CN102944528A - Method for measuring concentration of C60 nanocrystal particles in water medium - Google Patents
Method for measuring concentration of C60 nanocrystal particles in water medium Download PDFInfo
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- CN102944528A CN102944528A CN2012104582106A CN201210458210A CN102944528A CN 102944528 A CN102944528 A CN 102944528A CN 2012104582106 A CN2012104582106 A CN 2012104582106A CN 201210458210 A CN201210458210 A CN 201210458210A CN 102944528 A CN102944528 A CN 102944528A
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Abstract
The invention discloses a method for measuring the concentration of C60 nanocrystal particles in water medium. The method comprises the following steps: pure glacial acetic acid is added into nC60 water suspension which contains a surface active agent to destabilize; toluene is used to extract C60 in the destabilized water suspension; the water suspension is stirred; the water suspension is frozen and stirred; then, an ultraviolet-visible spectrophotometer is used to measure the absorbance of the upper layer of toluene solution of the frozen water suspension; the concentration of C60 in a sample is calculated according to a standard curve through the absorbance; and the rate of the C60 concentration which is obtained through calculating to the standard C60 concentration is used as the recovery rate of the C60 concentration measurement. According to the method, the glacial acetic acid is used as a destabilizing agent to eliminate the phenomenon that emulsification and foams are generated during the C60 concentration measurement process under the condition of containing the surface active agent, so that the C60 concentration measurement can be enabled to be normally carried out, and moreover, the higher C60 recovery rate can be obtained.
Description
Technical field
The wood invention relates to field of nanometer material technology, relates in particular to improve the method that nC60 takes off steady efficient in a kind of aqueous medium in the C60 nano crystal particles concentration determination process.
Background technology
C60 is the third allotrope of carbon, is a member in the fullerene family.The structure of C60 uniqueness makes it be widely used in the fields [1-5] such as electronics, optics and pharmacy.Because C60 uses widely, it can discharge into by the approach of point source or non-point source in the water environment, such as the cosmetics that contain nano material of production plant, landfill yard, atmospheric sedimentation, storm runoff, consumer's discharging and nano pesticide etc.The cumulative concentration of C60 in water body environment can reducing and the continuous research and development of new product and increase gradually [6] along with the increasing gradually of market, its producing cost gradually.If C60 enters in the surface water and groundwater as the drinking water source by point source or non-point pollution, then certainly will cause larger potential threat to human health.Be the potential risk of correct evaluation C60 to environment and the mankind, the Concentration Detection of C60 is very necessary in the development environment.
C60 has the three-dimensional aromatic structure of symmetrical hollow cage shape, has strong-hydrophobicity, and is water-soluble hardly, also insoluble or be slightly soluble in most organic solvents [7,8].But studies show that, C60 can form stable nano crystal particles (water stable crystalline nano-scale C60 aggregates by long-term stirring in water, nC60), size in several nanometers between 200 nanometers, surface charge arrives-30mV-9, simultaneously, researchers have also developed the technology [9-13] of utilizing organic solvent displacement and ultrasonic quick preparation stable C60 nano crystal particles in water.
The detection technique of generally using for the concentration determination of the nC60 that forms in the aqueous medium at present comprises two steps: at first nC60 is taken off surely, make it enter the organic solvent phase from water, the organic solvent of extraction C60 commonly used is toluene at present; The second step detecting instrument is such as the C60 concentration in the detection organic solvents such as infrared spectrum, high performance liquid chromatography, mass spectrum, uv-vis spectra.Wherein, the nC60 in first step takes off the organic efficiency that steady rate directly determines C60, and and then affects the accuracy of C60 concentration determination.After C60 discharged into water environment, the aqueous medium environmental factor can obviously change the physicochemical characteristics of C60 nano crystal particles, such as natural organic substance (NOM) thereby and surfactant can diffusion, depolymerization further stablizes the C60 nano crystal particles.The variation of C60 nano crystal particles physicochemical property exerts an influence to its concentration determination meeting, easily causes in the mensuration process to produce emulsion, and produce foam in taking off steady agitation.Wood invention proposes to adopt glacial acetic acid (GAA) to eliminate emulsion layer and foam as coagulant for emulsification and bubble-related issues in the C60 nano crystal particles concentration determination process, improves and takes off steady efficient, and and then improve the recovery of C60.
