JP2000310589A - Gas permeable quantity measuring apparatus for film - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a gas permeable quantity measuring apparatus capable of arbitrarily setting the kind of a film and the conditions (pressure, tempera ture, humidity) of gas to be exposed and capable of measuring the gas perme able quantities of a large number of films in a short time. SOLUTION: A measuring container comprises first and second container forming members 41, 42 enabling the reduction of pressure and the introduction of gas and the container forming members have a structure capable of holding a measuring film in a gastight state as partition walls and an introducing means of specific gas for measuring the gas permeable quantity of the film is provided in the measuring container 4 and, when a plurality of the measuring container 4 are connected to a vacuum container from the first container forming member 41 through valves, as a connection mode, they are radially connected through respective valves centering around the vacuum container.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a gas permeation amount measuring device for measuring a gas permeation amount for a film.
In particular, the present invention relates to an apparatus for measuring the gas permeation amount of a film in which the gas barrier property is important, with high efficiency.

[0002]

2. Description of the Related Art Gas barrier properties of film materials are important technologies in many fields such as food and medicine, packaging of precision electronic components, and sealing technology of electronic components. Accordingly, methods for measuring and evaluating gas barrier properties of a film include, for example, JIS K7126 and ASTM D143.
4. There is a method for measuring gas permeability or oxygen permeability as specified in ASTM D3985. As a specific example of a commercially available apparatus, there is an OX-TRAN series (Nissan Sangyo) of MOCON as an apparatus based on ASTM D3985. Also, JP-A-6-2419
There is also known a measuring device having a higher measuring sensitivity as described in JP-A-78-78.

However, the method proposed in JIS or ASTM is a method capable of detecting only the permeation amount of a specific gas type such as total pressure or oxygen, and therefore cannot perform measurement for an arbitrary gas.

In the method described in Japanese Patent Application Laid-Open No. 6-241978, the above-mentioned problem has been solved. However, the combination of the type of film for which measurement data is required and the conditions of the gas to be exposed (pressure, temperature, humidity) is not sufficient. For a wide variety, 1
One mass spectrometer has one measurement container, and one measurement requires about 8 hours. Therefore, it takes a very long time to collect all the measurement results. The gas barrier properties of films are improving year by year, and the production methods are diversifying. Accordingly, there has been a long-awaited need for a measurement method capable of obtaining the gas permeation amount of a large number of films in a short time in addition to the arbitrary setting of measurement conditions.

[0005]

SUMMARY OF THE INVENTION It is an object of the present invention to set the type of film and the conditions of the gas to be exposed (pressure, temperature, humidity) arbitrarily and to achieve gas permeation of many films in a short time. An object of the present invention is to provide a film gas transmission amount measuring device capable of measuring the amount.

[0006]

Conventionally, one mass spectrometer corresponds to one measuring vessel, and the cost of the mass spectrometer is 400 to 500 times that of the measuring vessel. In addition, in order to check the gas permeability of the film, it takes time, for example, about 8 hours for the gas to permeate the film, whereas the operation of the mass spectrometer for measuring the amount of the permeated gas is required. The time was as short as no more than five minutes.

Therefore, the present inventors have paid attention to the fact that mass spectrometers are actually used only for a short time, and have made it possible to sequentially analyze gas in a large number of measurement vessels using one mass spectrometer. That the gas permeability of a specific film under various measurement conditions and the gas permeability of various films can be measured with high efficiency, despite the fact that only one mass spectrometer exists, and complete the present invention. Reached.

The invention according to claims 1 to 3 of the present invention relates to: (1) connecting a measuring container radially through a valve (A) to a vacuum container connected to a mass spectrometer; (2) Another valve (B) is provided between the measuring container and the valve (A), and the valve (A) and the valve (B) are made detachable. The set consisting of a large number of measurement vessels and valves (B) is sequentially replaced, and the gas amount in each measurement vessel is introduced into the mass spectrometer and measured sequentially. (3) The measurement vessel and valves (1) A) Insert the valve (B) between (A) and (2) as in (1) and (2).
Except that the requirements of (d) to connect a larger number of measuring vessels to one mass spectrometer are different from each other, except that the requirements of (a), (b), and (c) are different. It is an invention in which the two requirements are a common technical idea.

