WO2013098487A1 - Method and device for taking samples and use of the method and the device - Google Patents

Method and device for taking samples and use of the method and the device Download PDF

Info

Publication number
WO2013098487A1
WO2013098487A1 PCT/FI2012/051303 FI2012051303W WO2013098487A1 WO 2013098487 A1 WO2013098487 A1 WO 2013098487A1 FI 2012051303 W FI2012051303 W FI 2012051303W WO 2013098487 A1 WO2013098487 A1 WO 2013098487A1
Authority
WO
WIPO (PCT)
Prior art keywords
filter
cleaning
flow
fluid
sample
Prior art date
Application number
PCT/FI2012/051303
Other languages
French (fr)
Inventor
Erkki Iikka Sakari RÄSÄNEN
Original Assignee
Kemira Oyj
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 Kemira Oyj filed Critical Kemira Oyj
Publication of WO2013098487A1 publication Critical patent/WO2013098487A1/en

Links

Classifications

    • 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
    • G01N1/20—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials
    • G01N1/2035—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials by deviating part of a fluid stream, e.g. by drawing-off or tapping
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D35/00—Filtering devices having features not specifically covered by groups B01D24/00 - B01D33/00, or for applications not specifically covered by groups B01D24/00 - B01D33/00; Auxiliary devices for filtration; Filter housing constructions
    • B01D35/02—Filters adapted for location in special places, e.g. pipe-lines, pumps, stop-cocks
    • B01D35/027—Filters adapted for location in special places, e.g. pipe-lines, pumps, stop-cocks rigidly mounted in or on tanks or reservoirs
    • B01D35/0276—Filtering elements with a vertical rotation or symmetry axis mounted on tanks or reservoirs
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D35/00—Filtering devices having features not specifically covered by groups B01D24/00 - B01D33/00, or for applications not specifically covered by groups B01D24/00 - B01D33/00; Auxiliary devices for filtration; Filter housing constructions
    • 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
    • G01N2001/1006—Dispersed solids
    • G01N2001/1012—Suspensions
    • 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
    • G01N1/20—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials
    • G01N1/2035—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials by deviating part of a fluid stream, e.g. by drawing-off or tapping
    • G01N2001/205—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials by deviating part of a fluid stream, e.g. by drawing-off or tapping using a valve

