Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
  • B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
  • B01D61/425—Electro-ultrafiltration
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
  • B01D65/02—Membrane cleaning or sterilisation ; Membrane regeneration
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
  • B01D67/0081—After-treatment of organic or inorganic membranes
  • B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
  • B01D69/12—Composite membranes; Ultra-thin membranes
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
  • B01D71/06—Organic material
  • B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
  • B01D71/68—Polysulfones; Polyethersulfones
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
  • C23C14/04—Coating on selected surface areas, e.g. using masks
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
  • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
  • C23C14/14—Metallic material, boron or silicon
  • C23C14/20—Metallic material, boron or silicon on organic substrates
  • C23C14/205—Metallic material, boron or silicon on organic substrates by cathodic sputtering
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
  • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
  • C23C14/34—Sputtering
  • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
• • 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
  • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
  • G01N27/416—Systems
  • G01N27/447—Systems using electrophoresis
  • G01N27/44756—Apparatus specially adapted therefor
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2311/00—Details relating to membrane separation process operations and control
  • B01D2311/26—Further operations combined with membrane separation processes
  • B01D2311/2684—Electrochemical processes
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2313/00—Details relating to membrane modules or apparatus
  • B01D2313/24—Specific pressurizing or depressurizing means
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2313/00—Details relating to membrane modules or apparatus
  • B01D2313/34—Energy carriers
  • B01D2313/345—Electrodes

Definitions

• the present invention relates to a method for the at least temporary retention of charged biologically active substances, for example endotoxins, viruses, proteins from liquids, and possible later release for better determination.
• charged biologically active substances for example endotoxins, viruses, proteins from liquids, and possible later release for better determination.
• Endotoxins are lipopolysaccharides (LPS) and components of the outer membrane of the cell wall of Gram-negative bacteria. They consist of a lipophilic and anchored in the membrane lipid and a hydrophilic polysaccharide, which stands for the antigenic properties. Endotoxins are released upon lysis of the bacterial cell. They are extremely heat-stable and can even be detected after sterilization, that is to say after the bacteria have been killed. Because of their ability to induce an immune response, endotoxins are among the pyrogens. Endotoxins in the amount of 1 ng / kg body weight are already considered sufficient to trigger a febrile reaction (ARDUINO (1 989)). In addition to fever as a result of inflammation, they can cause numerous physiological reactions in humans after contact with mucous membranes and especially in the passage into the bloodstream. These include blood pressure drop, blood coagulation and complement activation as well as life-threatening shock states.
• Endotoxins are usually detected in the rabbit or limulus amoebocyte lysate (LAL) test.
• LAL test is based on the blood of the horseshoe crab, which reacts extremely sensitively to endotoxins of gram negative bacteria. Due to its sensitivity, the LAL test is the most widely used test in the pharmacological and medical environment. However, with this test, endotoxins can only be determined in clear undyed liquids. A direct determination of endotoxins in the blood of humans is therefore not possible. Therefore, the so-called monocyte activation test has been developed in recent years. This works through different levels of enzymatic reactions that mimic the human fever response. It also requires the creation of a standard curve for each determination, since the reactants of each test kid react differently.
• Microporous membranes have been known for a long time. These are mainly made of polymers and used for water treatment (wastewater, drinking water, industrial waters) as well as in the pharmaceutical industry for the production of ultrapure water as well as in medical technology as a sterile filter or respiratory filter. The areas of application are many and very divergent. Microporous membranes generally have a pore size between 0.01 ⁇ and 10 ⁇ and hold back according to these pore sizes substances.
• Microporous filters are typically used to separate substances dissolved in water and to obtain a clear filtrate. This is usually done mechanically via the pore size. All substances larger than the size of the pores are mechanically retained. In addition to this property, there is another mechanism that takes place to retain substances when passing the membrane. This is an undefined adsorption by the materials that make up the membrane itself, such as polyethersulfone, polypropylene or polyvinylidene fluoride (PVDF). Different materials adsorb varying amounts of different solutes ("Analyte Loss Due to Membrane Filter Adsorption as Determined by High-Performance Liquid Chromatography" M. Carlson and R.D.
