CN104677846A - Quantitative analysis method for graphene dispersion liquid - Google Patents
Quantitative analysis method for graphene dispersion liquid Download PDFInfo
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- graphene
- dispersion degree
- dispersion liquid
- absorbance
- dispersing solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000006185 dispersion Substances 0.000 title claims abstract description 189
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 161
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 134
- 239000007788 liquid Substances 0.000 title claims abstract description 88
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000004445 quantitative analysis Methods 0.000 title claims abstract description 15
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 48
- 238000002835 absorbance Methods 0.000 claims description 44
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000004458 analytical method Methods 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 230000007480 spreading Effects 0.000 claims description 5
- 238000003892 spreading Methods 0.000 claims description 5
- 238000012360 testing method Methods 0.000 abstract description 21
- 230000008569 process Effects 0.000 abstract description 2
- 238000000870 ultraviolet spectroscopy Methods 0.000 abstract description 2
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 12
- 238000005259 measurement Methods 0.000 description 11
- 229910002804 graphite Inorganic materials 0.000 description 8
- 239000010439 graphite Substances 0.000 description 8
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 238000004064 recycling Methods 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- -1 graphite alkene Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012113 quantitative test Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- 229920001214 Polysorbate 60 Polymers 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510090327.7A CN104677846A (en) | 2015-02-28 | 2015-02-28 | Quantitative analysis method for graphene dispersion liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510090327.7A CN104677846A (en) | 2015-02-28 | 2015-02-28 | Quantitative analysis method for graphene dispersion liquid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104677846A true CN104677846A (en) | 2015-06-03 |
Family
ID=53313194
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510090327.7A Pending CN104677846A (en) | 2015-02-28 | 2015-02-28 | Quantitative analysis method for graphene dispersion liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104677846A (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106248605A (en) * | 2016-08-05 | 2016-12-21 | 常州第六元素材料科技股份有限公司 | The quantitative detecting method of a kind of graphene oxide degree of oxidation and the building method of standard curve used |
| CN106644812A (en) * | 2016-12-02 | 2017-05-10 | 山东圣泉新材料股份有限公司 | Method for quantitatively detecting graphene in solution |
| CN106770262A (en) * | 2017-02-22 | 2017-05-31 | 济宁利特纳米技术有限责任公司 | A kind of method of graphene oxide powder manganese content detection |
| CN106841529A (en) * | 2017-03-10 | 2017-06-13 | 南京信息工程大学 | A kind of method for determining carbon nanotubes aqueous dispersion concentration |
| CN107202770A (en) * | 2017-08-03 | 2017-09-26 | 中国科学院青岛生物能源与过程研究所 | A kind of method of quick detection poly-dopamine stable dispersions concentration |
| CN107860689A (en) * | 2017-11-07 | 2018-03-30 | 青岛大学 | A kind of assay method of silver nano material particle size and its content |
| CN108180846A (en) * | 2017-11-30 | 2018-06-19 | 广州兴森快捷电路科技有限公司 | Organic guarantor welds the process control method of film and film thickness acquisition methods |
| CN108693129A (en) * | 2018-03-21 | 2018-10-23 | 常州第六元素材料科技股份有限公司 | The method and graphene oxide dispersion degree characterization model of quantitatively characterizing graphene oxide dispersion degree |
| 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 |
| TWI694054B (en) * | 2015-09-18 | 2020-05-21 | 日商東麗股份有限公司 | Graphene dispersion liquid and manufacturing method thereof, manufacturing method of graphene-electrode active material composite particles, and manufacturing method of electrode paste |
| CN111795939A (en) * | 2020-07-21 | 2020-10-20 | 郑州安图生物工程股份有限公司 | Method for monitoring subpackaging uniformity of magnetic particle suspension |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102879348A (en) * | 2012-09-26 | 2013-01-16 | 攀枝花学院 | Quantitative analysis method for oxidized graphene |
| CN103398965A (en) * | 2013-08-19 | 2013-11-20 | 济宁利特纳米技术有限责任公司 | Method for detecting manganese content in graphene oxide and graphene samples |
| CN104211053A (en) * | 2014-09-04 | 2014-12-17 | 济宁利特纳米技术有限责任公司 | Preparation method of modified graphene aqueous dispersion |
-
2015
- 2015-02-28 CN CN201510090327.7A patent/CN104677846A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102879348A (en) * | 2012-09-26 | 2013-01-16 | 攀枝花学院 | Quantitative analysis method for oxidized graphene |
| CN103398965A (en) * | 2013-08-19 | 2013-11-20 | 济宁利特纳米技术有限责任公司 | Method for detecting manganese content in graphene oxide and graphene samples |
| CN104211053A (en) * | 2014-09-04 | 2014-12-17 | 济宁利特纳米技术有限责任公司 | Preparation method of modified graphene aqueous dispersion |
Non-Patent Citations (2)
| Title |
|---|
| G. WANG ET AL.: "Synthesis of enhanced hydrophilic and hydrophobic graphene oxide nanosheets by a solvothermal method", 《CARBON》 * |
| 叶炜宗 等: "石墨烯在有机溶剂中的分散性能研究", 《中国化工贸易》 * |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI694054B (en) * | 2015-09-18 | 2020-05-21 | 日商東麗股份有限公司 | Graphene dispersion liquid and manufacturing method thereof, manufacturing method of graphene-electrode active material composite particles, and manufacturing method of electrode paste |