List of references:
[1]Kroto,H.W.,A.Allaf，and?S.Balm,C60:Buckminsterfullerene.Chemical?Reviews,1991.91(6):p.1213-1235.
[2]Innocenzi,P.and?G.Brusatin,Fullerene-based?organic-inorganic?nanocomposites?and?their?applications.Chemistry?of?materials,2001.13(10):p.3126-3139.
[3]Ungurenasu,C.and?A.Airinei,Highly?stable?C60/poly(vinylpyrrolidone)charge-transfer?complexes?afford?new?predictions?for?biological?applications?of?underivatized?fullerenes.Journal?of?medicinal?chemistry,2000.43(16):p.3186-3188.
[4]Palstra,T.,et?al.,Superconductiviry?at?40K?in?cesium?doped?C<sub>60</sub>.Solid?state?communications,1995.93(4):p.327-330.
[5]Rouse,J.G.,et?al.,Effects?of?mechanical?flexion?on?the?penetration?of?fullerene?amino?acid-derivatized?peptide?nanoparticles?through?skin.Nano?Letters,2007.7(1):p.155-160.
[6]Zhang,Y.,Chen,Y.S.,Westerhoff，P.,Hristovski,K.,Crittenden,J.Stability?of?commercial?metal?oxide?nanoparticles?in?water.Water?Res.,2008,42,2204-2212.
[7]Heymann,D.Solubility?of?C
60?and?C
70?in?water.Lunar?Planet.Sci.,1996,27,543-544.
[8]Heymann,D.Solubility?of?C
60?and?C
70?in?seven?normal?alcohols?and?their?deduced?solubility?in?water.Fullerene?Sci.Technol.,1996,4,509-515.
[9]Deguchi,S.,Alargova,R.G.,Tsujii,K.Stable?dispersions?of?fullerenes,C
60and?C
70,in?water.Preparation?and?Characterization.Langmuir,2001,17,6013-6017.
[10]Deguchi,S.,Mukai,S.-a.,Tsudome,M.,Horkoshi,K.Facile?generation?of?fullerene?nanoparticles?by?hand-granding.Adv.Mater.,2006,18,729-732.
[11]Andrievsky,G.V.,Kosevich,M.V.,Vovk,O.M.,Shelkovsky,V.S.,Vashchenko,L.A.On?the?production?of?an?aqueous?colloidal?solution?of?fullerenes.J.Chem.Soc.Chem.Commun.,1995,1281-1282.
[12]Fortner,J.D.,Lyon,D.Y.,Sayes,C.M.,Boyd,A.M.,Falkner,J.C.,Hotze,E.M.,Alemany,L.B.,Tao,Y.J.,Guo,W.,Ausman,K.D.,Colvin,V.L.,Hughes,J.B.C
60?in?water:nanocrystal?formation?and?microbial?response.Environ.Sci.Technol.,2005,39,4307-4316.
[13]Duncan,L.K.,Jinschek,J.R.,Vikesland,P.J.C
60?colloid?formation?in?aqueous?systems:effects?of?preparation?method?on?size,structure,and?surface?charge.Environ.Sci.Technol.,2008,42,173-178.
Summary of the invention
Because the defects of prior art, the object of the invention is to solve the emulsification and the frothing that occur in the C60 nano crystal particles concentration determination process in the aqueous medium, a kind of method of removing breast and froth breaking is provided, in the concentration determination process, take off steady rate to improve nC60, and and then improve the recovery of C60.
For achieving the above object, the invention provides the method for C60 nano crystal particles concentration determination in a kind of aqueous medium, specifically may further comprise the steps:
1, adding pure glacial acetic acid (GAA) in containing the nC60 water slurry of surfactant takes off surely;
2, with the C60 in the described water slurry that takes off after steady of toluene extraction step 1;
3, whipping step 2 described water slurries;
4, the water slurry after the described stirring of freezing step 3;
5, with the absorbance of ultraviolet-visible pectrophotometer at the described water slurry upper toluene solution after freezing of determination step under the 336nm wavelength 4;
6, the absorbance that step 5 is recorded is according to the C60 concentration in the typical curve calculation sample, and described typical curve is to set up according to the relational expression of C60 concentration and solution absorbance in the toluene;
7, step 6 calculate the C60 concentration of gained and C60 normal concentration be compared to the recovery of C60 in concentration determination.
