JP2010049763A - Method and device for evaluating permeability of organic gas - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method and a device for evaluating permeability of organic gas, capable of accurately evaluating permeability of the organic gas targeting a sealed casing, and improving accuracy of permeability evaluation of the organic gas. <P>SOLUTION: An inert gas is supplied to a heating thermostat 1 having a magnetic disk device 10 disposed therein. The inert gas supplied into the heating thermostat 1 is adsorbed and collected by an adsorption pipe 6 connected to the outside of the heating thermostat 1. When the inert gas supplied into the heating thermostat 1 enters the inside of the magnetic disk device 10, the organic gas component of the inert gas is adsorbed by an adsorbent 11 disposed in the magnetic disk device 10, the concentration of organic gas by the adsorption pipe 6 and the concentration of organic gas by the adsorbent 11 are analyzed, and permeability of the organic gas is evaluated based on the ratio of organic gas of both. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to an organic gas permeability evaluation method and a permeability evaluation apparatus for evaluating the permeability of an organic gas, and more particularly, to provide a sealed casing such as a magnetic disk device by making the evaluation organic gas concentration constant. The present invention relates to an organic gas permeability evaluation method and a permeability evaluation apparatus capable of accurately evaluating the permeability of an organic gas as a target and improving the evaluation accuracy.

  Generally, a magnetic disk device includes a drive unit such as a magnetic head that reads / writes data to / from the magnetic disk, a head suspension that supports the magnetic head, and a spindle motor that rotates the magnetic disk. These components are housed in the housing in a state of being sealed by an exterior cover to prevent the entry of dust and dirt.

  By the way, in the case of a magnetic disk device having such a sealed structure, organic gas may enter from the outside in addition to dust and dirt.

  Here, if a large amount of organic gas such as silicone gas enters the inside of the magnetic disk device, it may cause problems such as head crashes and head flying fluctuations. (1) Analyzing organic gas by using a gas collector or a gas analyzer in advance for the permeability of the organic gas.

  Specifically, a permeability test by a gas differential pressure method (JISK7126) is generally applied. In addition to organic gases, a water vapor permeability evaluation method by a cup method (JISZ0208) or a humidity sensor method (JISK7129) is generally applied (see, for example, Patent Document 1).

  In addition, (2) a method of analyzing generated organic gas using a gas collection device, a gas analysis device, or the like is performed (for example, see Non-Patent Document 1). In the analysis method in this case, two through holes are formed in the cover of the magnetic disk device, and on one side, polymer porous beads (for example, Tenax resin) are fixed as an adsorbent, and from the other side, N2 gas or the like is used. Carrier gas is supplied to collect gas generated from the inside of the magnetic disk device.

  Then, the collected adsorption tube is used as a pretreatment device, and analysis is performed using an analysis device provided with a mass spectrometer (MSD) or the like as a detector in a gas chromatograph (hereinafter abbreviated as GC) provided with a heat desorption device. Yes.

  In addition, (3) an evaluation method has been performed in which gas adsorption on a medium inside a magnetic disk device is analyzed using a gas exposure device, an analysis device, or the like (see, for example, Patent Document 2). Specifically, a method is known in which a medium is put into a heating container, and a gas such as water vapor is conveyed by a carrier gas, and then introduced into a measurement cell to analyze the adsorbed gas.

JP 2003-141872 A JP 2000-20950 A IDEMA STANDARDS Microcontamination Document No. M11-99

  However, the organic gas permeability evaluation method described above has the following problems. That is, in the case of an organic gas permeability evaluation method in which an adsorbent is disposed inside the magnetic disk device to be evaluated, the magnetic disk device is transmitted from the packing, that is, flows from the inside to the outside, or from the outside to the inside. Intrusion is considered.

  For this reason, since all the target samples to be measured are not sampled, there is a problem that accurate evaluation cannot be performed. In addition, since the adsorbent basically causes the adsorption phenomenon by collision (contact with the air flow) of the air current, there is a stagnation in the adsorption by the natural convection phenomenon. As a result, the permeability of organic gas is accurate. There is a problem that cannot be evaluated.

  Further, in the case of such a method, when the concentration inside and outside the magnetic disk device becomes constant (equilibrium state), the evaluation end point can be obtained. However, considering the actual phenomenon, for example, the amount of gas in a general indoor environment or clean room environment is that gas is generated from building materials and the space volume is large, so the gas is adsorbed by the adsorbent. Even if there is an amount that is infinite with respect to the amount, that is, the amount adsorbed by the adsorbent, it is very small and the amount of the surrounding environment (concentration / partial pressure) is considered not to change, so it is different from the actual phenomenon There's a problem.

  Further, since the sealed container in which the magnetic disk device is arranged is a glass container composed of a container and a lid, there is a concern that organic gas may escape (outflow) from the gap between the joints and be adsorbed inside the container. In addition, the inside of the container may not always have a predetermined initial concentration.

  That is, after the organic gas was evaluated, the amount of the permeable gas charged was collected by the adsorbent inside the container, the amount of penetration into the inside of the magnetic disk device, the amount of leakage to the outside of the container, the amount of adsorption inside the container. It should be the sum of the amount, the amount collected in the adsorbent inside the magnetic disk device, and the amount drifting inside the container and inside the magnetic disk device (the amount not collected in the adsorbent) Each of these amounts actually has a problem that there are items that cannot be measured, so that the evaluation of organic gas is not accurate.

  Further, through holes are formed in two places, a supply port and a discharge port, in the cover of the magnetic disk device disclosed in Non-Patent Document 1, an inert gas is flowed from one side, and an adsorption tube is installed on the other side to sample the generated gas In the case of this method, the inert gas may not be discharged from the discharge port due to the inside of the magnetic disk device or the resistance of the adsorption tube, or it may be sucked with a pump from behind the adsorption tube in order to facilitate sampling on the discharge side. .

