WO2013064140A1 - Procédé et dispositif destinés à mesurer le potentiel d'interface de particules et de macromolécules dans des milieux liquides polaires. logiciel permettant de mettre en œuvre ledit procédé et support lisible par ordinateur à cet effet - Google Patents

Procédé et dispositif destinés à mesurer le potentiel d'interface de particules et de macromolécules dans des milieux liquides polaires. logiciel permettant de mettre en œuvre ledit procédé et support lisible par ordinateur à cet effet Download PDF

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Publication number
WO2013064140A1
WO2013064140A1 PCT/DE2012/001056 DE2012001056W WO2013064140A1 WO 2013064140 A1 WO2013064140 A1 WO 2013064140A1 DE 2012001056 W DE2012001056 W DE 2012001056W WO 2013064140 A1 WO2013064140 A1 WO 2013064140A1
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WO
WIPO (PCT)
Prior art keywords
sample
metal cylinder
ring
measuring
sample container
Prior art date
Application number
PCT/DE2012/001056
Other languages
German (de)
English (en)
Inventor
Hanno Wachernig
Margret BÖCK
Original Assignee
Particle Metrix Gmbh
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 Particle Metrix Gmbh filed Critical Particle Metrix Gmbh
Publication of WO2013064140A1 publication Critical patent/WO2013064140A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/60—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrostatic variables, e.g. electrographic flaw testing

