CN113884558A - Detection method for accurately detecting Zeta potential of suspension system based on phase analysis light scattering technology and capillary electrode detection device - Google Patents
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Abstract
The invention relates to a detection method for accurately detecting Zeta potential of a suspension system based on a phase analysis light scattering technology and a capillary electrode detection device. The invention analyzes signals through a phase-locked amplification technology to obtain the phase offset of scattered light along with time, further obtains the frequency offset amplitude of the scattered light through the offset and the slope of a time curve, the offset amplitude is calculated through a formula to obtain the electrophoretic mobility, and the direction of the frequency offset relative to the original incident light is related to the sign of the Zeta potential of the particle. And substituting the obtained electrophoretic mobility into a Herry equation, and calculating to obtain the Zeta potential of the particles. The invention can effectively avoid the influence of capillary electroosmosis on the test in the test process.
Description
Technical Field
The invention relates to the technical field of detection devices for Zeta potential of a suspension system, in particular to a detection method for accurately detecting the Zeta potential of the suspension system based on a phase analysis light scattering technology and a capillary electrode detection device.
Background
Particles dispersed in a polar dispersion, such as water, tend to carry some amount of charge on the surface, which causes the particles to form an electric double layer in solution beyond the limits of the particle's surface. The potential of the particle is highest at the surface position of the particle and is called surface potential (surface potential), the potential at the strict potential layer is called strict layer potential (stern potential), the potential value at the position of the slip layer of the particle is called Zeta potential, and the potential value of the particle tends to zero at the position of infinity. Inside the slip layer, all components including solvent molecules and ions move with the particles, while outside the slip layer, the solution environment is considered. The Zeta potential has a sign, with positively charged particles having a positive potential and negatively charged particles having a negative potential.
The magnitude of the Zeta potential is closely related to the stability of the particle system. Under a higher Zeta potential, the interaction force between the particles is stronger, the system is in a more stable state, and under a lower Zeta potential, the repulsive force between the particles is weaker, the particles are easy to agglomerate and flocculate, and the stability of the system is poorer. Factors that primarily affect Zeta potential include the pH of the solution system, ionic strength (salt concentration), and the concentration of small molecule additives. The Zeta potential test has wide application in chemical, biological and medical fields, and the application range covers drug release systems, liposomes, hydrogels, microemulsions, emulsions, polymer solutions, protein samples, gold nanoparticles and the like.
The Zeta potential instrument is an analytical instrument for detecting Zeta potential of a suspension system. The principle is based on an electrophoresis light scattering technology ELS, a laser light source emits light and then splits the light through a light splitting sheet or a light splitting prism, one laser (detection light) irradiates a sample, and the other laser as reference light is directly refracted through a light path and enters a detector. An electric field is applied to two ends of a particle suspension system, the charged particles move electrophoretically under the action of the electric field force, the frequency of scattered light changes due to the electrophoretic motion, and the change amplitude is related to the electrophoretic speed. The photodetector is set at an angle (usually the forward angle for resolution reasons) to detect the scattered light and the beat signal formed after the reference beam has been combined. A piezoelectric ceramic PZT component is embedded in the optical path of the reference light, and the PZT component is applied with voltage to generate displacement under proper periodic frequency, so that the frequency of the reference light is changed, and a fixed fundamental frequency signal is generated. The fundamental frequency signal can be used for judging the direction of electrophoretic motion, so that the symbol of ZETA is obtained, the noise interference of the Brownian motion of particles near 0 frequency can be avoided to a certain extent, and the fundamental frequency signal has an important function of participating in phase-locked amplification signal analysis of a phase analysis light scattering technology.
In the classical ELS technology, correlation calculation is carried out on an original beat frequency signal through a correlator, frequency spectrum distribution is obtained through Fourier transform of a correlation curve, frequency change delta f of a scattering signal and the electrophoretic motion speed of particles are further obtained through Lorentz fitting, and Zeta potential information of the particles is obtained through a Henry equation. A problem with one of the classical ELS techniques is that due to its low resolution of signal resolution and poor noise immunity, it is difficult to obtain accurate and reproducible results for samples with low electrophoretic mobility, i.e. near the electrical midpoint and at high salt concentrations.
The phase analysis light scattering technology PALS is a more advanced electrophoretic light scattering signal processing technology developed on the basis of ELS. And analyzing the original signal by a phase-locked amplification technology to obtain phase information of the scattered light. The change in phase with time reflects the change in frequency. The PALS technology can more accurately detect the electrophoresis speed of the sample with low electrophoresis mobility.