  At this time, depending on the pressure balance, the inert gas may leak from the packing or the like to the outside of the magnetic disk device, or the ambient environment gas may enter the inside from the outside of the magnetic disk device through the packing or the like. However, there is a problem that the generated gas leaking from the inside of the magnetic disk apparatus cannot be accurately analyzed / evaluated.

  In addition, when polluting gas is forcibly introduced into the inside of the magnetic disk device, etc., the amount of leakage between the two is unknown, so the net amount of gas introduced varies, and experimental conditions that control or take account of it are established. There is a problem that is difficult.

  Furthermore, it is conceivable that the substance for evaluating organic gas such as polluted gas is generated as gas due to contamination inside the magnetic disk device or inside the sealed container. For this reason, it is unclear whether the generated gas or the permeated gas is due to an evaluation gas or a contamination gas, and thus cannot be said to be an accurate organic gas permeation evaluation method.

Therefore, the present invention has been made to solve the above-described problems of the prior art,
Organic gas permeability evaluation method capable of accurately evaluating the permeability of organic gas for sealed enclosures such as magnetic disk devices and improving the evaluation accuracy by making the evaluation organic gas concentration constant. And it aims at providing the permeability evaluation apparatus.

  In order to solve the above-described problems and achieve the object, the present invention supplies an inert gas into a sealed container in which a sealed casing is disposed, and the inert gas supplied into the sealed container is supplied to the outside of the sealed container. When the inert gas that is adsorbed and collected by the adsorption pipe connected to the inside of the sealed container and enters the inside of the sealed casing, the organic gas component of the inert gas is removed from the sealed casing. The organic gas that is adsorbed by the adsorbent adsorbent placed in the adsorbent and collected by the adsorption tube and the concentration of the organic gas adsorbed by the adsorbent are analyzed, and the organic gas permeability is evaluated by the ratio of the two. This is a method for evaluating gas permeability.

  According to the present invention, by making the organic gas concentration for evaluation constant, it is possible to accurately evaluate the permeability of the organic gas for a sealed casing such as a magnetic disk device, and to evaluate the permeability of the organic gas. Accuracy can be improved.

  Embodiments 1 to 5 according to the organic gas permeability evaluation method and permeability evaluation apparatus of the present invention will be described below in detail with reference to the accompanying drawings. In addition, this invention is not limited by Example 1-Example 5 shown below.

[Outline and features of organic gas permeability evaluation method]
First, the outline and characteristics of the organic gas permeability evaluation method according to the first embodiment will be described. FIG. 1 is an explanatory diagram for explaining the outline and characteristics of the organic gas permeability evaluation method according to the first embodiment.

  As shown in the figure, in the first embodiment, in the organic gas permeability evaluation method for the magnetic disk device 10, the heating thermostat 1 in which the magnetic disk device 10 is disposed, and the heating thermostat 1 An inert gas generator P for supplying an inert gas into the interior of the magnetic disk device 10, an adsorbent 11 that is disposed inside the magnetic disk device 10 and adsorbs the inert gas, and discharges the inert gas in the heating thermostat 1. It is carried out using an adsorption tube 6 that adsorbs and collects through the tube 4.

  Here, in the first embodiment, in particular, helium gas (He) or nitrogen gas (in which a gas component to be evaluated from the inert gas generator P is added to the heating thermostat 1 in which the magnetic disk device 10 is disposed is added. While supplying a constant flow rate of N2), the generated gas is collected in the adsorption pipe 6 on the discharge side of the magnetic disk device 10 and the outflow to the heating thermostat 1 (organic gas permeating from the inside of the magnetic disk device 10 to the outside) ) Is collected in the adsorption tube 6 on the discharge side of the heating thermostat 1.

  In other words, the concentration of the organic gas component to be evaluated that has passed through the magnetic disk device 10 is measured by supplying the gas concentration at a constant and constant flow rate inside the heating thermostat 1.

  That is, as shown in the figure, an inert gas is generated at a predetermined position (the left side and the right side in FIG. 1) of the heating thermostat 1 (sealed container) in which the magnetic disk device 10 to be evaluated is disposed. A through hole 2 through which the supply pipe 5 of the inert gas generator P is inserted and a through hole 3 through which the inert gas supplied into the heating thermostat 1 is discharged are formed. Further, a discharge pipe 4 for introducing the inert gas to the adsorption pipe 6 for collecting and adsorbing the inert gas supplied into the heating thermostat 1 is connected to the through hole 3.

  The inert gas generator P is an apparatus that generates an inert gas such as helium gas (He) or nitrogen gas (N 2), for example, and the inert gas generator P is a gas component to be evaluated as an inert gas. Is a device for generating and mixing.

  In addition, the apparatus which supplies an inert gas to the inside of the heating thermostat 1 may be a permeable gas component addition cylinder instead of an inert gas generator. Specifically, a gas cylinder having a known concentration containing a gas component whose permeability is to be evaluated may be used.

  In addition, the adsorption tube 6 that collects the permeable gas is measured with a GC-MS analyzer or the like when the concentration is confirmed even when the permeable gas has an unknown concentration or a known concentration. Here, when a cylinder with a clear traceability of gas concentration is used, the gas concentration collected by the adsorption tube 6 may not necessarily be measured.

  Further, when the inert gas supplied from the inert gas generator P enters the magnetic disk device 10 at a predetermined position inside the magnetic disk device 10, the organic gas component of the inactive gas that has entered the magnetic disk device 10. An adsorbent 11 (or a solid layer adsorbent) that collects and adsorbs is adsorbed.

  As will be described later, the organic gas concentration inside the magnetic disk device 10 is measured by taking out the adsorbent 11 and using a GC-MS analyzer or the like in the same manner. For the adsorbent 11, for example, a porous polymer material such as porous polymer beads can be used.

