A flow mode nanoparticle sizer based on dynamic and static light scattering techniques and a detection method thereof

By combining dynamic and static light scattering technology with a flow-mode nanoparticle size analyzer based on a field-flow separation system, the problems of low resolution and large molecular weight detection error in traditional nanoparticle size analyzers for wide-distribution samples are solved. This achieves high-resolution particle size and molecular weight distribution detection and provides more accurate detection results.

CN116067847BActive Publication Date: 2025-12-12DANDONG BETTERSIZE INSTR LTD
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Patent Information

Application Number
CN202310109470.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-02-14
Publication Date
2025-12-12
Estimated Expiration
2043-02-14

AI Technical Summary

Technical Problem

Traditional nanoparticle size analyzers have low resolution for particle size detection in samples with a wide particle size distribution, large errors in molecular weight detection results, low repeatability, and cannot provide molecular weight distribution results.

Method used

A flow-mode nanoparticle size analyzer based on dynamic and static light scattering technology was used, combined with a field flow separation system FFF or gel permeation chromatography GPC/SEC. The scattered light of the particles was detected by APD and PD detectors, respectively. The particle size and molecular weight were calculated using the Stokes-Einstein equation and the Rayleigh scattering equation. High-resolution particle size and molecular weight distribution were obtained by combining differential refractive index or ultraviolet detector.

Benefits of technology

It achieves high-resolution particle size and molecular weight distribution detection, and can simultaneously provide weight-average, number-average and Z-average molecular weights, as well as molecular weight distribution curves and structural information of polymers, thereby improving the accuracy and repeatability of detection.

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Abstract

The application discloses a flow mode nanoparticle size analyzer based on dynamic and static light scattering technology and a detection method thereof. The technology and method are suitable for being connected with a complete front-end separation equipment-field flow separation system or gel permeation chromatography, wherein the front-end separation equipment can separate each component according to the size of the sample components and flow out in sequence. The nanoparticle size analyzer comprises a flow-through sample cell, an APD detector for dynamic light scattering technology, a PD detector for static light scattering technology, a laser, a lens group, first and second data acquisition cards and a control unit. The laser emitted by the laser irradiates on the sample in the flow-through sample cell through the lens group, the two detectors simultaneously receive the scattered light of the sample, and the signals are transmitted to the control unit through the first and second data acquisition cards respectively. The application realizes accurate and high-resolution detection of the size and molecular weight of the sample, and meanwhile, the intrinsic viscosity information can also be obtained.
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Description

TECHNICAL FIELD

[0001] The present application relates to a kind of nanoparticle size analyzer, specifically, a kind of flow mode nanoparticle size analyzer based on dynamic and static light scattering technology and its detection method. BACKGROUND

[0002] Traditional nanoparticle size analyzer is based on dynamic light scattering technology, uses a laser beam to illuminate sample, and detects the fluctuation of scattered light caused by Brownian motion of particles suspended in liquid by photodetector. The fluctuation signal of original scattered light intensity over time is obtained by correlation calculation to obtain the correlation curve of the system, and then the particle size and particle size distribution are obtained by different mathematical models, such as cumulative method or multi-exponential method.

[0003] Generally speaking, nanoparticle size analyzer has dynamic light scattering and static light scattering testing capability. The particle system in the particle size range of about 1 nanometer to 1000 nanometers can be effectively detected by dynamic light scattering technology, which has the characteristics of fast test speed, wide range, good repeatability and accuracy, and has been widely used. However, the traditional quartz or plastic cuvette test mode (often referred to as batch mode in literature) is widely used in nanoparticle size analyzer, which has low resolution for particle size distribution test of wide distribution sample, and the limit resolution can only distinguish narrow distribution single component with 2.5-3 times difference in particle size, which greatly limits the quantification of particle size distribution results. Nanoparticle size analyzer can also use static light scattering (Rayleigh scattering equation) to detect the net scattering intensity of a series of protein or polymer solutions with different concentrations, then draw Debye curve and linear extrapolation to obtain the average molecular weight Mw of the sample. Since this method is complicated, the accuracy of sample concentration and the cleanliness of sample are required to be very high, and the operation personnel and operating environment are required to be high, which leads to large error (±10% or more) in detection result, low repeatability (±10% or more), and cannot give molecular weight distribution result, so actual application and literature report are less. SUMMARY

