in the solution to be detected 3+ Will produce different color changes, i.e. Cr can be determined from the color changes 3+ Concentration interval of (2) and then according to standard curve method, for Cr 3+ The concentration is subjected to more accurate quantitative analysis, the accuracy of the quantitative analysis is improved, and the method has wide application prospect and high market application in the fields of environmental science, inspection chemistry, analysis chemistry and the likeThe use value;
3. the nano silver colorimetric sensor provided by the invention utilizes the SPR performance, and the modification group is modified on the surface of the nano silver particles through electrostatic acting force, so that the nano silver particles are stabilized and kept in a relatively dispersed state. Characteristic plasma absorption peaks of the nano silver particles are at 380-420nm, macroscopically show that the solution is yellowish, and when the particle size is increased or the particle spacing is reduced, the positions of the absorption peaks of the nano silver are subjected to red shift; macroscopically showing that the color of the solution changes from light yellow to orange red or blue-violet; the invention utilizes the specific combination of metal ions and the modification groups used in the invention to lead the specific aggregation or disaggregation of nano silver and the color change to achieve the detection purpose.
Drawings
FIG. 1 is an ultraviolet-visible spectrum of a nanosilver colorimetric sensor made in accordance with the present invention;
FIG. 2 shows the nano silver colorimetric sensor obtained by the invention when Cr is added 3+ The ultraviolet visible absorption intensity and peak value change graph with time;
FIG. 3 is a graph showing the ratio of the UV-visible absorption intensity at 550nm to 392nm of the nano-silver colorimetric sensor prepared according to the present invention (A 550 /A 392 ) A plot of change over time;
FIG. 4 is a graph showing the ratio of the UV-visible absorption intensity at 550nm to 392nm of the nano-silver colorimetric sensor obtained by the present invention when different metal ions are added (A 550 /A 392 )；
FIG. 5 is a graph of ultraviolet-visible spectrum of the nano-silver colorimetric sensor prepared by the invention when different metal ions are added;
FIG. 6 shows the addition of Cr at different concentrations in the nano-silver colorimetric sensor according to the present invention 3+ An ultraviolet visible spectrum chart;
FIG. 7 shows the nano silver colorimetric sensor obtained by the present invention when Cr is added 3+ When Cr 3+ Concentration and Lg (A) 550 /A 392 ) The relation between the two is compared with a quantitative detection standard curve chart.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the particular embodiments described herein are illustrative only and are not intended to limit the invention, i.e., the embodiments described are merely some, but not all, of the embodiments of the invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by a person skilled in the art without making any inventive effort, are intended to be within the scope of the present invention.
It is noted that relational terms such as "first" and "second", and the like, are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
The embodiment 1 provides a nano silver colorimetric sensor and a preparation method thereof, and specifically comprises the following steps: 100mL (0.01 mmol) of 0.1mM silver nitrate solution is added into a 250mL conical flask (fresh aqua regia is soaked overnight, ultra-pure water is washed and dried for later use), 0.3mL (0.0102 mmol) of 0.034M nitrilotriacetic acid trisodium salt solution is respectively added under magnetic stirring, 10mg (0.26 mmol) of sodium borohydride is stirred at room temperature for 30min, the solution is changed from transparent colorless to light yellow, and the nano silver colorimetric sensor is obtained, is stored at normal temperature in a dark place, and has no change in color after two weeks, so that the nano silver colorimetric sensor prepared by the invention is very stable and can be stored for a long time.
The synthetic circuit of the preparation process flow is shown as the following formula:
example 2
This example 2 provides a nano-silver colorimetric sensor and a method for preparing the same, which differ from example 1 only in that: 100mL of 0.1mM silver nitrate solution was replaced with 100mL of 0.1mM silver fluoride solution, 10mg of sodium borohydride was replaced with 7.7mg of citric acid, and the other steps and parameters were the same.
Example 3
This example 3 provides a nano-silver colorimetric sensor and a method for preparing the same, which differ from example 1 only in that: 100mL of 0.1mM silver nitrate solution was replaced with 100mL of 0.1mM silver ammonia solution, 10mg of sodium borohydride was replaced with 4.5mg of oxalic acid, and the other steps and parameters were the same.
Example 4
This example 4 provides a nano-silver colorimetric sensor and a method for preparing the same, which differ from example 1 only in that: the sodium borohydride amount was 3.7mg, and the remaining steps and parameters were the same.
Comparative example 1
The comparative example 1 provides a nano silver colorimetric sensor and a preparation method thereof, and specifically comprises the following steps: 100mL of 0.1mM silver nitrate solution is added into a 250mL conical flask (fresh aqua regia is soaked overnight, cleaned by ultrapure water and dried for later use), 0.6mL of 0.034M nitrilotriacetic acid trisodium salt solution is respectively added under magnetic stirring, stirring is carried out for 30min at room temperature, the color of the solution is unchanged, and finally the nano silver colorimetric sensor is not prepared.
