CN105115929B - A kind of method that critical micelle concentration of surfactant is determined based on terahertz time-domain spectroscopic technology - Google Patents
A kind of method that critical micelle concentration of surfactant is determined based on terahertz time-domain spectroscopic technology Download PDFInfo
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Abstract
The present invention relates to the method that one kind determines critical micelle concentration of surfactant (Critical Micelle Concentration, CMC) based on terahertz time-domain spectroscopic technology, comprise the following steps：S1：Prepare the sample cell for being adapted to tera-hertz spectra detection；S2：Prepare across four orders of magnitude：The surfactant solution sample of 0.1 to 100mM various concentrations；S3：Measure and obtain the terahertz time-domain spectroscopy of testing sample solution；The concentration and Terahertz absorption coefficient or the relation spectrum of refractive index for obtaining sample are calculated using formula, determines that the corresponding surfactant samples concentration in turning point occurs in image；S4：It is determined that sample turnover concentration or so select and prepare a series of aqueous surfactant solution sample of interval smaller concentration；S5：The terahertz time-domain spectroscopy of testing sample solution is measured and obtained again；S6：The concentration and Terahertz absorption coefficient or the relation spectrum of refractive index for obtaining testing sample solution are calculated again, and the CMC of surfactant is determined by image information.This method has the advantages that quick, unmarked, simple to operate, applied widely, reproducible, result accuracy is high.
Description
Technical field
The invention belongs to Surfactants Analysis technical field, it is related to one kind and table is determined based on terahertz time-domain spectroscopic technology
The method of face activating agent critical micelle concentration (Critical Micelle Concentration, CMC).
Background technology
Surfactant has multifrequency nature, such as wetting, emulsification, foaming, dissolving, scattered, washing, corrosion-resistant, antistatic
Deng being widely used in multiple fields, such as pharmaceutical chemistry, synthesis chemistry, material science, biology.Under certain concentration,
That is CMC, surfactant initially forms thermodynamically stable micella, meanwhile, significant change occurs for various properties.Therefore, CMC
Measure have very important significance in actual applications, be physical chemistry and analytical chemistry research a focus.At present
The CMC assay methods of development are surfactant solution optical turbidity, surface tension, viscosity, diffusion when reaching CMC using concentration
The mutation of the physical quantitys such as coefficient, electrical conductivity determines CMC value.
THz wave refers to electromagnetic wave of the frequency in the range of 0.1-10THz, between microwave and it is infrared between, with it is high thoroughly
Property, low energy, instantaneity, acuteness, high s/n ratio the features such as, these features cause Terahertz non-destructive testing technology biology cure
Many methods such as, biochemistry, chemical industry have critically important application.THz wave covering dielectric nanosecond the fortune to psec yardstick
Dynamic, this exactly combines the time scale of water vibration, diffusion and solvent molecule low-frequency vibration, therefore THz spectral techniques are adapted to detection
The interaction of solution reclaimed water and solute molecule.Due to surfactant monomer and micella with water molecules state in the presence of poor
It is different, cause surfactant solution to absorb THz wave and transfer.Terahertz time-domain spectroscopy skill is not used also so far
Art detects the Patents and document report of CMC of surfactant.
The content of the invention
In view of this, surfactant is determined based on terahertz time-domain spectroscopic technology it is an object of the invention to provide one kind
The method of critical micelle concentration (Critical Micelle Concentration, CMC), this method have it is quick, unmarked,
It is simple to operate, applied widely, reproducible, the advantages of result accuracy is high.
