A method for determining at least one property related to dry particulate matter.
By dispersing dry particulate matter in a liquid medium and analyzing light transmission images, the method addresses the inefficiencies of existing methods, providing rapid and precise determination of particle properties, particularly for small particles, suitable for quality control in manufacturing.
Patent Information
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- PARTICLETECH APS
- Filing Date
- 2024-07-16
- Publication Date
- 2026-07-23
AI Technical Summary
Existing methods for analyzing dry particulate matter, such as particle size and shape, are time-consuming and lack precision, especially for small particles, and fail to distinguish between particle types due to electrostatic interactions.
A method involving dispersing dry particulate matter in a liquid medium to create a dispersed sample, acquiring multiple light transmission images, and processing these images to determine morphological properties with high precision, including shape and size, without damaging the particles.
Enables rapid, accurate, and cost-effective determination of morphological properties of dry particulate matter, including size, shape, and type, suitable for on-site quality control in manufacturing.
Smart Images

Figure 2026524711000001_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to a method for determining at least one property related to dry particulate matter such as particulate matter, crystallized matter, crushed matter, or any other particulate matter.
Background Art
[0002] It is well known to analyze particles to determine one or more properties. For example, particle size analysis is important for research projects, product development, process control, quality control, and other technical activities where particle size effects may be important, such as accurate particle size determination in paints, inks, filled plastics, ore processing, agricultural pharmaceuticals, and cosmetics, which are often very important for many other technical activities. Applying laser diffraction technology to perform such particle size determination is well known. In many prior art analyses of dry particles, it is not even possible to distinguish between particle types due to the lack of morphological information. The aggregation effect of particles is particularly prominent when the particulate matter contains relatively small particles, for example, particles less than a few millimeters due to electrostatic interactions between particles.
[0003] CN211978616 describes a dynamic particle image particle size and particle shape analyzer that uses dry electromagnetic vibration to separate particles. The analyzer exposes the particles to vibration, injects the particles into a blanking channel, from where the particles can slide to the right and finally fall through the blanking channel. The particle group forms a waterfall-type material curtain, so that the particles are dispersed, and the camera can photograph the particles in the falling state over time, facilitating subsequent analysis.
[0004] This image particle size and particle shape analyzer is very time-consuming to operate, and furthermore, obtaining an image of the particles in the falling state may not result in a reliable analysis. Additionally, this method may not be suitable for particulate matter containing relatively small particles.
[0005] IN201731020161 describes an alternative method for analyzing dry particulate matter using images, which involves using an automated diffusion array of chili on a moving bed machine system and machine vision technology backed by an advanced image analysis algorithm for rapid and automated quality characterization of the dry chili based on physical characteristics such as size, color, and shape. A vibrating dispensing unit separates the chili sample on a moving bed as it drops from a hopper, ensuring that the chili samples do not overlap or come into contact with each other. A digital camera continuously captures image frames of the chili sample in the moving bed, and the images are automatically analyzed by an advanced image analysis algorithm to extract appearance-based quality parameters of the chili sample, ultimately providing the user with an estimate of the output quality parameters as output.
[0006] US2010326213 describes an apparatus for dispersing a sample of particulate material, comprising a carrier having a sample bearing surface for placing the sample, and a housing for forming a dispersion chamber when closed at least at the base. The carrier is positioned such that the sample bearing surface is removed from contact with the sample when a sufficient pressure difference is applied across the carrier between the sample bearing surface and the opposite side of the carrier. The housing has an inlet that faces at least partially the base. The apparatus includes a device for passing the carrier through the inlet to a certain volume of gas, such as air, by exposing the carrier to a pulsed positive pressure different from that of the dispersion chamber.
[0007] None of the prior art solutions described above provide the desired solution; therefore, a novel and effective method for analyzing dry particulate matter is still needed.
[0008] Disclosure of the invention The object of the present invention is to provide a method for determining at least one property related to dry particulate matter, which is relatively rapid, cost-effective, and capable of determining at least one desired property with high accuracy.
[0009] In one embodiment, the objective is to provide a method for determining one or more desired properties related to dry particulate matter, such as determining one or more morphological properties, including one or more shapes and one or more sizes, with high precision.
[0010] In one embodiment, the objective is to provide a method for determining at least one characteristic relating to the type (one or more) of particles, preferably a method that enables the distinction of particle types based on morphological determination.
[0011] In one embodiment, the objective is to provide a method for determining at least one property of dry particulate matter, such as the size of the particulate matter, the size distribution, the shape factor, and / or spectral information of the particulate matter.
[0012] In one embodiment, the objective is to provide a method for determining at least one chemical property of a dry particulate matter.
[0013] These and other objectives are addressed by the present invention or embodiments thereof, as defined in the claims and / or described below herein.
[0014] The present invention or its embodiments have been found to have several further advantages, which will be apparent to those skilled in the art from the following description.
[0015] Particulate matter, such as powders, has diverse applications in many different manufacturing fields, including dyes, ceramics, petroleum, cosmetics, pharmaceuticals, and food. Therefore, the need for inspection methods in the production and processing of such particulate matter is extremely important.
[0016] The inventors of the present invention have found a remarkably effective method for determining at least one property related to dry particulate matter, comprising providing a liquid dispersion of dry particulate matter and obtaining multiple light transmission images of the dispersed particulate matter. This method has been found to be effective and highly accurate, and can result in very precise and valuable morphological determination of the particulate matter. In addition, the method is relatively easy to implement and can be carried out on-site, for example, in a factory for quality control of intermediate or final products.
[0017] The terms "image" and "frame" are used interchangeably.
[0018] The phrase “properties related to dry particulate matter” is used herein to describe properties of dry particulate matter, or properties that are involved with or at least partially caused by dry particulate matter. In one embodiment, at least one property related to dry particulate matter includes at least one property of dry particulate matter. In one embodiment, at least one property related to dry particulate matter includes at least one property of dry particulate matter in combination with at least one other substance. In one embodiment, at least one property related to dry particulate matter includes at least one property of dry particulate matter when exposed to one or more other substances. In one embodiment, at least one property related to dry particulate matter includes at least one property of another substance when exposed to a substance.
[0019] The terms "user" and "operator" are used interchangeably.
[0020] It should be emphasized that the term “comprises / comprising,” when used herein, should be interpreted as an open term, meaning to identify the presence of one or more specifically described features, such as one or more elements, one or more units, one or more integers, one or more steps, one or more components, and combinations thereof, but not precluding the presence or addition of one or more other features.
[0021] Throughout this specification or the claims, unless otherwise specified or required by context, the singular form encompasses the plural form and the plural form encompasses the singular form.
[0022] "Embodiments" should be interpreted as including examples of the present invention that include one or more features of the embodiments mentioned.
[0023] The term “substantially” should be interpreted herein as including normal product variances and tolerances. All features and embodiments of the present invention as described herein, including ranges and preferred ranges, may be combined in various ways within the scope of the invention unless there is a particular reason not to combine such features.
[0024] Unless otherwise specified, any properties, property ranges and / or determination and / or assay conditions are given or provided at 1 atmosphere and 25°C.
[0025] All features and embodiments of the present invention as described herein, including their ranges and preferred ranges, may be combined in various ways within the scope of the invention, unless there is a particular reason not to combine such features.
[0026] A method for determining at least one property related to particulate matter, wherein the particulate matter is dry particulate matter. (a) A step of providing a sample support capable of containing a liquid medium, (b) A step of providing a dispersed sample in a sample support, the step including dispersing a part of the dry particulate matter in a part of the liquid dispersion medium; (c) A step of performing at least one scanning procedure; (d) A step of determining at least one property; A method comprising.
[0027] The dry particulate matter preferably includes powders such as free-flowing powders. <Advantageously, the method includes preparing a dispersed sample by a method comprising the step of mixing dry particulate matter with a liquid dispersion medium, wherein the concentration of particulate matter does not exceed 40 mg of particulate matter per 1 mL of liquid dispersion medium, and the method preferably includes providing the particulate matter and liquid dispersion medium in a flow such as a gentle flow onto a sample support, and preferably the concentration of particulate matter is 1 to 35 mg / ml of liquid dispersion medium, for example 5 to 20 mg / ml of liquid dispersion medium, for example 8 to 15 mg / ml of liquid dispersion medium.
[0033] Surprisingly, it was found that interparticle forces could be eliminated by preparing a dispersed sample using a relatively large amount of liquid dispersion medium, and no increase in interparticle aggregates due to humidity was observed.
