WO2004069377A1 - Dispositif de filtrage de flux transversal et procede pour le faire fonctionner - Google Patents

Dispositif de filtrage de flux transversal et procede pour le faire fonctionner Download PDF

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Publication number
WO2004069377A1
WO2004069377A1 PCT/CH2004/000023 CH2004000023W WO2004069377A1 WO 2004069377 A1 WO2004069377 A1 WO 2004069377A1 CH 2004000023 W CH2004000023 W CH 2004000023W WO 2004069377 A1 WO2004069377 A1 WO 2004069377A1
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WO
WIPO (PCT)
Prior art keywords
filter element
flow
mixture
substances
filtration
Prior art date
Application number
PCT/CH2004/000023
Other languages
German (de)
English (en)
Inventor
Eduard Hartmann
Original Assignee
Bucher-Guyer Ag
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 Bucher-Guyer Ag filed Critical Bucher-Guyer Ag
Publication of WO2004069377A1 publication Critical patent/WO2004069377A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
    • B01D63/06—Tubular membrane modules
    • B01D63/069—Tubular membrane modules comprising a bundle of tubular membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
    • B01D63/06—Tubular membrane modules
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/70—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
    • A23L2/72—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter by filtration
    • A23L2/74—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter by filtration using membranes, e.g. osmosis, ultrafiltration
    • 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
    • B01D61/14—Ultrafiltration; Microfiltration
    • B01D61/145—Ultrafiltration
    • B01D61/146—Ultrafiltration comprising multiple ultrafiltration steps
    • 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
    • B01D61/14—Ultrafiltration; Microfiltration
    • B01D61/22—Controlling or regulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
    • B01D63/06—Tubular membrane modules
    • B01D63/068—Tubular membrane modules with flexible membrane tubes
    • 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
    • B01D65/08—Prevention of membrane fouling or of concentration polarisation
    • 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
    • B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
    • B01D2321/16—Use of chemical agents