To reach above-mentioned purpose, the present invention provides following technical scheme：
A kind of method that critical micelle concentration of surfactant is determined based on terahertz time-domain spectroscopic technology, including following step
Suddenly：
S1：Prepare the sample cell for being adapted to tera-hertz spectra detection；
S2：Prepare across four orders of magnitude：The surfactant solution sample of 0.1 to 100mM various concentrations；
S3：Measure and obtain the terahertz time-domain spectroscopy of testing sample solution；The concentration for obtaining sample is calculated using formula
With Terahertz absorption coefficient or the relation spectrum of refractive index, determine that the corresponding surfactant samples in generation turning point are dense in image
Degree；
S4：It is determined that sample turnover concentration or so select and prepare a series of surfactant of interval smaller concentration
Aqueous sample；
S5：The terahertz time-domain spectroscopy of testing sample solution is measured and obtained again；
S6：The concentration and Terahertz absorption coefficient or the relation spectrum of refractive index for obtaining testing sample solution are calculated again,
The CMC of surfactant is determined by image information.
Further, in step sl, the sample cell of the preparation is divided into：Two panels polythene strip is with striking out square-outside and round-inside type
Hollow PET double faced adhesive tapes, construction method is to utilize adhered by double sided plaster two panels polythene strip one hollow liquid sample pool of formation, tool
Body step is injected fluid sample, another polythene strip covered, liquid first to bond double faced adhesive tape with wherein a piece of polythene strip
Body thickness determines that 100um, 50um may be selected in the thickness of PET double faced adhesive tapes according to PET double faced adhesive tapes thickness.
Further, in step s 2, the solution example to be measured be by surfactant to be detected and solvent by than
The surfactant solution for the concentration known that example is mixedly configured into；The concentration of the testing sample of detection is from 0.1 to 100mM for the first time
It is incremented by successively, 3-4 different concentration are taken in each magnitude；The concentration of the testing sample of second of detection is detected according to first time
As a result determine.
Further, in step s3, the liquid sample pool by empty liquid sample pool and equipped with sample is sequentially placed into transmission
In formula terahertz time-domain spectroscopy device, the time-domain spectroscopy letter of the liquid sample pool of sky and the liquid cell equipped with sample is obtained respectively
Number；Using the former signal as reference signal, the latter carries out Fourier transformation as sample signal and obtains corresponding Terahertz respectively
The information such as frequency-domain waveform, amplitude；In order to reduce experimental error, with reference to the measurement with sample signal in triplicate；
The Terahertz absorption coefficient of surfactant solution or the calculating of refractive index are all based on above with reference to signal and sample
The information acquisitions such as corresponding Terahertz frequency-domain waveform, the amplitude that the Fourier transformation of product signal is obtained, surfactant solution sample
Refractive index n (f) calculation formula are as follows：
Wherein, IrefAnd IsThe transmission energy of the reference signal that can be captured and sample signal is represented respectively,Respectively IsAnd IrefThe phase information obtained after Fourier transformation is carried out, c represents the light velocity, and d represents Terahertz
Penetrate the thickness of sample；
Extinction coefficient κ (f) calculation formula is as follows：
Wherein ρ (f) is IsAnd IrefThe amplitude ratio of Fourier transformation,
The calculation formula of surfactant solution sample absorption coefficient is as follows：
Further, Terahertz frequency range is 0.3-1.7THz.
The beneficial effects of the present invention are：Compared with prior art, the present invention utilizes terahertz time-domain spectroscopic technology to table
The CMC of face activating agent is detected that this method has quick, unmarked, simple to operate, applied widely, reproducible, result
The advantages of accuracy is high.
Brief description of the drawings
In order that the purpose of the present invention, technical scheme and beneficial effect are clearer, the present invention provides drawings described below and carried out
Explanation：
Fig. 1 is sample pool structure schematic diagram；
Fig. 2 is the glycol ether (C of single dodecyl nine of various concentrations in embodiment 112E9) aqueous solution wave in time domain；
Fig. 3 is the C of various concentrations in embodiment 112E9The absorption coefficient figure of the aqueous solution；
Fig. 4 is the C of various concentrations in embodiment 112E9The index of refraction diagram of the aqueous solution；
Fig. 5 is the C of various concentrations in embodiment 212E9PBS solution absorption coefficient figure；
Fig. 6 is the C of various concentrations in embodiment 312E9HCl solution absorption coefficient figure；
Fig. 7 is the absorption coefficient figure of lauryl sodium sulfate (SDS) aqueous solution of various concentrations in embodiment 4；
Fig. 8 is the absorption coefficient figure of TTAB (TTAB) aqueous solution of various concentrations in embodiment 5；
Fig. 9 is the schematic flow sheet of the method for the invention.
