CN108037046A - A kind of method of nano-scale particle size distribution in separation detection sewage - Google Patents
A kind of method of nano-scale particle size distribution in separation detection sewage Download PDFInfo
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- CN108037046A CN108037046A CN201711437596.1A CN201711437596A CN108037046A CN 108037046 A CN108037046 A CN 108037046A CN 201711437596 A CN201711437596 A CN 201711437596A CN 108037046 A CN108037046 A CN 108037046A
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- sewage
- size distribution
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- asymmetric field
- field flow
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
- G01N15/0205—Investigating particle size or size distribution by optical means, e.g. by light scattering, diffraction, holography or imaging
- G01N15/0211—Investigating a scatter or diffraction pattern
Abstract
The invention discloses a kind of method of nano-scale particle size distribution in separation detection sewage, comprise the following steps:Step 1, sewage to be measured are through cellulose mixture membrane filtration with except the suspended matter in decontaminated water;After step 2, sewage carry out ultrafiltration, concentration, cellulose mixture film secondary filter obtains sewage sample to be measured;Step 3, carry out asymmetric field flow shape by sewage sample to be measured and elute;Step 4, using laser light scattering instrument carry out droplet measurement to the mobile phase that elutes, analyzes the nano particle size distribution of sewage to be measured.The method of nano-scale particle size distribution in separation detection sewage of the present invention, improve the particle diameter of nano particle and number concentration accuracy in detection in sewage, the particle diameter and the relation of amounts of particles concentration and the size distribution of nano particle of nano particle, make the result of size distribution more accurate in clear and intuitive reflection sample to be tested;Method is easy to operate, and separation condition is gentle, and separation detection is repeated and has good stability.
Description
Technical field
The present invention relates to nano-scale particle ruler in scantling distribution technique field, more particularly to a kind of separation detection sewage
Spend the method for distribution.
Background technology
With developing rapidly for nano science, artificial synthesized nano material has been widely used for the various of life production
Field, including coating, dyestuff, sun-proof, semiconductor and agent photochemical catalyst etc..The mankind will inevitably receive in life and production
Rice grain brings water body into.Nano particle in natural water, it is likely that influenced into aquatile body, and by biological concentration
The health of the mankind.Nano particle can also be after the modes such as intestines and stomach, skin, respiratory tract, intravenous injection enter organism, can be by blood
Liquid circulation is carried to various body organs, and is deposited in Different Organs.With nanotechnology research progressively deeply, people by
Gradually start to recognize health of the nano-particle to the mankind that there are unforeseeable harm.Detect water body in nano particle object amount with
And distribution, it is major issue urgently to be resolved hurrily at present.Sewage treatment plant is the necessary approach of city water cycle, due to human lives
The nano particle for bringing water body into industrial production certainly will be by municipal sewage plant.Therefore, nano particle in sewage plant is analyzed
Research there are characteristic is of great significance.
Asymmetric field flow (Asymmetrical field flow, AFF) technology couples multiple angle laser light scattering detector
(MALS) it is a kind of new method efficiently separated with accurate characterization nano particles, can separates from several nanometers to tens microns
Particle.In the prior art, 201410509976.1 applications, which disclose, utilizes asymmetric field flow instrument separation detection C60 nanocrystals
The report of particle size distribution, it is detected as the size distribution of single nano particle.At present, due to nano particle species in sewage
Complexity, water body environment is various, and method for separating and detecting is generally using extraction, electrophoresis, three kinds of chromatography.Extraction is according to similar
The principle to mix, using solute, solubility is more than the property of solubility in former solvent in extractant, is handled with fluid extractant
Immiscible bi-component or Multi component therewith, realize the separated process of component, this method can be in nanometer by phase transfer
Organic solvent is mixed into grain thing, influences the accuracy of detection;Electrophoresis be under electric field action, charged particle towards with its electric charge
The phenomenon of opposite direction migration.Electrophoresis usually requires to add stabilizer, surface particles is carried certain electric charge, with increase
The dispersiveness and stability of nano material, stabilizer meeting partial adsorbates are on nanoparticles surface, so that particulate matter structure is influenced,
Further influence the accuracy of detection;Chromatography, as mobile phase, can produce one using organic solvent to nanoparticles structure
Determine the destruction of degree, the huge surface-active of nano particle can also interact with stationary phase, destroy the original physics of particulate matter
Chemical property, makes detection and analysis result error larger, and above-mentioned three kinds of methods can not all be realized and different-grain diameter rank is received
The distribution of rice grain impersonal language is detected.At present, separation detection is carried out also using asymmetric field stream to nano particle in sewage
Have no report.