Definitions

  • the invention relates to a plant for crossflow filtration according to the preamble of claim 1 and to a method for its operation according to the preamble of claim 7.
  • Such systems are used to advantage when it comes to filtering molecularly disperse or colloidally disperse substance mixtures, if necessary with proportions of solids or suspended matter.
  • mixtures of substances are mixtures of substances which initially arise in the production of fruit and fruit juices. These mixtures of substances are then separated on the one hand by filtration into clear fruit or fruit juice and on the other hand the essentially remaining turbid substances.
  • activated carbon, gelatin, bentonite or silica sol, etc. can also be added to the mixture of substances in order to achieve certain effects. These additives must then also be separated from the liquid with the cloudy substances.
  • a system for cross-flow filtration of the type mentioned in the preamble of claims 1 and 7 is known from WO-Al-01/51186.
  • a solution is shown here how blockages of the filtration module can be removed by fixed retentate portions.
  • the problem with systems of this type is that the filter elements can become blocked, so that production must be interrupted in order to first remove the blockages. Production interruptions are undesirable.
  • a membrane filtration system in which a part of the medium fed to the filter element from a batch tank is passed through a vessel in which the medium is stirred.
  • the torque on the shaft of the agitator is measured and is intended to provide information about the viscosity of the material to be filtered. If the viscosity exceeds a certain limit value, the feed pump to the filter element is stopped, whereby the filtration is interrupted.
  • the molecularly disperse or colloidally disperse substance mixtures mentioned at the outset if these substance mixtures exhibit pseudoplastic behavior and have a high viscosity, the stoppage of the pump would inevitably lead to immediate blocking of the filter element.
  • the problem that the filtration modules can clog exists on the one hand during the filtration operation when the return of retentate to the batch tank increases the solids content in the material to be filtered and finally a critical limit that leads to clogging of the filtration modules is exceeded.
  • the problem may already exist at the beginning of the filtration process if the mixture of substances filled into the batch tank has an excessively high viscosity from the outset.
  • a problem can also arise in the batch tank if, due to the separation processes occurring when the filtration system is at a standstill, there is a mixture of substances with a very high solids content in the batch tank at the bottom of the batch tank, which then enters the filtration circuit first at the start of the filtration process. This can lead to blocking of the filtration modules right at the beginning of the filtration.
  • the invention has for its object to provide a system whose operational safety is improved.
  • a measuring section is connected in parallel to the filter element, in which a flow meter for detecting the flow through this measuring section is arranged.
  • the measuring section is designed in such a way that it has a flow behavior that largely corresponds to that of the individual modules of the filter element.
  • FIG. 1 shows a diagram of a plant according to the invention for crossflow filtration
  • Fig. 5 is a flow chart for the flow
  • Fig. 6 is a flow chart.
  • 1 means a filter element in which the desired liquid phase is separated from the mixture of substances.
  • the design of the filter element 1 is not important.
  • the invention is primarily used when the filter element 1 contains, for example, wound or linear tubular membranes, since such filter elements 1 mostly process substance mixtures with high turbid contents.
  • the filter element 1 can consist of a large number of tubular membranes, which are connected in parallel, or of a series connection of several bundles of several tubular membranes. If parts of the filter element 1 become blocked, this regularly leads to an interruption in operation with all of its adverse consequences. Blocking of such tubular membranes of the filter element 1 can be prevented by the invention.
  • the mixture of substances to be filtered is located in a batch tank 2. From there it passes through a feed line 3 to the filter element 1.
  • a feed pump 4, a flow control valve 5 and a flow sensor 6 are used in the feed line 3, the flow sensor 6 being known in this way the flow control valve 5 acts so that the flow in the feed line 3 remains constant. It is also known that the flow sensor 6 directly affects the speed of the feed pump 4, which also keeps the flow in the supply line 3 constant. This control effect is shown in FIG. 1 with a dashed line. Then can be dispensed with the flow control valve 5. A constant flow rate, however it is achieved, enables an even production.
  • a filter shut-off valve 7 is inserted in the feed line 3 in front of the filter element 1 in order to be able to interrupt the material flow to the filter element 1.
  • a permeate line 8 is connected to it, through which the permeate separated off in the filter element 1, for example the clear fruit juice, can be removed.
  • a return line 9 leads from the filter element 1 to the batch tank 2.
  • a second shut-off valve 10 is installed behind the filter element 1 in the return line 9 in order to also be able to shut off the filter element 1 against the return line 9.
  • the switching state of the second shut-off valve 10 corresponds to the switching state of the filter shut-off valve 7. Both valves 7, 10 are therefore always either open or closed, which is no longer mentioned in the following.
  • the retentate leaving the filter element 1 is returned to the batch tank 2 by the return line 9.
  • a pressure control valve 11 is inserted behind the second shut-off valve 10.
  • This pressure control valve 11 can be controlled by a supply line pressure sensor 12 which detects the pressure in the supply line 3 and thus, when the filter shut-off valve 7 is open at the retentate inlet of the filter element 1.
  • the pressure in the feed line 3, which can be detected by the feed line pressure sensor 12 directly in front of the filter element 1, is related to the delivery rate of the feed pump 4 and the state of the filter element 1.
  • the longer the filtration the more the concentration of solids or suspended matter in the mixture of substances and thus also the viscosity of the mixture of substances in the batch tank 2 increases. Depending on this increasing flow resistance caused by the change in viscosity, the pressure control valve 11 is now increasingly opened.
  • a bypass line 13 is connected in parallel to the filter element 1 and branches off from the supply line 3 in front of the filter shut-off valve 7 and opens into the return line 9 behind the second shut-off valve 10 and before the pressure control valve 11.
  • a bypass shut-off valve 14 is inserted in the bypass line 13.