Embodiment
The change of the Terahertz absorption coefficient of surfactant solution sample can reflect surfactant molecule in water
State in which.When surfactant molecule in the solution does not form micella, because solute concentration is relatively low, according to binary model
Terahertz absorption coefficient is calculated, the absorption coefficient of solution contributes two parts by the absorption contribution and the absorption of solvent of surfactant
Constitute, because the absorption coefficient of surfactant is less than the absorption coefficient of aqueous solvent, so with the increase of solute, the contribution of water
Proportion is reduced, and the absorption coefficient of solution declines；After micella is formed, according to ternary model, micella outer layer can form combination
Water layer, has higher Terahertz absorption coefficient, more solutes can form more micellas, bring more with reference to water than Free water
Many combination water so that the absorption coefficient of solution rises.
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail.
Fig. 9 is the schematic flow sheet of the method for the invention, as illustrated, method of the present invention includes following step
Suddenly：
S1：The sample cell for being adapted to tera-hertz spectra detection is prepared, as shown in Figure 1；
S2：Prepare across four orders of magnitude：The surfactant solution sample of 0.1 to 100mM various concentrations；
S3：Measure and obtain the terahertz time-domain spectroscopy of testing sample solution；The concentration for obtaining sample is calculated using formula
With Terahertz absorption coefficient or the relation spectrum of refractive index, determine that the corresponding surfactant samples in generation turning point are dense in image
Degree；
S4：It is determined that sample turnover concentration or so select and prepare a series of surfactant of interval smaller concentration
Aqueous sample；
S5：The terahertz time-domain spectroscopy of testing sample solution is measured and obtained again；
S6：The concentration and Terahertz absorption coefficient or the relation spectrum of refractive index for obtaining testing sample solution are calculated again,
The CMC of surfactant is determined by image information.
In step sl, the sample cell of preparation is divided into：Two panels polythene strip is two-sided with striking out the hollow PET of square-outside and round-inside type
Glue, construction method is, using adhered by double sided plaster two panels polythene strip one hollow liquid sample pool of formation, to concretely comprise the following steps elder generation
Double faced adhesive tape is bonded with wherein a piece of polythene strip, fluid sample is injected, another polythene strip is covered, liquid thickness according to
PET double faced adhesive tapes thickness determines that 100um, 50um may be selected in the thickness of PET double faced adhesive tapes.
In step s 2, solution example to be measured is mixedly configured into proportion with solvent by surfactant to be detected
Concentration known surfactant solution；The concentration of the testing sample of detection is incremented by successively from 0.1 to 100mM for the first time, often
3-4 different concentration are taken in individual magnitude；The concentration of the testing sample of second of detection is determined according to first time testing result.
In step s3, the liquid sample pool by empty liquid sample pool and equipped with sample is sequentially placed into transmission-type Terahertz
In time-domain spectroscopy device, the time-domain spectroscopy signal of the liquid sample pool of sky and the liquid cell equipped with sample is obtained respectively；With the former
Signal as reference signal, the latter carried out respectively as sample signal Fourier transformation obtain corresponding Terahertz frequency-domain waveform,
The information such as amplitude；In order to reduce experimental error, with reference to the measurement with sample signal in triplicate；
The Terahertz absorption coefficient of surfactant solution or the calculating of refractive index are all based on above with reference to signal and sample
The information acquisitions such as corresponding Terahertz frequency-domain waveform, the amplitude that the Fourier transformation of product signal is obtained, surfactant solution sample
Refractive index n (f) calculation formula are as follows：
Wherein, IrefAnd IsThe transmission energy of the reference signal that can be captured and sample signal is represented respectively,Respectively IsAnd IrefThe phase information obtained after Fourier transformation is carried out, c represents the light velocity, and d represents Terahertz
Penetrate the thickness of sample；
Extinction coefficient κ (f) calculation formula is as follows：
Wherein ρ (f) is IsAnd IrefThe amplitude ratio of Fourier transformation,
The calculation formula of surfactant solution sample absorption coefficient is as follows：
Terahertz frequency range is 0.3-1.7THz.