Therefore, those skilled in the art is directed to developing nanoscale in a kind of detection sewage using asymmetric field flow separation
The method of particle size distribution, solves the above-mentioned prior art to insufficient existing for nano particle separation detection in sewage.
The content of the invention
In view of the drawbacks described above of the prior art, the technical problems to be solved by the invention are the prior arts to being received in sewage
Rice grain detection accuracy and result error are big, nano particle size distribution detection characterize data existing defects.
To achieve the above object, the present invention provides a kind of side of nano-scale particle size distribution in separation detection sewage
Method, comprises the following steps:
Step 1, sewage to be measured are through cellulose mixture membrane filtration except the suspended matter in decontaminated water, to obtain filter sewage;
Step 2, will the filter sewage that obtained in step 1 carry out ultrafiltration, concentration after, cellulose mixture film secondary filter must be treated
Survey sewage sample;
Step 3, the sewage sample to be measured for obtaining step 2 carry out asymmetric field flow shape and elute;
Step 4, the mobile phase eluted using laser light scattering instrument to step 3 carry out droplet measurement, analyze sewage to be measured
Nano particle size distribution.
Wherein, the aperture of the cellulose mixture film is 0.1~0.45 μm;
In the step 2, the ultrafiltration membrane that when ultrafiltration uses is 10KDa regenerated cellulose films;
In the step 3, when asymmetric field flow shape elutes, 1.5~2.5mL/min of level stream flow velocity;Cross-current flow velocity 1.5
~2.5mL/min;10~20min of elution time;Elute chamber and grow 20~30cm.
Further, in the step 1, the aperture of cellulose mixture film is 0.45 μm;
Further, in the step 2, the cellulose mixture membrane aperture of secondary filter is 0.1 μm;
Further, in the step 2, cycles of concentration is 50~100;
Further, in the step 3, when asymmetric field flow shape elutes, level stream flow velocity 2mL/min;
Further, in the step 3, when asymmetric field flow shape elutes, cross-current flow velocity 2mL/min;
Further, in the step 3, when asymmetric field flow shape elutes, 15~20min of elution time;
Further, in the step 3, when asymmetric field flow shape elutes, elution chamber grows 25~30cm;
Further, in the step 3, when asymmetric field flow shape elutes, using 5~30KDa regenerated cellulose film conducts
Seperation film.
In the better embodiment of the present invention, in the step 2, cycles of concentration 50;
In another better embodiment of the present invention, in the step 2, cycles of concentration 100;
In the better embodiment of the present invention, in the step 3, when asymmetric field flow shape elutes, elution time
15min;
In another better embodiment of the present invention, in the step 3, when asymmetric field flow shape elutes, elution time
20min;
In the better embodiment of the present invention, in the step 3, when asymmetric field flow shape elutes, elution chamber length
25cm;
In another better embodiment of the present invention, in the step 3, when asymmetric field flow shape elutes, chamber is eluted
Long 27.5cm;
In another better embodiment of the present invention, in the step 3, when asymmetric field flow shape elutes, chamber is eluted
Long 30cm;
In the better embodiment of the present invention, in the step 3, when asymmetric field flow shape elutes, regenerated using 5KDa
Cellulose membrane is as seperation film;
In another better embodiment of the present invention, in the step 3, when asymmetric field flow shape elutes, using 10KDa
Regenerated cellulose film is as seperation film;
In another better embodiment of the present invention, in the step 3, when asymmetric field flow shape elutes, using 30KDa
Regenerated cellulose film is as seperation film;
In the better embodiment of the present invention, in the step 3, when asymmetric field flow shape elutes, level stream flow velocity
2mL/min, cross-current flow velocity 2mL/min, elution chamber long 27.5cm, elution time 15min;
In the better embodiment of the present invention, in the step 3, when asymmetric field flow shape elutes, elution chamber is flat
Flat chamber, thickness are 350 μm;
In the better embodiment of the present invention, in the step 3, when asymmetric field flow shape elutes, sewage sample to be measured
Sample size be 100 μ L;
In the better embodiment of the present invention, in the step 3, the elution of asymmetric field flow shape be asymmetric field flow
Carried out in instrument;
In the better embodiment of the present invention, in the step 3, asymmetric field flow shape elution is in model AF4
Carried out in asymmetric field flow instrument;
In the better embodiment of the present invention, nano-scale particle size distribution method uses in the separation detection sewage
Asymmetric field flow instrument is carried out with multiple angle laser light scattering detector combination.
