CN113125429A - Nano-silver colorimetric sensor and preparation method and application thereof - Google Patents

Nano-silver colorimetric sensor and preparation method and application thereof Download PDF

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CN113125429A
CN113125429A CN202110429619.4A CN202110429619A CN113125429A CN 113125429 A CN113125429 A CN 113125429A CN 202110429619 A CN202110429619 A CN 202110429619A CN 113125429 A CN113125429 A CN 113125429A
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杨璐铭
张林杉
王巍
晏诗阳
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Sichuan University
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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 chemistry. The sensor has a series of advantages of convenience in carrying, high sensitivity, strong selectivity, good stability and the like, and can realize Cr3+The rapid detection has the advantages of high detection speed, high sensitivity and the like, can effectively solve the problems of strict sample storage condition, high cost of an analysis method, long analysis time and strong operation specificity in the conventional trivalent chromium ion detection technology, and has wide application prospect and higher market application value.

Description

Nano-silver colorimetric sensor and preparation method and application thereof
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
Generally, chromium elements are widely present in nature in two forms of cr (iii) and cr (vi), and trivalent chromium and hexavalent chromium in the environment can be interconverted. Wherein, the trace Cr (III) is a trace element which is necessary for human body and plays an important role in the sugar metabolism and the lipid metabolism of the human body. However, excessive intake of Cr (III) can cause cytotoxic reaction, even mutation and cancer, and meanwhile, Cr (III) has certain teratogenic effect. As trivalent chromium is increasingly applied to the industrial production of electroplating, leather production, metal processing and the like, and the excessive content of the trivalent chromium can cause harm to human bodies. Therefore, the research of a rapid, convenient and sensitive detection method for trivalent chromium ions in an aqueous solution is very necessary.
At present, the conventional trivalent chromium ion detection and analysis instruments mainly include an electric coupling plasma emission spectrometer (ICP), Atomic Absorption Spectroscopy (AAS), atomic fluorescence absorption spectroscopy (AFS), and the like. However, most of the detection methods have the defects of strict sample storage conditions, high analysis method cost, long analysis time, strong operation specificity and the like. In view of the above, it would be very useful 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 storage condition, high analysis method cost, long analysis time and strong operation specificity in the existing trivalent chromium ion detection technology.
In order to achieve the 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 sequentially adding a nitrilotriacetic acid trisodium solution and a reducing agent into the silver salt solution under the stirring state at room temperature, and continuously stirring to obtain a faint yellow solution, namely the nano-silver colorimetric sensor.
Furthermore, 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, after the nitrilotriacetic acid trisodium solution and the reducing agent are sequentially added into the silver salt solution, the stirring is continued for 20-40 minutes, preferably for 30 minutes.
The invention also provides the nano-silver colorimetric sensor prepared by the preparation method.
Furthermore, the maximum ultraviolet-visible absorption peak 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 the detection of trivalent chromium ions is as follows: placing a certain amount of nano-silver colorimetric sensor in a container, adding a sample to be detected with the same volume into the container, shaking uniformly, standing for 1-30 min, observing the color change of the mixed solution or detecting the change of the ultraviolet visible absorption spectrum of the mixed solution, and thus realizing the Cr colorimetric detection3+Qualitative and quantitative analysis is carried out.
Further, the macroscopic distinguishable 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 is present3+When the concentration of the compound is 1.5 mu M-5 mu M, the color of the solution is changed from light yellow to blue purple; when Cr is present3+When the concentration of (D) is more than 5 mu M, the color of the solution is changed from light yellow to orange red; when Cr is present3+When the concentration of (B) is greater than or equal to 0.4. mu.M, a characteristic absorption peak of an 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 a stable water-soluble nano-silver colorimetric sensor is obtained by a method of taking silver salt as a silver nanoparticle source, taking nitrilotriacetic acid trisodium salt as a ligand and adding a reducing agent under stirring at room temperature; the preparation method is different from the prior nano gold or nano silver prepared by the hydrothermal reduction method, does not need additional experimental conditions such as heating and the like, is simpler and safer, and is more stable in storage because the particle size of the nano silver prepared by introducing other reducing agents is smaller than that of the nano silver prepared by the hydrothermal reduction method;
2. the nano-silver colorimetric sensor provided by the invention can realize Cr pairing3+The rapid detection 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 is different from other conventional nano-gold colorimetric sensors or nano-silver colorimetric sensors which only have single color change, and the nano-silver colorimetric sensor prepared by the invention is based on Cr in a solution to be detected3+Will produce different color changes, i.e. the Cr can be determined according to the color changes3+The concentration range of (3) is adjusted according to a standard curve method for Cr3+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 value in the fields of environmental science, inspection chemistry, analytical chemistry and the like;
3. the nano-silver colorimetric sensor provided by the invention utilizes the SPR performance of the sensor, and the modifying group is modified on the surface of the nano-silver particles through electrostatic acting force, and simultaneously plays a role in stabilizing the nano-silver particles and keeping the nano-silver particles in a relatively dispersed state. The characteristic plasma absorption peak of the nano-silver particles is at 380-420nm, the solution is shown to be light yellow in a macroscopic view, and when the particle size is increased or the particle distance is reduced, the position of the absorption peak of the nano-silver generates red shift; macroscopically, the solution changes from light yellow to orange red or blue-purple; the invention achieves the purpose of detection by utilizing the specific combination of metal ions and the modification groups used in the invention to lead the specific aggregation or depolymerization of the nano-silver and the color change.
