JPH0251135B2 - - Google Patents
Info
- Publication number
- JPH0251135B2 JPH0251135B2 JP16734383A JP16734383A JPH0251135B2 JP H0251135 B2 JPH0251135 B2 JP H0251135B2 JP 16734383 A JP16734383 A JP 16734383A JP 16734383 A JP16734383 A JP 16734383A JP H0251135 B2 JPH0251135 B2 JP H0251135B2
- Authority
- JP
- Japan
- Prior art keywords
- pressure
- primary side
- membrane filter
- filter
- predetermined
- Prior art date
- Legal status (The legal status 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 status listed.)
- Expired
Links
- 239000012528 membrane Substances 0.000 claims description 35
- 238000012360 testing method Methods 0.000 claims description 33
- 239000007788 liquid Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 10
- 230000007423 decrease Effects 0.000 claims description 4
- 239000007789 gas Substances 0.000 description 25
- 239000011148 porous material Substances 0.000 description 16
- 238000001514 detection method Methods 0.000 description 5
- 230000005856 abnormality Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000011146 sterile filtration Methods 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 229920002302 Nylon 6,6 Polymers 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011016 integrity testing Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 229940127557 pharmaceutical product Drugs 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/082—Investigating permeability by forcing a fluid through a sample
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Description
【発明の詳細な説明】
この発明は、メンブランフイルタ（膜濾過器）
の試験方法および装置に関する。[Detailed description of the invention] This invention is a membrane filter (membrane filter).
The present invention relates to a test method and apparatus.
メンブランフイルタは、たとえば、注射剤その
他の医薬品を製造するさいの無菌濾過工程などで
使用されるものであり、フイルタの完全性をこれ
を破壊したり汚染したりすることなく容易に再現
性良く試験できる方法として、ASTM、F316−
70で標準化されているバブルポイントテスト（以
下BPTと略す）が広く用いられている。BPT
は、フイルタの濾孔を細管とみなし、後の表面張
力の式(1)で表わされる圧力と濾孔の最大半径との
関係を利用して、圧力を測定することにより濾孔
の最大半径を求める方法であり、従来は第１図に
示すような装置を使用して次のように行なわれて
いる。すなわち、内部に板状メンブランフイルタ
１０が装着されたハウジング１１の一次側に、指
示圧力計１２を接続するとともに、ボール弁１３
を備えたパイプ１４を介して空気、窒素、二酸化
炭素などの気体源１５を接続し、ハウジング１１
の二次側に気泡検出用のパイプ１６を接続して、
このパイプ１６の先端を容器１７に入れた水１８
の中に導いておく。そして、フイルタ１０を蒸留
水または被濾過液などの液体で湿潤させて毛細管
現象により濾孔を液体で満たし、弁１３を適当な
開度に開き、フイルタの一次側を気体によつて
徐々に加圧する。そして、人がハウジングからの
液洩れの目視チエツクを行ないながら、圧力計１
２および気泡検出用のパイプ１６の先端を観察す
る。フイルタ１０の一次側を気体によつて加圧す
ると、圧力が比較的小さい間は、この圧力と濾孔
中の液体が平衡を保ち、液体が濾孔から排除され
ることは無視できるが、圧力が一定の値に達する
と、径の大きい濾孔中の液体が濾孔から二次側に
排除され、気体がこれらの濾孔を通つて二次側に
出てくる。このことは気泡検出用のパイプ１６の
先端から気泡が発生することによつて知ることが
でき、このときの圧力をバブルポイント圧（以下
BP圧と略す）とする。そして、この圧力Ｐと濾
孔の最大半径ｒとの間には、次の表面張力の式(1)
で表わされる関係がある。 Membrane filters are used, for example, in sterile filtration processes in the manufacture of injectables and other pharmaceutical products, and the integrity of the filter can be easily and reproducibly tested without destroying or contaminating it. ASTM, F316−
The bubble point test (hereinafter abbreviated as BPT), which has been standardized in the 70s, is widely used. BPT
regards the pores of the filter as thin tubes, and uses the relationship between the pressure and the maximum radius of the pores expressed by the surface tension equation (1) below to calculate the maximum radius of the pores by measuring the pressure. This method is conventionally carried out as follows using an apparatus as shown in FIG. That is, the indicating pressure gauge 12 is connected to the primary side of the housing 11 in which the plate membrane filter 10 is installed, and the ball valve 13
A gas source 15 such as air, nitrogen, carbon dioxide, etc. is connected via a pipe 14 with a housing 11
A pipe 16 for bubble detection is connected to the secondary side of the
Water 18 containing the tip of this pipe 16 in a container 17
I'll lead you inside. Then, the filter 10 is moistened with a liquid such as distilled water or a liquid to be filtered to fill the filter pores with the liquid by capillary action, the valve 13 is opened to an appropriate opening degree, and the primary side of the filter is gradually heated with gas. Press. Then, while a person visually checks for leakage from the housing,
2 and the tip of the pipe 16 for bubble detection. When the primary side of the filter 10 is pressurized with gas, while the pressure is relatively small, this pressure and the liquid in the filter pores are in equilibrium, and the removal of liquid from the filter pores can be ignored, but the pressure increases. When reaches a certain value, the liquid in the large-diameter pores is expelled from the pores to the secondary side, and gas exits through these pores to the secondary side. This can be known by the generation of bubbles from the tip of the bubble detection pipe 16, and the pressure at this time is called the bubble point pressure (hereinafter referred to as bubble point pressure).