[0034] Dry particulate matter can be dispersed in a liquid dispersion medium in a very gentle manner to achieve a desired dispersion of the particulate matter, and it has been found that even small particles, such as those with a particle size of 1 mm or less, e.g., 0.5 mm or less, e.g., 0.1 mm or less, can be dispersed without any significant damage to the particles. For example, it has been found that excellent dispersion of particulate matter can be achieved without any observed collapse of particles or aggregates. Thereafter, the method ensures that at least one property related to dry particulate matter can be determined with very high precision.
[0035] Advantageously, the step of providing the dispersed sample involves dispersing particulate matter without requiring stirring or shaking, which further reduces the risk of modifying or damaging the particles, such as the risk of breaking up aggregates.
[0036] In one embodiment, the step of performing at least one scanning procedure includes performing one single scanning procedure.
[0037] In one embodiment, the step of performing at least one scanning procedure includes performing two or more scanning procedures, such as three or more scanning procedures or a number of scanning procedures that may be desired for a particular evaluation. Advantageously, the number of scanning procedures required or desired to determine at least one property related to dry particulate matter may be 1 to 100 or more. Preferably, the number of scanning procedures required or desired to determine at least one property related to dry particulate matter may be 1 to 25, for example, 10. In a particular embodiment, at least two scanning procedures may be required, as will become apparent from the following description.
[0038] Each of the one or more scanning steps is: (1) Image acquisition including acquiring multiple light transmission images of an image acquisition region translated along a scanning path through a dispersed sample in a sample support using an image acquisition device having an optical axis, and Processing multiple acquired images, Includes.
[0039] If the method involves performing two or more scanning steps, each scanning step may be performed sequentially in one embodiment. In one embodiment, two or more scanning steps may be performed interleaved, for example, by starting one scanning step before the previous one has finished. In one embodiment, two or more scanning steps may be performed in a combined manner, for example, by performing image acquisition for two or more scanning steps, followed by processing for two or more scanning steps. In one embodiment, two or more scanning steps may be performed in time slots between the two or more scanning steps.
[0040] The image acquisition area may be perpendicular to the optical axis of the image acquisition device.
[0041] Advantageously, the image processing step includes acquiring a set of images. Acquiring a set of acquired images may conveniently include, for example, preprocessing the images acquired by a filtering process to remove blur or other artifacts using a known filtering process. Preprocessing may further include compositing one or more of the acquired images with previously acquired images to improve image quality. Such preprocessing activities are known in the art. Preferably, determining at least one characteristic includes determining at least one characteristic at least partially from the set of images.
[0042] Advantageously, the image set includes at least two different images containing the same particles of particulate matter in the dispersed sample. This allows for obtaining a perspective view of the particles and, preferably, generating a 3D view from at least a portion of the particles. Advantageously, the image set includes three or more different images containing the same particles of particulate matter in the dispersed sample, thereby increasing the view of the particles and revealing desired morphological details.
[0043] In one embodiment, the scanning procedure includes performing a subdetermination of at least one characteristic. The determination of at least one characteristic may then conveniently include determining at least one characteristic at least partially from the subdetermination of at least one characteristic. In this embodiment, the method may conveniently include processing the subdetermination of at least one characteristic in combination with one or more other known parameters, such as a reference parameter, a calibration curve, and / or a parameter correlated with the liquid partitioning medium.
[0044] In one embodiment, the step of performing at least one scanning procedure includes the step of performing two or more scanning procedures, and the determination of at least one characteristic includes the step of determining at least one characteristic at least partially from the subdetermination of at least one characteristic of the two or more scanning procedures.
[0045] In this embodiment, the method advantageously includes performing two or more scanning steps, each of which a subdetermination of at least one characteristic may be performed in each of two or more scanning steps, and after the determination of at least one characteristic, performing two or more scanning steps that are performed at least partially on the two or more subdeterminations. In this embodiment, the at least one characteristic advantageously includes the determination of one or more changes related to dry particulate matter.
[0046] The two or more scanning procedures may be, for example, consecutive scanning procedures, or selected from a series of scanning procedures. The two or more scanning procedures may be performed, for example, in a time slot between the two or more scanning procedures, and the time slot may be selected to have a duration selected in accordance with one or more changes related to the dry particulate matter being determined. If one or more changes or suspected changes are estimated to occur quickly, the duration of the time slot may be favorably relatively short; if one or more changes or suspected changes are estimated to take longer, the duration of the time slot may be favorably longer; and / or one or more additional scanning procedures, including performing one or more additional sub-determinants, may be performed and compared with one or more previous sub-determinants.
[0047] Acquiring multiple light-transmitted images of an image acquisition region along a scanning path through a dispersed sample in a sample support may advantageously involve illuminating at least the image acquisition region along the scanning path by emitting light from an illumination device through the dispersed sample toward an image acquisition device and using the image acquisition device to acquire light-transmitted images. Thereafter, the acquired images may be sharper and of higher quality.
[0048] In one embodiment, the step of illuminating an image acquisition area includes emitting a light beam from an illumination device toward an image acquisition device, wherein at least a portion of the light beam passes through the acquisition area to the image acquisition device, and the method includes shaping the light beam such that it converges a beam of light rays in the acquisition area. It has been found that by ensuring that the light beam includes a beam of light rays that converges in the acquisition area, the acquired image can reveal more morphological detail than when the light beam is not converged.
[0049] The step of converging the beam of light can, advantageously, have a vertex angle of up to 75°, for example, 5° to 65°.
[0050] In one embodiment, acquiring multiple light-transmitted images of an image acquisition region along a scanning path through a dispersed sample in a sample support advantageously includes acquiring a light-transmitted image of the image acquisition region at each selected position along the scanning path.
[0051] The scanning path may have any length or shape, and advantageously, the scanning path may be at least a path-length section along the optical path of the image acquisition device, and the acquisition of multiple light-transmitted images of the image acquisition device includes the acquisition of multiple light-transmitted images of an image acquisition region translated along two or more scanning paths through a dispersed sample.
[0052] One or more scan paths may include at least a straight path length section perpendicular to the horizontal plan or at an angle to the horizontal plan, for example, perpendicular to the horizontal plan.
[0053] In one embodiment, one or more scanning paths include at least one linear path length section perpendicular to the interface plan between the sample support and the dispersed sample, or at an angle such as a right angle to the interface plan between the sample support and the dispersed sample.
[0054] In a preferred embodiment in which one or more scan paths include at least one linear path length section in the horizontal plan, the image acquisition area has a plan that is slightly inclined with respect to the horizontal plan, such as at an angle of 2 to 20 degrees with respect to the path length, and preferably the image acquisition area has an angle of 5 to 15 degrees with respect to the path length, for example, 6 to 7 degrees.
[0055] As a result, highly detailed 3D images of particulate matter particles can be obtained by stitching together sub-images of the same particle from two or more light-transmitted images.
[0056] The angle of the image acquisition area with respect to the horizontal plan can preferably be selected depending on the height of the dispersed sample in the sample support and the size of the image acquisition area, such that the image acquisition area extends across the entire height of the dispersed sample in the sample support.
[0057] The eight dispersed samples in the sample support may be 50 μm to 500 μm in size, for example, 100 μm to 200 μm.
[0058] Acquiring multiple light-transmitted images of an image acquisition region along a scanning path through a dispersed sample in a sample support may conveniently involve stepwise translation of the image acquisition region along the scanning path and acquiring light-transmitted images between each step of the stepwise translation. The steps in each step may be the same or different from each other. Examples of suitable step lengths include steps up to 1 cm, such as 1 μm to 0.5 cm.
[0059] The step length can be advantageously selected depending on the particulate material being analyzed and the properties (one or more) to be determined.
[0060] The dispersion medium can, in principle, be any liquid medium having a relatively low viscosity, such as 0.5 mPa*s to 100 Pa*s, at the temperature and pressure used to provide the dispersed sample, preferably up to about 100 Pa*s.
[0061] The liquid dispersion medium can be usefully selected depending on the dry particulate matter and at least one property to be determined.
[0062] In one embodiment, the method includes selecting a liquid dispersion medium that is non-reactive and / or insoluble with respect to dry particulate matter when mixed with the dry particulate matter. When dry particulate matter is mixed with a liquid dispersion medium to provide a dispersed sample, the former dry particulate matter is referred to as particulate matter. Advantageously, the liquid dispersion medium is selected to be non-reactive and / or insoluble with respect to the particulate matter during the acquisition of at least a plurality of light transmission images, for example, during the time required to acquire a plurality of light transmission images in the execution of at least one scanning procedure.
