IP Library Granted Patent US 11,906,412
Granted Patent B2
US 11,906,412 · App. 17/531,021 · Granted Feb 20, 2024

Particle characterisation

Inventors: Jason Corbett (Malvern, GB); Alex Malm (Malvern, GB)
Assignee: Malvern Panalytical Limited
G01N15/0211G01N2015/0222
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Quick Facts
Patent No.
US 11,906,412
App. No.
17/531,021
Granted
Feb 20, 2024
Kind
B2
Abstract

A method of characterising particles in a sample, comprising: obtaining a scattering measurement comprising a time series of measurements of scattered light from a detector, the scattered light produced by the interaction of an illuminating light beam with the sample; producing a corrected scattering measurement, comprising compensating for scattering contributions from contaminants by reducing a scattering intensity in at least some time periods of the scattering measurement; determining a particle characteristic from the corrected scattering measurement.

Claims (28)

1. A method of characterising particles in a sample, comprising:

obtaining a plurality of scattering measurements, each scattering measurement comprising a time series of measurements of scattered light from a detector, the scattered light produced by the interaction of an illuminating light beam with the sample;

identifying contaminated scattering measurements, in which a contaminant was contributing to the scattered light; and

determining a particle characteristic from scattering measurements that have not been identified as contaminated scattering measurements by:

determining an autocorrelation function for each scattering measurement that has not been identified as a contaminated scattering measurement;

combining the autocorrelation functions to produce an average autocorrelation function from which the particle characteristic is derived.

2. The method of claim 1 , wherein identifying contaminated scattering measurements comprises identifying scattering measurements within a predetermined time window from a time when the scattered light intensity exceeds a threshold.

3. The method of claim 2 , wherein the threshold is determined after a measurement.

4. The method of claim 3 , wherein the threshold is determined from the ensemble characteristics of the scattering measurements.

5. The method of claim 4 , wherein the threshold is derived from an average intensity taken across the scattering measurements.

6. The method of claim 2 , wherein the threshold is determined dynamically as the measurements are taken.

7. The method of claim 1 , wherein identifying contaminated scattering measurements comprises identifying scattering measurements within a predetermined time window from a time when fluctuations in the time series of measurements have a frequency below a cut-off frequency.

8. The method of claim 1 , wherein identifying contaminated scattering measurements comprises identifying scattering measurements within a predetermined time window from a time when the scattered light intensity exceeds a threshold and fluctuations in the time series of measurements have a frequency below a cut-off frequency.

9. The method of claim 1 , wherein identifying contaminated scattering measurements comprises; partitioning the scattering measurements, determining a comparative particle characteristic for each partitioned portion, and identifying partitioned portions where the comparative particle characteristic exceeds a threshold.

10. The method of claim 9 , wherein the comparative particle characteristic is particle size.

11. The method of claim 9 , wherein the comparative particle characteristic is polydispersity index.

12. The method of claim 11 , wherein the threshold is determined from a best fit normal distribution.

13. The method of claim 12 , wherein the threshold is three standard deviations from the average value determined from the best fit normal distribution.

14. The method of claim 9 , wherein the plurality of measurements is taken until a convergence criterion is met.

15. An apparatus for characterising particles, comprising: a light source, a sample cell, a detector and a processor; wherein

the light source is operable to illuminate a sample within the sample cell with a light beam so as to produce scattered light by interactions of the light beam with the sample;

the detector is configured to detect the scattered light and produce a time series of measurements; and

the processor is configured to:

obtain a scattering measurement comprising a time series of measurements of the scattered light from the detector;

identify contaminated scattering measurements, in which a contaminant was contributing to the scattered light; and

determine a particle characteristic from scattering measurements that have not been identified as contaminated scattering measurements by:

determining an autocorrelation function for each scattering measurement that has not been identified as a contaminated scattering measurement;

combining the autocorrelation functions to produce an average autocorrelation function from which the particle characteristic is derived.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 11, 2025
From: CORBETT, JASON; MALM, ALEX
To: MALVERN PANALYTICAL LIMITED
Reel/Frame 070181/0961 →
Priority Claims (1)
EP 17162676 · Mar 23, 2017 · regional
Continuity (2)
Continuation 16496027
Related Publication 20220326128A1 · Oct 13, 2022