CN108279228B - Method for measuring concentration of acetate ions in acidic solution by utilizing Raman spectrum of silica particles containing methylene blue - Google Patents
Method for measuring concentration of acetate ions in acidic solution by utilizing Raman spectrum of silica particles containing methylene blue Download PDFInfo
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Abstract
The invention provides a method for measuring the concentration of acetate ions in an acidic solution by utilizing Raman spectrum of silicon dioxide particles containing methylene blue, belonging to the technical field of ion concentration detection methods. The method is characterized by comprising the following steps: preparing silicon dioxide particles containing methylene blue by using absolute ethyl alcohol, deionized water, concentrated ammonia water, methylene blue and ethyl orthosilicate; preparing an acid solution with the known acetate ion concentration and the pH = 3.8-6.0, adsorbing the acetate ions in the acid solution by using silica particles containing methylene blue, and measuring the Raman spectrum of the acid solution to obtain the description of the acetate ion concentration in the acid solution and 525 cm‑1A standard curve of the relation of the Raman spectrum values; adsorbing acetate ions in the acidic solution to be detected by using silica particles containing methylene blue and measuring the acetate ions at 525 cm‑1And processing the Raman spectrum data, and calculating by using a standard curve to obtain the concentration of the acetate ions in the acidic solution to be detected. The adopted test flow is simple and is beneficial to wide application.
Description
Technical Field
A method for measuring the concentration of acetate ions in an acid solution by utilizing the Raman spectrum of silicon dioxide particles containing methylene blue belongs to the technical field of ion concentration detection methods, and particularly relates to a method for detecting the concentration of acetate ions.
Background
As an important anion, acetate ions are widely applied to the fields of food, chemical product processing, medical care and the like. The acetate ions can be used for preparing a hemodialysis agent and matched with a hemodialyzer, so that the acid-base balance of blood can be improved, toxic substances in the blood can be dispersed into dialysate to be discharged out of the body, and the effect of treating uremia is achieved clinically. If the content of acetate ions in the dialysate is too high, adverse reactions such as nausea, tiredness, muscle spasm and the like can be caused, so that the identification and detection of the acetate ions are very necessary work.
At present, the technical methods for detecting acetate ions mainly comprise ion chromatography, high performance liquid chromatography, gas-liquid chromatography and the like. Chinese patent CN200810185480.8 discloses an anion receptor based on nitrophenylhydrazone and phenolic hydroxyl in DMSO/H2A method for selective colorimetric detection of acetate ions in O solution. Chinese patent CN201310300618.5 discloses a new compound of N, N' -di- [ 3-hydroxy-4- (2-benzoxazole) phenyl]Urea acts as an acetate fluorescent probe compound and detects the concentration of acetate ions as a fluorescent signal. Chinese patent CN201410677027.4 discloses a method for measuring acetate ions by using quercetin as a fluorescent probe.
Application research of Raman spectroscopy in ion concentration detection is also carried out, and Chinese invention patent CN201710384604.4 discloses a method for detecting methylene blue molecules in an ethanol solution by using borax-corroded monocrystalline silicon as a surface-enhanced Raman substrate. To date, no method has been found for measuring the acetate ion concentration in acidic solutions using raman spectroscopic data of methylene blue.