  The GC-MS analyzer accurately analyzes the mass of a substance by using gas chromatograph mass spectrometry (GC-MS), which is a combination of a gas chromatograph as a separation analyzer and a mass spectrometer as a qualitative analyzer. Device.

[Treatment procedure by organic gas permeability evaluation method]
Next, the processing procedure of the organic gas permeability evaluation method according to the first embodiment will be described with reference to FIG. FIG. 2 is a flowchart showing a processing procedure according to the organic gas permeability evaluation method.

  That is, as shown in the flowchart of FIG. 1, first, an inert gas supply process is performed for supplying an inert gas to the heating thermostat 1 (FIG. 1) in which the magnetic disk device 10 (FIG. 1) is disposed (step). S1). Through this inert gas supply step, a permeable gas having a constant concentration and a constant flow rate can be supplied to the outside of the magnetic disk device 10. Here, the amount of the inert gas supplied is preferably a constant flow rate.

  Next, the inert gas supplied in the heating thermostat 1 by the inert gas supply process in step S1 is adsorbed and collected by the adsorption pipe 6 (FIG. 1) connected to the outside of the heating thermostat 1. A gas collecting step is performed (step S2).

  Next, when the inert gas supplied into the heating thermostat 1 enters the magnetic disk device 10, the organic gas component of the inert gas is absorbed by the adsorbent 11 disposed in the magnetic disk device 10. An adsorbing organic gas component adsorption step is performed (step S3). As described above, the adsorbent 11 can adsorb the organic gas transmitted from the outside existing inside the magnetic disk device 10.

  Next, an organic gas concentration analysis step is performed for analyzing the concentration of the organic gas collected by the adsorption tube 6 and the concentration of the organic gas adsorbed by the adsorbent 11 (step S4). Specifically, qualitative determination is performed by a GC-MS analyzer equipped with a heat desorption device.

  Then, based on the measurement data finally analyzed by the organic gas component analysis step, the organic gas permeability evaluation step of evaluating the permeability by the ratio between the permeability gas concentration for evaluation and the gas concentration inside the magnetic disk device 10 (Step S5).

  Here, in the case of the present Example 1, when performing the organic gas permeability evaluation method, it is supposed to be performed manually based on the flowchart shown in FIG. The organic gas permeability evaluation method may be performed.

  As described above, in the organic gas permeability evaluation method of the first embodiment, the inert gas is supplied to the heating thermostat 1 in which the magnetic disk device 10 is disposed, and the inert gas supplied into the heating thermostat 1 is supplied. The gas is adsorbed and collected by the adsorption tube 6 connected to the outside of the heating thermostat 1, and the inert gas supplied into the heating thermostat 1 enters the inside of the magnetic disk device 10. The organic gas component of the active gas is adsorbed by the adsorbent 11 disposed in the magnetic disk device 10, and the concentration of the organic gas collected by the adsorption tube 6 and the concentration of the organic gas adsorbed by the adsorbent 11 are analyzed. Since the permeability of the organic gas is evaluated based on the ratio between the two, the ambient environment concentration of the magnetic disk device 10 is constant. Therefore, the permeability evaluation gas concentration inside the magnetic disk device 10 at a certain time with respect to the unchanged concentration. It is possible to measure. Therefore, the accuracy is improved with few variations, and the evaluation can be close to an actual phenomenon. As a result, it is possible to accurately evaluate and improve the evaluation accuracy of organic gas permeability for a sealed casing such as a magnetic disk device.

  Further, as described above, in the first embodiment, the amount adsorbed on the inner wall surface of the heating thermostat 1 in which the magnetic disk device 10 is installed by supplying a constant flow rate with a constant evaluation gas concentration. Appears to be “0”, and the surrounding gas concentration is constant. Further, even when organic gas leaks outside the heating thermostat 1, the concentration in the heating thermostat 1 remains unchanged, so that the evaluation data can reduce the variation factor.

[Outline and features of organic gas permeability evaluation method]
Next, the outline and characteristics of the organic gas permeability evaluation method according to the second embodiment will be described. FIG. 3 is an explanatory diagram for explaining the outline and characteristics of the organic gas permeability evaluation method according to the second embodiment. Here, as shown in FIG. 3, in the second embodiment, the analysis method of the generated gas flowing out from the magnetic disk device 10 or the generated gas flowing out from the inside of the magnetic disk device 10 is used as the permeability evaluation method. There are features. In addition, the organic gas generated from the components of the magnetic disk device 10 is evaluated.

  As shown in FIG. 3, in the organic gas permeability evaluation method for the magnetic disk device 10 according to the second embodiment, the heating thermostat 1 in which the magnetic disk device 10 is disposed, and the heating thermostat 1 An inert gas generator P for supplying an inert gas to the inside of the magnetic disk device 10 disposed inside through the supply pipe 5 and an inert gas existing inside the magnetic disk device 10 are collected through the discharge pipe 7. The outline is to perform using the adsorption tube 8 and the adsorbent 20 disposed inside the heating thermostat 1.

  That is, as shown in the figure, an inert gas generator P for generating an inert gas is supplied to predetermined positions (the left side and the right side in FIG. 1) of the heating thermostat 1 in which the magnetic disk device 10 is disposed. A through hole 2 through which the tube 5 is inserted and a through hole 3 through which the inert gas supplied into the heating thermostat 1 is discharged are formed.

  Further, a through hole 14 through which the supply pipe 5 from the inert gas generator P is inserted and a through hole 15 through which the discharge pipe 7 is inserted are formed at the upper position of the magnetic disk device 10. A discharge pipe 7 for introducing an inert gas existing inside the magnetic disk device 10 into the adsorption pipe 8 is connected to the through hole 15. Further, an adsorbent 20 (or a solid layer adsorbent) is disposed inside the heating thermostat 1 and outside the magnetic disk device 10.

