CN108279228A - A method of utilizing acetate ion concentration in the Raman spectroscopy acid solution of the silica dioxide granule containing methylene blue - Google Patents
A method of utilizing acetate ion concentration in the Raman spectroscopy acid solution of the silica dioxide granule containing methylene blue Download PDFInfo
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- CN108279228A CN108279228A CN201810417186.9A CN201810417186A CN108279228A CN 108279228 A CN108279228 A CN 108279228A CN 201810417186 A CN201810417186 A CN 201810417186A CN 108279228 A CN108279228 A CN 108279228A
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- acetate ion
- methylene blue
- acid solution
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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Abstract
The method that the present invention provides acetate ion concentration in a kind of Raman spectroscopy acid solution using the silica dioxide granule containing methylene blue, belongs to ion concentration detection method technical field.It is characterized in that including the following steps：The silica dioxide granule containing methylene blue is prepared using absolute ethyl alcohol, deionized water, concentrated ammonia liquor, methylene blue and ethyl orthosilicate；The acid solution for preparing pH=3.8~6.0 of known acetate ion concentration obtains acetate ion concentration and 525 cm in description acid solution with its Raman spectrum is measured again after the acetate ion in the silica dioxide granule absorption acid solution containing methylene blue‑1Locate the standard curve of the relationship of Raman spectrum numerical value；The acetate ion in acid solution to be measured is adsorbed with the silica dioxide granule containing methylene blue and measures it in 525 cm‑1Locate Raman spectrum data, then acetate ion concentration in acid solution to be measured is calculated by standard curve.Used testing process is simple, is conducive to be widely used.
Description
Technical field
Acetate ion is dense in a kind of Raman spectroscopy acid solution using the silica dioxide granule containing methylene blue
The method of degree belongs to ion concentration detection method technical field, and in particular to a kind of acetate ion concentration detection method.
Background technology
As a kind of important anion, acetate ion is widely used in food, chemical products processing and medical treatment
The fields such as health care.Acetate ion can be used for preparing haemodialysis agent, and cooperation haemodialyser uses, and can improve blood soda acid
Balance, enables the toxicant in blood to permeate into dialyzate and excretes, and clinically reaches the uremic effect for the treatment of
Fruit.If acetate ion too high levels in dialyzate, the adverse reactions such as nauseous, tired and muscle cramp can be caused, thus to vinegar
The identification of acid ion and detection are a very necessary job.
Currently, the technical method of detection acetate ion mainly has the chromatography of ions, high performance liquid chromatography and gas phase liquid
Spectrometry etc..Chinese invention patent CN200810185480.8 discloses a kind of anion receptor based on nitro phenylhydrazone and phenolic hydroxyl group
In DMSO/H2The method of the selective colorimetric detection of Dichlorodiphenyl Acetate radical ion in O solution.Chinese invention patent
CN201310300618.5 discloses one kind with N, and N'- bis--[3- hydroxyls -4- (2- benzoxazoles) phenyl] urea is glimmering as acetate
Light probe compound and the concentration that acetate ion is detected with fluorescence signal.Chinese invention patent CN201410677027.4 is public
Opened a kind of Li Yong Quercetin as fluorescence probe Dichlorodiphenyl Acetate radical ion assay method.
Raman spectrum has also been carried out in the application study of ion concentration context of detection, Chinese invention patent
CN201710384604.4 disclose a kind of monocrystalline silicon corroded using borax as the substrate of surface-enhanced Raman, in ethanol solution
The method that is detected of methylene blue molecule.Up to the present, the Raman spectrum data pair using methylene blue is not yet found
The method that acetate ion concentration is tested in acid solution.