Further, wherein, the described volume ratio that contains the nC60 water slurry of surfactant, pure glacial acetic acid, toluene of step 1 and step 2 is 1: 3: 1.
Further, wherein, the described stir speed (S.S.) of step 3 is 1750 rev/mins, and mixing time is 6 hours.
Further, wherein, the described freezing temperature of step 4 is-20 ℃, and the freezing time is 1 hour.
Further, wherein, the normal concentration of the described C60 of step 7 is for utilizing Mg (ClO
4)
2As coagulant, do not containing under the surfactant condition, the C60 concentration of mensuration specifically may further comprise the steps:
A, in the nC60 water slurry, add Mg (ClO
4)
2Solution takes off surely, described Mg (ClO
4)
2The concentration of solution is 100mmol/L;
B, with the C60 in the described water slurry that takes off after steady of toluene extraction step a;
C, the described water slurry of whipping step b;
Water slurry after d, the described stirring of freezing step c;
E, with the absorbance of ultraviolet-visible pectrophotometer at the described water slurry upper toluene solution after freezing of determination step d under the 336nm wavelength;
F, absorbance that step e is recorded are according to the C60 concentration in the typical curve calculation sample, and described typical curve is to set up according to the relational expression of C60 concentration and solution absorbance in the toluene.
Further, wherein, the described nC60 water slurry of step a and step b, Mg (ClO
4)
2The volume ratio of solution, toluene is 2: 1: 2.
Further, wherein, the described stir speed (S.S.) of step c is 1750 rev/mins, and mixing time is 6 hours.
Further, wherein, the described freezing temperature of steps d is-20 ℃, and the freezing time is 1 hour.
The present invention utilizes GAA as coagulant, the nC60 water slurry that contains surfactant is taken off surely, compare with other coagulant of employing, GAA can eliminate as coagulant and contain under the surfactant condition, the emulsification and the frothing that produce in the C60 concentration determination process can guarantee normally carrying out of C60 concentration determination.In the better embodiment of wood invention, utilize C60 concentration that GAA measures as coagulant and C60 normal concentration be compared to the recovery of C60 in concentration determination, wherein, normal concentration is for utilizing Mg (ClO
4)
2As coagulant, do not containing under the surfactant condition C60 concentration of mensuration.The result shows that utilizing GAA can obtain Billy as coagulant uses Mg (ClO
4)
2As the higher C60 recovery of coagulant.
Embodiment
In the better embodiment of wood invention, adopt the phase transfer of toluene and water to prepare C60 nano crystal particles water slurry, may further comprise the steps:
1, with the C60 powder dissolution of 8mg drying in 20ml toluene, vibrating was dissolved in the toluene C60 in 24 hours fully, was mixed with 400mg/L solution.
2, also made C60 progressively be transferred to aqueous phase in ultrasonic 48 hours C60 toluene solution and the mixing of 20ml water.
3, use Rotary Evaporators (Rotary Evaporators R-215, step fine jade rotary evaporation instrument system, vacuum controller V-850, V-700 vacuum pump) with toluene evaporates.
4, the aqueous solution behind the rotary evaporation is filtered by the nylon membrane of 0.22 μ m, obtains transparent brown color suspending liquid.
In another better embodiment of wood invention, the normal concentration of C60 is for utilizing Mg (ClO
4)
2As coagulant, do not containing under the surfactant condition, the C60 concentration of mensuration may further comprise the steps:
A, in 4ml nC60 water slurry, add 2ml Mg (ClO
4)
2Solution takes off surely, wherein Mg (ClO
4)
2The concentration of solution is 100mmol/L.
B, add 4mL toluene in the water slurry that takes off after steady, the C60 in the water slurry after steady is taken off in extraction.
C, under 1750 rev/mins rotating speed, stirred 6 hours.
D, water slurry is put into refrigerator under-20 ℃ of conditions freezing 1 hour.