  As in the first embodiment, the inert gas generator P is a device that generates an inert gas such as helium gas (He) or nitrogen gas (N2), and the inert gas generator P is an inert gas generator. This is a device for adding and mixing gas components to be evaluated to the active gas.

  Further, the adsorbent 20 disposed inside the heating thermostat 1 has a function of adsorbing and collecting the organic gas that has flowed out (permeated) from the inside of the magnetic disk device 10 to the outside of the heating thermostat 1. Yes. As the adsorbent 20, a porous polymer material such as porous polymer beads can be used as in the first embodiment.

  If the permeability evaluation gas concentration is unknown, a part where the adsorption pipe 8 can be installed may be installed by branching the pipe immediately before being introduced into the magnetic disk device 10. Here, the organic gas collected by the adsorption tube 8 is subjected to qualitative quantitative analysis by a GC-MS analyzer equipped with a heat desorption device.

In the second embodiment, when the organic gas permeability evaluation method is performed, the inert gas generated from the inert gas generator P is supplied into the magnetic disk device 10 through the supply pipe 5.
In this case, the inert gas supplied into the magnetic disk device 10 has a constant concentration (the internal environment concentration is constant).

  Further, the inert gas supplied into the magnetic disk device 10 is adsorbed and collected by the adsorption tube 8 through the discharge pipe 7 connected to the through hole 15 of the magnetic disk device 10.

  Then, the permeable gas from the magnetic disk device 10 is adsorbed and collected by the adsorbent 20, and the amount of the permeable gas is measured. And the permeability | transmittance of organic gas is evaluated based on the ratio of the permeable gas density | concentration of the evaluation objective, and the density | concentration inside the heating thermostat 1. Here, as in the first embodiment, when a gas cylinder with a clear traceability of gas concentration is used, it is not always necessary to measure the gas concentration by the adsorption tube 8.

  Here, in the second embodiment, an example is described in which the permeability evaluation gas is mixed into the inert gas generated from the inert gas generator P. However, when such a permeability evaluation gas is not mixed, It can be used as a method for analyzing generated gas from components arranged inside the magnetic disk device 10 or inside the heating thermostat 1.

  In this case, the amount of gas generated is the total value of the amount measured by the adsorption tube 8 and the amount measured by the adsorbent 20. As a result, it is possible to consider the amount of leakage from the magnetic disk device 10 and to provide a more accurate organic gas permeability evaluation method.

  As described above, in the organic gas permeability evaluation method according to the second embodiment, the inert gas is supplied from the inert gas generator P to the inside of the magnetic disk device 10 arranged in the heating thermostat 1. 5, the inert gas existing inside the magnetic disk device 10 is adsorbed and collected by the adsorption tube 8 through the discharge pipe 7, and is removed from the magnetic disk device 10 by the adsorbent 20 disposed inside the heating thermostat 1. Since the leaked organic gas (permeable gas) is adsorbed and the organic gas concentration is analyzed based on the ratio between the two, the internal environment concentration of the magnetic disk device 10 is constant. It is possible to measure the gas concentration for evaluating permeability to the outside of the magnetic disk device 10 at a certain time. Therefore, the variation factor due to the evaluation can be reduced, the evaluation accuracy can be improved, and an evaluation method close to the actual phenomenon can be realized.

[Outline and features of organic gas permeability evaluation method]
Next, the outline and characteristics of the organic gas permeability evaluation method according to the third embodiment will be described. FIG. 4 is an explanatory diagram for explaining the outline and characteristics of the organic gas permeability evaluation method according to the third embodiment. Here, the third embodiment is an organic gas permeability evaluation method configured to provide an inert gas flow path for supplying an inert gas to the inside of the heating thermostat 1 and the magnetic disk device 10, respectively. There are features.

  As shown in FIG. 4, a through hole 2 is formed at an upper position (upper left side in FIG. 4) of the heating thermostat 1 in which the magnetic disk device 10 is arranged. A supply pipe 5 of an inert gas generator P for generating an inert gas to which a gas component to be evaluated is added to helium gas (He) or nitrogen gas (N2) is inserted into the through hole 2.

  In addition, a through hole 12 through which the supply pipe 13 of the inert gas generator P ′ that similarly generates an inert gas is inserted is formed at a lower position of the heating thermostat 1 (lower left portion in FIG. 4). A through hole 3 is formed at the upper position of the heating thermostat 1 (upper right side in FIG. 4). Connected to the through hole 3 is a discharge pipe 4 for discharging the inert gas supplied into the heating thermostat 1 to the adsorption pipe 6.

  Further, a through hole 14 through which the supply pipe 13 from the inert gas generator P ′ is inserted and a through hole 15 through which the discharge pipe 7 is connected are formed at the upper position of the magnetic disk device 10.

  An inert gas is supplied to the inside of the magnetic disk device 10 through a supply pipe 13 from the inert gas generator P ′, and the inert gas supplied to the inside of the magnetic disk device 10 is discharged. It is adsorbed and collected by the adsorption tube 8 through the tube 7.

  Here, an IA-MS analyzer or the like that can perform real-time measurement according to the concentration of the organic gas to be collected may be connected to the adsorption tube 8. In addition, when the gas concentration targeted for the permeability evaluation is unknown, a part where the adsorption pipe 8 can be installed may be installed by branching the pipe immediately before entering the heating thermostat 1.

  The inert gas generator P ′ is, for example, an inert gas such as helium gas (He) or nitrogen gas (N 2) in the same manner as the inert gas generator P provided above the inert gas generator P ′. This inert gas generator P is a device that generates and mixes gas components to be evaluated as an inert gas.

  In Example 3, when the organic gas permeability evaluation method is performed, the inert gas generated from the inert gas generator P is supplied into the heating thermostat 1 through the supply pipe 5. In this case, the inert gas supplied into the heating thermostat 1 has a constant concentration. Here, the inert gas inside the heating thermostat 1 is collected by the adsorption pipe 6 through the discharge pipe 4.

