EP2430411A2 - Analyse automatique de fines particules de matière solide - Google Patents

Analyse automatique de fines particules de matière solide

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Publication number
EP2430411A2
EP2430411A2 EP10718197A EP10718197A EP2430411A2 EP 2430411 A2 EP2430411 A2 EP 2430411A2 EP 10718197 A EP10718197 A EP 10718197A EP 10718197 A EP10718197 A EP 10718197A EP 2430411 A2 EP2430411 A2 EP 2430411A2
Authority
EP
European Patent Office
Prior art keywords
sample
solids
analysis
finely divided
vessels
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP10718197A
Other languages
German (de)
English (en)
Inventor
Karen Vercruysse
Frans Suykerbuyk
Sven Veelaert
Veron Nsunda
Kris Wullus
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BASF SE
Original Assignee
BASF SE
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by BASF SE filed Critical BASF SE
Priority to EP10718197A priority Critical patent/EP2430411A2/fr
Publication of EP2430411A2 publication Critical patent/EP2430411A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01F—MEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
    • G01F11/00—Apparatus requiring external operation adapted at each repeated and identical operation to measure and separate a predetermined volume of fluid or fluent solid material from a supply or container, without regard to weight, and to deliver it
    • G01F11/10—Apparatus requiring external operation adapted at each repeated and identical operation to measure and separate a predetermined volume of fluid or fluent solid material from a supply or container, without regard to weight, and to deliver it with measuring chambers moved during operation
    • G01F11/12—Apparatus requiring external operation adapted at each repeated and identical operation to measure and separate a predetermined volume of fluid or fluent solid material from a supply or container, without regard to weight, and to deliver it with measuring chambers moved during operation of the valve type, i.e. the separating being effected by fluid-tight or powder-tight movements
    • G01F11/20—Apparatus requiring external operation adapted at each repeated and identical operation to measure and separate a predetermined volume of fluid or fluent solid material from a supply or container, without regard to weight, and to deliver it with measuring chambers moved during operation of the valve type, i.e. the separating being effected by fluid-tight or powder-tight movements wherein the measuring chamber rotates or oscillates
    • G01F11/24—Apparatus requiring external operation adapted at each repeated and identical operation to measure and separate a predetermined volume of fluid or fluent solid material from a supply or container, without regard to weight, and to deliver it with measuring chambers moved during operation of the valve type, i.e. the separating being effected by fluid-tight or powder-tight movements wherein the measuring chamber rotates or oscillates for fluent solid material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/10—Devices for withdrawing samples in the liquid or fluent state
    • G01N1/12—Dippers; Dredgers
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0091—Powders
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
    • G01N35/1009—Characterised by arrangements for controlling the aspiration or dispense of liquids
    • G01N35/1016—Control of the volume dispensed or introduced

