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WO1996042006A2 - Systeme et procede de caracterisation de particules a angles longueurs d'onde multiples - Google Patents

Systeme et procede de caracterisation de particules a angles longueurs d'onde multiples Download PDF

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Publication number
WO1996042006A2
WO1996042006A2 PCT/US1996/010342 US9610342W WO9642006A2 WO 1996042006 A2 WO1996042006 A2 WO 1996042006A2 US 9610342 W US9610342 W US 9610342W WO 9642006 A2 WO9642006 A2 WO 9642006A2
Authority
WO
WIPO (PCT)
Prior art keywords
sample
system recited
light energy
particle
spectrophotometer
Prior art date
Application number
PCT/US1996/010342
Other languages
English (en)
Other versions
WO1996042006A3 (fr
Inventor
Luis Humberto Garcia-Rubio
Original Assignee
University Of South Florida
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by University Of South Florida filed Critical University Of South Florida
Priority to AU63854/96A priority Critical patent/AU6385496A/en
Priority to JP9503355A priority patent/JPH11507735A/ja
Publication of WO1996042006A2 publication Critical patent/WO1996042006A2/fr
Publication of WO1996042006A3 publication Critical patent/WO1996042006A3/fr

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/02Investigating particle size or size distribution
    • G01N15/0205Investigating particle size or size distribution by optical means
    • G01N15/0211Investigating a scatter or diffraction pattern