[0004] In view of the low resolution of particle size detection of wide distribution sample, the large error of molecular weight detection, the low repeatability, and the inability to give molecular weight distribution result in the existing nanoparticle size analyzer technology, the present application solves the problem by providing a flow mode nanoparticle size analyzer based on dynamic and static light scattering technology and its detection method.

[0005] To solve the above technical problems, the technical solution adopted by the present application is:

[0006] The application provides a flow mode nanoparticle size analyzer based on dynamic and static light scattering technology, which is suitable for being connected with a complete front-end particle separation device-field flow fractionation system (FFF) or a polymer and protein separation device-gel permeation chromatography (GPC / SEC), wherein the front-end separation device comprises at least one differential refractive detector or one ultraviolet detector, each component of a sample can be separated according to the size of the component, and the components are sequentially discharged. The nanoparticle size analyzer comprises a flow-through sample cell, an APD detector for dynamic light scattering technology, a PD detector for static light scattering technology, a laser, a focusing lens, a first data acquisition card and a control unit, and a second data acquisition card and a control unit, wherein the laser emitted by the laser irradiates the sample in the flow-through sample cell through the focusing lens, the two detectors simultaneously receive the scattered light of the sample, and the signals are transmitted to the control unit through the first data acquisition card and the second data acquisition card, respectively.

[0007] A detection method of a flow mode nanoparticle size analyzer based on dynamic and static light scattering technology, preferably, the 90° or backscatter arranged optical fiber receiving assembly connected with the APD detector collects the dynamic light scattering scattered light fluctuation signal, calculates the correlation curve, calculates the diffusion coefficient of the sample particles, obtains the particle size of each discharged component through the Stokes Einstein equation, and obtains the high-resolution particle size distribution independent of the calculation model in combination with the concentration signal obtained by the differential refractive detector or the ultraviolet detector. The 90° optical fiber receiving assembly is suitable for detecting samples with moderate concentration, strong scattered light and no multiple light scattering, and the backscatter arranged optical fiber receiving assembly can detect samples with lower concentration, weaker scattered light or higher concentration and multiple light scattering on the basis of the detection capability of the 90° optical fiber receiving assembly.

[0008] The detection method of the flow mode nanoparticle size analyzer based on dynamic and static light scattering technology, preferably, the PD detector is arranged at an angle of 90° with respect to the incident laser beam to collect the static light scattering signal, the signals of the differential refractive detector or the ultraviolet detector are combined, and the absolute molecular weight and the molecular weight distribution information of each discharged component are calculated through the Rayleigh scattering equation. The application realizes more accurate and high-resolution detection of the particle size distribution, and simultaneously obtains the molecular weight and the molecular weight distribution information of the sample.

[0009] The preferred solution of the detection method of the flow mode nanoparticle size analyzer based on dynamic and static light scattering technology is that the first data acquisition card can collect analog signals output by the differential refractive detector or the ultraviolet detector and the trigger signal of the front-end separation device, the scattering light fluctuation of each outflow component is detected by dynamic light scattering, and the particle size information is calculated, the concentration corresponding to each outflow component is calculated by the signal of the differential refractive detector or the ultraviolet detector, and the high-resolution particle size distribution information is calculated by combining the particle size information and the concentration information of the outflow component.

[0010] The preferred solution of the detection method of the flow mode nanoparticle size analyzer based on dynamic and static light scattering technology is that the second data acquisition card can collect analog signals output by the differential refractive detector or the ultraviolet detector and the trigger signal of the front-end separation device, the scattering light intensity information of each outflow component is detected by static light scattering, the concentration corresponding to each outflow component is calculated by the signal of the differential refractive detector or the ultraviolet detector, and the absolute molecular weight of each outflow component is calculated by combining the scattering light intensity information and the concentration information of the outflow component, and then the weight average molecular weight Mw, the number average molecular weight Mn, the Z-average molecular weight Mz and the molecular weight distribution information are obtained.