Definitions

  • the present invention relates to a solids metering device for finely divided solids, comprising removal means for removing a sample from a sample vessel and dosing means for introducing a predetermined amount of finely divided solid into a test vessel.
  • the invention relates to an automatic analyzer for determining properties of finely divided solids comprising a depot for sample vessels and test vessels, analysis devices for analyzing samples, manipulators for moving and positioning sample vessels, solids metering devices and metering devices for liquids.
  • the invention relates to a method for the automatic analysis of finely divided solids.
  • powders and solids in the form of pourable bulk solids are termed "finely divided solids.”
  • the particle sizes are in the range from 1 to 1500 micrometers ( ⁇ m).
  • water-absorbing polymers which are also referred to as superabsorbents. They consist of hydrophilic polymers that are so strongly cross-linked that they are no longer soluble. Their preparation is described, for example, in the monograph "Modern Superabsorbent Polymer Technology", FL Buchholz and AT Graham, Wiley-VCH, 1998, pages 71 to 103, and in Ullmann's Encyclopedia of Industrial Chemistry, 6th Edition, Volume 35, pages 73 to 93 Sieve analysis can be used to determine typical particle size distributions, with 90%, 95% or 98% of the particles in each case being in the range 150 to 850 ⁇ m.
  • WO 93/15407 describes a universal laboratory robot, in particular for use in the medical field. Samples of substances are provided in containers in a warehouse. In accordance with a defined sequence of steps, the robot transports the vessels from the warehouse to different analysis stations. There, the samples are automatically examined and then transported back by the robot back into the camp.
  • WO 97/47974 discloses a laboratory robot for the analysis of liquid, solid or powdered samples.
  • the laboratory is divided into a so-called robot zone and an operator zone, which are separated by a wall.
  • samples to be analyzed are exchanged between the zones.
  • different analysis stations are set up in which the samples can be automatically examined.
  • An at least five-axis robot can be moved on a longitudinal rail so that it can transport samples between different conveyor belts and the analysis stations.
  • JP 10077121 describes the dosage of finely divided solids in small amounts (1 to 5 mg), primarily for use in drug development.
  • the respective sample bottle is detected by a robot, the lid removed and set the bottle with the opening turned down on the metering device. By turning a brush, the required amount of solid is removed from the sample bottle and drizzled into the test vessel.
  • the invention described below was based on the object of providing an apparatus and a method for the automated analysis of finely divided solids, wherein it should be ensured that representative and comparable statements can be made with regard to the product properties.
  • another object was to develop a metering device for finely divided solids for use in said device.
  • the solids metering device comprises removal means for removing a sample from a sample vessel and dosing agent for introducing a predetermined amount of finely divided solid into a test vessel.
  • samples are usually taken, for example from the product tion process or the product ready for sale.
  • the sample should have a certain minimum amount to minimize statistical variations in particle sizes and their distribution. With a particle size of 150 to 850 microns, a sample amount of 1000 cm 3 has proven to be favorable.
  • Sample containers in which the sample is provided for analysis can be designed differently.
  • bottle-shaped vessels are also common in which the diameter narrows towards the opening.
  • the cross section may have different shapes such as circles, ovals, rectangles, hexagons, for example, with rounded corners.
  • the sample containers may also be closable, e.g. by turning, tilting or snap closures. Lockable sample containers are preferably used when the finely divided solids to be tested can change their properties by contact with the surrounding atmosphere, for example due to the oxygen content or the moisture in the air.
  • the sample is a mixture of many particles with different properties such as size and shape.
  • the properties of the mixture of interest in turn depend on the particle properties and thus on the composition of the mixture. It is therefore expedient to ensure the most uniform possible mixing of the sample in the sample vessel and to counteract adverse effects such as segregation. This can be done manually or automatically, for example by shaking or rotating the sample vessels or by stirring in the sample vessel.
  • test vessels To carry out the individual analyzes, partial quantities of the sample in test vessels are required.
  • the size, shape and nature of the test vessels depend on the method and the specific apparatus of the respective analysis to be performed.
  • Suitable test vessels may e.g. Beakers, bowls or measuring cells, which may be made of glass, plastic, metal or other materials.
  • the amounts of finely divided solids required in each test vessel vary depending on the substances to be analyzed and the analytical methods.
  • the required amounts in the test vessels are in a range of 0.2 to 2.0 g.
  • representative quantities of the sample of finely divided solids are taken from the sample vessels with the aid of removal means.
  • Representative in this context means that characteristics of the sample in the sample vessel as well as the particle size distribution are also found in the extracted subset.
