# US 11,906,412 B2 · Particle characterisation

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- Number: US 11,906,412 B2
- Document ID: US11906412B2
- Status: Granted
- Kind: B2
- Application number: 17/531,021
- Filed: 2021-11-19
- Published: 2022-10-13
- Granted: 2024-02-20
- Earliest claimed: 2017-03-23
- Assignees: Malvern Panalytical Limited
- Applicants: Malvern Panalytical Limited
- Inventors: Jason Corbett; Alex Malm
- Web page: https://patentgrep.com/patent/US11906412B2

## CPC

- G01N 15/0211: {Investigating a scatter or diffraction pattern}
- G01N 2015/0053: {in liquids, e.g. trouble}
- G01N 2015/0222: {from dynamic light scattering, e.g. photon correlation spectroscopy}
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)

## 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

### Claim 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.

### Claim 2 (depends on 1)

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.

### Claim 3 (depends on 2)

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

### Claim 4 (depends on 3)

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

### Claim 5 (depends on 4)

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

### Claim 6 (depends on 2)

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

### Claim 7 (depends on 1)

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.

### Claim 8 (depends on 1)

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.

### Claim 9 (depends on 1)

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.

### Claim 10 (depends on 9)

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

### Claim 11 (depends on 9)

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

### Claim 12 (depends on 11)

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

### Claim 13 (depends on 12)

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

### Claim 14 (depends on 9)

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

### Claim 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.