[0063] If the liquid dispersion medium is selected to be nonreactive and / or non-soluble for particulate matter, then at least one property to be determined may appropriately be, or include, one or more properties of the dry particulate matter, such as morphological characteristic parameters of the dry particulate matter, particle size characteristic parameters of the dry particulate matter, shape characteristic parameters of the dry particulate matter, purity characteristics of the particulate matter, quantification of one or more particle types of the dry particulate matter, residual water content of the dry particulate matter, density characteristics of the particulate matter, flowability characteristics of the particulate matter, wetting characteristics of the particulate matter, and / or any combination of one or more of these properties.
[0064] In one embodiment, the method includes selecting a liquid dispersion medium that is reactive and / or soluble to at least a portion of the particulate matter. Thereafter, the method may be suitable for determining one or more properties including one or more interactions between the particulate matter and the liquid dispersion medium, one or more impacts of the liquid dispersion medium on the particulate matter, and / or one or more impacts of the particulate matter on the liquid dispersion medium.
[0065] A liquid dispersion medium that has (or is suspected to have) reactivity with respect to at least one compound or element of particulate matter and / or a dissolving effect on at least one compound or element of particulate matter is referred to herein as an active liquid dispersion medium, and the reaction or dissolution caused by the liquid dispersion medium is referred to as a dynamic property.
[0066] A liquid dispersion medium that is inactive with respect to at least one compound or element of particulate matter and / or does not have a dissolving effect on at least one compound or element of particulate matter is referred to herein as an inert liquid dispersion medium, and properties determined when no change is observed or cannot be observed are referred to as static properties.
[0067] The liquid dispersion medium may be selected, for example, to have or be suspected of having reactivity with at least one compound or element of the particulate matter. The reactivity or suspected reactivity may be, beneficially, a chemical or physical reaction, such as a reaction that causes decomposition, a reaction that causes structural change, a substitution reaction, a polymerization reaction, a swelling reaction, a gelling reaction, or any combination thereof.
[0068] Examples of reactions may include one or more of the following reactions that can be caused by chemical, physical, and / or thermal changes: Particle swelling / gelation (observable as changes in particle morphology and / or particle size, for example) Particle dissolution (observable, for example, as changes in particle size, particle morphology, and / or optical changes in the liquid dispersion medium), Particle transformation (observable as changes in particle morphology, changes in particle size and / or the formation of gas bubbles, for example), (1) Conversion from solid to solid (2) Conversion from solid to liquid to solid (3) Conversion from solid to gas, Particle surface modification / functionalization (observable, for example, as changes in attractive and / or repulsive forces between particles and / or between the surface of a particle-sample support), Particle sedimentation / suspension (observable as changes in the position and / or motion of particles), (1) This is due to the change in particle density compared to the liquid density. (2) Due to changes in the magnetic field, Particle crosslinking (observable as a change in particle size or shape, for example), Gas generation (observable, for example, as the formation of gas bubbles), Reactions in a fluid (for example, optically observable in a liquid dispersion medium).
[0069] In one embodiment, the liquid dispersion medium has, or is suspected to have, a dissolving effect on at least one compound or element of particulate matter, such as a salt. This embodiment is particularly suitable for determining whether a specific component, such as a mineral, is present in dry particulate matter, and optionally includes providing an estimate of the qualitative and / or quantitative content of such component in the dry particulate matter.
[0070] Advantageously, the step of performing at least one scanning procedure includes, for example, the step of performing two or more consecutive scanning procedures as described above, which apply interleaved and / or integrated scanning procedures, and the step of determining at least one characteristic includes the step of determining whether a reaction and / or dissolution has occurred. Preferably, the method includes determining the extent of the reaction and / or dissolution that occurred, such as determining the extent of the reaction and / or dissolution that occurred as a function of time.
[0071] In one embodiment, performing at least one scanning procedure includes performing two or more consecutive scanning procedures, wherein the liquid dispersion medium in the first of the two or more scanning procedures is different from the liquid dispersion medium in the second of the two or more scanning procedures. This embodiment may advantageously include providing a first dispersion sample comprising a portion of particulate matter dispersed in a portion of a first liquid dispersion medium in a first sample support, and providing a second dispersion sample comprising a portion of particulate matter dispersed in a portion of a second liquid dispersion medium in a second sample support, wherein at least one scanning procedure is performed on each of the first and second dispersion samples, and at least one property is determined.
[0072] Preferably, the liquid dispersion medium in the first scanning procedure differs from the liquid dispersion medium in the first scanning procedure in terms of temperature and / or in terms of the addition of additives, such as pH adjusting additives, reactants, surfactants, refractive index adjusters such as salts, or any combination thereof.
[0073] This embodiment may include, for example, providing a dispersion sample in which the liquid dispersion medium is at a first temperature and performing at least one first scanning procedure. Thereafter, preferably, changing the temperature by increasing the temperature, performing at least one second scanning procedure and determining at least one property based on at least one first scanning procedure and at least one second scanning procedure.
[0074] Another example of implementing this embodiment may include providing a first dispersion sample comprising a portion of particulate matter dispersed in a portion of a first liquid dispersion medium in a first sample support, and providing a second dispersion sample comprising a portion of particulate matter dispersed in a portion of a second liquid dispersion medium in a second sample support, wherein at least one scanning procedure is performed on each of the first and second dispersion samples, and at least one property is determined based on at least one scanning procedure on each of the first dispersion samples. The second liquid dispersion medium may differ from the first liquid dispersion medium, for example, in that it contains the components described above, or the second liquid dispersion medium may differ from the first liquid, for example, in terms of concentration, composition, polarity, color, or in any other way that may contribute to determining one or more properties.
[0075] Depending on the dry particulate matter and the liquid dispersion medium, the dispersed sample may have any temperature during the scanning procedure. The sample support can be appropriately selected for the desired or selected temperature to be applied. Advantageously, the dispersed sample has a temperature at which it is in a liquid state during the scanning procedure. In some embodiments, the dispersed sample has a temperature that may be up to the sintering temperature of the dry particulate matter or its components.
[0076] The temperature can be set to, for example, 900°C, or up to 1500°C if convenient. For most dry particulate matter, a temperature of 0–100°C may be appropriate.
[0077] In embodiments in which the performance of at least one scanning procedure includes the performance of two or more consecutive scanning procedures, the method includes exposing a dispersed sample to the effects of selected radiation and / or fields selected from electromagnetic radiation, magnetic fields and / or electric fields in at least one first scanning procedure of the two or more scanning procedures, wherein the dispersed sample is not exposed to the selected electromagnetic radiation, magnetic fields and / or electric fields, or is exposed to different levels of selected electromagnetic radiation, magnetic fields and / or electric fields.
[0078] The method conveniently includes selecting a liquid dispersion medium that is transparent to at least one wavelength of light emitted from an illuminator through the dispersion sample in order to ensure the desired quality of the acquired image.
[0079] In one embodiment, the method includes the step of selecting a liquid dispersion medium such that it has a refractive index determined by at least one wavelength of light emitted from an illumination device, which is different from the refractive index of the dry particulate matter. It has been found that if the refractive index of the liquid dispersion medium is different at at least one wavelength of light emitted from an illumination device, high-quality images can be obtained. However, it has been found that, in order to obtain acquired images that enable the reveal of morphological detainment, the refractive index of the liquid dispersion medium at at least one wavelength of light emitted from an illumination device should not be advantageously different. Therefore, the liquid dispersion medium can be advantageously selected such that it has a refractive index determined by at least one wavelength of light emitted from an illumination device, and this refractive index differs from the refractive index of at least a portion of the dry particulate matter by only 0.01 to 0.1, for example, 0.2 to 0.5.
[0080] In one embodiment, the method includes selecting a liquid dispersion medium that has a neutralizing effect on the electrostatic interactions between particles of dry particulate matter. Thereafter, the dry particulate matter can be dispersed very easily without the risk of damaging the particulate matter or its structure.
[0081] The liquid dispersion medium may be, or may contain, a nonpolar liquid such as oil, which is beneficial for facilitating the easy dispersion of dry particulate matter.
[0082] In some embodiments, the liquid dispersion medium is a polar liquid, such as an aqueous liquid like tap water, distilled water, and / or deionized water, or contains a polar liquid. If the liquid dispersion medium is selected to induce a chemical or physical reaction with or to particulate matter, the liquid dispersion medium advantageously contains water, such as laboratory water, along with an activator.
[0083] The light emitted from the lighting device may include one or more wavelengths, such as one or more wavelengths in the visible range of 380 to 700 nm and / or one or more wavelengths in the ultraviolet and / or infrared wavelength range.