  • Suitable extraction means are, for example, grippers, which dive into the sample in the opened state, close there and remove a partial amount of the sample from the sample vessel in the closed state.
  • a preferred embodiment Form forms a hollow lance, as will be explained below with reference to the drawings by way of example. It has an advantageous effect if a removal means displaces as small a volume as possible in the sample vessel or exerts only slight pressure on the solid particles in order to largely avoid unequal distribution, compression or damage of the solid particles. This effect can be achieved for example by a small cross-sectional area or a shape of the removal means, in which the diameter decreases in the direction of the immersed end or forms a tip.
  • dosing agents are used according to the invention. This may be e.g. to act conveyors in which the withdrawn subset is fed via a hopper on a screw. About the speed of the screw while the metered into a test vessel amount of finely divided solids can be influenced. In a variant, the screw can be replaced by a conveyor belt, the rotational speed can be controlled. In a preferred embodiment, the dosing agent contains a metering wheel as an essential element, which is explained in more detail with reference to the following drawings.
  • dosing agents should be designed so that dosing accuracies of at least 0.1 g, 0.01 g or 0.001 g are guaranteed.
  • the pitch of the screw, its diameter and the minimum to be set rotational speed can be selected accordingly.
  • the metering accuracy can e.g. be influenced by the choice of the roughness of the strip, its width and loading height and the rotational speed.
  • the amount of finely divided solids to be metered can be specified and controlled in various ways.
  • One possibility is to specify the filling level in the test vessel and to check the actually metered amount by a level measurement, for example by means of laser techniques or imaging techniques.
  • the mass of the dosed solid is determined, for example, by the fact that the test vessel is located on a weighing device during the dosing process.
  • a dosing agent according to the invention therefore provides the possibility of introducing the metered, finely divided solid into a test vessel in such a way that, with regard to the local distribution of the solid mixture and the distribution of the characteristics of the particles in the test chamber. mixed homogeneity. In one embodiment, this is ensured by providing a stirring tool which, during the dosing operation, mixes the solid particles dosed into the test vessel and, after completion of the dosing operation, smoothes the surface of the dosed solid amount. In a further embodiment, the test vessel is moved in one or more planes during the dosing process.
  • an analysis machine is used to determine the properties of the finely divided solids, which comprises a depot, analysis equipment, manipulators, solids metering devices and metering devices for liquids.
  • the solids metering devices are preferably embodiments according to the invention.
  • the depot provides an interface between the automated analysis of the samples and the operator of the automated analyzer. On the one hand, it enables the operator to set and remove sample containers and test containers. On the other hand, the corresponding vessels can be removed from a depot by a manipulator of the machine and set in the depot. Furthermore, a depot is used for the storage of sample containers and test vessels, for example, if a waiting time between analysis preparation and evaluation of the results is provided for an analysis method.
  • the automated analyzer includes one or more analyzers for analysis of particulate solids samples.
  • the specific configuration of the analysis devices depends on the respective analysis method. Examples of concrete analysis methods are given below for water-absorbing polymers.
  • At least one programmable manipulator is provided. Its design and functionality is closely related to the spatial arrangement of the other components of the automatic analyzer.
  • a manipulator capable of moving in three spatial directions (x, y, z) is suitable.
  • the manipulator may also have additional rotation axes, e.g. if it is necessary to perform a dosing or analysis, to turn a vessel.
  • depot on the one hand and metering devices and analysis devices on the other hand are arranged in two different spatial planes.
  • the manipulator can be advantageously arranged between the planes and can be about a rotational axis, in the radial direction perpendicular move to the axis and parallel to the axis.
  • further rotation axes can be provided, for example for rotation of a gripper.
  • manipulator which provides for the transport of sample containers and test vessels
  • further programmable manipulators can be provided in the automatic analyzer, for example in order to be able to move removal means and dosing means relative to one another. Often it is sufficient if such a manipulator is movable in a spatial direction.
  • the automated analyzer therefore comprises one or more metering devices for liquids.
  • a predetermined amount of liquid is metered into a test vessel. This can be realized by a weighing device detecting the weight of the test vessel and a controller based on this information influencing the inflow of liquid.
  • a flow meter can be used to detect the metered amount. For some test methods, a certain level in a test vessel must be ensured.
  • An embodiment of the invention provides for a metering device based on the principle of communicating tubes.
  • the level is detected by means of sensors and the metered addition, for example via a peristaltic pump, influenced accordingly.