Definitions

  • the stability or functionalization of dispersions and macromolecular solutions is often influenced by the effect of electrostatic repulsion. This is caused by the presence of ionic end groups at the interfaces of particles and macromolecules, the latter being called polyelectrolytes when carrying charged end groups. At lower
  • Such dispersions can occur as emulsions such as milk, as
  • Powder dispersions such as pigment suspensions or printer ink or in the form of all possible coatings such as the so-called
  • Such dispersions may also be biopolymers such as proteins or beverage suspensions. Next come also here, for example, Baustoffschiicker and adhesives into consideration.
  • Macromolecules in the form of polyelectrolytes occur, inter alia, in the natural form of juices or artificially produced in the form of
  • Electrostatic attraction targeted to cause the respective desired reactions are the cationic poly-DADMAC (diallyldimethylammonium chloride) and the anionic PVS (sodium polyvinylsulfate). Of these, the amount of charge in units of the elementary charge is known. They can also be used for calibration purposes assuming stoichiometric 1 to 1 charge reactions.
  • the targeted stabilization of dispersions to increase the shelf life is achieved by a high ionic interfacial charge of the particles.
  • the targeted destabilization of dispersions or emulsions for flocculation and precipitation of dispersions in water recycling processes is achieved by charge neutralization of the particles. This can also be used to break an emulsion.
  • magnetic particles are surrounded by a body-compatible shell, and in turn are bound to end groups which serve as a link to the desired functional end groups.
  • These functional end groups may be, for example, proteins selected in a diagnostic kit.
  • ionic end groups are often attached to particles.
  • Double layer the outer ions are mobile. That means they can be shorn off. This can be done electrically, mechanically or acoustically. Only by shearing can the interfacial charge be analyzed. In each experiment, therefore, care is taken to ensure that a differential speed between liquid and
  • Boundary layer of the particles occurs.
  • the analysis method presented here is based on the measurement of the (oscillating) flow potential.
  • the particles or polyelectrolytes to be measured are retained by adsorption on the vessel wall of the measuring cell or by inertial forces of the larger particles.
  • the sensor element is a planar electrode, which is substantially parallel to the particle flight direction and is held at tube potential, wherein the charge of the electrically moving particles passing by are influenced by varying charge displacements
  • Electrode devices The underlying objective of this document is to further develop the prior art that the
  • the first electrode is embedded in a wall of a flow channel of the first electrode device in such a way that it protrudes maximally with its diameter into the flow channel transversely to the flow direction.
  • the method described here relates to the principle of holding the solids by means of a filter or sieve in order to establish a relative flow between the liquid
  • Solid dispersion and the solids contained in it This principle is preferably applicable to pulps and particles larger than about 0.1 mm.
  • This device contains a measuring cell with sieve and electrodes and a measuring cell with sieve and electrodes and a measuring cell with sieve and electrodes and a measuring cell with sieve and electrodes and a measuring cell with sieve and electrodes and a measuring cell with sieve and electrodes and a measuring cell with sieve and electrodes and a measuring cell with sieve and electrodes and a measuring cell with sieve and electrodes and a measuring cell with sieve and electrodes and a measuring cell with sieve and electrodes and a
  • Suction tube wherein at least two integrated in the device vacuum pumps are separately connected to a respective vacuum vessel via lines. It is the object of this invention to provide a well transportable and inexpensive device for the flow potential measurement of fibers and particles in suspensions, in particular a device for determining the zeta potential of the particles of fibrous or particle-containing aqueous suspensions by measuring the
  • Polyelectrolytes (0.5 nm - 300 ⁇ ) based on a cylindrical measuring cell made of a non-conductive material with a weakly charged surface as possible and a displacer of the same material.
  • the most commonly used material for this is PTFE.
  • the laboratory version is usually open at the top, with 10 mL of sample, typically 1 volume percent, being filled in after cleaning. Titration solutions are also added from above during the measurement process.
  • the electronic signal processing is carried out either by a
  • Charge shift is measured as current and converted into a potential, or there is a pure potential measurement.
  • the above-mentioned cylinder is closed, so that the dispersion can flow through the measuring cylinder accordingly.
  • the advantage of the open - topped version is its suitability for fast charge titrations for charge fingerprinting, for screening work and for formulating dispersions and colloidal systems. Also for cleaning with brush and liquids, this cell construction is well suited.
  • the disadvantage of the open top version is that it is too expensive to be used only once and therefore the risk of carryover is very high. In addition, the required sample volume is very large, which definitely plays a role in expensive sample liquids.
  • the advantage of the closed version is the monitor function itself.
  • the disadvantage is the risk of carryover of the sample and the so-called "fullness" of the signal due to the increasing occupancy of the cell walls.
  • the object of the present invention results from the above-described disadvantages of the prior art. It should be created a measuring device that is inexpensive and can be easily replaced by a new because of the risk of carryover. It should be possible to operate by means of a pump or a printing device, wherein the measuring capillary comes into contact neither with the pump nor with the printing device.
  • the amount of sample should be as low as possible.
  • the range of application in terms of the particle size of the sample should be as far as possible.
  • the sample should be preserved.
  • a device for measuring the boundary layer potential of particles and macromolecules in liquid polar media in the form of individual samples, with the following features: a) a sample container (5) with the sample to be examined points at its upper side of a tightly sealable, and easily removable from the sample container lid in the form of a
  • the metal cylinder (4) has in its interior a, in the metal cylinder (4) out, essentially also
  • a plug-in, collecting channel tube (2) in the form of a hollow metal cylinder with a collecting channel (1) having at its lower end a cross-sectional constriction to the diameter of the capillary tube (11) and at its upper end on the Teflon core (3) protrudes, d) the Teflon core (3) projecting, part of the collecting channel tube (2) is of a cylindrical plastic cylinder (9) enclosed, this having longitudinal bores, which spread it, distributed over the circumference, in the direction of its longitudinal axis, and wherein the plastic cylinder (9) has a length such that on the one hand, attached to its inner diameter, metallic contact ring (7) on the On the other hand, the underside of the plastic cylinder (9) is flush with the metal cylinder (4), and wherein the contact ring (7) serves as a connection - opening (8) for a pump or a pressure unit,
  • the plastic cylinder (9) is of a cylindrical
  • Metal cylinder (4) is seated and flush with the upper surface of the plastic cylinder (9),
