JPH0437935B2 - - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an apparatus for automatically collecting a clear sample liquid from a suspension such as a fermentation liquid.

In devices that collect clear sample liquid from suspensions containing solids, such as fermentation liquids, the suspension filtration tubes tend to become clogged, and the filtration tubes must be replaced within a relatively short period of time. Maintenance is not easy.

In order to eliminate these drawbacks, two filter tubes and a liquid circulation device are used, and the suspension in the liquid tank is filtered through the first filter tube, and the resulting clear sample liquid is sampled. The required amount of clarified sample liquid is collected in this sample collection cell, and the remaining clarified sample liquid is returned to the liquid tank via the second filtration cylinder.Then, the direction of the liquid flow is reversed and a second A sampling device has been proposed that is configured to alternately repeat the operations of filtering the suspension through two filter tubes and returning the remaining clear sample liquid to the liquid tank via the first filter tube.
(Japanese Unexamined Patent Publication No. 57-68781) In this device, while one filter tube is performing filtration, the other filter tube is backwashed, so clogging of the filter tube can be effectively prevented. However, the structure is somewhat complicated in that it requires two filter tubes, and depending on the type of suspension, clogging may occur depending on the type of suspension. In that case, it is necessary to replace both filter tubes with new ones.

The present invention is configured so that a suspension is filtered using one filter cylinder, and backwashing is performed during a suspension period of supply of the clear sample liquid obtained by the filtration to the analyzer. Therefore, with a relatively simple configuration, it is possible to effectively prevent clogging of the filter cylinder without interfering with analysis operations, and to prevent clogging in a relatively short period of time depending on the type of suspension. The object of the present invention is to realize an automatic liquid sampling device in which only a part of the filtration tube and the cylindrical porous body can be replaced, and there is no need to replace the entire filtration tube, thereby reducing maintenance costs.

FIG. 1 is a diagram showing an embodiment of the present invention, in which 1 is a liquid tank made of metal such as stainless steel, 2 is a suspension of fermentation liquor, etc., and 3 is a filter tube made of metal such as stainless steel. The area from the lower end to an appropriate height, that is, the entire circumference of the part immersed in the fermentation liquid 2,
A filter 4 is formed of a cylindrical porous body capable of blocking solid matter such as fermentation bacteria and allowing liquid to pass through, and its lower end is airtightly and watertightly sealed by a sealing bottom wall 5 made of metal such as stainless steel. It has been done.

Reference numeral 6 denotes a stopper that is detachably attached to the upper opening of the filter cylinder 3 to airtightly seal the opening, and is made of, for example, silicone rubber.

7 is a liquid suction tube, for example, the inner diameter is 1 mm to 2 mm.
It is made of a metal tube made of stainless steel or the like, and is inserted into the filtration tube 3 while maintaining airtightness between it and the sealing plug 6.

8 is a gas suction tube, for example, the inner diameter is 1 mm to 2 mm.
It is made of a metal tube made of stainless steel or the like, and is inserted into the filtration tube 3 while maintaining airtightness between it and the sealing plug 6, and its inner end is positioned relatively at the upper part of the filtration tube 3.

Note that the filter tube 3 is inserted into the liquid tank 1 while maintaining airtightness between it and the upper opening of the liquid tank 1.

9 is a three-way valve, 10 is a liquid suction pump, and 11 is a gas delivery pump, which pressurizes gas into the filter cylinder 3 via the three-way valve 9 and the liquid suction pipe 7. 12 is a gas suction pump, 13 is an on-off valve, and 14 is an analyzer, which is a conventionally known suitable analyzer.

FIG. 2 is an enlarged cross-sectional view showing an example of the specific structure of the filter 4 and sealing bottom wall 5 provided at the lower end of the filter cylinder 3, and FIG. 3 is an X-Y cross-sectional view of FIG. , In both figures, 23 is a support cylinder, which corresponds to the part of the cylinder above the filter 4 of the filter cylinder 3 shown in Fig. 1, and has an outer diameter of about 10 mm to 20 mm and a wall thickness of 2 mm to 3 mm. It is made of a metal tube made of stainless steel or the like, and has a connecting step with a filter at its lower end.