[0084] In one embodiment, the light emitted from the lighting device preferably includes one or more wavelengths selected in the range of 380 to 940 nm, and preferably includes at least one wavelength in the range of 400 to 900 nm.
[0085] Examples of suitable wavelength ranges include wavelengths from 250 to 2500 nm, such as 250 to 900 nm or 900 to 2500 nm. Advantageously, the lighting device includes one or more wavelengths in the visible range.
[0086] In one embodiment, the light emitted from the lighting device includes light from a light source adapted to emit monochromatic or nearly monochromatic light having a bandwidth of up to 50 nm, preferably up to 10 nm, for example, up to 5 nm.
[0087] Here, the term "bandwidth" of a light source refers to the bandwidth of the optical signal emitted from the light source, which includes wavelengths greater than half the maximum intensity of the central wavelength (CW). This is also known as the full width at half maximum (FWHM).
[0088] For example, this method may include illuminating the image acquisition area using two or more light sources having the same or different wavelengths, and / or by two or more light beams having the same or different wavelengths.
[0089] In one embodiment, the light emitted from the illuminator includes structured light, such as structured light, which comprises a group of electromagnetic waves emitted from the illuminator and propagating along a parallel or convergent direction, the structured light being textured as seen in a cross-sectional view perpendicular to the central axis of the group of electromagnetic waves (also referred herein to as the optical axis of the emitted light), and the light preferably has an intensity distribution in the cross-sectional view that includes regions of higher intensity and regions of lower intensity or no intensity, the intensity distribution being different from the natural Gaussian intensity distribution of the light beam.
[0090] Structured light may have, for example, an intensity distribution in a cross-sectional view that includes lines in the high-intensity region.
[0091] In one embodiment, the dispersed sample in the sample support has an uncoated surface during the acquisition of at least several light transmission images, and the multiple light transmission images are acquired through the uncoated surface. This can reduce the risk of image artifacts caused by undesirable reflections.
[0092] Advantageously, at least a portion of the sample wall, such as the bottom wall and / or top wall of the sample support, such as the entire sample support, is transparent to at least one wavelength of light emitted from the illuminator through the dispersed sample.
[0093] Examples of suitable materials for sample supports include polymers (e.g., polypropylene, polyethylene terephthalate, and polystyrene) and / or glass.
[0094] In one embodiment, the sample support is in the form of a sample container that includes an inlet for supplying a dispersed sample to the sample support and an outlet for air or the previously dispersed sample. An example of such a suitable sample support is shown in Figure 1.
[0095] In one embodiment, at least one of a plurality of light-transmitted images is acquired through a polarizing filter, such as a polarizing lens, of the image acquisition device. This allows the acquired image to be of very high quality. It has been found that the risk of glare and reflection can be reduced compared to acquiring all or some of the images through a polarizing filter, thereby resulting in sharper and clearer images that can reveal additional morphological and topological details compared to not using a polarizing filter. In one embodiment, the method includes the steps of performing at least one scanning procedure using a polarizing filter and performing at least one scanning procedure without using a polarizing filter.
[0096] Dry particulate matter may, in principle, contain particles of any size that may be present in the dispersed sample within the sample support. In practice, it is desirable that the particle size does not exceed 5 cm.
[0097] The dry particulate matter may, for example, contain particles up to 2 cm in size, preferably in the range of 0.1 μm to 1 cm.
[0098] Dry particulate matter may, conveniently, include non-biological particles selected from inorganic particles (e.g., sand, minerals, clay and / or salts) and / or organic particles (e.g., food, pharmaceuticals, polymers and / or components).
[0099] In one embodiment, the method includes pre-drying the particulate matter to remove at least a portion of the unbound water.
[0100] This embodiment may be desirable when unbound water may affect the dispersion and / or one or more properties determined. Pre-drying may include drying to a certain weight at a selected temperature. Advantageously, the temperature selected for pre-drying is one that does not chemically affect the particulate matter, e.g., below 100°C, e.g., 30–90°C.
[0101] The dried particulate matter may, advantageously, have or be dried to have an unbound water content of up to 15% by weight, for example, 10% by weight. In one embodiment, the method includes drying the dried particulate matter to an unbound water content of up to 5% by weight, for example, 1% by weight.
[0102] Advantageously, each execution of at least one scanning procedure includes acquiring a plurality of light transmission images, preferably, for one or more particles of particulate matter, acquiring an image set including at least one image in which the particle is in focus and at least one image in which the particle is out of focus, wherein the image set preferably includes at least three images. Advantageously, the method includes processing the acquired light transmission images to synthesize a 3D image of at least a certain volume of particulate matter in the dispersed sample.
[0103] In one embodiment, the step of performing at least one scanning procedure includes the step of performing two or more scanning procedures, each including the step of acquiring an image of the common portion of the dispersed sample, and optionally the step of determining whether changes such as changes over time, for example, degradation, have occurred. The two or more scanning procedures may be consecutive or not, as described above.
[0104] In one embodiment, the method comprises performing two or more runs of determining at least one property related to dry particulate matter, wherein the two or more runs differ in time, in liquid dispersion medium, in physical influence of the dispersed sample, and / or in the concentration difference of particulate matter in the liquid dispersion medium. Thereafter, the desired property may be determined, for example, as described elsewhere in this specification.
[0105] Providing a dispersed sample in a sample support may include dispersing at least a portion of dry particulate matter in at least a portion of a liquid dispersion medium, and coating the sample support with the dispersed sample containing the portion of dry particulate matter dispersed in the liquid dispersion medium. Alternatively or additionally, providing a dispersed sample in a sample support may include applying the portion of dry particulate matter and the portion of the liquid dispersion medium in the sample support simultaneously or successively, and being conditional on dispersing the portion of dry particulate matter in the portion of the liquid dispersion medium in the sample support.
[0106] In one embodiment, the method includes preparing a dispersed sample by mixing dry particulate matter with a liquid dispersion medium, where the concentration of particulate matter is 40 mg of particulate matter per 1 mL of liquid dispersion medium, for example, 1 mg of particulate matter per 10 mL of liquid dispersion medium. Optionally, the method includes the steps of preparing a parent sample and taking a dispersed sample from the parent sample. The latter may be desirable if some portion of the dispersed sample is to be analyzed using the method of the embodiment of the present invention.
[0107] At least one property related to dry particulate matter is, conveniently, Morphological characteristic parameters of dry particulate matter, Particle size characteristic parameters of dry particulate matter, Shape characteristic parameters of dry particulate matter, Characteristics of the purity of particulate matter, Quantification of one or more particle types in dry particulate matter, Residual water content of dry particulate matter, Particle distribution of one or more individual particle characteristics of dry particulate matter, Gas generation related to dry particulate matter, Characteristics of particulate matter density, Characteristics of the fluidity of particulate matter, Characteristics of the reactivity of particulate matter, Characteristics of the solubility of particulate matter, Characteristics of the wetting properties of particulate matter, The hygroscopic characteristics of particulate matter, and / or This includes any combination of one or more of these properties.
[0108] In one embodiment, at least one property related to the dry particulate matter includes density parameters such as the homogeneity / heterogeneity of the density of the particles of the dry particulate matter, such as the density level of one or more particles of the dry particulate matter.
[0109] In one embodiment, the liquid dispersion medium is selected to have a density to be measured, and the method includes determining the density of one or more particles of particulate matter relative to the density to be measured, for example, determining whether one or more particles of particulate matter in a sample have a density higher, lower, or similar to the density to be measured.
[0110] In one embodiment, at least one property related to the dry particulate matter includes determining the setting time, such as the setting time in two different liquid dispersion media.
[0111] In one embodiment, at least one property related to the dry particulate matter includes the qualitative and / or quantitative determination of the presence of impurities.
[0112] The method of the present invention has been found to include qualitative and / or quantitative determination of the presence of impurities, which can be identified, for example, by morphological parameters, shape parameters, and / or density parameters. The method of the present invention has been found to be very rapid and effective for identifying impurities in dry particulate matter. This may be particularly desirable for quality control of raw materials.
[0113] [Claim 48] A processing method comprising determining at least one property relating to the particulate matter, wherein the particulate matter is dry particulate matter, and the processing method comprises the method according to any one of claims 1 to 46.
[0114] The present invention also includes the use of the above-described method as a tool for performing at least one of process optimization, process development, and quality control of a manufacturing process that involves producing a product containing dry particulate matter.
[0115] The present invention further includes a processing method comprising determining at least one property relating to particulate matter, wherein the particulate matter is dry particulate matter, and the processing method comprises the method described above.