Definitions

  • the invention relates to a method and a device for taking a sample / samples from a suspension containing solids and fluid.
  • the invention also relates to use of the method and the device for taking a sample / samples from a suspension containing solids and fluid, for example from process waters.
  • Especially the invention relates to a method according to the preamble part of claim 1 and to a device according to the preamble part of claim 6.
  • Filtration of fluid samples from suspensions is an important sample processing operation in chemical process analytics. Solid fractions must be removed by filtration before determinations, titrations, charge measurements etc. can be made.
  • Sampling filters with different operating principles has been realized for process measurement purposes.
  • Two main principles are cross-flow principle and dead end principle. It is also known from prior art to combine this two principles in sample taking devices and methods.
  • the present invention relates to filtration based on cross-flow principle. Taking filtrate samples from suspensions is not straightforward. Solids in suspensions easily clog the filter, and thus the filter must be cleaned or replaced frequently. In prior art methods for keeping the filter clean are used for example high turbulent shear near the filter surface or shear and ultrasonic sound. Mechanical and physical methods of prior art do not entirely prevent clogging. It is known from prior art also to use chemical cleaning but the known technical realizations have been complex.
  • Prior art cleaning systems are normally based on some mechanical/physical principle, e.g. by applying shear or ultrasonic cavitations near the surface of filter. Washing the filter by chemicals (detergents, solvents, acids, bases, oxida- tive chemicals plus water and pressurized air) would provide very efficient cleaning, but the chemicals must not contaminate the sample or the process flow which leads to complicated technical structures. Especially online separation of filtrate samples is very difficult and cleaning the clogged filter is often the most difficult challenge to overcome. In WO publication 2007/135225 a prior art method for taking samples is disclosed.
  • one or several samples are fractionated from the feed suspension in a fractionating chamber by means of one or several fractionating elements so that the formation of a cake onto the surface of the fractionating element or the blocking of the fractionating element is prevented during fractionation by using ultrasonic technology and/or by rotating the fractionating element.
  • WO Publication 2007/135226 method for taking a liquid sample according to prior art is disclosed.
  • the filter has a rotatable filtering element, filtering means not rotating in relation to the filtering element for the continuous filtering of the liquid through the filtering element and cleaning means not rotating in relation to the filtering element for the continuous cleaning of the filtering element.
  • EP patent application publication 1292816 a filtering device for taking a filtrate sample from liquid matter containing solid particles is disclosed.
  • This prior art device comprises two filter parts and at least one filtering slot between the filter parts, which are adapted to move in relation to each other in such a manner that the width of the filtering slot changes when the filter parts move in rela- tion to each other.
  • the filtering slot between the filter parts is at its smallest and it is adapted to filter the sample while the liquid matter being measured flows from the process to the measurement.
  • the filter parts are adapted to move away from each other whereby the filtering slot widens.
  • US patent publication 5625157 a device for taking a filtrate sample from slush pulp through the wall of a container containing pulp is disclosed.
  • This prior art device comprises a cylinder mounted on the wall so that it goes through the wall, with its open end towards the container, a piston placed in the cylinder space and forming a sampling duct from the open cylinder end into the cylinder space behind the piston and an actuator for moving the piston into an intermediate position in which the piston end forms a pocket limited by the cylinder walls and the piston end for gathering fibrous slush pulp and forming a pillow-like filter in the pocket and into a front position for removing the pillowlike filter into the container, the cylinder is provided with a drain duct for drain- ing off the sample penetrating through the filter and the sampling duct into the space behind the piston for analysis.
  • An object of the invention is to create method and device for taking samples, especially filtrate samples in which the cleaning problems of the filter are elimi- nated or at least minimized.
  • a further object of the invention is to create a cleaning system that does not disturb the sample taking.
  • a further object of the invention is to create a non-complicated device for taking samples.
  • the method according to the invention is mainly characterized by the features of the characterizing part of claim 1 .
  • the device according to the invention is mainly characterized by the features of the characterizing part of claim 6.
  • a process analyzer based on a new sampling device is provided.
  • many practical problems related to online process analytics are solved and thus development of accurate and reliable chemical dosage and process control applications is facilitated.
  • the sampling filter located in connection with a flow tube comprises a rotating valve with filter and a support with cleaning channel.
  • the sampling filter may also comprise the flow tube.
  • the rotating valve is according to an advantageous embodiment at least partly of conical cylinder form.
  • the filter is of cross-flow type i.e. the filtration principle of sampling filter is cross-flow filtration in the device according to one advantageous feature of the invention.
  • the suspension to be filtered flows over the filter, which is positioned substantially perpendicular to flow, and the filtrate sample is separated from the flow through the filter. Thus the formation of cake or mat of solids is minimized by the cross-flow.
  • the filter is cleaned during the process between the sample taking times without the need to stop the suspension flow for cleaning of the filter. According to an advantageous feature of the invention the filter can be cleaned chemically when clogging occurs.
  • the sample channel of the sampling filter In the operating stage and in the operating position the sample channel of the sampling filter is open to the flow tube and the sample channel is closed in respect the cleaning channel such that a sample can be taken by cross-flow and passed through the filter and via the sample channel to for example analytical device.
  • the axial direction of the sample channel is ad- vantageously substantially perpendicular in respect to the axial direction of the cleaning channel.
  • the rotating valve of the sampling filter is in such position that the filter connects to the flow tube.
  • the sample channel of the sampling filter In cleaning stage and in cleaning position the sample channel of the sampling filter is closed to the flow tube and open to the cleaning channel such that the cleaning fluid flow passes through the filter and the sample channel that in this cleaning position forms middle part of the cleaning channel for the cleaning fluid flow.
  • the axial direction of the sample channel is advantageously substantially parallel to the axial direction of the cleaning channel and the filter is positioned by the rotating valve such that the cleaning fluid passes through it.
  • the sample channel of the rotating valve is open to the flow tube and the sample channel is open to the flow tube and closed in respect the cleaning channel such that a sample can be taken by cross-flow and passed through the filter and via the sample channel to for example analytical device.
  • the axial direction of the sample channel is advantageously substantially perpendicular in respect to the axial direction of the cleaning channel.
  • the rotating valve is in such position that the filter connects to the flow tube.
  • the sample channel of the rotating valve In cleaning stage and in cleaning position the sample channel of the rotating valve is closed to the flow tube and open to the cleaning channel such that the cleaning fluid flow passes through the filter and the sample channel that in this cleaning position forms middle part of the cleaning channel for the cleaning fluid flow.
  • the axial direction of the sample channel is advantageously substantially parallel to the axial direction of the cleaning channel and the filter is positioned by the rotating valve such that the cleaning fluid passes through it.
  • a pressure difference is created over the filter by the cross-flow.