E, get the top toluene solution, under the 336nm wavelength, measure the absorbance of toluene solution with ultraviolet-visible pectrophotometer (UV-1800).
F, with the absorbance that records according to the C60 concentration in the typical curve calculation sample, wherein typical curve is to set up according to the relational expression of C60 concentration and solution absorbance in the toluene.
Embodiment 1:
Contain the preparation of the C60 nano crystal particles water slurry of lauryl sodium sulfate (SDS), may further comprise the steps:
I, SDS is joined in the C60 nano crystal particles water slurry, wherein C60 concentration is 5mg/L, and the concentration of SDS is 20g/L (at it more than critical micelle concentration).
II, under 25 ℃ of conditions, stirred 24 hours at magnetic stirring apparatus, made the C60 nano crystal particles water slurry that contains SDS.
Utilize GAA as coagulant, be determined in the nC60 water slurry that contains SDS, the recovery of C60 in concentration determination may further comprise the steps:
A, contain in the nC60 water slurry of SDS at 4ml, add the pure GAA of 12ml and take off surely.
B, add 4mL toluene in the water slurry that takes off after steady, the C60 in the water slurry after steady is taken off in extraction.
C, under 1750 rev/mins rotating speed, stirred 6 hours.
D, water slurry is put into refrigerator under-20 ℃ of conditions freezing 1 hour.
E, get the top toluene solution, under the 336nm wavelength, measure the absorbance of toluene solution with ultraviolet-visible pectrophotometer (UV-1800).
F, with the absorbance that records according to the C60 concentration in the typical curve calculation sample, wherein typical curve is to set up according to the relational expression of C60 concentration and solution absorbance in the toluene.
G, to utilize C60 concentration that GAA records as coagulant and the ratio of the normal concentration of C60 be the recovery of C60 in concentration determination, and wherein, the normal concentration of C60 is for utilizing Mg (ClO
4)
2As coagulant, do not containing under the surfactant condition C60 concentration of mensuration.
Measurement result shows, as coagulant, between water and the toluene phase clear layering arranged with GAA, compares with the normal concentration of C60, and in containing the nC60 water slurry of SDS, the recovery of C60 in concentration determination is 86.8%.
Embodiment 2:
Contain the preparation of the C60 nano crystal particles water slurry of cetyl trimethyl ammonium bromide (CTAB), may further comprise the steps:
I, CTAB is joined in the C60 nano crystal particles water slurry, wherein C60 concentration is 5mg/L, and the concentration of CTAB is respectively 4g/L (at it more than critical micelle concentration).
II, under 25 ℃ of conditions, stirred 24 hours at magnetic stirring apparatus, made the C60 nano crystal particles water slurry that contains CTAB.
Utilize GAA as coagulant, be determined in the nC60 water slurry that contains CTAB, the recovery of C60 in concentration determination may further comprise the steps:
A, contain in the nC60 water slurry of CTAB at 4ml, add the pure GAA of 12ml and take off surely.
B, add 4mL toluene in the water slurry that takes off after steady, the C60 in the water slurry after steady is taken off in extraction.
C, under 1750 rev/mins rotating speed, stirred 6 hours.
D, water slurry is put into refrigerator under-20 ℃ of conditions freezing 1 hour.
E, get the top toluene solution, under the 336nm wavelength, measure the absorbance of toluene solution with ultraviolet-visible pectrophotometer (UV-1800).
F, with the absorbance that records according to the C60 concentration in the typical curve calculation sample, wherein typical curve is to set up according to the relational expression of C60 concentration and solution absorbance in the toluene.
G, to utilize concentration that GAA records as coagulant and the ratio of the normal concentration of C60 be the recovery of C60 in concentration determination, and wherein, normal concentration is for utilizing Mg (ClO
4)
2As coagulant, do not containing under the surfactant condition C60 concentration of mensuration.
Measurement result shows, as coagulant, between water and the toluene phase clear layering arranged with GAA, compares with the normal concentration of C60, contains in the nC60 water slurry of CTAB, and the recovery of C60 in concentration determination is 81.5%.