  • the metering devices for liquids can be fixedly mounted in the automatic analyzer. In this case, a manipulator transports the test vessels to be filled to the metering devices.
  • a metering device for liquids can also be mounted in a manipulator, for example in the gripper, so that a liquid metering can take place at different locations in the automated analyzer. There may also be several metering devices for liquids.
  • the manipulators are programmed in such a way that their movements do not run jerkily and do not have too great an acceleration.
  • the setting of suitable parameters can, for example, be carried out in advance by simulation calculations or by tests during operation of the relevant manipulator.
  • the automated analyzer is particularly suitable for carrying out standardized analyzes of a large number of samples.
  • the analysis results are preferably provided in a form that they can be further processed electronically.
  • the analysis machine can have, for example, interfaces to a laboratory data information system (LIMS, Laboratory Information Management System) or an operating data information system (PIMS, Process Information Management System).
  • LIMS Laboratory Information Management System
  • PIMS Process Information Management System
  • data output by the automated analyzer can be archived and further processed for the respective samples, eg quantities of metered finely divided solids or liquids, fill levels, time periods, analysis results or status information.
  • the analysis machine can have further interfaces that allow it to be connected to a higher-level automation, for example to a process control system (PLS) or an enterprise resource planning (ERP) tool.
  • PLS process control system
  • ERP enterprise resource planning
  • the automatic analyzer according to the invention and the method according to the invention for the automatic analysis of finely divided solids can be used in different fields. They find advantageous use in the routine, routine analysis of a large number of samples, for example for quality control in continuous or discontinuous production processes.
  • Fig. 1a Top view of an arrangement of an automatic analyzer according to the invention
  • Fig. 1 b view of a manipulator in an arrangement according to Fig. 1 a
  • FIG. 2a shows a schematic diagram of a hollow lance as an embodiment of the invention a removal means in the open state
  • Fig. 2b Detail of a hollow lance of Fig. 2a in the closed state
  • Fig. 2c Schematic diagram of an alternative embodiment of a removal means in
  • FIG. 3 Schematic diagram of an embodiment according to the invention of a dosing agent with metering wheel
  • FIG. 1 a shows a possible arrangement of an automatic analyzer 1 according to the invention.
  • Depot 10, metering devices 30 and analysis devices 40 are located substantially in one plane.
  • a manipulator 20 which can transport sample containers and test vessels between the individual units.
  • 1 b schematically shows an embodiment of a manipulator 20 movable in three axes.
  • a manipulator carrier 22 In order to be movable in the x-direction, a manipulator carrier 22 is guided in guide rails 21, which are fastened to a wall of the analysis machine 1, for example.
  • a manipulator arm 23 can be displaced along the manipulator carrier 22 in the y direction.
  • Manipulator arm 23 and a gripper 24 located thereon realize the movement in the z-direction.
  • a hollow lance 310 as an inventive embodiment of a removal means is shown schematically.
  • the removal means is movably mounted in the y direction in order to be able to dip into a sample vessel 1 1. This can be realized in that the sampling means falls under the influence of gravity in the sample vessel 1 1 and immersed in the solid.
  • the removal means can also be actively introduced by a drive in the sample vessel 11.
  • the removal means is designed as a hollow lance 310.
  • the hollow lance 310 consists of a main body 311 with a substantially circular cross-section. In the lower part of the diameter of the body 31 1 of the hollow lance over a certain length is less than in the upper part.
  • the section of reduced diameter is limited downwards in that at the lower end of the main body 31 1, the diameter again corresponds at least to that above the recessed portion.
  • the main body 31 1 is enclosed by a sleeve 312, which is mounted relative to the base body 31 1 movable.
  • the sleeve 312 is configured to be moved over the portion of the reduced diameter body 311.
  • 2b shows the lower part of the hollow lance 310 as a cutout in the closed state, in which the sleeve 312 completely reduces the section with reduced
  • Diameter of the body 311 encloses.
  • the closing process can be done due to gravity or active by a drive.
  • the hollow lance 310 immersed in the solid state in the open state. It is also possible the
  • immersion depths of 40% to 80%, preferably 50% to 70%, of the filling level have proved to be advantageous, in each case based on the center of the section of reduced diameter of the main body 311 and calculated from the surface of the solids bed.
  • the filling level in the sample vessel 11 is, for example, 10 cm
  • the center of the recessed portion should be 4 to 8 cm, preferably 5 to 7 cm, below the surface of the bed. Even if, for example during the transport of the sample vessel 1 1 inhomogeneities in the characteristics of the sample, e.g. the grain size distribution, it is ensured by immersion in a central region of the solid bed a sample as representative as possible.
  • a predetermined withdrawal volume 313 is then enclosed in the hollow lance 310.
  • this withdrawal volume 313 is selected so that the amount of finely divided solid removed is sufficient for all individual analyzes provided in order to avoid a further removal process from the same sample vessel.