Disclosure of Invention
The invention aims to provide a detection method for accurately detecting Zeta potential of a suspension system based on a phase analysis light scattering technology and a capillary electrode detection device, which has the following specific scheme:
a detection method for accurately detecting a Zeta potential of a suspension system based on a phase analysis light scattering technology and a capillary electrode detection device comprises a capillary electrode, a beam splitter, a detector, a laser, a lens group, a reflector driven by piezoelectric ceramic PZT, a data acquisition card and an operation unit, wherein the laser is emitted and then is divided into two beams of light by the beam splitter, one beam of light is incident light, and the other beam of light is reference light;
the incident light is irradiated on the sample in the capillary electrode through the lens group;
the reference light is combined with the beam by scattering light at an incident light angle of 12 degrees and the sample;
the incident light irradiates on a sample, periodic reverse voltage is applied to two ends of a capillary electrode to form a periodic reverse electric field distributed along the capillary, charged particles suspended in the sample perform electrophoretic motion under the action of the electric field force, and the frequency deviation of scattered light of the sample is caused by the optical Doppler effect generated by the electrophoretic motion of the particles;
the reference light is scattered by a reflector driven by piezoelectric ceramics PZT and a sample to form beam combination to form beat frequency, and then enters a detector;
the output signal of the detector is transmitted to the arithmetic unit by a data acquisition card;
performing signal analysis by a phase-locked amplification technology to obtain the phase offset of scattered light along with time, further obtaining the frequency offset amplitude of the scattered light through the offset and the slope of a time curve, calculating the offset amplitude through a formula to obtain the electrophoretic mobility, wherein the direction of the frequency offset relative to the original incident light is related to the sign of the Zeta potential of the particle;
and substituting the obtained electrophoretic mobility into a Herry equation, and calculating to obtain the Zeta potential of the particles.
The detection method for accurately detecting the Zeta potential of the suspension system based on the phase analysis light scattering technology and the capillary electrode detection device has the preferred scheme that the detection point position of the capillary electrode is arranged in the middle of the bottom of a U-shaped capillary tube of the electrode, the electrode is arranged at the top of the capillary tube, and the distance between the two electrodes is more than 50 mm; the influence of joule heat generated in the process of applying voltage on the electrophoresis movement of the detection point position can be effectively avoided.
The detection method for accurately detecting the Zeta potential of the suspension system based on the phase analysis light scattering technology and the capillary electrode detection device has the preferred scheme that the optical path of the light passing part of the capillary electrode is less than or equal to 4 mm; compared with the traditional sample cell with a 10mm optical path, the optical path is shorter, forward-angle scattered light signals can be more effectively transmitted, and the detection concentration of a sample can be improved.
The detection method for accurately detecting the Zeta potential of the suspension system based on the phase analysis light scattering technology and the capillary electrode detection device has the preferred scheme that high-frequency periodically reversed voltage within the range of 10-30Hz is applied to two ends of a capillary electrode in the test process. The influence of electroosmosis generated by the inner wall of the capillary electrode on the test result in the voltage applying process can be effectively avoided.
The detection method for accurately detecting the Zeta potential of the suspension system based on the phase analysis light scattering technology and the capillary electrode detection device has the preferred scheme that a phase-locked amplification technology is adopted to analyze beat signals formed after scattered light and reference light are combined to obtain a scattered light phase time change curve, namely a phase diagram;
obtaining the frequency change delta f of the scattered light through the slope of the change of the phase signal with the time curve in the phase diagram; and then by the formula
Obtaining the electrophoretic mobility mu of the particles, wherein n is the refractive index of the dispersion liquid, lambda is the laser wavelength, theta is the included angle of scattered light and incident light, and E is the electric field intensity;
the electrophoretic mobility of the system is substituted into the Herry equation:
calculating Zeta potential information of the particles; where f (κ α) is the Henry function, κ is the reciprocal Debye radius, α represents the particle size, and α κ represents the ratio of the bilayer thickness to the particle radius.
The detection method for accurately detecting the Zeta potential of the suspension system based on the phase analysis light scattering technology and the capillary electrode detection device has the preferred scheme that high-frequency periodically reversed voltage within the range of 10-30Hz is applied to two ends of a capillary electrode in a test process, two phase signals corresponding to particle electrophoretic motion in opposite directions are obtained in each period, and the frequency change amplitude delta f of two groups of scattered light is obtained by solving the absolute value of the slope of each phase signal changing along with time; the frequency change amplitude value deltaf of scattered light is obtained by multiplying the number of applied cycles by 2 times in a test, and the average frequency change amplitude value of the scattered light is obtained by averaging
The preferable scheme of the detection method for accurately detecting the Zeta potential of the suspension system based on the phase analysis light scattering technology and the capillary electrode detection device is that the electrophoresis direction of particles is judged according to the change trend of the phase in a phase diagram along with time, namely the sign of the change slope of the phase along with time, so that the sign of the charged surface of the particles is obtained.