• Directed adsorption of substances smaller than the pore size of the microporous membrane by means of the material properties of the membrane material is achieved by the treatment of the chemical composition of the membrane material.
• a positive charge is generated, for example, by combining the membrane material with positively charged quaternary ammonium compounds.
• Positively charged membranes are known from US 5,282,971 or from US 7,396,465 B2, negatively charged membranes from US
• positively charged microporous membranes are used to mechanically retain bacteria and allow positively charged material to pass through to avoid undirected, unquantifiable adsorption by the membrane material.
• positively and negatively charged membranes are also used to bind and concentrate proteins by adsorption.
• Positively charged microporous membranes are also used to bind endotoxins and viruses via adsorption, as in DE, for example
• CH 678403 discloses a metal-coated membrane with possibly slightly porous passages between macropores on one side and micropores on the metallic side. Also, for example from DE 1 01 64 21 4 A1 metal membranes with tunnel-like passages known. These differ from in the parlance of the application porous passages, as they are known for example from porous polymer membranes, in that they form no cavities outside of the actual passage channel within the membrane. Porous is therefore not to be equated with the statement that the membrane has pores, ie passages, such as in DE 1 01 64 21 4 A1. Porous passages thus have a surface within the membrane which clearly exceeds the surface of a circular tunnel with the same pore size by a membrane of the same thickness, at least by 50%, in particular by a multiple, in particular by at least 3 times.
• Electrosorption is accomplished by forming an electrically charged field on surfaces by applying a positive and negative voltage to two electrodes.
• a combination of electrosorption and ultraporous filtration is described in "Removal of arsenic and humic substances (HSs) by electro-ultrafiltration (EUF)" (Weng, Y.-H. et al., Chem. Eng.
• An electrosorption membrane is described in EP0872278A1.
• a ceramic membrane is provided with a conductive layer of pyrolytic carbon. The pores are closed with pyrolytic charcoal and the ceramic surface then conductive over high temperature by conversion of the ceramic surface to carbide. done well. With this ceramic membrane, salts were adsorptively bound to the surface via electrosorption.
• a possible electrosorption on the conductive surface of a ceramic membrane allows a more flexible sorption of substances, but is very expensive to manufacture.
• the pores of the membrane are sealed within the process for producing the conductive surface in order to provide the ceramic surface with a conductive carbide layer in a subsequent production step by means of very high temperatures.
• the object is to establish a method for the at least temporary separation and / or detection of charged biologically active substances, in particular endotoxins from liquids, in particular from colored liquids.
• Another object is also to provide a corresponding device.
• the production of a polymer membrane for use in the method and / or the apparatus having a flat and porous coating of metal is known, for example, from Divorce possible with magnetron sputtering.
• This allows the large-scale production of thin layers with a homogeneous layer thickness and complex layer structure.
• the basis of the magnetron is a plasma discharge in an inert gas atmosphere, z. Argon, which is amplified by a static magnetic field (A. Anders, Handbook of Plasma Immersion Ion Implantation and Deposition, Wiley-VHC, 2004).
• the ions of the process gas are accelerated cathode, knocking out these when hitting atoms. Consequently, the cathode (target) must be made of the material to be deposited.
• the atoms precipitated out of the target then condense on the substrate to be coated and form a continuous thin layer.
• This layer thickness can be generated controlled from a few nanometers to several micrometers.
• round magnetrons are mainly for the coating of large areas, eg. As in architectural glass coating, rectangular variants with several meters in length widespread. Here by surfaces of membranes can be coated.
• a polymer membrane for example, polysulfone, polyethersulfone, polypropylene or polyvinylidene fluoride
• the residence time of the membrane in the process is chosen so low that the temperature remains below 200 ° C, in particular below 1 00 ° C, and the polymer membrane is not affected in its original chemical structure.