[0116] Advantageously, the processing method includes determining whether at least one determined characteristic meets a quality criterion. The criterion may be any criterion related to particulate matter. The quality criterion may preferably include at least one threshold or threshold range for at least one characteristic. The at least one threshold may include, for example, a threshold value, and if it is determined that the determined characteristic has a value exceeding the threshold, then the determined characteristic meets the quality criterion.
[0117] In one embodiment, the process includes producing a product using dried particulate matter as a raw material, and / or producing dried particulate matter as a precursor product or final product.
[0118] In one embodiment, the process includes analyzing raw materials for use in the manufacture of a product, wherein the dried particulate matter forms part of the raw materials. The raw materials may include, for example, natural materials, pre-treated natural materials such as mechanical treatments, such as crushing, grinding, washing, drying, filtering, or any combination including at least one of the above treatments.
[0119] Examples of natural materials include sand, soil, and rocks (crushed and ground).
[0120] In embodiments in which the process involves analyzing raw materials for use in the manufacture of a product, at least one characteristic may include qualitative and / or quantitative content of at least one element, such as qualitative and / or quantitative content of a mineral. The method may conveniently include a step of determining whether the content of at least one element meets a quality criterion. The quality criterion may include, for example, a minimum threshold, a maximum threshold, and / or a threshold range for the required content of at least one element. In some embodiments, the quality criterion may include a quality criterion for the mineral and / or a criterion related to how easy or difficult it may be to extract from dry particulate matter.
[0121] In one embodiment, the process includes producing a dry particulate matter as a precursor product. The method may advantageously include taking a sample of the particulate matter during or after a process step, such as a granulation process step, a grinding process step, a washing step, a reaction step, or any other process step from which a sample of the particulate matter can be taken for analysis. The particulate matter may optionally be dried to obtain a dry particulate matter. At least one property related to the dry particulate matter can then be determined as described above.
[0122] In one embodiment, the process includes producing dry particulate matter as a final product, such as a final product ready for packaging and / or a final product ready for transport to a distributor or purchaser. The method may conveniently include taking a sample of the produced dry particulate matter and determining at least one property related to the sample of dry particulate matter using the method described above.
[0123] In one embodiment, the method includes the steps of taking a sample of dry particulate matter, such as dried particulate matter, after storage for a selected period under selected storage conditions, and determining at least one property related to the stored dry particulate matter. This can determine whether the dry particulate matter has changed during storage, for example, in a negative or positive way.
[0124] Advantageously, the method includes monitoring at least one property associated with the dry particulate matter. Monitoring may include, for example, taking samples of the stored dry particulate matter at selected time intervals and determining at least one property associated with the stored dry particulate matter. Thereafter, potential changes in at least one property associated with the stored dry particulate matter can be monitored in a relatively simple manner. The time slots between sample taking may be selected depending on prior experience and / or the expected duration for the occurrence of a detectable change in at least one property.
[0125] In one embodiment, the method may be applied to optimize storage conditions by, for example, storing a portion of the dry particulate matter under different conditions such as different temperatures and / or humidity. After a selected period, the stored portion of the dry particulate matter may be subjected to the determination of at least one property related to the stored dry particulate matter using the method described above, and the quality of each portion of the stored dry particulate matter may be compared to determine the best storage conditions. This method can be repeated until satisfactory storage conditions are determined.
[0126] At least one property may, advantageously, include at least one chemical or physical property, and the method may conveniently include determining whether at least one determined property meets a quality criterion. Optionally, the quality criterion may include two or more thresholds, for example, as described above.
[0127] If it is determined that at least one determined characteristic meets the quality standard, the method may preferably include continuing production. Optionally, the method may also include adjusting the quality standard to improve the quality of the dry particulate matter (e.g., raising the quality bar).
[0128] If it is determined that at least one determined characteristic does not meet the quality standard, the method may, advantageously, ultimately involve adjusting one manufacturing parameter. The dry particulate matter or particulate matter from which the sample is taken may optionally be subjected to additional processing as needed, or used for another purpose for which the quality standard is lower than that in the first intended use. Optionally, the method may include, on the day before, discharging the dry particulate matter or particulate matter from the location from which the sample was taken if the quality of the dry particulate matter or particulate matter is too low. This prevents further resource consumption of particulate matter that is too low in quality.
[0129] Brief Description of Embodiments and Examples The present invention will be further described below by a description of some exemplary and non-limiting embodiments and examples of the present invention with reference to the attached drawings.
[0130] The drawings are schematic, not drawn to scale, and may be simplified for clarity. Throughout, the same reference numbers are used for the same or corresponding parts. [Brief explanation of the drawing]
[0131] [Figure 1] This is a perspective top view of a sample support suitable for use in embodiments of the method of the present invention. [Figure 2] The diagram shows a process diagram of an embodiment of the method of the present invention, in which dry particulate matter is a raw material or precursor material for the production of the product. [Figure 3] Another process diagram of an embodiment of the method of the present invention is shown, in which the dry particulate matter is a raw material or precursor material for the production of the product. [Figure 4] The diagram shows a process diagram of one embodiment of the processing method of the present invention, which includes controlling and optionally adjusting one or more operating parameters. [Figure 5a] This shows different procedures for embodiments of the processing method of the present invention. [Figure 5b] This shows different procedures for embodiments of the processing method of the present invention. [Figure 5c] This shows different procedures for embodiments of the processing method of the present invention. [Figure 6] The scanning results of a scanning procedure according to one embodiment of the method of the present invention, in which the dry particulate matter is sand, are shown. [Figure 7] The scanning results of a scanning procedure according to one embodiment of the method of the present invention, in which the dried particulate matter is a food product, are shown. [Figure 8] The results of four scanning steps in one embodiment of the method of the present invention are shown, in which the dry particulate matter is a food product and the liquid dispersion medium is an active liquid dispersion medium. [Figure 9] Figure 8 shows the determined reaction derived from the scanning results.
[0132] The sample support shown in Figure 1 is in the form of a sample container 1 comprising a sample chamber 2, an inlet pipe section 3 into the sample chamber 2, and an outlet pipe section 4 from the sample chamber 2. The inlet pipe section 3 is equipped with a backflow prevention valve 3a to resist or prevent backflow from the sample chamber, and the outlet pipe section 4 is equipped with a backflow prevention valve 4a to resist or prevent backflow into the sample chamber. In its modifications, the backflow prevention valves 3a and 4a may be omitted, and undesirable backflow may optionally be controlled by a pump system (not shown) that controls the supply of dispersed sample into and out of the sample chamber 2. The sample container 1 is equipped with a handgrip 5 with a protruding flange 5a for better gripping. The sample container 1 is fitted to be inserted into a sample container slot of the sample container 1 which is fitted to perform one or more scanning procedures, and is optionally programmed to determine at least one characteristic based on the acquired image and / or processed acquired image. Alternatively, determining at least one characteristic based on the acquired image and / or processed acquired image may be performed by an external computer such as a laptop, tablet, or smartphone, which may conveniently communicate data with the scanning device via wired or wireless means. Examples of suitable scanning devices are described in US7634129 and US8780181.
[0133] When inserting the sample container 1 into the slot of the scanning device, the operator can shape the sample container 1 with the handgrip 5 and insert the sample container into the slot until the sample container 1 reaches a position where the projections 6a and 6b engage with the snap-lock cavity, ensuring that the sample container is securely positioned in the correct fixed position.
[0134] Here, the operator may stipulate that the first sample portion of the dispersed sample is supplied to the sample chamber 2 via the inlet pipe section 3. While the first sample portion of the dispersed sample is supplied into the sample chamber 2, the gas flows out of the sample chamber 2 via the outlet pipe section 4 until the sample chamber is full.
[0135] At this point, the supply of the first sample portion is complete, and one or more scanning procedures on the first sample portion can be initiated. Once the acquisition of the light transmission image is complete, the first sample portion can be pushed out of the sample chamber 2 by supplying the second sample portion into the sample chamber 2 via the inlet tube section 3, or by supplying gas and / or washing solution into the sample chamber 2 via the inlet tube section 3. The procedure can then proceed.
[0136] The supply of the sample portion, gas, and / or washing solution may be performed manually, or partially or fully automatically.
[0137] The process diagram in Figure 2 illustrates the process for controlling, selecting, and / or modifying raw or precursor materials for preparing products, for example, in construction applications. For many products, quality, such as one or more properties of the raw material, can vary significantly to such an extent that it may be difficult to achieve the desired quality of the final product.
[0138] By determining the static and / or dynamic properties of the raw material components and precursor material components, it is possible to accurately estimate the properties of the final product. This enables dynamic formulation optimization, depending on the determined static and / or dynamic properties of the raw material components, which are arbitrarily combined, taking into account requirements for the properties of the final product, such as the cost of the raw materials and / or the quality standards of the final product.