The preferable scheme of the detection method for accurately detecting the Zeta potential of the suspension system based on the phase analysis light scattering technology and the capillary electrode detection device is that a periodic voltage is applied to the piezoelectric ceramic to drive the piezoelectric ceramic to do periodic linear reciprocating motion through a reflector driven by the piezoelectric ceramic PZT on a reference light path, so that a fundamental frequency signal with fixed frequency is applied to the reference light, and the fundamental frequency signal participates in the phase-locked amplification technology to analyze the frequency offset of scattered light.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention combines the phase analysis light scattering technology and the capillary electrode to realize the accurate detection of the low electrophoretic mobility, the device has good popularization and practical value, and good economic and social benefits can be generated after wide popularization and application;
2. the invention avoids the influence of electroosmotic flow on the test result by applying high-frequency periodic reversal voltage within the range of 10-30Hz in the test process, and because the capillary electrode device is adopted, electroosmotic flow along the wall of the capillary tube can be generated in the process of applying an electric field, and the electroosmotic flow can influence the electrophoretic movement of particles. Electroosmotic flow typically reaches a steady increasing stage above 250ms of applied electric field, while its contribution is negligibly small below 250 ms. Therefore, the invention applies a periodic reverse electric field of 10-30Hz in the test process, and each voltage application period is far less than 250ms, thereby effectively avoiding the influence of electroosmotic flow generated by the inner wall of the capillary electrode in the voltage application process on the test result;
3. the optical path of the light-transmitting part of the capillary tube electrode adopted in the invention is less than or equal to 4mm, and is shorter than the optical path of 10mm of the traditional sample cell, so that forward-angle scattered light signals can be more effectively transmitted, and the detection concentration of a sample can be improved;
4. the invention is widely applied to precise electricians, electronics, instruments and meters and other products, and is mainly applied to the research and application fields of medical treatment and health, biological pharmacy, agricultural scientific research, environmental protection and the like.
Drawings
FIG. 1 is an electrical schematic diagram of a detection method for accurately detecting Zeta potential of a suspension system based on a phase analysis light scattering technology and a capillary electrode detection device according to the present invention;
FIG. 2 is a schematic diagram of the optical path structure of the present invention;
FIG. 3 is a schematic diagram illustrating the positions of detection points and the included angles between scattered light and incident light;
FIG. 4 is a cross-sectional view and a side sectional view of a capillary electrode in accordance with the present invention;
FIG. 5 is a schematic diagram showing the application of a periodic inversion voltage to a capillary electrode and the phase change over time of a corresponding scattered light signal in accordance with the present invention.
In the figure, 1, a capillary electrode 2, a beam splitter 3, a detector 4, a laser 5, a lens group 6, a reflector 7, a reflector 8 driven by piezoelectric ceramic PZT, a data acquisition card 9, incident light 10, reference light 11, scattered light 12, a signal 13 after scattered light and reference light combination, an electrode 14, a detection point position 15, a capillary channel 16 and an arithmetic unit are arranged.
Detailed Description
The technical solutions in the present invention will be described clearly and completely with reference to the accompanying drawings, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1-5, a detection method for accurately detecting Zeta potential of a suspension system based on a phase analysis light scattering technology and a capillary electrode detection device includes a capillary electrode 1, a beam splitter 2, a detector 3, a laser 4, a lens group 5, a reflector 6, a reflector 7 driven by piezoelectric ceramic PZT, a data acquisition card 8 and an arithmetic unit 16, wherein the laser 4 splits two beams of light through the beam splitter after being emitted, one path is incident light 9, and the other path is reference light 10;
the incident light 9 is irradiated on the sample in the capillary electrode 1 through the lens group 5;
the incident light 9 irradiates at a detection point position and penetrates through an electrode, and the detector 3 detects scattered light 11 forming an included angle of 12 degrees with the incident light 9; the reference light 10 is combined with the scattered light of the sample at an angle of 12 degrees of incident light, and a beam combining signal 12 is emitted from the scattered light and the reference light;
the incident light 9 irradiates on the sample, a periodic reversal voltage is applied to two ends of the capillary electrode 1 to form a periodic reversal electric field distributed along the capillary, the charged particles suspended in the sample perform electrophoretic motion under the action of the electric field force, and the frequency shift of the scattered light 11 of the sample is caused by the optical Doppler effect generated by the electrophoretic motion of the particles;
the reference light 10 is combined with sample scattered light 11 to form beat frequency through a reflector 7 driven by piezoelectric ceramic PZT, and then enters a detector 3;
the output signal of the detector 3 is transmitted to an arithmetic unit 16 by a data acquisition card 8;
performing signal analysis by a phase-locked amplification technology to obtain the phase offset of the scattered light 11 along with time, further obtaining the frequency offset amplitude of the scattered light 11 through the offset and the slope of a time curve, calculating the offset amplitude by a formula to obtain the electrophoretic mobility, wherein the direction of the frequency offset relative to the original incident light is related to the sign of the Zeta potential of the particle;
and substituting the obtained electrophoretic mobility into a Herry equation, and calculating to obtain the Zeta potential of the particles.