24 is a filter, which is similar to the filter 4 shown in FIG.
It is made of a cylindrical porous body formed by sintering a cylindrical metal such as stainless steel or a cylindrical ceramic having an outer diameter approximately equal to that of the support cylinder 23.

A sealing bottom wall 25 corresponds to the sealing bottom wall 5 shown in FIG. 1 and is made of metal such as stainless steel.
A connecting step with the lower end of the filter 24 is provided around it, and an insertion hole 27 for a fixing screw 26 is bored in the center.

Reference numeral 28 denotes a support at the upper end of the fixing screw 26, which is formed, for example, into an elongated plate-like body so as not to obstruct the insertion of the liquid suction tube 7, and whose both ends are fixed to the inner wall of the support cylinder 23. The upper end of a fixing screw 26 is fixed to the portion.

Numeral 29 is a tightening screw, for example, a butterfly screw. 30 is a washer, and 31 to 33 are O-rings.

Note that the fixing screw 26, support body 28, tightening screw 29, washer 30, etc. are also made of metal materials such as stainless steel.

As shown in FIG. 2, an O-ring 31 is interposed between the connecting stage at the lower end of the supporting cylinder 23 and the upper end of the filter 24, and the connecting stage at the lower end of the filter 24 and around the sealing bottom wall 25. O between the part
With the ring 32 interposed, the sealing bottom wall 2
When the O-ring 33 is interposed between the O-ring 33 and the washer 30 and the tightening screw 29 is tightened, the supporting cylinder 23, the filter 24 and the sealing bottom wall 25 are joined together, and each joint becomes watertight. retained filter tube,
That is, a filtration tube for collecting a clear sample liquid corresponding to the filtration tube 3 shown in FIG. 1 is formed.

The sealing plug 6 is fitted into the upper opening of the support cylinder 23, and the liquid suction tube 7 is maintained airtight with the sealing plug 6.
and the gas suction tube 8 is inserted into the filtration tube, and the filtration tube is inserted into the liquid tank 1 while maintaining airtightness between the support cylinder 23 and the upper opening of the liquid tank 1. That's right.

In the device of the present invention, a liquid tank 1, a support cylinder 2
3, filter 24, sealing bottom wall 25, sealing plug 6,
Since the liquid suction pipe 7, gas suction pipe 8, etc. are all made of heat-resistant material, these parts are
As shown in Figures 3 to 3, the combined state can be heated and sterilized.

After sterilization, put the fermented liquid 2 into the liquid tank 1, keep the liquid tank 1 at an appropriate temperature to allow fermentation to proceed, and after a predetermined period of time, when controlling and analyzing the fermented liquid, first turn on/off valve 13. When opening the gas suction pump 12
is activated to suck the air inside the filtration cylinder and lower the air pressure inside the filtration cylinder appropriately below the air pressure in the liquid tank 1. Then, the fermented liquid 2 in the liquid tank 1 is filtered by the filter 24 and flows into the filtration cylinder. Inflow.

After the filtrate that has flowed into the filtration cylinder, that is, the clarified sample liquid, reaches an appropriate amount, the gas suction pump 12 is stopped, the on-off valve 13 is closed, and the liquid suction pump 10 is activated, and the liquid suction pipe 7 and the three-way Valve 9
An appropriate amount of the clarified sample liquid in the filtration cylinder is suctioned through the filtration cylinder and introduced into the analyzer 14.

In the analyzer 14, the introduced clarified sample liquid is accurately collected in a required amount and subjected to the required analysis.
Discard the remaining clear sample solution.