[0139] In step 11a, a first portion of the particulate raw material or precursor product is prepared for analysis. In step 12a, a sample of the first portion is analyzed according to an embodiment of the method of the present invention. The dispersed sample is provided in a sample container, and at least one scanning procedure is performed to determine one or more properties related to the first portion of the particulate raw material or precursor product.
[0140] This procedure is repeated for the second portion of the particulate raw material or precursor product, as shown in steps 11b and 12b.
[0141] Further portions of particulate raw materials or precursor products may be analyzed, for example, in the same manner in which such portions are supplied at the factory and / or prepared for use in the production of the product.
[0142] Each portion of the particulate raw material or precursor product may, advantageously, be each batch that can be received from a lower-level feeder or produced in a previous production step, for example, as an intermediate product.
[0143] Step 13 involves estimating product characteristics based on each part of the particulate raw material or precursor product. Step 14 involves formula optimization calculations and / or selection of raw materials or precursor products. This may include, for example, that parts of the particulate raw material or precursor product that are estimated to yield a final product having a quality that meets one or more quality criteria of the final product may be sent directly for use in production. Parts of the particulate raw material or precursor product that are estimated to yield a final product having a quality that does not meet one or more quality criteria of the final product may be discharged, or, where possible, mixed with one or more other parts of the particulate raw material or precursor product, or sent for use in production as desired, or returned to a step to be tested for further analysis.
[0144] The process diagram shown in Figure 3 illustrates a process that includes inspection and / or monitoring of raw materials or precursor materials, such as incoming raw materials or pre-treated or produced raw materials. Raw materials may include, for example, natural materials, such as dry sand, soil or gravel or other extractable materials. In one embodiment, particulate material is precursor material in the form of crushed material from a mining process. Here, it is usually important to evaluate the quality, such as mineral composition and concentration or the content of mineral material containing target minerals or metals. Using static and dynamic powder analysis according to one embodiment of the present invention, it is possible to determine in a relatively quick and effective way whether the raw material or precursor material meets quality criteria, for example, whether a sufficient amount of target minerals or metals is present, and if the mined material meets certain quality constraints, the extraction of such target minerals or metals can be continued, and stopped if the extraction becomes unfeasible.
[0145] In step 21, a portion of the particulate raw material or precursor product is prepared for analysis. In step 22, the first portion of the sample is analyzed according to an embodiment of the method of the present invention. The dispersed sample is provided in a sample container, and at least one scanning procedure is performed to determine one or more properties related to the portion of the particulate raw material or precursor product.
[0146] In step 23, it is determined whether the incoming raw materials / precursor materials meet the quality standards, for example, whether a sufficient amount of the target mineral or metal is present.
[0147] If one or more quality criteria are not met, the manufacturing process, including further extraction, is stopped at step 24.
[0148] If one or more quality criteria are met, the manufacturing process, including further extraction, continues in step 25.
[0149] If one or more quality criteria are partially met, the manufacturing process, including further extraction, is stopped in step 26, and the raw materials or precursor products may be further processed or pre-treated, for example, by a further crushing step, and the raw materials or precursor products are returned to step 22 for further analysis.
[0150] The process diagram shown in Figure 4 illustrates a process involving the dynamic optimization of one or more operating conditions for powder production, such as a spray drying process. Here, obtaining high-quality granulation, particle size distribution, and / or shape distribution of the produced product may be important. Furthermore, in processes such as multi-component spray drying and / or encapsulation, it may be beneficial to simultaneously obtain measurements of bulk powder properties and particle composition. If the obtained properties do not meet selected quality constraints, the process may be dynamically controlled by changing the selection of operating parameters.
[0151] In step 31, production is initiated by forming one or more starting materials. In step 32, preferably, a sample is taken at least after the production process has been carried out for a sufficiently long time for one or more starting materials to be affected by the process. In step 33, the sample is analyzed according to an embodiment of the method of the present invention. The dispersed sample is provided in a sample container and at least one scanning procedure is performed to determine one or more properties related to one or more particulate matter.
[0152] In step 34, it is determined that at least one quality criterion is met. If one or more quality criteria are met, manufacturing continues in step 35 with the operating parameters unchanged. If one or more quality criteria are not met, a feedback loop is provided to correct one or more operating parameters of the process before sampling. One or more further samples may be taken to control the operating parameters along the production process until final production.
[0153] The process diagrams shown in Figures 5a to 5c illustrate examples of different procedures in embodiments of the processing method of the present invention.
[0154] The process diagram in Figure 5a shows an example of a method for determining at least one static property.
[0155] In step 41, a dry particulate matter (in this case, a powder) is provided, and the sample is dispersed in an inert dispersion medium, such as a liquid dispersion medium, which does not react with or dissolve the particulate matter or any portion thereof before or during image acquisition.
[0156] In step 42, the sample is analyzed by an embodiment of the method of the present invention, which includes providing a dispersed sample in a sample container and performing at least one scanning procedure. In step 43, at least one static property is determined, for example, as described above.
[0157] In step 44, it is determined, for example, whether the dry particulate matter meets at least one quality criterion by correlating at least one determined static property with a selected threshold and / or by correlating at least one determined static property with a reference curve.
[0158] The process diagram in Figure 5b shows an example of a method for determining at least one dynamic characteristic.
[0159] In step 51, a dry particulate matter (here, a powder) is provided, and the sample is dispersed in an active dispersion medium, such as a liquid dispersion medium, which has or is suspected to have reactivity with and / or a dissolving effect on at least one compound or element of the particulate matter.
[0160] In step 52, the sample is analyzed by an embodiment of the method of the present invention, which includes providing a dispersed sample in a sample container and preferably performing at least two scanning procedures having time slots between them, the time slots having a duration sufficient to allow the liquid dispersion medium to react with and dissolve at least one compound or element of the particulate matter. One or more additional scanning procedures can be performed over time to observe the reaction and / or dissolution as a function of time.
[0161] In step 53, at least one dynamic characteristic is determined, for example, as described above. It should be noted that steps 52 and 53 may be determined interleaved or integrated, for example, as described above.
[0162] In step 54, it is determined, for example, whether the dry particulate matter meets at least one quality criterion by correlating at least one determined static property with a selected threshold and / or by correlating at least one determined static property with a reference curve.
[0163] In step 61, a first sample of dry particulate matter (in this case, powder) is provided, and the sample is dispersed in a liquid dispersion medium, which may be an active liquid dispersion medium or an inert liquid dispersion medium.
[0164] In step 62, the first sample is analyzed by an embodiment of the method of the present invention, which includes providing a dispersed sample in a sample container and performing at least one scanning procedure.
[0165] After a selected time slot, for example, after the dry particulate matter has been stored under selected storage conditions for several days, several weeks, several months, or even several years, a second sample of the dry particulate matter is withdrawn in step 63 and dispersed in a liquid dispersion medium.
[0166] In step 64, the first sample is preferably analyzed in the same manner as the first sample.
[0167] In step 65, it is determined whether any changes have occurred, such as deterioration including a moisture absorption reaction or decomposition of the dry particulate matter.
[0168] This embodiment may be very useful for storing dry particulate matter or controlling its storage conditions, and / or optimizing those storage conditions.
[0169] Figure 6 shows the scanning results of the analysis of a sand sample. It can be seen that embodiments of the method of the present invention provide detailed information regarding the particles of the sand sample. Based on the processed images, the particle size distribution, morphological details, and other properties described above can be determined. In this example, three target mineral particle types A, B, and C are identified, and their magnified images are provided. Based on the processed images, the quantitative content of each mineral can be determined.
[0170] Figure 7 shows the scanning results of an analysis of a food product, such as an instant dried food product, containing multiple components. Based on the processed image, particles of each component, such as component A, component B, and component C, were identified. Size, size distribution, morphological details, and other properties (e.g., those described above) can be determined. Furthermore, the homogeneity of the food product can be determined. The particle size and particle distribution of the various components can significantly affect the texture and rheology of the final product manufactured from the food product or dried instant food product.
[0171] Figure 8 shows the scanning results of four scanning steps of one embodiment of the method of the present invention, in which the dry particulate matter is a food product and the liquid dispersion medium is an active liquid dispersion medium. The four scanning steps are performed at time 1, time 2, time 3, and time 4, respectively. Four different particles are analyzed, and it can be seen that the liquid dispersion medium caused gelation in at least particles 1 and 2, but no significant signs of gelation were observed in particles 3 and 4.