  • the sample taking according to cross-flow principle provides for sample taking of high quality and if clogging of the filter for example due to cake forming occurs the cross-flow is disturbed and cleaning is needed.
  • the method and the device for taking samples according to the invention pro- vides for continuous long term sampling without disturbing the process to be sampled.
  • the cleaning of the filter of the device can be done during the process running and the cleaning is automatic.
  • the sample taking is followed by cleaning of the filter.
  • a sensor that checks the state of the filter and gives a signal to the control system of the device if cleaning is needed.
  • the sensor can be for example a pressure sensor observing the pressure difference over the filter i.e. between the flow channel and sample channel. When the magnitude of pressure difference rises above a certain level it gives a control signal to activate the cleaning automatically or to the maintenance personnel for setting the device to cleaning.
  • the device according to the invention can be used as a part of a larger monitoring / dosage concept.
  • the present invention is suitable to be used in sampling of any fluid-like sus- pensions containing solid particles that are filterable and that have solid content advantageously up to 20 %, even up to 50 %. It is even possible to use invention in sampling of suspensions even up to 70% solid contents as long as the suspension is of fluid-like behavioral type.
  • the device according to the invention is less expensive than those of prior art due to simple and robust mechanics and absence of parts that require advanced manufacturing techniques.
  • the invention is usable in connection with different kinds of processes, for example in connection with fiber web producing, processes of food industry, waste water cleaning processes, water handling processes of mining industry, polymerizing processes in which the polymer is in emulsion state, gas handling processes and in processes handling gases with solid particles.
  • the invention is also usable in connection with filtering fractions.
  • the filter of the sample taking device is selected based on the requirements of the particle size of the suspension.
  • the invention also makes is possible to automate analyzer and thus decreases the need of manual work of the laboratory technicians in process monitoring.
  • the filter module is also ideal for fractionation and preparation of samples for online particle size analysis. Filter elements of different pore size can be used, and cross-flow filtration principle ensures precise fractionation.
  • FIG. 1 schematically shows one advantageous example of the device according to the invention
  • Figure 2 schematically shows one advantageous embodiment of the filter device according to the invention during operating stage
  • Figure 3 schematically shows one advantageous embodiment of the filter device according to the invention during cleaning stage.
  • the sampling filter 10 i.e. the filter module comprise a flow tube 1 1 , a rotating valve 21 with filter 20 and a support 25 with cleaning fluid channel 29.
  • the flow tube 1 1 in which the suspension to be sampled flows is connected to the sample channel 26 via rotating valve 21 with filter 20.
  • the cleaning channel 29 is provided with cleaning fluid openings 27A, 27B, 27C.
  • a pump (not shown) is provided in the suction side of the flow tube 1 1 1 . This creates under-pressure into the flow tube 1 1 and into the sample channel 26.
  • the under pressure is beneficial because it prevents leaking of fluid through the connection of flow tube 1 1 and rotating valve 21 . Due to the under pressure in sample channel 26 a sampling pump is provided in the sampling channel. This compensates the pressure difference between the flow channel 1 1 and sample channel 26 and facilitates flow of sample fluid through the filter 20 to sample channel.
  • the size of the device 10 depends on the intended use. For example in a flow tube 1 1 with diameter about 3 cm a rotating valve with diameter 4 - 5 cm is used.
  • the rotating valve 21 is of slightly conical cylinder form tapering in the depth direction of the figure.
  • the conical form is advantageous in view of sealing.
  • the sample channel 26 in the rotating valve can be of any suitable form, e.g. of cylinder form.
  • the sample channel of the rotating valve is substantially perpendicular in respect to the axial direction of the rotating valve.
  • the rotating valve 21 with the filter 20 can be replaceably connected to the flow tube 1 1 for maintenance purposes.
  • FIG 2 is schematically shown the principle of cross-flow filtration in the sampling filter.
  • the suspension to be filtered flows, as shown by arrow Z2 in the flow tube 1 1 over the filter 20 of the rotating valve 21 .
  • the filter 20 is positioned perpendicular to the suspension flow Z2.
  • a filtrate sample as indicated by arrow Z2, is separated from the suspension flow Z1 through the filter 20 of the rotating valve 21 .
  • the fluid sample i.e. the filtrate sample flow Z2 is directed through the sample channel 26 to an analytical device.
  • the valve 21 is rotated 90 degrees so that the sampling channel 26 is closed in respect of the flow tube 1 1 and the cleaning channel 29 is opened so that the cleaning fluid flows through the cleaning channel and through the sampling channel 26 in this cleaning position opened to cleaning channel.
  • the filter 20 is washed with cleaning fluid that can be water, acetone, alcohol, acid, alkali, oxidative chemical etc. After washing the filter 20 can be dried with a purge of air or other gas. After cleaning the filter 20 is ready for sampling again and is rotated back 90 degrees to the operating position as shown in figure 2.
  • the cleaning fluid is led in via cleaning fluid opening 27A and flown through the filter 20 and out via cleaning fluid opening 27C.
  • the rotating valve is advantageously at least partly of conical cylinder form, tapering in the direction of the axis of the cylinder form, advantageously of conical cylinder form.
  • the rotating valve is according to an advantageous embodiment of conical cylinder form at least for a distance around the openings of the sample channel in the rotating valve.
  • the conical form is advantageous in view of sealing.
  • any other suitable form of the rotating valve is also advantageous which form provides sealing around the sample channel openings of the rotating valve.
  • the form of surfaces facing the rotating valve surfaces e.g. surfaces of the support 25, are advantageously formed and arranged to fit with the outer surfaces of the rotating valve, preferably at least for a distance around the openings of the sample channel in the rotating valve. This is advantageous in view of sealing.
  • a fluid sample is filtered through a small filter element 20 that is located in a rotating valve 21 that is located perpendicular to the suspension flow Z1 in the flow tube 1 1 .
  • the valve 21 When the valve 21 is in sampling position, figure 2, the filter 20 is in contact with the suspension from Z1 where the filtrate sample flow Z2 is taken.
  • the valve 21 When the filter 20 becomes clogged, the valve 21 is turned to cleaning position, figure 3. In this position the sample channel 26 is closed to the flow tube 1 1 so that the filter 20 is not in contact with the suspension flow Z1 in the flow tube 1 1 and the cleaning channel 29 is opened for the cleaning fluid.
  • the cleaning fluid is lead to the cleaning channel 29 via cleaning fluid inlet opening 27A, as shown by arrow Z5.
  • the cleaning fluid flows through the sample channel 26 and the filter 20 in the rotating valve 21 as shown by arrows Z6 and to the cleaning fluid outlet opening 27C, as shown by arrow Z7.
  • the excess cleaning fluid is removed via excess cleaning fluid outlet opening 27B.
  • the filter 20 can be washed utilizing chemicals, water and pressurized air. After cleaning, the filter 20 is turned again to sampling position, figure 2.
  • the sample channel 26 of the rotating valve 21 is open to the flow tube 1 1 and the sample channel 26 is open to the flow tube 1 1 and closed in respect the cleaning channel 29 such that a sample can be taken by cross-flow and passed through the filter 20 and via the sample channel 26 to for example analytical device.
  • the axial direction of the sample channel 26 is substantially perpendicular in respect to the axial direction of the cleaning channel 29.
  • the rotating valve 21 is in such position that the filter 20 connects to the flow tube 1 1 .
  • the sample channel 26 of the rotating valve 21 is closed to the flow tube 1 1 and open to the cleaning channel 29 such that the cleaning fluid flow passes through the filter 20 and the sample channel 26 that in this cleaning position forms middle part of the cleaning channel 29 for the cleaning fluid flow.
  • the axial direction of the sample channel 26 is substantially parallel to the axial direction of the cleaning channel 29 and the filter is positioned by the rotating valve 21 such that the cleaning fluid passes through it.

