JPH0553223B2 - - Google Patents
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- Publication number
- JPH0553223B2 JPH0553223B2 JP61280497A JP28049786A JPH0553223B2 JP H0553223 B2 JPH0553223 B2 JP H0553223B2 JP 61280497 A JP61280497 A JP 61280497A JP 28049786 A JP28049786 A JP 28049786A JP H0553223 B2 JPH0553223 B2 JP H0553223B2
- Authority
- JP
- Japan
- Prior art keywords
- thin film
- substance
- amount
- evaluating
- photodetector
- 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 - Fee Related
Links
- 239000000126 substance Substances 0.000 claims description 41
- 239000010409 thin film Substances 0.000 claims description 35
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 18
- 239000003094 microcapsule Substances 0.000 claims description 12
- HWYHZTIRURJOHG-UHFFFAOYSA-N luminol Chemical compound O=C1NNC(=O)C2=C1C(N)=CC=C2 HWYHZTIRURJOHG-UHFFFAOYSA-N 0.000 claims description 7
- 238000004020 luminiscence type Methods 0.000 claims description 2
- 230000035515 penetration Effects 0.000 claims 1
- 108010010803 Gelatin Proteins 0.000 description 7
- 229920000159 gelatin Polymers 0.000 description 7
- 239000008273 gelatin Substances 0.000 description 7
- 235000019322 gelatine Nutrition 0.000 description 7
- 235000011852 gelatine desserts Nutrition 0.000 description 7
- 239000011521 glass Substances 0.000 description 7
- 238000001514 detection method Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000012466 permeate Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 102000003992 Peroxidases Human genes 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 108040007629 peroxidase activity proteins Proteins 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 238000011481 absorbance measurement Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、薄膜の物質透過性能を評価する方法
に関する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for evaluating the substance permeation performance of a thin film.
（従来の技術）
薄膜やマイクロカプセルによる物質透過制御
は、化学工業、医薬品工業における基本技術のひ
とつである。(Prior art) Controlling substance permeation using thin films and microcapsules is one of the basic technologies in the chemical and pharmaceutical industries.
目的に合致した最適の薄膜やマイクロカプセル
の設計は、この技術の使用に際して不可欠な過程
である。透過性能の評価には、実際に使用する物
質の透過量を測定する方法と、それと化学的性質
の類似したモデル化合物の透過量を測定する方法
とがある。 Designing optimal thin films and microcapsules for the purpose is an essential step in using this technology. There are two methods for evaluating permeation performance: one method is to measure the amount of permeation of the substance actually used, and the other method is to measure the amount of permeation of a model compound with similar chemical properties.
とくに、微量の透過物について、従来は、定量
が比較的容易なモデル化合物を透過させ、透過後
のモデ化合物の濃度を定量することにより、物質
透過性能を評価する方法が用いられている。 In particular, for trace amounts of permeate, conventional methods have been used to evaluate substance permeation performance by permeating a model compound, which is relatively easy to quantify, and quantifying the concentration of the model compound after permeation.
具体的には、色素をモデル化合物とする吸光度
あるいは蛍光強度の変化の測定、電解質をモデル
化合物とする電気伝導度の変化の測定などであ
る。 Specifically, this includes measuring changes in absorbance or fluorescence intensity using a dye as a model compound, and measuring changes in electrical conductivity using an electrolyte as a model compound.
（発明が解決しようとする問題点）
前述した従来の方法は、いずれも一定時間内の
透過総量を定量するもので、微少時間の膜の透過
性能を評価することはできない。(Problems to be Solved by the Invention) The conventional methods described above all quantify the total amount of permeation within a certain period of time, and cannot evaluate the permeation performance of a membrane over a minute period of time.
また、検出できる最少の物質量は、吸光度測
定、蛍光強度測定、電導度測定でそれぞれ10-11
モル、10-12モル、10-9モル程度であり、極微量
の透過物質（毎秒10-15モル程度）を検出するの
に長時間を要する。 In addition, the minimum amount of substance that can be detected is 10 -11 for absorbance measurement, fluorescence intensity measurement, and conductivity measurement, respectively.
mol, 10 -12 mol, or 10 -9 mol, and it takes a long time to detect an extremely small amount of permeating substance (about 10 -15 mol per second).
本発明の目的は、化学発光法と光電的方法を導
入することにより、高感度かつ迅速に薄膜の物質
透過量を測定し物質透過性能を評価する方法を提
供するところである。 An object of the present invention is to provide a method of highly sensitive and rapid measurement of the amount of substance permeation through a thin film and evaluation of substance permeation performance by introducing a chemiluminescence method and a photoelectric method.