Therefore, by appropriately setting the operating time of the liquid suction pump 10 to appropriately adjust the amount of clarified sample liquid sucked from the inside of the filtration cylinder, the analyzer 14 can be
The amount of surplus clarified sample liquid that is discarded can be reduced to an extremely small amount.

In addition, by positioning the inner end of the liquid suction tube 7 as low as possible, for example, at a height of 1 mm to 2 mm from the sealing bottom wall 25 of the filtration tube, it is possible to prevent The time required to introduce the clarified sample liquid into the analyzer 14 can be extremely shortened.

After introducing the clarified sample liquid into the analyzer 14, the liquid suction pump 10 is stopped, the three-way valve 9 is switched, and the gas delivery pump 11 is activated to supply a sterile gas that does not adversely affect the fermentation liquid 2 in the liquid tank 1. ,
For example, if the fermentation liquid 2 is an aerobic fermentation liquid, sterile air is supplied, and if it is an anaerobic fermentation liquid, for example, sterile nitrogen gas (a gas source such as a gas cylinder is not shown) is supplied to the three-way valve 9 and the liquid is sucked. When the gas is pressurized into the filtration cylinder through the pipe 7, the clarified sample liquid remaining in the filtration cylinder flows back into the liquid tank 1 from the filter 24, and the pressurized gas is forced into the liquid tank 1 through the filter 24, and the filter 24 to prevent clogging by peeling off the solid matter adhering to it.

If water vapor is injected into the filtration cylinder instead of sterile air or sterile nitrogen gas, and the filter 24 is backwashed with hot water that liquefies due to the temperature drop in the filtration cylinder, clogging of the filter 24 can be prevented. It can be prevented even more effectively.

Depending on the proportion of solids contained in the fermentation liquor, the viscosity of the fermentation liquor, the time interval of analysis, etc., backwashing of the filter 24 in the filtration tube is performed continuously until the start of the next analysis (in this case, the filter 24 in the filtration tube is After the atmospheric pressure inside the liquid tank 1 is in equilibrium with the atmospheric pressure inside the liquid tank 1, backwashing is performed while maintaining that state.) Alternatively, after backwashing is performed for a certain period of time as appropriate, the gas delivery pump 11 is stopped and the three-way valve 9 and open the on-off valve 13 to prepare for collection of the clarified sample liquid for the next analysis. However, if backwashing is performed continuously until the start of the next analysis, the Depending on the gas delivery pump 11
is stopped, the three-way valve 9 is switched, the on-off valve 13 is opened, the gas suction pump 12 is activated, and the required amount of clarified sample liquid is introduced into the analyzer 14 in the same manner as the previous time.

After backwashing for a certain period of time, when preparing to collect the next clear sample liquid, the gas delivery pump 11 is already stopped, the three-way valve 9 is switched, and the on-off valve 1 is switched off.
3 is open, the gas suction pump 12 is activated in response to the arrival of the next analysis start time.
to be introduced.

As mentioned above, the clear sample liquid obtained by filtering through the filter tube installed in the device of the present invention is transferred to the analyzer 14.
After introduction into the filter, the filter 24 in the filtration tube is backwashed for a certain period of time or until the next analysis, but in general, the control analysis of fermentation liquid is carried out once every 30 to 60 minutes. The time required for each analysis is several minutes), so there is no risk of backwashing the filter 24 interfering with the analysis, and the backwashing time can be long enough to effectively prevent clogging of the filter 24. It can be prevented.

In the device of the present invention, the filter 24 in the filtration tube can be
As mentioned above, clogging can be extremely effectively prevented by sufficiently backwashing the fermented liquid. However, depending on the viscosity of the fermented liquid, the size and content of solids contained in the fermented liquid, There is a possibility that the filter 24 may become clogged during repeated filtration of the fermentation liquid.

If the filter 24 becomes clogged, remove the filter tube from the liquid tank 1, loosen the butterfly screw 29, break the screw connection with the fixing screw 26, and remove the washer 30, sealing bottom wall 25, and filter 24. By removing it, the filter 24 can be replaced with a new one.

