Method and equipment for the characterization of suspensions

• US 6,029,507 A
• Filed: 04/10/1997
• Issued: 02/29/2000
• Est. Priority Date: 04/10/1996
• Status: Expired due to Term

• Current Assignee: Nederlandse Organisatie Voor Toegepast-Natuurwetenschappelijk Onderzoek Tno
• Original Assignee: Nederlandse Organisatie Voor Toegepast-Natuurwetenschappelijk Onderzoek Tno
• Inventors: Faber, Gerard, De Kroon, Mathilde Gertrudis Maria, Vos, Hugo Cornelis Lucas
• Primary Examiner(s): Williams, Hezron
• Assistant Examiner(s): FAYYAZ, NASHMIYA SAQIB
• Application Number:
  US08/834,049
• Time in Patent Office: 1,055 Days
• Field of Search: 73/61.75, 73/64.53, 73/865.5, 73/866, 73/597, 73/629, 73/599, 73/602, 73/600, 73/614
• US Class Current: 73/61.75
• CPC Class Codes: G01N 15/02 Investigating particle size or size distribution by measuring osmotic pressure G01N7/10; investigating sedimentation of particle suspensions G01N15/04; investigating individual particles G01N15/10
• CPC Class Codes: G01N 2291/015 Attenuation, scattering
• CPC Class Codes: G01N 2291/02408 Solids in gases, e.g. particle suspensions
• CPC Class Codes: G01N 2291/02416 Solids in liquids
• CPC Class Codes: G01N 2291/02818 Density, viscosity
• CPC Class Codes: G01N 2291/044 Internal reflections (echoes), e.g. on walls or defects
• CPC Class Codes: G01N 29/032 by measuring attenuation of acoustic waves
• CPC Class Codes: G01N 29/11 by measuring attenuation of acoustic waves
• CPC Class Codes: G01N 29/2456 Focusing probes focusing arrangements G01N29/221
• CPC Class Codes: G01N 29/40 by amplitude filtering, e.g. by applying a threshold or by gain control
• CPC Class Codes: G01N 29/4427 with stored values, e.g. threshold values
• CPC Class Codes: G01N 29/4472 Mathematical theories or simulation
• CPC Class Codes: G01N 29/52 using inversion methods other that spectral analysis, e.g. conjugated gradient inversion

Abstract

Method and equipment for the detection and identification of particles in a suspension with the aid of acoustic signals, directed at at least one measurement volume within the suspension, via reception of acoustic reflection signals, conversion of the acoustic reflection signals into electrical reflection signals, counting the number of electrical reflection signals which have an amplitude in excess of a predetermined value and converting the count into numbers of particles which are larger than a certain size, at least one curve being composed on the basis of a cumulative count of the number of reflection signals which have an amplitude in excess of a specific value as a function of the amplitude and the at least one curve being compared with predetermined standard cumulative count curves and material properties, particle concentration, particle size distribution and/or particle characteristics, such as particle shape, particle size and standard deviation thereof, are deduced from the comparison.

Claims

1. A method for the detection and identification of particles in a suspension, comprising the following steps:

a. generation of acoustic signals having the form of a beam along a predetermined axis using an acoustic source;

b. directing the acoustic signals at at least one measurement volume within the suspension, said at least one measurement volume having axial boundaries defined as boundaries in an axial direction of said axis, and lateral boundaries defined as boundaries in a direction lateral to said axis, said axial boundaries being defined with the aid of time windows;

c. reception of acoustic reflection signals produced by reflection of the acoustic signals by the particles in the at least one measurement volume;

d. conversion of the acoustic reflection signals into electrical reflection signals;

e. counting numbers of electrical reflection signals which have an amplitude value in excess of at least one predetermined threshold and conversion thereof into numbers of particles which are larger than a certain size;

wherein the method also comprises the following steps;

f. composing at least one cumulative count curve showing for each amplitude value the number of electrical reflection signals having amplitude values in excess of said each amplitude value;

g. comparison of the at least one cumulative count curve with predetermined standard cumulative count curves and deduction of at least one feature selected from the group consisting of material properties, particle concentration, particle shapes, particle size and standard deviation thereof and particle size distribution;

the standard cumulative count curves being derived with at least the following steps;

derivation of a probability density function for plural amplitude values of the electrical reflection signals within the measurement volume as a function of a given particle shape, and particle size distribution thereof, and

derivation of the standard cumulative count curves from the probability density function for the plural amplitude values.

2. A method according to claim 1, wherein derivation of the standard cumulative count curves also includes the step of:

definition of the lateral boundaries of the at least one measurement volume as being the boundaries beyond which amplitudes of the electrical reflection signals are smaller than a predetermined noise level.

3. A method according to claim 1, wherein the following equation is used for the probability density function for the amplitude values:

space="preserve" listing-type="equation">p(A)=∫

g(A|D) h(D) dD

where;

g(A|D)=probability density function for measured amplitude A of an electrical reflection signal originating from an arbitrary particle having a diameter D;

h(D)=probability density function for particle diameter D,

the equation being integrated between two predetermined limits for the particle diameter D.

