CN104677846A - Quantitative analysis method for graphene dispersion liquid - Google Patents
Quantitative analysis method for graphene dispersion liquid Download PDFInfo
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- CN104677846A CN104677846A CN201510090327.7A CN201510090327A CN104677846A CN 104677846 A CN104677846 A CN 104677846A CN 201510090327 A CN201510090327 A CN 201510090327A CN 104677846 A CN104677846 A CN 104677846A
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Abstract
The invention discloses a quantitative analysis method for graphene dispersion liquid. According to the method, absorbencies at different standard concentrations can be tested by virtue of an ultraviolet-visible spectrophotometer, and a standard dispersity-absorbency curve of the graphene dispersion liquid is established according to a corresponding relation between the standard dispersity and dispersion liquid absorbency of known dispersion liquid. In actual testing, the dispersity of graphene can be calculated through a standard curve only by testing the absorbency of the graphene in the to-be-detected dispersion liquid. The quantitative analysis method disclosed by the invention is broad in application scope and suitable for testing the dispersity of the graphene in different dispersing agents, so as to offer real and authentic data basis for evaluating the dispersity of the graphene. The method disclosed by the invention is low in cost and capable of overcoming the shortcomings of an existing dispersion liquid testing method which is complex in step, long in cycle, failing to quantify and poor in accuracy, so that the testing process is simple and easy in implementation, free from large and expensive instrument, low in testing cost and strong in practicability.
Description
Technical field
The present invention relates to analytical chemistry field, be specifically related to a kind of quantitative analysis method of graphene dispersing solution.
Background technology
Graphene (Graphene) is a kind of new material of the individual layer schistose texture be made up of carbon atom.Graphene has desirable two dimensional crystal structure, and its carbon atom is with the mutual bonding of sp2 hybrid form, and form the rigid disk Rotating fields only comprising hexagonal cellular, be two-dimensional material the thinnest in the world, its thickness is only 0.35 nm.
The uniqueness of Graphene because of its structure and the excellence of performance, become study hotspot rapidly.Along with being constantly explored in the application of electronics, energy storage, biology, medicine and other fields of Graphene, the problem of Graphene production and application is hindered to become the key of research.Prepare the chemical reduction method of Graphene as most possible scale, also there is the problems such as product is easily reunited, difficult dispersion.Therefore, be present study hotspot by carrying out modification to Graphene to obtain polymolecularity grapheme material, and how to carry out quantitative test to Graphene dispersion degree in the solution be also current urgent problem.
The traditional method of testing of Graphene generally all adopts atomic force microscope or transmission electron microscope.But be that atomic force microscope or transmission electron microscope all exist the high problem purchasing difficulty of cost.For graphene dispersing solution, more difficultly, its dispersion dispersion degree cannot carry out quantitative measurement by above-mentioned any method.
As can be seen here, be badly in need of a kind of new cost effective method of research and quantitative test is carried out to graphene dispersion degree.
Summary of the invention
In order to solve the deficiencies in the prior art, the invention provides a kind of simple, can quantitative test Graphene, modified graphene dispersion degree in water or in other organic solvents method, for the dispersive property of evaluating graphite alkene, there is provided genuine and believable data supporting, to solve existing technical barrier; The method carries out test analysis to obtain its dispersion degree by adopting ultra-violet and visible spectrophotometer to the Graphene prepared, modified graphene dispersion liquid.
The technical solution adopted in the present invention is as follows: a kind of quantitative analysis method of graphene dispersing solution, comprises the following steps:
1) different dispersion degree Graphene standard disperse liquid is configured;
2) drawing standard curve: adopt ultraviolet-visible pectrophotometer at 660 nm wavelength places respectively determination steps 1) absorbance of described standard disperse liquid, by the corresponding relation of known Graphene standard scores divergence and absorbance, draw the typical curve of absorbance-dispersion degree;
3) sample analysis: by the graphene dispersing solution of unknown dispersion degree to be measured, its absorbance is measured with ultraviolet-visible pectrophotometer, by and step 2) identical method measures the absorbance of the graphene dispersing solution to be measured of unknown dispersion degree, draws the dispersion degree of described graphene dispersing solution to be measured according to described typical curve.