• a polyethersulfone membrane having a microporous structure was provided with a 20 nm thin layer of aluminum. Porosity studies were performed on this membrane. The following table shows the results of the measurement of the porosity of the membrane on the one hand in the original state on the other hand with a defined thick layer of 20 nm aluminum.
• Tab.1. Pore sizes of a microporous polyethersulfone membrane in the original and with a 20 nm thick aluminum layer.
• the porosity of the membrane is influenced to less than 10%.
• the metal coating is applied at least in a planar manner on a first side of the polymer membrane and / or at least on the surfaces accessible from one side, in particular until the layer thickness of the coating of metal of the polymer membrane based on the initial bubble point pore and / or the average pore size of the uncoated Polymer membrane is between 1% and 45%.
• the coating is particularly porous and in particular applied directly.
• the metal used for the coating is in particular copper, aluminum, silver, gold, nickel, platinum and / or tungsten or alloys containing copper, aluminum, silver, gold, nickel, platinum and / or tungsten.
• membranes of polysulfone, polypropylene, polyethersulfone, polyethermide, polyacrylonitrile, polycarbonate, polyethylene terephthalate, polyvinylidene fluoride (PVDF) and / or polytetrafluoroethylene or such polysulfone, polyphenylene sulfide are known as polymer membranes.
• metal has been deposited until the layer thickness of the metal coating of the polymer membrane based on the initial bubble point pore and / or the mean pore size of the uncoated polymer membrane is between 1% and 45%.
• metal has been deposited until the porosity of the polymer membrane with coating of metal based on the initial bubble point pore and / or the average pore size compared to the uncoated polymer membrane between 1% and 50%, in particular 1 and 20% is reduced.
• These values also combine good conductivity with good throughput and high porosity.
• metal has been deposited until the initial bubble point pore and / or the mean pore size of the polymer membrane with coating of metal and / or aluminum oxide is 0.01 to 10 ⁇ m.
• the polymer membrane is selected with an initial bubble point pore and / or average pore size of more than 0.01 to 10 / vm.
• the polymer membrane on the first and one of the first side opposite second side is coated with metal directly porous surface.
• the two-dimensional coatings, including metallizations, are electrically insulated from one another.
• metal has been deposited until the thickness of the metal coating or the average thickness of the metal coating is at least 1 nm, in particular at least 5 nm and at most 50 nm. At these values, a good conductivity with at least 5 nm can be combined with good throughput and high porosity.
• the pore size of the uncoated polymer membrane is between 0.01 and 1 5 / vm, in particular up to 1 0 / vm and / or greater or equal to 0, 1 / vm selected.
• metal has been deposited until the thickness of the metal coating of the pores within the membrane or the average thickness of the metal coating of the pores within the membrane is at least 1 and at most 50 nm.
• the metal-coated polymer membrane having porous passageways
• the metal-coated polymer membrane having an internal polymer membrane with porous passages and a coating of metal, characterized in that the polymer membrane is completely encapsulated by the metal coating and that the coating of metal has a thickness of 1 nm, in particular 5 nm, to 500 nm, the problem is solved.
• the coating is applied in particular directly to the polymer membrane.
• the coated polymer membrane consists exclusively of the polymer membrane and the metal coating.
• the polymer membrane with a coating of metal based on the initial bubble point pore and / or the mean pore size compared to the uncoated polymer membrane, has a porosity of between 1% and 50%, in particular 1% and 20%.
• the membrane can also be folded and / or folded, for example, as is known in conventional membranes.
• at least one insulating folding aid in particular on each side of the membrane at least one, is used and / or included. These allow a passage of liquid and provide in particular for isolation of the individual folds from each other.
• the at least one folding aid is arranged on one or both sides of the membrane prior to the folding and folded together with the membrane.
• the folding aids need not be formed from completely insulating material, so for example a polymer fleece can be used, which is in particular coated on one side or both sides electrically conductive, but the fleece itself provides insulation.