（問題点を解決するための手段）
前記目的を達成するために、本発明による薄膜
の物質透過性能を評価する方法は、相互に混合さ
れると化学発光を生じる第１および第２の物質を
当初被試験用薄膜を介して分離して配置し、前記
いずれか一方の物質が前記薄膜への浸透、透過に
より他方の物質と混合する結果生じる発光を光検
出器により面的に計測することにより薄膜の物質
透過性能を測定するように構成されている。(Means for Solving the Problems) In order to achieve the above object, a method for evaluating the substance permeation performance of a thin film according to the present invention includes first and second substances that produce chemiluminescence when mixed with each other. Initially, they are separated through a thin film to be tested, and one of the substances mixes with the other substance by permeation and transmission through the thin film, and the resulting light emission is measured across the area using a photodetector. The device is configured to measure the substance permeation performance of a thin film.
前記一方の物質は過酸化水素、他方の物質はル
ミノールを含むものとすることができる。 One of the substances may include hydrogen peroxide and the other substance may include luminol.
前記被試験用薄膜をマイクロカプセル外皮とす
ることができる。 The thin film to be tested can be a microcapsule shell.
前記光検出器は光電子増倍管または像増強管と
することができる。 The photodetector may be a photomultiplier tube or an image intensifier tube.
（実施例）
以下、図面等を参照して本発明をさらに詳しく
説明する。(Example) Hereinafter, the present invention will be described in more detail with reference to the drawings and the like.
第１図は、本発明による方法を実施するための
薄膜の物質透過量測定装置の実施例を示す略図で
ある。 FIG. 1 is a schematic diagram showing an embodiment of an apparatus for measuring the amount of substance permeation through a thin film for carrying out the method according to the invention.
暗箱８の内部に設けられた開口を持つ棚９の上
にガラス基板１を配置する。 A glass substrate 1 is placed on a shelf 9 having an opening provided inside a dark box 8.
ガラス基板１の上には、混合されると化学発光
を生じる一方の化学光物質を含むゼラチン薄膜２
が配置されている。 On the glass substrate 1 is a gelatin thin film 2 containing one of the chemiluminescent substances that produces chemiluminescence when mixed.
is located.
ゼラチン薄膜２は、化学発光物質であるルミノ
ールと接触ペルオキシダーゼとルミノールの溶解
度を調整するための有機溶剤ジメチルスルホキシ
ドとを適量含むゼラチン水溶液を約40℃に加温し
てガラス基板１上に展開して形成されたものであ
る。 The gelatin thin film 2 is prepared by heating an aqueous gelatin solution containing an appropriate amount of organic solvent dimethyl sulfoxide for adjusting the solubility of luminol, a chemiluminescent substance, peroxidase, and an organic solvent for adjusting the solubility of luminol, and spreading it on the glass substrate 1. It was formed.
被試験用の高分子薄膜３は前記ゼラチン薄膜２
上に形成される。 The polymer thin film 3 to be tested is the gelatin thin film 2.
formed on top.
この被試験用の高分子薄膜３は一定量のポリス
チレンを一定量のクロロホルムに溶解したものを
ゼラチン薄膜２の上に展開し、クロロホルムを蒸
発させることより形成されたものである。 The polymer thin film 3 to be tested was formed by dissolving a certain amount of polystyrene in a certain amount of chloroform and spreading it on the gelatin thin film 2, and then evaporating the chloroform.
過酸化水素溶液４はトリス（ヒドロキシメチ
ル）アミノメタンと塩酸によつて調整したPH8.5
の水溶液に過酸化水素を溶解させたもので、セル
５に収容されて一定定面積の被試験用薄膜３と接
触している。 Hydrogen peroxide solution 4 had a pH of 8.5 adjusted with tris(hydroxymethyl)aminomethane and hydrochloric acid.
Hydrogen peroxide is dissolved in an aqueous solution of , which is housed in a cell 5 and is in contact with a thin film 3 to be tested having a constant area.
暗箱８の内部に設けられた開口を持つ棚９の下
には検出開口板６が配置されており、検出開口板
６の開口を通過した光は光検出器（光電子増倍
管）７により検出される。 A detection aperture plate 6 is arranged below a shelf 9 with an opening provided inside the dark box 8, and light passing through the aperture of the detection aperture plate 6 is detected by a photodetector (photomultiplier tube) 7. be done.
薄膜３を透過した極微量の過酸化水素は、ゼラ
チン薄膜２内のルミノールと反応して460nm付近
に極大を持つ微弱光を発する。 The extremely small amount of hydrogen peroxide that has passed through the thin film 3 reacts with luminol within the gelatin thin film 2 to emit weak light having a maximum around 460 nm.
光検出器７の出力により、極微量の透過物の量
を推定することができる。 Based on the output of the photodetector 7, it is possible to estimate the amount of the extremely small amount of transmitted matter.