  Further, the inert gas generated from the inert gas generator P ′ is supplied into the magnetic disk device 10 through the supply pipe 13. Also in this case, the inert gas supplied into the magnetic disk device 10 has a constant concentration. Then, the inert gas supplied to the inside of the magnetic disk device 10 is adsorbed and collected by the adsorption tube 8 through the discharge pipe 7 connected to the through hole 15 of the magnetic disk device 10.

  Then, the concentration of the permeable gas collected by the adsorption tube 6 and the adsorption tube 8 is measured, and the organic gas is determined by the ratio between the concentration of the permeable gas supplied for evaluation and the concentration of the permeable gas discharged from the magnetic disk device 10. Assess the permeability.

  Here, when evaluating the permeability of the organic gas, the timing of collecting the permeated organic gas is, for example, after supplying the evaluation gas around the magnetic disk device 10 for a certain period of time and then inside the magnetic disk device 10. The permeated gas may be collected.

  Further, the concentration of the organic gas adsorbed by the adsorption tube 8 and the concentration of the gas permeated into the magnetic disk device 10 from the amount of inert gas supplied into the magnetic disk device 10 are determined from the concentration of the evaluation gas supplied to the heating thermostat 1. Calculate the permeability ratio. Then, the amount of gas that has permeated in a predetermined time is calculated, and the permeability is analyzed from the calculated amount of gas.

  Here, the amount of permeation with respect to various times can be calculated, and the permeability of the organic gas can be determined based on the inclination and the graph shape. Specifically, when the slope is low, it can be analyzed that the gas permeability is low. Further, when the slope of the graph is high, it can be analyzed that the gas amount is highly permeable.

  As described above, in the organic gas permeability evaluation method according to the third embodiment, the inert gas generated from the inert gas generator P is supplied into the heating thermostat 1 through the supply pipe 5 and heated. The inert gas inside the thermostat 1 is collected by the adsorption pipe 6 through the discharge pipe 4, and the inert gas generated from the inert gas generator P ′ is supplied into the magnetic disk device 10 through the supply pipe 13. Then, the inert gas supplied to the inside of the magnetic disk device 10 is adsorbed and collected by the adsorption tube 8 through the discharge pipe 7 connected to the through hole 15 of the magnetic disk device 10, and the adsorption tube 6 and the adsorption tube 8. The permeability of the organic gas is measured by the ratio of the permeability gas supply side concentration for the purpose of evaluation and the discharge side concentration from the magnetic disk device 10 for the purpose of evaluation. apparatus Since ambient concentrations of 0 becomes constant with respect to the invariant density, it is possible to measure the permeability evaluation gas concentration inside the magnetic disk device 10 at a certain time. Therefore, the accuracy is improved with few variations, and the evaluation can be close to an actual phenomenon.

[Outline and features of organic gas permeability evaluation method]
Next, the outline and characteristics of the organic gas permeability evaluation method according to the fourth embodiment will be described. FIG. 5 is an explanatory diagram for explaining the outline and characteristics of the organic gas permeability evaluation method according to the fourth embodiment. Here, in the fourth embodiment, an organic gas permeability evaluation method for evaluating the permeability of the organic gas by forcibly supplying the contaminated gas into the magnetic disk device is adopted.

  Here, the configuration requirements of the fourth embodiment are substantially the same as the configuration requirements of the third embodiment described above, but as a method of evaluating the durability against the gas targeting the magnetic disk device 10 and each internal component, The outline is that the inert gas is mixed with the pollutant gas that deteriorates the durability from the supply port side of the magnetic disk device 10. In other words, the durability and reliability of the magnetic disk device 10 or parts with respect to the amount of contamination gas mixed is used as the organic gas permeability evaluation method.

  As shown in the figure, helium gas (He), nitrogen gas (N2), etc. are located at the upper position (the upper left portion in FIG. 5) of the heating thermostat 1 in which the magnetic disk device 10 (or parts) is disposed. A through hole 2 is formed through which the supply pipe 5 of the inert gas generator P for generating the inert gas is inserted.

  Further, a supply pipe 13 of an inert gas generator P ′ that generates an inert gas mixed with a pollutant gas (for example, siloxane) is inserted into a lower position of the heating thermostat 1 (lower left portion in FIG. 5). The through-hole 12 to be made is formed. Further, a through hole 3 for discharging the inert gas supplied to the inside of the heating thermostat 1 through the discharge pipe 4 is formed at a lower position of the heating thermostat 1 (upper right side in FIG. 5).

  Further, a through hole 14 through which the supply pipe 13 from the inert gas generator P ′ is inserted and a through hole 15 through which the discharge pipe 7 is inserted are formed at the upper position of the magnetic disk device 10. The discharge pipe 7 collects and adsorbs the inert gas supplied into the magnetic disk device 10 through the through hole 3 formed in the lower position of the heating thermostat 1 (lower right side in FIG. 5). 8 is connected.

  As in the first embodiment, the inert gas generator P is a device that generates an inert gas such as helium gas (He) or nitrogen gas (N2), and the inert gas generator P is an inert gas generator. This is a device that generates and mixes gas components to be evaluated in the active gas.

  The inert gas generator P ′ is, for example, an inert gas such as helium gas (He) or nitrogen gas (N 2) in the same manner as the inert gas generator P provided above the inert gas generator P ′. In the fourth embodiment, in particular, a contaminant gas (for example, siloxane or the like) that deteriorates the durability of the magnetic disk device 10 or parts is mixed in the inert gas.

  In the fourth embodiment, when performing the organic gas permeability evaluation method, the inert gas is supplied into the heating thermostat 1 and the inert gas is supplied into the heating thermostat 1, and the magnetic disk device 10. An inert gas mixed with a pollutant gas is supplied to the inside of the disk, and the amount of the gas adsorbed and collected by the adsorption pipe 8 through the discharge pipe 4 of the heating thermostat 1 is the net pollution quantity. calculate.