Drawings
FIG. 1 is a diagram of the UV-Vis spectrum of a nano-silver colorimetric sensor made according to the present invention;
FIG. 2 shows that Cr is added into the nano-silver colorimetric sensor prepared by the invention3+The change of the ultraviolet visible absorption intensity and the peak value with time;
FIG. 3 shows the ratio of the UV-visible absorption intensity at 550nm to 392nm of the nano-silver colorimetric sensor prepared by the present invention (A)550/A392) A graph of change over time;
FIG. 4 is a graph of the nano-silver colorimetric sensor prepared by the present invention when different metal ions are added, and the ratio of the ultraviolet-visible absorption intensity at 550nm to 392nm (A)550/A392)；
FIG. 5 is a diagram of the UV-Vis spectra of the nano-silver colorimetric sensor prepared by the present invention when different metal ions are added;
FIG. 6 shows that Cr with different concentrations is added into the nano-silver colorimetric sensor prepared by the invention3+Ultraviolet-visible spectrum of time;
FIG. 7 shows that the nano-silver colorimetric sensor prepared by the invention is added with Cr3+In time, Cr3+Concentration and Lg (A)550/A392) The relationship between the two is shown in a curve chart of quantitative detection standard.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention. The components of 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 present invention, 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 derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
It is noted that relational terms such as "first" and "second," and the like, may be 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. Also, 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 an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
This embodiment 1 provides a nano-silver colorimetric sensor and a method for manufacturing the same, which specifically includes the following steps: adding 100mL (0.01mmol) of 0.1mM silver nitrate solution into a 250mL conical flask (newly prepared aqua regia is soaked overnight, and is cleaned and dried by ultrapure water for standby), respectively adding 0.3mL (0.0102mmol) of 0.034M nitrilotriacetic acid trisodium salt solution and 10mg (0.26mmol) of sodium borohydride under magnetic stirring, stirring for 30min at room temperature, and changing the solution from transparent colorless to light yellow to obtain the nano-silver colorimetric sensor.
The synthetic route of the preparation process flow is shown as the following formula:
Figure BDA0003030889110000061
example 2
This example 2 provides a nano silver colorimetric sensor and a method for preparing the same, which are different from those of 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 remaining 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 are different from those of example 1 only in that: 100mL of 0.1mM silver nitrate solution is replaced by 100mL of 0.1mM silver ammonia solution, 10mg of sodium borohydride is replaced by 4.5mg of oxalic acid, and the rest steps and parameters are the same.
Example 4
This example 4 provides a nano silver colorimetric sensor and a method for preparing the same, which are different from those of example 1 only in that: the amount of sodium borohydride used was 3.7mg, and the other 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: adding 100mL of 0.1mM silver nitrate solution into a 250mL conical flask (newly prepared aqua regia is soaked overnight, and is cleaned and dried by ultrapure water for standby), respectively adding 0.6mL of 0.034M nitrilotriacetic acid trisodium salt solution under magnetic stirring, and stirring at room temperature for 30min, wherein the solution color is unchanged, and finally, the nano-silver colorimetric sensor is not prepared.
Experimental example 1
This experimental example measured the uv-vis absorption spectrum of the nano-silver colorimetric sensor prepared in example 1, as shown in fig. 1. As can be seen from FIG. 1, a characteristic absorption peak appears at 392 nm.
In the embodiment, the particle size of the nano-silver colorimetric sensor prepared in the embodiment 1 is measured to be 10-100 nm by TEM.
Experimental example 2
In this experimental example, the nano-silver colorimetric sensor prepared in example 1 was mixed with an equal volume of 5 × 10-6And (3) mixing the aqueous solution of the chromium trichloride, and detecting the change of a corresponding ultraviolet-visible spectrum within 1-11 min by using an ultraviolet-visible spectrometer (Uv-Vis), wherein 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; wherein, the curve from 1min to 11min added in fig. 2 is relatively stable, which shows that the NTA modified nano-silver can rapidly respond and reach stability after the chromium trichloride is addedAnd (4) a fixed state.