(abbreviated as BP pressure). The following surface tension equation (1) exists between this pressure P and the maximum radius r of the filter pores.
There is a relationship expressed as
ｒ＝ｋ（2σcosθ／Ｐ） ……(1)
ここで、σは表面張力、θは接触角、ｋは形状
補正係数である。したがつて、上記のようにして
BP圧を測定することによりフイルタ１０の濾孔
径を知ることができる。ところが、上記の方法で
は、パイプ１６から気泡が発生するまで人が常に
圧力計１２およびパイプ１６の先端を観察して気
泡が発生したときの圧力を読取る必要があり、作
業が面倒で、かつ自動化が困難である。 r=k(2σcosθ/P)...(1) Here, σ is surface tension, θ is contact angle, and k is shape correction coefficient. Therefore, as above
By measuring the BP pressure, the pore diameter of the filter 10 can be determined. However, in the above method, it is necessary for a person to constantly observe the pressure gauge 12 and the tip of the pipe 16 until bubbles are generated from the pipe 16 and read the pressure when bubbles are generated, which is cumbersome and requires automation. is difficult.
また、メンブランフイルタの完全性を自動的に
試験する装置として、フイルタの一次側にBP圧
の約80％の圧力をかけたときの二次側への気体の
拡散流量を測定するものやフイルタの一次側に断
続的に圧力をかけてこの圧力の変化を測定するこ
とによりBP圧に達したことを知るものが提案さ
れている。ところが、前者の場合は、フイルタの
濾過面積によつて試験値が異なり、小形のフイル
タでは誤差が大きくなるという問題があり、後者
の場合は、ハウジングの容量により測定条件が異
なるという問題がある。また、いずれの場合も、
上記のように微妙な試験条件の設定が必要であ
り、装置が複雑で高価なものになり、メンテナン
スが困難である。また、試験自体は自動的に行な
われるが、完全性の良否は測定結果に基いて人が
判断しなければならない。したがつて、このよう
な従来の装置は、ラインに組込まれたフイルタの
試験装置すなわちインラインでの試験装置として
ラインに組込むことが困難である。 In addition, there are devices that automatically test the integrity of membrane filters, such as those that measure the flow rate of gas diffusion to the secondary side when a pressure of approximately 80% of the BP pressure is applied to the primary side of the filter, and It has been proposed to know when the BP pressure has been reached by applying pressure intermittently to the primary side and measuring changes in this pressure. However, in the former case, there is a problem that the test value varies depending on the filtration area of the filter, and the error becomes large with a small filter, and in the latter case, there is a problem that the measurement conditions differ depending on the capacity of the housing. Also, in any case,
As mentioned above, it is necessary to set delicate test conditions, making the apparatus complicated and expensive, and making maintenance difficult. Furthermore, although the test itself is performed automatically, the integrity must be determined by humans based on the measurement results. Therefore, it is difficult to incorporate such a conventional device into a line as a testing device for a filter installed in the line, that is, as an in-line testing device.