  As described above, in the organic gas permeability evaluation method of the fourth embodiment, the inert gas is supplied into the heating thermostat 1 and the inert gas is supplied into the heating thermostat 1 so as to be magnetic. Since the inert gas mixed with the contaminated gas is supplied to the inside of the disk device 10, the amount of the contaminated gas leaked from the magnetic disk device 10 is accurately detected by the adsorption pipe 6 connected to the discharge pipe 4 of the heating thermostat 1. Since it can be calculated, it is possible to improve the accuracy of the effect evaluation of the durability (reliability) by the organic gas and the amount of pollutant gas for the magnetic disk device 10, and the magnetic disk device 10 with respect to the amount of contaminated gas mixed or The durability and reliability of parts can be efficiently evaluated.

[Outline and features of organic gas permeability evaluation method]
Next, the outline and characteristics of the organic gas permeability evaluation method according to the fifth embodiment will be described. FIG. 6 is an explanatory diagram for explaining the outline and characteristics of the organic gas permeability evaluation method according to the fifth embodiment. Here, the fifth embodiment is characterized by an organic gas permeability evaluation method capable of performing generated gas analysis that can correct leakage and mixing of organic gas.

  Here, the configuration for performing the organic gas permeability evaluation method in the fifth embodiment is substantially the same as that in the third and fourth embodiments, but in this fifth embodiment, the inert gas generators P and P are used. The substances D1 and D2 (for example, compounds such as toluene-d8, acetone-d6 and methanol-d3) having deuterium which is an isotope element of hydrogen (H) which is not found in nature in the inert gas supplied from Each high-purity gas is mixed with different concentrations (substances D1 and D2 having deuterium) at a constant concentration. And it is set as the structure which grasps | ascertains the leak and mixing amount of organic gas by measuring them with a GC-MS apparatus, for example.

  That is, since the deuterium-containing substances D1 and D2 are substances that do not exist in nature, there is no generation from the inside of the magnetic disk device 10 and no generation from the heating thermostat 1.

  This makes it possible to calculate from which side the gas has leaked from the amount of gas collected in both adsorption pipes 6 and 8, and the amount of leakage and contamination. It becomes possible to calculate the gas concentration with high accuracy.

  More specifically, the inert gas supplied to the heating thermostat 1 and the magnetic disk device 10 is mixed with trace amounts of components (substances D1 and D2 having deuterium) serving as markers of permeation amount and leakage amount. Yes.

  Here, since the component which becomes a marker of permeation amount / leakage amount is not preferable when it is present in the generated gas, deuterium (D) which is an isotope element of hydrogen (H) which does not exist in nature in the inert gas. A substance having a certain concentration, for example, a compound such as toluene-d8, acetone-d6, or methanol-d3, is mixed with different substances (D1, D2) in a high concentration. Then, by measuring this gas concentration with, for example, a GC-MS apparatus, it becomes possible to analyze which amount of leakage has entered on which side.

  As described above, when the organic gas permeability evaluation method is performed in the fifth embodiment, a marker capable of grasping the leakage and mixing amount of organic gas, for example, toluene-d8 (molecular weight 100) as an inert gas as an inert gas. Even when toluene (molecular weight 92) is generated from the magnetic disk device 10 by mixing into the magnetic disk device 10, an evaluation method for distinguishing between toluene having a molecular weight of 100 and toluene having a molecular weight of 92 by using a mass spectrometer for the measurement To do. That is, this allows the net transmission amount (gas generation amount) from the magnetic disk device 10 to be grasped.

  As described above, in the organic gas permeability evaluation method of the fifth embodiment, it is possible to grasp the net gas introduction amount (injection amount), so that an improvement effect of evaluation accuracy can be obtained. Further, by adopting the same method for the polluted gas, it becomes possible to perform the separation, and the effect of improving the evaluation accuracy can be obtained. That is, it is possible to minimize the influence of gas flow in and out of the magnetic disk device 10 which has been a problem as a factor of decreasing accuracy in the evaluation of the magnetic disk device 10 so far, and it is possible to realize a highly accurate evaluation method.

(Other examples)
The first to fifth embodiments of the present invention have been described so far, but the present invention is not limited to the above-described embodiments, and various other embodiments can be used within the scope of the technical idea described in the claims. Can also be implemented.

  That is, the gas introduction method in the organic gas permeability evaluation method described in Example 5 described above accurately grasps the gas supply amount / introduction amount (injection amount) also in Examples 1 to 4 described above. be able to.

  More specifically, for example, by using the deuterium-containing substance D1 as the pollutant gas itself of the fourth embodiment, it is possible to determine whether the substance is an intended substance or a substance due to contamination.

  Examples of the contaminating compounds shown in Example 5 include (1) aromatic compounds such as toluene-d8 and (2) alcohol compounds having an —OH group as methanol-d4, ethanol-d6, Isopropyl alcohol-d8 and the like are (3) diethyl phthalate-3, 4, 5, 6-d4, dibutyl phthalate-3, 4, 5, 6-d4, dibutyl phthalate-3, 4, 5 as phthalic acid ester compounds. , 6-d22, di-2 ethyl phthalate-3, 4, 5, 6-d4, etc., (4) As adipic acid ester compounds, di-2-ethylhexyl adipate-d8 and the like that are actually sold are adopted. be able to.

  (5) As the silicon compound, hexamethyl-d18-disiloxane, tedramethylsilane-d12, tetraethoxy-d20-silane, etc., (6) As the hydrocarbon compound, hexane-d143, heptane-d14, etc. (7) As the nitrogen-containing compound, dichloromethane-d2, chloroform-d1, etc. can be used, and (8) as the oxygen-containing compound, those actually sold such as acetone-d6 can be adopted.