Embodiment 1：
Using terahertz time-domain spectroscopic technology to nonionic surfactant C12E9The method that solution C MC is detected, its
Comprise the following steps：
1st, the sample cell for being adapted to Terahertz detection is built：Utilize the two-sided glue sticking two panels transparent plastic sheets of PET, circular cavity
Room contains C12E9The volume of solution is about 17.7 μ l；
2nd, C is prepared12E9Aqueous sample：By C12E9Mixed in proportion with deionized water, be configured to the surface of concentration known
Activator solution sample mother liquor, in proportion dilution obtains a series of concentration range 0.1mM to 100mM solution examples to be measured；
3rd, the detection of solution example and signal transacting：Transmitted light path is used with empty sample using terahertz time-domain spectroscopy device
Pond is reference, and solution example is carried out to detect each sample duplicate measurements three times.Time domain beamformer progress Fourier transformation is obtained
To its amplitude collection of illustrative plates, phase collection of illustrative plates etc. calculates absorption coefficient, refractive index according to formula, utilizes the corresponding frequency model of various concentrations
The result mapping in 0.3-1.7THz is enclosed, turnover concentration is obtained；
4th, C is prepared according to turnover concentration again12E9Solution example：Turnover concentration obtained in step 3 or so sets at least 7
Individual concentration point, solution example to be measured is configured with step 2 identical method；
5th, C is determined12E9CMC：It is identical with step 3, draw surfactant concentration and absorption coefficient or the pass of refractive index
System's figure, determines that turnover (absorption coefficient and concentration relationship figure) occurs for curve in image or intersection (refractive index and concentration relationship figure) is right
The concentration answered, as CMC.Fig. 2 is the C of various concentrations in embodiment 112E9The wave in time domain of the aqueous solution；Fig. 3 is in embodiment 1
The C of various concentrations12E9The absorption coefficient figure of the aqueous solution；Fig. 4 is the C of various concentrations in embodiment 112E9The refractive index of the aqueous solution
Figure.
Embodiment 2：
The present embodiment provides one kind using terahertz time-domain spectroscopic technology to C under hypersaline environment12E9The side of solution C MC detections
Method, operating procedure is identical with embodiment 1, and simply testing sample is ionic surfactant C12E9PBS solution.Fig. 5
For the C of various concentrations in embodiment 212E9Phosphate buffer (PBS) absorption coefficient figure.
Embodiment 3：
The present embodiment provides one kind using terahertz time-domain spectroscopic technology to C under sour environment12E9The side of solution C MC detections
Method, operating procedure is identical with embodiment 1, and simply testing sample is ionic surfactant C12E9Acid solution.Fig. 6 is
The C of various concentrations in embodiment 312E9Hydrochloric acid solution absorption coefficient figure.
Embodiment 4：
The present embodiment provides one kind using terahertz time-domain spectroscopic technology to anionic surfactant SDS solution Cs MC
The method of detection, operating procedure is identical with embodiment 1, and simply testing sample is ionic surfactant SDS.Fig. 7 is
The absorption coefficient figure of the SDS aqueous solution of various concentrations in embodiment 4.
Embodiment 5：
The present embodiment is provided one kind and cationic surfactant TTAB solution Cs MC is examined using terahertz time-domain spectroscopic technology
The method of survey, operating procedure is identical with embodiment 1, and simply testing sample is ionic surfactant TTAB.Fig. 8 is real
Apply the absorption coefficient figure of the TTAB aqueous solution of various concentrations in example 5.
