IP Library Granted Patent US 11,237,106
Granted Patent B2
US 11,237,106 · App. 16/434,571 · Granted Feb 1, 2022

Dynamic light scattering based microrheology of complex fluids with improved single-scattering mode detection

Inventors: Samiul Amin (Westfield, NJ); Carlos Alberto Rega (Worcestershire, GB)
Assignee: Malvern Panalytical Limited
G01N21/51G01N11/00G01N15/1436G01N21/03G01N2011/008G01N2021/0346G01N2021/4707G01N2021/4709G01N2021/513G01N2201/08
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Quick Facts
Patent No.
US 11,237,106
App. No.
16/434,571
Granted
Feb 1, 2022
Kind
B2
Abstract

A fluid characterization measuring instrument is disclosed that comprises a sample vessel for a bulk complex sample fluid having a capacity that is substantially larger than a domain size of the complex sample fluid and that is sufficiently large to cause bulk scattering effects to substantially exceed surface effects for the complex fluid sample, a coherent light source positioned to illuminate the bulk complex sample fluid in the sample vessel and a first fibre having a first end positioned to receive backscattered light from the sample after it has interacted with the sample. The first fibre can also be positioned close enough to an optical axis of the coherent light source and to the sample vessel to substantially decrease a contribution of multiply scattered light in the backscattered light. The instrument can further comprise a first photon-counting detector positioned to receive the backscattered light from a second end of the fibre, correlation logic responsive to the first photon-counting detector and single-scattering fluid property analysis logic responsive to the correlation logic and operative to derive at least one fluid property for the sample fluid.

Claims (37)

1. A fluid characterization measuring instrument, comprising:

a sample vessel for a sample fluid,

a coherent light source positioned to illuminate the sample fluid in the sample vessel with coherent light,

a first photon-counting detector that produces electronic pulses for each photon detected and is positioned to receive a first portion of the coherent light from the coherent light source scattered by the sample,

a second photon-counting detector that produces electronic pulses for each photon detected and is positioned to receive a second portion of the coherent light from the coherent light source scattered by the sample,

cross-correlation logic responsive to pulses from the first photon-counting detector and to pulses from the second photon-counting detector, and

single-scattering fluid property analysis software running on a processor and responsive to the cross-correlation logic and operative to derive at least one fluid property for the sample fluid in the fluid vessel from a cross-correlation signal from the cross-correlation logic resulting from cross correlation of the pulses from the first photon-counting detector and the pulses from the second photon-counting detector.

2. The instrument of claim 1 wherein the instrument is constructed and adapted to allow the first and/or second photon-counting detector to allow scattered light to be detected over a range of different angles ranging from 173° to 13.5°.

3. The instrument of claim 1 wherein the instrument is constructed and adapted to allow the first and/or second photon-counting detector to be further responsive to forward scattered light.

4. The instrument of claim 1 further comprising a beam splitter that splits the coherent light source into first and second light source portions.

5. The instrument of claim 1 wherein the first photon-counting detector is positioned to receive the scattered light through a first optical fiber and the second photon-counting detector is positioned to receive the scattered light through a second optical fiber.

6. The instrument of claim 1 wherein the sample vessel is a capillary tube.

7. A viscoelasticity measuring method, including the steps of:

illuminating a sample fluid with coherent light,

detecting photons from a first portion of the coherent light that has been scattered by the sample, wherein the step of detecting from a first portion of scattered coherent light received from the sample includes producing electronic pulses for each photon detected,

detecting photons from a second portion of the coherent light that has been scattered by the sample, wherein the step of detecting from a second portion of scattered coherent light received from the sample includes producing electronic pulses for each photon detected,

performing a cross-correlation operation between pulses from a first detection signal representative of the backscattered photons in the first portion and pulses from a second detection signal representative of the backscattered photons in the second portion, and

deriving at least one fluid property for the sample fluid from results of the cross-correlation operation for the sample fluid based on single-scattering analysis from a cross-correlation signal from the cross-correlation operation between the pulses from the first photon-counting detector and the pulses from the second photon-counting detector.

8. The method of claim 7 wherein the cross-correlation operation is an autocorrelation operation.

9. The method of claim 7 wherein scattered light is detected over a range of different angles ranging from 173° to 13.5° and wherein the steps of performing a cross-correlation operation and deriving are performed for the light detected over a range of angles.

10. The method of claim 7 wherein steps of detecting are carried out in both backscattering mode and forward transmission mode in order to obtain an extended region of frequency response.

11. The method of claim 7 wherein steps of detecting are carried out using a range of different probe sizes ranging from 30 nm to 1 μm in order to extend obtained frequency and/or minimise multiple scattering by adjusting volume of required probe particles.

12. The method of claim 7 wherein steps of detecting are carried out using a range of different probe chemistries to minimise interactions with the complex fluid of interest.

13. The method of claim 7 wherein illuminating the sample fluid with coherent light comprises splitting a coherent light source into first and second light source portions.

14. The method of claim 7 wherein illuminating the sample fluid with coherent light comprises illuminating the sample fluid with coherent light from first and second light sources.

15. A fluid characterization measuring instrument, comprising:

a sample vessel for a sample fluid,

a first coherent light source positioned to illuminate the sample fluid in the sample vessel with coherent light,

a second coherent light source positioned to illuminate the sample fluid in the sample vessel with coherent light,

a first photon-counting detector that produces electronic pulses for each photon detected and is positioned to receive a first portion of scattered coherent light received from the sample,

a second photon-counting detector that produces electronic pulses for each photon detected and is positioned to receive a second portion of scattered light received from the sample,

cross-correlation logic responsive to pulses from the first photon-counting detector and to pulses from the second photon-counting detector, and

single-scattering fluid property analysis software running on a processor and responsive to the cross-correlation logic and operative to derive at least one fluid property for the sample fluid in the fluid vessel from a cross-correlation signal from the cross-correlation logic resulting from cross correlation of the pulses from the first photon-counting detector and the pulses from the second photon-counting detector, wherein the single-scattering fluid property analysis software is operative to derive the fluid property from thermally driven motion of probe particles suspended in the sample fluid.

16. The instrument of claim 15 wherein the instrument is constructed and adapted to allow the first and/or second photon-counting detector to allow scattered light to be detected over a range of different angles ranging from 173° to 13.5°.

17. The instrument of claim 15 wherein the instrument is constructed and adapted to allow the first and/or second photon-counting detector to be further responsive to forward scattered light.

18. The instrument of claim 15 wherein the first photon-counting detector is positioned to receive the scattered light through a first optical fiber and the second photon-counting detector is positioned to receive the scattered light through a second optical fiber.

19. The instrument of claim 15 wherein the single-scattering fluid property analysis software is operative to derive an elastic modulus and a viscous modulus of the sample fluid from the correlation function based on single-scattering analysis.

Assignments (3)
CHANGE OF NAME Recorded Jan 7, 2020
From: MALVERN INSTRUMENTS LTD
To: MALVERN PANALYTICAL LIMITED
Reel/Frame 051442/0258 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 6, 2020
From: AMIN, SAMIUL
To: MALVERN INSTRUMENTS, LTD
Reel/Frame 051428/0269 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 6, 2020
From: REGA, CARLOS
To: MALVERN INSTRUMENTS, LTD
Reel/Frame 051428/0345 →
Continuity (4)
Continuation 15013084 · Feb 2, 2016
Continuation 13390915
Provisional Application 61274480 · Aug 17, 2009
Related Publication 20200096443A1 · Mar 26, 2020