Disclosure of Invention
The invention provides a method for measuring the concentration of acetate ions in an acidic solution by utilizing Raman spectrum of silica particles containing methylene blue, which is characterized by comprising the following steps:
(1) adding 92 ml of absolute ethyl alcohol, 17.2 ml of deionized water, 2.48 ml of concentrated ammonia water and 0.10 g of methylene blue into a beaker in sequence, stirring for 15 minutes, adding 3.44 ml of ethyl orthosilicate, reacting for 4 hours, centrifuging to obtain colloid particles, washing the colloid particles twice by using 100 ml of absolute ethyl alcohol, and centrifuging to obtain silicon dioxide particles containing the methylene blue;
(2) preparing an acidic solution containing acetate ions with the concentration of 3.9-802.4 millimoles per liter and the pH = 3.8-6.0 by using acetic acid, sodium acetate and deionized water, and carrying out the step (1) to obtain the acidic solution containing methylene blueAdsorbing the acetate ions in 12.5 ml of the acid solution by using the silica particles, centrifuging after 1 minute to obtain a sediment, adsorbing the acetate ions in 12.5 ml of the acid solution again by using the sediment, centrifuging after 1 minute to obtain the sediment, and drying the obtained sediment at 70 ℃ for 24 hours to prepare the methylene blue-containing silica particles adsorbing the acetate ions. Testing the methylene blue-containing silicon dioxide particles adsorbing acetate ions by using a Raman spectrometer to obtain Raman spectrum data of the particles, taking the concentration of the acetate ions in an acid solution as a horizontal coordinate, and normalizing the concentration to obtain 525 cm-1Drawing a standard curve by taking the Raman spectrum numerical value as a vertical coordinate;
(3) adsorbing acetate ions in 12.5 ml of acid solution to be detected by the silica particles containing methylene blue prepared in the step (1), wherein the pH value of the acid solution in the step (2) is the same as that of the acid solution to be detected, centrifuging the solution after 1 minute to obtain sediment, adsorbing the acetate ions in 12.5 ml of acid solution to be detected again by the sediment, centrifuging the solution after 1 minute to obtain sediment, and drying the obtained sediment at 70 ℃ for 24 hours to obtain the silica particles containing methylene blue and adsorbing the acetate ions. Testing the silica particles containing methylene blue adsorbing acetate ions by using a Raman spectrometer to obtain Raman spectrum data of the silica particles, and recording 525 cm obtained after normalization treatment-1And (3) processing the Raman spectrum value, and calculating by using the standard curve obtained in the step (2) to obtain the concentration of the acetate ions in the acidic solution to be detected.
Wherein, the pH value range of the acidic solution mentioned in the step (2) is pH = 3.8-6.0, and the optimal pH value of the acidic solution is 3.8. The pH value of the acidic solution mentioned in the step (2) is the same as the pH value of the solution to be measured mentioned in the step (3), that is, when the technical method is used for measuring acetate ions in the acidic solution to be measured, the pH value of the acidic solution mentioned in the step (2) is selected according to the pH value of the acidic solution to be measured mentioned in the step (3), and then the acidic solution with the relevant pH value is prepared. The concentration of acetate ions in the acidic solution mentioned in the step (2) is 3.9-802.4 millimoles per liter, and the optimal concentration of acetate ions is 3.9-150.1 millimoles per liter. And (3) normalizing the Raman spectrum values obtained in the steps (2) and (3) to obtain the Raman spectrum relative intensity.
The technical method has the beneficial effects that:
(1) the adopted test flow is simple, the chemical reagent price is low, and the wide application is facilitated;
(2) the adsorption time of the silicon dioxide particles containing methylene blue to acetate ions in the acid solution is short, and the efficiency of measuring the acetate ions can be improved.
Drawings
FIG. 1 is a Raman spectrum of silica particles containing methylene blue and adsorbing acetate ions obtained by the steps (1) and (2) in example 1.
FIG. 2 is a standard curve obtained by plotting the results of steps (1) and (2) in example 1, wherein the abscissa is the concentration of acetate ions and the ordinate is the normalized value of the particles at 525 cm-1The raman spectrum values (solid squares) of (b) are obtained from the silica particles containing methylene blue having adsorbed acetate ions prepared by the steps (1) and (2) of example 1. The open circles in the figure are the normalized particles at 525 cm-1The raman spectrum value of (a), wherein the particles are silica particles containing methylene blue, which are prepared by the step (3) of example 1 and adsorb acetate ions in the acidic a solution to be detected.