That is, the first aspect of the present invention is that (a) a plurality of measuring vessels for measuring the gas permeation amount of a film are used for one vacuum vessel connected to one mass spectrometer. An apparatus for measuring the amount of gas permeation of a film, wherein (b) the first measuring container is capable of performing both decompression and gas introduction.
A container forming member, and a second container forming member capable of performing both decompression and gas introduction, and the first container forming member and the second container forming member keep the measurement film airtight. (C) the measuring container has a specific gas introducing means for measuring the gas permeation amount of the film inside the measuring container,
(D) When connecting the plurality of measurement containers to the true container via the valve (A) from the first container forming member, the plurality of measurement containers are radially arranged around a vacuum container as a connection mode. The present invention relates to an apparatus for measuring a gas permeation amount of a film, which is connected via a valve (A).

A second aspect of the present invention is (a) a film using a plurality of measurement containers for measuring the gas permeation amount of a film with respect to one vacuum container connected to one mass spectrometer. A gas permeation amount measuring apparatus, wherein (b) the measurement container is a first container forming member capable of both decompression and gas introduction, and a second container formation member capable of both decompression and gas introduction. The first container-forming member and the second container-forming member have a structure capable of being sandwiched as a partition wall for keeping the measurement film airtight. A means for introducing a specific gas for measuring the gas permeation amount of the film therein; and (d) a valve (B) and a valve (C) provided before and after the measurement container to form a measurement container set, A plurality of this measurement container set is When connecting to the vacuum vessel via (A), the structure is made detachable between the valve (A) and the valve (B) so that the measurement vessel set can be exchanged with another measurement vessel set. The present invention relates to a film gas permeation amount measurement apparatus.

A third aspect of the present invention is that (a) a single vacuum container connected to one mass spectrometer uses a plurality of measurement containers for measuring the gas permeation amount of the film. A gas permeation amount measuring apparatus, wherein (b) the measurement container is a first container forming member capable of both decompression and gas introduction, and a second container formation member capable of both decompression and gas introduction. The first container-forming member and the second container-forming member have a structure capable of being sandwiched as a partition wall for keeping the measurement film airtight. A means for introducing a specific gas for measuring the gas permeation amount of the film therein; and (d) a valve (B) and a valve (C) provided before and after the measurement container to form a measurement container set, A plurality of this measurement container set is In connecting to the vacuum vessel via (A), the structure is detachable between the valve (A) and the valve (B), so that the measurement vessel set can be exchanged with another measurement vessel set, Further, the present invention relates to an apparatus for measuring a gas permeation amount of a film, wherein a plurality of measurement container sets are radially connected via a valve (A) around a vacuum container.

The concept of the present invention described in claim 1 can be roughly understood from the perspective view of FIG. 1 and the plan view of FIG. As shown in the figure,
A characteristic feature is that a large number of measurement vessels 4 are radially connected to the vacuum vessel 1 connected to the mass spectrometer 2.

As shown in FIG. 4, the measuring container 4 mainly includes a first container forming member 41 and a second container forming member 42, and the first container forming member 41 and the second container forming member 41. The measurement film 10 is airtightly held between the members 42 using the O-rings 16, 16, 16, 16, and the measurement gas is supplied to the second container forming member 42 under predetermined conditions. Until the measurement gas permeates the measurement film 10 and moves to the space between the first container forming member 41 and the measurement film 10 kept under reduced pressure or vacuum,
For example, keep it for 8 hours. Although this time is long, since a large number of measurement containers 4 are attached radially, in the case of FIG. 3A, eight tests can be performed simultaneously and the measurement efficiency can be improved. .