この発明の目的は、上記の問題を解決し、メン
ブランフイルタの完全性を容易にかつ正確に試験
できる方法と、この方法を実施する装置を提供す
ることにある。 SUMMARY OF THE INVENTION An object of the present invention is to solve the above-mentioned problems and to provide a method for easily and accurately testing the integrity of a membrane filter, and an apparatus for implementing this method.
この発明の第１のものは、ハウジング内に固定
されて液体で湿潤されたメンブランフイルタの一
次側を気体によつて所定の割合で昇圧し、所定時
間経過後にメンブランフイルタの一次側の圧力が
所定の判定値に達しているか否かを調べることを
特徴とするメンブランフイルタの試験方法であ
り、この発明の第２のものは、上記方法の発明の
実施に直接使用する装置であつて、この装置は、
ハウジング内に固定されて液体で湿潤されたメン
ブランフイルタの一次側に接続される気体源と、
この気体によるメンブランフイルタの一次側の昇
圧速度を所定の値に保つために気体源とメンブラ
ンフイルタの一次側の間に設けられる昇圧速度設
定弁と、メンブランフイルタの一次側に設けられ
る圧力計とを備えていることを特徴とするもので
ある。 The first aspect of the invention is to increase the pressure of the primary side of a membrane filter fixed in a housing and moistened with liquid with gas at a predetermined rate, and after a predetermined time elapses, the pressure on the primary side of the membrane filter reaches a predetermined level. A second aspect of the present invention is a method for testing a membrane filter, which is characterized by examining whether or not a judgment value has been reached. teeth,
a gas source connected to the primary side of a membrane filter fixed within the housing and wetted with a liquid;
In order to maintain the rate of pressure increase on the primary side of the membrane filter by this gas at a predetermined value, a pressure increase rate setting valve is provided between the gas source and the primary side of the membrane filter, and a pressure gauge is provided on the primary side of the membrane filter. It is characterized by the fact that it is equipped with
発明者らは、メンブランフイルタの完全性試験
について研究を重ねた結果、次のような事実を見
出し、この発明を完成した。すなわち、液体で湿
潤された欠陥のないフイルタの一次側を気体によ
つて所定の割合で昇圧した場合、一次側がBP圧
に到達したのちは、一次側からの気体の供給量と
二次側への気体の排出量が平衡を保ち、一次側の
圧力が一定に維持される。この場合、欠陥のない
フイルタの一次側がBP圧に達するまでの時間は、
このフイルタのBP圧と昇圧速度によつて決まる
ほぼ一定のものであり、したがつて、これより長
い所定時間経過後に一次側の圧力が所定の判定値
に達しているか否かを調べることによつてフイル
タの完全性を容易にかつ正確に試験することがで
きる。そして、従来のBPTの結果との間に測定
値の誤差がなく、フイルタの完全性を定量的に判
断できることが実験により確かめられている。な
お、上記の判定は、所定時間経過後に人が圧力計
を見て行なつてもよい。また、所定時間経過する
まで一次側の圧力を記録計に記録して人がこれを
見て判定するようにしてもよいし、所定時間経過
後に装置で自動的に判定するようにしてもよい。 As a result of repeated research on integrity testing of membrane filters, the inventors discovered the following facts and completed this invention. In other words, when the pressure of the primary side of a defect-free filter moistened with liquid is increased with gas at a predetermined rate, after the primary side reaches the BP pressure, the amount of gas supplied from the primary side and the amount of gas supplied to the secondary side will increase. The amount of gas discharged is balanced, and the pressure on the primary side is maintained constant. In this case, the time it takes for the primary side of a non-defective filter to reach BP pressure is:
This is a nearly constant value determined by the BP pressure and pressure increase rate of this filter. Therefore, by checking whether the primary side pressure has reached a predetermined judgment value after a longer predetermined time has elapsed. The integrity of the filter can then be easily and accurately tested. Experiments have confirmed that there is no error in the measured values compared to conventional BPT results, and that the integrity of the filter can be determined quantitatively. Note that the above determination may be made by a person looking at the pressure gauge after a predetermined period of time has elapsed. Further, the pressure on the primary side may be recorded on a recorder until a predetermined time has elapsed so that a person can make a judgment by looking at this, or the device may automatically make a judgment after a predetermined time has elapsed.