FIG. 3 is a standard curve obtained by plotting the results of steps (1) and (2) in example 2, wherein the abscissa is the concentration of acetate ions and the ordinate is the normalized value of the particles at 525 cm-1The raman spectrum values (solid squares) of (b) are obtained from the silica particles containing methylene blue having adsorbed acetate ions prepared by the steps (1) and (2) of example 2. The hollow diamond symbols in the figure are the particles normalized to 525 cm-1(ii) Raman spectroscopy, wherein the particles are the absorbate prepared in step (3) of example 2Silica particles containing methylene blue to which acetate ions in the acidic B solution to be measured are attached.
Detailed Description
Example 1
(1) Adding 92 ml of absolute ethyl alcohol, 17.2 ml of deionized water, 2.48 ml of concentrated ammonia water and 0.10 g of methylene blue into a beaker in sequence, stirring for 15 minutes, adding 3.44 ml of ethyl orthosilicate, reacting for 4 hours, centrifuging to obtain colloid particles, washing the colloid particles twice by using 100 ml of absolute ethyl alcohol, and centrifuging to obtain silicon dioxide particles containing the methylene blue;
(2) preparing an acid solution with the concentration of acetate ions of 3.9-150.1 millimoles per liter and the pH =3.8 by using acetic acid, sodium acetate and deionized water, adsorbing the acetate ions in 12.5 milliliters of the acid solution by using the silica particles containing methylene blue prepared in the step (1), centrifuging after 1 minute to obtain a sediment, adsorbing the acetate ions in 12.5 milliliters of the acid solution again by using the sediment, centrifuging after 1 minute to obtain the sediment, and drying the obtained sediment at 70 ℃ for 24 hours to prepare the silica particles containing methylene blue and adsorbing the acetate ions. Testing the methylene blue-containing silicon dioxide particles adsorbing acetate ions by using a Raman spectrometer to obtain Raman spectrum data of the particles, taking the concentration of the acetate ions in an acid solution as a horizontal coordinate, and normalizing the concentration to obtain 525 cm-1Drawing a standard curve by taking the Raman spectrum numerical value as a vertical coordinate;
(3) adsorbing acetate ions in 12.5 ml of acid solution to be detected by the silica particles containing methylene blue prepared in the step (1), wherein the pH value of the acid solution to be detected is 3.8, the acid solution to be detected is marked as acid solution A to be detected, centrifuging the solution after 1 minute to obtain sediment, adsorbing the acetate ions in 12.5 ml of acid solution A to be detected again by the sediment, centrifuging the solution after 1 minute to obtain sediment, and drying the obtained sediment at 70 ℃ for 24 hours to obtain the silica particles containing methylene blue and adsorbing the acetate ions. Testing the silica particles containing methylene blue and adsorbing acetate ions by using a Raman spectrometer to obtain Raman spectrum data of the silica particles,record 525 cm after normalization-1And (3) calculating the Raman spectrum value by using the standard curve obtained in the step (2) to obtain the concentration of acetate ions in the to-be-detected acidic A solution of 50.2 millimoles per liter.