In the measuring container 4, the measuring film 1
With respect to the measurement container 4 in which the predetermined time for exposing the measurement gas to 0 has expired, the valve (A) 3 is then opened,
The permeated gas is sent to the mass spectrometer 2, and the gas amount is measured to calculate the gas permeation amount.

The general concept of the present invention can be understood from the perspective view of FIG. 2 and the plan view of FIG. In this case, a large number of measurement container sets 7 including the measurement container 4, the valve (B) 43 and the valve (C) 44 shown in the dotted frame of FIG. 11 are prepared, and the measurement is performed via the valve (C) 44. The measurement gas is supplied to the second container forming member 42 side, and is kept in this state for a predetermined time for the measurement gas to pass through the measurement film 10. Next, the valve (B) 43 and the valve (A) 3 are opened, and the permeated gas is sent to the mass spectrometer 2 to measure the gas amount.

Although it takes a long time for the measurement gas to pass through the measurement film in the measurement container set 7, it is necessary to increase the overall processing efficiency by preparing a large number of measurement container sets. Can be.

The measuring container set 7 can be separated from the vacuum container 1 at any time by the connecting member 12 as shown in FIG.
After about 5 minutes have passed, a new measuring vessel set 7 can be connected at any time to effectively use the mass spectrometer. It is a matter of course that the connection member 12 is required to be a device capable of connecting the internal system while completely sealing the outside from the nature of the device.

In the case of the invention of claim 3, for example, the measuring container set 7 shown in FIG. 2 is connected via a connecting member 12 instead of the measuring container 4 of FIG. In the case of FIG. 1, the measurement container 4 is not detachable, but by using the measurement container set 7 instead of the measurement container 4, the mass spectrometer can be reduced to one mass spectrometer as compared with the case of FIG. 1 (the invention of claim 1). On the other hand, a larger number of measurement vessels can be analyzed.

Incidentally, regarding the gas permeation amount, if it is a relative comparison between films, the signal intensity (current value) of the mass spectrometer 2
Is sufficient, but in order to obtain a quantitative value (flow rate) as defined in JIS or ASTM, it is necessary to calibrate with a standard leak whose flow rate is known.

In addition, the signal intensity of the mass spectrometer 2 varies with time due to the consumption of the filament in the ionization part and the deterioration of the detector, and there has been a problem that calibration must be performed as necessary. As shown in FIG.
Is always connected to the vacuum vessel 1, there is no need to break the vacuum for the standard leak installation every time calibration is performed,
Calibration to the flow value is always possible, and even when the number of measurements is large, consistency of the measurement results can be ensured.

Table 1 for a plurality of flow rates and gas types
By attaching various types of standard leaks to the vacuum vessel 1 as shown in (1), expandability of the measurement range and gas types can be improved. As a specific standard leak, for example, according to a commercially available calibration standard leak manufactured by VTI, each product and its flow rate (atm ^- cc / sec) are as shown in Table 1 below.

[0022]

[Table 1] Product name Flow rate welding (cc) CL-5 1.0 × 10 ^{-5 to} 9.9 × 10 ^-5 1000 CL-6 1.0 × 10 ^{-6 to} 9.9 × 10 ^-6 1000 CL −7 1.0 × 10 ^{−7 to} 9.9 × 10 ⁻⁷ 300 CL-8 1.0 × 10 ^{−8 to} 9.9 × 10 ⁻⁸ 215

Thus, the standard leak is a wide range of flow rate
(For example, 10^-2-10^-8 atm⁻cc / sec)
Among them, set the desired flow rate and set it to the standard flow rate.
It is a leak generator for measuring the amount.

The connection mode of the standard leak includes a case connected to a vacuum container via a valve as shown in FIGS. 6 and 12, and a film for measurement set via a valve (D) as shown in FIG. An empty measurement container and a case connected to the vacuum container via the valve (A), as shown in FIG. 13, an empty measurement container set, a case connected to the vacuum container via the connecting member and the valve (A), and the like. is there.