この発明の方法によれば、ハウジング内に固定
されて液体で湿潤されたメンブランフイルタの一
次側を気体によつて所定の割合で昇圧し、所定時
間経過後にメンブランフイルタの一次側の圧力が
所定の判定値に達しているか否かを調べるだけで
よいから、必ずしも昇圧中に一次側の圧力を監視
する必要がなく、メンブランフイルタの完全性試
験を容易にかつ正確に行なうことができる。すな
わち、上記の判定を人が行なう場合でも、従来の
ように常に圧力計および気泡検出用のパイプの先
端を観察している必要がなく、作業が非常に楽に
なる。また、上記の判定を装置で自動的に行なう
場合でも、所定時間経過後の圧力を所定の判定値
と比較するだけでよいから、装置の構成とくに試
験の自動制御や判定を行なう部分の電子回路の構
成が非常に簡単なものになる。さらに、ハウジン
グの一次側に気体源と圧力計を接続するだけでよ
く、従来のように二次側に気泡検出用のパイプを
接続する必要もないから、インラインでの試験が
容易になる。また、この発明による装置は、気体
源と、昇圧速度設定弁と、圧力計とを備えた簡単
なものであり、上記のようにその電子回路も非常
に簡単なものになるから、安価に製作可能であつ
てメンテナンスも容易であり、しかもインライン
での自動試験装置としてラインに組込むことも容
易である。 According to the method of the present invention, the pressure on the primary side of a membrane filter fixed in a housing and moistened with liquid is increased at a predetermined rate with gas, and after a predetermined time elapses, the pressure on the primary side of the membrane filter reaches a predetermined value. Since it is only necessary to check whether the determination value has been reached, it is not necessary to monitor the pressure on the primary side during pressure increase, and the integrity test of the membrane filter can be easily and accurately performed. That is, even when the above-mentioned judgment is made by a person, there is no need to constantly observe the pressure gauge and the end of the pipe for bubble detection as in the past, making the work much easier. In addition, even when the above judgment is performed automatically by a device, it is only necessary to compare the pressure after a predetermined period of time with a predetermined judgment value. The configuration becomes very simple. Furthermore, it is only necessary to connect a gas source and a pressure gauge to the primary side of the housing, and there is no need to connect a pipe for bubble detection to the secondary side as in the conventional case, making in-line testing easier. Furthermore, the device according to the present invention is simple, comprising a gas source, a pressure increase rate setting valve, and a pressure gauge, and as mentioned above, its electronic circuit is also very simple, so it can be manufactured at low cost. It is possible, easy to maintain, and easy to incorporate into a line as an in-line automatic test device.
メンブランフイルタの一次側を昇圧していく場
合、メンブランフイルタの一次側の圧力が上記判
定値より小さい所定の圧力に達したときに所定時
間だけ昇圧を停止し、この間にメンブランフイル
タの一次側の圧力が減少するか否かを調べるのが
望ましい。このようにすれば、ハウジングや配管
のシール不良およびフイルタの湿潤不良などをチ
エツクすることができる。 When increasing the pressure on the primary side of the membrane filter, when the pressure on the primary side of the membrane filter reaches a predetermined pressure that is lower than the above judgment value, the pressure increase is stopped for a predetermined period of time, and during this time the pressure on the primary side of the membrane filter is increased. It is desirable to investigate whether or not this decreases. In this way, it is possible to check for poor sealing of the housing or piping, poor wetting of the filter, etc.
以下第２図〜第５図を参照してこの発明の実施
例を説明する。 Embodiments of the present invention will be described below with reference to FIGS. 2 to 5.