In the better embodiment of the present invention, nano-scale particle size distribution uses AF4- in the separation detection sewage
MALS combinations carry out.
Using above scheme, the method for nano-scale particle size distribution, has in separation detection sewage disclosed by the invention
Advantages below:
The method of nano-scale particle size distribution in separation detection sewage of the present invention, is eluted using asymmetric field flow shape, is led to
Optimization elution flow rate and elution time are crossed, the nano particle in sample to be tested is sufficiently separated in chamber is eluted, nano particle
Substantially according in the follow-up droplet measurement device of sequential flow from small to large, the particle diameter and number concentration of nano particle in sewage are improved
Accuracy in detection, clear and intuitive reflects the particle diameter of nano particle and the relation and nanometer of amounts of particles concentration in sample to be tested
The size distribution of grain, makes the result of size distribution more accurate;
The method of nano-scale particle size distribution in separation detection sewage of the present invention, sewage sample to be tested need not pre-process,
Can direct injected;Without using stationary phase, therefore shearing force is not present;Numerous mobile phase conditions can be used, therefore can be with hanging
Lock out operation is carried out under the identical solvent background of float formation condition;Allow to be up to 10mM using deionized water or ionic strength
Buffer solution, without separately plus other mobile phase modifying agents;Easy to operate, separation condition is gentle, and high resolution, safety and environmental protection, has
Promoted and applied beneficial to realizing;
In conclusion in separation detection sewage of the present invention nano-scale particle size distribution method, improve in sewage and receive
The particle diameter and number concentration accuracy in detection of rice grain, the clear and intuitive particle diameter and particle that reflect nano particle in sample to be tested
The relation of number concentration and the size distribution of nano particle, make the result of size distribution more accurate;Method is easy to operate, separation
Mild condition, separation detection is repeated and has good stability.
Below with reference to design of the drawings and examples to the present invention, concrete technical scheme and generation technique effect make into
One step illustrates, to be fully understood from the purpose of the present invention, feature and effect.
Brief description of the drawings
Fig. 1 is the detection spectrogram of AF4-MALS in nano-scale particle size distribution method in 1 separation detection sewage of embodiment;
Fig. 2 is concentrations of nanoparticles and scale in nano-scale particle size distribution method in 1 separation detection sewage of embodiment
Graph of a relation;
Fig. 3 is each other accumulation of grain-size grade in nano-scale particle size distribution method in 1 separation detection sewage of embodiment
Number concentration compare curve map;
Fig. 4 is AF4- in the nanoparticles size distribution method in 5 separation detection sewage plant secondary clarifier effluent of embodiment
The detection spectrogram of MALS;
Fig. 5 is AF4-MALS in the nanoparticles size distribution method in 6 separation detection sewage effluents of embodiment
Detect spectrogram.
Embodiment
Multiple preferred embodiments of the invention introduced below, make its technology contents more clear and readily appreciate.The present invention
It can be emerged from by many various forms of embodiments, these embodiments are exemplary description, protection model of the invention
Enclose the embodiment for being not limited only to mention in text.
If there is the experimental method that actual conditions is not specified, usually according to normal condition, such as instructions book or handbook
Implemented.