Definitions

  • the present invention relates to particle characterization and detection techniques and systems and, more particularly, to characterization and detection systems and methods using the light scattering and absorption properties of a particle.
  • Absorption spectroscopy is usually conducted in the spectral region in which scattering effects can be minimized. Absorption data are used to estimate particle concentration and chemical density and composition.
  • This equation (1) is the fundamental equation for the scattering of unpolarized light by nonabsorbing monodisperse polymer molecules in solution.
  • the refractive index of the solution n and the specific refractive index increments dn/dc are inversely proportional to the wavelength ⁇ , generally increasing the contrast and, therefore, the sensitivity of light scattering measurements as the wavelength is decreased. Furthermore, at a given angle ⁇ the ratio
  • Eq. (1) has to be corrected by the form factor P( ⁇ ) :
  • the form factor can be expressed in terms of the root-mean-square radius of gyration R g :
  • I s 2 ⁇ 2 Fn. ( dn/dc) 1 2 C(1 + cos 2 _>) .C (7)
  • V represents the volume of the molecule.
  • Eqs. (8) and (9) indicate that, under the assumption of additivity of chromophore absorption, the combination of angular measurements at several wavelengths may allow for the estimation of the sample composition, molecular weight, and shape. Since complementary information is available from both light scattering and absorption measurements, it is considered advantageous to conduct them simultaneously.
  • the system and method of the present invention accomplish these simultaneous multiwavelength multiangle measurements that yield information on the size, shape, and composition of particles.
  • the system comprises illumination means positioned to provide light energy to a volume portion of the sample. Typically the light energy is provided over a predetermined wavelength range encompassing the ultraviolet and visible portions of the spectrum, but it may also include the near- infrared portion.
  • a plurality of light-energy sensing means are radially disposed about the sample at a plurality of observation angles. This arrangment permits the simultaneous sensing of light energy- emerging from the sample volume portion at the plurality of angles.
  • the system comprises transducing means in communication with the sensing means. The transducing means provide from the sensed light energy a signal representative of an intensity spectrum as a function of wavelength for each observation angle. In a preferred embodiment the transducing means comprises a spectrophotometer card for communicating with a processor.
  • FIG. 1 is a schematic diagram of the multiangle multiwavelength system.
  • FIG. 2 illustrates theoretical intensity ratio spectra for (a) a sphere, (b) a thin rod, and a random coil illuminated with (c) unpolarized and (d) polarized light.
  • FIG. 3 shows the system in use for a flowing sample.
  • FIG. 4 shows the sample subjected to an electromagnetic field.
  • the system of the present invention is for the characterization of a sample containing a particle in suspension such as a macromolecule or a polymer in solution.
  • a sample suspension 20 is contained in a sample cell 30 that is held in position on an optical bench.
  • the system 10 comprises illumination means positioned to provide light energy to a volume portion 22 the sample 20 over a predetermined wavelength range.
  • the wavelength range comprises the ultraviolet-visible (uv-vis) range, which can be provided by any of a number of sources, including a xenon light source 102.
  • the light is delivered to the sample 20 with an optical fiber 202.
  • the sample is illuminated with polarized light, produced by the insertion of a polarizer 104 in the incident light path between the light source 102 and the sample 20.
  • the polarization properties of the sample are measured.
  • a plurality of light-energy sensing means is radially disposed about the sample 20 at a plurality of observation angles 106. These sensors are for simultaneously sensing light energy emerging from the sample volume portion 22 at the plurality of angles 106. It can be seen that alignment is important; so the sensors must be arrayed to permit the detection of an optimal quantity of light energy from the portion of the sample volume being illuminated. Typically the sensors are sensitive to light energy generally in the range of 180-1000 nm. In a preferred embodiment at least four sensors are used, with six being an optimal number.
  • a first sensor 110 is placed at a 180 degree observation angle 108. Backscattering measurements are made by having the optical fiber 202 comprise a split optical fiber having an illumination portion 204 and a sensing portion 206, thus proving sensing capabilities at 0 degrees.
  • each sensor comprises a charge- coupled device 114, to which light energy is fed by an optical fiber 116 that has received the light energy to be transmitted from a collimating lens 118, which produces a parallel beam of light energy from that impinging on it .
  • a reference sensor 120 for sensing light energy emerging directly from the light source 102. This may be accomplished, for instance, with the use of a beam splitter 122 between the light source 102 and the sample 20, the first pathway 124 leading to the sample and the second pathway 126 leading to the reference sensor 120.
  • An additional element of the system is transducing means in communication with the sensors.
  • the transducing means provides from the sensed light energy a signal representative of an intensity spectrum as a function of wavelength for each observation angle 106.
  • the signal from each sensor is fed to a processor 40 into which a spectrophotometer card 50 has been integrated.
  • one spectrophotometer card 50 can handle one sensor input; therefore, there are provided the same number of spectrophotometer cards 50 as the number of sensors. In an embodiment having six sensors, for instance, six spectrophotometer cards 50 would be required.
  • the output from the reference sensor 120 is also fed to the a spectrophotometer card 50 in processor 40, wherein software means are provided for correcting the spectra for incident light energy intensity fluctuations .
  • software means resident in the processor 40 can be utilized to calculate any of a number of particle characteristics based on theories such as those outlined above. For example, particle size distribution, shape, particle composition, and changes with time in particle shape and composition can be calculated using imaging software from collected scattering and/or absorption spectra.
  • FIG. 2 In FIG. 2 are shown calculated multiangle multiwavelength scattering spectra for a variety of ideal objects.
  • FIG. 2(a) is shown the intensity ratio of a spherically shaped particle as a function of the angle of observation and the angle of unpolarized incident light; in FIG. 2(b), that for a rod-shaped particle; in FIGS. 2(c) and (d) , that for a coil-shaped particle, for, respectively, unpolarized and polarized light.
  • These spectra are indicative of the type of information that can be obtained from the system and method of the present invention, including polarization properties of the sample.
  • multiangle multiwavelength spectra may be collected on a flowing sample (see FIG. 3) .
  • An exemplary use of this embodiment is for the detection of microorganisms in a water supply 602.
  • a particular particle characteristic is chosen to indicate the presence of the microorganism.
  • the "sample cell" in this case comprises a diverted section 608 of pipe 606 having a transparent portion 604 through which measurements may be made.
  • FIG. 4 Yet another embodiment 70 of the system is illustrated in FIG. 4, which further comprises means for imposing an electromagnetic field on the sample, such as a magnet 702. Imposing such a field permits the measurement of the field- dependent properties of the sample.

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  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

Cette invention concerne un système ainsi qu'un procédé de caractérisation d'un échantillon contenant une macromolécule en solution. Une source de lumière illumine l'échantillon, généralement dans la plage des fréquences de l'ultraviolet visible, tandis que plusieurs capteurs, disposés radialement autour de l'échantillon et selon plusieurs angles d'observation, détectent simultanément l'énergie lumineuse émanant dudit échantillon. Un spectre d'intensité est calculé en fonction de la longueur d'onde pour chaque angle d'observation, lequel spectre permet de calculer une caractéristique de la particule, telle que la forme, les modifications de conformation, la composition, ou encore la répartition granulométrique. Les données sur la dispersion et sur l'absorption sont également utilisées afin d'obtenir des informations complémentaires.
PCT/US1996/010342 1995-06-13 1996-06-13 Systeme et procede de caracterisation de particules a angles longueurs d'onde multiples WO1996042006A2 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU63854/96A AU6385496A (en) 1995-06-13 1996-06-13 Multi-angle, multiwavelength particle characterization syste m and method
JP9503355A JPH11507735A (ja) 1995-06-13 1996-06-13 多重角度多重波長粒子特性決定装置および方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US48994095A 1995-06-13 1995-06-13
US08/489,940 1995-06-13

Publications (2)

