CN112683878A - Method for detecting pH of solution based on surface enhanced Raman effect - Google Patents
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Abstract
A method for detecting the pH of a solution based on a surface enhanced Raman effect comprises the following steps: (1) loading a noble metal nanoparticle single-layer film with a macroscopic size on a clean support substrate to obtain a single-layer film substrate; (2) preparing a pH sensitive probe molecule containing carboxyl into a solution by using absolute ethyl alcohol, and respectively preparing hydrochloric acid and sodium hydroxide into solutions with different standard pH values by using ultrapure water; (3) soaking the single-layer film substrate in a pH sensitive probe molecular solution containing carboxyl, and fishing out and drying to obtain a functionalized substrate; (4) and soaking the functionalized substrate in standard solutions with different pH values, drawing a standard curve of the pH value of the solution according to the characteristic peak intensity of carboxyl groups in the spectrum, and comparing the signal intensity of the characteristic peak of the substrate in the solution to be detected with the standard curve to obtain the pH value of the solution to be detected. The invention realizes simple and effective detection of pH in the aqueous solution and can realize linear quantitative detection in the range of pH 3-10.
Description
Technical Field
The invention relates to a method for detecting the pH value of a solution, in particular to a method for detecting the pH value of the solution based on the surface enhanced Raman effect of a gold nanoparticle single-layer film with a macroscopic size, and belongs to the technical field of solution pH detection.
Background
The surface enhanced Raman scattering spectroscopy (SERS) has the spectral characteristics of simplicity, no damage, rapidness, sensitivity and molecular fingerprint identification, and is widely applied to the fields of optical sensing, biological detection, chemical analysis and the like. CN108526487B discloses a method for preparing a macro-size close-packed gold nanoparticle single-layer film, which prepares a macro-size nanoparticle single-layer film by an interface assembly method.
Because the noble metal (gold and silver) nanoparticles in the single-layer film have a periodic ordered arrangement structure, gaps among the noble metal (gold and silver) nanoparticles are uniformly distributed in the single-layer film and serve as hot spots of the SERS substrate. Based on the noble metal nanoparticle monolayer film with uniform and repeatable Surface Plasmon Resonance (SPR) effect, some related applications of the noble metal nanoparticle monolayer film in the field of analysis and detection can be realized through further functional modification treatment.
At present, the common main methods for detecting the pH of a solution comprise a test paper method, an indicator method, a pH meter method and the like, but the method has the defects of inaccurate numerical value result, complicated calibration, incapability of dynamically obtaining a result and the like. The existing single-layer nano-particle film is not commonly applied to solution pH detection, mainly because of the obvious defects of poor pH feedback signal quality, complicated method, difficult quantification and the like in the detection technology.
Therefore, the application of the nanoparticle monolayer film in solution for pH detection is still a little challenge, and the solution of the problems can greatly broaden the application of the nanoparticle monolayer film in the solution pH detection field without doubt.
Disclosure of Invention
Aiming at the defects of the existing solution pH detection technology and the problem that the application of a precious metal (gold and silver) nanoparticle single-layer film in solution pH detection is deficient, the invention provides a method for detecting the solution pH based on the surface enhanced Raman effect, which is efficient, simple and convenient.