  Also, (9) sulfur-containing compounds such as dimethyl sulfoxide-d6, (10) nitrogen-containing compounds such as N, N′-dimethylacetamide-d9, and (11) phosphorus-containing compounds such as trimethyl phosphate -d9, tributyl phosphate-d27, etc. (12) As tin-containing compounds, those actually sold such as trifel tin chloride-d15, tributyltin chloride-d27, tetraphenyltin-d36 can be adopted. .

  As described above, in the organic gas permeability evaluation method of the fifth embodiment, from which side the gas is leaked from the amount of gas collected in both adsorption tubes 6 and 8, and Since the leakage and mixing amount can be calculated, the amount of gas introduced and the concentration of gas can be accurately calculated.

  The following supplementary notes are further disclosed with respect to the embodiments including the above examples.

(Appendix 1) An organic gas permeability evaluation method for evaluating the permeability of an organic gas for a sealed casing,
A constant concentration gas supply step of continuously supplying an inert gas, to which an evaluation substance is added, into a sealed container in which the sealed casing is disposed;
An organic gas permeability evaluation method comprising: a gas concentration component measuring step of measuring a gas concentration supplied into the sealed container by the constant concentration gas supplying step.

(Appendix 2) An organic gas permeability evaluation method for evaluating the permeability of an organic gas for a sealed casing,
An inert gas supply step of supplying an inert gas to which an evaluation substance is added in a sealed container in which the sealed casing is disposed;
An inert gas collecting step of adsorbing and collecting the inert gas supplied by the inert gas supply step by an adsorption tube connected to the outside of the sealed container;
An adsorbent that adsorbs and collects organic gas components is disposed in the sealed casing, and the inert gas supplied into the sealed container by the inert gas supply step is placed inside the sealed casing. An organic gas component adsorption step of adsorbing the organic gas component of the inert gas by the adsorbent when invading,
An organic gas concentration analyzing step for analyzing the concentration of the organic gas collected by the inert gas collecting step and the concentration of the organic gas adsorbed by the adsorbent;
An organic gas permeability evaluation method comprising: an organic gas permeability evaluation step of evaluating organic gas permeability based on a ratio of the amount of organic gas components analyzed in the organic gas concentration analysis step.

(Appendix 3) An organic gas permeability evaluation method for evaluating the permeability of an organic gas for a sealed casing,
An inert gas supply step of supplying an inert gas to which an evaluation substance is added in a sealed container having the sealed casing disposed therein;
An inert gas collecting step of adsorbing and collecting the inert gas supplied by the inert gas supply step by an adsorption tube connected to the outside of the sealed container;
An adsorbent that collects and adsorbs the organic gas component in the sealed container is disposed outside the sealed casing, and the inert gas supplied to the sealed casing is An organic gas component adsorption step of adsorbing the organic gas component of the inert gas by the adsorbent when leaking from the outside of the housing;
An organic gas concentration analyzing step for analyzing the concentration of the organic gas collected by the inert gas collecting step and the concentration of the organic gas adsorbed by the adsorbent;
An organic gas permeability evaluation method comprising: an organic gas permeability evaluation step of evaluating organic gas permeability based on a ratio with the amount of organic gas components analyzed in the organic gas concentration analysis step.

(Additional remark 4) It is the components which comprise the said sealed housing | casing in the inside of the said sealed housing | casing, and the said organic gas permeability evaluation process is permeability | transmittance evaluation of the organic gas for the said components The organic gas permeability evaluation method according to supplementary note 3, characterized by:

(Additional remark 5) It is the permeability evaluation method of the organic gas which evaluates the permeability | transmittance of the organic gas which targets a sealed housing | casing,
A first inert gas supply step of supplying an inert gas added with an evaluation substance in a sealed container having the sealed casing disposed therein;
A second inert gas supply step for supplying an inert gas into the sealed casing;
A first inert gas collection step for adsorbing and collecting the inert gas supplied by the first inert gas supply step by an adsorption tube connected to the outside of the sealed container;
A second inert gas collecting step for adsorbing and collecting the inert gas supplied by the second inert gas supply step by an adsorption tube connected to the outside of the sealed container;
An organic gas concentration analyzing step for analyzing the concentration of the organic gas collected by the first inert gas collecting step and the concentration of the organic gas collected by the second inert gas collecting step;
An organic gas permeability evaluation step for evaluating the permeability of the organic gas by a ratio with the amount of the organic gas component analyzed by the organic gas concentration analysis step;
An organic gas permeability evaluation method comprising:

(Additional remark 6) The additional remark which further includes the permeation amount acquisition process which acquires permeation amount per unit time of the inactive gas which penetrated the inside of the above-mentioned closed type case as real time or permeation amount for every fixed time 5. The organic gas permeability evaluation method according to 5.

(Supplementary note 7) Any one of Supplementary notes 1 to 6, wherein the organic gas permeability determination step evaluates a substance having deuterium which is an isotope element of hydrogen that does not exist in nature in the evaluation substance. The organic gas permeability evaluation method according to claim 1.

(Appendix 8) The substance having deuterium includes toluene-d8, acetone-d6, methanol-d3, ethanol-d5, isopropyl alcohol-d8, diethyl phthalate-d4, di-2-ethylhexyl adipate-d8, di-2. The organic gas permeability evaluation method according to appendix 7, which is a compound of any one of -ethylhexyl phthalate-d4.

(Supplementary Note 9) The quantitative analysis / qualitative analysis of the gas concentration collected in the adsorbent or the adsorption tube uses any one of the apparatuses having a mass spectrometer as a detector. The organic gas permeability evaluation method according to any one of appendices 2 to 8.

(Appendix 10) An organic gas permeability evaluation apparatus for evaluating the permeability of an organic gas intended for a sealed casing,
A constant concentration gas supply means for continuously supplying an inert gas, to which an evaluation substance is added, in a sealed container in which the sealed casing is disposed;
An organic gas permeability evaluation apparatus, comprising: a gas concentration component measurement unit that measures a gas concentration supplied into the sealed container by the constant concentration gas supply unit.