  • a monitoring device 15 is arranged between the feed line 3 and the return line 9 parallel to the filter element 1 and to the bypass line 13 and serves to detect a quantity which is directly related to the flow of the substance mixture, ie is not a viscosity meter.
  • the monitoring device 15 consists of a
  • the flow meter 16 transmits the value it has measured for the flow through the monitoring device 15 to a control unit 18, with which the system for cross-flow filtration in a known and, as will be explained, additionally also in a manner according to the invention is controlled.
  • the monitoring device 15 can be shut off at least with respect to the feed line 3 by means of a slide 19.
  • the measuring section 17 of the monitoring device 15 is designed in such a way that it has approximately the same flow conditions as in the individual tube membranes of the filter element 1. Accordingly, the flow rate through the measuring section 17 is comparable to the expected flow rate through the individual tube membranes of the filter element 1 ,
  • the pressure control valve 11 is controlled by the supply line pressure sensor 12 even before the start of the filtration with the filter shut-off valve 7 closed, so that the pressure drop across the bypass line 13 is approximately as great as it will later be during the filtration Filter element 1 is regulated.
  • the flow through the measuring section 17 is representative of the later Flow through the filter element 1. If the flow rate in the measuring section 17 is equal to or greater than the flow rate in the filter element 1 required for the filtration, the filtration can be started. If, on the other hand, the flow rate in the measuring section 17 is lower than the flow rate in the filter element 1 required when the filtration is carried out, there is a risk of the filter element 1 becoming blocked. The mixture of substances must then not be fed to the filter element 1, and the filtration must therefore not be started.
  • a product line 20 is shown in FIG. 1, by means of which the batch tank 2 can be refilled.
  • Batch tank 2 the mixture of substances to be filtered. If it has been there for a long time, this can result in solid or suspended matter partially settling in batch tank 2 during this shutdown of the plant. In batch tank 2, segregation and / or viscosity change has therefore taken place during standstill, which has been indicated in FIG. 1 by the hatching lines in batch tank 2 having smaller distances in the lower region. If the system is now put into operation, a mixture of substances with a much higher solids content is first required for filter element 1. The viscosity can also be increased by cooling the mixture of substances. Here, and even if the mixture of substances in the batch tank 2 is generally too viscous, there is a risk that the filter element 1 will block immediately.
  • the filter shut-off valve 7 initially remains closed, as a result of which no mixture of substances can flow to the filter element 1.
  • the bypass shut-off valve 14 is opened.
  • the substance mixture conveyed by the feed pump 4 is passed through the bypass line 13 and then back to the batch tank 2.
  • the pressure control valve 11 is controlled by the supply line pressure sensor 12.
  • the mixture of substances also flows through the monitoring device 15.
  • the flow meter 16 supplies the value of the current flow rate through the monitoring device 15 to the control device 18. If this flow rate is compared to the expected flow rate through the Filter element 1 small, this is a sign that the mixture has too high a viscosity. If this mixture of substances were passed to filter element 1, there would be a risk of blocking filter element 1.
  • the viscosity of the required mixture of substances due to the segregation in the batch tank 2 is very high, there is a risk that the measuring section 17 of the monitoring device 15 will block. This should be avoided as far as possible, since the measuring section 17 would then have to be cleaned and even replaced, which would mean an interruption in production. According to the method according to the invention, it is therefore provided that at the beginning of a filtration process the measuring section 17 of the monitoring device 15 is not yet flowed through by the substance mixture. This is achieved that the slide 19 remains closed first. Now at the beginning of the process flow, the mixture of substances to be filtered initially flows only from batch tank 2 through the bypass line 13 back to batch tank 2.
  • the mixture of substances conveyed first for example mixture of substances with a much higher solids content, now returns to batch tank 2 and mixes in Introduce with the mixture of substances located in the top of the batch tank 2 with a much lower solids content.
  • the slide 19 can be opened so that the mixture of substances flows through the monitoring device 15 as mentioned. It is now possible to determine how large the flow through the monitoring device 15 is. If the flow meter 16 determines that there is a flow through the monitoring device 15, the magnitude of the flow rate is tracked over time. Does that change
  • the measuring section 17 of the monitoring device 15 would block under certain circumstances after opening the slide 19. This is in one Case quite acceptable. The measuring section 17 can then be replaced, which does not cause great costs. The blocking of parts of the filter element 1, which would cause enormous costs, is definitely prevented.
  • the filter shutoff valve 7 can be opened and the bypass shutoff valve 14 can be closed approximately simultaneously. This is how the filtration begins. This start-up of the system can be triggered automatically by the control unit 18, to which the signal from the flow meter 16 is fed. It is then not necessary to start up the system based solely on experience, which also includes the possibility of errors. At the same time, there is no need for an agitator in the batch tank 2, with which the segregation could be reduced before starting.
  • the measuring section 17 continues to flow through even after the start of the filtration, it can now also be checked whether the measuring section 17 of the monitoring device 15 is actually representative of the filter element 1. This test is possible by comparing the values for the flow rate, which the flow transmitter 6 on the one hand and the flow meter 16 on the other hand determine.
  • the measuring section 17 is designed here as a tube winding. It is advantageously made of a flexible plastic tube. Their dimensions such as length and inner diameter, advantageously also the winding diameter, correspond to coiled tubular membranes as are installed in the filter element 1.
  • each tube membrane of the filter element 1 has an inner diameter of 5.5 mm and a length of 32 m, this results in a throughput of 80 m 3 / h, for example, corresponding to a flow speed of 2.6 m / sec. If this flow rate is not reached when the cross-flow filtration system is started up when the mixture of substances flows through the bypass line 13 and through the monitoring device 15, the mixture of substances should not be introduced into the filter element 1. The filter shut-off valve 7 then remains closed, so the filtration process is not started.