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Hydrology & Water Resources (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention relates to a method for taking a fluid sample from a suspension flow (Z1) of fluid, in particular containing fluid, i.e. liquid and/or gas, and solid matter by filtering with a filter (20). In the method in operating position of the filter (20) in which position the filter (20) is in cross-flow position in relation to the suspension flow fluid samples are taken from the suspension flow (Z1) and in cleaning position of the filter (20) in which position the filter (20) is in a cleaning channel (29) cleaning fluid flow (Z6) is flown through the filter (20).The invention also relates to a device for taking a fluid sample from a suspension flow (Z1) of fluid, in particular containing fluid, i.e. liquid and/or gas, and solid matter by filtering with a filter (20) located in connection with a flow tube (11) for the suspension flow. The device (10) is a filter module that comprises a rotating valve (21) with filter (20) and a support (25) with cleaning channel (29) and that the rotating valve (21) is turnable between at least two positions; operating position in which the filter is in cross-flow position in relation to the suspension flow for taking fluid samples and cleaning position in which the filter (20) is in cleaning channel (29) for flowing a cleaning fluid flow through the filter (20).

Description

Method and device for taking samples and use of the method and the de-
The invention relates to a method and a device for taking a sample / samples from a suspension containing solids and fluid. The invention also relates to use of the method and the device for taking a sample / samples from a suspension containing solids and fluid, for example from process waters. Especially the invention relates to a method according to the preamble part of claim 1 and to a device according to the preamble part of claim 6. In process industry there are many processes in which it is required that a sample / samples are taken from suspensions of fluids and solids. Filtration of fluid samples from suspensions is an important sample processing operation in chemical process analytics. Solid fractions must be removed by filtration before determinations, titrations, charge measurements etc. can be made. Sampling filters with different operating principles has been realized for process measurement purposes. Two main principles are cross-flow principle and dead end principle. It is also known from prior art to combine this two principles in sample taking devices and methods. The present invention relates to filtration based on cross-flow principle. Taking filtrate samples from suspensions is not straightforward. Solids in suspensions easily clog the filter, and thus the filter must be cleaned or replaced frequently. In prior art methods for keeping the filter clean are used for example high turbulent shear near the filter surface or shear and ultrasonic sound. Mechanical and physical methods of prior art do not entirely prevent clogging. It is known from prior art also to use chemical cleaning but the known technical realizations have been complex.
Prior art cleaning systems are normally based on some mechanical/physical principle, e.g. by applying shear or ultrasonic cavitations near the surface of filter. Washing the filter by chemicals (detergents, solvents, acids, bases, oxida- tive chemicals plus water and pressurized air) would provide very efficient cleaning, but the chemicals must not contaminate the sample or the process flow which leads to complicated technical structures. Especially online separation of filtrate samples is very difficult and cleaning the clogged filter is often the most difficult challenge to overcome. In WO publication 2007/135225 a prior art method for taking samples is disclosed. In this method for taking a sample from a suspension containing solids and liquid one or several samples are fractionated from the feed suspension in a fractionating chamber by means of one or several fractionating elements so that the formation of a cake onto the surface of the fractionating element or the blocking of the fractionating element is prevented during fractionation by using ultrasonic technology and/or by rotating the fractionating element.
In WO Publication 2007/135226 method for taking a liquid sample according to prior art is disclosed. In this method for taking a liquid sample from a suspen- sion containing liquid and solid matter by filtering the filter has a rotatable filtering element, filtering means not rotating in relation to the filtering element for the continuous filtering of the liquid through the filtering element and cleaning means not rotating in relation to the filtering element for the continuous cleaning of the filtering element. In EP patent application publication 1292816 a filtering device for taking a filtrate sample from liquid matter containing solid particles is disclosed. This prior art device comprises two filter parts and at least one filtering slot between the filter parts, which are adapted to move in relation to each other in such a manner that the width of the filtering slot changes when the filter parts move in rela- tion to each other. When taking a sample from a process, the filtering slot between the filter parts is at its smallest and it is adapted to filter the sample while the liquid matter being measured flows from the process to the measurement. When rinsing the filtering device against the sampling direction the filter parts are adapted to move away from each other whereby the filtering slot widens. In US patent publication 5625157 a device for taking a filtrate sample from slush pulp through the wall of a container containing pulp is disclosed. This prior art device comprises a cylinder mounted on the wall so that it goes through the wall, with its open end towards the container, a piston placed in the cylinder space and forming a sampling duct from the open cylinder end into the cylinder space behind the piston and an actuator for moving the piston into an intermediate position in which the piston end forms a pocket limited by the cylinder walls and the piston end for gathering fibrous slush pulp and forming a pillow-like filter in the pocket and into a front position for removing the pillowlike filter into the container, the cylinder is provided with a drain duct for drain- ing off the sample penetrating through the filter and the sampling duct into the space behind the piston for analysis.
In WO publication 96/38719 method and apparatus for working up a sample of liquid is disclosed. In this prior art method and apparatus the building up of a mat of solid substances on the inlet side of the filter is prevented by inducing in the sample flow chamber turbulence or a high flow velocity of sample liquid adjacent the filter.
An object of the invention is to create method and device for taking samples, especially filtrate samples in which the cleaning problems of the filter are elimi- nated or at least minimized.
A further object of the invention is to create a cleaning system that does not disturb the sample taking.