• a polymer membrane with flat and porous coating of metal in particular as described above, at least on a first side, in particular two sides, of the polymer membrane provided;
• a counter electrode provided;
• a voltage is applied between the coating of metal of the polymer membrane and the counter electrode;
• the polymer membrane and in particular the counter electrode brought into contact with the liquid, wherein bringing into contact in particular of the kind that the liquid generates at least one connection between the polymer membrane and the counter electrode.
• Such a method makes it possible to adsorb and / or retain, in particular separate, from liquids, for example from blood, charged substances, in particular biologically active charged substances, but also other charged substances, at least temporarily by binding to the polymer membrane with metal coating.
• liquids for example from blood
• charged substances in particular biologically active charged substances, but also other charged substances, at least temporarily by binding to the polymer membrane with metal coating.
• a much more adapted and flexible process management is possible than is possible with known (ionically) charged membranes.
• a separation, for example, for recovery, for example into another liquid can be facilitated , in particular without the need for a pH change.
• the amount of voltage is advantageously at most 1, 5 V. In particular, the amount of voltage even after a polarity reversal maximum 1, 5 V.
• the voltage or the energy required for their production for example, capacitive, inductive and / or transmitted by cable ,
• the voltage or the energy required for its generation can be transferred into a housing, which encloses the polymer membrane and counterelectrode, in particular inductively.
• the voltage or the energy required for its generation can be inductively coupled into the housing and brought into the housing via cables on the polymer membrane and the counter electrode.
• Charged biologically active substances are to be understood as meaning a multiplicity of substances.
• a more or less specific retention, separation or a more or less specific detection of individual or numerous substances can be made possible, for example by selective selection of the voltage and / or the membrane surface.
• a retention and / or an adsorption to / through the / the membrane of more charged particles is possible even at lower voltages than less charged particles. This allows a certain selectivity by selecting the voltage. It is not absolutely necessary just a single substance to separate and / or prove.
• suitable biologically active substances are viruses, bacteria, endotoxins, proteins, amino acids, zwitterions, substances with an isoelectric point, exosomes and / or vesicles.
• polymer membrane with metal coating and in particular also the counter electrode are extensively brought into contact with the liquid, in particular wetted over a large area. Sufficient is already a small-area contact or the small-area connection, for example, by a drop between the counter electrode and polymer membrane with metal coating. Also, the contacting can be achieved by filling one or a plurality of pores of a two-sided metallic coated polymer membrane, one side of which is used as a counter electrode.
• the counterelectrode is formed either by a further flat, porous coating of metal on a second, the first side opposite side, wherein the two-dimensional coatings of metal are isolated from each other by the polymer membrane, or by an interposition of an insulating and permeable spacer and / or spaced apart permeable electrode, in particular formed by a metallic mesh and / or a rod electrode.
• the porosity of the polymer membrane with coating of metal with respect to the initial bubble point pore and / or the average pore size compared to the uncoated polymer membrane between 1% and 50%, in particular 1 and 20% is reduced.
• a reliable conductivity is given at the same time great porosity.
• the polymer membrane is selected such that the thickness of the metal coating is 1 nm, in particular 5 to 50 nm, and / or the pore size of the uncoated polymer membrane is in particular greater than 0.01 ⁇ m and in particular less than 1 5 ⁇ m.
• a reliable conductivity is given at the same time great porosity.
• a reference electrode is provided for measurement purposes and the potential at the reference electrode is measured.
• polymer membrane with metal coating which is used according to the invention as an electrode and counter electrode and optionally reference electrode provided at least one further electrode, in particular at least one further polymer membrane with metal coating or another side of the polymer membrane with metal coating, in particular as explained above, as further electrode.
• this additional electrode is likewise arranged in the common housing and is insulated electrically from the polymer membrane with metal coating and the counterelectrode.
• the common housing may also be an outer housing that encloses an inner housing in which polymer membrane and counter electrode are arranged.
• a voltage is applied to the at least one further electrode which is chosen such that the potential of the counterelectrode comes to lie between the potential of the polymer membrane with metal coating and the at least one further electrode.
• the counterelectrode is arranged in the housing between the polymer membrane with metal coating and the at least one further electrode.