  The present invention is useful when performing an organic gas permeability evaluation method, and relates to an organic gas permeability evaluation method for evaluating the permeability of an organic gas that penetrates into a sealed casing, and more particularly to the organic gas permeability. It is effective as a permeability evaluation method and a permeability evaluation apparatus that can improve the accuracy of organic gas permeability evaluation.

FIG. 4 is a diagram for explaining a method for evaluating permeability of organic gas according to Example 1. It is a flowchart explaining the procedure of the permeability evaluation method of organic gas. It is a figure explaining the permeability evaluation method of organic gas concerning Example 2. It is a figure explaining the permeability evaluation method of organic gas concerning Example 3. It is a figure explaining the permeability evaluation method of organic gas concerning Example 4. It is a figure explaining the permeability evaluation method of organic gas concerning Example 5.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Heating thermostat 2, 3, 12, 14, 15 Through-hole 4,7 Ejection pipe 5,13 Supply pipe 10 Magnetic disk apparatus 11,20 Adsorbent P, P 'Inert gas generator

Claims (9)

An organic gas permeability evaluation method for evaluating the permeability of an organic gas for a sealed casing,
A constant concentration gas supply step of continuously supplying an inert gas, to which an evaluation substance is added, into a sealed container in which the sealed casing is disposed;
An organic gas permeability evaluation method comprising: a gas concentration component measuring step of measuring a gas concentration supplied into the sealed container by the constant concentration gas supplying step. An organic gas permeability evaluation method for evaluating the permeability of an organic gas for a sealed casing,
An inert gas supply step of supplying an inert gas to which an evaluation substance is added in a sealed container in which the sealed casing is disposed;
An inert gas collecting step of adsorbing and collecting the inert gas supplied by the inert gas supply step by an adsorption tube connected to the outside of the sealed container;
An adsorbent that adsorbs and collects organic gas components is disposed in the sealed casing, and the inert gas supplied into the sealed container by the inert gas supply step is placed inside the sealed casing. An organic gas component adsorption step of adsorbing the organic gas component of the inert gas by the adsorbent when invading,
An organic gas concentration analyzing step for analyzing the concentration of the organic gas collected by the inert gas collecting step and the concentration of the organic gas adsorbed by the adsorbent;
An organic gas permeability evaluation method comprising: an organic gas permeability evaluation step of evaluating organic gas permeability based on a ratio of the amount of organic gas components analyzed in the organic gas concentration analysis step. An organic gas permeability evaluation method for evaluating the permeability of an organic gas for a sealed casing,
An inert gas supply step of supplying an inert gas to which an evaluation substance is added in a sealed container having the sealed casing disposed therein;
An inert gas collecting step of adsorbing and collecting the inert gas supplied by the inert gas supply step by an adsorption tube connected to the outside of the sealed container;
An adsorbent that collects and adsorbs the organic gas component in the sealed container is disposed outside the sealed casing, and the inert gas supplied to the sealed casing is An organic gas component adsorption step of adsorbing the organic gas component of the inert gas by the adsorbent when leaking from the outside of the housing;
An organic gas concentration analyzing step for analyzing the concentration of the organic gas collected by the inert gas collecting step and the concentration of the organic gas adsorbed by the adsorbent;
An organic gas permeability evaluation method comprising: an organic gas permeability evaluation step of evaluating organic gas permeability based on a ratio with the amount of organic gas components analyzed in the organic gas concentration analysis step. An organic gas permeability evaluation method for evaluating the permeability of an organic gas for a sealed casing,
A first inert gas supply step of supplying an inert gas added with an evaluation substance in a sealed container having the sealed casing disposed therein;
A second inert gas supply step for supplying an inert gas into the sealed casing;
A first inert gas collection step for adsorbing and collecting the inert gas supplied by the first inert gas supply step by an adsorption tube connected to the outside of the sealed container;
A second inert gas collecting step for adsorbing and collecting the inert gas supplied by the second inert gas supply step by an adsorption tube connected to the outside of the sealed container;
An organic gas concentration analyzing step for analyzing the concentration of the organic gas collected by the first inert gas collecting step and the concentration of the organic gas collected by the second inert gas collecting step;
An organic gas permeability evaluation method comprising: an organic gas permeability evaluation step of evaluating organic gas permeability based on a ratio with the amount of organic gas components analyzed in the organic gas concentration analysis step.   The permeation amount acquisition step of acquiring the permeation amount per unit time of the inert gas that has entered the inside of the hermetic casing as real time or permeation amount per fixed time is further included. Evaluation method of organic gas permeability.   The organic gas permeability evaluation step is performed by evaluating a substance having deuterium, which is an isotope element of hydrogen that does not exist in nature, in the evaluation substance. The organic gas permeability evaluation method described in 1.   The deuterium-containing substance is toluene-d8, acetone-d6, methanol-d3, ethanol-d5, isopropyl alcohol-d8, diethyl phthalate-d4, di-2-ethylhexyl adipate-d8, di-2-ethylhexyl phthalate- The organic gas permeability evaluation method according to claim 6, wherein the compound is any compound of d4.   The quantitative analysis / qualitative analysis of the gas concentration collected in the adsorbent or the adsorption tube uses any one of devices in general having a mass spectrometer as a detector. 8. The organic gas permeability evaluation method according to any one of 7 above. An organic gas permeability evaluation apparatus for evaluating the permeability of an organic gas for a sealed casing,
A constant concentration gas supply means for continuously supplying an inert gas, to which an evaluation substance is added, in a sealed container in which the sealed casing is disposed;
An organic gas permeability evaluation apparatus, comprising: a gas concentration component measurement unit that measures a gas concentration supplied into the sealed container by the constant concentration gas supply unit.

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