The method for detecting the pH of the solution based on the surface enhanced Raman effect comprises the following steps:
(1) loading a noble metal nano particle single-layer film with a macroscopic size on a clean support substrate (a silicon wafer and a glass sheet) to obtain a single-layer film substrate;
(2) preparing pH sensitive probe molecules (4-mercaptobenzoic acid, dimercaptobenzoic acid and the like) containing carboxyl into solutions with the molar concentration of 0.001-1 mol/L by using absolute ethyl alcohol, and respectively preparing hydrochloric acid and sodium hydroxide into different standard pH solutions with the pH of 3-10 by using ultrapure water;
(3) soaking the single-layer film substrate obtained in the step (1) in a pH sensitive probe molecule (4-mercaptobenzoic acid, dimercaptobenzoic acid and the like) solution containing carboxyl, standing at normal temperature for 1-24 hours, taking out, washing the surface of the single-layer film substrate with absolute ethyl alcohol, and drying in a nitrogen atmosphere to obtain a functionalized substrate;
(4) and (3) soaking the functionalized substrate obtained in the step (3) in standard solutions with different pH values, standing at normal temperature for 1-3 minutes, collecting the surface enhanced Raman scattering spectrum of the functionalized substrate in the solution, drawing a standard curve of the pH value of the solution according to the characteristic peak intensity of carboxyl (or carbonyl) groups in the spectrum, and comparing the characteristic peak signal intensity of the substrate in the solution to be detected with the standard curve to obtain the pH value of the solution to be detected.
The preparation process of the macro-sized noble metal nanoparticle monolayer film in the step (1) is as follows:
preparing amines (oleylamine, octadecylamine and the like) into an amine-containing organic solution with the molar concentration of 0.001 mol/L by using an organic solvent (toluene, n-hexane and the like), completely mixing a water-soluble monodisperse spherical noble metal nanoparticle sol (with the average particle size of 16 nanometers) and the amine-containing organic solution in a volume ratio of 5:1, naturally standing after violently shaking, and separating and collecting the organic solution containing the noble metal nanoparticles on the upper layer;
completely and uniformly mixing ultrapure water and diethylene glycol in a volume ratio of 1: 9-4 to obtain a diethylene glycol solution;
and thirdly, adding the organic solution containing the noble metal nano-particles to the diethylene glycol solution, naturally standing until the organic solution is completely volatilized, and obtaining the noble metal nano-particle single-layer film with macroscopic size above the diethylene glycol solution.
Wherein, the preparation process of the water-soluble monodisperse spherical noble metal nano-particle sol in the step (i) is as follows:
a, respectively preparing sodium citrate and chloroauric acid or silver nitrate into a sodium citrate solution with the mass percent concentration of 1% and a chloroauric acid or silver nitrate solution with the mass percent concentration of 1% by using ultrapure water;
b, sequentially adding a sodium citrate solution and chloroauric acid or a silver nitrate solution into boiling water, wherein the volume ratio of the sodium citrate solution to the chloroauric acid or the silver nitrate solution to the ultrapure water is 1:3: 96;
and c, keeping boiling, heating and refluxing for 30 minutes, and cooling to room temperature to obtain the water-soluble monodisperse spherical gold nanoparticle sol or silver nanoparticle sol with the average particle size of 16 nanometers.
The noble metal nanoparticle sol is gold nanoparticle sol or silver nanoparticle sol, and chloroauric acid is used as a precursor when the gold nanoparticle sol is prepared; silver nitrate was used as a precursor in the preparation of the silver nanoparticle sol.
The preparation of the macroscopic size precious metal nanoparticle single-layer film in the step (1) can also be carried out according to the preparation method of macroscopic size close-packed gold nanoparticle single-layer film disclosed in CN 108526487B. The water-soluble monodisperse spherical Gold nanoparticle sol in step I can also be prepared according to the method described in paper High-Yield Production of form Gold Nanoparticles with Sizes from 31to 577nm via One-point selected Growth and Size-Dependent SERS Property (part.part.Syst. Character. 2016,33,924-932), published in part.part.Syst. Charact.J., 2016. When the silver nanoparticle sol is prepared by the method, silver nitrate is used as a precursor instead of chloroauric acid.
The pH sensitive probe molecules used in the step (3) mainly comprise organic matters containing carboxyl groups (such as 4-mercaptobenzoic acid, dimercaptobenzoic acid and the like).
The characteristic peak intensity of the carboxyl group in the step (4) not only comprises simple characteristic peak intensity values, but also covers the intensity ratio among the characteristic peaks.
