CN105572259A - Method for determining critical micelle concentration of surfactant - Google Patents
Method for determining critical micelle concentration of surfactant Download PDFInfo
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- CN105572259A CN105572259A CN201610034805.7A CN201610034805A CN105572259A CN 105572259 A CN105572259 A CN 105572259A CN 201610034805 A CN201610034805 A CN 201610034805A CN 105572259 A CN105572259 A CN 105572259A
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- surfactant
- critical micelle
- micelle concentration
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
Abstract
The invention discloses a method for determining the critical micelle concentration of a surfactant and particularly provides a method for determining the critical micelle concentration of the surfactant by utilizing tracer agent headspace gas chromatography. The surfactant is added into a volumetric flask, and then 0.5 L of distilled water and a toluene-methanol solution are added into the volumetric flask to prepare a stock solution of the surfactant; different masses of the stock solution are respectively taken and put into 10 headspace bottles, dilution is performed by using 5 mL of distilled water, and sealing is performed by using press caps; the headspace bottles containing the surfactant solution are subjected to headspace gas chromatography and balanced in a headspace sampling device, and then gas-phase signal values of toluene are recorded through gas chromatography detection; drawing is performed based on the gas-phase signal values of the toluene and the corresponding concentrations of the surfactant in the headspace bottles. The method is quick in determination, objective and accurate in result and simple and convenient to operate, is especially suitable for determination of the critical micelle concentration at the rising temperature. The shortcomings of an existing method for detecting the critical micelle concentration of the surfactant are effectively overcome.
Description
Technical field
The present invention relates to critical micelle concentration detection technique field, particularly relate to a kind of method measuring critical micelle concentration of surfactant.
Background technology
Surfactant industry, agricultural and the medium every field of daily life application widely, therefore the research of Surfactant is very active.Micella is a key concept in surface chemistry, when the concentration of surfactant molecule increases, its structure can change spherical, bar-shaped and lamellar micelle into from unimolecule. and the concentration forming micella its solution of certain surfactant is called the critical micelle concentration (criticalmicelleconcentration, cmc) of this surfactant.Because many physicochemical property such as conductivity, surface tension, osmotic pressure, vapor pressure, optical property, dirt-removing power, density, viscosity, osmotic pressure and the light scatter intensity etc. of surfactant solution are undergone mutation along with the formation of micella.Therefore, it is possible to the critical micelle concentration of chart surface-active agent, for a lot of research field, has important practical significance fast and accurately.
The influence factor of CMC value is a lot, and the change of temperature, inorganic salts, alcohols, pressure, pH value etc. all can change the size of CMC value.In above influence factor, temperature is very large to the influence of cmc.The cmc method of chart surface-active agent is a lot. and conventional has surface tension method, conductance method, dye method, solubilising method, osmometry, pulse radiolysis method, fluorescence method, ultrasonic absorption method, nephelometry, pH value method, rheological method, ion-selective electrode method and cyclic voltammetry etc.But various method all has its limitation.As conductance method is not obvious and insensitive to comparatively large, that surfactivity the is low surfactant turning point of cmc value, and the existence of inorganic salts also can reduce the sensitivity of mensuration greatly; Densimetry due to the density difference of variable concentrations solution little, accuracy is not good; It is complicated, time-consuming that viscosimetry surveys cmc Value Operations, and error is also large; Surface tension method can be subject to some restrictions when the surface tension of Accurate Measurement surfactant solution, as the radius of kapillary, the density of solution and solution will be measured in capillary tube technique exactly to the contact angle of glass, drop-volume method and drop-weight method need to know correction factor, and maximum bubble pressure method solution can bubble strongly.Further, above method is not suitable for the mensuration of high temperature lower surface activating agent critical micelle concentration.Therefore, be necessary to develop the critical micelle concentration that a kind of new detection method carrys out rapid and accurate determination surfactant.
Summary of the invention
The object of the invention is to the shortcoming and defect overcoming above-mentioned prior art, provide a kind of fast, the method for result precision, mensuration critical micelle concentration of surfactant easy and simple to handle.Overcome the drawback existing for method detecting critical micelle concentration of surfactant at present.
The present invention adopts a small amount of toluene as tracer agent, if the concentration of surfactant does not reach capacity in ml headspace bottle solution, in system, toluene balance exists solution-air biphase equilibrium.So in ml headspace bottle, the partition factor of toluene meets Henry's law, that is:
In formula: C
g, C
lbe expressed as the concentration in toluene concentration in the gas phase and liquid phase.