As preferably, described spreading agent is water, 1-METHYLPYRROLIDONE, dinethylformamide, any one in dimethyl sulfoxide (DMSO).
As preferably, the divergence criteria curve of described graphene dispersing solution is drawn by following methods: the graphene dispersing solution configuring different dispersion degree, measures its absorbance respectively at 660 nm wavelength places; Get the solution of above-mentioned different dispersion degree more respectively, dried, record the solution dispersion degree separately of different dispersion degree, then draw out typical curve according to the corresponding relation of dispersion degree and absorbance.
As preferably, described graphene dispersing solution dispersion degree rises in gradient.
As preferably, described graphene dispersing solution dispersion degree scope is 5 mg/L-100 mg/L.
The beneficial effect that technical scheme provided by the invention is brought is: graphene dispersing solution has good Lambert-Beer behavior, and the dispersion degree of graphene dispersing solution and ultraviolet absorptivity have good linear relationship, A/l=aC.A/1 is the absorbance of unit cell length, and C is the dispersion degree of the rare dispersion liquid of graphite, and a is the extinction coefficient of the rare dispersion liquid of graphite.Utilize this principle, namely by testing the absorbance of the graphene dispersing solution of known dispersion degree, drawing the typical curve of dispersion degree and absorbance, and then testing the absorbance of unknown dispersion degree dispersion liquid, calculating its dispersion degree.The Graphene adopting the method to obtain multiple preparation means, modified graphene dispersion liquid are tested, and result shows that it is correct.
The present invention adopts ultraviolet-visible spectrophotometer to test various criterion concentration absorbance, according to the standard scores divergence of known dispersion liquid and the corresponding relation of dispersion liquid absorbance, sets up the standard scores divergence-absorbance curve of graphene dispersing solution.Only need the absorbance of testing Graphene in dispersion liquid to be measured when reality is tested, namely calculate the dispersion degree of Graphene by typical curve.The present invention is applied widely, be applicable to the test of Graphene dispersion degree in different spreading agent, dispersion degree for evaluating graphite alkene provides genuine and believable data foundation, and the present invention can also test and carry out the dispersion degree of the modified graphene dispersion liquid that modification obtains through different modifier to Graphene in addition.
It is low that method provided by the invention has cost, the feature that operation is simple, overcome complex steps in existing dispersion liquid method of testing, cycle is long, cannot be quantitative, the shortcoming of poor accuracy, make simple testing process easy, without the need to Large expensive instrument, and reduce testing cost, there is very strong practicality.
As can be seen here, compared with prior art, have outstanding substantive distinguishing features and significant progress, its beneficial effect implemented also is apparent in the present invention.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme in the embodiment of the present invention, below the accompanying drawing used required in describing embodiment is briefly described, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the embodiment of the present invention two Graphene, modified graphene 1-METHYLPYRROLIDONE (NMP) dispersion liquid absorbance curve at different wavelengths;
Fig. 2 is the typical curve of Graphene at 1-METHYLPYRROLIDONE (NMP) dispersion liquid of the embodiment of the present invention three gained; Typical curve linear relationship is: y=0.0269x-0.0209, R2=0.9913.Wherein, R2 must >0.99; prove that this is a linear feature obviously empirical model; namely illustrate that fitting a straight line can be explained, cover measured data to be greater than 99.99% ground; there is good generality, the measurement of other unknown dispersion degree dispersion liquids can be used for as standard working curve;
Fig. 3 is the typical curve of Graphene at aqueous dispersions of the embodiment of the present invention four gained; Typical curve linear relationship is: y=0.0253x-0.1006, R2=0.9924.Wherein, R2 must >0.99; prove that this is a linear feature obviously empirical model; namely illustrate that fitting a straight line can be explained, cover measured data to be greater than 99.99% ground; there is good generality, the measurement of other unknown dispersion degree dispersion liquids can be used for as standard working curve;
Fig. 4 is the typical curve of Graphene at dinethylformamide (DMF) dispersion liquid of the embodiment of the present invention five gained; Typical curve linear relationship is: y=0.0246x-0.0394, R2=0.9925.Wherein, R2 must >0.99; prove that this is a linear feature obviously empirical model; namely illustrate that fitting a straight line can be explained, cover measured data to be greater than 99.99% ground; there is good generality, the measurement of other unknown dispersion degree dispersion liquids can be used for as standard working curve;
Fig. 5 is the typical curve of Graphene at dimethyl sulfoxide (DMSO) (DMSO) dispersion liquid of the embodiment of the present invention six gained; Typical curve linear relationship is: y=0.0252x-0.0231, R2=0.9932.Wherein, R2 must >0.99; prove that this is a linear feature obviously empirical model; namely illustrate that fitting a straight line can be explained, cover measured data to be greater than 99.99% ground; there is good generality, the measurement of other unknown dispersion degree dispersion liquids can be used for as standard working curve;
Fig. 6 is the typical curve of CTAB modified graphene 1-METHYLPYRROLIDONE (NMP) dispersion liquid of the embodiment of the present invention seven gained; Typical curve linear relationship is: y=0.0264x-0.0355, R2=0.9919.Wherein, R2 must >0.99, prove that this is a linear feature obviously empirical model, namely illustrate that fitting a straight line can be explained, cover measured data to be greater than 99.99% ground, there is good generality, the measurement of other unknown dispersion degree dispersion liquids can be used for as standard working curve.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly, below in conjunction with accompanying drawing, embodiment of the present invention is described further in detail.