| CN106248605A (en) * | 2016-08-05 | 2016-12-21 | 常州第六元素材料科技股份有限公司 | The quantitative detecting method of a kind of graphene oxide degree of oxidation and the building method of standard curve used |
| CN106644812B (en) * | 2016-12-02 | 2019-10-15 | 山东圣泉新材料股份有限公司 | The quantitative detecting method of graphene in a kind of solution |
| CN106644812A (en) * | 2016-12-02 | 2017-05-10 | 山东圣泉新材料股份有限公司 | Method for quantitatively detecting graphene in solution |
| CN106770262A (en) * | 2017-02-22 | 2017-05-31 | 济宁利特纳米技术有限责任公司 | A kind of method of graphene oxide powder manganese content detection |
| CN106841529A (en) * | 2017-03-10 | 2017-06-13 | 南京信息工程大学 | A kind of method for determining carbon nanotubes aqueous dispersion concentration |
| CN107202770A (en) * | 2017-08-03 | 2017-09-26 | 中国科学院青岛生物能源与过程研究所 | A kind of method of quick detection poly-dopamine stable dispersions concentration |
| CN107860689B (en) * | 2017-11-07 | 2019-11-08 | 青岛大学 | A kind of measuring method of particle size and content of silver nano material |
| CN107860689A (en) * | 2017-11-07 | 2018-03-30 | 青岛大学 | A kind of assay method of silver nano material particle size and its content |
| CN108180846A (en) * | 2017-11-30 | 2018-06-19 | 广州兴森快捷电路科技有限公司 | Organic guarantor welds the process control method of film and film thickness acquisition methods |
| CN108180846B (en) * | 2017-11-30 | 2020-11-17 | 广州兴森快捷电路科技有限公司 | Process control method and film thickness obtaining method of organic solderability preservative film |
| CN108693129A (en) * | 2018-03-21 | 2018-10-23 | 常州第六元素材料科技股份有限公司 | The method and graphene oxide dispersion degree characterization model of quantitatively characterizing graphene oxide dispersion degree |
| 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 |
| CN111795939A (en) * | 2020-07-21 | 2020-10-20 | 郑州安图生物工程股份有限公司 | Method for monitoring subpackaging uniformity of magnetic particle suspension |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104677846A (en) | Quantitative analysis method for graphene dispersion liquid | |
| Zhang et al. | Fe (III)-based metal–organic framework-derived core–shell nanostructure: Sensitive electrochemical platform for high trace determination of heavy metal ions | |
| Wang et al. | An ionic liquid-modified graphene based molecular imprinting electrochemical sensor for sensitive detection of bovine hemoglobin | |
| Zhu et al. | Hierarchical flower-like zinc oxide nanosheets in-situ growth on three-dimensional ferrocene-functionalized graphene framework for sensitive determination of epinephrine and its oxidation derivative | |
| Ling et al. | QSARs to predict adsorption affinity of organic micropollutants for activated carbon and β-cyclodextrin polymer adsorbents | |
| Fu et al. | Sensitive detection of ketamine with an electrochemical sensor based on UV-induced polymerized molecularly imprinted membranes at graphene and MOFs modified electrode | |
| Gong et al. | A highly sensitive photoelectrochemical detection of perfluorooctanic acid with molecularly imprined polymer-functionalized nanoarchitectured hybrid of AgI–BiOI composite | |
| Teng et al. | Electrochemical sensor for paracetamol recognition and detection based on catalytic and imprinted composite film | |
| CN104610486B (en) | A kind of super cross-linked polymer of ion liquid functionalization and preparation method and application | |
| Lin et al. | Ultrasensitive detection of formaldehyde in gas and solutions by a catalyst preplaced sensor based on a pillar [5] arene derivative | |
| Chen et al. | Highly sensitive electrochemical sensor for sunset yellow based on the enhancement effect of alumina microfibers | |
| Liu et al. | Electrochemical sensor based on covalent organic frameworks/MWCNT for simultaneous detection of catechol and hydroquinone | |
| Kazemi et al. | Development of a novel mixed hemimicelles dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene for the separation and preconcentration of fluoxetine in different matrices before its determination by fiber optic linear array spectrophotometry and mode-mismatched thermal lens spectroscopy | |
| Mao et al. | A novel and green CTAB-functionalized graphene nanosheets electrochemical sensor for Sudan I determination | |
| Kumar et al. | Electrochemical activation of copper oxide decorated graphene oxide modified carbon paste electrode surface for the simultaneous determination of hazardous Di-hydroxybenzene isomers | |
| Zheng et al. | N-doped carbon nanotube frameworks modified electrode for the selective sensing of hydroquinone and catechol | |
| Ni et al. | Voltammetric investigation of DNA damage induced by nitrofurazone and short-lived nitro-radicals with the use of an electrochemical DNA biosensor | |
| Damodaran | Recent advances in NMR spectroscopy of ionic liquids | |
| Lian et al. | A highly selective melamine sensor relying on intensified electrochemiluminescence of the silica nanoparticles doped with [Ru (bpy) 3] 2+/molecularly imprinted polymer modified electrode | |
| Lin et al. | Voltammetric analysis with the use of a novel electro-polymerised graphene-nafion film modified glassy carbon electrode: Simultaneous analysis of noxious nitroaniline isomers | |
| Prashanth et al. | Fabrification of electroreduced graphene oxide–bentonite sodium composite modified electrode and its sensing application for linezolid | |
| Hou et al. | Graphene oxide reinforced ionic liquid-functionalized adsorbent for solid-phase extraction of phenolic acids | |
| Aich et al. | Preparation and characterization of stable aqueous higher-order fullerenes | |
| CN109187687B (en) | Preparation of conjugated organic microporous material modified electrode and application of modified electrode as peroxynitroso anion electrochemical sensor | |
| Misiuk et al. | Spectroscopic investigations on the inclusion interaction between hydroxypropyl-β-cyclodextrin and bupropion |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150603 |