Publication Number Publication Date
WO1996042006A2 true WO1996042006A2 (fr) 1996-12-27
WO1996042006A3 WO1996042006A3 (fr) 1997-01-30

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Application Number Title Priority Date Filing Date
PCT/US1996/010342 WO1996042006A2 (fr) 1995-06-13 1996-06-13 Systeme et procede de caracterisation de particules a angles longueurs d'onde multiples

Country Status (3)

Country Link
JP (1) JPH11507735A (fr)
AU (1) AU6385496A (fr)
WO (1) WO1996042006A2 (fr)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0878701A2 (fr) * 1997-05-03 1998-11-18 H & W Optical Instruments GmbH Procédé de détermination du contenu en particules d'un fluide d'entraínement liquide ou gaseux
WO2000014510A1 (fr) * 1998-09-09 2000-03-16 The University Of Nottingham Forme de particules
WO2003062798A1 (fr) * 2002-01-18 2003-07-31 Newton Laboratories, Inc. Methodes et systeme de diagnostic par spectroscopie
WO2003062799A2 (fr) * 2002-01-18 2003-07-31 Newton Laboratories, Inc. Methodes et systeme de diagnostic par spectroscopie
GB2544716A (en) * 2015-09-15 2017-05-31 Photonic Measurements Ltd Measurement of turbidity
CN108287126A (zh) * 2018-03-23 2018-07-17 中国计量科学研究院 纳米颗粒粒径测量系统
US12216036B2 (en) 2019-11-19 2025-02-04 Horiba, Ltd. Particle size distribution measuring apparatus and particle size distribution measuring method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4361403A (en) * 1978-06-26 1982-11-30 Loos Hendricus G Multiple wavelength instrument for measurement of particle size distributions
US4541719A (en) * 1982-07-20 1985-09-17 Wyatt Philip J Method and apparatus for characterizing microparticles and measuring their response to their environment
US4676641A (en) * 1986-01-08 1987-06-30 Coulter Electronics Of New England, Inc. System for measuring the size distribution of particles dispersed in a fluid
US5164787A (en) * 1990-11-17 1992-11-17 Horiba, Ltd. Apparatus for measuring particle size distribution

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4361403A (en) * 1978-06-26 1982-11-30 Loos Hendricus G Multiple wavelength instrument for measurement of particle size distributions
US4541719A (en) * 1982-07-20 1985-09-17 Wyatt Philip J Method and apparatus for characterizing microparticles and measuring their response to their environment
US4676641A (en) * 1986-01-08 1987-06-30 Coulter Electronics Of New England, Inc. System for measuring the size distribution of particles dispersed in a fluid
US5164787A (en) * 1990-11-17 1992-11-17 Horiba, Ltd. Apparatus for measuring particle size distribution

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0878701A2 (fr) * 1997-05-03 1998-11-18 H & W Optical Instruments GmbH Procédé de détermination du contenu en particules d'un fluide d'entraínement liquide ou gaseux
EP0878701A3 (fr) * 1997-05-03 1999-08-18 H & W Optical Instruments GmbH Procédé de détermination du contenu en particules d'un fluide d'entraínement liquide ou gaseux
WO2000014510A1 (fr) * 1998-09-09 2000-03-16 The University Of Nottingham Forme de particules
WO2003062798A1 (fr) * 2002-01-18 2003-07-31 Newton Laboratories, Inc. Methodes et systeme de diagnostic par spectroscopie
WO2003062799A2 (fr) * 2002-01-18 2003-07-31 Newton Laboratories, Inc. Methodes et systeme de diagnostic par spectroscopie
WO2003062799A3 (fr) * 2002-01-18 2003-10-16 Newton Lab Inc Methodes et systeme de diagnostic par spectroscopie
US7333189B2 (en) 2002-01-18 2008-02-19 Pentax Corporation Spectroscopic diagnostic methods and system
US7404929B2 (en) 2002-01-18 2008-07-29 Newton Laboratories, Inc. Spectroscopic diagnostic methods and system based on scattering of polarized light
GB2544716A (en) * 2015-09-15 2017-05-31 Photonic Measurements Ltd Measurement of turbidity
GB2544716B (en) * 2015-09-15 2021-07-14 Photonic Measurements Ltd Measurement of turbidity
CN108287126A (zh) * 2018-03-23 2018-07-17 中国计量科学研究院 纳米颗粒粒径测量系统
US12216036B2 (en) 2019-11-19 2025-02-04 Horiba, Ltd. Particle size distribution measuring apparatus and particle size distribution measuring method

Also Published As

Publication number Publication date
WO1996042006A3 (fr) 1997-01-30
AU6385496A (en) 1997-01-09
JPH11507735A (ja) 1999-07-06

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