JPH043062B2 - - Google Patents
Info
- Publication number
- JPH043062B2 JPH043062B2 JP61209560A JP20956086A JPH043062B2 JP H043062 B2 JPH043062 B2 JP H043062B2 JP 61209560 A JP61209560 A JP 61209560A JP 20956086 A JP20956086 A JP 20956086A JP H043062 B2 JPH043062 B2 JP H043062B2
- Authority
- JP
- Japan
- Prior art keywords
- orifice plate
- envelope
- gas
- sample chamber
- resistance evaluation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 238000004458 analytical method Methods 0.000 claims description 33
- 238000012360 testing method Methods 0.000 claims description 28
- 238000011156 evaluation Methods 0.000 claims description 22
- 230000007613 environmental effect Effects 0.000 claims description 15
- 238000004868 gas analysis Methods 0.000 claims description 10
- 239000007789 gas Substances 0.000 description 26
- 238000004949 mass spectrometry Methods 0.000 description 11
- 230000033001 locomotion Effects 0.000 description 10
- 230000005540 biological transmission Effects 0.000 description 7
- 239000003463 adsorbent Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 230000000274 adsorptive effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Electron Tubes For Measurement (AREA)
Description
【発明の詳細な説明】
〔産業上の利用分野〕
この発明は各種材料の耐環境性評価試験におい
て、耐環境性評価試験装置の試料室内の材料から
放出されるガスおよび試料室内の雰囲気ガスの分
析を行うためのガス分析システムに関するもので
ある。[Detailed Description of the Invention] [Industrial Application Field] This invention is used in environmental resistance evaluation tests of various materials to evaluate the gas emitted from the material in the sample chamber of an environmental resistance evaluation test device and the atmospheric gas in the sample chamber. The present invention relates to a gas analysis system for performing analysis.
第３図は従来の耐環境性評価試験装置の試料室
に備えられたガス分析システムの断面図である。
図において、１は試料、２は試料１を収容する耐
環境性評価試験装置の試料室、３は試料室２の中
にガス成分の質量分析を行うための四重極質量分
析計の分析管、４は分析管３を収納するエンベロ
ープ、５はエンベロープ４の中を高真空に保持す
るための真空排気装置、６はエンベロープ４と真
空排気装置５の間を開閉するための高真空バル
ブ、７は試料室２からエンベロープ４の中へ流入
するガスの量を制限するためのオリフイス板であ
る。
FIG. 3 is a sectional view of a gas analysis system installed in a sample chamber of a conventional environment resistance evaluation test device.
In the figure, 1 is a sample, 2 is a sample chamber of the environmental resistance evaluation test device that accommodates sample 1, and 3 is an analysis tube of a quadrupole mass spectrometer for performing mass spectrometry of gas components in sample chamber 2. , 4 is an envelope for storing the analysis tube 3, 5 is a vacuum evacuation device for maintaining the inside of the envelope 4 at a high vacuum, 6 is a high vacuum valve for opening and closing between the envelope 4 and the vacuum evacuation device 5, 7 is an orifice plate for restricting the amount of gas flowing from the sample chamber 2 into the envelope 4.
次に動作について説明する。まず真空排気装置
５を稼働させ、次いで試料室２の中に試料１を取
付けて耐環境性評価試験装置を稼働させる。試験
開始前に高真空バルブ６を開き、分析管３を収納
しているエンベロープ４の中を真空排気する。そ
してエンベロープ４の中の圧力が１×10-4torrよ
りも低く、かつ試料室２の圧力よりも低くなつた
ら四重極質量分析計を稼働させ、試料室２からオ
リフイス板７のオリフイスを通してエンベロープ
４の中に流入してきたガスの質量分析を行う。 Next, the operation will be explained. First, the evacuation device 5 is operated, then the sample 1 is installed in the sample chamber 2, and the environment resistance evaluation test device is operated. Before starting the test, the high vacuum valve 6 is opened to evacuate the inside of the envelope 4 housing the analysis tube 3. When the pressure inside the envelope 4 is lower than 1×10 -4 torr and lower than the pressure in the sample chamber 2, the quadrupole mass spectrometer is started, and the envelope is passed from the sample chamber 2 through the orifice of the orifice plate 7. 4. Perform mass spectrometry on the gas that has flowed into the chamber.