Example 2
(1) Adding 92 ml of absolute ethyl alcohol, 17.2 ml of deionized water, 2.48 ml of concentrated ammonia water and 0.10 g of methylene blue into a beaker in sequence, stirring for 15 minutes, adding 3.44 ml of ethyl orthosilicate, reacting for 4 hours, centrifuging to obtain colloid particles, washing the colloid particles twice by using 100 ml of absolute ethyl alcohol, and centrifuging to obtain silicon dioxide particles containing the methylene blue;
(2) preparing an acid solution with the concentration of acetate ions of 3.9-150.1 millimoles per liter and the pH =3.8 by using acetic acid, sodium acetate and deionized water, adsorbing the acetate ions in 12.5 milliliters of the acid solution by using the silica particles containing methylene blue prepared in the step (1), centrifuging after 1 minute to obtain a sediment, adsorbing the acetate ions in 12.5 milliliters of the acid solution again by using the sediment, centrifuging after 1 minute to obtain the sediment, and drying the obtained sediment at 70 ℃ for 24 hours to prepare the silica particles containing methylene blue and adsorbing the acetate ions. Testing the methylene blue-containing silicon dioxide particles adsorbing acetate ions by using a Raman spectrometer to obtain Raman spectrum data of the particles, taking the concentration of the acetate ions in an acid solution as a horizontal coordinate, and normalizing the concentration to obtain 525 cm-1Drawing a standard curve by taking the Raman spectrum numerical value as a vertical coordinate;
(3) adsorbing acetate ions in 12.5 ml of acid solution to be detected by the silica particles containing methylene blue prepared in the step (1), wherein the pH value of the acid solution to be detected is 3.8, the acid solution to be detected is marked as acid B solution to be detected, centrifuging the solution after 1 minute to obtain sediment, adsorbing the acetate ions in 12.5 ml of acid B solution to be detected again by the sediment, centrifuging the solution after 1 minute to obtain sediment, and drying the obtained sediment at 70 ℃ for 24 hours to obtain the silica particles containing methylene blue and adsorbing the acetate ions. Testing the content of adsorbed acetate ions by Raman spectrometerObtaining Raman spectrum data of the silica particles of methylene blue, and recording 525 cm obtained after normalization treatment-1And (3) calculating the Raman spectrum value by using the standard curve obtained in the step (2) to obtain that the concentration of acetate ions in the to-be-detected acidic B solution is 6.8 millimoles per liter.
Claims (1)
1. A method for measuring the concentration of acetate ions in an acidic solution by using Raman spectroscopy of silica particles containing methylene blue is characterized by comprising the following steps of:
step 1, sequentially adding 92 ml of absolute ethyl alcohol, 17.2 ml of deionized water, 2.48 ml of concentrated ammonia water and 0.10 g of methylene blue into a beaker, stirring for 15 minutes, adding 3.44 ml of ethyl orthosilicate, reacting for 4 hours, centrifuging to obtain colloid particles, washing the colloid particles twice by using 100 ml of absolute ethyl alcohol, and centrifuging to obtain silicon dioxide particles containing methylene blue;
step 2, preparing an acid solution with the concentration of acetate ions of 3.9-802.4 millimoles per liter and the pH = 3.8-6.0 by using acetic acid, sodium acetate and deionized water, adsorbing the acetate ions in 12.5 ml of the acid solution by using the silica particles containing methylene blue prepared in the step 1, centrifuging the solution after 1 minute to obtain a sediment, adsorbing the acetate ions in 12.5 ml of the acid solution again by using the sediment, centrifuging the sediment after 1 minute to obtain a sediment, drying the obtained sediment at 70 ℃ for 24 hours, preparing the silica particles containing methylene blue and adsorbing acetate ions, testing the silica particles containing methylene blue and adsorbing acetate ions by using a Raman spectrometer to obtain Raman spectrum data of the silica particles, the concentration of acetate ions in the acidic solution is used as the abscissa, and the concentration is 525 cm after normalization treatment.-1Drawing a standard curve by taking the Raman spectrum numerical value as a vertical coordinate;
step 3, adsorbing acetate ions in 12.5 ml of acid solution to be detected by the silica particles containing methylene blue prepared in the step 1, wherein the pH value of the acid solution in the step 2 is the same as that of the acid solution to be detected, centrifuging the solution after 1 minute to obtain sediment, and re-centrifuging the sedimentAdsorbing the acetate ions in 12.5 ml of to-be-detected acidic solution for the second time, centrifuging after 1 minute to obtain a sediment, drying the obtained sediment at 70 ℃ for 24 hours to obtain methylene blue-containing silica particles adsorbing the acetate ions, testing the methylene blue-containing silica particles adsorbing the acetate ions by using a Raman spectrometer to obtain Raman spectrum data of the methylene blue-containing silica particles, and recording 525 cm of the Raman spectrum data obtained after normalization treatment-1And (4) processing the Raman spectrum numerical value, and calculating by using the standard curve obtained in the step (2) to obtain the concentration of the acetate ions in the acidic solution to be detected.
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