Aperture System for Multi-Angle Light Scattering Detectors

• US 20130100433A1
• Filed: 10/18/2012
• Published: 04/25/2013
• Est. Priority Date: 10/18/2011
• Status: Active Grant

• Current Assignee: Postnova Analytics GmbH
• Original Assignee: Postnova Analytics GmbH
• Inventors: Welz, Roland, Frose, Diethelm
• Granted Patent: US 8,760,652 B2
• Time in Patent Office: Days
• US Class Current: 356/36
• CPC Class Codes: G01N 2021/4711 Multiangle measurement
• CPC Class Codes: G01N 21/51 inside a container, e.g. in an ampoule G01N21/53 takes precedence
• CPC Class Codes: G01N 21/53 within a flowing fluid, e.g. smoke
• CPC Class Codes: G01N 2201/064 Stray light conditioning
• CPC Class Codes: G01N 30/74 Optical detectors measurement of intensity, velocity, spectral content, polarisation, or phase of infrared, visible or ultraviolet light G01J

Abstract

An apparatus for measuring the light scattering properties of a sample in a liquid medium, wherein the liquid medium with the sample is illuminated by a laser beam in a measuring cell transversely to the direction of filling the liquid medium in the measuring cell or transversely to the flow direction of the liquid medium within the measuring cell, comprising a laser, a cylindrical measuring cell, a first inner aperture system, a second outer aperture system and at least two detectors, wherein the detectors are arranged outside of the second outer aperture system so that they collect the light scattered on the sample within set, different angle ranges, wherein the first inner aperture system and the second outer aperture system are formed and arranged circularly and concentrically around the axis of the measuring cell. Use of the apparatus and a method that makes use of the apparatus are also disclosed.

Claims

1. Apparatus for measuring the light scattering properties of a sample in a liquid medium, wherein the liquid medium with the sample is illuminated by a laser beam (2) in a measuring cell (3) transversely to the direction of filling the liquid medium in the measuring cell or transversely to the flow direction of the liquid medium within the measuring cell (3), comprising a laser (1), a cylindrical measuring cell (3), a first inner aperture system (4), a second outer aperture system (5) and at least two detectors (6), wherein

the detectors (6) are arranged outside of the second outer aperture system (5) so that they collect the light scattered on the sample within set, different angle ranges,

characterized in that the first inner aperture system (4) and the second outer aperture system (5) are formed and arranged circularly and concentrically around the axis of the measuring cell (3).

2. The apparatus according to claim 1, wherein

the cylindrical measuring cell (3) has a bore hole (8) along its axis which allows the feed and discharge of the liquid medium that contains the sample and is formed from a translucent material that allows the laser beam (2) to pass in, through and out, and wherein

the liquid medium with the sample is conveyed along the axis of the measuring cell into/through the bore hole (8) of the measuring cell (3) and is illuminated in the bore hole (8) of the measuring cell (3) transversely to the axis of the measuring cell (3) by the laser beam (2).

3. The apparatus according to claim 1, characterized in that the first inner aperture system (4) and the second outer aperture system (5) are both formed as slot apertures, wherein the number of slots in the two aperture systems corresponds to the number of detectors (6), and each of the aperture systems additionally has an inlet opening (9) and an outlet opening (10) for the laser beam (2).

4. The apparatus according to claim 3, characterized in that the measuring cell (3), the first inner aperture system (4) and the second outer aperture system (5) as well as the detectors (6) lie on an optical axis so that the individual detectors (6) collect set, different angle ranges of the light, which is scattered on the sample and leaves the measuring cell (3).

5. The apparatus according to claim 3, characterized in that the first inner aperture system (4) and the second outer aperture system (5) have different slot widths depending on the observed angle range of the light scattered on the sample, wherein the slot widths of the first inner aperture system (4) and of the second outer aperture system (5) are the same for a given observed angle range of the light scattered on the sample.

6. The apparatus according to claim 1, characterized in that the measuring cell (3) is produced from glass, polymer or a combination of said materials or a liquid and has a refractive index that substantially corresponds to the refractive index of the liquid medium that contains the sample to be measured and which is higher than the refractive index of air.

7. The apparatus according to claim 1, characterized in that the apparatus enables the observation of the light scattered on the sample within set, different angle ranges of 7°

to 164°

.

8. The apparatus according to claim 1, characterized in that the apparatus comprises 2-25, preferably 7-21, and particularly preferably 7, 14 or 21 detectors (6).

9. The apparatus according to claim 1, further comprising a support for holding the laser (1), the cylindrical measuring cell (3), the first inner aperture system (4), the second outer aperture system (5) and the at least two detectors (6), characterized in that

in the region for holding the measuring cell (3) the support has three radially arranged grooves via which the liquid medium that contains the sample to be measured is conveyed into the measuring cell (3), and

the measuring cell is fixed in the desired position within the support with the aid of a molding in the support, wherein the lateral area of the measuring cell is partially enclosed by the support, and the measuring cell is sealed by means of two flat seals arranged on the flat sides of the cylindrical measuring cell.

12. Use of an apparatus according to claim 1 for measuring the light scattered on a sample located within a liquid medium.

13. The use according to claim 12, wherein the measurement of the light scattered on the sample is taken by means of a batch measurement or an online measurement.

14. The use according to claim 13, wherein the sample was separated before the measurement by means of a chromatographic or a quasi-chromatographic separating method into individual fractions each having a substantially uniform particle size and/or a substantially uniform molar mass.

15. The use according to claim 14, wherein the sample separation takes place by means of HPLC, such as e.g. Size Exclusion Chromatography (SEC) or Gel Permeation Chromatography (GPC), or Field-Flow Fractionation.

10. A method for measuring the light scattered on a sample located within a liquid medium, comprising the following steps:

a) introducing the liquid medium that contains the sample into a cylindrical measuring cell (3),

b) illuminating the sample located within the measuring cell (3) transversely to the direction of filling the liquid medium in the measuring cell or transversely to the flow direction of the liquid medium within the measuring cell (3) with a laser beam (2), and

c) detecting the resulting scattered light beams (7) with at least two detectors (6) arranged circularly and concentrically around the measuring cell (3) which collect the light scattered on the sample within set, different angle ranges,

characterized in that the detectors are shielded from scattered light beams, which do not come within the respectively set angle ranges, and remissions by a first inner aperture system (4) and a second outer aperture system (5) which are formed and arranged circularly and concentrically around the axis of the measuring cell (3).

11. The method according to claim 10, wherein

the cylindrical measuring cell (3) into which the liquid medium that contains the sample is introduced has a bore hole (8) along its axis and is formed from a translucent material,

the liquid medium that contains the sample is introduced into the bore hole (8) along the axis of the measuring cell (3), and

the sample located within the bore hole (8) of the measuring cell (3) is illuminated transversely to the axis of the measuring cell by a laser beam (2).