第２図はラインに組込まれていないオフライン
での試験装置を示しており、この装置は、次のよ
うに、内部にカートリツジ状メンブランフイルタ
２０が装着されたハウジング２１の一次側に接続
されている。すなわち、ハウジング２１の一次側
に十字継手２２の一端部が接続され、継手２２の
他の２つの端部に指示圧力計２３と歪ゲージなど
を使用した圧力検出器（圧力計）２４が接続され
ている。継手２２の残りの端部にパイプ２５を介
して気体源２６が接続され、このパイプ２５に
は、気体源２６側から順に、ニードル弁を使用し
た昇圧速度設定弁２７、三方切換電磁弁（三方
弁）２８および二方電磁弁（二方弁）２９が設け
られている。そして、三方弁２８の１つのポート
は大気に開放されている。圧力検出器２４、三方
弁２８および二方弁２９は制御回路３０に接続さ
れ、制御回路３０には自動記録計３１が接続され
ている。 FIG. 2 shows an off-line testing device that is not installed in the line, and this device is connected to the primary side of a housing 21 in which a cartridge-like membrane filter 20 is installed as follows. . That is, one end of a cross joint 22 is connected to the primary side of the housing 21, and an indicating pressure gauge 23 and a pressure sensor (pressure gauge) 24 using a strain gauge or the like are connected to the other two ends of the joint 22. ing. A gas source 26 is connected to the remaining end of the joint 22 via a pipe 25, and a pressure increase speed setting valve 27 using a needle valve and a three-way switching solenoid valve (three-way switching solenoid valve) are connected to the gas source 26 in this order from the gas source 26 side. valve) 28 and a two-way solenoid valve (two-way valve) 29 are provided. One port of the three-way valve 28 is open to the atmosphere. The pressure detector 24, the three-way valve 28, and the two-way valve 29 are connected to a control circuit 30, and an automatic recorder 31 is connected to the control circuit 30.
次に、濾孔径0.2μｍのメンブランフイルタの完
全性試験を行なう場合を例にとつて、上記の試験
装置の動作を説明する。なお、セルロースエステ
ル、ナイロン６−６またはポリビニリデンフルオ
リドなどの親水性のメンブランフイルタの場合、
濾孔径0.2μｍの欠陥のないもののBP圧は約3.5
Kg／cm2である。 Next, the operation of the above-mentioned test apparatus will be explained using as an example a case where a membrane filter with a pore diameter of 0.2 μm is tested for integrity. In addition, in the case of a hydrophilic membrane filter such as cellulose ester, nylon 6-6 or polyvinylidene fluoride,
The BP pressure of a filter without defects with a pore diameter of 0.2 μm is approximately 3.5.
Kg/ cm2 .
試験開始前には、二方弁２９は閉じ、三方弁２
８は設定弁２７側から二方弁２９側に気体が流れ
るように切換えられている。そして、試験に先立
ち、所定の昇圧速度が得られるように、人が設定
弁２７を一定の開度に開いておく。なお、この場
合は、１秒につき0.1Kg／cm2の割合で昇圧する。
また、液体で湿潤させたフイルタ２０をハウジン
グ２１に装着しておく。 Before starting the test, the two-way valve 29 is closed and the three-way valve 2 is closed.
8 is switched so that gas flows from the setting valve 27 side to the two-way valve 29 side. Prior to the test, a person opens the setting valve 27 to a constant opening degree so that a predetermined pressure increase rate can be obtained. In this case, the pressure is increased at a rate of 0.1 Kg/cm 2 per second.
Further, a filter 20 moistened with liquid is attached to the housing 21.
このような状態で始動スイツチを押すことによ
り、次のように自動的に試験が行なわれ、試験途
中に検出器２４により連続的に検出されるハウジ
ング２１の一次側の圧力が第３図〜第５図に示す
ように記録計３１に記録される。なお、第３図〜
第５図において、横軸は時間（sec）を、縦軸は
ハウジング２１の一次側の圧力（Kg／cm2）を表わ
している。 By pressing the start switch in this state, a test is automatically performed as follows, and during the test, the pressure on the primary side of the housing 21, which is continuously detected by the detector 24, is as shown in Figs. The information is recorded on the recorder 31 as shown in FIG. In addition, Figure 3~
In FIG. 5, the horizontal axis represents time (sec), and the vertical axis represents the pressure (Kg/cm 2 ) on the primary side of the housing 21.