4. A method according to claim 3, wherein, for detecting a particle in the measurement volume, a Gaussian amplitude profile of the acoustic signals in a first direction in the measurement volume lateral to said axis and a substantially negligible amplitude variation in the acoustic signals in a second direction in the measurement volume parallel to said axis are assumed for determination of g(A|D), resulting in the relation:

##EQU10## where A_n =noise level, A_o is the amplitude which would be detected from said particle if said particle where located on the axis.

5. A method according to claim 1, wherein standard cumulative count curves are determined experimentally with the aid of suspensions containing particles of a pre-known shape, size and standard deviation of the size.

6. A method according to claim 1 where the particle concentration is calculated from the number of electrical reflection signals with amplitude values above a predetermined noise level.

7. A method according to claim 6, where the calculated particle concentration is corrected for the fact that smaller particles cannot be detected through the whole measurement volume, resulting in a true particle concentration.

8. A method according to claim 7, wherein, for detecting a particle in the measurement volume, a Gaussian amplitude profile of the acoustic signals in a first direction in the measurement volume lateral to said axis and a substantially negligible amplitude variation in the acoustic signals in a second direction in the measurement volume parallel to said axis are assumed for correcting said calculated particle concentration, resulting in the following relation for the true particle concentration C:

##EQU11## where;

A=measured amplitude of an electrical reflection signal

A_n =noise level

N( . . . ) gives the number of measurements for which the condition given in brackets applies, N_tot is the total number of measurements, V_meas is the measurement volume, ε

is a normalizing factor and q_true is a true particle size distribution.

9. A method according to claim 1, wherein said beam is focussed in a focus and the measurement volume is chosen to be around the focus of the acoustic beam and to be so small that the likelihood of the presence of more than one particle in the measurement volume during a measurement is negligibly small.

10. A method according to claim 1, wherein

in step a, the acoustic beam generated is a focussed beam and has such a large aperture, and the time which elapses between two successive measurements is so short, that each particle is exposed several times while passing through the beam and that, depending on the position of a particle lateral to said axis in the measurement volume, a varying angle-dependent reflection of the acoustic signals is produced;

prior to step f, one or more different types of particles present in the suspension are identified on the basis of a series of angle-dependent reflection signals received successively over time;

when composing the curve in step f, the maximum value of each amplitude value of said series of successive angle-dependent reflection signals, received over time, from a detected particle from the one or more types is taken as the amplitude of the electrical signals, which are produced after conversion of the acoustic reflection signals from said detected particle.

11. A method according to claim 10, wherein in step a, the focused acoustic beam with a predetermined focus is generated and in step b the focus remains outside the measurement volume.

12. A method according to claim 10, wherein an acoustic source having dimensions smaller than the wavelengths of the generated acoustic signals is used.

13. A method according to claim 1, wherein the acoustic signals comprise sound signals having a frequency of 10-40 MHz.

14. A method according to claim 13, wherein the acoustic signals comprise sound signals having a frequency of 20-30 MHz.

15. Equipment for the detection and identification of particles in a suspension, comprising:

a. an acoustic source for the generation of acoustic signals;

b. means for directing the acoustic signals at at least one measurement volume within the suspension, each measurement volume having axial boundaries defined as boundaries in an axial direction of said axis, and lateral boundaries defined as boundaries in a direction lateral to said axis, said axial boundaries being defined with the aid of time windows;

c. means for receiving acoustic reflection signals produced by reflection of the acoustic signals by the particles in the at least one measurement volume;

d. means for converting the acoustic reflection signals into electrical reflection signals;

e. means for counting numbers of electrical reflection signals which have an amplitude value in excess of at least one predetermined threshold and for converting said counted numbers into numbers of particles which are larger than a certain size;

wherein the equipment also comprises;

f. means for composing at least one cumulative count curve showing for each amplitude value the number of electrical reflection signals having amplitude values in excess of said each amplitude value;

g. means for comparing the at least one cumulative count curve with predetermined standard cumulative count curves and for deducing at least one feature from a set of features comprising;

material properties, particle concentration, particle shapes, particle size and standard deviation thereof and particle size distribution;

the standard cumulative count curves being derived with at least the following steps;

derivation of a probability density function for plural amplitude values of the electrical reflection signals within the measurement volume as a function of a given particle shape, and particle size distribution thereof, and

derivation of the standard cumulative count curves from a probability density function for the plural amplitude values.

16. Equipment according to claim 15, wherein

during operation, the acoustic source generates an acoustic beam which is focussed and has such a large aperture, and makes the time which elapses between two successive measurements so short, that each particle is exposed several times while passing through the beam and that, depending on the position of the particles lateral to said axis in the measurement volume, a different angle-dependent reflection of the acoustic signals is produced;

identification means are also present for identification of one or more different groups of particles present in the suspension on the basis of a series of successive angle-dependent reflection signals received over time;

the means for composing the at least one cumulative count curve compose the at least one cumulative count curve, the maximum value of the amplitude values of said series of successive angle-dependent reflection signals, received over time, from a detected particle being taken as the amplitude value of the electrical signals, which are produced after conversion of the acoustic reflection signals from said detected particle.