  • the control unit 18 can now start the actual filtration process by opening the filter shut-off valve 7 by the control unit 18.
  • FIG. 3 A variant is shown in FIG. 3, in which a wound tubular membrane of the type used in the filter element 1 several times, for example 200 to 300 times, is used as the measuring section 17 instead of the flexible plastic hose. Because permeate emerges from the measuring section 17, the measuring section 17 is placed in a housing 30 in which the permeate passing through the tubular membrane is collected and then fed directly or indirectly to the return line 9 by means of a drain line 31.
  • the measuring section 17 here consists of a bundle 40 of linear tubular membranes 41 arranged in parallel.
  • the structure of the bundle 40 corresponds to the corresponding bundles of tubular membranes as they are arranged several times in the filter element 1.
  • the filter element 1 can consist of a large number of tubular membranes which are connected in parallel, or of a series connection of several bundles of several tubular membranes.
  • a known filter element 1 consists, for example, of twenty bundles connected in series, each of the bundles consisting of nineteen tubular membranes arranged in parallel.
  • the measuring section 17 In adaptation to such a filter element 1, the measuring section 17 according to this embodiment consists of nineteen parallel tubular membranes 41, which, however, are connected in series within the bundle 40, which is achieved in a simple manner in that in each case one end of a tubular membrane 41 with a End of a following tubular membrane 41 is connected by a crimper 42.
  • the measuring section 17 thus consists of nineteen tubular membranes 41 connected in series. This results in a very good approximation of the properties of the entire filter element 1 without great effort.
  • FIG. 5 shows a diagram in which the time profile of the flow rate v determined by the flow meter 16 (FIG. 1) is shown.
  • the course of the flow velocity v is shown when the system starts up, as previously described.
  • a dashed line shows a limit value G v for the flow rate v, below which the filtration should not take place. If there is a mixture of substances with a higher solids content or a mixture of substances with a higher viscosity in the lower area of the batch tank 2, this is conveyed first.
  • the flow meter 16 therefore initially measures a value of the flow velocity v which is too small. This value increases as soon as a mixture of substances with a lower solids content is conveyed. The value can then drop again, however, because a mixture of substances with a higher solids content is fed back into the batch tank 2, as described above.
  • a pre-mixing time is designated by t v during which the required mixture of substances is returned to the batch tank 2.
  • a setpoint t v soi ⁇ for this premix time t v can be stored in the control unit 18. If the premixing time t v has expired, the course of the flow rate v is further monitored during a further measuring time t mess . If the flow rate v does not fall below the limit value G v during this time, the switchover to filtration can take place, for example, by closing the bypass shut-off valve 14 (FIG. 1) and opening the filter shut-off valve 7 and the pressure control valve 11.
  • the process just described is also shown as a flow chart.
  • the process of the premix time t v is monitored. If this has expired, that is to say the premixing time t v is greater than the target value t v s o i ⁇ 5 , the measuring time t meS s begins.
  • the premixing time t v is advantageously chosen to be at least sufficiently long that during this time approximately one third of the content of the batch tank 2 has been circulated.
  • the effective size of the premixing time t v thus also depends on the delivery capacity of the pump 4. The size of the premixing time t v is therefore determined according to the circumstances of the entire system.
  • the measurement of the flow rate v begins. If the measured values for the speed v are less than the limit value G v , a fault message is issued and the system is then stopped. If the measured values of the flow rate v are greater than the limit value G v , the decision is made as to whether the measuring time t meS s has expired. Once this has expired, the filtration is released. Then the filter shutoff valve 7 and the pressure control valve 11 are opened and the bypass shutoff valve 14 is closed.
  • the flow chart thus contains the teaching that during the measuring time t mess the measured speed v never less than the threshold G may be v, to be able to release the filtration. If a drop in the flow velocity v occurs during the measuring time t mess , which is shown in FIG. 6 with a broken line, the filtration is not released.
  • the measuring section 17 should advantageously also be flowed through by the mixture of substances during the filtration. This even if, after the start of the filtration in the filter element 1, the monitoring device 15 does not have to be flowed through because, as described above, its measured values are not taken into account in the control of the system.
  • the purpose of the measure that the measuring section 17 is also flowed through by the mixture of substances in these cases during the filtration operation is that the measuring section 17 and filter element 1 experience the same influence by the mixture of substances during the filtration process.
  • substances settle in or on the membrane tubes, which changes the filtration effect of the membrane tubes.
  • the measuring section 17 continues to flow through the measuring section 17 as well as during the ongoing filtration, the same change in the filtration effect takes place both in the membrane tubes of the filter element 1 and in the measuring section 17. During the entire filtration process, the flow properties of the measuring section 17 are therefore an image of the flow properties of the filter element 1.
  • the measuring section 17 is such that it has a flow which largely corresponds to that of the individual modules of the filter element 1, it is advantageous that this also applies to the ongoing filtration process, even if during the Filtration process the values determined on the measuring section 17 for the control of the system are not taken into account. Since the properties of the filter element 1 change during the filtration process, the System are operated so that the measuring section 17 is subject to the same influences as the filter element 1. Thus, for example, if the filter element 1 is rinsed or chemically cleaned, it is advantageous if the measuring section 17 is also rinsed or chemically cleaned. If the system is operated with a new filter element 1, a new measuring section 17 is also installed.
  • the solutions shown are not limited to the hydraulic circuit shown in FIG. 1. They can be used in the same way in systems with continuous retentate removal and also in systems with only partial return of the retentate to the batch tank 2, in which part of the retentate is thus returned to the feed line 3 bypassing the batch tank 2.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