1420cm in the surface enhanced Raman scattering spectrum of the functionalized substrate in the solution in the step (4)-1The strength of the characteristic peak of carboxyl and the pH value of the solution are in a linear function relationship within the range of 3-10, and the linear fitting coefficient R2At 0.998, the fit function relationship is: 85.902 x-104.886.
The nano-particle monolayer film is used as a surface enhanced Raman substrate, the substrate is modified by using a pH sensitive probe molecule containing carboxyl, the simple and effective detection of the pH in the aqueous solution is realized through the change of the Raman enhanced spectrum characteristic peak intensity of the substrate after the functionalization treatment in the solution, and the linear quantitative detection can be realized in the range of the pH 3-10.
The invention solves the obvious defects of poor pH feedback signal quality, complicated method, difficult quantification and the like existing in the application of the nano-particle single-layer film to pH detection, and the solution of the problems can undoubtedly greatly widen the application of the nano-particle single-layer film in the field of pH detection.
Drawings
FIG. 1 is a surface enhanced Raman spectrum of a gold nanoparticle monolayer film substrate treated with 4-mercaptobenzoic acid modification in example 1.
FIG. 2 is a surface enhanced Raman spectrum obtained by detecting the gold nanoparticle monolayer film substrate modified and treated by 4-mercaptobenzoic acid in a standard solution with pH of 3 in example 1.
FIG. 3 is a surface enhanced Raman spectrum obtained by detecting the gold nanoparticle monolayer film substrate modified and treated by 4-mercaptobenzoic acid in a standard solution with pH of 5 in example 1.
FIG. 4 is a surface enhanced Raman spectrum obtained by detecting the gold nanoparticle monolayer film substrate modified and treated by 4-mercaptobenzoic acid in a standard solution with pH of 7 in example 1.
FIG. 5 is a surface enhanced Raman spectrum obtained by detecting the gold nanoparticle monolayer film substrate modified and treated by 4-mercaptobenzoic acid in a standard solution with pH of 10 in example 1.
FIG. 6 is 1420cm of Surface Enhanced Raman Spectroscopy (SERS) obtained by detecting the gold nanoparticle monolayer film substrate modified and treated by 4-mercaptobenzoic acid in standard solutions with different pH values in example 1-1The intensity of the characteristic peak of carboxyl groups is plotted linearly with the pH of the solution (3-10). 1420cm in the spectrum-1The strength of the characteristic peak of carboxyl and the pH value of the solution are in a linear function relationship within the range of 3-10, and the linear fitting coefficient R2At 0.998, the fit function relationship is: 85.902 x-104.886.
Detailed Description
Example 1
Firstly, putting the glassware (100 ml double-mouth flask, 25 ml beaker, glass sheet and culture dish) into king water for soaking for 3 hours, then cleaning the glassware with saturated sodium nitrate solution and ultrapure water, and drying the glassware for later use.
(1) Preparing the required solution
Firstly, respectively preparing required raw materials of sodium citrate and chloroauric acid into solutions by using ultrapure water, wherein the mass percentage concentration of the sodium citrate solution is 1%, and the mass percentage concentration of the chloroauric acid solution is 1%.
② preparing oleylamine into an organic solution with the molar concentration of 0.001 mol/L by using a toluene organic solvent.
③ using absolute ethyl alcohol to prepare 4-mercaptobenzoic acid into 4-mercaptobenzoic acid ethyl alcohol solution with the molar concentration of 0.1 mol/L.
(2) 48 ml of ultrapure water is added into a double-neck flask, and after the double-neck flask is rapidly heated to boiling, 1.5 ml of sodium citrate solution and 0.5 ml of chloroauric acid solution are sequentially and rapidly added into boiling water. And keeping heating reflux for 30 minutes, and then slowly cooling to room temperature to obtain the water-soluble monodisperse spherical gold nanoparticle sol with the average particle size of 16 nanometers.