Embodiment 3:
Contain the preparation of the C60 nano crystal particles water slurry of polyoxydivinyl ether type non-ionic surfactant (TX100), may further comprise the steps:
I, TX100 is joined in the C60 nano crystal particles water slurry, wherein C60 concentration is 5mg/L, and the concentration of TX100 is 50g/L (at it more than critical micelle concentration).
II, under 25 ℃ of conditions, stirred 24 hours at magnetic stirring apparatus, made respectively the C60 nano crystal particles water slurry that contains TX100.
Utilize GAA as coagulant, be determined in the nC60 water slurry that contains TX100, the recovery of C60 in concentration determination may further comprise the steps:
A, contain in the nC60 water slurry of TX100 at 4ml, add the pure GAA of 12ml and take off surely.
B, add 4mL toluene in the water slurry that takes off after steady, the C60 in the water slurry after steady is taken off in extraction.
C, under 1750 rev/mins rotating speed, stirred 6 hours.
D, water slurry is put into refrigerator under-20 ℃ of conditions freezing 1 hour.
E, get the top toluene solution, under the 336nm wavelength, measure the absorbance of toluene solution with ultraviolet-visible pectrophotometer (UV-1800).
F, with the absorbance that records according to the C60 concentration in the typical curve calculation sample, wherein typical curve is to set up according to the relational expression of C60 concentration and solution absorbance in the toluene.
G, to utilize concentration that GAA records as coagulant and the ratio of the normal concentration of C60 be the recovery of C60 in concentration determination, and wherein, normal concentration is for utilizing Mg (ClO
4)
2As coagulant, do not containing under the surfactant condition C60 concentration of mensuration.
Measurement result shows, as coagulant, water and toluene have clear layering between mutually, compare with the normal concentration of C60 with GAA, and in containing the nC60 water slurry of TX100, the recovery of C60 in concentration determination is above 100%.
Comparative Examples 1:
Contain the preparation of the C60 nano crystal particles water slurry of TX100, may further comprise the steps:
I, TX100 is joined in the C60 nano crystal particles water slurry, wherein C60 concentration is 5mg/L, and the concentration of TX100 is 50g/L (at it more than critical micelle concentration).
II, under 25 ℃ of conditions, stirred 24 hours at magnetic stirring apparatus, made the C60 nano crystal particles water slurry that contains TX100.
Utilize Mg (ClO
4)
2As coagulant, be determined in the nC60 water slurry that contains TX100, the recovery of C60 in concentration determination may further comprise the steps:
A, contain in the nC60 water slurry of TX100 at 4ml, add 2ml Mg (ClO
4)
2Solution takes off surely, wherein Mg (ClO
4)
2The concentration of solution is 100mmol/L.
B, add 4mL toluene in the water slurry that takes off after steady, the C60 in the water slurry after steady is taken off in extraction.
C, under 1750 rev/mins rotating speed, stirred 6 hours.
D, water slurry is put into refrigerator under-20 ℃ of conditions freezing 1 hour.
E, get the top toluene solution, under the 336nm wavelength, measure the absorbance of toluene solution with ultraviolet-visible pectrophotometer (UV-1800).
F, with the absorbance that records according to the C60 concentration in the typical curve calculation sample, wherein typical curve is to set up according to the relational expression of C60 concentration and solution absorbance in the toluene.
G, utilize Mg (ClO
4)
2The concentration that records as coagulant is the recovery of C60 in concentration determination with the ratio of the normal concentration of C60, and wherein, normal concentration is for utilizing Mg (ClO
4)
2As coagulant, do not containing under the surfactant condition C60 concentration of mensuration.
Measurement result shows, utilizes Mg (ClO
4)
2As coagulant, after stirring 6 hours, foam appears in the nC60 water slurry that contains TX100, and after freezing, forms emulsion layer between water and the toluene phase, utilizes ultraviolet-visible pectrophotometer to be difficult to measure C60 concentration.
Comparative Examples 2:
Contain the preparation of the C60 nano crystal particles water slurry of SDS, may further comprise the steps:
I, SDS is joined in the C60 nano crystal particles water slurry, wherein C60 concentration is 5mg/L, and the concentration of SDS is 50g/L (at it more than critical micelle concentration).
II, under 25 ℃ of conditions, stirred 24 hours at magnetic stirring apparatus, made the C60 nano crystal particles water slurry that contains SDS.