The detection point position 14 of the capillary electrode 1 is arranged in the middle of the bottom of the U-shaped capillary tube, the two sides of the upper end of the capillary tube are respectively provided with an electrode plate 13, the distance between the two electrodes is more than 50mm, and a sample is contained in a capillary tube channel 15.
The optical path of the light-transmitting part of the capillary tube electrode 1 is less than or equal to 4 mm; the small light transmission length is beneficial to scattering light of a high-concentration sample, and the concentration upper limit of the sample corresponding to the Zeta potential test is effectively increased.
A high frequency periodically reversed voltage in the range of 10-30Hz was applied across the capillary electrode 1 during the test.
Analyzing beat frequency signals formed after the scattered light and the reference light are combined by adopting a phase-locked amplification technology to obtain a scattered light phase time-varying curve, namely a phase diagram;
obtaining the frequency change delta f of the scattered light through the slope of the change of the phase signal with the time curve in the phase diagram; and then by the formula
Obtaining the electrophoretic mobility mu of the particles, wherein n is the refractive index of the dispersion liquid, lambda is the laser wavelength, theta is the included angle of scattered light and incident light, and E is the electric field intensity;
the electrophoretic mobility of the system is substituted into the Herry equation:
calculating Zeta potential information of the particles; where f (κ α) is the Henry function, κ is the reciprocal Debye radius, α represents the particle size, and α κ represents the ratio of the bilayer thickness to the particle radius.
Applying high-frequency periodically reversed voltage within the range of 10-30Hz to two ends of the capillary electrode 1 in a test process, obtaining two phase signals corresponding to the electrophoretic movement of the particles in opposite directions in each period, and obtaining frequency change amplitude values delta f of two groups of scattered light by solving the absolute value of the slope of each phase signal along with the change of time; the frequency change amplitude value deltaf of scattered light is obtained by multiplying the number of applied cycles by 2 times in a test, and the average frequency change amplitude value of the scattered light is obtained by averaging
The electrophoretic direction of the particles is judged according to the change trend of the phase along with time in the phase diagram, namely the sign of the change slope of the phase along with time, so as to obtain the sign of the surface charge of the particles.
A periodic voltage is applied to the piezoelectric ceramics to drive the piezoelectric ceramics to do periodic linear reciprocating motion on a reference light path 10 through a piezoelectric ceramics PZT driven reflector 7, so that a fundamental frequency signal with a fixed frequency is applied to the reference light 10, and the fundamental frequency signal participates in the phase-locked amplification technology to analyze the frequency offset of the scattered light 11.
The capillary electrode 1 is entirely made of a highly light-transmitting polycarbonate PC material.
Claims (9)
1. A detection method for accurately detecting Zeta potential of a suspension system based on a phase analysis light scattering technology and a capillary electrode detection device is characterized by comprising the following steps: the device comprises a capillary electrode, a beam splitter, a detector, a laser, a lens group, a reflector driven by piezoelectric ceramics PZT, a data acquisition card and an arithmetic unit, wherein the laser is emitted and then is divided into two beams of light by the beam splitter, one beam is incident light, and the other beam is reference light;
the incident light is irradiated on the sample in the capillary electrode through the lens group;
incident light irradiates at a detection point and penetrates through an electrode, and a detector detects scattered light forming an included angle of 12 degrees with the incident light; the reference light is combined with the beam by scattering at an incident light angle of 12 degrees and the sample;
the incident light irradiates on a sample, periodic reverse voltage is applied to two ends of a capillary electrode to form a periodic reverse electric field distributed along the capillary, charged particles suspended in the sample perform electrophoretic motion under the action of the electric field force, and the frequency deviation of scattered light of the sample is caused by the optical Doppler effect generated by the electrophoretic motion of the particles;
the reference light is scattered by a reflector driven by piezoelectric ceramics PZT and a sample to form beam combination to form beat frequency, and then enters a detector;
the output signal of the detector is transmitted to the arithmetic unit by a data acquisition card;
performing signal analysis by a phase-locked amplification technology to obtain the phase offset of scattered light along with time, further obtaining the frequency offset amplitude of the scattered light through the offset and the slope of a time curve, calculating the offset amplitude through a formula to obtain the electrophoretic mobility, wherein the direction of the frequency offset relative to the original incident light is related to the sign of the Zeta potential of the particle;
and substituting the obtained electrophoretic mobility into a Herry equation, and calculating to obtain the Zeta potential of the particles.