Embodiment one: the preparation method of Graphene.
The preparation method of Graphene has mechanical stripping method, Hummers oxidation-reduction method, ultrasonic dispersion, prepared by solvent-thermal method, by the step that Hummers method prepares Graphene be wherein: 1g graphite, the 23mL98% concentrated sulphuric acid are placed in 100mL beaker and mix and be placed in ice bath, stir 30min, make it fully mix; Take 4g KMnO
4add in beaker after continuing to stir 1h, move in the tepidarium of 40 ° of C and continue to stir 30min; In beaker, add distilled water, control temperature adds appropriate 5% H after reactant liquor is diluted to 80-100mL by 100 ° of below C
2o
2, filter while hot; Fully wash to close to neutral with 5% HCl and distilled water, filter, 60 ° of C are dried, and obtain graphite oxide; In beaker, prepare the NaOH solution that pH is 11, graphite oxide is ground, adds in beaker and prepare 0.3g × L
-1graphite oxide suspending liquid 100mL, be placed in ultrasonic cleaner ultrasonic 30min under 200W power, centrifugal treating removing is a small amount of impurity wherein, obtain the graphene oxide colloidal suspensions of isotropic stable, graphene oxide suspension is filtered, is then placed in vacuum drying chamber 60 ° of C and dries and can obtain graphene oxide; In the graphene oxide colloidal suspensions after centrifugal, add 0.5mL hydrazine hydrate, 90 ° of C isothermal reaction 10h, obtain stable Graphene colloidal suspensions; Adopt miillpore filter to filter graphene suspension, be placed in vacuum drying chamber and dry in 60 ° of C, can Graphene be obtained.
Embodiment two: the absorbance curve of Graphene different wave length as shown in Figure 1, Graphene, the absorbance of modified graphene all can reach high value at 350-700nm in the absorbance of different solutions, and therefore the present invention selects the wavelength coverage of visible ray is 350-700nm.
Due to Graphene, modified graphene characteristic ultraviolet absorption spike length is 660 nm, therefore the test wavelength of ultraviolet-visible pectrophotometer is chosen as λ=660 nm by the present invention.
Embodiment three: the present embodiment is tested for the dispersion degree of Graphene in 1-METHYLPYRROLIDONE (NMP) solution.
1) preparation method of Graphene is with embodiment one.
2) configure Graphene NMP standard disperse liquid and draw the typical curve of Graphene NMP dispersion liquid.The Graphene of 50mg, 100mL NMP are placed in the beaker of 200mL, mix and ultrasonic 1h, make it fully mix dispersion, the graphene dispersing solution of 500 mg/L can be obtained.The graphene dispersing solution of configuration is diluted, get respectively 1mL, 2mL, 3mL, 4 mL, 5 mL, 6mL above-mentioned graphene dispersing solution be placed in the volumetric flask of 50 mL, add NMP, be settled to the standard disperse liquid that 50 mL can obtain 10mg/L, 20mg/L, 30mg/L, 40mg/L, 50mg/L, 60mg/L.Adopt Shanghai unit to analyse the absorbance of UV-5200 ultraviolet-visible photometer test wavelength λ=660 nm standard specimen, draw the typical curve of standard specimen absorbance and dispersion degree, as shown in Figure 2.