  • a substantially circular cross-section of the main body 311 and the sleeve 312 is advantageous, as in the above example.
  • other cross-sectional shapes are suitable such as ellipse, rectangle, hexagon or octagon.
  • Base body 31 1 and sleeve 312 only have to enclose a suitable removal volume 313 in the closed state. Both elements can be made of the same or different materials, for example of metals such as aluminum or steel, but also of plastic, ceramic or glass.
  • the inclusion of the sample material in the removal volume 313 is characterized in that the sleeve in the longitudinal direction over the
  • FIG. 2c shows an alternative embodiment of a removal means according to the invention, in which the inclusion of the sample material by a Rotary movement of the sleeve 312 relative to the base body 31 1 takes place.
  • the sleeve 312 has an opening which extends at most over half the circumference.
  • the reduced-cross-section portion of the base 31 1 in this case is not circumferentially formed in the circumferential direction, but as a one-sided depression, which can be completely covered by the continuous portion of the sleeve 312 to form a removal volume 313.
  • the removal of finely divided solid takes place analogously to the procedure described above.
  • the relevant parts of the sampling means are exposed to a gas under pressure, for example air or nitrogen.
  • a gas under pressure for example air or nitrogen.
  • bores may be provided as extraction means in the base body 31, which holes open into the area of reduced cross-section and through which, for example Compressed air can flow out.
  • the relevant parts of the sampling means can also be treated from the outside with compressed air, e.g. by a cleaning device is guided by means of a manipulator to the removal means.
  • a cleaning device in addition to the supply of a pressurized gas also contain a deduction for resulting from the cleaning gas-solid mixture.
  • mechanical cleaning tools such as brushes may be included.
  • FIG. 3 shows a preferred embodiment of a dosing means 320 according to the invention.
  • a dosing means housing 321 has an inlet 322 and an outlet 323 for finely divided solids.
  • the protruding from the housing 321 part of the inlet 322 may be advantageously configured as a funnel.
  • a metering wheel 324 is mounted inside the housing 321.
  • the running surface of the metering wheel 324 encloses with an inner wall of the housing 321 a volume through which due to the rotation of the metering wheel 324 finely divided solids are transported from the inlet 322 to the outlet 323.
  • the distance between the lower end of the inlet 322 and the tread of the Dosierrades corresponds to 1, 2 to 3 times the largest particle dimension.
  • the diameter of the inlet 322 at the lower end preferably corresponds to 1.5 times to 2.5 times the largest particle dimension.
  • the running surface of the metering wheel 324 is typically trough-shaped, for example U-shaped or V-shaped.
  • the tread and inner wall of the housing 321, which comes into contact with the finely divided solids, is typically smooth, preferably polished, to avoid sticking of the finely divided solids.
  • the Dosierradgekoruse can further Ein and have outlets, for example, to pressurize the interior with compressed air and blow out residues of finely divided solids or to suck.
  • FIG. 3 also shows a test vessel 12 which is located on a base.
  • an amount of solids from an extraction means described above is preferably introduced into the inlet 322.
  • removal means and dosing means 320 are mounted relative to each other movable in the automatic analyzer.
  • the dosing means 320 can be moved between the removal means and the test vessel 12, e.g. by a linearly movable in the x direction manipulator.
  • the dosing means 320 it is also possible for the dosing means 320 to be stationary if the extraction means can be moved between sample vessel 11 and dosing means 320. Flexibility is increased when both extraction means and metering means 320 are movably mounted.
  • the mass of the dosed solid is detected by a weighing device and used to control the dosing 320.
  • the speed and thus the peripheral speed of the metering wheel 324 can be controlled as a function of the metered amount.
  • the wheel can turn faster and thus dose more solid. If the total mass of the solid in the test vessel 12 approaches the nominal value, the wheel rotates more slowly until it finally comes to a complete standstill and no more solid matter is metered. Weighing equipment and control are selected and designed so that dosing accuracies of 0.1 g to 0.001 g can be guaranteed.
  • test vessel 12 or pad on which the test vessel 12 is located may be moved in the x-z direction during the dosing operation, e.g. linear, circular, elliptical, in the shape of an eight, or in another predetermined manner.
  • a uniform distribution is both in terms of equal fill level at each point in the test vessel, as well as with respect to the characteristics of the solid, e.g. the grain size distribution, to understand.
  • a predetermined amount of finely divided solids is metered into a test vessel 12. Subsequently, the metered amount is distributed as uniformly as possible, for example by movements of the test vessel 12 or with the aid of a stirrer. example
  • An automatic analyzer according to the invention and an automatic analytical method according to the invention were used to control the product quality of water-absorbing polymers. Two samples were subjected to the following analysis procedure per hour:
  • the arrangement of the elements of the automatic analyzer 1 corresponds to that shown in Fig. 1a.