  • Method for measuring the boundary layer potential of particles and macromolecules in liquid polar media in the form of individual samples having the following features: a) the sample (12) to be examined is filled into a sample container (5),
  • the sample container (5) supplemented in this way is mechanically and electrically connected from below to an evaluation unit, this being a pump (13), an electronic signal processor and an output unit for the
  • the capillary tube (11) is mounted horizontally, wherein the ring electrode (7) and the head ring (10) are each mounted in a flat manner
  • Design are executed and by means of an electrical connection through a corresponding housing (21) are accessible from the outside.
  • sample containers (5) are examined in a production line - like process, the individual sample containers (5) being made identifiable by means of a barcode.
  • Fig.1 the operating principle of the device
  • FIG. 4 shows the connection to an evaluation unit Fig.5: a special design of the container for the sample
  • FIG. 1 conveys the functional principle of the device according to the invention.
  • the base container 5 is used to hold the sample to be examined 12.
  • this sample 12 of the immersed from above Teflon core 3 is shown with its capillary tube further into the stylized collecting channel 1.
  • the collecting channel 1 is closed at its upper part by a pump 13. It can be seen that the collecting channel 1 essentially serves as a kind of storage container, because the pump 13 pumps the sample liquid 12 in an oscillating rhythm through the capillary tube of the Teflon core 3 from the basic container 5 into the collecting channel 1 - Liquid 12 at high speed past the contact ring 7, since the liquid in the narrow capillary tube must flow much faster than in an area with a larger
  • the output of the pump 13 is connected via the overflow channels 6, which were symbolized here by a single line, with the basic container 5 and the sample in connection.
  • the mentioned measurable electrical signal provides a measure of the sum of the
  • the colloidal particles in the sample carrying the charge to be measured are adsorbed on the measuring vessel walls.
  • the differential velocity acting on a particle relative to the flow rate of the sample causes the mobile part of the charge cloud on it to be sheared off and measured at the moment of shearing.
  • the outer layer of the charge cloud is less strongly bound, as indicated above, and can therefore be sheared off.
  • the potential at the shear plane is called zeta potential. Only by shearing off the mobile external charges can this zeta potential be measured.
  • Reference potential for the zeta potential serves the potential of the sample, which is discharged by means of the head ring 10, which is located in this stylized representation below.
  • the measuring line 14, which detects the potential difference between the contact ring 7 and the head ring 10, carries the determined potential difference to the electronic processing further.
  • the directly measurable signal is the so-called oscillating flow potential. It is proportional to the zeta potential, which is considered to be the best calculated one, and can be calculated from electrophoretic mobility according to Smoluchowski. The determination of the oscillating
  • Flow potential has the great advantage over all other methods, such as electrophoresis and ultrasound, that offers the widest range of application in terms of sample particle size.
  • macromolecules (10 nm in size and below) can not be measured in many state-of-the-art analyzers. Also in the upper part of the listens
  • Measuring range at 10 m for most other methods.
  • a method with the oscillating flow potential is applicable to particles of a size up to 300 ⁇ .
  • the scope of the device according to the invention thus ranges for particle sizes from 0.3 nm to 300 ⁇ .
  • Reference numeral 19 denotes the possibility of supplying additives, for example a titrant.
  • a special feature of the measuring principle according to the invention is that the sample is retained.
  • FIG. 1 The technical embodiment of the functional principle illustrated in FIG. 1 is shown in FIG. As it is technically in the sense of the solution of the invention
  • the underlying object was to make the measuring device so that it can be easily and easily attached to an evaluation - unit, the designated in Fig.1 10, head ring was moved to the top of the device.
  • the Teflon core 3 with its inner capillary tube was designed as a cylindrical tube with a press fit in a metal tube
  • the metal tube 4 is in connection with the detection of the potential of the sample with this, since it almost to the bottom of the base container
  • Sectional drawing can be seen. This allows the sample liquid 12 in the Teflon core 3 to rise and occupy the required space. The lowest part of the Teflon core 3 has been lowered in order to allow the sample liquid 12 rapid access into the associated capillary tube.
  • the capillary tube is provided to reduce its cross section with a central web 20.
  • the collecting channel pipe 2 is fitted in the middle with a constriction at the lowermost end. The cross section of this constriction corresponds in his Diameter of the diameter of the capillary tube and has the function of
  • the technical design of the upper part of the measuring device which adjoins the sample measuring range can be seen in FIG.
  • the cylindrical adaptation part placed in the longitudinal direction onto the collecting channel pipe 2 establishes the mechanical and electrical connection to an evaluation unit.
  • This evaluation unit essentially comprises a pump 13 and the
  • the adaptation part consists of a
  • Plastic cylinder 9 encloses, which in turn sits on the manifold 2.
  • the plastic cylinder 9 has eight holes extending in the longitudinal axis as overflow channels 6, as can be seen from the sectional drawing of Figure 3. These overflow channels 6 ensure that components of the sample liquid 12 that pass beyond the pump can safely flow back into the sample container 5.
  • a corresponding line is provided in the evaluation unit. Since the metallic head ring 10 is seated on the metal cylinder 4, which carries the potential of the sample liquid, this potential is also applied to the upper side of the head ring 10 and can be detected there by corresponding contacts of the evaluation unit. Similar happens with the at the ring electrode of the
  • Sammelkanalrohrs 2 tapped potential which is also on the contact ring 7, which simultaneously represents the connection for the pump 13, can be detected by corresponding contacts of the evaluation - unit. These two potentials provide the desired measurement result.
  • FIG. 4 shows the connection to an evaluation unit.
  • This consists of a housing 15, a lifting unit 17 with a hand lever 16 and an associated base 18.
  • the device according to the invention after filling of the sample container 5 with a sample 12 placed on the base 18 and the Investigation of a corresponding holder of the housing 15 are pressed.
  • the hand lever 16 is used here only for pleasing presentation of the function.
  • the process of inserting the device according to the invention into the evaluation unit can be carried out hydraulically and by means of corresponding electrical control devices.
  • the measuring system described also makes it possible, in a further expansion stage, for the specimens 12 to be examined to be located on one
  • Evaluation unit is automatic. This can either be done in such a way that the device according to the invention moves upwards, or the, correspondingly higher arranged, evaluation unit is moved downwards. For such an automatic evaluation of samples, quasi on the assembly line, it is intended to provide the individual samples or sample containers with a bar code for the purpose of unambiguous identification.
  • the housing of this design is preferably made of Teflon.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)