(3) 5 ml of gold nanoparticle sol was mixed with 1 ml of oleylamine organic solution at a ratio of 5:1, fully mixing, standing for 5 minutes, separating and collecting the upper layer gold-containing nanoparticle organic solution. Placing 2 ml of ultrapure water and 18 ml of diethylene glycol in a 25 ml glass beaker according to the volume ratio of 1:9, fully and uniformly mixing, slowly dropwise adding the collected gold-containing nanoparticle organic solution right above the diethylene glycol solution, and obtaining the gold nanoparticle single-layer film with the macroscopic size on the surface of the diethylene glycol solution after the organic solution is completely volatilized after 12 hours.
(4) And transferring and loading the gold nanoparticle single-layer film onto a glass substrate (or a silicon chip), and washing the surface with absolute ethyl alcohol to obtain the functionalized substrate. Soaking the substrate in 5 ml of 4-mercaptobenzoic acid ethanol solution prepared in the third step (1), standing at normal temperature for 3 hours, fishing out, washing the surface with absolute ethyl alcohol, drying in nitrogen atmosphere, and finishing functional modification treatment on the substrate to obtain the functional substrate.
When the gold nanoparticle single-layer film needs to be prepared, silver nitrate is used for replacing chloroauric acid.
The surface-enhanced raman spectrum of the gold nanoparticle monolayer film substrate modified and treated with 4-mercaptobenzoic acid in this example is shown in fig. 1.
(5) Soaking the functionalized substrate obtained in the step (4) in standard solutions with different pH values, standing for 1-3 minutes at normal temperature, and collecting the surface enhanced Raman scattering spectrum of the functionalized substrate in the solution, wherein the specific steps are as follows:
a solution having a pH of 3 was prepared using ultrapure water and hydrochloric acid, and the pH of the solution was calibrated using a pH meter. Placing 2 ml of standard solution with the pH value of 3 in a culture dish, completely soaking the functionalized and modified gold nano-film substrate in the standard solution, focusing a laser beam of a Raman spectrometer on the surface of the substrate in the standard solution after 1 minute, wherein the laser wavelength of the Raman spectrometer is 633 nanometers, and collecting under a 50-time long-focus lens to obtain the surface enhanced Raman spectrum of the standard solution with the pH value of 3.
The surface enhanced Raman spectrum of the standard solution with pH3 detected by using the 4-mercaptobenzoic acid modified gold nanoparticle monolayer film obtained in the step (4) as a surface enhanced Raman substrate is shown in FIG. 2.
② preparing a solution with pH 5 by using ultrapure water and hydrochloric acid, and calibrating the pH of the solution by using a pH meter. Placing 2 ml of standard solution with the pH value of 5 in a culture dish, completely soaking the functionalized and modified gold nano-film substrate in the standard solution, focusing a laser beam of a Raman spectrometer on the surface of the substrate in the standard solution after 1 minute, wherein the laser wavelength of the Raman spectrometer is 633 nanometers, and collecting under a 50-time long-focus lens to obtain the surface enhanced Raman spectrum of the standard solution with the pH value of 5.
The surface enhanced raman spectrum of the standard solution with pH 5 detected by using the obtained 4-mercaptobenzoic acid modified gold nanoparticle monolayer film obtained in the step (4) as a surface enhanced raman substrate is shown in fig. 3.
③ using ultrapure water and hydrochloric acid to prepare a solution with pH of 7, and utilizing a pH meter to calibrate the pH of the solution. Placing 2 ml of standard solution with the pH value of 7 in a culture dish, completely soaking the functionalized and modified gold nano-film substrate in the standard solution, focusing a laser beam of a Raman spectrometer on the surface of the substrate in the standard solution after 2 minutes, wherein the laser wavelength of the Raman spectrometer is 633 nanometers, and collecting under a 50-time long-focus lens to obtain the surface enhanced Raman spectrum of the standard solution with the pH value of 7.
The surface enhanced raman spectrum of the standard solution with pH of 7 detected by using the gold nanoparticle monolayer film modified by 4-mercaptobenzoic acid obtained in the step (4) as a surface enhanced raman substrate is shown in fig. 4.