  • the samples were mixed thoroughly by hand and set in cylindrical sample vessels 1 1 with a diameter of 90 mm, a height of 160 mm and a capacity of about 1000 cm 3 in a shelf as a depot 10.
  • the sample containers 11 were provided with a bar code which was recorded manually when the sample containers 11 were set.
  • a manipulator 20 which can be moved in three spatial directions x, y and z moved the sample containers 11 back out of the depot 10 to the metering device 30 and after removal of a sample.
  • a hollow lance 310 according to FIG. 2 a and FIG. 2 b was used as removal means, about 10 g of the finely divided solid were taken.
  • the sampling device was fixed in the x- and z-direction in the automatic analyzer, but could be moved in the y-direction.
  • dosing means 320 a device with a metering wheel 324 was used as shown in FIG. 3, which was movable in the x direction. After removal of a sample from the sample vessel 1 1, the sample vessel 1 1 was returned by the manipulator 20 in the depot 10.
  • the dosing agent 320 was then brought into a position below the extraction means that its contents emptied into the hopper of the dosing means 320 by opening the hollow lance 310. To carry out the individual analyzes, different amounts of finely divided solids were metered into different test vessels 12.
  • AAP Absorption against Pressure
  • the absorption under a pressure of 49.2 g / cm 2 was determined analogously to the EDANA recommended test method no. WSP 242.2-05 "Absorption under Pressure", whereby instead of a pressure of 21, 0 g / cm 2 (AULO.3psi) a pressure of 49.2 g / cm 2 (AULO.7psi) was set.
  • the EDANA test methods are available, for example, from the issuing institution: EDANA, Avenue Eugene Plasky 157, B-1030 Brussels, Belgium.
  • a cylindrical Plexiglas measuring cell having an inner diameter of 60 mm and a height of 50 mm provided in the depot 10 was used for this method.
  • a full-surface stamp with a weight of 368 g was in the empty measuring cell.
  • the measuring cell was placed by the manipulator 20 on a plate on a balance of the type Sartorius LP620S, removed the punch and the dosing 320 placed in a position above the measuring cell.
  • 0.9 g of finely divided solids were metered into the measuring cell with an accuracy of 0.005 g, the plate being moved in the form of an eight in the x-z direction in order to ensure a uniform distribution of the solid particles in the measuring cell.
  • the stamp was used again in the measuring cell.
  • the measuring cell was transported by the manipulator 20 into the depot and placed there on a glass filter plate covered with a filter paper in a Petri dish with a diameter of 200 mm and a height of 30 mm. Via lines in the gripper 24 of the manipulator 20, 0.9% by weight saline solution was filled into the petri dish until the liquid level had reached the upper edge of the glass filter plate. The achievement of the desired level was ensured by contact electrodes in the gripper 24 of the manipulator 20.
  • the measuring cell was removed from the depot 10 by the manipulator 20 and placed on a balance. From the current weight after fluid intake and the original weight after dosing, the AAP value was calculated and stored for this sample. Finally, the measuring cell was returned to the depot 10.
  • the SFC determination method of analysis provides information about the ability of a hydrogel layer to conduct fluid under a given pressure and is e.g. in the patent US 5,599,335 read.
  • the first method steps correspond to those of the AAP determination described above.
  • no full-area stamp was used, but a punch with holes, as shown for example in Figures 7 to 9 of US 5,599,335.
  • the metering accuracy was 0.001 g at a solids dosage of 0.9 g.
  • the measuring cell was removed from the depot 10 by the manipulator 20 and transported to a holding device under which a vessel stood on a scale.
  • the height of the gel bed was determined by means of a laser and stored for later evaluation.
  • a liquid reservoir 2 liters of 0.9 wt .-% saline solution were kept. An outlet of the reservoir was moved across the measuring cell and the outlet valve was opened, so that the liquid ran through the measuring cell into the vessel below it.
  • This level was maintained for a period of 10 minutes with the flow being measured and stored every 20 seconds.
  • the flow was determined with the help of the balance on which stood the vessel that received the liquid running out of the measuring cell.
  • the SFC value was calculated from this data and stored for this sample.
  • the measuring cell was returned to the depot 10 by the manipulator 20.
  • a beaker with an internal diameter of 30 mm and a height of 50 mm was used as test vessel 12, which was also provided in depot 10.
  • the metering of the finely divided solid proceeded analogously to the above-described methods for AAP and SFC determination, with the difference that 1 g of the particles was metered with an accuracy of 0.1 g.
  • the beaker was placed by the manipulator 20 on a scale over which a light source and a CCD camera were located at a distance of about 40 cm. Using a pump, 20 ml of 0.9% strength by weight saline solution were metered into the beaker through a liquid line and the time taken for the entire liquid to be absorbed by the polymer particles was measured.
  • the criterion used was the change in the reflection of the light on the liquid surface, which was recorded by the CCD camera as a gray value change. From the amount of dosed solid, the metered amount of liquid and the measured time, the FSR value was calculated and stored for each sample.
  • the stored information for a sample was combined in a data set and stored in a laboratory data information system (LIMS) for documentation.
  • LIMS laboratory data information system