• Endotoxins were introduced into the clean water in the receiving vessel so that an endotoxin concentration of 1,000 IU (International Units Endotoxin) was established in the clean water in the receiving vessel.
• the filtration was carried out without pressure. Filtration of the membrane in the original state without coating and filtration with a membrane of a coating of 1 5 nm.
• the coated membrane was a Voltage of + 500 mV applied. The results are shown in the following table.
• the adsorbed endotoxins can be redissolved by reversing the voltage and purging the membrane and removing it from the membrane.
• virus maintenance may also be achieved. It is known that viruses have a negative charge above their isoelectric point and can be adsorbed to surfaces with a positive charge (Adsorption of Viruses to charged-modified silica, Zerda et al., Applied and Environmental Microbiology, Jan. 1 985, p. 91-95). With the same experimental set-up as described above concerning the retention of bacteria, attempts to retain viruses were carried out. Bacteriophages MS2 with a size of 25 nm (diameter) were used. The isoelectric point of these bacteriophages is at pH 3.9.
• the object is also achieved by a method for determining the occupation of the binding sites of the polymer membrane with flat and porous coating of metal and / or for determining at least one at least relative concentration in the liquid, which method can make use of the method for the at least temporary separation and / or detection of charged biologically active substances in a liquid of all advantageous embodiments and is characterized by that the current flow caused by the applied voltage is detected and / or evaluated, in particular evaluated with respect to the undershooting of a limit and / or the exceeding of a positive and / or negative rate of change and / or its time course and in particular triggers an alarm when falling below or exceeding becomes.
• concentration limits or rates of change of concentrations can be monitored.
• Such monitoring can be done very closely and even in real time.
• the endotoxin concentration in the blood can be monitored.
• the current flow depends on the occupation of the binding sites on the membrane. If fewer binding sites are available, the current flow drops.
• the concentration does not have to be determined as an absolute value, it is sufficient. Underlying or exceeding of reference values, the reference values can also be given in the form of current flows.
• an alarm can occur when certain concentration limits and / or rates of change are exceeded, in particular measured as the rate of change of the current flow, for example acoustically, optically and or electrically.
• the object is solved by electrosorption and / or electrofiltration apparatus comprising a counterelectrode and a polymer membrane having a flat and porous coating of metal on at least one side of the polymer membrane, in particular as described above, and contacting the coating of metal to create a metal Tension against the counterelectrode.
• electrosorption and / or electrofiltration apparatus comprising a counterelectrode and a polymer membrane having a flat and porous coating of metal on at least one side of the polymer membrane, in particular as described above, and contacting the coating of metal to create a metal Tension against the counterelectrode.
• the polymer membrane and in particular also the counter electrode are arranged in a housing which is designed in particular as a syringe attachment and / or a low hold-up volume, in particular of at most 10 ml and / or maximum 20 mm 3 / mm 2 coating of metal on the polymer membrane, in particular a maximum of 2 mm ⁇ 3 / mm ⁇ 2 coating of metal on the polymer membrane, and / or the polymer membrane and the counter electrode are adapted to be connected to a voltage source or are connected to such is set up form a voltage between the polymer membrane and the counter electrode and wherein in particular the voltage source with the polymer membrane and the counter electrode is arranged in a common housing and / or a current measuring device is provided which measures the current flowing between the polymer membrane and counter electrode and / or its rate of change and / or is compared with a threshold and / or the voltage source is set up to reverse the voltage.
• the metal coating of the membrane for example, directly with an electrical conductor, for.
• an electrical conductor for example, for example, soldering or welding.
• it can additionally or alternatively be brought into contact, for example, with other electrically conductive components, for example with a cage into which the membrane is inserted, and / or with at least one conductive coated folding aid, and by means of these and optionally further components and / or cables be connected to the power source and / or be contacted and / or.
• connection to the voltage source it is also possible to incorporate an inductive and / or capacitive coupling into the connection to the voltage source so that, for example, it is also possible to connect the voltage source through a closed housing without corresponding cable feedthroughs.