If the concentration of surfactant is higher than its critical micelle concentration in ml headspace bottle, unnecessary surfactant forms granule.Therefore there is airwater mist cooling balance in toluene balance in system, and toluene also exists partition factor in liquid phase and solid phase, that is:
In formula: C
mbe expressed as the concentration of toluene in solid phase.
Based on above principle, head space gas chromatography is utilized to detect a series of surfactant solution (surfactant concentration ranges is never saturated to higher than critical micelle concentration) containing toluene tracer agent.Gained toluene gas-phase signal value drawn with the concentration of surfactant in corresponding ml headspace bottle, horizontal ordinate concentration corresponding to the joining of gained two straight lines is the critical micelle concentration of this surfactant.
The present invention is achieved through the following technical solutions:
Measure a method for critical micelle concentration of surfactant, specifically utilize tracer agent headspace gas chromatography to measure critical micelle concentration of surfactant, realize by following steps:
Step (1) Sample Preparation Procedure:
Surfactant is added in volumetric flask, then in volumetric flask, adds 0.5L distilled water and toluene-methanol solution, the stoste of obtained surfactant;
The stoste of getting different quality respectively in 10 ml headspace bottle, with distilled water diluting to 5mL, then gland packing;
Step (2) sample detection: the ml headspace bottle containing surfactant solution after step (1) process puts into headspace gas chromatography, in head-space sampler after overbalance, by gas chromatographic detection, the gas-phase signal value of record toluene;
Step (3) interpretation of result: drawn by surfactant concentration in the ml headspace bottle corresponding to step (2) gained toluene gas-phase signal value and step (1), horizontal ordinate concentration corresponding to the joining of gained two straight lines is the critical micelle concentration of this surfactant.
Join the toluene-methanol solution in stoste in above-mentioned steps (1), toluene concentration is 10g/L, and volume is 50 μ L.
In stoste obtained in above-mentioned steps (1), the concentration of surfactant is measuring the critical micelle concentration at temperature higher than this surfactant.
Stoste obtained in above-mentioned steps (1) should at room temperature balance 24 hours, and when joining ml headspace bottle first ultrasound wave 1 hour, be evenly distributed to make the surfactant in stoste.
In 10 ml headspace bottle obtained in above-mentioned steps (1), the concentration range of surfactant is for be never saturated to supersaturation concentration.
Above-mentioned steps (2) head-space sampler condition is as follows: equilibrium temperature is for measuring temperature, and equilibration time 40min, vibration condition is set to intense oscillations, ml headspace bottle 10s pressing time, quantitative loop filling time 15s, transfers to GC time 20s.
During above-mentioned steps (2) gas chromatographic detection, operating conditions is: hydrogen ion flame detector, and carrier gas is nitrogen, flow velocity 3.8mL/min, pressure 30psi, injector temperature 250 DEG C, and capillary column temperature 80 DEG C, does not shunt, detection time 2min.
The present invention, relative to prior art, has following advantage and effect:
The present invention establishes a kind of method utilizing tracer agent Headspace-Gas Chromatography rapid and accurate determination critical micelle concentration of surfactant, the method is by optimizing tracer agent addition and equilibration time, effectively raise the degree of accuracy of detection, detection method is easy and simple to handle, degree of accuracy is high, is applicable to the mensuration of critical micelle concentration of surfactant at an elevated temperature.
This method not only technological means is simple and easy to do, is also specially adapted to the mensuration of critical micelle concentration at an elevated temperature.Overcome the ubiquitous drawback of method detecting critical micelle concentration of surfactant at present.
Accompanying drawing explanation
Fig. 1 is that toluene level affects collection of illustrative plates to neopelex Determination of Critical Micelle Concentration.
Fig. 2 is that equilibration time affects collection of illustrative plates to toluene-neopelex solution.
Fig. 3 is the HS-GC response signal change collection of illustrative plates of neopelex temperature 40 DEG C of variable concentrations.
Fig. 4 is the HS-GC response signal change collection of illustrative plates of potassium stearate at temperature 50 C of variable concentrations.
Fig. 5 is the HS-GC response signal change collection of illustrative plates of OPEO at temperature 50 C of variable concentrations.
Embodiment
Below in conjunction with specific embodiment, the present invention is more specifically described in detail.
Instrument and equipment used in the present invention: the automatic headspace sampler of HP-7694 type, Agilent A7890 type gas chromatograph (hydrogen ion flame detector, DB-5 type capillary chromatographic column), ml headspace bottle (21.6ml), white Teflon/white silica gel dottle pin (containing aluminium lid), gland device.