始動スイツチを押すと、まず、二方弁２９が開
かれて、気体源２６からハウジング２１の一次側
に気体が供給され、フイルタ２０の破損や装着不
良などがない場合は、一次側の圧力は第３図およ
び第４図に直線ａで示すように上記の割合で上昇
する。そして、一次側の圧力が２Kg／cm2に達した
ならば、二方弁２９が閉じられて、一定時間（t2
＝20sec）昇圧が停止される。ハウジング２１や
配管のシール不良またはフイルタ２０の湿潤不良
などがある場合、昇圧を停止している間に一次側
の圧力が２Kg／cm2から減少するので、警報が発せ
られ、試験が中断される。このような異常がない
場合は、一次側の圧力は第３図および第４図に直
線ｂで示すように一定に維持され、上記時間
（t2）が経過したのち昇圧が再開される。そして、
昇圧再開後一定時間（t3＝60sec）経過したとき
に、一次側の圧力が所定の判定値（３Kg／cm2）よ
り大きいか否かが自動的に調べられる。 When the start switch is pressed, the two-way valve 29 is first opened, and gas is supplied from the gas source 26 to the primary side of the housing 21. If the filter 20 is not damaged or improperly installed, the pressure on the primary side will decrease. As shown by straight line a in FIGS. 3 and 4, it increases at the above rate. Then, when the pressure on the primary side reaches 2 kg/cm 2 , the two-way valve 29 is closed and the pressure is maintained for a certain period of time (t2
= 20sec) Boosting is stopped. If there is a seal failure in the housing 21 or piping, or a wetting failure in the filter 20, the pressure on the primary side will decrease from 2Kg/cm 2 while the pressure increase is stopped, so an alarm will be issued and the test will be interrupted. . If there is no such abnormality, the pressure on the primary side is maintained constant as shown by the straight line b in FIGS. 3 and 4, and after the above-mentioned time (t2) has elapsed, the pressure increase is resumed. and,
When a certain period of time (t3=60 sec) has elapsed after restarting the pressure increase, it is automatically checked whether the pressure on the primary side is greater than a predetermined determination value (3 Kg/cm 2 ).
濾孔径0.2μｍの欠陥のないフイルタの場合、昇
圧再開後の一次側の圧力は、第３図に直線ｃで示
すように上記の割合で上昇し、BP圧（3.5Kg／
cm2）に達したのちは同図に直線ｄで示すように一
定に維持される。そして、昇圧再開後上記時間
（t3）が経過したときの圧力（3.5Kg／cm2）は判定
値（３Kg／cm2）より大いので、正常であると判定
され、正常ランプが点灯したのち、三方弁２８が
切換えられて、ハウジング２１の一次側の空気が
この弁２８から大気に排出され、試験が終了す
る。 In the case of a defect-free filter with a pore diameter of 0.2 μm, the pressure on the primary side after the pressure rise resumes increases at the above rate as shown by the straight line c in Figure 3, and the BP pressure (3.5 kg/
cm 2 ), it remains constant as shown by the straight line d in the figure. Then, the pressure (3.5Kg/cm 2 ) when the above time (t3) has passed after restarting pressurization is greater than the judgment value (3Kg/cm 2 ), so it is judged to be normal, and the normal lamp lights up. , the three-way valve 28 is switched, the air on the primary side of the housing 21 is exhausted to the atmosphere from this valve 28, and the test is completed.
フイルタの濾孔径が0.2μｍより大きい場合たと
えば誤つて濾孔径0.45μｍのフイルタが装着され
た場合は、昇圧再開後の一次側の圧力は、第４図
に直線ｅで示すように上記の割合で上昇し、BP
圧（2.4Kg／cm2）に達したのちは同図に直線ｆで
示すように一定に維持される。そして、昇圧再開
後上記時間（t3）が経過したときの圧力（2.4
Kg／cm2）は判定値（３Kg／cm2）より小さいので、
異常であると判定され、警報が発せられたのち、
異常内容を明確にするためにさらに一定時間（t4
＝40sec）圧力が維持され、上記同様に一次側の
気体が排出されて、試験が終了する。 If the pore diameter of the filter is larger than 0.2 μm, for example, if a filter with a pore diameter of 0.45 μm is installed by mistake, the pressure on the primary side after restarting the pressure increase will be at the above rate as shown by the straight line e in Figure 4. rise, BP
After reaching the pressure (2.4 Kg/cm 2 ), it remains constant as shown by the straight line f in the figure. Then, the pressure (2.4
Kg/cm 2 ) is smaller than the judgment value (3Kg/cm 2 ), so
After it was determined that there was an abnormality and an alarm was issued,
In order to clarify the abnormality contents, a certain period of time (t4
=40sec) The pressure is maintained, the gas on the primary side is exhausted as above, and the test is completed.