[0011] The preferred solution of the detection method of the flow mode nanoparticle size analyzer based on dynamic and static light scattering technology is that the static light scattering principle is used to realize uniform scattering based on sample scattering independent of angle. According to the Rayleigh scattering equation, the molecular size of the sample, the mean square rotation radius Rg, is not more than 1 / 20 of the wavelength of the laser, and it is considered to be uniform scattering. Taking 671 nm incident light as an example, the upper limit of the sample size corresponding to uniform scattering is Rg, which is not more than 33.5 nm, and the theoretical calculation value of the molecular weight of the spherical protein is about 22.2 million Da, the theoretical calculation value of the linear polysaccharide molecule is about 560 thousand Da, and the theoretical calculation value of the hyperbranched polymer is 15.53 million Da to 274 million Da.

[0012] The preferred solution of the detection method of the flow mode nanoparticle size analyzer based on dynamic and static light scattering technology is that in a test process, for suitable samples such as polymer solutions or protein solutions, dynamic light scattering and static light scattering tests can be performed at the same time to obtain high-resolution particle size distribution and molecular weight of the sample, the molecular weight includes Mw, Mn, Mz, the molecular weight distribution coefficient PD=Mw / Mn, and the actual molecular weight distribution curve information.

[0013] The detection method of the flow mode nanoparticle size analyzer based on dynamic and static light scattering technology, preferably, for a suitable sample such as a high polymer solution, the intrinsic viscosity IV of the corresponding component can be calculated by combining the particle size and molecular weight information of each component, and the Mark-Houwink curve and the Mark-Houwink α value and K value are further plotted by the intrinsic viscosity IV versus the molecular weight, so as to obtain the information of the molecular structure of the high polymer.

[0014] The detection method of the flow mode nanoparticle size analyzer based on dynamic and static light scattering technology, preferably, under the premise that the refractive index increment dn / dc and the ultraviolet absorption increment dA / dc of the sample are known, the absolute concentration of the sample in the corresponding range can also be calculated by setting the baseline and the integral range for the differential refractometer or the ultraviolet detector signal, and the concentration unit is mg / mL.

[0015] The detection method of the flow mode nanoparticle size analyzer based on dynamic and static light scattering technology, preferably, the flow sample cell has an extremely low volume (less than 30 μL), which can maximize the prevention of the diffusion effect of the sample in the flow sample cell.

[0016] The detection method of the flow mode nanoparticle size analyzer based on dynamic and static light scattering technology, preferably, the flow sample cell has a standard chromatographic tube interface, which is suitable for connecting tubes with an outer diameter of 1 / 16 inch and an inner diameter of 0.01 inch-0.04 inch.

[0017] The detection method of the flow mode nanoparticle size analyzer based on dynamic and static light scattering technology, preferably, when the dynamic light scattering technology is used for testing, it has an extremely high sampling rate, and the fastest sampling time of one data point is 0.4 seconds, that is, one particle size result of the outflow component can be obtained by testing for 0.4 seconds.

[0018] The detection method of the flow mode nanoparticle size analyzer based on dynamic and static light scattering technology, preferably, when the static light scattering technology is used for testing, it has an extremely high sampling rate, and the fastest sampling time of one data point is 0.2 seconds, that is, one molecular weight result of the outflow component can be obtained by testing for 0.2 seconds.

[0019] The detection method of the flow mode nanoparticle size analyzer based on dynamic and static light scattering technology, preferably, the data acquisition card 1 and the data acquisition card 2 can receive the trigger signal of the analog or digital signal emitted by the front-end separation device, and the testing is automatically started by the trigger signal. The time when the software receives the trigger signal is the starting time of the testing, and the total testing time is determined by the operator according to the actual sample outflow time.