In FIG. 3, reference numeral 1 denotes a vacuum vessel and 2 denotes a mass spectrometer. The plurality of measurement containers 4 each include a first container forming member 41 capable of decompressing and introducing a gas and a second container forming member 42 capable of decompressing and introducing a gas. The container forming member 42 sandwiches the measurement film 10 via an O-ring 16 as an airtight partition. The first container forming member 41 is connected to the vacuum container 1 via a valve (A) 3.
71 and 72 are vacuum pumps, and 73 is a gas supply system. The vacuum vessel 1 is preferably made of stainless steel or an aluminum alloy, but is not necessarily limited to these materials.

The mass spectrometer 2 uses a magnetic field,
Any of those using high frequency and those using a combination of magnetic field and high frequency may be used, but a quadrupole mass spectrometer using high frequency is preferable as the one which is easy to handle, and a quadrupole with a secondary electron multiplier is preferred. A quadrupole mass spectrometer is more preferred. As a specific example of a commercially available quadruple mass spectrometer, there is AQA-200 of Anelva Co., Ltd. In the present invention, by using a mass spectrometer, it is possible to measure a rare gas that cannot be detected by a normal gas sensor.

As the valve (A), any of a manual valve, a valve driven by compressed air, and a valve driven by electromagnetic force can be used. As a specific example, there is an ultra-high vacuum valve (VUH / VULH / VULP series) of Japan Vacuum Engineering Co., Ltd.

The measuring vessel 4 can be used without any particular limitation as long as it is a metal that emits little gas, but stainless steel or an aluminum alloy is desirable. It is preferable that the inner surfaces of these measurement containers 4 are mirror-finished by electrolytic polishing or the like so that the amount of released gas is suppressed. Note that a temperature control mechanism for performing measurement at a temperature other than room temperature may be attached to the measurement container 4.

As the vacuum pump, a high vacuum pump is preferable. As such a high vacuum pump, any of a diffusion pump, a turbo molecular pump, a cryopump, a sputter ion pump, a getter pump and the like can be used. .

When it is desired to control the humidity of the gas, a gas bubbled with water can be appropriately introduced into the gas supply system 73. Further, a temperature control mechanism for performing measurement at a temperature other than room temperature may be attached to the measurement container 4.

As a measuring method using the first aspect of the present invention, as shown in FIG. 3, both the inside of the first container forming member 41 and the inside of the second container forming member 42 are evacuated and decompressed to a vacuum state. Thereafter, the gas to be measured is introduced into the second container forming member 42 side to expose the film, the valve (A) is opened, and only the gas to be measured is measured by the mass spectrometer 2 attached to the vacuum container 1. Can be monitored, and the increase in the signal intensity can be detected as the gas permeation amount.

In the present invention, for example, FIG.
In the apparatus shown in (B), the type of film and the conditions of the gas to be exposed (pressure, temperature, humidity) can be individually set for each of the plurality of measurement containers 4, and moreover, each of the measurement containers 4 Since the condition setting does not affect the gas permeation amount of the other measurement containers 4, a plurality of measurements can be continuously performed by sequentially opening and measuring the valves 3 one by one. Here, the number of measurement containers 4 is not particularly limited, and can be prepared according to the number of measurement conditions.

In the gas permeation amount measurement, a lot of time may be required for an exhausting process for reducing gas emission from a film serving as a background and a wall surface of a measuring container and a storing process of permeated gas in preparation for measurement. However, these steps do not necessarily need to be performed by connecting the exhaust of the measurement container 4 to the vacuum vessel 1, and the exhaust steps of a plurality of measurement vessels are performed at once regardless of the number of exhaust ports of the vacuum vessel 1. Preparation time can be shortened. This is also effective in securing the number of measurements under the same conditions within a limited time to confirm reproducibility.