フイルタの破損や装着不良があるような場合
は、最初に昇圧を始めたのちの一次側の圧力は、
第５図に曲線ｇで示すように上昇し、昇圧開始後
一定時間（t1＝40sec）経過しても２Kg／cm2に達
しないので、異常であると判定される。そして、
警報が発せられたのち、上記同様に一次側の気体
が排出され、試験が終了する。 If the filter is damaged or improperly installed, the pressure on the primary side after starting pressure increase for the first time should be
The pressure rises as shown by curve g in FIG. 5, and since it does not reach 2 kg/cm 2 even after a certain period of time (t1=40 sec) has passed after the start of pressure increase, it is determined that there is an abnormality. and,
After the alarm is issued, the gas on the primary side is exhausted in the same manner as above, and the test is completed.
上記実施例の装置および方法は、オフラインで
の試験を行なうものであるが、上記のような装置
をラインに組込んでインラインでの試験を行なう
ようにすることももちろん可能である。すなわ
ち、現在各工場で行なわれている無菌濾過システ
ムにおいて、圧力検出器だけを無菌室内のライン
に組込んでおくことにより、インラインでの試験
を無菌状態で自動的に行なうことができる。この
場合、工場全体の試験結果を１箇所で集中的に監
視したり記録したりすることも可能である。ま
た、たとえば、洗瓶機仕上水の最終濾過用フイル
タまたは蒸留水タンクのエアベントフイルタなど
長時間にわたつて何回も使用される複数のフイル
タのハウジングの一次側に圧力検出器を組込んで
装置の他の部分はこれらのフイルタで共用するよ
うにしておけば、ラインを分解することなく、定
期的な試験を短時間で自動的に行なうことができ
る。 Although the apparatus and method of the above embodiments are for performing off-line testing, it is of course possible to incorporate the above-described apparatus into a line to perform in-line testing. That is, in the sterile filtration system currently used in each factory, by incorporating only the pressure detector into the line in the sterile room, in-line tests can be automatically performed under sterile conditions. In this case, it is also possible to centrally monitor and record test results for the entire factory at one location. In addition, pressure detectors can be installed on the primary side of the housings of multiple filters that are used many times over long periods of time, such as final filtration filters for finished water from bottle washers or air vent filters for distilled water tanks. If the other parts of the line are shared by these filters, periodic tests can be automatically performed in a short period of time without disassembling the line.
第１図はバブルポイントテストを行なうための
従来の装置を示す管系統図、第２図〜第５図はこ
の発明の実施例を示し、第２図は試験装置の管系
統図、第３図〜第５図は試験結果の３つの例をそ
れぞれ示すグラフである。
２０……メンブランフイルタ、２１……ハウジ
ング、２３……指示圧力計、２４……圧力検出器
（圧力計）、２６……気体源、２７……昇圧速度設
定弁。
Fig. 1 is a pipe system diagram showing a conventional device for performing a bubble point test, Figs. 2 to 5 show an embodiment of the present invention, Fig. 2 is a pipe system diagram of the test device, and Fig. ~Figure 5 is a graph showing three examples of test results. 20... Membrane filter, 21... Housing, 23... Indicating pressure gauge, 24... Pressure detector (pressure gauge), 26... Gas source, 27... Pressure increase rate setting valve.
Claims (1)
メンブランフイルタの一次側を気体によつて所定
の割合で昇圧し、所定時間経過後にメンブランフ
イルタの一次側の圧力が所定の判定値に達してい
るか否かを調べることを特徴とするメンブランフ
イルタの試験方法。 ２ メンブランフイルタの一次側の圧力が上記判
定値より小さい所定の圧力に達したときに所定時
間だけ昇圧を停止し、この間にメンブランフイル
タの一次側の圧力が減少するか否かを調べること
を特徴とする特許請求の範囲第１項に記載のメン
ブランフイルタの試験方法。 ３ ハウジング内に固定されて液体で湿潤された
メンブランフイルタの一次側に接続される気体源
と、この気体によるメンブランフイルタの一次側
の昇圧速度を所定の値に保つために気体源とメン
ブランフイルタの一次側の間に設けられる昇圧速
度設定弁と、メンブランフイルタの一次側に設け
られる圧力計とを備えていることを特徴とするメ
ンブランフイルタの試験装置。[Claims] 1. Pressurize the primary side of a membrane filter fixed in a housing and moistened with liquid with gas at a predetermined rate, and after a predetermined time elapses, the pressure on the primary side of the membrane filter reaches a predetermined determination. A method for testing a membrane filter, characterized by checking whether a value has been reached. 2. When the pressure on the primary side of the membrane filter reaches a predetermined pressure that is lower than the above-mentioned judgment value, the pressure increase is stopped for a predetermined period of time, and it is checked whether the pressure on the primary side of the membrane filter decreases during this period. A method for testing a membrane filter according to claim 1. 3. A gas source connected to the primary side of the membrane filter fixed in the housing and moistened with liquid, and a gas source connected to the membrane filter in order to maintain the pressure increase rate of the primary side of the membrane filter by this gas at a predetermined value. 1. A membrane filter testing device comprising: a pressure increase rate setting valve provided between the primary side; and a pressure gauge provided on the primary side of the membrane filter.