Abstract

L'invention concerne un procédé et un dispositif destinés à mesurer le potentiel d'interface de particules et de macromolécules dans des milieux liquides polaires se présentant sous la forme d'échantillons isolés, présentant les caractéristiques suivantes : a) l'échantillon (12) à analyser est introduit dans un récipient pour échantillons (5), b) un cylindre métallique (4) lequel permet de faire l'étanchéité et lequel est pourvu d'une bague de tête (10) y prenant appui, d'un noyau en téflon (3) se trouvant à l'intérieur et comportant un tube capillaire, et d'un tube à canal collecteur (2) y prenant appui et comportant une électrode annulaire, est introduit dans récipient pour échantillons (5), la bague de tête (10) et l'électrode annulaire étant accessibles de l'extérieur et ledit tube à canal collecteur permettant de brancher une pompe sur la face supérieure, c) le bas du récipient pour échantillons (5) ainsi complété est relié mécaniquement et électriquement à une unité d'analyse laquelle comporte une pompe (13), un dispositif de traitement électronique du signal et une unité permettant d'afficher le résultat de mesure.
PCT/DE2012/001056 2011-11-04 2012-11-02 Procédé et dispositif destinés à mesurer le potentiel d'interface de particules et de macromolécules dans des milieux liquides polaires. logiciel permettant de mettre en œuvre ledit procédé et support lisible par ordinateur à cet effet WO2013064140A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102011117681.4 2011-11-04
DE201110117681 DE102011117681B4 (de) 2011-11-04 2011-11-04 Verfahren und Vorrichtung zur Messung des Grenzschichtpotentials von Partikeln und Makromolekülen in flüssigen polaren Medien