Preparing a solution with the pH value of 10 by using ultrapure water and hydrochloric acid, and calibrating the pH value of the solution by using a pH meter. Placing 2 ml of standard solution with the pH value of 10 in a culture dish, completely soaking the functionalized and modified gold nano-film substrate in the standard solution, focusing a laser beam of a Raman spectrometer on the surface of the substrate in the standard solution after 3 minutes, wherein the laser wavelength of the Raman spectrometer is 633 nanometers, and collecting under a 50-time long-focus lens to obtain the surface enhanced Raman spectrum of the standard solution with the pH value of 10.
The surface enhanced raman spectrum of the standard solution with the pH of 10 detected by using the gold nanoparticle monolayer film modified by 4-mercaptobenzoic acid obtained in the step (4) as a surface enhanced raman substrate is shown in fig. 5.
According to the above different pH standard solutions, the surface enhanced Raman spectrum is 1420cm-1And fitting and drawing a standard linear relation graph between the pH value of the solution and the characteristic peak intensity. Test spectrum in unknown solution 1420cm-1And comparing the signal intensity of the characteristic peak of the carboxyl group with a standard curve to determine the pH of the unknown solution. Raman spectrum in solution 1420cm-1The linear relationship between the characteristic peak signal intensity of carboxyl group and the pH of the solution (3-10) is shown in FIG. 6. 1420cm in the spectrum-1The strength of the characteristic peak of carboxyl and the pH value of the solution are in a linear function relationship within the range of 3-10, and the linear fitting coefficient R2At 0.998, the fit function relationship is: 85.902 x-104.886.
Example 2
The present embodiment is different from embodiment 1 in that:
(1) preparing the required solution
② preparing the octadecylamine into an organic solution with the molar concentration of 0.001 mol/L by using toluene.
③ using absolute ethyl alcohol to prepare 4-mercaptobenzoic acid into 4-mercaptobenzoic acid ethyl alcohol solution with the molar concentration of 0.1 mol/L and 0.001 mol/L.
(3) 2 ml of ultrapure water and 16 ml of diethylene glycol were placed in a 25 ml glass beaker in a volume ratio of 1:8, and completely and uniformly mixed to obtain a diethylene glycol solution.
(4) The substrate was immersed in 5 ml of 4-mercaptobenzoic acid ethanol solution prepared from (1) ③ and left at room temperature for 1 hour.
Example 3
The present embodiment is different from embodiment 1 in that:
(1) preparing the required solution
② preparing the oleylamine into an organic solution with the molar concentration of 0.001 mol/L by using normal hexane.
③ using absolute ethyl alcohol to prepare 4-mercaptobenzoic acid into 4-mercaptobenzoic acid ethyl alcohol solution with the molar concentration of 0.1 mol/L and 1 mol/L.
(3) 2 ml of ultrapure water and 14 ml of diethylene glycol were placed in a 25 ml glass beaker in a volume ratio of 1:7, and were completely and uniformly mixed to obtain a diethylene glycol solution.
(4) The substrate is soaked in 5 ml of 4-mercaptobenzoic acid ethanol solution prepared by the third step (1) and is placed for 18 hours at normal temperature.
Example 4
The present embodiment is different from embodiment 1 in that:
(1) preparing the required solution
② preparing the octadecylamine into an organic solution with the molar concentration of 0.001 mol/L by using normal hexane.
③ using absolute ethyl alcohol to prepare the dimercaptobenzoic acid into a dimercaptobenzoic acid ethyl alcohol solution with the molar concentration of 0.1 mol/L.
(3) 2 ml of ultrapure water and 10 ml of diethylene glycol were placed in a 25 ml glass beaker in a volume ratio of 1:5, and were completely and uniformly mixed to obtain a diethylene glycol solution.
(4) The substrate was immersed in 5 ml of ethanol dimercaptobenzoic acid solution prepared from (1) ③ and left at room temperature for 24 hours.