光検出器７として像増倍管や撮像管のような２
次元検出器を用いると、極微量の透過物の量、透
過位置の分布をリアルタイムで測定することがで
きる。 2, such as an image intensifier or an image pickup tube, as the photodetector 7.
Using a dimensional detector, it is possible to measure the amount of extremely small amount of permeate and the distribution of the permeate position in real time.
第２図は、本発明による方法でマイクロカプセ
ルの物質透過量を測定する物質透過量測定装置の
実施例を示す略図である。 FIG. 2 is a schematic diagram showing an embodiment of a substance permeation amount measuring device for measuring the amount of substance permeation through microcapsules using the method according to the present invention.
暗箱１６の内部に設けられた開口を持つ棚１７
にはガラス容器１３が配置されている。 A shelf 17 with an opening provided inside the dark box 16
A glass container 13 is arranged.
ガラス容器１３は、過酸化水素溶液１２が満た
されており底に前記マイクロカプセル１１が多数
個収容されている。 The glass container 13 is filled with a hydrogen peroxide solution 12, and a large number of the microcapsules 11 are housed in the bottom thereof.
ポリスチレン薄膜のマイクロカプセル１１は、
ルミノールとペルオキシダーゼを内包している。 The polystyrene thin film microcapsule 11 is
Contains luminol and peroxidase.
前述した実施例と同様に過酸化水素がマイクロ
カプセル１１の内部へ浸透するに伴い、マイクロ
カプセル１１の内部で、極微量の過酸化水素はル
ミノールと反応して460nm付近に極大を持つ微弱
光を発する。 As in the above embodiment, as hydrogen peroxide permeates into the microcapsules 11, a very small amount of hydrogen peroxide reacts with luminol inside the microcapsules 11, producing weak light with a maximum around 460 nm. emanate.
暗箱１６の内部に設けられた開口を持つ棚１７
の下には検出開口板１４が配置されており、検出
開口板１４の開口を通過した光は光検出器（光電
子増倍管）１５により検出される。 A shelf 17 with an opening provided inside the dark box 16
A detection aperture plate 14 is arranged below the detection aperture plate 14, and light passing through the aperture of the detection aperture plate 14 is detected by a photodetector (photomultiplier tube) 15.
光検出器１５として像増強管や撮像管のような
２次元検出器を用いると、極微量の透過物の量、
透過位置の分布をリアルタイムで測定することが
できる。 If a two-dimensional detector such as an image intensifier tube or an image pickup tube is used as the photodetector 15, the amount of transmitted matter will be extremely small.
The distribution of transmission positions can be measured in real time.
（発明の効果）
以上詳しく説明したように、本発明による薄膜
の物質透過性能を評価する方法は、相互に混合さ
れると化学発光を生じる第１および第２の物質を
当初被試験用薄膜を介して分離して配置し、前記
いずれか一方の物質が前記薄膜への浸透、透過に
より他方の物質と混合する結果生じる微弱発光を
光検出器により面的に計測することにより薄膜の
物質透過性能を評価するように構成されている。(Effects of the Invention) As explained in detail above, the method of evaluating the substance permeation performance of a thin film according to the present invention uses first and second substances that produce chemiluminescence when mixed with each other to form a thin film to be tested. The substance permeation performance of the thin film can be determined by measuring the weak luminescence generated as a result of one of the substances mixing with the other substance by permeation and transmission through the thin film with a photodetector. is configured to evaluate.
本発明方法によれば、薄膜（マイクロカプセル
の外皮等）の物質透過の位置分布のリアルタイム
の計測が可能となつた。 According to the method of the present invention, it has become possible to measure the positional distribution of substance permeation through a thin film (such as the outer skin of a microcapsule) in real time.
また検出器として検出感度が高いものを利用で
きるから、10-18モル程度まで極微量の透過物を
検出することが可能になり、物質透過量の測定感
度を著しく向上させることができた。 Furthermore, since a detector with high detection sensitivity can be used, it has become possible to detect extremely small amounts of permeated matter, down to about 10 -18 moles, and the sensitivity of measuring the amount of permeated substances has been significantly improved.
第１図は、本発明による方法を実施するための
薄膜の物質透過量測定装置の実施例を示す略図で
ある。第２図は、本発明による方法でマイクロカ
プセルの物質透過量を測定する物質透過量測定装
置の実施例を示す略図である。
１……ガラス基板、２……ゼラチン薄膜、３…
…被試験用薄膜、４……過酸化水素溶液、５……
過酸化水素溶液セル、６……開口板、７……光検
出器、８……暗箱、９……暗箱の棚、１１……マ
イクロカプセル、１２……過酸化水素溶液、１３
……過酸化水素溶液を収容するガラス容器、１４
……開口板、１５……光検出器、１６……暗箱、
１７……暗箱の棚。
FIG. 1 is a schematic diagram showing an embodiment of an apparatus for measuring the amount of substance permeation through a thin film for carrying out the method according to the invention. FIG. 2 is a schematic diagram showing an embodiment of a substance permeation amount measuring device for measuring the amount of substance permeation through microcapsules using the method according to the present invention. 1... Glass substrate, 2... Gelatin thin film, 3...