When the pressure inside the first container forming member 41 is reduced, a pressure difference occurs in the film 10. As the jig 11 that supports the film from the stress caused by the pressure difference and does not hinder the ventilation, a metal plate having a plurality of holes or a porous metal body as shown in FIG. 4 can be used.

When the film has a high gas barrier property and the signal intensity of the mass spectrometer 2 is weak, the inside of the first container forming member 41 is depressurized to reach a sufficient vacuum state, and then the valve (A) 3 Is closed, then the gas to be measured is exposed to the film from the second container forming member 42 side, and the permeated gas is stored in the first container forming member 41 for a certain period of time, and then the valve (A) 3 is opened. By monitoring only the gas to be measured by the mass spectrometer 2, the time integral of the signal intensity can be detected as the gas permeation amount as shown in FIG. In this case, not only the step of exhausting the inside of the measurement container but also the step of storing the permeated gas requires a lot of time. However, since this step can be performed at one time, the time can be greatly reduced while improving the measurement sensitivity.

If the gas barrier property of the film is lower than expected and the amount of accumulated gas is too large, the valve (A) 3 is set to either fully open or fully closed. When the valve 3 is opened, the pressure in the vacuum vessel 1 exceeds the pressure range in which the mass spectrometer 2 can operate, and the measurement must be restarted from the beginning. By using a valve capable of continuously adjusting the opening degree up to the fully opened state, the pressure in the vacuum vessel 1 can be adjusted within the operable range of the mass spectrometer 2 by the opening degree of the valve (A) 3. Measurement can be performed. As a result, a measurement result can be reliably obtained only once for a film whose gas permeation amount is unknown.

As another measurement method, FIG. 1 (FIG. 3)
Using the same device, the gas to be measured is exposed to the film from the side of the second container forming member 42, and the gas other than the target of equal pressure is exposed to the film from the side of the first container forming member 41. After a certain time, the valve (A) 3 is opened,
By monitoring only the gas component to be measured by the mass spectrometer 2, the time integration amount of the signal intensity can be detected as the gas permeation amount. Since no pressure difference is generated in the film by this method, the method is effective for a film having an extremely small strength against stress caused by the pressure difference, for example, an extremely thin film such as a wrap film for food packaging.

As another measuring method using the apparatus according to the second aspect of the present invention, the apparatus shown in FIG. 10 is used, and the gas to be measured (the gas supply system 73 is supplied from the second container forming member 42 side). Is exposed to the film, and from the first container forming member 41 side, a gas other than the target of equal pressure measurement (using a gas source 23 different from the measurement gas) is exposed to the film,
After a certain period of time, the valve 43 is connected to the valve (A) 3, the valve (A) 3 is gradually opened, and only the gas component to be measured is monitored by the mass spectrometer 2. It can be detected as a transmission amount. Even with this method, there is no pressure difference in the film,
This is effective for a film having extremely small strength against stress caused by a pressure difference, for example, an extremely thin film such as a food packaging wrap film.

As for the gas permeation amount, comparison of the signal intensity of the mass spectrometer 2 is sufficient for relative comparison between films. However, in order to obtain a quantitative value as specified in JIS or ASTM. Must be calibrated with a standard leak of known flow. In addition, the signal intensity of the mass spectrometer 2 varies with time due to the consumption of the filament in the ionization part and the deterioration of the detector, and there has been a problem that calibration must be performed as necessary. In such a case, as shown in FIG. 9, since the standard leak 21 is always connected to the vacuum vessel 1, there is no need to break the vacuum for attaching the standard leak every time calibration is performed. Calibration is possible, and even when the number of measurements is large, consistency of the measurement results can be ensured. In addition, by attaching standard leaks for a plurality of flow rates and gas types to the vacuum vessel 1, it is possible to enhance the expandability of the measurement range and gas types. As the standard leak, for example, there is a calibration standard leak manufactured by Vti [Tech Science Corporation].