A further object of the invention is to create a non-complicated device for taking samples. In order to achieve the above objects and those described later the method according to the invention is mainly characterized by the features of the characterizing part of claim 1 .
The device according to the invention is mainly characterized by the features of the characterizing part of claim 6. By the invention a process analyzer based on a new sampling device is provided. By the invention many practical problems related to online process analytics are solved and thus development of accurate and reliable chemical dosage and process control applications is facilitated.
According to an advantageous feature in the device according to the invention the sampling filter located in connection with a flow tube comprises a rotating valve with filter and a support with cleaning channel. The sampling filter may also comprise the flow tube.
The rotating valve is according to an advantageous embodiment at least partly of conical cylinder form. The filter is of cross-flow type i.e. the filtration principle of sampling filter is cross-flow filtration in the device according to one advantageous feature of the invention. The suspension to be filtered flows over the filter, which is positioned substantially perpendicular to flow, and the filtrate sample is separated from the flow through the filter. Thus the formation of cake or mat of solids is minimized by the cross-flow. The filter is cleaned during the process between the sample taking times without the need to stop the suspension flow for cleaning of the filter. According to an advantageous feature of the invention the filter can be cleaned chemically when clogging occurs. In the operating stage and in the operating position the sample channel of the sampling filter is open to the flow tube and the sample channel is closed in respect the cleaning channel such that a sample can be taken by cross-flow and passed through the filter and via the sample channel to for example analytical device. During operating state the axial direction of the sample channel is ad- vantageously substantially perpendicular in respect to the axial direction of the cleaning channel. The rotating valve of the sampling filter is in such position that the filter connects to the flow tube. In cleaning stage and in cleaning position the sample channel of the sampling filter is closed to the flow tube and open to the cleaning channel such that the cleaning fluid flow passes through the filter and the sample channel that in this cleaning position forms middle part of the cleaning channel for the cleaning fluid flow. During cleaning stage the axial direction of the sample channel is advantageously substantially parallel to the axial direction of the cleaning channel and the filter is positioned by the rotating valve such that the cleaning fluid passes through it. In the operating stage and in the operating position, the sample channel of the rotating valve is open to the flow tube and the sample channel is open to the flow tube and closed in respect the cleaning channel such that a sample can be taken by cross-flow and passed through the filter and via the sample channel to for example analytical device. During operating state the axial direction of the sample channel is advantageously substantially perpendicular in respect to the axial direction of the cleaning channel. The rotating valve is in such position that the filter connects to the flow tube. In cleaning stage and in cleaning position the sample channel of the rotating valve is closed to the flow tube and open to the cleaning channel such that the cleaning fluid flow passes through the filter and the sample channel that in this cleaning position forms middle part of the cleaning channel for the cleaning fluid flow. During cleaning stage the axial direction of the sample channel is advantageously substantially parallel to the axial direction of the cleaning channel and the filter is positioned by the rotating valve such that the cleaning fluid passes through it.
According to an advantageous feature of the invention a pressure difference is created over the filter by the cross-flow.
The sample taking according to cross-flow principle provides for sample taking of high quality and if clogging of the filter for example due to cake forming occurs the cross-flow is disturbed and cleaning is needed.
The method and the device for taking samples according to the invention pro- vides for continuous long term sampling without disturbing the process to be sampled. The cleaning of the filter of the device can be done during the process running and the cleaning is automatic.
Advantageously in connection with the invention the sample taking is followed by cleaning of the filter. It is also possible according to an advantageous fea- ture to provide the device according the invention with a sensor that checks the state of the filter and gives a signal to the control system of the device if cleaning is needed. The sensor can be for example a pressure sensor observing the pressure difference over the filter i.e. between the flow channel and sample channel. When the magnitude of pressure difference rises above a certain level it gives a control signal to activate the cleaning automatically or to the maintenance personnel for setting the device to cleaning.
The device according to the invention can be used as a part of a larger monitoring / dosage concept.
The present invention is suitable to be used in sampling of any fluid-like sus- pensions containing solid particles that are filterable and that have solid content advantageously up to 20 %, even up to 50 %. It is even possible to use invention in sampling of suspensions even up to 70% solid contents as long as the suspension is of fluid-like behavioral type.
The device according to the invention is less expensive than those of prior art due to simple and robust mechanics and absence of parts that require advanced manufacturing techniques. The invention is usable in connection with different kinds of processes, for example in connection with fiber web producing, processes of food industry, waste water cleaning processes, water handling processes of mining industry, polymerizing processes in which the polymer is in emulsion state, gas handling processes and in processes handling gases with solid particles. The invention is also usable in connection with filtering fractions.
The filter of the sample taking device is selected based on the requirements of the particle size of the suspension.
The invention also makes is possible to automate analyzer and thus decreases the need of manual work of the laboratory technicians in process monitoring.
The filter module is also ideal for fractionation and preparation of samples for online particle size analysis. Filter elements of different pore size can be used, and cross-flow filtration principle ensures precise fractionation.
In the following the invention is explained in detail with the reference to the ac- companying drawing in which
Figure 1 schematically shows one advantageous example of the device according to the invention,