従来の耐環境性評価試験装置に備えられている
ガス分析システムは以上のように構成されている
ので、四重極質量分析計による試料室２内のガス
の測定はオリフイス板７のオリフイスの径に応
じ、試料室２の圧力の狭い範囲でしか実施できな
かつた。そして測定不可能な試料室２内の圧力に
おいては、その圧力に応じた径のオリフイスに変
えるために、試料室２と分析管３の接続部を外し
てオリフイス板７を取扱えなければならなかつ
た。また高真空の試料室２内において、測定対象
ガスが微量ないし吸着性の場合は、分析管３まで
到達する測定対象ガスの量が少ないため、測定が
非常に困難であるなどの問題点があつた。
Since the gas analysis system provided in the conventional environment resistance evaluation test device is configured as described above, the measurement of gas in the sample chamber 2 by the quadrupole mass spectrometer is performed using the diameter of the orifice of the orifice plate 7. Therefore, it could only be carried out within a narrow range of pressure in the sample chamber 2. When the pressure inside the sample chamber 2 is unmeasurable, it is necessary to remove the connection between the sample chamber 2 and the analysis tube 3 and handle the orifice plate 7 in order to change the orifice to a diameter that corresponds to the pressure. Ta. In addition, if the gas to be measured is in trace amounts or adsorbent in the high vacuum sample chamber 2, the amount of gas to be measured that reaches the analysis tube 3 is small, making measurement extremely difficult. Ta.
この発明は上記のような問題点を解決するため
になされたもので、耐環境性評価試験装置の試料
室内の圧力が大気圧から高真空に至るまで、試料
室内のガスの質量分析ができるとともに、高真空
の試料室内において測定対象ガスが微量であつて
も、また吸着性のものであつても、質量分析がで
きるガス分析システムを得ることを目的とする。 This invention was made to solve the above-mentioned problems, and it is possible to perform mass analysis of gases in the sample chamber of the environment resistance evaluation test device, even when the pressure in the sample chamber ranges from atmospheric pressure to high vacuum. The object of the present invention is to provide a gas analysis system that can perform mass spectrometry even if the gas to be measured is small or adsorbent in a high-vacuum sample chamber.
この発明に係る耐環境性評価試験用ガス分析シ
ステムは、質量分析計の分析管と、この分析管を
収納しかつ前後にベローズを有するエンベロープ
と、このエンベロープ内の圧力を高真空に保つ真
空排気装置と、耐環境性評価試験装置の試料室側
から質量分析計の分析管側へのガス流入量を制御
するためのコンダクタンス可変の回転式オリフイ
ス板と、この回転式オリフイス板を回転させるた
めの回転導入機と、前記回転式オリフイス板に接
触するエンベロープ前面を前後に移動させる直線
導入機とを設けたものである。
The gas analysis system for environmental resistance evaluation testing according to the present invention includes an analysis tube of a mass spectrometer, an envelope that houses the analysis tube and has bellows at the front and rear, and a vacuum exhaust system that maintains the pressure inside the envelope at a high vacuum. The device, a rotary orifice plate with variable conductance for controlling the amount of gas flowing from the sample chamber side of the environmental resistance evaluation test device to the analysis tube side of the mass spectrometer, and a rotary orifice plate for rotating the rotary orifice plate. It is equipped with a rotational introduction device and a linear introduction device that moves the front surface of the envelope in contact with the rotary orifice plate back and forth.
この発明による耐環境性評価試験用ガス分析シ
ステムにおいては、回転式オリフイス板は回転導
入機により回転運動伝達部を介して回転され、耐
環境性評価試験装置の試料室内の圧力や測定対象
ガスに応じて適切な径のオリフイスに切換えら
れ、試料室側から質量分析計の分析管側へ流入す
るガスを適切な量にする。これにより試料室内の
圧力が大気圧から高真空に至つても試料室内のガ
スの質量分析を可能にする。Ｏリングが取付けら
れているエンベロープ前面は、エンベロープの前
部にベローズが設けられているため、直線導入機
により前後に移動され、エンベロープ前面と回転
式オリフイス板の接触部のシールおよび回転式オ
リフイス板の固定および回転がスムーズに行われ
る。質量分析計の分析管は、分析管を収納してい
るエンベロープ後部のベローズにより前方に移動
され、回転式オリフイス板のオリフイスを全開に
して分析管の前部（イオン源）を試料に近づけ、
高真空の試料室内において試料から放出される微
量ガスや吸着性ガスの質量分析が可能になる。
In the gas analysis system for environmental resistance evaluation testing according to the present invention, the rotary orifice plate is rotated by the rotation introducer via the rotational motion transmission part, and the rotary orifice plate is rotated by the rotation introduction device to adjust the pressure in the sample chamber of the environmental resistance evaluation testing device and the gas to be measured. Accordingly, the orifice is changed to an appropriate diameter to allow an appropriate amount of gas to flow from the sample chamber side to the analysis tube side of the mass spectrometer. This makes it possible to perform mass spectrometry of the gas in the sample chamber even when the pressure in the sample chamber ranges from atmospheric pressure to high vacuum. The front surface of the envelope, where the O-ring is attached, is moved back and forth by the linear feeder because a bellows is provided at the front of the envelope, sealing the contact area between the front surface of the envelope and the rotary orifice plate, and sealing the rotary orifice plate. is fixed and rotated smoothly. The analysis tube of the mass spectrometer is moved forward by the bellows at the rear of the envelope that houses the analysis tube, and the orifice of the rotary orifice plate is fully opened to bring the front of the analysis tube (ion source) close to the sample.