In the case of connecting a standard leak, FIG.
As shown in FIG. 3, if the standard leak 21 is connected to the vacuum vessel via the empty measuring vessel set, the connecting member and the valve (A), the leak at a very small flow rate, which is difficult to measure directly by the mass spectrometer, can be obtained. By closing the valve (A) 3 and storing the leak gas in the first container forming member 41 for a certain period of time, the valve (A) 3 is opened, and the target leak gas is monitored by the mass spectrometer 2 to obtain a signal. The time integral of the intensity can be calibrated as the standard leak amount.

In order to reduce the noise gas other than the gas permeating the film, as shown in FIGS. 8 and 14, the measuring container 4 is kept in a vacuum state, for example, placed in the vacuum container 8. Is a more preferred embodiment. This can prevent gas entering from the O-ring portion and the valve (B) 43 and the like. In that case, a rotary pump is sufficient as the vacuum pump 74 to be used, but it is of course possible to use a pump capable of obtaining a higher vacuum.

Alternatively, as shown in FIG. 9 or 15, the measuring container 4 is equal to the inside of the second container forming member 42.
Alternatively, a means for holding the gas in a gas other than the object to be measured having a pressure lower than that, for example, by placing it in a gas-replaceable glove box 9, also makes it possible to prevent noise from the O-ring portion of the gas component and the valve (B) 43. Ingress can be prevented.

In the case where it is necessary to measure the amount of air permeated under the condition that the humidity is stable in addition to the temperature, FIG.
As shown in FIG. 6, the measurement container 4 in a state where the valve (C) 44 is opened and the inside of the second container forming member 42 is opened to the outside of the container is controlled in a thermo-hygrostat with the temperature and humidity controlled. 6 can be realized. The number of measurement containers 4 can be used as many as can be put into the thermo-hygrostat 6. As a commercially available thermo-hygrostat, for example, there is a Hi-Flex I series thermo-humidity tester manufactured by Enomoto Kasei Co., Ltd.

A specific method of using FIGS. 1 and 3 (A) and (B) will be described. (1) The valve (A) 3 and the valve (E) 51 are closed, the valves 52, 53 and 54 are opened, and the vacuum pump 72 is driven to exhaust the air in the measuring container 4. (2) The valves 52 and 54 and the valve (A) 3 are closed, the valve (E) 51 and the valve 53 are opened, and the measurement gas is transferred from the measurement gas storage container 22 to the second container forming member 42 side of the measurement container 4. To be introduced. Second container forming member 42
The valve (E) 51 and the valve 53 are closed when the pressure in the space between and the measurement film 10 reaches a predetermined pressure (usually atmospheric pressure). (3) A predetermined time (normally about 8 hours) until the measurement gas permeates the measurement film in this state.
put. (4) Next, the valve (A) 3 is opened, and the gas that has passed through the measurement film 10 and accumulated between the first container forming member 41 and the measurement film 10 is transferred to the mass spectrometer 2 via the vacuum container 1. Perform through analysis.

The measuring method using FIGS. 2 and 11 will be described. (1) First, the measurement container set 7 is set in the piping system shown in FIG. Then, the valve (E) 51 and the valve (A) 3 are closed, and the valve (B) 43 and the valve (C) 4
4. The valves 52, 53 and 54 are opened, and the inside of the measuring container 4 is evacuated by the vacuum pump 72. (2) Valve (B) 43
And the valve 54 are closed, and the valve (E) 51, the valve 53,
The valve (C) 44 is opened, and the measurement gas is introduced from the measurement gas storage container 22 to the second container forming member 42 side of the measurement container 4. When the pressure in the space between the second container forming member 42 and the measurement film 10 reaches a predetermined pressure (normally, atmospheric pressure), the valve (C) 44, the valve (E) 51, and the valve 53 are closed. (3) At this stage, the measurement container set 7
Is separated from the piping system, and if necessary, a new set of measurement containers is incorporated into the piping system, and under the desired conditions (1), (2)
repeat. (4) The measurement container set after the treatments (1) and (2) is left for a time sufficient for the measurement gas to pass through the measurement film. During the standing, the measurement container set 7 can be placed in the vacuum container shown in FIG. 14, in the glove box shown in FIG. 15, or in the thermo-hygrostat 6 shown in FIG. (5) The measurement container set 7 having passed the predetermined time in this way is connected to the valve (A) 3 via the connection member 12. (6) Next, the valve (B) 43 and the valve (A) 3 are opened, the permeated gas is moved to the mass spectrometer 2 in the vacuum vessel 1, and the permeated gas amount is measured.