From accompanying drawing 2, R
2=0.9913, this typical curve linear relationship is better.
3) measurement of unknown dispersion degree dispersion liquid: by the Graphene NMP dispersion liquid of unknown dispersion degree, adopt Shanghai unit to analyse UV-5200 ultraviolet-visible photometer and measure its absorbance at λ=660 nm wavelength, obtaining dispersion degree according to aforementioned gained typical curve is again 485mg/L, then the measured value (X) of the dispersion degree of above-mentioned Graphene NMP dispersion liquid is 485mg/L.
Separately get the unknown dispersion degree Graphene NMP dispersion liquid that 50ml is identical, by its evaporate to dryness, weigh its quality, then the actual value (T) calculating Graphene NPM dispersion liquid is 475mg/L.
The Graphene NMP dispersion liquid getting two groups of unknown dispersion degree again operates according to preceding method, obtains measured value (X) and actual value (T) respectively, the results are shown in Table 1.
According to the relative error once between formulae discovery gained measured value and weighing value, result is equally in table 1.
Relative error=∣ measured value-Zhen is real is worth ∣/actual value × 100%
Table 1, the relative error magnitudes that in Graphene NMP dispersion liquid, dispersion degree is measured
| Numbering | 1-① | 2-② | 3-③ |
| Measured value (X) (mg/L) | 485 | 400 | 525 |
| Actual value (T) (mg/L) | 495 | 395 | 543 |
| Relative error (%) | 2% | 1% | 3% |
Table 1 shows, ultraviolet-visible photometer is utilized to measure its absorbance at λ=660 nm wavelength to Graphene NMP dispersion liquid, and the typical curve drawn, the dispersion degree relative error that recycling typical curve measures unknown Graphene NMP dispersion liquid is less, accuracy is higher, and the quantitative analysis method of visible the present invention to Graphene NMP dispersion liquid has outstanding substantive distinguishing features and significant progress.
Embodiment four: the present embodiment is tested for Graphene dispersion degree in aqueous.
1) preparation method of Graphene is with embodiment one.
2) configure Graphene-water quality standard dispersion liquid and draw the typical curve of Graphene-aqueous dispersions.The Graphene of 50mg, 100mL water are placed in the beaker of 200mL, mix and ultrasonic 1h, make it fully mix dispersion, the graphene dispersing solution of 500 mg/L can be obtained.The graphene dispersing solution of configuration is diluted, get respectively 1mL, 2mL, 3mL, 4 mL, 5 mL, 6mL above-mentioned graphene dispersing solution be placed in the volumetric flask of 50 mL, add water, be settled to the standard disperse liquid that 50 mL can obtain 10mg/L, 20mg/L, 30mg/L, 40mg/L, 50mg/L, 60mg/L.Adopt Shanghai unit to analyse the absorbance of UV-5200 ultraviolet-visible photometer test wavelength λ=660 nm standard specimen, draw the typical curve of standard specimen absorbance and dispersion degree, as shown in Figure 3.
From accompanying drawing 3, R
2=0.9924, this typical curve linear relationship is better.
3) measurement of unknown dispersion degree dispersion liquid: by the Graphene-aqueous dispersions of unknown dispersion degree, adopt Shanghai unit to analyse UV-5200 ultraviolet-visible photometer and measure its absorbance at λ=660 nm wavelength, obtaining dispersion degree according to aforementioned gained typical curve is again 515mg/L, then the measured value (X) of the dispersion degree of above-mentioned Graphene NMP dispersion liquid is 515mg/L.
Separately get unknown dispersion degree Graphene-aqueous dispersions that 50ml is identical, by its evaporate to dryness, weigh its quality, then the actual value (T) calculating Graphene-aqueous dispersions is 509mg/L.
Graphene-the aqueous dispersions getting two groups of unknown dispersion degree again operates according to preceding method, obtains measured value (X) and actual value (T) respectively, the results are shown in Table 2.
According to the relative error once between formulae discovery gained measured value and weighing value, result is equally in table 1.