Finally illustrate, preferred embodiment above is merely illustrative of the technical solution of the present invention and unrestricted, although logical
Cross above preferred embodiment the present invention is described in detail, it is to be understood by those skilled in the art that can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (4)
1. a kind of method that critical micelle concentration of surfactant is determined based on terahertz time-domain spectroscopic technology, it is characterised in that：
Comprise the following steps：
S1：Prepare the sample cell for being adapted to tera-hertz spectra detection；
S2：Prepare across four orders of magnitude：The surfactant solution sample of 0.1 to 100mM various concentrations；
S3：Measure and obtain the terahertz time-domain spectroscopy of testing sample solution；Using formula calculate obtain sample concentration with too
The relation spectrum of hertz absorption coefficient or refractive index, determines that the corresponding surfactant samples concentration in turning point occurs in image；
S4：It is determined that sample turnover concentration or so select and prepare a series of interval smaller concentration surfactant it is water-soluble
Liquid sample；
S5：The terahertz time-domain spectroscopy of testing sample solution is measured and obtained again；
S6：The concentration and Terahertz absorption coefficient or the relation spectrum of refractive index for obtaining testing sample solution are calculated again, are passed through
Image information determines the critical micelle concentration of surfactant；
In the step S3, when empty liquid sample pool and the liquid sample pool equipped with sample are sequentially placed into transmission-type Terahertz
In the spectral device of domain, the time-domain spectroscopy signal of the liquid sample pool of sky and the liquid cell equipped with sample is obtained respectively；Believed with the former
Number as reference signal, the latter carries out Fourier transformation as sample signal and obtains corresponding Terahertz frequency-domain waveform, shakes respectively
The information such as width；In order to reduce experimental error, with reference to the measurement with sample signal in triplicate, the terahertz of surfactant solution
The hereby calculating of absorption coefficient or refractive index be all based on above with reference to the Fourier transformation of signal and sample signal obtain it is corresponding
The information acquisitions such as Terahertz frequency-domain waveform, amplitude, surfactant solution sample refractive index n (f) calculation formula are as follows：
Wherein, IrefAnd IsThe transmission energy of the reference signal that can be captured and sample signal is represented respectively,Point
Wei not IsAnd IrefThe phase information obtained after Fourier transformation is carried out, c represents the light velocity, and d represents the thickness that Terahertz penetrates sample
Degree, f represents frequency；
Extinction coefficient κ (f) calculation formula is as follows：
<mrow>
<mi>&kappa;</mi>
<mrow>
<mo>(</mo>
<mi>f</mi>
<mo>)</mo>
</mrow>
<mo>=</mo>
<mi>ln</mi>
<mi>&lsqb;</mi>
<mfrac>
<mrow>
<mi>4</mi>
<mi>n</mi>
<mrow>
<mo>(</mo>
<mi>f</mi>
<mo>)</mo>
</mrow>
</mrow>
<mrow>
<mi>&rho;</mi>
<mrow>
<mo>(</mo>
<mi>f</mi>
<mo>)</mo>
</mrow>
<msup>
<mrow>
<mo>&lsqb;</mo>
<mi>n</mi>
<mrow>
<mo>(</mo>
<mi>f</mi>
<mo>)</mo>
</mrow>
<mo>+</mo>
<mn>1</mn>
<mo>&rsqb;</mo>
</mrow>
<mn>2</mn>
</msup>
</mrow>
</mfrac>
<mo>&rsqb;</mo>
<mfrac>
<mi>c</mi>
<mrow>
<mn>2</mn>
<mi>&pi;</mi>
<mi>f</mi>
<mi>d</mi>
</mrow>
</mfrac>
</mrow>
Wherein ρ (f) is IsAnd IrefThe amplitude ratio of Fourier transformation, n (f) represents refractive index, and f represents frequency；
The calculation formula of surfactant solution sample absorption coefficient is as follows：
<mrow>
<mi>&alpha;</mi>
<mrow>
<mo>(</mo>
<mi>f</mi>
<mo>)</mo>
</mrow>
<mo>=</mo>
<mfrac>
<mrow>
<mn>4</mn>
<mi>&pi;</mi>
<mi>f</mi>
<mi>&kappa;</mi>
<mrow>
<mo>(</mo>
<mi>f</mi>
<mo>)</mo>
</mrow>
</mrow>
<mi>c</mi>
</mfrac>
<mo>.</mo>
</mrow>
2. the side according to claim 1 that critical micelle concentration of surfactant is determined based on terahertz time-domain spectroscopic technology
Method, it is characterised in that：In step sl, the sample cell of the preparation is divided into：Two panels polythene strip is with striking out square-outside and round-inside type
Hollow PET double faced adhesive tapes, construction method is to utilize adhered by double sided plaster two panels polythene strip one hollow liquid sample pool of formation, tool
Body step is injected fluid sample, another polythene strip covered, liquid first to bond double faced adhesive tape with wherein a piece of polythene strip
Body thickness determines that 100um, 50um may be selected in the thickness of PET double faced adhesive tapes according to PET double faced adhesive tapes thickness.