Embodiment 1
Nano-scale particle size distribution, concrete operations are as follows in separation detection sewage:
Step 1, sewage to be measured are dirty except the suspended matter in decontaminated water, to obtain filtering through 0.45 μm of cellulose mixture membrane filtration
Water;
Step 2, using 10KDa regenerated cellulose films as ultrafiltration membrane, by the filter sewage obtained in step 1 through 8400 types
Stirring-type ultrafiltration cup concentrates 100 times;
Step 3, by the concentrate that step 2 obtains obtain sewage sample to be measured through 0.1 μm of cellulose mixture film secondary filter;
Step 4, using 10KDa regenerated cellulose films as seperation film, the 100 μ L of sewage sample to be measured that step 3 is obtained
Sample introduction carries out asymmetric field flow shape elution, the asymmetric field flow instrument of AF4 elutes the thickness of flat chamber to the asymmetric field flow instrument of AF4
For 350 μm, length 27.5cm, level stream flow velocity 2mL/min when eluting separation detection, cross-current flow velocity 2mL/min, elution time
15min;
Step 5, the mobile phase eluted using MALS to the asymmetric field flow instrument of AF4 in step 4 carry out droplet measurement, analysis
The nano particle size distribution of sewage to be measured.
As shown in Figure 1, the test map of the AF4-MALS for the present embodiment;
In figure, ordinate represents particle diameter, and abscissa represents the time;
1 is detection sample UV signal response curve, and 1 correspondence ordinate is signal strength, and intensity is bigger, represents the moment
Solution concentration into DAD detectors is bigger;
3 be detection sample light scattering signal response curve, and 3 correspondence ordinates are signal strengths, and signal strength is bigger, represents
The solution light scattering ability that the moment enters MALS detectors is bigger;
2 be the particle diameter situation for entering MALS detectors with the time;
Fig. 1 shows since the centrifugation of asymmetric field flow, nano particle are flowed into substantially according to order from small to large
MALS detectors, have appropriate centrifugation.
The data of above-mentioned Fig. 1 are subjected to software analysis and obtain the graph of a relation (Fig. 2) of concentrations of nanoparticles and scale, and it is each
The number concentration of the other accumulation of grain-size grade is than curve map (Fig. 3);
As shown in Fig. 2, in the graph of a relation of concentrations of nanoparticles and scale, abscissa represents nano particle geometric diameter, indulges
Coordinate representation nano particle number concentration (numbers of particles of unit volume), clear and intuitive obtains nano particle in sample to be tested
Particle diameter and amounts of particles concentration relation, the preferable size distribution for reflecting nano particle.
As shown in figure 3, the number concentration of each other accumulation of grain-size grade is than in curve map, abscissa represents that nano particle is several
What diameter, ordinate represent cumulative amount concentration ratio, and Fig. 3 intuitively obtains the particle diameter of nano particle and accumulation in middle sample to be tested
The relation of grain number concentration, the size distribution of nano particle is reflected from the angle of accumulation;For example, in the abscissa 75nm of Fig. 3
Place, cumulative concentration ratio are 0.2, i.e., particulate matter quantity of the nano particle diameter less than 75nm accounts for total particle in explanation detection sample
Several 20%.
Embodiment 2
Nano-scale particle size distribution, concrete operations are as follows in separation detection sewage:
Step 1, sewage to be measured are dirty except the suspended matter in decontaminated water, to obtain filtering through 0.4 μm of cellulose mixture membrane filtration
Water;
Step 2, using 10KDa regenerated cellulose films, by the filter sewage obtained in step 1 through 8400 type stirring-type ultrafiltration
50 times of cup concentration;
Step 3, by the concentrate that step 2 obtains obtain sewage sample to be measured through 0.15 μm of cellulose mixture film secondary filter;
Step 4, using 5KDa regenerated cellulose films as seperation film, by the 100 μ L of sewage sample to be measured that step 3 obtains into
Sample carries out asymmetric field flow shape elution, the thickness that the asymmetric field flow instrument of AF4 elutes flat chamber is to the asymmetric field flow instrument of AF4
350 μm, length 30cm, level stream flow velocity 1.5mL/min when eluting separation detection, cross-current flow velocity 1.5mL/min, elution time
20min;
Step 5, the mobile phase eluted using MALS to the asymmetric field flow instrument of AF4 in step 4 carry out droplet measurement, analysis
The nano particle size distribution of sewage to be measured.