[0046]

According to the present invention, it is possible to arbitrarily set the type of film and the conditions of the gas to be exposed (pressure, temperature, humidity), and it is possible to measure the gas permeation amount of many films in a short time. .

[Brief description of the drawings]

FIG. 1 is a perspective view showing a specific example of the first embodiment of the present invention.

FIG. 2 is a perspective view showing a concrete example of the invention of claim 2;

FIG. 3A is a plan view schematically showing the relationship between one specific main constituent member of the present invention. (B) is 1
One specific example of what kind of components are arranged around the four measuring devices [in (A), which is indicated by a set of a first container 41 and a second container 42] 4 is shown. FIG.

FIG. 4 is an enlarged view of a specific configuration example of one measurement container 4 in the present invention.

FIG. 5 (A) is a graph in which the vertical axis represents pressure and the horizontal axis represents time,
4 is a graph showing a pressure change of the container of FIG. (B) is a graph showing a pressure change in the first container, with the vertical axis representing pressure and the horizontal axis representing time. (C) is a graph showing changes in signal intensity in the mass spectrometer, with the vertical axis representing current and the horizontal axis representing time.

FIG. 6 is a structural example of an apparatus showing one specific example of the present invention when a standard leak 21 is constantly connected to the vacuum vessel 1;

FIG. 7 shows a specific example of the present invention in the case where the standard leak 21 is connected to the vacuum vessel 1 via the valve 45, the empty measurement vessel 4 in which no measurement film is set, and the valve (A) 3. It is a structural example of an apparatus.

FIG. 8 is a flow sheet showing one specific example of the device of the present invention when the entire measuring device 4 is inserted into the vacuum vessel 8;

FIG. 9 is a flow sheet showing one specific example of the device of the present invention when the entire measuring device 4 is inserted into the glove box 9;

FIG. 10 is a diagram illustrating the operation of separating the measurement container set 7 from the vacuum container 1 connected to the mass spectrometer 2 and allowing the measurement gas to pass through the measurement film 10 in the state of the measurement container set 7 alone. Shows the piping system that can be used.

FIG. 11 is a plan view schematically showing the relationship between one specific main constituent member of the device of the present invention according to claim 2;

FIG. 12 is a configuration example of an apparatus showing one specific example of the present invention when a standard leak 21 is constantly connected to the vacuum vessel 1;

FIG. 13 shows a mode in which the standard leak 21 is always connected to the vacuum vessel via the measuring vessel set including the empty measuring vessel 4, the valve (B) 43, the connecting member 12, and the valve (A) 3.

FIG. 14 is a flow sheet showing another specific example of the apparatus of the present invention when a large number of measurement vessel sets 7 are inserted into the vacuum vessel 8;

FIG. 15 is a flow sheet showing another specific example of the apparatus of the present invention when a number of measurement container sets 7 are inserted into the glove box 9.