[0020] Beneficial effects

[0021] 1. The device and method in the present application are suitable for use in connection with a complete front-end particle separation device-field flow fractionation system (FFF) or a polymer and protein separation device-gel permeation chromatography (GPC / SEC), wherein the separation device can separate each component according to the size of the sample components and sequentially flow out, and the theoretical resolution of the FFF and GPC / SEC separation devices is better than 1.1 times the particle or molecular size difference, and high-resolution particle size distribution test results and molecular weight distribution test results can be obtained by detecting each flow-out component. The device has good popularization and practical value, and will produce good economic and social benefits after wide popularization and application.

[0022] 2. The static light scattering test, i.e. the molecular weight test, in the present application does not need to configure a series of concentrations of samples to obtain molecular weight information by extrapolating from the detection of the net scattering light intensity of each concentration sample, but only needs to configure one sample concentration, and after sampling, the GPC / SEC is used for separation and flow-out, and the concentration information of each flow-out component is calculated from the differential refractive detector or ultraviolet detector signal in the flow path for molecular weight calculation. Not only the weight average molecular weight Mw can be obtained, but also the number average molecular weight Mn and the Z-average molecular weight Mz can be obtained, and the molecular weight distribution coefficient PD = Mw / Mn can be obtained, and the actual molecular weight distribution curve information can be obtained.

[0023] 3. The technology in the present application calculates the intrinsic viscosity IV of the corresponding flow-out component for suitable samples such as polymer solutions, and further plots the intrinsic viscosity IV against the molecular weight to obtain the Mark-Houwink curve and the Mark-Houwink α value and K value, so as to obtain information such as molecular density and branching degree of the molecular structure of the polymer.

[0024] 4. The present application is widely used in the research and application fields of biopharmaceuticals, high polymer materials, food, agricultural scientific research, electronics, environment, instruments and meters, etc. BRIEF DESCRIPTION OF DRAWINGS

[0025] Figure 1 It is an electrical principle block diagram of a flow mode nanoparticle size analyzer based on dynamic and static light scattering technology;

[0026] Figure 2 It is a structure schematic diagram of the present application and a front-end separation device;

[0027] Figure 3 It is a schematic diagram of 90° light path dynamic light scattering test and 90° light path static light scattering test;

[0028] Figure 4 It is a schematic diagram of back light path dynamic light scattering test and 90° light path static light scattering test;

[0029] Figure 5 Schematic diagrams of the original dynamic light scattering results and the calculated particle size distribution results.

[0030] Figure 6 Schematic diagrams of static light scattering results and calculated molecular weight results;

[0031] Figure 7 This is a schematic diagram of the correlation curves for dynamic light scattering;

[0032] Figure 8 Schematic diagram of the flow sample cell;

[0033] Figure 9 This is a Mark-Houwink curve.

[0034] In the figure: 1-Laser, 2-Fiber optic cable, 3-Flow sample cell, 4-Flow sample cell inlet, 5-Optical trap, 6-Sample, 7-90° angular scattered light, 8-PD detector, 9-PD signal transmission line, 10-Flow sample cell outlet, 11-Backscattered light, 12-Focusing lens, 13-Fiber optic support, 14-Motor bearing. Detailed Implementation

[0035] The invention will now be further described with reference to the accompanying drawings.

[0036] like Figure 1 As shown, the present invention provides a flow-mode nanoparticle size analyzer based on dynamic and static light scattering technology, including a flow sample cell 3, an APD detector and a PD detector 8 connected to an optical fiber 2, a laser 1, a focusing lens 12, a first data acquisition card, and a second data acquisition card. The laser 1 emitted from the laser irradiates the sample 6 in the flow sample cell 3 through the focusing lens. The APD detector and the PD detector 8 connected to the optical fiber 2 simultaneously receive the scattered light from the sample and transmit the signals to the computer through the first data acquisition card and the second data acquisition card, respectively.