Observing the ratio (A) of the absorption values corresponding to the characteristic absorption wavelengths550/A392) As a function of time, as shown in fig. 3. As can be seen from FIG. 3, the values are substantially stable after 2 min. Therefore, the nano-silver colorimetric sensor prepared by the invention can rapidly detect Cr3+。
Experimental example 3
This experimental example the nano-silver colorimetric sensor prepared in example 1 was used in 2 × 10-5M Cr3+1.5mL of the solution was measured at a concentration of 4X 10-5M of chromium chloride aqueous solution, and then sequentially measuring 1.5mL of other metal ions (FeCl)3,FeCl2,KCl,CuCl2,MnCl2,CdCl2,CoCl2,NiCl2,Pb(NO3)2,ZnCl2,MgCl2,CaCl2,AlCl3,Cr2O7 2-) The concentration is 4X 10-5M, the above-mentioned nano silver colorimetric sensor and the above-mentioned metal ion-containing solution were mixed, respectively, and the color change was observed, and the experimental result is shown in fig. 4. As a result, it was found that: it was found that only Cr contained3+The color of the nano silver solution is changed from light yellow to orange red.
Meanwhile, the uv-vis absorption spectrum of the nano silver modified with nitrilotriacetic acid trisodium salt and the mixed solution containing the above metal ions was measured, as shown in fig. 5. The experimental result shows that only Cr is contained3+The ultraviolet-visible absorption spectrum of the mixed solution is obviously red-shifted. Making the ratio (A) of the ultraviolet-visible absorption peaks corresponding to the detected metal ions550/A392) The results show that: detecting Cr with a certain concentration3+The ratio of the ultraviolet-visible absorption spectrum to the absorption value of the nano silver solution (A)550/A392) Is obviously different from pure nano silver solution used as blank reference in the ultraviolet-visible absorption spectrum and the ratio of absorption values (A)550/A392) (ii) a Detecting the ratio of the ultraviolet-visible absorption spectrum and the absorption value (A) of the nano-silver solution containing a certain concentration of other metal ions550/A392) The ratio of the UV-visible absorption spectrum to the absorption value (A) of a pure nano-silver solution as a blank reference550/A392) The variation is not large.
Experimental example 4
In this experimental example, a standard curve is drawn according to the nano-silver colorimetric sensor prepared in example 1, and the specific steps are as follows:
preparing ultrapure water solutions of chromium trichloride with different concentrations (the concentrations are respectively 0.6 muM, 1 muM, 1.5 muM, 2 muM, 3 muM, 4 muM, 6 muM, 8 muM, 10 muM, 20 muM and 40 muM), adding 1.5mL of nano-silver colorimetric sensor solution into 1.5mL of aqueous solutions of chromium chloride with different concentrations, mixing uniformly, standing for 2min, and measuring the ultraviolet visible absorption spectra of the mixed solutions respectively, as shown in FIG. 6; in FIG. 6, the test results are shown 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, and 20. mu.M in the order from top to bottom at a wavelength of 400 nm.
In lg (A)550/A392) Is ordinate, Cr3+Concentration is plotted on the abscissa, and a standard curve is plotted, as shown in FIG. 7. As can be seen from fig. 7, the linear relationship is satisfied in the range of 0.25 μ M to 3 μ M (the nano silver solution and the chromium ion solution are mixed one by one according to the volume ratio, and the measured chromium ion concentration becomes one half of the initial concentration), the linear relationship is satisfied, the Y is-1.41819 +0.46023X, and the linear correlation coefficient R is20.99219, can be used for Cr3+And (4) carrying out quantitative detection.
Experimental example 5
In this example, 1.5mL of the nano-silver colorimetric sensor prepared in example 1 was added to 1.5mL of the sample solution 1 to be tested (known as Cr)3+The concentration is 10 mu M), standing for 15min after uniform mixing, wherein the color of the mixed solution is changed from light yellow to orange red, and the sample solution to be detected contains Cr3+Is 1.5. mu.M or more, and the ultraviolet-visible absorption spectrum of the mixed solution is measured to obtain lg (A)550/A392) -0.072, out of the linear relationship range; therefore, Cr can be obtained in a semi-quantitative manner3+Is more than 1.5. mu.M.
Experimental example 6
In this example, 1.5mL of the nano-silver colorimetric sensor prepared in example 1 was added with 1.5mL of the sample to be detectedSample solution (known as Cr)3+Concentration of 1 μ M), mixing uniformly, standing for 2min, and observing the color change of the solution. If the color of the solution changes but does not change from light yellow to blue purple, the Cr contained in the sample solution to be detected3+The concentration is less than 1.5. mu.M.