Invention content
The present invention provides vinegar in a kind of Raman spectroscopy acid solution using the silica dioxide granule containing methylene blue
The method of acid ion concentration, feature include the following steps：
（1）Sequentially added in beaker 92 milliliters of absolute ethyl alcohols, 17.2 ml deionized waters, 2.48 milliliters of concentrated ammonia liquors and
3.44 milliliters of ethyl orthosilicates are added in 0.10 gram of methylene blue, stirring after 15 minutes, reaction centrifuges after 4 hours and obtains colloid
Grain, then colloidal solid is washed twice with 100 milliliters of absolute ethyl alcohols, the centrifuged silica dioxide granule containing methylene blue；
（2）It prepares to obtain by acetic acid, sodium acetate and deionized water and contains a concentration of 3.9~802.4 mMs every liter of acetate ion
PH=3.8~6.0 acid solution, will be through step（1）12.5 milli of silica dioxide granule pair containing methylene blue being prepared
The acetate ion risen in acid solution is adsorbed, and is centrifuged after 1 minute and is obtained sediment, by sediment again to 12.5 milliliters
Acetate ion in acid solution is adsorbed, and is centrifuged after 1 minute and is obtained sediment, by obtained sediment at 70 DEG C
It is 24 hours dry, the silica dioxide granule containing methylene blue of absorption acetate ion is prepared.It is tested with Raman spectrometer
The silica dioxide granule containing methylene blue for adsorbing acetate ion, obtains its Raman spectrum data, with the vinegar in acid solution
A concentration of abscissa of acid ion, with 525 cm obtained after normalized-1Locate Raman spectrum numerical value to draw for ordinate
Standard curve；
（3）It will be through step（1）In the 12.5 milliliters of acid solutions to be measured of silica dioxide granule pair containing methylene blue being prepared
Acetate ion adsorbed, wherein step（2）In acid solution pH value it is identical as the pH value of acid solution to be measured, 1
Centrifugation obtains sediment after minute, and sediment again inhales the acetate ion in 12.5 milliliters of acid solutions to be measured
It is attached, it is centrifuged after 1 minute and obtains sediment, obtained sediment is 24 hours dry at 70 DEG C, obtain absorption acetate ion
The silica dioxide granule containing methylene blue.The titanium dioxide containing methylene blue of absorption acetate ion is tested with Raman spectrometer
Silicon particle obtains its Raman spectrum data, records 525 cm obtained after normalized-1Locate Raman spectrum numerical value, utilizes
Through step（2）The acetate ion concentration in acid solution to be measured is calculated in obtained standard curve.
Wherein, step（2）The pH value range of mentioned acid solution is pH=3.8~6.0, best acid solution
PH value is 3.8.Step（2）The pH value and step of mentioned acid solution（3）Mentioned in solution to be measured pH value it is identical,
That is, when being measured to the acetate ion in acid solution to be measured using this technology method, by step（3）It is carried
And the pH value of acid solution to be measured select step（2）Mentioned in acid solution pH value, and then prepare associated pH
Acid solution.Step（2）A concentration of 3.9~802.4 mMs every liter of acetate ion in mentioned acid solution, most preferably
A concentration of 3.9~150.1 mMs every liter of acetate ion.Step（2）With（3）It is obtained after mentioned normalized
Raman spectrum numerical value is the relative intensity of Raman spectrum.
The advantageous effect of this technology method is：
（1）Used testing process is simple, chemical reagent price is low, is conducive to be widely used；
（2）Silica dioxide granule containing methylene blue is short to the acetate ion adsorption time in acid solution, can improve survey
Determine the efficiency of acetate ion.
Description of the drawings
Fig. 1 is through 1 step of embodiment（1）With（2）The silica containing methylene blue of obtained absorption acetate ion
The Raman spectroscopy of particle.
Fig. 2 is through 1 step of embodiment（1）With（2）Draw obtained standard curve, wherein abscissa is acetate ion
Concentration, ordinate be particle obtained after normalized in 525 cm-1The Raman spectrum numerical value at place（Closed square accords with
Number）, particle is through 1 step of embodiment（1）With（2）The silica containing methylene blue for the absorption acetate ion being prepared
Particle.Hollow circle symbol in figure be particle obtained after normalized in 525 cm-1The Raman spectrum numerical value at place,
Wherein, particle is through 1 step of embodiment（3）Acetate ion contains methylene in the absorption acid solution A to be measured being prepared
Blue silica dioxide granule.
Fig. 3 is through 2 step of embodiment（1）With（2）Draw obtained standard curve, wherein abscissa is acetate ion
Concentration, ordinate be particle obtained after normalized in 525 cm-1The Raman spectrum numerical value at place（Closed square accords with
Number）, particle is through 2 step of embodiment（1）With（2）The silica containing methylene blue for the absorption acetate ion being prepared
Particle.Open diamond symbols in figure be particle obtained after normalized in 525 cm-1Locate Raman spectrum numerical value,
Wherein, particle is through 2 step of embodiment（3）Acetate ion contains methylene in the absorption acid B solution to be measured being prepared
Blue silica dioxide granule.