Reagent used in the present invention: neopelex, potassium stearate, OPEO, toluene (analyzing pure), methyl alcohol (analyzing pure).
Embodiment 1
With the concentration of neopelex determination tracer agent toluene of the present invention
One, the preparation of stoste
The toluene pipetting 0.1mL is in the volumetric flask of 10mL, and by methanol constant volume to scale, namely toluene concentration is 10g/L.
Take 1.86g neopelex respectively in three volumetric flasks, then add 0.5L distilled water in volumetric flask.In volumetric flask, add 50 μ L, 75 μ L, the above-mentioned toluene-methanol solution purchased of 100 μ L respectively, be namely respectively 1mg/L, 1.5mg/L, 2mg/L containing toluene concentration in the stoste of surfactant.The stoste of purchasing is put equilibrate at room temperature 24 hours.
Two, the preparation of sample
The above-mentioned three kinds of stoste ultrasonic echographies purchased are shaken 1 hour.Then the same stoste of different quality is taken respectively in 10 ml headspace bottle, with distilled water diluting to 5g, namely obtain the surfactant solution (0,0.5mmol/L, 0.8mmol/L, 1mmol/L, 1.2mmol/L, 1.4mmol/L, 1.6mmol/L, 1.8mmol/L, 2mmol/L, 2.2mmol/L) of variable concentrations.Then use the gland packing of gland device, detect in headspace gas chromatography and analyze.
Three, detection method
Head-space sampler condition: equilibrium temperature is 40 DEG C, equilibration time 40min, and vibration condition is set to intense oscillations, sample bottle 10s pressing time, quantitative loop filling time 15s, transfer to GC time 20s.
Gas chromatography operating conditions: hydrogen ion flame detector (FID), carrier gas is nitrogen, flow velocity 3.8mL/min, pressure 30psi, injector temperature 250 DEG C, and capillary column temperature 80 DEG C, does not shunt, detection time 2min.
This method adopts toluene as tracer agent, is because toluene is hydrophobic material (atomic water-soluble), so be more easily adsorbed in low volatility surfactant.And toluene is volatile material, its signal can be detected by GC.
The concentration joining the tracer agent toluene in low volatility surfactant solution will affect the sensitivity of the method.Fig. 1 describes the impact of toluene level on neopelex Determination of Critical Micelle Concentration, and toluene level is lower, and turning point is in the drawings more obvious.But, if toluene level is too low will reduce the detection sensitivity of headspace gas chromatography.Therefore, by considering, the present invention selects best toluene addition to be 1mg/L.
Embodiment 2
Equilibration time is on the impact of testing result
Take the neopelex stoste containing toluene 1mg/L prepared by example 1.Get 4.0g (lower than triacetyl glycerine critical micelle concentration at this temperature) respectively and 5.0g (higher than neopelex critical micelle concentration at this temperature), in different top empty bottle, is settled to 5g with distilled water.Analyze under different head space equilibration time and detect, obtain curve shown in Fig. 2.As seen from Figure 2, when the concentration of surfactant is lower than critical micelle concentration, balance 20min can reach balance.When higher than critical micelle concentration, required time just reaches balance at 40min.In order to ensure to reach balance completely in operation, the present invention selects equilibration time to be 40min.
Embodiment 3
The reappearance of method and accuracy
The reappearance evaluation of method is that detecting acquired results relative standard deviation is 3.5% by detecting lauryl sodium sulfate the critical micelle concentration of 40 DEG C, preparing 3 Duplicate Samples according to method described in Application Example 1.Therefore, can think that the critical micelle concentration detection at an elevated temperature of this method Surfactant has good reappearance.
The accuracy of the method is the critical micelle concentration by detecting 5 surfactants, and measured result and present data is contrasted.Interpretation of result in table 1, the critical micelle concentration data relative error very little (relative error <9.0%) as seen from Table 1 in the method acquired results and present list of references.Show that this tracer agent Headspace-Gas Chromatography can the critical micelle concentration of Accurate Determining surfactant, especially detect higher than the critical micelle concentration under room temperature.
The contrast of table 1 method
The head space automatic sampling apparatus of Current commercial does not have condensing unit, therefore sample can not be balanced under room temperature or lower temperature.But this problem can solve by introducing condensing unit.
As mentioned above, just the present invention can be realized preferably.