Cr in sample by standard curve method3+The concentrations were quantitatively analyzed and Cr was added at different concentrations according to the standard curve (FIG. 7) obtained in Experimental example 43+Lg (A) of trisodium nitrilotriacetate-modified nanosilver solution650/A524) Value and Cr3+The linear relation between the concentrations is-1.41819 +0.46023X, and the linear correlation coefficient R20.99219 according to the standard curve equation and lg (A) of the mixed solution550/A392) The value can be calculated to obtain Cr in the sample3+The concentration of (c). Obtaining Cr in the sample to be detected by calculation3+The concentration is 1.03 mu M and is close to Cr in the solution of a sample to be detected3+The actual concentration of (c).
Experimental example 7
In this example, 1.5mL of the nano-silver colorimetric sensor prepared in example 1 was added to 1.5mL of the sample solution 1 to be measured prepared in example 5, and the mixture was uniformly mixed and then allowed to stand for 2min, and the color change of the solution was observed. If the color of the solution is not changed, the solution to be tested 1 does not contain Cr3+Or Cr in the solution to be tested 13+The concentration is below the visual detection limit.
The above experimental results show that: the nano-silver colorimetric sensor prepared in the embodiment 1 of the invention detects Cr3+Has extremely high sensitivity and can quickly achieve the aim 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 exemplary and illustrative of the present invention and it is within the purview of one skilled in the art to modify or supplement the embodiments described or to substitute similar ones without the exercise of inventive faculty, and still fall within the scope of the claims.

Claims (10)

1. A preparation method of a nano-silver colorimetric sensor is characterized by comprising the following steps: and sequentially adding a nitrilotriacetic acid trisodium solution and a reducing agent into the silver salt solution under the stirring state at room temperature, and continuously stirring to obtain a faint yellow solution, namely the nano-silver colorimetric sensor.
2. The method for preparing the nano-silver colorimetric sensor according to claim 1, wherein 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.
3. The method of claim 1 or 2, 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 method of preparing a nanosilver colorimetric sensor according to claim 1 or 2, wherein the reducing agent is one or more of sodium borohydride, ascorbic acid, citric acid, citrate, tannic acid, glucose and oxalic acid.
5. The nano-silver colorimetric sensor manufactured by the method for manufacturing a nano-silver colorimetric sensor according to any one of claims 1 to 4.
6. The nano-silver colorimetric sensor according to claim 5, wherein the nano-silver colorimetric sensor has a maximum ultraviolet-visible absorption peak of 380 to 420nm and a particle size of 10 to 100 nm.
7. Use of the nanosilver colorimetric sensor of claim 5 or 6 for the detection of trivalent chromium ions.
8. The application of the nano-silver colorimetric sensor in the detection of trivalent chromium ions, which is characterized by comprising the following steps: placing a certain amount of nano silver colorimetric sensor in a container, adding the sample to be detected with the same volume into the container, shaking uniformly, standingObserving the color change of the mixed solution or detecting the change of the ultraviolet visible absorption spectrum of the mixed solution for 1-30 min, and then realizing Cr3+Qualitative and quantitative analysis is carried out.
9. The use of the nanosilver colorimetric sensor of claim 7 in the detection of trivalent chromium ions, wherein the nanosilver colorimetric sensor has a macroscopic discernable detection limit of 1.5 μ Μ for trivalent chromium ions; when Cr is present3+When the concentration of the compound is 1.5 mu M-5 mu M, the color of the solution is changed from light yellow to blue purple; when Cr is present3+At a concentration of greater than 5. mu.M, the solution changed from pale yellow to orange-red in color.
10. The use of the nanosilver colorimetric sensor of claim 7 in the detection of trivalent chromium ions, wherein the nanosilver colorimetric sensor has a detection limit of 0.4 μ M for the ultraviolet-visible spectrometer of trivalent chromium ions; the characteristic absorption peak of the ultraviolet-visible spectrum is red-shifted.
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CN106370612A (en) * 2016-10-31 2017-02-01 中国工程物理研究院材料研究所 Preparation method of nano gold colorimetric sensor, and sensor prepared by method and application thereof
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WO2012059943A2 (en) * 2010-11-02 2012-05-10 Indian Institute Of Technology, Delhi Pale yellow coloured aqueous dispersion of silver nanoparticles, a process for preparation and compositons thereof
CN106370612A (en) * 2016-10-31 2017-02-01 中国工程物理研究院材料研究所 Preparation method of nano gold colorimetric sensor, and sensor prepared by method and application thereof
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