Priority Applications (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16734383A JPS6058530A (en) | 1983-09-09 | 1983-09-09 | Method and apparatus for testing membrane filter |
| AT84110712T ATE42145T1 (en) | 1983-09-09 | 1984-09-07 | DEVICE FOR TESTING FILTER MEMBRANES, AND DEVICE FOR STERILIZING LIQUIDS BY MEANS OF A FILTER MEMBRANE. |
| EP84110712A EP0139202B1 (en) | 1983-09-09 | 1984-09-07 | Apparatus for testing membrane filters, and apparatus for sterilizing liquids with use of membrane filter |
| DE8484110712T DE3477691D1 (en) | 1983-09-09 | 1984-09-07 | Apparatus for testing membrane filters, and apparatus for sterilizing liquids with use of membrane filter |
| US07/291,395 US4872974A (en) | 1983-09-09 | 1988-12-27 | Apparatus for testing membrane filters, and for sterilizing liquids with use of membrane filter |
| US07/396,912 US5064529A (en) | 1983-09-09 | 1989-08-22 | Apparatus for testing membrane filters |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16734383A JPS6058530A (en) | 1983-09-09 | 1983-09-09 | Method and apparatus for testing membrane filter |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6058530A JPS6058530A (en) | 1985-04-04 |
| JPH0251135B2 true JPH0251135B2 (en) | 1990-11-06 |
Family
ID=15847965
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16734383A Granted JPS6058530A (en) | 1983-09-09 | 1983-09-09 | Method and apparatus for testing membrane filter |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6058530A (en) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63199053U (en) * | 1987-06-13 | 1988-12-21 | ||
| KR100569943B1 (en) * | 1999-01-19 | 2006-04-10 | 현대자동차주식회사 | Air filter test device |
| KR100621610B1 (en) * | 1999-05-10 | 2006-09-06 | 삼성전자주식회사 | Simulation device for filter testing |
| HUP0105236A3 (en) * | 1999-11-18 | 2006-05-29 | Zenon Environmental Inc Oakvil | Immersed membrane filtration system and overflow process |
| KR20010054415A (en) * | 1999-12-06 | 2001-07-02 | 박종섭 | Device tu check the filter codition |
| JP3845067B2 (en) * | 2003-03-24 | 2006-11-15 | 日本碍子株式会社 | Method for measuring pore size of porous filter |
| US7587927B2 (en) * | 2006-11-14 | 2009-09-15 | Millipore Corporation | Rapid integrity testing of porous materials |
| JP2008253888A (en) * | 2007-04-02 | 2008-10-23 | Metawater Co Ltd | Membrane damage detection method |
| JP4895053B2 (en) * | 2008-07-14 | 2012-03-14 | 三菱自動車工業株式会社 | Left / right driving force distribution device |
| JP5519478B2 (en) * | 2010-11-16 | 2014-06-11 | フィルテック株式会社 | Membrane filter integrity test method |
| HRP20200399T1 (en) | 2016-01-22 | 2020-06-12 | Baxter International Inc. | PROCEDURE AND MACHINE FOR THE PRODUCTION OF BAGS FOR STERILE SOLUTIONS |
| PT3405161T (en) | 2016-01-22 | 2020-01-29 | Baxter Healthcare Sa | Sterile solutions product bag |
| CN110430935B (en) * | 2017-03-30 | 2022-04-29 | 日本碍子株式会社 | Inspection method of separation membrane structure, manufacturing method of separation membrane module, and manufacturing method of separation membrane structure |
-
1983
- 1983-09-09 JP JP16734383A patent/JPS6058530A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6058530A (en) | 1985-04-04 |
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