Utilize Mg (ClO
4)
2As coagulant, be determined in the nC60 water slurry that contains SDS, the recovery of C60 in concentration determination may further comprise the steps:
A, contain in the nC60 water slurry of SDS at 4ml, add 2ml Mg (ClO
4)
2Solution takes off surely, wherein Mg (ClO
4)
2The concentration of solution is 100mmol/L.
B, add 4mL toluene in the water slurry that takes off after steady, the C60 in the water slurry after steady is taken off in extraction.
C, under 1750 rev/mins rotating speed, stirred 6 hours.
D, water slurry is put into refrigerator under-20 ℃ of conditions freezing 1 hour.
E, get the top toluene solution, under the 336nm wavelength, measure the absorbance of toluene solution with ultraviolet-visible pectrophotometer (UV-1800).
F, with the absorbance that records according to the C60 concentration in the typical curve calculation sample, wherein typical curve is to set up according to the relational expression of C60 concentration and solution absorbance in the toluene.
G, utilize Mg (ClO
4)
2The concentration that records as coagulant is the recovery of C60 in concentration determination with the ratio of the normal concentration of C60, and wherein, normal concentration is for utilizing Mg (ClO
4)
2As coagulant, do not containing under the surfactant condition C60 concentration of mensuration.
Measurement result shows, utilizes Mg (ClO
4)
2As coagulant, after stirring 6 hours, foam appears in the nC60 water slurry that contains SDS, and after freezing, forms emulsion layer between water and the toluene phase, utilizes ultraviolet-visible pectrophotometer to be difficult to measure the concentration of C60.
Comparative Examples 3:
Contain the preparation of the C60 nano crystal particles water slurry of CTAB, may further comprise the steps:
I, CTAB is joined in the C60 nano crystal particles water slurry, wherein C60 concentration is 5mg/L, and the concentration of CTAB is 50g/L (at it more than critical micelle concentration).
II, under 25 ℃ of conditions, stirred 24 hours at magnetic stirring apparatus, made the C60 nano crystal particles water slurry that contains CTAB.
Utilize Mg (ClO
4)
2As coagulant, be determined in the nC60 water slurry that contains CTAB, the recovery of C60 in concentration determination may further comprise the steps:
A, contain in the nC60 water slurry of CTAB at 4ml, add 2ml Mg (ClO
4)
2Solution takes off surely, wherein Mg (ClO
4)
2The concentration of solution is 100mmol/L.
B, add 4mL toluene in the water slurry that takes off after steady, the C60 in the water slurry after steady is taken off in extraction.
C, under 1750 rev/mins rotating speed, stirred 6 hours.
D, water slurry is put into refrigerator under-20 ℃ of conditions freezing 1 hour.
E, get the top toluene solution, under the 336nm wavelength, measure the absorbance of toluene solution with ultraviolet-visible pectrophotometer (UV-1800).
F, with the absorbance that records according to the C60 concentration in the typical curve calculation sample, wherein typical curve is to set up according to the relational expression of C60 concentration and solution absorbance in the toluene.
G, utilize Mg (ClO
4)
2The concentration that records as coagulant is the recovery of C60 in concentration determination with the ratio of the normal concentration of C60, and wherein, normal concentration is for utilizing Mg (ClO
4)
2As coagulant, do not containing under the surfactant condition C60 concentration of mensuration.
Measurement result shows, utilizes Mg (ClO
4)
2As coagulant, after stirring 6 hours, foam appears in the water slurry that contains CTAB, and after freezing, forms emulsion layer between water and the toluene phase, utilizes ultraviolet-visible pectrophotometer to be difficult to measure the concentration of C60.
More than describe preferred embodiment of the present invention in detail.The ordinary skill that should be appreciated that this area need not creative work just can make many modifications and variations according to the design of wood invention.Therefore, the technician all should be in the determined protection domain by claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment in all wood technologies field.