Specific implementation mode
Embodiment 1
（1）Sequentially added in beaker 92 milliliters of absolute ethyl alcohols, 17.2 ml deionized waters, 2.48 milliliters of concentrated ammonia liquors and
3.44 milliliters of ethyl orthosilicates are added in 0.10 gram of methylene blue, stirring after 15 minutes, reaction centrifuges after 4 hours and obtains colloid
Grain, then colloidal solid is washed twice with 100 milliliters of absolute ethyl alcohols, the centrifuged silica dioxide granule containing methylene blue；
（2）It prepares to obtain by acetic acid, sodium acetate and deionized water and contains a concentration of 3.9~150.1 mMs every liter of acetate ion
PH=3.8 acid solution, will be through step（1）The 12.5 milliliters of acid of silica dioxide granule pair containing methylene blue being prepared
Property solution in acetate ion adsorbed, after 1 minute centrifugation obtain sediment, by sediment again to 12.5 milliliters of acidity
Acetate ion in solution is adsorbed, and is centrifuged after 1 minute and is obtained sediment, and obtained sediment is dry at 70 DEG C
24 hours, the silica dioxide granule containing methylene blue of absorption acetate ion is prepared.It is tested and is adsorbed with Raman spectrometer
The silica dioxide granule containing methylene blue of acetate ion, obtains its Raman spectrum data, with the acetate in acid solution
Ion concentration is abscissa, with 525 cm obtained after normalized-1It is that ordinate draws standard to locate Raman spectrum numerical value
Curve；
（3）It will be through step（1）In the 12.5 milliliters of acid solutions to be measured of silica dioxide granule pair containing methylene blue being prepared
Acetate ion adsorbed, wherein the pH value of acid solution to be measured is 3.8, labeled as acid solution A to be measured, after 1 minute
Centrifugation obtains sediment, the acetate ion in sediment again acid solution A to be measured to 12.5 milliliters is adsorbed, 1 point
Centrifugation obtains sediment after clock, and obtained sediment is 24 hours dry at 70 DEG C, and obtain absorption acetate ion contains Asia
The silica dioxide granule of methyl blue.The silica containing methylene blue of absorption acetate ion is tested with Raman spectrometer
Grain obtains its Raman spectrum data, records 525 cm obtained after normalized-1Locate Raman spectrum numerical value, using through step
（2）A concentration of 50.2 mMs every liter of acetate ion in acid solution A to be measured is calculated in obtained standard curve.
Embodiment 2
（1）Sequentially added in beaker 92 milliliters of absolute ethyl alcohols, 17.2 ml deionized waters, 2.48 milliliters of concentrated ammonia liquors and
3.44 milliliters of ethyl orthosilicates are added in 0.10 gram of methylene blue, stirring after 15 minutes, reaction centrifuges after 4 hours and obtains colloid
Grain, then colloidal solid is washed twice with 100 milliliters of absolute ethyl alcohols, the centrifuged silica dioxide granule containing methylene blue；
（2）It prepares to obtain by acetic acid, sodium acetate and deionized water and contains a concentration of 3.9~150.1 mMs every liter of acetate ion
PH=3.8 acid solution, will be through step（1）The 12.5 milliliters of acid of silica dioxide granule pair containing methylene blue being prepared
Property solution in acetate ion adsorbed, after 1 minute centrifugation obtain sediment, by sediment again to 12.5 milliliters of acidity
Acetate ion in solution is adsorbed, and is centrifuged after 1 minute and is obtained sediment, and obtained sediment is dry at 70 DEG C
24 hours, the silica dioxide granule containing methylene blue of absorption acetate ion is prepared.It is tested and is adsorbed with Raman spectrometer
The silica dioxide granule containing methylene blue of acetate ion, obtains its Raman spectrum data, with the acetate in acid solution
Ion concentration is abscissa, with 525 cm obtained after normalized-1It is that ordinate draws standard to locate Raman spectrum numerical value
Curve；
（3）It will be through step（1）In the 12.5 milliliters of acid solutions to be measured of silica dioxide granule pair containing methylene blue being prepared
Acetate ion adsorbed, wherein the pH value of acid solution to be measured is 3.8, labeled as acid B solution to be measured, after 1 minute
Centrifugation obtains sediment, the acetate ion in sediment again acid B solution to be measured to 12.5 milliliters is adsorbed, 1 point
Centrifugation obtains sediment after clock, and obtained sediment is 24 hours dry at 70 DEG C, and obtain absorption acetate ion contains Asia
The silica dioxide granule of methyl blue.The silica containing methylene blue of absorption acetate ion is tested with Raman spectrometer
Grain obtains its Raman spectrum data, records 525 cm obtained after normalized-1Locate Raman spectrum numerical value, using through step
（2）A concentration of 6.8 mMs every liter of acetate ion in acid B solution to be measured is calculated in obtained standard curve.