Experimental example 1
The ultraviolet-visible absorption spectrum of the nano-silver colorimetric sensor prepared in example 1 was measured in this experimental example, as shown in fig. 1. As can be seen from FIG. 1, a characteristic absorption peak appears at 392 nm.
In this example, the particle size of the nano silver colorimetric sensor prepared in example 1 was also measured by TEM and was 10 to 100nm.
Experimental example 2
Experimental example the nano silver colorimetric sensor prepared in example 1 was measured to have an equivalent volume concentration of 5X 10 -6 The aqueous solution of chromium trichloride of M is mixed, and the corresponding ultraviolet-visible spectrum change within 1-11 min is detected by using an ultraviolet-visible spectrometer (Uv-Vis), and the experimental result is shown in figure 2. As can be seen from fig. 2, the uv-visible absorption peak of the nano-silver solution starts to decrease significantly at 1 min; the graph of fig. 2, which is relatively stable for 1min to 11min, shows that the NTA-modified nano-silver can rapidly respond and reach a stable state after adding chromium trichloride.
The ratio of absorption values corresponding to the absorption wavelengths of the observation features (A 550 /A 392 ) Over time, as shown in fig. 3. As can be seen from fig. 3, the values were substantially stable after 2 min. Therefore, the nano silver colorimetric sensor prepared by the invention can rapidly detect Cr 3+ 。
Experimental example 3
Experimental example the nano silver colorimetric sensor prepared in example 1 was used for 2×10 -5 M Cr 3+ 1.5mL was taken at a concentration of 4X 10 -5 M, and then sequentially weighing 1.5mL of chromium chloride aqueous solution containing other metal ions (FeCl) 3 ,FeCl 2 ,KCl,CuCl 2 ,MnCl 2 ,CdCl 2 ,CoCl 2 ,NiCl 2 ,Pb(NO 3 ) 2 ,ZnCl 2 ,MgCl 2 ,CaCl 2 ,AlCl 3 ,Cr 2 O 7 2- ) The concentration is 4 multiplied by 10 -5 M aqueous solution, mix the above-mentioned nano silver colorimetric sensor with solution comprising above-mentioned metal ion separately, observe its color change, the experimental result is shown in figure 4. As a result ofNow: found to contain only Cr 3+ The nano silver solution of (2) is changed from light yellow to orange red.
Meanwhile, the ultraviolet-visible absorption spectrum of the mixed solution of the nitrilotriacetic acid trisodium salt modified nano silver and the metal ions is measured, and is shown in fig. 5. Experimental results show that only Cr is contained 3+ The ultraviolet-visible absorption spectrum of the mixed solution of (2) is obviously red shifted. Making a ratio (A) of the corresponding ultraviolet-visible absorption peaks of each metal ion 550 /A 392 ) The results show that: detecting Cr with a certain concentration 3+ Ultraviolet-visible absorption spectrum of nano silver solution (A) and ratio of absorption values (A) 550 /A 392 ) The ratio of the UV-visible absorption spectrum and the absorption value of the pure nano-silver solution which is obviously different from that of the blank reference (A 550 /A 392 ) The method comprises the steps of carrying out a first treatment on the surface of the Detecting the ratio of the ultraviolet-visible absorption spectrum and the absorption value of the nano silver solution containing other metal ions with a certain concentration (A 550 /A 392 ) Ratio of UV-visible absorption spectrum and absorption value of pure nanosilver solution to blank reference (A 550 /A 392 ) The variation is not great.
Experimental example 4
The experimental example is that according to the nano silver colorimetric sensor prepared in the embodiment 1, a standard curve is drawn, and the specific steps are as follows:
preparing ultrapure water solutions of chromium trichloride with different concentrations (the concentrations are respectively 0.6 mu M, 1 mu M, 1.5 mu M, 2 mu M, 3 mu M, 4 mu M, 6 mu M, 8 mu M, 10 mu M, 20 mu M and 40 mu M), taking 1.5mL of nano silver colorimetric sensor solution, respectively adding 1.5mL of aqueous solution of chromium chloride with different concentrations, uniformly mixing, standing for 2min, and respectively measuring the ultraviolet-visible absorption spectrum of the mixed solution, as shown in FIG. 6; wherein, the experimental result curves are represented as blank, 0.3. Mu.M, 0.5. Mu.M, 0.75. Mu.M, 1. Mu.M, 1.5. Mu.M, 2. Mu.M, 3. Mu.M, 4. Mu.M, 5. Mu.M, 10. Mu.M, 20. Mu.M in the order from top to bottom at a wavelength of 400nm in FIG. 6.
In lg (A) 550 /A 392 ) On the ordinate, cr 3+ The concentrations are plotted on the abscissa and a standard curve is plotted as shown in fig. 7. As can be seen from FIG. 7, the concentration of the silver nanoparticles is 0.25 μm to 3. Mu.M (the volume ratio of the nano silver solution to the chromium ion solution is oneCompared with a mixture, the measured chromium ion concentration becomes one half of the initial concentration) accords with a linear relation, and the fitting linear relation is Y= -1.41819+0.460233X, and the linear correlation coefficient R 2 0.99219, can be used for Cr 3+ Is a quantitative detection of (a).