[0172] In Figure 9, the particles are further analyzed for changes in particle size, and the particle size as a function of time is plotted. It can be seen that particle 1 and particle 2 each have a substantial increase in particle size over time, but no signs of increase in particle size are observed for particle 3 and particle 4.
Claims
1. A method for determining at least one property relating to particulate matter, comprising providing a portion of the particulate matter, wherein the particulate matter and the portion thereof are dry particulate matter. The method is, [a] A step of providing a sample support capable of containing a liquid medium, [b] A step of providing a dispersed sample which includes a portion of the particulate matter dispersed in a portion of the liquid dispersion medium in the sample support, [c] A step of performing at least one scanning procedure, A procedure for acquiring multiple light-transmitted images of an image acquisition region translated along a scanning path through the dispersed sample in the sample support using an image acquisition device having an optical axis, (c1) A procedure for processing multiple acquired images, and a procedure having (c2) A step comprising a procedure for determining the at least one characteristic, The method wherein the image acquisition region is perpendicular to the optical axis of the image acquisition device.
2. The aforementioned dry particulate matter includes powder. The method according to feature 1.
3. The aforementioned dry particulate matter includes particles having a particle size of 1 mm or less, for example, 0.5 mm or less, for example, 0.1 mm or less. The method according to 1 or 2, characterized by the features described above.
4. The method includes the step of preparing a dispersed sample by a method comprising mixing the dry particulate matter with the liquid dispersion medium, wherein the concentration of the particulate matter does not exceed 40 mg per 1 mL of the liquid dispersion medium, and the method preferably includes the step of providing the particulate matter and the liquid dispersion medium to the sample support in a flow such as a gentle flow, and preferably the concentration of the particulate matter is 1 to 35 mg / ml of the liquid dispersion medium, for example 5 to 20 mg / ml of the liquid dispersion medium, for example 8 to 15 mg / ml of the liquid dispersion medium. A method according to any one of the prior claims, characterized in that
5. The step of providing a dispersed sample includes the step of dispersing the particulate matter without requiring stirring. A method according to any one of the prior claims, characterized by the following:
6. The step of processing the image includes the step of obtaining a set of images of the acquired image, and preferably the step of determining the at least one characteristic includes the step of determining the at least one characteristic at least partially from the set of images. A method according to any one of the prior claims, characterized by the following:
7. The image set includes at least two different images containing the same particles of the particulate matter of the dispersed sample, and preferably the image set includes three or more different images containing the same particles of the particulate matter of the dispersed sample. The method according to feature 6.
8. The method according to any one of the prior claims, wherein the scanning procedure includes the step of performing a subdetermination of the at least one characteristic, and the determination of the at least one characteristic includes the step of determining the at least one characteristic at least partially from the subdetermination of the at least one characteristic.
9. The step of performing at least one scanning procedure includes performing two or more scanning procedures, and the determination of the at least one characteristic includes the step of determining the at least one characteristic at least partially from the subdeterminations of the at least one characteristic of the two or more scanning procedures. The method according to feature 8.
10. Acquiring multiple light-transmitted images of the image acquisition region along the scanning path through the dispersed sample in the sample support includes the steps of illuminating at least the image acquisition region along the scanning path by emitting light from an illumination device through the dispersed sample toward the image acquisition device, and acquiring the light-transmitted images using the image acquisition device. A method according to any one of the prior claims, characterized by the following:
11. The step of illuminating the image acquisition area includes emitting a light beam from the illumination device toward the image acquisition device, wherein at least a portion of the light beam passes through the acquisition area and reaches it, and the method includes shaping the light beam such that it is focused in the acquisition area. A method according to any one of the prior claims, characterized by the following:
12. Acquisition of multiple light-transmitted images of the image acquisition region along the scanning path through the dispersed sample in the sample support includes the step of acquiring the light-transmitted image of the image acquisition region at each selected position along the scanning path. A method according to any one of the prior claims, characterized by the following:
13. Acquisition of multiple light-transmitted images of the image acquisition region along the scanning path through the dispersed sample in the sample support comprises the steps of translating the image acquisition region stepwise along the scanning path and acquiring the light-transmitted images between the movements of each step of the stepwise translation, wherein the lengths of each step are preferably equal or different, more preferably up to 1 cm, for example, 1 μm to 0.5 cm. A method according to any one of the prior claims, characterized by the following:
14. The scanning path includes at least one linear path length section in the horizontal plan, and the image acquisition area has an angle of 2 to 20 degrees with respect to the path length, preferably an angle of 5 to 15 degrees with respect to the path length, such as 6 to 7 degrees. A method according to any one of the prior claims, characterized by the following:
15. The method includes the step of selecting the liquid dispersion medium such that it is non-reactive and / or non-soluble with the particulate matter during the acquisition of at least a plurality of light transmission images. A method according to any one of the prior claims, characterized by the following:
16. The method includes selecting a liquid dispersion medium that is reactive and / or soluble with respect to at least a portion of the particulate matter. The method according to any one of the prior claims 1 to 14, characterized in that
17. The liquid dispersion medium is reactive, or suspected to be reactive, with respect to at least one compound or element of the particulate matter, such as a chemical or physical reaction including a reaction that causes decomposition, a reaction that causes structural change, a substitution reaction, a polymerization reaction, a swelling reaction, a gelling reaction, or any combination thereof. The method according to 16, characterized by...
18. The liquid dispersion medium has, or is suspected to have, a dissolving effect on at least one compound or element of the particulate matter, such as a salt. The method according to 16 or 17, characterized by the features described herein.
19. The step of performing at least one scanning procedure includes the step of performing two or more consecutive scanning procedures, and the determination of at least one characteristic includes the step of determining whether a reaction and / or dissolution has occurred, preferably the method includes the step of determining the extent of the reaction and / or dissolution that has occurred, more preferably the step of determining the extent of the reaction and / or dissolution that has occurred as a function of time. A method according to any one of the prior claims, characterized by the following:
20. The step of performing at least one scanning procedure includes the step of performing two or more consecutive scanning procedures, wherein the liquid dispersion medium in the first scanning procedure of the two or more scanning procedures differs from the liquid dispersion medium in the second scanning procedure of the two or more scanning procedures, preferably the liquid dispersion medium in the first scanning procedure differs in temperature and / or in that it contains additives such as pH adjusting additives, reactants, surfactants, refractive index adjusting agents such as salts, or any combination thereof. A method according to any one of the prior claims, characterized by the following:
21. The step of performing at least one scanning procedure includes the step of performing two or more consecutive scanning procedures, wherein the dispersed sample in at least one first scanning procedure of the two or more scanning procedures is affected by selected radiation and / or fields selected from electromagnetic radiation, magnetic fields and / or electric fields, and the dispersed sample in at least one second operating procedure of the two or more scanning procedures is not exposed to the selected electromagnetic radiation, magnetic fields and / or electric fields, or is exposed to different levels of selected electromagnetic radiation, magnetic fields and / or electric fields. A method according to any one of the prior claims, characterized by the following:
22. The method includes the step of selecting the liquid dispersion medium such that it is transparent to at least one wavelength of light emitted from the illumination device through the dispersed sample. A method according to any one of the prior claims, characterized by the following:
23. The method includes the step of selecting the liquid dispersion medium such that it has a refractive index determined by at least one wavelength of light emitted from an illumination device, which is different from the refractive index of the dry particulate matter, preferably the liquid dispersion medium is selected such that it has a refractive index determined by at least one wavelength of light emitted from an illumination device, and which is different from the refractive index of at least a portion of the dry particulate matter by 0.01 to 0.