• the common housing may also be an outer housing that encloses an inner housing in which polymer membrane and counter electrode are arranged.
• a residence volume for liquid is provided in the housing, can dwell in the liquid or can be moved through the liquid.
• the planar and porous coating of metal of the polymer membrane and in particular the counter electrode is then arranged.
• This residence volume is arranged in particular with at least one, in particular two connections for hoses and / or syringes, in particular formed as Luer-Lock connection, in liquid-permeable connection.
• this residence volume together with the volume of the at least one, in particular the two, connections and the liquid-permeable compound represents the hold-up volume.
• the device can, in particular in the common housing, also include a device for generating a voltage, for example a battery, which is in particular arranged and / or contacted such that it can generate a potential between metal coating of the polymer membrane and counterelectrode.
• a device for generating a voltage for example a battery, which is in particular arranged and / or contacted such that it can generate a potential between metal coating of the polymer membrane and counterelectrode.
• the device is designed in particular as an intent filter and / or syringe attachment.
• Counter electrode and Polymermennbran with two-dimensional and porous coating of metal are particularly electrically insulated from each other.
• Electrosorption and / or electrofiltration device has for this purpose in particular a vessel and / or housing, for the arrangement and / or passage of liquid by the polymer membrane and the counter electrode are arranged electrically insulated from each other.
• the electrosorption and / or electrofiltration device may include one or more reference electrodes.
• the other features described in relation to this method can also be advantageously implemented in the electrosorption and / or electrofiltration apparatus.
• the polymer membrane with metal coating is advantageously a metal-coated polymer membrane as described above. These are particularly well, especially if the porous passages are coated with metal. Since the electrically active surface then significantly larger fails. However, other metal-coated polymer membranes can also be used.
• the counterelectrode is either a further sheet-like, porous coating of metal on a second side opposite the first side or a permeable electrode arranged with the interposition of an insulating and permeable spacer, in particular formed by a metallic mesh.
• the device for carrying out the method for at least temporary separation and / or for the detection of charged biologically active substances in particular with some or all advantageous characteristics, set up.
• it is also adapted for carrying out the method for determining the occupation of the binding sites of the polymer membrane with a planar and porous coating of metal and / or for determining at least one concentration in the liquid.
• the method is carried out in particular with a device according to the invention.
• Figure 1 an inventive electrofiltration device
• FIG. 2 shows an electrofiltration device according to the invention as a syringe attachment filter
• Figure 3 an electro-filtration device according to the invention with a folded membrane formed as a cartridge in a housing.
• FIG. 1 shows an electrofiltration device according to the invention. With this, the electrofiltration process according to the invention can be carried out.
• a liquid is charged into the master vessel (5) and passed through the membrane (6) formed by a metal-coated polymer membrane under voltage applied by a potentiostat (4) between the membrane (6) formed as an electrode and counter electrode (2 ) into the collecting vessel (3).
• the frit (7) serves to stabilize the membrane.
• FIG. 2 shows an electrofiltration device according to the invention designed as a syringe attachment filter. Shown is a round membrane (8) of polymer material, metallized on one side or both sides. The metallization can be applied on one side, upstream of the membrane (in the figure above) or downstream of the membrane (in the figure below) or on both sides. In mutual application, the metallized sides are in particular isolated from each other.
• Figure 2 shows two possible embodiments in a figure. It either accounts for all parts designated by the addition b or all parts designated by addition a.
• the filter also has at least one counterelectrode (10a or 10b, 1aa or 1b). This can be performed for example as a metal grid.
• the syringe attachment filter has a filter inlet (1 3). He also has a filter outlet (1 4). These can include feedthroughs for contacting. These can be realized by cable but also inductively, capacitively, by plug and / or the like.
• the conductors (1 2a or 1 2b) can also serve as a counter electrode and thus replace the counter electrodes (1 0a or 1 0b).