FIG. 16 is a flow sheet showing one specific example of the apparatus of the present invention when a large number of measurement container sets 7 are inserted into the thermo-hygrostat 6.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Vacuum container 2 Mass spectrometer 3 Valve (A) 4 Measurement container 6 Constant temperature / humidity device 7 Measurement container set 8 Vacuum container 9 Glove box 10 Measurement film 11 Jig which does not inhibit ventilation 12 Connecting member 16 O-ring 21 Standard leak 22 Storage container for measurement gas 23 Gas source different from measurement gas 41 First container forming member 42 Second container forming member 43 Valve (B) 44 Valve (C) 45 Valve (D) 51 Valve (E) 52 valve 53 valve 54 valve 71 vacuum pump 72 vacuum pump 73 gas supply system 74 vacuum pump

Claims (9)

[Claims] 1. A film gas permeation amount measuring apparatus using a plurality of measurement containers for measuring a film gas permeation amount with respect to one vacuum container connected to one mass spectrometer. (B) the measurement container includes a first container forming member capable of performing both pressure reduction and gas introduction, and a second container forming member capable of performing both pressure reduction and gas introduction; And the first
The member for forming a container and the member for forming a second container have a structure capable of being sandwiched as a partition wall for keeping the film for measurement airtight. (C) The measurement container measures the gas permeation amount of the film therein. (D) connecting the plurality of measurement containers to the vacuum container via the valve (A) from the first container forming member. A plurality of measurement containers are radially connected to each other via respective valves (A). 2. A film gas permeation amount measuring apparatus using a plurality of measurement containers for measuring the gas permeation amount of a film with respect to one vacuum container connected to one mass spectrometer. (B) the measurement container includes a first container forming member capable of performing both pressure reduction and gas introduction, and a second container forming member capable of performing both pressure reduction and gas introduction; And the first
The member for forming a container and the member for forming a second container have a structure capable of being sandwiched as a partition wall for keeping the film for measurement airtight. (C) The measurement container measures the gas permeation amount of the film therein. (D) a valve (B) and a valve (C) are provided before and after the measuring container to form a measuring container set, and a plurality of the measuring container sets are respectively provided. When connecting to the vacuum container via the valve (A), the measurement container set can be exchanged with another measurement container set by making the structure detachable between the valve (A) and the valve (B). An apparatus for measuring a gas permeation amount of a film. 3. A film gas permeation amount measuring apparatus using a plurality of measurement containers for measuring a film gas permeation amount with respect to one vacuum container connected to one mass spectrometer. (B) the measurement container includes a first container forming member capable of performing both pressure reduction and gas introduction, and a second container forming member capable of performing both pressure reduction and gas introduction; And the first
The member for forming a container and the member for forming a second container have a structure capable of being sandwiched as a partition wall for keeping the film for measurement airtight. (C) The measurement container measures the gas permeation amount of the film therein. (D) a valve (B) and a valve (C) are provided before and after the measuring container to form a measuring container set, and a plurality of the measuring container sets are respectively provided. When connecting to the vacuum container via the valve (A), the measurement container set can be exchanged with another measurement container set by making the structure detachable between the valve (A) and the valve (B). A gas permeation amount measuring device for a film, wherein a plurality of measurement container sets are further connected radially around a vacuum container via a valve (A). 4. The valve (A) is capable of continuously adjusting the opening from a fully closed state to a fully opened state.
3. The gas permeation amount measuring device for a film according to any one of 3. 5. The gas permeation measuring device for a film according to claim 1, wherein a standard leak is connected to the vacuum container. 6. The gas permeation amount measuring device for a film according to claim 1, wherein a standard leak is connected to the vacuum container via a measuring container in which the film for measurement is not set. 7. The gas permeation amount measurement for a film according to any one of claims 1 to 6, wherein the measurement container is housed in a container containing a gas other than the gas to be measured having a pressure equal to or lower than its internal pressure. apparatus. 8. The gas permeation measuring device for a film according to claim 1, wherein the measuring container is housed in a container kept in a vacuum state. 9. The film gas permeation amount measuring device according to claim 1, wherein the measuring container is housed in a container whose temperature and humidity are controlled.