Figure 2 schematically shows one advantageous embodiment of the filter device according to the invention during operating stage, Figure 3 schematically shows one advantageous embodiment of the filter device according to the invention during cleaning stage.
In the following same reference signs are used to respective parts of the device if not otherwise mentioned and one advantageous example is described to which the invention is not to be narrowly limited. As shown in figure 1 the sampling filter 10 i.e. the filter module comprise a flow tube 1 1 , a rotating valve 21 with filter 20 and a support 25 with cleaning fluid channel 29. The flow tube 1 1 in which the suspension to be sampled flows is connected to the sample channel 26 via rotating valve 21 with filter 20. The cleaning channel 29 is provided with cleaning fluid openings 27A, 27B, 27C. In the suction side of the flow tube 1 1 a pump (not shown) is provided. This creates under-pressure into the flow tube 1 1 and into the sample channel 26. The under pressure is beneficial because it prevents leaking of fluid through the connection of flow tube 1 1 and rotating valve 21 . Due to the under pressure in sample channel 26 a sampling pump is provided in the sampling channel. This compensates the pressure difference between the flow channel 1 1 and sample channel 26 and facilitates flow of sample fluid through the filter 20 to sample channel. The size of the device 10 depends on the intended use. For example in a flow tube 1 1 with diameter about 3 cm a rotating valve with diameter 4 - 5 cm is used.
In figure 1 the rotating valve 21 is of slightly conical cylinder form tapering in the depth direction of the figure. The conical form is advantageous in view of sealing. The sample channel 26 in the rotating valve can be of any suitable form, e.g. of cylinder form. In figure 1 the sample channel of the rotating valve is substantially perpendicular in respect to the axial direction of the rotating valve. The rotating valve 21 with the filter 20 can be replaceably connected to the flow tube 1 1 for maintenance purposes.
In figure 2 is schematically shown the principle of cross-flow filtration in the sampling filter. The suspension to be filtered flows, as shown by arrow Z2 in the flow tube 1 1 over the filter 20 of the rotating valve 21 . The filter 20 is positioned perpendicular to the suspension flow Z2. A filtrate sample, as indicated by arrow Z2, is separated from the suspension flow Z1 through the filter 20 of the rotating valve 21 . The fluid sample i.e. the filtrate sample flow Z2 is directed through the sample channel 26 to an analytical device.
As shown schematically in figure 3, when the filter 20 clogs up, the valve 21 is rotated 90 degrees so that the sampling channel 26 is closed in respect of the flow tube 1 1 and the cleaning channel 29 is opened so that the cleaning fluid flows through the cleaning channel and through the sampling channel 26 in this cleaning position opened to cleaning channel. The filter 20 is washed with cleaning fluid that can be water, acetone, alcohol, acid, alkali, oxidative chemical etc. After washing the filter 20 can be dried with a purge of air or other gas. After cleaning the filter 20 is ready for sampling again and is rotated back 90 degrees to the operating position as shown in figure 2. The cleaning fluid is led in via cleaning fluid opening 27A and flown through the filter 20 and out via cleaning fluid opening 27C. Excess cleaning fluid is removed from the cleaning channel via cleaning fluid opening 27B. The rotating valve is advantageously at least partly of conical cylinder form, tapering in the direction of the axis of the cylinder form, advantageously of conical cylinder form. The rotating valve is according to an advantageous embodiment of conical cylinder form at least for a distance around the openings of the sample channel in the rotating valve. The conical form is advantageous in view of sealing.
Any other suitable form of the rotating valve is also advantageous which form provides sealing around the sample channel openings of the rotating valve. The form of surfaces facing the rotating valve surfaces, e.g. surfaces of the support 25, are advantageously formed and arranged to fit with the outer surfaces of the rotating valve, preferably at least for a distance around the openings of the sample channel in the rotating valve. This is advantageous in view of sealing.
According to the invention as shown in figures 1 - 3 a fluid sample is filtered through a small filter element 20 that is located in a rotating valve 21 that is located perpendicular to the suspension flow Z1 in the flow tube 1 1 . When the valve 21 is in sampling position, figure 2, the filter 20 is in contact with the suspension from Z1 where the filtrate sample flow Z2 is taken. When the filter 20 becomes clogged, the valve 21 is turned to cleaning position, figure 3. In this position the sample channel 26 is closed to the flow tube 1 1 so that the filter 20 is not in contact with the suspension flow Z1 in the flow tube 1 1 and the cleaning channel 29 is opened for the cleaning fluid. The cleaning fluid is lead to the cleaning channel 29 via cleaning fluid inlet opening 27A, as shown by arrow Z5. The cleaning fluid flows through the sample channel 26 and the filter 20 in the rotating valve 21 as shown by arrows Z6 and to the cleaning fluid outlet opening 27C, as shown by arrow Z7. The excess cleaning fluid is removed via excess cleaning fluid outlet opening 27B. In cleaning position, the filter 20 can be washed utilizing chemicals, water and pressurized air. After cleaning, the filter 20 is turned again to sampling position, figure 2. In the operating stage and in the operating position, figures 1 and 2, the sample channel 26 of the rotating valve 21 is open to the flow tube 1 1 and the sample channel 26 is open to the flow tube 1 1 and closed in respect the cleaning channel 29 such that a sample can be taken by cross-flow and passed through the filter 20 and via the sample channel 26 to for example analytical device. During operating state the axial direction of the sample channel 26 is substantially perpendicular in respect to the axial direction of the cleaning channel 29. The rotating valve 21 is in such position that the filter 20 connects to the flow tube 1 1 . In cleaning stage and in cleaning position the sample channel 26 of the rotating valve 21 is closed to the flow tube 1 1 and open to the cleaning channel 29 such that the cleaning fluid flow passes through the filter 20 and the sample channel 26 that in this cleaning position forms middle part of the cleaning channel 29 for the cleaning fluid flow. During cleaning stage the axial direction of the sample channel 26 is substantially parallel to the axial direction of the cleaning channel 29 and the filter is positioned by the rotating valve 21 such that the cleaning fluid passes through it.
Reference signs used in the drawing
10 filter module
1 1 flow tube
20 filter
21 rotating valve
25 support
26 sample channel
27A, 27B, 27C cleaning fluid opening
29 cleaning channel
Z1 flow of suspension
Z2 fluid sample flow
Z3 flow to analytical device
Z4 excess cleaning fluid flow out
Z5 cleaning fluid flow in
Z6 cleaning fluid flow through filter
Z7 cleaning fluid flow out