Experimental example 5
This experimental example 1.5mL of the nano silver colorimetric sensor prepared in example 1 was taken and 1.5mL of the sample solution 1 to be measured (known Cr 3+ Concentration of 10 μm), uniformly mixing, standing for 15min, and changing the color of the mixed solution from light yellow to orange red to obtain a sample solution containing Cr 3+ The concentration of (C) is 1.5. Mu.M or more, and the ultraviolet-visible absorption spectrum of the mixed solution is measured to obtain lg (A) 550 /A 392 ) -0.072, out of linear relationship range; thus, cr can be obtained semi-quantitatively 3+ Is greater than 1.5. Mu.M.
Experimental example 6
This experimental example 1.5mL of the nanosilver colorimetric sensor prepared in example 1 was taken and 1.5mL of a sample solution to be measured (known Cr 3+ Concentration of 1 μm), and after uniform mixing, standing for 2min, the color change of the solution was observed. The color of the solution changes, but the light yellow color is not changed into blue-violet color, and Cr contained in the sample solution to be detected 3+ The concentration is less than 1.5. Mu.M.
Cr in sample by standard curve method 3+ The concentrations were quantitatively analyzed, and Cr was added at various concentrations according to the standard curve (FIG. 7) obtained in Experimental example 4 3+ Is modified by trisodium nitrilotriacetate (A) 650 /A 524 ) Value and Cr 3+ The linear relation between the concentrations is Y= -1.41819+0.460233, the linear correlation coefficient R 2 0.99219, lg (A 550 /A 392 ) The value can calculate Cr in the sample 3+ Is a concentration of (3). Obtaining Cr in the sample to be detected through calculation 3+ The concentration is 1.03 mu M and is close to Cr in the sample solution to be detected 3+ Is a function of the actual concentration of (a).
Experimental example 7
This experimental example takes 1.5mL of the nano silver colorimetric sensor prepared in example 1, and 1.5m of the nano silver colorimetric sensor is addedL test example 5 the sample solution 1 to be tested prepared was mixed uniformly and then left to stand for 2 minutes, and the color change of the solution was observed. The solution color is not changed, and the solution 1 to be measured does not contain Cr 3+ Or Cr in the liquid 1 to be tested 3+ The concentration is below the visual limit of detection.
The experimental results show that: the nano silver colorimetric sensor prepared in the embodiment 1 of the invention detects Cr 3+ Has extremely high sensitivity and can rapidly achieve the purpose of quantitative detection. In the detection, the detection limit which can be distinguished by naked eyes is 1.5 mu M, and the detection limit can reach 0.4 mu M by using an ultraviolet-visible spectrometer (Uv-Vis); and the nano silver colorimetric sensor prepared in comparative example 1.
The foregoing is merely illustrative and explanatory of the invention as it is claimed, as modifications and additions may be made to, or similar to, the particular embodiments described, without the benefit of the inventors' inventive effort, and as alternatives to those of skill in the art, which remain within the scope of this patent.
Claims (4)
1. The application of the nano silver colorimetric sensor in trivalent chromium ion detection is characterized by comprising the following specific processes: placing a certain amount of nano silver colorimetric sensor in a container, adding a sample solution to be detected with the same volume into the container, shaking uniformly, standing for 1-30 min, and observing the color change of the mixed solution or detecting the change of the ultraviolet visible absorption spectrum of the mixed solution, wherein the visible detection limit of the nano silver colorimetric sensor on trivalent chromium ions is 1.5 mu M; when Cr 3+ When the concentration of the solution is 1.5 mu M-5 mu M, the color of the solution is changed from light yellow to blue-violet; when Cr 3+ At a concentration of greater than 5 μm, the color of the solution changes from pale yellow to orange-red;
the nano silver colorimetric sensor is prepared through the following steps:
adding trisodium nitrilotriacetate solution and reducing agent into 100mL of silver salt solution with concentration of 0.1mM in sequence under stirring at room temperature, and continuing stirring to obtain a pale yellow solution; the molar ratio of the silver salt, the trisodium nitrilotriacetate and the reducing agent in the silver salt solution is 1:1-8:10-30; the reducing agent is one of sodium borohydride, ascorbic acid, citric acid, citrate, tannic acid, glucose and oxalic acid.
2. Use of a nanosilver colorimetric sensor according to claim 1 for detection of trivalent chromium ions, wherein the nanosilver colorimetric sensor has a detection limit of 0.4 μm for uv-vis spectrometer of trivalent chromium ions.
3. The use of a nanosilver colorimetric sensor as claimed in claim 1 wherein the silver salt solution is one or more of a silver nitrate solution, a silver fluoride solution and a silver ammonia solution.
4. The use of the nanosilver colorimetric sensor according to claim 1 for detecting trivalent chromium ions, wherein the nanosilver colorimetric sensor has an ultraviolet visible maximum absorption peak of 380 to 420nm and a particle size of 10 to 100nm.
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