...Thin film to be tested, 4...Hydrogen peroxide solution, 5...
Hydrogen peroxide solution cell, 6...Aperture plate, 7...Photodetector, 8...Dark box, 9...Dark box shelf, 11...Microcapsule, 12...Hydrogen peroxide solution, 13
...Glass container containing hydrogen peroxide solution, 14
...Aperture plate, 15...Photodetector, 16...Dark box,
17...Dark box shelf.
Claims (1)
よび第２の物質を当初被試験用薄膜を介して分離
して配置し、 前記いずれか一方の物質が前記薄膜への浸透、
透過により他方の物質と混合する結果生じる発光
を光検出器により面的に計測することにより薄膜
の物質透過性能を評価する方法。 ２ 前記一方の物質は過酸化水素、他方の物質は
ルミノールを含むものである特許請求の範囲第１
項記載の薄膜の物質透過性能を評価する方法。 ３ 前記被試験用薄膜がマイクロカプセルである
特許請求の範囲第１項記載の薄膜の物質透過性能
を評価する方法。 ４ 前記光検出器が光電子増倍管または像増強管
である特許請求の範囲第１項記載の薄膜の物質透
過性能を評価する方法。[Scope of Claims] 1. A first and a second substance that produce chemiluminescence when mixed with each other are initially separated and arranged via a thin film to be tested, and one of the substances is introduced into the thin film. penetration,
A method of evaluating the substance permeation performance of a thin film by measuring the luminescence generated as a result of mixing with another substance by means of a photodetector. 2. Claim 1, wherein the one substance contains hydrogen peroxide and the other substance contains luminol.
Method for evaluating the substance permeation performance of the thin film described in Section 3. 3. The method for evaluating the substance permeation performance of a thin film according to claim 1, wherein the thin film to be tested is a microcapsule. 4. The method for evaluating the substance permeation performance of a thin film according to claim 1, wherein the photodetector is a photomultiplier tube or an image intensifier tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28049786A JPS63133039A (en) | 1986-11-25 | 1986-11-25 | Evaluation of material permeation performance of thin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28049786A JPS63133039A (en) | 1986-11-25 | 1986-11-25 | Evaluation of material permeation performance of thin film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63133039A JPS63133039A (en) | 1988-06-04 |
| JPH0553223B2 true JPH0553223B2 (en) | 1993-08-09 |
Family
ID=17625910
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP28049786A Granted JPS63133039A (en) | 1986-11-25 | 1986-11-25 | Evaluation of material permeation performance of thin film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63133039A (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8647876B2 (en) | 2010-03-31 | 2014-02-11 | Fujifilm Corporation | Oxygen permeability measuring apparatus and method, and defect inspection apparatus and method |
| JP5307754B2 (en) * | 2010-03-31 | 2013-10-02 | 富士フイルム株式会社 | Defect detection method and apparatus for oxygen barrier body |
| JP6464921B2 (en) * | 2015-05-19 | 2019-02-06 | 日立化成株式会社 | Permeability evaluation method |
| CN106872315A (en) * | 2017-02-22 | 2017-06-20 | 江苏虹创新材料有限公司 | The method of testing of milliosmolarity is returned in a kind of super absorbent resin pressurization |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4916513A (en) * | 1972-04-17 | 1974-02-14 | ||
| JPS553702A (en) * | 1978-05-30 | 1980-01-11 | Kazuo Tsubone | Chemically illuminating float |
| JPS5861446A (en) * | 1981-10-07 | 1983-04-12 | Fuji Photo Film Co Ltd | Quantitative determination method of hydrogen peroxide |
| JPS60149950A (en) * | 1984-01-17 | 1985-08-07 | Hitachi Ltd | Detection of chemiluminescence |
-
1986
- 1986-11-25 JP JP28049786A patent/JPS63133039A/en active Granted
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4916513A (en) * | 1972-04-17 | 1974-02-14 | ||
| JPS553702A (en) * | 1978-05-30 | 1980-01-11 | Kazuo Tsubone | Chemically illuminating float |
| JPS5861446A (en) * | 1981-10-07 | 1983-04-12 | Fuji Photo Film Co Ltd | Quantitative determination method of hydrogen peroxide |
| JPS60149950A (en) * | 1984-01-17 | 1985-08-07 | Hitachi Ltd | Detection of chemiluminescence |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63133039A (en) | 1988-06-04 |
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