La présente invention concerne un dispositif de filtrage de flux transversal comprenant au moins un élément de filtrage (1) qui peut recevoir un mélange de substances à filtrer issu d'un réservoir de mélange (2), via une conduite d'amenée (3). Dans la conduite d'amenée (3) se trouvent une pompe de transport (4) et un capteur d'écoulement (6), le capteur d'écoulement (6) permettant la régulation de la capacité de transport à travers la conduite d'amenée (3). Selon l'invention, parallèlement à l'élément de filtrage (1) et à une conduite de dérivation (13) se trouve un système de surveillance (15) qui comprend une section de mesure (17) et un élément de mesure de débit (16) grâce auxquels le débit du mélange de substances à travers la section de mesure (17) du système de surveillance (15) peut être mesuré. Grâce aux données fournies par le système de surveillance (15), le dispositif peut être commandé par un dispositif de commande (18) de sorte que la sécurité de fonctionnement du dispositif se trouve augmentée. Un dispositif de ce type convient au filtrage de mélanges de substances composés d'un liquide et de substances solides ou en suspension, et peut être utilisé par exemple pour la production de jus de fruits.
PCT/CH2004/000023 2003-01-29 2004-01-19 Dispositif de filtrage de flux transversal et procede pour le faire fonctionner WO2004069377A1 (fr)

Applications Claiming Priority (2)

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CH126/03 2003-01-29
CH1262003 2003-01-29

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04371218A (ja) * 1991-06-19 1992-12-24 Kurita Water Ind Ltd 膜分離装置の給液装置
WO2001051186A1 (fr) * 2000-01-13 2001-07-19 Bucher-Guyer Ag Procede et dispositif pour liberer des chemins d'ecoulement dans des modules de filtration

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04371218A (ja) * 1991-06-19 1992-12-24 Kurita Water Ind Ltd 膜分離装置の給液装置
WO2001051186A1 (fr) * 2000-01-13 2001-07-19 Bucher-Guyer Ag Procede et dispositif pour liberer des chemins d'ecoulement dans des modules de filtration

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
PATENT ABSTRACTS OF JAPAN vol. 17, no. 243 17 May 1993 (1993-05-17) *

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