Relative error=∣ measured value-Zhen is real is worth ∣/actual value × 100%
Table 2, the relative error magnitudes that in Graphene-aqueous dispersions, dispersion degree is measured
| Numbering | 1-① | 2-② | 3-③ |
| Measured value (X) (mg/L) | 515 | 385 | 459 |
| Actual value (T) (mg/L) | 509 | 380 | 451 |
| Relative error (%) | 1% | 1.3% | 1.8% |
Table 2 shows, ultraviolet-visible photometer is utilized to measure its absorbance at λ=660 nm wavelength to Graphene-aqueous dispersions, and the typical curve drawn, the dispersion degree relative error that recycling typical curve measures unknown Graphene-aqueous dispersions is less, accuracy is higher, and the quantitative analysis method of visible the present invention to Graphene-aqueous dispersions has outstanding substantive distinguishing features and significant progress.
Embodiment five: the present embodiment is tested for the dispersion degree of Graphene in dinethylformamide (DMF) solution.
1) preparation method of Graphene is with embodiment one.
2) configure Graphene DMF standard disperse liquid and draw the typical curve of Graphene DMF dispersion liquid.The Graphene of 50mg, 100mL water are placed in the beaker of 200mL, mix and ultrasonic 1h, make it fully mix dispersion, the graphene dispersing solution of 500 mg/L can be obtained.The graphene dispersing solution of configuration is diluted, get respectively 1mL, 2mL, 3mL, 4 mL, 5 mL, 6mL above-mentioned graphene dispersing solution be placed in the volumetric flask of 50 mL, add DMF, be settled to the standard disperse liquid that 50 mL can obtain 10mg/L, 20mg/L, 30mg/L, 40mg/L, 50mg/L, 60mg/L.Adopt Shanghai unit to analyse the absorbance of UV-5200 ultraviolet-visible photometer test wavelength λ=660 nm standard specimen, draw the typical curve of standard specimen absorbance and dispersion degree, as shown in Figure 4.
From accompanying drawing 4, R2=0.9925, this typical curve linear relationship is better.
3) measurement of unknown dispersion degree dispersion liquid: by the Graphene DMF dispersion liquid of unknown dispersion degree, adopt Shanghai unit to analyse UV-5200 ultraviolet-visible photometer and measure its absorbance at λ=660 nm wavelength, obtaining dispersion degree according to aforementioned gained typical curve is again 498mg/L, then the measured value (X) of the dispersion degree of above-mentioned Graphene DMF dispersion liquid is 498mg/L.
Separately get unknown dispersion degree Graphene-aqueous dispersions that 50ml is identical, by its evaporate to dryness, weigh its quality, then the actual value (T) calculating Graphene DMF dispersion liquid is 490mg/L.
The Graphene DMF dispersion liquid getting two groups of unknown dispersion degree again operates according to preceding method, obtains measured value (X) and actual value (T) respectively, the results are shown in Table 3.
According to the relative error once between formulae discovery gained measured value and weighing value, result is equally in table 1.
Relative error=∣ measured value-Zhen is real is worth ∣/actual value × 100%
Table 3, the relative error magnitudes that in Graphene DMF dispersion liquid, dispersion degree is measured
| Numbering | 1-① | 2-② | 3-③ |
| Measured value (X) (mg/L) | 498 | 510 | 367 |
| Actual value (T) (mg/L) | 490 | 502 | 362 |
| Relative error (%) | 1.6% | 1.6% | 1.4% |
Table 3 shows, ultraviolet-visible photometer is utilized to measure its absorbance at λ=660 nm wavelength to Graphene DMF dispersion liquid, and the typical curve drawn, the dispersion degree relative error that recycling typical curve measures unknown Graphene DMF dispersion liquid is less, accuracy is higher, and the quantitative analysis method of visible the present invention to Graphene DMF dispersion liquid has outstanding substantive distinguishing features and significant progress.
Embodiment six: the present embodiment is tested for the dispersion degree of Graphene in dimethyl sulfoxide (DMSO) (DMSO) solution.
1) preparation method of Graphene is with embodiment one.