2. The detection method for accurately detecting the Zeta potential of the suspension system based on the phase analysis light scattering technology and the capillary electrode detection device as claimed in claim 1, wherein the detection method comprises the following steps: the detection point position of the capillary electrode is arranged in the middle of the bottom of the U-shaped capillary tube, two sides of the upper end of the capillary tube are respectively provided with an electrode plate, the distance between the two electrodes is larger than 50mm, and a sample is contained in a capillary channel.
3. The detection method for accurately detecting the Zeta potential of the suspension system based on the phase analysis light scattering technology and the capillary electrode detection device as claimed in claim 1, wherein the detection method comprises the following steps: the optical path of the light-transmitting part of the capillary electrode is less than or equal to 4 mm; the small light transmission length is beneficial to scattering light of a high-concentration sample, and the concentration upper limit of the sample corresponding to the Zeta potential test is effectively increased.
4. The detection method for accurately detecting the Zeta potential of the suspension system based on the phase analysis light scattering technology and the capillary electrode detection device as claimed in claim 1, wherein the detection method comprises the following steps: a high frequency periodically reversed voltage in the range of 10-30Hz was applied across the capillary electrodes during the test.
5. The detection method for accurately detecting the Zeta potential of the suspension system based on the phase analysis light scattering technology and the capillary electrode detection device as claimed in claim 1, wherein the detection method comprises the following steps: analyzing beat frequency signals formed after the scattered light and the reference light are combined by adopting a phase-locked amplification technology to obtain a scattered light phase time-varying curve, namely a phase diagram;
obtaining the frequency change delta f of the scattered light through the slope of the change of the phase signal with the time curve in the phase diagram; and then by the formula
Obtaining the electrophoretic mobility mu of the particles, wherein n is the refractive index of the dispersion liquid, lambda is the laser wavelength, theta is the included angle of scattered light and incident light, and E is the electric field intensity;
the electrophoretic mobility of the system is substituted into the Herry equation:
calculating Zeta potential information of the particles; where f (κ α) is the Henry function, κ is the reciprocal Debye radius, α represents the particle size, and α κ represents the ratio of the bilayer thickness to the particle radius.
6. The method for accurately detecting the Zeta potential of the suspension system based on the phase analysis light scattering technology and the capillary electrode detection device as claimed in claim 5, wherein the method comprises the following steps: applying high-frequency periodically reversed voltage within the range of 10-30Hz to two ends of a capillary electrode in a test process, obtaining two phase signals corresponding to the electrophoretic movement of particles in opposite directions in each period, and obtaining frequency change amplitude values delta f of two groups of scattered light by solving the absolute value of the slope of each phase signal along with the change of time; the frequency change amplitude value deltaf of scattered light is obtained by multiplying the number of applied cycles by 2 times in a test, and the average frequency change amplitude value of the scattered light is obtained by averaging
7. The method for accurately detecting the Zeta potential of the suspension system based on the phase analysis light scattering technology and the capillary electrode detection device as claimed in claim 5, wherein the method comprises the following steps: the electrophoretic direction of the particles is judged according to the change trend of the phase along with time in the phase diagram, namely the sign of the change slope of the phase along with time, so as to obtain the sign of the surface charge of the particles.
8. The detection method for accurately detecting the Zeta potential of the suspension system based on the phase analysis light scattering technology and the capillary electrode detection device as claimed in claim 1, wherein the detection method comprises the following steps: a periodic voltage is applied to the piezoelectric ceramics to drive the piezoelectric ceramics to do periodic linear reciprocating motion, so that a fundamental frequency signal with fixed frequency is applied to the reference light, and the fundamental frequency signal participates in a phase-locked amplification technology to analyze the frequency change amplitude of scattered light.
9. The detection method for accurately detecting the Zeta potential of the suspension system based on the phase analysis light scattering technology and the capillary electrode detection device as claimed in claim 1, wherein the detection method comprises the following steps: the capillary electrode is made of polycarbonate PC material with high light transmittance.
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