Embodiment 3
Nano-scale particle size distribution, concrete operations are as follows in separation detection sewage:
Step 1, sewage to be measured are dirty except the suspended matter in decontaminated water, to obtain filtering through 0.45 μm of cellulose mixture membrane filtration
Water;
Step 2, using 10KDa regenerated cellulose films, by the filter sewage obtained in step 1 through 8400 type stirring-type ultrafiltration
100 times of cup concentration;
Step 3, by the concentrate that step 2 obtains obtain sewage sample to be measured through 0.1 μm of cellulose mixture film secondary filter;
Step 4, using 30KDa regenerated cellulose films as seperation film, the 100 μ L of sewage sample to be measured that step 3 is obtained
Sample introduction carries out asymmetric field flow shape elution, the asymmetric field flow instrument of AF4 elutes the thickness of flat chamber to the asymmetric field flow instrument of AF4
For 350 μm, length 25cm, level stream flow velocity 2.5mL/min when eluting separation detection, cross-current flow velocity 2.5mL/min, during elution
Between 18min;
Step 5, the mobile phase eluted using MALS to the asymmetric field flow instrument of AF4 in step 4 carry out droplet measurement, analysis
The nano particle size distribution of sewage to be measured.
Embodiment 4
Nano-scale particle size distribution, concrete operations are as follows in separation detection sewage:
Step 1, sewage to be measured are dirty except the suspended matter in decontaminated water, to obtain filtering through 0.4 μm of cellulose mixture membrane filtration
Water;
Step 2, using 10KDa regenerated cellulose films, by the filter sewage obtained in step 1 through 8400 type stirring-type ultrafiltration
80 times of cup concentration;
Step 3, by the concentrate that step 2 obtains obtain sewage sample to be measured through 0.15 μm of cellulose mixture film secondary filter;
Step 4, using 20KDa regenerated cellulose films as seperation film, the 100 μ L of sewage sample to be measured that step 3 is obtained
Sample introduction carries out asymmetric field flow shape elution, the asymmetric field flow instrument of AF4 elutes the thickness of flat chamber to the asymmetric field flow instrument of AF4
For 350 μm, length 27.5cm, level stream flow velocity 2mL/min when eluting separation detection, cross-current flow velocity 1.5mL/min, during elution
Between 10min;
Step 5, the mobile phase eluted using MALS to the asymmetric field flow instrument of AF4 in step 4 carry out droplet measurement, analysis
The nano particle size distribution of sewage to be measured.
Contrast after testing, the method for separating and detecting of embodiment 2~4 has the separation detection effect similar with embodiment 1.
Embodiment 5
Nanoparticles size distribution in separation detection sewage plant secondary clarifier effluent
The nanoparticles in certain sewage plant secondary clarifier effluent are divided using the operating method similar with embodiment 1
From detection, the results are shown in Figure 4, similar to the testing result of embodiment 1, the nanoparticles grain in sewage plant secondary clarifier effluent
Son flows into MALS detectors (in Fig. 4 shown in 2) substantially according to order from small to large, can carry out subsequent software point according to this data
The size distribution of analysis detection sample nano particle.
Embodiment 6
Nanoparticles size distribution in separation detection sewage effluents
Using carrying out separating inspection to the nanoparticles in certain sewage effluents with the similar operating method of embodiment 1
Survey, the results are shown in Figure 5, similar to the testing result of embodiment 1, the nanoparticles particle in sewage effluents substantially according to
Order from small to large flows into MALS detectors (in Fig. 5 shown in 2), and subsequent software analysis detection sample can be carried out according to this data
The size distribution of nano particle.