1. A method according to any one of the prior claims, characterized by the following:
24. The method includes the step of selecting the liquid dispersion medium such that it has a neutralizing effect on the electrostatic interactions between particles of the dry particulate matter. A method according to any one of the prior claims, characterized by the following:
25. The aforementioned liquid dispersion medium is a non-polar liquid such as oil. A method according to any one of the prior claims, characterized by the following:
26. The liquid dispersion medium is a polar liquid such as an aqueous liquid like tap water, distilled water, and / or deionized water. A method according to any one of the prior claims, characterized by the following:
27. The light emitted from the lighting device preferably includes one or more wavelengths selected in the range of 380 to 940 nm, and preferably includes at least one wavelength in the range of 400 to 900 nm. A method according to any one of the prior claims, characterized by the following:
28. The light emitted from the lighting device includes light from a light source adapted to emit monochromatic or nearly monochromatic light having a bandwidth of up to 50 nm, preferably up to 10 nm, for example, up to 5 nm. A method according to any one of the prior claims, characterized by the following:
29. The method includes the step of illuminating the image acquisition area using two or more light sources having the same or different wavelengths, and / or by two or more light beams having the same or different wavelengths. A method according to any one of the prior claims, characterized by the following:
30. The light emitted from the lighting device includes structured light, such as structured light, which comprises a group of electromagnetic waves emitted from the lighting device and propagating along a parallel or convergent direction, the structured light being textured as seen in a cross-sectional view perpendicular to the central axis of the group of electromagnetic waves, and the light preferably having an intensity distribution in the cross-sectional view which includes regions of higher intensity and regions of lower intensity or no intensity, and the intensity distribution is different from the natural Gaussian intensity distribution of the light beam. A method according to any one of the prior claims, characterized by the following:
31. At least a portion of the sample wall, such as the bottom wall and / or top wall of the sample support, including the entire sample support, is transparent to at least one wavelength of light emitted from the illumination device through the dispersed sample. A method according to any one of the prior claims, characterized by the following:
32. The sample support is in the form of a sample container comprising an inlet for supplying a dispersed sample to the sample support and an outlet for air or a previously dispersed sample. A method according to any one of the prior claims, characterized by the following:
33. At least one of the multiple light transmission images is acquired through a polarizing filter, such as a polarizing lens, in the image acquisition device. A method according to any one of the prior claims, characterized by the following:
34. The aforementioned dry particulate matter includes particles up to 5 cm in size, for example, in the range of 0.1 μm to 1 cm. A method according to any one of the prior claims, characterized by the following:
35. The dry particulate matter includes inorganic particles, such as sand, minerals, clay and / or salt and / or organic particles, such as particles selected from food, pharmaceuticals, polymers and / or raw materials. A method according to any one of the prior claims, characterized by the following:
36. The method includes a step of pre-drying the particulate matter to remove at least some of the unbound water, the pre-drying step including drying to a certain weight at a selected temperature, the selected temperature being a temperature that does not chemically affect the particulate matter, for example, less than 100°C, for example, between 30 and 90°C. A method according to any one of the prior claims, characterized by the following:
37. The dry particulate matter has an unbound water content of up to 15% by weight, for example, up to 10% by weight. A method according to any one of the prior claims, characterized by the following:
38. Each step of performing at least one scanning procedure includes acquiring a plurality of light transmission images, preferably for one or more particles of the particulate matter, acquiring an image set which includes at least one image in which the particle is in focus and at least one image in which the particle is out of focus, and the image set preferably includes at least three images. A method according to any one of the prior claims, characterized by the following:
39. The method includes processing the acquired light transmission image to synthesize a 3D image of at least a certain volume of the particulate matter in the dispersed sample. A method according to any one of the prior claims, characterized by the following:
40. The step of performing at least one scanning procedure includes the step of performing two or more consecutive scanning procedures, each including the step of acquiring an image of the common portion of the dispersed sample, and optionally the step of determining whether changes such as changes over time, such as degradation, have occurred. A method according to any one of the prior claims, characterized by the following:
41. The method includes the step of performing two or more runs of determining at least one property relating to the dry particulate matter, wherein the two or more runs are different in time, different in the liquid dispersion medium, different in the physical influence of the dispersed sample, and / or in the difference in the concentration of the particulate matter in the liquid dispersion medium. A method according to any one of the prior claims, characterized by the following:
42. Providing the dispersed sample in the sample support comprises the steps of: dispersing at least a portion of the dry particulate matter in at least a portion of the liquid dispersion medium; applying the dispersed sample, which includes the portion of the dry particulate matter dispersed in the portion of the liquid dispersion medium in the sample support; or applying the portion of the dry particulate matter and the portion of the liquid dispersion medium to the sample support, provided that the portion of the dry particulate matter is dispersed in the portion of the liquid dispersion medium in the sample support. A method according to any one of the prior claims, characterized by the following:
43. The method includes the step of preparing a dispersed sample by a method that includes the step of mixing the dried particulate matter with the liquid dispersion medium, wherein the concentration of the particulate matter does not exceed 40 mg of the particulate matter per 1 mL of the liquid dispersion medium, and optionally the method includes the step of preparing a parent sample and the step of taking the dispersed sample from the parent sample. A method according to any one of the prior claims, characterized by the following:
44. At least one property relating to the dry particulate matter is, Morphological characteristic parameters of the dry particulate matter, The particle size characteristic parameters of the aforementioned dry particulate matter, The shape characteristic parameters of the dry particulate matter, The purity characteristics of the aforementioned particulate matter, Quantification of the dry particulate matter of one or more particle types, The residual water content of the aforementioned dried particulate matter, Particle distribution of one or more individual particle characteristics of the dry particulate matter, Gas (gas bubble) generation related to the aforementioned dry particulate matter, Characteristics of the density of the aforementioned particulate matter, The fluidity characteristics of the aforementioned particulate matter, The reactivity characteristics of the particulate matter, Characteristics of the solubility of the aforementioned particulate matter, The wetting characteristics of the particulate matter, The hygroscopic characteristics of the particulate matter, and / or, Any combination that includes one or more of these characteristics, including A method according to any one of the prior claims, characterized by the following:
45. At least one property relating to the dry particulate matter includes density parameters such as the homogeneity / heterogeneity of the density of the particles of the dry particulate matter, such as the density level of one or more particles of the dry particulate matter. A method according to any one of the prior claims, characterized by the following:
46. At least one property relating to the dry particulate matter includes determining the setting time, such as the setting time in two different liquid dispersion media. A method according to any one of the prior claims, characterized by the following:
47. At least one property related to the dry particulate matter includes qualitative and / or quantitative determination of the presence of impurities. A method according to any one of the prior claims, characterized by the following:
48. The use of the method of any one of the preceding claims, wherein the step of performing at least one of process optimization, process development and quality control of a manufacturing process includes the step of producing a product containing particulate matter.
49. A processing method comprising determining at least one property relating to the particulate matter, wherein the particulate matter is the dried particulate matter, and the processing method comprises the method according to any one of claims 1 to 47.
50. The method includes a step of determining whether at least one determined characteristic satisfies a quality criterion, preferably the quality criterion includes at least one threshold or threshold range for the at least one characteristic. The processing method according to feature 48.
51. The processing steps include a step of producing a product that uses the dried particulate matter as a raw material, and / or a step of producing the dried particulate matter as a precursor product or a final product. The processing method according to claim 49 or 50.
52. The processing step includes analyzing the raw materials for use in the manufacture of a product, wherein the dried particulate matter forms part of the raw materials. The processing method according to any one of claims 49 to 51.
53. The raw materials include natural materials that have undergone pretreatment, such as mechanical treatment including crushing, grinding, washing, drying, filtering, or any combination of at least one of the above treatments. The processing method according to feature 52.
54. At least one characteristic includes the content of at least one element, such as a mineral, and the method includes the step of determining whether the content of the at least one element meets a quality criterion, preferably the quality criterion includes a minimum threshold, a maximum threshold, and / or a threshold range for the required content of the at least one element. The processing method according to claim 52 or 53, characterized by the features described above.
55. The processing step includes producing the dried particulate matter as a precursor product, and the method includes taking a sample of the particulate matter during or after a processing step such as a granulation process, a grinding process, a washing step, or a reaction step, optionally drying the particulate matter to obtain the dried particulate matter, and determining at least one property related to the dried particulate matter. The method according to any one of claims 52 to 54.
56. The processing step includes producing the dried particulate matter as the final product, the method including taking a sample of the produced dried particulate matter and determining at least one property related to the sample of the dried particulate matter. The processing method according to any one of claims 52 to 55, characterized by the following:
57. The method includes the steps of taking a sample of the dried particulate matter produced after storage under selected storage conditions for a selected period of time, and determining at least one property related to the stored dried particulate matter, preferably the method includes monitoring the at least one property related to the dried particulate matter, which includes taking a sample of the stored dried particulate matter at selected time intervals and determining at least one property related to the stored dried particulate matter. The processing method according to claim 56, characterized in that it includes the following.
58. At least one property includes at least one chemical or physical property, and the method includes determining whether at least one determined property meets a quality criterion, optionally the quality criterion including two or more thresholds. The processing method according to any one of claims 55 to 57, characterized by the following:
59. If at least one determined characteristic meets the quality criteria, the method includes the step of continuing production, and optionally, the method includes the step of adjusting the quality criteria to improve the quality of the dry particulate matter. The processing method according to feature 58.
60. If at least one determined characteristic does not meet the quality standard, the method includes the steps of adjusting the last remaining manufacturing parameter and optionally, discharging the dry particulate matter / particulate matter from the location from which the sample was taken. The processing method according to feature 58.