Claims (8)
1. the method for C60 nano crystal particles concentration determination in the aqueous medium is characterized in that, specifically may further comprise the steps:
1. adding pure glacial acetic acid in containing the nC60 water slurry of surfactant takes off surely;
2. with the 1. C60 in the described water slurry that takes off after steady of toluene extraction step;
3. 2. described water slurry of whipping step;
4. the 3. water slurry after the described stirring of freezing step;
5. use ultraviolet-visible pectrophotometer in the 4. absorbance of described water slurry upper toluene solution after freezing of determination step under the 336nm wavelength;
6. the absorbance that 5. step is recorded is according to the C60 concentration in the typical curve calculation sample, and described typical curve is to set up according to the relational expression of C60 concentration and solution absorbance in the toluene;
7. step 6. calculate the C60 concentration of gained and C60 normal concentration be compared to the recovery of C60 in concentration determination.
The method of claim 1, wherein step 1. with step 2. the described volume ratio that contains the nC60 water slurry of surfactant, described pure glacial acetic acid, described toluene be 1: 3: 1.
The method of claim 1, wherein step 3. described stir speed (S.S.) be 1750 rev/mins, described mixing time is 6 hours.
The method of claim 1, wherein step 4. described freezing temperature be-20 ℃, the described freezing time is 1 hour.
The method of claim 1, wherein step 7. the normal concentration of described C60 for utilizing Mg (ClO
4)
2As coagulant, do not containing under the surfactant condition, the C60 concentration of mensuration is characterized in that, specifically may further comprise the steps:
A, in the nC60 water slurry, add Mg (ClO
4)
2Solution takes off surely, described Mg (ClO
4)
2The concentration of solution is 100mmol/L;
B, with the C60 in the described water slurry that takes off after steady of toluene extraction step a;
C, the described water slurry of whipping step b;
Water slurry after d, the described stirring of freezing step c;
E, with the absorbance of ultraviolet-visible pectrophotometer at the described water slurry upper toluene solution after freezing of determination step d under the 336nm wavelength;
F, absorbance that step e is recorded are according to the C60 concentration in the typical curve calculation sample, and described typical curve is to set up according to the relational expression of C60 concentration and solution absorbance in the toluene.
6. method as claimed in claim 5, wherein, the described nC60 water slurry of step a and step b, described Mg (ClO
4)
2The volume ratio of solution, described toluene is 2: 1: 2.
7. method as claimed in claim 5, wherein, the described stir speed (S.S.) of step c is 1750 rev/mins, described mixing time is 6 hours.
8. method as claimed in claim 5, wherein, the described freezing temperature of steps d is-20 ℃, the described freezing time is 1 hour.
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| CN106680230A (en) * | 2017-01-06 | 2017-05-17 | 中国科学院化学研究所 | Method for measuring content of C60 or C70 in fullerene oil |
| CN109030393A (en) * | 2018-06-25 | 2018-12-18 | 天津大学 | Fullerene C in a kind of assessment improving sludge soil60The method of pollution |
| CN111707624A (en) * | 2020-06-15 | 2020-09-25 | 南开大学 | Qualitative and quantitative analysis method for environmental nano-colloids in river water |
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| CN103712937A (en) * | 2013-12-17 | 2014-04-09 | 南京信息工程大学 | Method for determining concentration of stable dispersion water solution C60 |
| CN103712937B (en) * | 2013-12-17 | 2017-05-17 | 南京信息工程大学 | Method for determining concentration of stable dispersion water solution C60 |
| CN103743690A (en) * | 2014-01-20 | 2014-04-23 | 中国科学院高能物理研究所 | Quantitative fullerene analysis method |
| CN103743690B (en) * | 2014-01-20 | 2016-08-17 | 中国科学院高能物理研究所 | A kind of quantitative analysis method of fullerene |
| CN106680230A (en) * | 2017-01-06 | 2017-05-17 | 中国科学院化学研究所 | Method for measuring content of C60 or C70 in fullerene oil |
| CN106680230B (en) * | 2017-01-06 | 2019-10-22 | 北京福纳康生物技术有限公司 | The content assaying method of C60 or C70 during a kind of fullerene is oily |
| CN109030393A (en) * | 2018-06-25 | 2018-12-18 | 天津大学 | Fullerene C in a kind of assessment improving sludge soil60The method of pollution |
| CN111707624A (en) * | 2020-06-15 | 2020-09-25 | 南开大学 | Qualitative and quantitative analysis method for environmental nano-colloids in river water |
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