In conclusion in 1~6 separation detection sewage of the embodiment of the present invention nano-scale particle size distribution method, sewage
In nano particle substantially according to from small to large order flow into MALS detectors, there is appropriate centrifugation;Can be after
Continuous nano particle diameter detection and software analysis obtain the graph of a relation and nano particle of concentrations of nanoparticles and scale in sewage
In each other accumulation of grain-size grade number concentration than curve map, clear and intuitive obtains the particle diameter of nano particle in sample to be tested
With the relation of amounts of particles concentration, the preferable size distribution for reflecting nano particle in sewage;Technical method separation detection repeats
Property and have good stability.
In the separation detection sewage of other embodiment of the present invention the method for nano-scale particle size distribution have with it is above-mentioned
Similar beneficial effect.
Preferred embodiment of the invention described in detail above.It should be appreciated that the ordinary skill of this area is without wound
The property made work can conceive according to the present invention makes many modifications and variations.Therefore, all technician in the art
Pass through logic analysis, reasoning or the available technology of limited experiment on the basis of existing technology under this invention's idea
Scheme, all should be in the protection domain being defined in the patent claims.
Claims (10)
1. a kind of method of nano-scale particle size distribution in separation detection sewage, it is characterised in that comprise the following steps:
Step 1, sewage to be measured are through cellulose mixture membrane filtration except the suspended matter in decontaminated water, to obtain filter sewage;
Step 2, will the filter sewage that obtained in step 1 carry out ultrafiltration, concentration after, cellulose mixture film secondary filter obtains dirt to be measured
Water sample;
Step 3, the sewage sample to be measured for obtaining step 2 carry out asymmetric field flow shape and elute;
Step 4, the mobile phase eluted using laser light scattering instrument to step 3 carry out droplet measurement, analyze the nanometer of sewage to be measured
Particle size distribution.
2. method as claimed in claim 1, it is characterised in that
The aperture of the cellulose mixture film is 0.1~0.45 μm;
In the step 2, the ultrafiltration membrane that when ultrafiltration uses is 10KDa regenerated cellulose films;
In the step 3, when asymmetric field flow shape elutes, 1.5~2.5mL/min of level stream flow velocity;Cross-current flow velocity 1.5~
2.5mL/min;10~20min of elution time;Elute chamber and grow 20~30cm.
3. method as claimed in claim 1, it is characterised in that
In the step 1, the aperture of cellulose mixture film is 0.45 μm;
In the step 2, cycles of concentration is 50~100, and the cellulose mixture membrane aperture of secondary filter is 0.1 μm.
4. method as claimed in claim 2, it is characterised in that in the step 3, when asymmetric field flow shape elutes, level stream stream
Fast 2mL/min.
5. method as claimed in claim 2, it is characterised in that in the step 3, when asymmetric field flow shape elutes, cross-current stream
Fast 2mL/min.
6. method as claimed in claim 2, it is characterised in that in the step 3, when asymmetric field flow shape elutes, elution time
15~20min.
7. method as claimed in claim 2, it is characterised in that in the step 3, when asymmetric field flow shape elutes, elute chamber
Long 25~30cm.
8. method as claimed in claim 2, it is characterised in that in the step 3, during the elution of asymmetric field flow shape, using 5~
30KDa regenerated cellulose films are as seperation film.
9. method as claimed in claim 2, it is characterised in that in the step 3, asymmetric field flow shape elution is in asymmetric field
Carried out in stream instrument.
10. method as claimed in claim 1, it is characterised in that nano-scale particle size distribution side in the separation detection sewage
Method is carried out using asymmetric field flow instrument and multiple angle laser light scattering detector combination.
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CN102016543A (en) * | 2008-04-25 | 2011-04-13 | 新日本制铁株式会社 | Method of determining particle size distribution of fine particles contained in metallic material |
CN104483245A (en) * | 2014-09-28 | 2015-04-01 | 上海交通大学 | Method for separating C60 nanocrystalline particle size distribution by utilization of asymmetrical field flow meter |
CN104777081A (en) * | 2015-04-01 | 2015-07-15 | 上海交通大学 | Nano particle separation and detection method |
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Title |
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