[0037] like Figure 3 and Figure 4 As shown, the APD detector is used for dynamic light scattering testing. It receives the sample scattered light through an optical fiber 2 connected to it. The optical fiber 2 is mounted on the optical fiber support 13 and positioned on one side of the scattered light 7 at a 90° angle. Figure 3 ), or facing away from ( Figure 4 The APD signal is transmitted to the computer through the first data acquisition card; the PD detector 8 is used for static light scattering test and is set on one side of the laser beam at a 90° angle. The PD signal is transmitted to the computer through the second data acquisition card via the PD signal transmission line 9.

[0038] like Figure 2The nano particle size analyzer in the present application is applicable to be connected with a complete front-end particle separation device-field flow fractionation system FFF or a polymer and protein separation device-gel permeation chromatography GPC / SEC, wherein the front-end separation device comprises at least one differential refractive detector or one ultraviolet detector. The front-end separation device can be used for sample injection, and the sample can be separated into each component in the flow process through the FFF field flow separation channel or the gel permeation chromatography column according to the size of the sample components, and the separated sample components flow out in sequence, and pass through the differential refractive detector or the ultraviolet detector and the nano particle size analyzer in the present application in sequence. The trigger signal of the front-end separation device and the analog signal of the output of the differential refractive detector or the ultraviolet detector can be input into the nano particle size analyzer in the present application, collected through the first data acquisition card or the second data acquisition card, transmitted to the software of the nano particle size analyzer in the present application, and used for calculation. The front-end chromatography pump and the automatic sampler are directly communicated with the PC terminal software, and used for controlling the flow rate of the chromatography pump and the sample injection.

[0039] As shown in Figure 5 , in the dynamic light scattering test in the flow mode, the APD detector is used to collect the sample scattering light fluctuation signal, and the differential refractive detector or the ultraviolet detector signal is collected at the same time. The correlation calculation is performed on the scattering light fluctuation signal with time in a certain time period (the fastest 0.4 seconds per period, and one period is usually not more than 10 seconds), to obtain the correlation curve of the sample outflow components flowing through the nano particle size analyzer in the period, and the corresponding particle size d i information is calculated through the cumulative method. The baseline setting is performed on the differential refractive detector or the ultraviolet detector signal, the actual detected response signal value is subtracted by the baseline value corresponding to the outflow volume, to obtain the net response value of the signal, and the sample concentration information C i under the corresponding particle size can be calculated in combination with the dn / dc (differential refractive detector) or dA / dc (ultraviolet detector) of the sample. A group of particle sizes and the corresponding concentration data [C i , d i ] are plotted with the particle size as the horizontal coordinate and the concentration (or the relative concentration) as the vertical coordinate, to obtain the particle size distribution curve of the sample. The integral range of the outflow volume can also be set through the particle size analyzer software, the particle size distribution in the integral range is calculated, and the total concentration of the sample in the integral range is obtained through the concentration C i .

[0040] As shown in Figure 7 , it is a normalized correlation curve schematic diagram in the dynamic light scattering test through the method of the present application.

[0041] As shown in Figure 6As shown, in the static light scattering test under flow mode, a PD detector 8 is used to collect the intensity signal of the scattered light from the sample, and simultaneously, signals from a differential refractive index detector (DRID) or an ultraviolet (UV) detector are collected. The static light scattering light collection frequency is 1-5 Hz (as fast as 0.2 seconds per point), and the collection frequency of the DID or UV detector signal is the same as the static light scattering signal collection frequency. After the test, baseline and integration settings are performed for the static light scattering signal and the DID or UV detector signal to define the region to be calculated. By subtracting the baseline value of the corresponding effluent volume from the actual detected response signal value, the net response value of the signal is obtained. Combined with the sample's dn / dc (DRID) or dA / dc (UV detector), the concentration information C of the sample at the corresponding particle size can be calculated. i , will C i Substituting into the Rayleigh scattering equation and combining it with the scattered light intensity LS at the corresponding outflow volume... i The molecular weight M of the effluent component corresponding to the effluent volume is obtained. i A set of molecular weights and their corresponding concentration data [C] i M i Plotting molecular weight on the x-axis and concentration (or relative concentration) on the y-axis yields the molecular weight distribution curve of the sample. This can also be calculated using the following formula.