Claims (1)
1. acetate ion concentration in a kind of Raman spectroscopy acid solution using the silica dioxide granule containing methylene blue
Method, it is characterised in that realized by following steps：
Step 1. sequentially added in beaker 92 milliliters of absolute ethyl alcohols, 17.2 ml deionized waters, 2.48 milliliters of concentrated ammonia liquors and
3.44 milliliters of ethyl orthosilicates are added in 0.10 gram of methylene blue, stirring after 15 minutes, reaction centrifuges after 4 hours and obtains colloid
Grain, then colloidal solid is washed twice with 100 milliliters of absolute ethyl alcohols, the centrifuged silica dioxide granule containing methylene blue；
Step 2. is prepared to obtain by acetic acid, sodium acetate and deionized water contains a concentration of 3.9~802.4 mMs of acetate ion
The acid solution of every liter of pH=3.8~6.0, the silica dioxide granule pair 12.5 containing methylene blue that will be prepared through step 1
Acetate ion in milliliter acid solution is adsorbed, and is centrifuged after 1 minute and is obtained sediment, by sediment again to 12.5 millis
The acetate ion risen in acid solution is adsorbed, and is centrifuged after 1 minute and is obtained sediment, by obtained sediment in 70 DEG C
Lower drying 24 hours is prepared the silica dioxide granule containing methylene blue of absorption acetate ion, is surveyed with Raman spectrometer
The silica dioxide granule containing methylene blue of examination absorption acetate ion, obtains its Raman spectrum data, in acid solution
A concentration of abscissa of acetate ion, with 525 cm obtained after normalized-1Place's Raman spectrum numerical value is painted for ordinate
Standard curve processed；
12.5 milliliters of acid solutions to be measured of silica dioxide granule pair containing methylene blue that step 3. will be prepared through step 1
In acetate ion adsorbed, wherein the pH value of the acid solution in step 2 is identical as the pH value of acid solution to be measured, 1
Centrifugation obtains sediment after minute, and sediment again inhales the acetate ion in 12.5 milliliters of acid solutions to be measured
It is attached, it is centrifuged after 1 minute and obtains sediment, obtained sediment is 24 hours dry at 70 DEG C, obtain absorption acetate ion
The silica dioxide granule containing methylene blue, with Raman spectrometer test absorption acetate ion the titanium dioxide containing methylene blue
Silicon particle obtains its Raman spectrum data, records 525 cm obtained after normalized-1Locate Raman spectrum numerical value, utilizes
The acetate ion concentration in acid solution to be measured is calculated through the standard curve that step 2 obtains.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810417186.9A CN108279228B (en) | 2018-05-04 | 2018-05-04 | Method for measuring concentration of acetate ions in acidic solution by utilizing Raman spectrum of silica particles containing methylene blue |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810417186.9A CN108279228B (en) | 2018-05-04 | 2018-05-04 | Method for measuring concentration of acetate ions in acidic solution by utilizing Raman spectrum of silica particles containing methylene blue |
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| CN108279228B CN108279228B (en) | 2020-12-08 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109233806A (en) * | 2018-09-25 | 2019-01-18 | 山东理工大学 | A method of there is the silica dioxide granule containing methylene blue of high fluorescent using heat treatment auxiliary preparation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109233806A (en) * | 2018-09-25 | 2019-01-18 | 山东理工大学 | A method of there is the silica dioxide granule containing methylene blue of high fluorescent using heat treatment auxiliary preparation |
| CN109233806B (en) * | 2018-09-25 | 2021-09-17 | 山东理工大学 | Method for preparing silicon dioxide particles containing methylene blue with high fluorescence intensity by heat treatment assistance |
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