Claims

Claims
1 . Method for taking a fluid sample from a suspension flow (Z1 ) of fluid, in particular containing fluid, i.e. liquid and/or gas, and solid matter by filtering with a filter (20), characterized in that in the method in operating position of the filter (20) in which position the filter (20) is in cross-flow position in relation to the suspension flow fluid samples are taken from the suspension flow (Z1 ) and in cleaning position of the filter (20) in which position the filter (20) is in a cleaning channel (29) cleaning fluid flow (Z6) is flown through the filter (20).
2. Method according to claim 1 , characterized in that the cleaning fluid flow (Z5) is lead to the cleaning channel through a cleaning fluid inlet opening (27A) and via the cleaning channel (29) and through the filter (20) as cleaning flow (Z6) and removed via cleaning fluid outlet opening (27C).
3. Method according to claim 1 or 2, characterized in that excess cleaning fluid is removed from the cleaning channel (29) by excess cleaning fluid opening (27B).
4. Method according to any of claims claim 1 to 3, characterized in that suspension to be filtered flows over the filter (20), which is positioned substantially perpendicular to flow, and the filtrate sample is separated from the flow through the filter (20).
5. Method according to any of claims claim 1 to 4, characterized in that the filter is cleaned during the process between the sample taking times without the need to stop the suspension flow for cleaning.
6. Device for taking a fluid sample from a suspension flow (Z1 ) of fluid, in particular containing fluid, i.e. liquid and/or gas, and solid matter by filtering with a filter (20) located in connection with a flow tube (1 1 ) for the suspension flow, characterized in that the device (10) is a filter module that comprises a rotating valve (21 ) with filter (20) and a support (25) with cleaning channel (29) and that the rotating valve (21 ) is turnable between at least two positions; operating position in which the filter is in cross-flow position in relation to the suspension flow for taking fluid samples and cleaning position in which the filter (20) is in cleaning channel (29) for flowing a cleaning fluid flow through the filter (20).
7. Device according to claim 6, characterized in that the filter (20) is positioned substantially perpendicular to flow (Z1 ) in the flow tube (1 1 ) in operating position.
8. Device according to claim 6 or 7, characterized in that the cleaning channel (29) comprises cleaning fluid openings (27A, 27B, 27C).
9. Device according to any of claims 6 - 8, characterized in that the flow tube (1 1 ) is provided with a pump for compensating the under pressure in sample channel (26) and facilitating the flow of sample fluid.
10. Use of the method according to any of claims 1 - 5 in connection with pro- cesses, in particular in connection with fiber web producing, processes of food industry, waste water cleaning processes, water handling processes of mining industry, polymerizing processes in which the polymer is in emulsion state, gas handling processes and in processes handling gases with solid particles and in connection with filtering fractions.
1 1 . Use of the device according to any of claims 6 - 9 in connection with processes, in particular in connection with fiber web producing, processes of food industry, waste water cleaning processes, water handling processes of mining industry, polymerizing processes in which the polymer is in emulsion state, gas handling processes and in processes handling gases with solid particles and in connection with filtering fractions.
PCT/FI2012/051303 2011-12-30 2012-12-28 Method and device for taking samples and use of the method and the device WO2013098487A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FI20116338 2011-12-30
FI20116338A FI20116338A (en) 2011-12-30 2011-12-30 Method and apparatus for sampling and use of method and apparatus

Publications (1)

Publication Number Publication Date
WO2013098487A1 true WO2013098487A1 (en) 2013-07-04

Family

ID=47559543

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/FI2012/051303 WO2013098487A1 (en) 2011-12-30 2012-12-28 Method and device for taking samples and use of the method and the device

Country Status (2)

Country Link
FI (1) FI20116338A (en)
WO (1) WO2013098487A1 (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017104261A1 (en) * 2015-12-14 2017-06-22 株式会社村田製作所 Filtration device
WO2019058865A1 (en) * 2017-09-25 2019-03-28 株式会社村田製作所 Filtration device
WO2019063872A1 (en) * 2017-09-29 2019-04-04 Outotec (Finland) Oy A backfill slurry sampling apparatus, and backfill system equipped with such sampling apparatus
CN110595834A (en) * 2019-09-19 2019-12-20 合肥万丰油脂有限公司 Rapeseed oil sampling device
CN111093797A (en) * 2017-09-19 2020-05-01 株式会社村田制作所 Filtering device and filtering method
US12031970B2 (en) 2021-06-09 2024-07-09 Precision Planting Llc Agricultural sampling system and related methods