[0042]

[0043]

[0044]

[0045] Calculate the number-average molecular weight M n Weight-average molecular weight M w Z-mean average molecular weight M z and molecular weight distribution PD=M w / M n The particle size analyzer software can also be used to set the integration range of the effluent volume, calculate the molecular weight distribution within the integration range, and determine the concentration C. i The total concentration of the sample within the integration range is obtained by summing the concentrations.

[0046] like Figure 8 As shown, the flow-through sample cell 3 has a four-sided light-transmitting structure. Scattered light can be emitted from both sides at a 90° angle (7) and backscattered light (11) can be emitted from the back. The sample flows in through the inlet 4 and out through the outlet 10. The flow-through sample cell 3 has a very low volume, not exceeding 30 μL, which can minimize the impact of diffusion effects on detection resolution. This flow-through sample cell is compatible with all tubing with an outer diameter of 1 / 16 inch and an inner diameter of 0.01-0.04 inches.

[0047] As Figure 9 shown, the intrinsic viscosity IV of a component can be calculated using the formula IV = (5 / 12) • (N A • π • D i 3 / M i ) in combination with the particle size D i and molecular weight M i information of the component, where N A is Avogadro's constant. Further, the Mark-Houwink curve can be obtained by plotting the intrinsic viscosity IV against the molecular weight. The Mark-Houwink α value and K value can be obtained by fitting the curve using the formula IV = KM α , thus obtaining the information of the molecular structure of the polymer.

Claims

1. A method of detection for a flow mode nanoparticle sizer based on dynamic and static light scattering techniques, characterized by: The nanometer particle size analyzer is connected with a complete front-end particle separation device, a field flow fractionation system (FFF) or a polymer and protein separation device, a gel permeation chromatography (GPC / SEC), wherein the front-end separation device comprises at least one differential refractive detector or one ultraviolet detector, each component is separated according to the size of the sample component and flows out in sequence; the nanometer particle size analyzer comprises a flow-through sample cell, an APD detector for dynamic light scattering technology, a PD detector for static light scattering technology, a laser, a focusing lens, a first data acquisition card and a control unit, a second data acquisition card and a control unit, wherein the laser emitted by the laser irradiates the sample in the flow-through sample cell through the focusing lens, the two detectors simultaneously receive the scattered light of the sample, and the signals are transmitted to the control units of the first data acquisition card and the second data acquisition card respectively. The 90° or backscattering light fiber receiving assembly connected with the APD detector collects the dynamic light scattering fluctuation signal, calculates the correlation curve, calculates the diffusion coefficient of the sample particles, obtains the particle size of each flow-out component through the Stokes-Einstein equation, and obtains the high-resolution particle size distribution independent of the calculation model in combination with the concentration signal obtained by the differential refractive detector or the ultraviolet detector; wherein the 90° light fiber receiving assembly is suitable for detecting samples with moderate concentration range, strong scattering light intensity and no multiple light scattering, and the backscattering light fiber receiving assembly is used for detecting samples with low concentration, weak scattering light or high concentration and multiple light scattering on the basis of the detection capability of the 90° light fiber receiving assembly. The PD detector is arranged at the 90° laser beam to collect the static light scattering signal, and the absolute molecular weight and molecular weight distribution information of each flow-out component are calculated through the Rayleigh scattering equation in combination with the signal of the differential refractive detector or the ultraviolet detector; the more accurate and high-resolution detection of the particle size distribution is realized, and the molecular weight and molecular weight distribution information of the sample are obtained at the same time.