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  • Engineering & Computer Science (AREA)
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  • Sampling And Sample Adjustment (AREA)

Abstract

L'invention concerne un dispositif de dosage de matières solides destiné au dosage de fines particules de matière solide et comportant des moyens de prélèvement pour prélever un échantillon d'un récipient pour échantillon ainsi que des moyens de dosage pour introduire une quantité prédéfinie de fines particules de matière solide dans un récipient d'essai, le dispositif de dosage de matières solides permettant d'obtenir une précision de dosage d'au moins 0,1 g et les caractéristiques de la quantité dosée correspondant sensiblement à celles de l'échantillon se trouvant dans le récipient pour échantillon. L'invention concerne également un automate d'analyse destiné à déterminer des propriétés de fines particules de matière solide et comportant un dépôt pour récipients pour échantillons et récipients d'essai, des dispositifs d'analyse pour l'analyse d'échantillons, des manipulateurs pour déplacer et placer les récipients pour échantillons, des dispositifs de dosage de matières solides et des dispositifs de dosage de liquides. L'invention porte également sur un procédé d'analyse automatique de fines particules de matière solide.
EP10718197A 2009-05-15 2010-05-11 Analyse automatique de fines particules de matière solide Withdrawn EP2430411A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP10718197A EP2430411A2 (fr) 2009-05-15 2010-05-11 Analyse automatique de fines particules de matière solide

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP09160425 2009-05-15
PCT/EP2010/056398 WO2010130703A2 (fr) 2009-05-15 2010-05-11 Analyse automatique de fines particules de matière solide
EP10718197A EP2430411A2 (fr) 2009-05-15 2010-05-11 Analyse automatique de fines particules de matière solide

Publications (1)

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EP2430411A2 true EP2430411A2 (fr) 2012-03-21

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EP10718197A Withdrawn EP2430411A2 (fr) 2009-05-15 2010-05-11 Analyse automatique de fines particules de matière solide

Country Status (5)

Country Link
US (1) US8640557B2 (fr)
EP (1) EP2430411A2 (fr)
JP (1) JP2012526971A (fr)
CN (1) CN102428354A (fr)
WO (1) WO2010130703A2 (fr)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR3002465B1 (fr) * 2013-02-27 2016-09-02 Genomic Dispositif de prelevement simultane et de transfert de multiples echantillons
WO2015192913A1 (fr) 2014-06-20 2015-12-23 Genomic Dispositif de prélèvement simultané et de transfert de multiples échantillons
CN108844998B (zh) * 2018-06-25 2024-06-14 上海锐宇流体系统有限公司 重力自流式无水氟化氢液体取样及在线分析装置
CN108970720B (zh) * 2018-09-03 2023-09-12 力鸿智信（北京）科技有限公司 一种固体矿物制样系统
CN109107208B (zh) * 2018-10-08 2023-09-26 连云港德洋化工有限公司 一种甲醇蒸馏装置
TWI695982B (zh) * 2019-03-14 2020-06-11 總翔科學儀器股份有限公司 混凝劑添加濃度值的自動分析儀器及其自動分析方法
CN112881082B (zh) * 2021-01-18 2022-06-07 内蒙古京海煤矸石发电有限责任公司 基于ai视频技术的工业用微光环境下可视采样检测装置