The three-way valve 9 and the on-off valve 13 in the device of the present invention are formed, for example, by electromagnetic valves, and the switching and opening/closing of these electromagnetic valves, and the start and stop of operation of the liquid suction pump 10, gas delivery pump 11, and gas suction pump 12, etc. By configuring the system to be controlled by appropriate program signals, a series of operations such as collection of a clarified sample liquid, introduction of the collected sample liquid into the analyzer, and backwashing of the filter 24 can all be performed automatically and constantly. It can be repeated at every time interval.

The above description has been made of the case where a clear sample liquid is collected by filtration from a fermentation liquor, but it goes without saying that the present invention can be used not only when a clear sample liquid is collected by filtration not only from a fermentation liquor but also from a general suspension.

As is clear from the above explanation, in the device of the present invention, after introducing the clarified sample liquid into the analyzer, it is possible to backwash the filter in the filter column in parallel with the progress of the analysis process, and also to suspend the analysis process. Since sufficient backwashing can be performed during the analysis period, filter clogging can be effectively prevented without interfering with analysis processing.
If clogging occurs due to the type of suspension, etc., it is possible to replace only the filter, which reduces maintenance costs compared to replacing the entire filter cylinder. Since the purpose can be achieved only by using a filter cylinder, the overall structure can be made relatively simple, which is extremely effective.

[Brief explanation of drawings]

FIG. 1 is a diagram showing an embodiment of the present invention, and FIGS. 2 and 3 are enlarged cross-sectional views showing an example of the specific structure of the main parts. 1...Liquid tank, 2...Suspension liquid , 3...filtration tube, 4...filter, 5...bottom wall for sealing, 6...
... Sealing plug, 7 ... Liquid suction pipe, 8 ... Gas suction pipe, 9 ... Three-way valve, 10 ... Liquid suction pump, 1
DESCRIPTION OF SYMBOLS 1... Gas delivery pump, 12... Gas suction pump, 13... On-off valve, 14... Analyzer, 23...
... Support cylinder, 24 ... Filter, 25 ... Sealing bottom wall, 26 ... Fixing screw, 27 ... Insertion hole,
28...Support, 29...Tightening screw, 30
...Washer, 31 to 33...O ring.

Claims (1)

[Scope of Claims] 1. A support cylinder having a sealing plug removably attached to the upper opening thereof, and a support cylinder attached to the inside of the support cylinder to form a gap with the inner wall of the support cylinder. a fixing screw whose upper end is fixed to the center of the supporting body, a cylindrical porous body removably attached to the lower end of the support cylinder, a lower end of the cylindrical porous body A sealing bottom wall that is detachably attached and has an insertion hole for the fixing screw in the center thereof, and is screwed into the outer end of the fixing screw led out from the insertion hole bored in the sealing bottom wall. a filtration tube for collecting a clear sample liquid, the tube-shaped porous body portion being immersed in a suspension in a liquid tank, and an upper opening of the filtration tube for collecting a clear sample liquid; A liquid suction tube inserted into the filtration tube for collecting the clarified sample liquid while maintaining an airtight gap between the sealing stopper and the sealing stopper that is detachably attached to the holder, and the liquid suction tube inserted into the filtration tube for collecting the clarified sample liquid while keeping an airtight connection between the sealing stopper and the clear sample liquid. A gas suction pipe inserted into a sampling filtration cylinder; a liquid suction pump and a gas delivery pump that are selectively connected to the liquid suction pipe according to switching of a three-way valve; and an analyzer for sucking liquid from the liquid suction pump. piping for introducing the gas suction side of the gas suction pump into the atmosphere or connecting it to a gas source; a gas suction pump connected to the gas suction pipe; and a gas suction side piping of the gas suction pump. An automatic liquid sampling device characterized by comprising an on-off valve that opens and closes.