Publications (1)

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WO2013064140A1 true WO2013064140A1 (fr) 2013-05-10

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WO (1) WO2013064140A1 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102014001759B4 (de) 2014-02-10 2016-01-07 Particle Metrix Gmbh Verfahren und Vorrichtung zur schnellen Analyse der Ladungscharakteristik und der Größenverteilung von Partikeln
DE202014001232U1 (de) 2014-02-10 2014-02-21 Particle Metrix Gmbh Vorrichtung zur schnellen Analyse der Ladungscharakteristik und der Größenverteilung von Partikeln
DE102014104511A1 (de) * 2014-03-31 2015-10-01 Leibniz-Institut Für Analytische Wissenschaften - Isas - E.V. Verfahren und Vorrichtung zur nicht invasiven Bestimmung von Prozessparametern bei Mehrphasenströmungen
US10078043B2 (en) * 2016-03-08 2018-09-18 Ford Global Technologies, Llc Method and system for exhaust particulate matter sensing

Citations (6)

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Publication number Priority date Publication date Assignee Title
US3441956A (en) * 1967-01-23 1969-04-29 Willard Farnham Liquid treatment method and apparatus
DE4008916C1 (fr) * 1990-03-20 1991-05-23 Muetek Gmbh, 8036 Herrsching, De
DE19651611A1 (de) 1996-12-12 1998-06-18 Bosch Gmbh Robert Einrichtung zur Messung einer Teilchenzustandsgröße
US6176974B1 (en) * 1997-12-22 2001-01-23 International Paper Company Method for determining electrokinetic properties of papermaking furnish
DE202006000403U1 (de) 2006-01-12 2007-02-01 Emtec Elektronik Gmbh Vorrichtung für die Strömungspotentialmessung von Fasern und Partikeln in Suspensionen
DE102005061639B4 (de) 2005-12-22 2007-09-27 BTG Mütek GmbH Vorrichtung zur Messung eines Strömungspotentials an einer Feststoffe enthaltenden Flüssigkeit

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Publication number Priority date Publication date Assignee Title
SE510859C2 (sv) * 1993-12-02 1999-06-28 Innomatic Ab Anordning för samtidig mätning av strömningspotentialen för en fibersuspension och dess filtrat

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3441956A (en) * 1967-01-23 1969-04-29 Willard Farnham Liquid treatment method and apparatus
DE4008916C1 (fr) * 1990-03-20 1991-05-23 Muetek Gmbh, 8036 Herrsching, De
DE19651611A1 (de) 1996-12-12 1998-06-18 Bosch Gmbh Robert Einrichtung zur Messung einer Teilchenzustandsgröße
US6176974B1 (en) * 1997-12-22 2001-01-23 International Paper Company Method for determining electrokinetic properties of papermaking furnish
DE102005061639B4 (de) 2005-12-22 2007-09-27 BTG Mütek GmbH Vorrichtung zur Messung eines Strömungspotentials an einer Feststoffe enthaltenden Flüssigkeit
DE202006000403U1 (de) 2006-01-12 2007-02-01 Emtec Elektronik Gmbh Vorrichtung für die Strömungspotentialmessung von Fasern und Partikeln in Suspensionen

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SUERO: "ZETA POTENTIALS OF LONG ISLAND AQUIFER MATERIAL", 14 July 2010 (2010-07-14), XP055050139, Retrieved from the Internet <URL:http://dspace.sunyconnect.suny.edu/xmlui/bitstream/handle/1951/47963/Suero_abst.pdf?sequence=1> [retrieved on 20130117] *

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DE102011117681A1 (de) 2013-05-08

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