Embodiments of the present invention are not restricted to the described embodiments; other are any do not deviate from Spirit Essence of the present invention and principle under do change, modification, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (7)
1. measure a method for critical micelle concentration of surfactant, it is characterized in that, be utilize tracer agent headspace gas chromatography to measure critical micelle concentration of surfactant, comprise the steps:
Step (1) Sample Preparation Procedure:
Surfactant is added in volumetric flask, then in volumetric flask, adds 0.5L distilled water and toluene-methanol solution, the stoste of obtained surfactant;
The stoste of getting different quality respectively in 10 ml headspace bottle, with distilled water diluting to 5mL, then gland packing;
Step (2) sample detection: the ml headspace bottle containing surfactant solution after step (1) process puts into headspace gas chromatography, in head-space sampler after overbalance, by gas chromatographic detection, the gas-phase signal value of record toluene;
Step (3) interpretation of result: drawn by surfactant concentration in the ml headspace bottle corresponding to step (2) gained toluene gas-phase signal value and step (1), horizontal ordinate concentration corresponding to the joining of gained two straight lines is the critical micelle concentration of this surfactant.
2. measure the method for critical micelle concentration of surfactant according to claim 1, it is characterized in that:
Join the toluene-methanol solution in stoste in step (1), toluene concentration is 10g/L, and volume is 50 μ L.
3. measure the method for critical micelle concentration of surfactant according to claim 1, it is characterized in that:
In stoste obtained in step (1), the concentration of surfactant is measuring the critical micelle concentration at temperature higher than this surfactant.
4. according to any one of claims 1 to 3, measure the method for critical micelle concentration of surfactant, it is characterized in that:
Stoste obtained in step (1) should at room temperature balance 24 hours, and when joining ml headspace bottle first ultrasound wave 1 hour, be evenly distributed to make the surfactant in stoste.
5. measure the method for critical micelle concentration of surfactant according to claim 4, it is characterized in that:
In 10 ml headspace bottle obtained in step (1), the concentration range of surfactant is for be never saturated to supersaturation concentration.
6. measure the method for critical micelle concentration of surfactant according to claim 4, it is characterized in that:
Step (2) head-space sampler condition is as follows: equilibrium temperature is for measuring temperature, and equilibration time 40min, vibration condition is set to intense oscillations, ml headspace bottle 10s pressing time, quantitative loop filling time 15s, transfers to GC time 20s.
7. measure the method for critical micelle concentration of surfactant according to claim 4, it is characterized in that:
During step (2) gas chromatographic detection, operating conditions is: hydrogen ion flame detector, and carrier gas is nitrogen, flow velocity 3.8mL/min, pressure 30psi, injector temperature 250 DEG C, and capillary column temperature 80 DEG C, does not shunt, detection time 2min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107132298A (en) * | 2017-06-30 | 2017-09-05 | 华南理工大学 | A kind of method that utilization tracer Headspace-Gas Chromatography determines high hydroscopic resin water absorption rate |
| CN107941966A (en) * | 2018-01-09 | 2018-04-20 | 华南理工大学 | A kind of method based on headspace gas chromatography measurement guar gum molecular weight |
| KR102248106B1 (en) * | 2019-11-06 | 2021-05-04 | 서강대학교산학협력단 | Method of measuring the critical micelle concentration of a surfactant using mass spectrometry |
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| CN103558125A (en) * | 2013-11-26 | 2014-02-05 | 南京中医药大学 | System and method for detecting critical micelle concentration of surfactant |
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| CN103558125A (en) * | 2013-11-26 | 2014-02-05 | 南京中医药大学 | System and method for detecting critical micelle concentration of surfactant |
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| ABUL HUSSAM等: "General Method for the Study of Solute-Surfactant Association Equilibria of Volatile Solutes by Headspace Gas Chromatography", 《ANALYTICAL CHEMISTRY》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107132298A (en) * | 2017-06-30 | 2017-09-05 | 华南理工大学 | A kind of method that utilization tracer Headspace-Gas Chromatography determines high hydroscopic resin water absorption rate |
| CN107132298B (en) * | 2017-06-30 | 2019-10-18 | 华南理工大学 | A method of high hydroscopic resin water absorption rate is measured using tracer Headspace-Gas Chromatography |
| CN107941966A (en) * | 2018-01-09 | 2018-04-20 | 华南理工大学 | A kind of method based on headspace gas chromatography measurement guar gum molecular weight |
| KR102248106B1 (en) * | 2019-11-06 | 2021-05-04 | 서강대학교산학협력단 | Method of measuring the critical micelle concentration of a surfactant using mass spectrometry |
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Application publication date: 20160511 |