2) configure Graphene DMSO standard disperse liquid and draw the typical curve of Graphene DMSO dispersion liquid.The Graphene of 50mg, 100mL water are placed in the beaker of 200mL, mix and ultrasonic 1h, make it fully mix dispersion, the graphene dispersing solution of 500 mg/L can be obtained.The graphene dispersing solution of configuration is diluted, get respectively 1mL, 2mL, 3mL, 4 mL, 5 mL, 6mL above-mentioned graphene dispersing solution be placed in the volumetric flask of 50 mL, add DMSO, be settled to the standard disperse liquid that 50 mL can obtain 10mg/L, 20mg/L, 30mg/L, 40mg/L, 50mg/L, 60mg/L.Adopt Shanghai unit to analyse the absorbance of UV-5200 ultraviolet-visible photometer test wavelength λ=660 nm standard specimen, draw the typical curve of standard specimen absorbance and dispersion degree, as shown in Figure 5.
From accompanying drawing 5, R2=0.9932, this typical curve linear relationship is better.
3) measurement of unknown dispersion degree dispersion liquid: by the Graphene DMSO dispersion liquid of unknown dispersion degree, adopt Shanghai unit to analyse UV-5200 ultraviolet-visible photometer and measure its absorbance at λ=660 nm wavelength, obtaining dispersion degree according to aforementioned gained typical curve is again 433mg/L, then the measured value (X) of the dispersion degree of above-mentioned Graphene DMSO dispersion liquid is 433mg/L.
Separately get unknown dispersion degree Graphene-aqueous dispersions that 50ml is identical, by its evaporate to dryness, weigh its quality, then the actual value (T) calculating Graphene DMSO dispersion liquid is 428mg/L.
The Graphene DMSO dispersion liquid getting two groups of unknown dispersion degree again operates according to preceding method, obtains measured value (X) and actual value (T) respectively, the results are shown in Table 4.
According to the relative error once between formulae discovery gained measured value and weighing value, result is equally in table 1.
Relative error=∣ measured value-Zhen is real is worth ∣/actual value × 100%
Table 4, the relative error magnitudes that in Graphene DMSO dispersion liquid, dispersion degree is measured
| Numbering | 1-① | 2-② | 3-③ |
| Measured value (X) (mg/L) | 433 | 509 | 336 |
| Actual value (T) (mg/L) | 428 | 500 | 330 |
| Relative error (%) | 1.2% | 1.8% | 1.8% |
Table 4 shows, ultraviolet-visible photometer is utilized to measure its absorbance at λ=660 nm wavelength to Graphene DMSO dispersion liquid, and the typical curve drawn, the dispersion degree relative error that recycling typical curve measures unknown Graphene DMSO dispersion liquid is less, accuracy is higher, and the quantitative analysis method of visible the present invention to Graphene DMSO dispersion liquid has outstanding substantive distinguishing features and significant progress.
Example example seven: modified graphene can pass through cetyl trimethyl ammonium bromide (CTAB), polyvinylpyrrolidone (PVP), lauryl sodium sulfate (SDS), any one in Tween-60 carries out modification to Graphene, the spreading agent of modified graphene is water, 1-METHYLPYRROLIDONE (NMP), dinethylformamide (DMF), any one in dimethyl sulfoxide (DMSO) (DMSO), the present embodiment is tested for the dispersion degree of Graphene in nmp solution of cetyl trimethyl ammonium bromide (CTAB) modification.
1) graphene oxide is prepared by Hummers method, with embodiment one.
2) with cetyl trimethyl ammonium bromide (CTAB), modification is carried out to Graphene.
3) nmp solution of CTAB modified graphene is configured and drawing standard curve.50mg modified graphene, 100mL distilled water are placed in the beaker of 200mL, mix and ultrasonic 1h, make it fully mix dispersion, the modified graphene dispersion liquid of 500 mg/L can be obtained.The modified graphene dispersion liquid of configuration is diluted, obtains the standard disperse liquid of 10-60mg/L.The absorbance of test wavelength λ=660 nm standard specimen, draws the typical curve of standard specimen absorbance and dispersion degree, as shown in Figure 6.
From accompanying drawing 6, R2=0.9919, this typical curve linear relationship is better.