2. The method of claim 1, wherein the method is a method of detecting a flow mode nanoparticle sizer based on dynamic and static light scattering techniques. The first data acquisition card collects the analog signals output by the differential refractive detector or the ultraviolet detector and the trigger signals of the front-end separation device, detects the scattering light fluctuation of each flow-out component by dynamic light scattering, and calculates the particle size information; the concentration corresponding to each flow-out component is calculated by the signal of the differential refractive detector or the ultraviolet detector, and the high-resolution particle size distribution information is calculated in combination with the particle size information and the concentration information of the flow-out component. The second data acquisition card collects the analog signals output by the differential refractive detector or the ultraviolet detector and the trigger signals of the front-end separation device, detects the scattering light intensity information of each flow-out component by static light scattering, calculates the concentration corresponding to each flow-out component by the signal of the differential refractive detector or the ultraviolet detector, and calculates the absolute molecular weight of each flow-out component in combination with the scattering light intensity information and the concentration information of the flow-out component, and then obtains the weight average molecular weight Mw, the number average molecular weight Mn, the Z-average molecular weight Mz and the molecular weight distribution information.

3. The method of claim 1, wherein the method is a method of detecting a flow mode nanoparticle sizer based on dynamic and static light scattering techniques. The static light scattering principle is based on uniform scattering of sample scattering independent of angle; according to Rayleigh scattering equation, the molecular size - mean square radius of gyration Rg of the sample is not more than 1 / 20 of the wavelength of laser, that is, it is considered as uniform scattering.

4. The method of claim 1, wherein the method is a method of detecting a flow mode nanoparticle sizer based on dynamic and static light scattering techniques. In a test process, for suitable samples, high polymer solution or protein solution, dynamic light scattering and static light scattering test are carried out at the same time, and high resolution particle size distribution and molecular weight of the sample including Mw, Mn, Mz and molecular weight distribution information are obtained; The intrinsic viscosity IV of the corresponding component is calculated by combining the particle size and molecular weight information of each component, and the Mark-Houwink curve and Mark-Houwink a value and K value are obtained by plotting the intrinsic viscosity IV against the molecular weight, so as to obtain the molecular structure information of the high polymer.

5. The method of claim 1, wherein the method is a method of detecting a flow mode nanoparticle sizer based on dynamic and static light scattering techniques. Under the premise that the refractive index increment dn / dc and ultraviolet absorption increment dA / dc of the sample are known, the absolute concentration of the sample in the corresponding range is calculated by setting the baseline and integration range for the differential refractive detector or ultraviolet detector signal, and the concentration unit is mg / mL.

6. The method of claim 1, wherein the method is a method of detecting a flow mode nanoparticle sizer based on dynamic and static light scattering techniques. When the flow sample cell volume is less than 30 μL, the diffusion effect of the sample in the flow cell can be maximally prevented; The flow sample cell has a standard chromatographic pipe interface, which is suitable for connecting various pipes with an outer diameter of 1 / 16 inch and an inner diameter of 0.01 inch-0.04 inch.

7. The method of claim 1, wherein the method is a method of detecting a flow mode nanoparticle sizer based on dynamic and static light scattering techniques. When dynamic light scattering technology is used for testing, the sampling rate is high, and the fastest sampling time of one data point is 0.4 seconds, that is, the particle size result of one outflow component is obtained by testing for 0.4 seconds. When static light scattering technology is used for testing, the sampling rate is high, and the fastest sampling time of one data point is 0.2 seconds, that is, the molecular weight result of one outflow component is obtained by testing for 0.2 seconds.

8. The method of claim 1, wherein the method is a method of detecting a flow mode nanoparticle sizer based on dynamic and static light scattering techniques. The first data acquisition card and the second data acquisition card both receive the analog or digital signal trigger signal sent by the front-end separation equipment, and automatically start testing by the trigger signal command; wherein the time when the software receives the trigger signal is the test start time, and the total test time is determined by the operator according to the actual sample outflow time.

Citation Information

Patent Citations

  • Flow mode nanometer particle size analyzer based on dynamic and static light scattering technology

    CN219694830U