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3826281A (en) * 1969-10-29 1974-07-30 Us Navy Throttling ball valve
FI930766A (en) * 1993-02-19 1994-08-20 Keskuslaboratorio Method and apparatus for sampling solid media
US20020059996A1 (en) * 1996-12-10 2002-05-23 Petri Pursiheimo Sampling method and method for cleaning sampling apparatus
WO2007135226A1 (en) * 2006-05-24 2007-11-29 Valtion Teknillinen Tutkimuskeskus A method for taking a liquid sample
US20080169443A1 (en) * 2007-01-17 2008-07-17 Donald Loloff Ball valve
DE102008036650A1 (en) * 2008-08-01 2010-04-15 Holstein, Viktor, Dipl.-Ing. (FH) Ball valve for use in cooling tower of cooling system, has filter element attached inside throughflow opening of ball cock plug

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3826281A (en) * 1969-10-29 1974-07-30 Us Navy Throttling ball valve
FI930766A (en) * 1993-02-19 1994-08-20 Keskuslaboratorio Method and apparatus for sampling solid media
US20020059996A1 (en) * 1996-12-10 2002-05-23 Petri Pursiheimo Sampling method and method for cleaning sampling apparatus
WO2007135226A1 (en) * 2006-05-24 2007-11-29 Valtion Teknillinen Tutkimuskeskus A method for taking a liquid sample
US20080169443A1 (en) * 2007-01-17 2008-07-17 Donald Loloff Ball valve
DE102008036650A1 (en) * 2008-08-01 2010-04-15 Holstein, Viktor, Dipl.-Ing. (FH) Ball valve for use in cooling tower of cooling system, has filter element attached inside throughflow opening of ball cock plug

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017104261A1 (en) * 2015-12-14 2017-06-22 株式会社村田製作所 Filtration device
CN111093797A (en) * 2017-09-19 2020-05-01 株式会社村田制作所 Filtering device and filtering method
US11786847B2 (en) 2017-09-19 2023-10-17 Murata Manufacturing Co., Ltd. Filtration device and filtration method
WO2019058865A1 (en) * 2017-09-25 2019-03-28 株式会社村田製作所 Filtration device
CN111107920A (en) * 2017-09-25 2020-05-05 株式会社村田制作所 Filter device
JPWO2019058865A1 (en) * 2017-09-25 2020-07-30 株式会社村田製作所 Filtration device
US11529579B2 (en) 2017-09-25 2022-12-20 Murata Manufacturing Co., Ltd. Filtration device
WO2019063872A1 (en) * 2017-09-29 2019-04-04 Outotec (Finland) Oy A backfill slurry sampling apparatus, and backfill system equipped with such sampling apparatus
CN110595834A (en) * 2019-09-19 2019-12-20 合肥万丰油脂有限公司 Rapeseed oil sampling device
US12031970B2 (en) 2021-06-09 2024-07-09 Precision Planting Llc Agricultural sampling system and related methods

Also Published As

Publication number Publication date
FI20116338A (en) 2013-07-01

Similar Documents

Publication Publication Date Title
WO2013098487A1 (en) Method and device for taking samples and use of the method and the device
JP5054760B2 (en) Ultrafiltration system for online analyzer
US7208091B2 (en) Assembly for withdrawing and filtering partial volumes of process fluid
EP2510331A2 (en) Liquid to liquid biological particle concentrator with disposable fluid path
AU2005298601B2 (en) Filter assembly for sampling
EP1194217A1 (en) Method and apparatus for testing the integrity of filtering membranes
KR100775977B1 (en) Solid-liquid seperation and filteration apparatus
CN115060571A (en) Liquid-to-liquid bio-particle concentrator with disposable fluid path
CN101341389A (en) Method and device for testing the integrity of filtration membranes
US20080308494A1 (en) Fluid sampling interface apparatus
WO1996018100A1 (en) System for detecting contaminants
KR100776455B1 (en) Method of monitoring a papermaking process and system
CN102243156A (en) Cup-shaped water sample online filtering device
US6018989A (en) Method and apparatus for measuring the properties of a fiber or colloid suspension
US5964984A (en) Method and apparatus for working up a sample of liquid
EP2853304B1 (en) A device for cleaning a gas to be analyzed from a dispersed phase
KR200423610Y1 (en) The ultra filteration system for on-line analyzer
CN213456949U (en) Resistant dirty performance detection device of milipore filter material
US20230173414A1 (en) System for separating suspended substances from a liquid using a cyclone filter-type assembly
SU890116A1 (en) Sampler
CN108367215B (en) Device for filtering suspended matter
DE3519265A1 (en) Filtration system coupled to a reactor comprising automatic sample inlet for processing and analysing samples from fermentation processes
WO2013014475A1 (en) Apparatus for fluid sample filtration
WO2001002831A1 (en) Method and apparatus for measuring retention of a substance
JPH0641899B2 (en) Method for measuring physical properties of fluid in fluid treatment device

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 12815730

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 12815730

Country of ref document: EP

Kind code of ref document: A1