4) measurement of unknown dispersion degree dispersion liquid: by the modified graphene NMP dispersion liquid of unknown dispersion degree, adopt Shanghai unit to analyse UV-5200 ultraviolet-visible photometer and measure its absorbance at λ=660 nm wavelength, obtaining dispersion degree according to aforementioned gained typical curve is again 545mg/L, then the measured value (X) of the dispersion degree of above-mentioned modified graphene NMP dispersion liquid is 545mg/L.
Separately get the unknown dispersion degree modified graphene NMP dispersion liquid that 50ml is identical, by its evaporate to dryness, weigh its quality, then the actual value (T) calculating modified graphene NPM dispersion liquid is 537mg/L.
The modified graphene NMP dispersion liquid getting two groups of unknown dispersion degree again operates according to preceding method, obtains measured value (X) and actual value (T) respectively, the results are shown in Table 5.
According to the relative error once between formulae discovery gained measured value and weighing value, result is equally in table 1.
Relative error=∣ measured value-Zhen is real is worth ∣/actual value × 100%
Table 5, the relative error magnitudes that in modified graphene NMP dispersion liquid, dispersion degree is measured
| Numbering | 1-① | 2-② | 3-③ |
| Measured value (X) (mg/L) | 545 | 469 | 395 |
| Actual value (T) (mg/L) | 537 | 464 | 400 |
| Relative error (%) | 1.5% | 1.1% | 1% |
Table 5 shows, ultraviolet-visible photometer is utilized to measure its absorbance at λ=660 nm wavelength to modified graphene NMP dispersion liquid, and the typical curve drawn, the dispersion degree relative error that recycling typical curve measures unknown modified graphene NMP dispersion liquid is less, accuracy is higher, and the quantitative analysis method of visible the present invention to modified graphene dispersion liquid has outstanding substantive distinguishing features and significant progress.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. a quantitative analysis method for graphene dispersing solution, is characterized in that: comprise the following steps:
1) by graphene dispersion in spreading agent, configure different dispersion degree Graphene standard disperse liquid;
2) drawing standard curve: adopt ultraviolet-visible pectrophotometer at 660 nm wavelength places respectively determination steps 1) absorbance of described standard disperse liquid, by the corresponding relation of known Graphene standard scores divergence and absorbance, draw the typical curve of absorbance-dispersion degree;
3) sample analysis: by the graphene dispersing solution of unknown dispersion degree to be measured, its absorbance is measured with ultraviolet-visible pectrophotometer, by and step 2) identical method measures the absorbance of the graphene dispersing solution to be measured of unknown dispersion degree, draws the dispersion degree of described graphene dispersing solution to be measured according to described typical curve;
Described spreading agent is water, 1-METHYLPYRROLIDONE, dinethylformamide, any one in dimethyl sulfoxide (DMSO).
2. the quantitative analysis method of a kind of graphene dispersing solution according to claim 1, it is characterized in that: the divergence criteria curve of described graphene dispersing solution is drawn by following methods: the graphene dispersing solution configuring different dispersion degree, measure its absorbance respectively at 660 nm wavelength places; Get the dispersion liquid of above-mentioned different dispersion degree more respectively, dried, record the dispersion liquid dispersion degree separately of different dispersion degree, then draw out typical curve according to the corresponding relation of dispersion degree and absorbance.
3. the quantitative analysis method of a kind of graphene dispersing solution according to claim 2, is characterized in that: described graphene dispersing solution dispersion degree rises in gradient.
4. the quantitative analysis method of a kind of graphene dispersing solution according to claim 3, is characterized in that: described graphene dispersing solution dispersion degree scope is 5 mg/L-100 mg/L.
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| CN108693129B (en) * | 2018-03-21 | 2020-12-04 | 常州第六元素材料科技股份有限公司 | Characterization method and characterization model for graphene oxide dispersity |
| CN108872167A (en) * | 2018-04-12 | 2018-11-23 | 温州医科大学附属第二医院、温州医科大学附属育英儿童医院 | A kind of graphene oxide quantitative analysis method based on fluorescent quenching |
| CN110470576A (en) * | 2019-08-07 | 2019-11-19 | 哈工大机器人(中山)无人装备与人工智能研究院 | Dispersion degree detection system, production system and production control method |
| CN110470576B (en) * | 2019-08-07 | 2022-04-01 | 哈工大机器人(中山)无人装备与人工智能研究院 | Dispersion degree detection system, production system and production control method |
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