Family Cites Families (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2777324A (en) * 1953-01-21 1957-01-15 Ives Norton Conrad Apparatus for determining the storage quality of grain
JPS58206945A (ja) 1982-05-28 1983-12-02 Toshiba Corp 粉末試料採取装置
JPS6060532A (ja) 1983-09-13 1985-04-08 Chiyoukeiriyouki Seisakusho:Kk 微粉末試料の自動サンプリング装置
JPS6191326U (fr) 1984-11-21 1986-06-13
JPH0696619B2 (ja) * 1989-09-28 1994-11-30 三洋化成工業株式会社 高吸水性ポリマー組成物及びその製造方法ならびにそれからなる高吸水性物品
IT1260447B (it) 1992-01-27 1996-04-09 Procedimento e apparecchiatura per l'automazione integrale di un laboratorio di analisi
JP3091988B2 (ja) 1993-01-04 2000-09-25 信越化学工業株式会社 樹脂粉末の可塑剤吸収量自動測定装置
US5440941A (en) 1993-06-02 1995-08-15 Kalidindi; Sanyasi R. Multiple-sample segmented sampling device and method of use
US5337620A (en) * 1993-06-02 1994-08-16 Kalidini Sanyasi R Sampling tool
US5599335A (en) 1994-03-29 1997-02-04 The Procter & Gamble Company Absorbent members for body fluids having good wet integrity and relatively high concentrations of hydrogel-forming absorbent polymer
JPH08160028A (ja) * 1994-12-02 1996-06-21 Shin Etsu Chem Co Ltd セルロース誘導体の置換基の自動定量装置
JP3044367B2 (ja) * 1995-11-13 2000-05-22 三洋化成工業株式会社 抗菌性吸水剤組成物およびその製法
US5847294A (en) * 1996-04-09 1998-12-08 Amherst Process Instruments, Inc. Apparatus for determining powder flowability
FR2749662B1 (fr) 1996-06-11 1998-08-28 Elf Aquitaine Laboratoire robotise d'analyses d'echantillons
JPH1077121A (ja) 1996-09-03 1998-03-24 Toyo Eng Corp 粉体切出しバルブ
US6631650B1 (en) * 2000-07-31 2003-10-14 Geneva Pharmaceuticals, Inc. Thief sampling probe
US6339966B1 (en) * 2000-10-04 2002-01-22 Sanyasi R. Kalidindi Bulk powder sampler with removable partitions and method of using
JP3375609B2 (ja) * 2000-12-27 2003-02-10 川崎重工業株式会社 粉体定量採取装置
FR2824315B1 (fr) * 2001-05-07 2003-09-05 Flexilab Dispositif doseur de poudres
ATE333088T1 (de) * 2002-05-17 2006-08-15 Chemspeed Technologies Ag Vorrichtung zur dosierung von substanzen
US20070029342A1 (en) * 2002-10-04 2007-02-08 Alexander Cross Laboratory workstation for providing samples
DE102004051242A1 (de) * 2004-10-20 2006-05-04 Basf Ag Feinteilige wasserabsorbierende Polymerpartikel mit hoher Flüssigkeitstransport- und Absorptionsleistung
JP4083180B2 (ja) * 2005-03-30 2008-04-30 東亜機工株式会社 粉体物計量装置
TW200720347A (en) * 2005-09-30 2007-06-01 Nippon Catalytic Chem Ind Water-absorbent agent composition and method for manufacturing the same

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None *

Also Published As

Publication number Publication date
JP2012526971A (ja) 2012-11-01
US20120060592A1 (en) 2012-03-15
US8640557B2 (en) 2014-02-04
CN102428354A (zh) 2012-04-25
WO2010130703A3 (fr) 2011-06-23
WO2010130703A2 (fr) 2010-11-18

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