3. the side according to claim 1 that critical micelle concentration of surfactant is determined based on terahertz time-domain spectroscopic technology
Method, it is characterised in that：In step s 2, the solution example to be measured be by surfactant to be detected and solvent in proportion
The surfactant solution for the concentration known being mixedly configured into；For the first time detection testing sample concentration from 0.1 to 100mM according to
It is secondary incremental, 3-4 different concentration are taken in each magnitude；The concentration of the testing sample of second of detection is tied according to first time detection
Fruit determines.
4. the side according to claim 1 that critical micelle concentration of surfactant is determined based on terahertz time-domain spectroscopic technology
Method, it is characterised in that：Terahertz frequency range is 0.3-1.7THz.
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| CN105548050B (en) * | 2016-01-05 | 2019-03-22 | 河南大学 | A method of utilizing cromoci self assembly peroxidase determination critical micelle concentration of surfactant |
| CN107219187A (en) * | 2017-05-25 | 2017-09-29 | 中国科学院重庆绿色智能技术研究院 | A kind of leather species fast non-destructive detection method based on terahertz light spectral technology |
| CN107917893A (en) * | 2017-11-21 | 2018-04-17 | 深圳市太赫兹科技创新研究院 | Load sample component and tera-hertz spectra test method for terahertz light spectrometry |
| CN108267416A (en) * | 2017-12-25 | 2018-07-10 | 中国科学院重庆绿色智能技术研究院 | A kind of circulating tumor cell screening system and method based on tera-hertz spectra |
| CN109490245A (en) * | 2019-01-04 | 2019-03-19 | 上海理工大学 | Acetone liquid concentration detection method based on terahertz time-domain spectroscopic technology |
| US11761874B2 (en) * | 2020-05-15 | 2023-09-19 | Saudi Arabian Oil Company | CMC-based method for surfactant concentration determination |
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| CN101876633A (en) * | 2009-11-13 | 2010-11-03 | 中国矿业大学 | Terahertz time domain spectroscopy-based textile fiber identification method |
| CN103335976A (en) * | 2013-06-04 | 2013-10-02 | 中国石油大学(北京) | Method for measuring concentrations of sulfate, nitrate solutions by utilizing terahertz time-domain spectroscopy |
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| JP5540236B2 (en) * | 2010-09-22 | 2014-07-02 | 王子ホールディングス株式会社 | Method for measuring weight per unit area and in-plane uniformity |
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| CN101876633A (en) * | 2009-11-13 | 2010-11-03 | 中国矿业大学 | Terahertz time domain spectroscopy-based textile fiber identification method |
| CN103335976A (en) * | 2013-06-04 | 2013-10-02 | 中国石油大学(北京) | Method for measuring concentrations of sulfate, nitrate solutions by utilizing terahertz time-domain spectroscopy |
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| 《Dielectric relaxation change of water upon phase transition of a lipid bilayer probed by terahertz time domain spectroscopy》;Da-Hye Choi等;《THE JOURNAL OF CHEMICAL PHYSICS》;20121231;第137卷;第175101-1至175101-5页 * |
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