• Filter inlet and filter outlet are in particular part of a housing for hermetic sealing of the entire filter, so that a liquid loss is only possible between the filter inlet and filter outlet and only by passing the arranged in the liquid flow elements, such as round membrane, trend foil and counter electrode, if designed as a permeable or grid ,
• the syringe filter is designed so that it makes it possible to apply a potential between metallization of the circular membrane and counter electrode.
• it has in particular corresponding conductors, feedthroughs and / or contacting and / or transmission devices (in particular inductive and / or capacitive).
• the application of voltage can be realized, for example, via a voltage source (1 5a or 1 5b) and electrical conductors 1 2a or 1 2b and 1 1 a or 1 1 b).
• FIG. 3 shows a cartridge according to the invention in a housing with a folded membrane (1 6).
• Filtfilterkartuschen are prepared as follows:
• the membrane (16) is positioned and folded between two fold aids (17a and 17b), in particular from a polymer flow and / or foil.
• the fabricated folded membrane is pressed into a round cage (Cage) (1 8) so that they do not unfold again and provided with a core.
• Cage and core are in particular made of plastic and in particular designed so that liquid can pass through, in particular provided with rectangular or round holes.
• the membrane with folding aid and cage and core are welded to the upper closure of a closed plastic cap and then welded to the lower closure (plate with opening).
• the method was also used in this exemplary embodiment and can generally be moved with the membrane included and / or used according to the invention.
• Shown in Figure 3 is a folded membrane (1 6) of polymer material, metallized on one side or both sides.
• the metallization may be applied on one side, upstream of the membrane (in the figure outside) or downstream of the membrane (in the figure inside) or on both sides. In mutual application, the metallized sides are in particular isolated from each other by the membrane itself.
• the folding of the membrane takes place, in particular, by means of folding aids folded with the membrane, which in particular consist of a polymer flow (FIG. 7a, b).
• the polymer flow can be designed both as a conductive (with double-sided metal coating) or as stress-insulating flow.
• Figure 3 shows two possible embodiments in a figure. It accounts for either all designated by the addition b parts or all designated with the addition of a parts.
• the membrane is contacted via an electrical line as an electrode directly in the variant in which the designated with the addition of a parts, or in the variant in which the parts designated by the additive b are included, the membrane as an electrode via an electrically conductive folding aid (1 7b) and via an electrically conductive core (core), which holds the folded membrane, contacted.
• the filter also has at least one counterelectrode (25a or 25c).
• This can for example be designed as a metal grid and / or rod electrode.
• the designed as a cartridge with a folded membrane filter has a filter inlet (22). He also has a filter outlet (23). These can include feedthroughs for contacting. These can be realized by cable but also inductively, capacitively, by plug and / or the like.
• the filter inlet and filter outlet are in particular part of a housing for hermetic sealing of the entire filter, so that a liquid loss is only possible between the filter inlet and filter outlet and only by passing the arranged in the liquid flow elements, such as membrane and counter electrode, if formed as a permeable or grid.
• the cartridge with folded membrane is designed so that it makes it possible to apply a potential between metallization of the membrane and counter electrode.
• it has in particular corresponding conductors, feedthroughs and / or contacting and / or transmission devices (in particular inductive and / or capacitive).
• the application of voltage can be realized, for example, via a voltage source (26a or 26b) and electrical conductors 25a or 25b and 24a or 24b).
• 1 7 a and b Electrically insulating, permeable release film in front of or behind the membrane cartridge conductive outer sleeve cartridge conductive inner sleeve upper lock & seal Cartridge baffle Bottom cap and cartridge outlet Filter inlet and filter housing Filter outlet and filter housing
• a Contact bushing for electrical contacting of the upstream metallization of the membrane 1 6 b
• Contact bushing for electrical contacting of downstream metallization of the membrane 1 6 a
• Contact bushing for electrical contacting of the counterelectrode on the downstream Side of the metallized membrane 1 6 c counter electrode on the downstream side of the metallized membrane 1 6 a voltage source for application of electrode and counterelectrode with electrical potential

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• 2016
  • 2016-12-28 DE DE102016125818.0A patent/DE102016125818A1/de active Pending
• 2017
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