Claims (6)
1. A method for detecting the pH value of a solution based on a surface enhanced Raman effect is characterized by comprising the following steps:
(1) loading a noble metal nanoparticle single-layer film with a macroscopic size on a clean support substrate to obtain a single-layer film substrate;
(2) preparing a pH sensitive probe molecule containing carboxyl into a solution with the molar concentration of 0.001-1 mol/L by using absolute ethyl alcohol, and respectively preparing hydrochloric acid and sodium hydroxide into different standard pH solutions with the pH of 3-10 by using ultrapure water;
(3) soaking the single-layer film substrate obtained in the step (1) in a pH sensitive probe molecular solution containing carboxyl, standing at normal temperature for 1-24 hours, taking out, washing the surface of the single-layer film substrate with absolute ethyl alcohol, and drying in a nitrogen atmosphere to obtain a functionalized substrate;
(4) and (3) soaking the functionalized substrate obtained in the step (3) in standard solutions with different pH values, standing at normal temperature for 1-3 minutes, collecting the surface enhanced Raman scattering spectrum of the functionalized substrate in the solution, drawing a standard curve of the pH value of the solution according to the characteristic peak intensity of carboxyl groups in the spectrum, and comparing the characteristic peak signal intensity of the substrate in the solution to be detected with the standard curve to obtain the pH value of the solution to be detected.
2. The method for detecting the pH of a solution based on the surface enhanced raman effect of claim 1, wherein the macro-sized monolayer of noble metal nanoparticles prepared in step (1) is prepared as follows:
preparing amine into amine-containing organic solution with the molar concentration of 0.001 mol/L by using an organic solvent, completely mixing water-soluble monodisperse spherical noble metal nano particle sol and the amine-containing organic solution according to the volume ratio of 5:1, naturally standing after violent shaking, and separating and collecting the organic solution containing noble metal nano particles on the upper layer;
completely and uniformly mixing ultrapure water and diethylene glycol in a volume ratio of 1: 9-4 to obtain a diethylene glycol solution;
and thirdly, slowly adding the collected organic solution containing the noble metal nano-particles to the diethylene glycol solution, naturally standing until the organic solution is completely volatilized, and obtaining a macro-sized noble metal nano-particle single-layer film above the diethylene glycol solution.
3. The method for detecting the pH of a solution based on the surface-enhanced Raman effect according to claim 2, wherein the water-soluble monodisperse spherical noble metal nanoparticle sol in the step (i) is prepared as follows:
a, respectively preparing sodium citrate and chloroauric acid or silver nitrate into a sodium citrate solution with the mass percent concentration of 1% and a chloroauric acid or silver nitrate solution with the mass percent concentration of 1% by using ultrapure water;
b, sequentially adding a sodium citrate solution and chloroauric acid or a silver nitrate solution into boiling water, wherein the volume ratio of the sodium citrate solution to the chloroauric acid or the silver nitrate solution to the ultrapure water is 1:3: 96;
and c, keeping boiling, heating and refluxing for 30 minutes, and cooling to room temperature to obtain the water-soluble monodisperse spherical gold nanoparticle sol or silver nanoparticle sol with the average particle size of 16 nanometers.
4. The method for detecting the pH of a solution based on the surface-enhanced Raman effect according to claim 1, wherein the pH sensitive probe molecule used in the step (3) comprises an organic substance containing a carboxyl group.
5. The method for detecting pH of a solution according to claim 1, wherein the characteristic peak intensity of the carboxyl group in step (4) includes not only simple characteristic peak intensity values but also intensity ratios between characteristic peaks.
6. The method for detecting pH of a solution according to claim 1, wherein the functionalized substrate in the solution collected in step (4) has surface enhanced Raman scattering spectrum of 1420cm-1To the carboxyl groupThe characteristic peak intensity and the pH value of the solution are in a linear function relationship within the range of 3-10, and the linear fitting coefficient R2At 0.998, the fit function relationship is: 85.902 x-104.886.
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Application publication date: 20210420 |