This enables mass spectrometry of trace gases and adsorbent gases released from samples in a high-vacuum sample chamber.
以下、この発明の一実施例を図について説明す
る。第１図はこの発明の一実施例を示す断面図、
第２図はＡ方向矢視図であり、図において、１〜
７は第３図と同一または相当部分を示す。分析管
３を収納するエンベロープ４は前後部にベローズ
１１，１２を備え、分析管３を前後に移動できる
ようになつている。１３は試料室２側から四重極
質量分析計の分析管３側へ導入するガスを適切な
量にするための回転式オリフイス板で、回転軸１
４を中心に回転可能となつており、同一円周上に
異なつた径のオリフイス１５（最大径62mmφ）を
有し、コンダクタンス可変となつている。１６は
試料室２の中にある回転式オリフイス板１３を外
部から回転させるための回転導入機、１７は回転
導入機１６の回転を回転式オリフイス板１３に伝
えるための回転運動伝達部であり、回転式オリフ
イス板１３の外周に形成された歯車にかみ合う歯
車からなる。１８は回転式オリフイス板１３の固
定および回転をスムーズにするため、分析管３を
収納しているエンベロープ４の前面を前後に動か
すための直線導入機、１９は直線導入機１８によ
る直線運動をエンベロープ４の前部に伝達するた
めの直線運動伝達部、２０は回転式オリフイス板
１３のオリフイス１５の周囲に接するようにエン
ベロープ４の前面にはめ込まれたＯリングであ
る。
An embodiment of the present invention will be described below with reference to the drawings. FIG. 1 is a sectional view showing an embodiment of the present invention;
FIG. 2 is a view in the direction of arrow A, and in the figure, 1 to
7 indicates the same or equivalent portion as in FIG. An envelope 4 that accommodates the analysis tube 3 is provided with bellows 11 and 12 at the front and rear so that the analysis tube 3 can be moved back and forth. 13 is a rotary orifice plate for introducing an appropriate amount of gas from the sample chamber 2 side to the analysis tube 3 side of the quadrupole mass spectrometer;
4, and has orifices 15 of different diameters (maximum diameter 62 mmφ) on the same circumference, making the conductance variable. 16 is a rotation introducing machine for externally rotating the rotary orifice plate 13 in the sample chamber 2; 17 is a rotational motion transmission unit for transmitting the rotation of the rotation introducing machine 16 to the rotary orifice plate 13; It consists of a gear that meshes with a gear formed on the outer periphery of the rotary orifice plate 13. 18 is a linear introduction machine for moving the front surface of the envelope 4 housing the analysis tube 3 back and forth in order to fix and rotate the rotary orifice plate 13 smoothly; 19 is a linear introduction machine for moving the linear movement by the linear introduction machine 18 into the envelope; A linear motion transmitting part 20 for transmitting the linear motion to the front part of the envelope 4 is an O-ring fitted into the front surface of the envelope 4 so as to be in contact with the circumference of the orifice 15 of the rotary orifice plate 13.
次に動作について説明する。まず耐環境性評価
試験装置の試料室２の中が１×10-4torrよりも高
い圧力における動作について説明する。通常、耐
環境性評価試験装置稼働前は回転式オリフイス板
１３および高真空バルブ６が閉じた状態であるの
で、まず真空排気装置５を稼働させる。次いで試
料１を取付け、耐環境性評価試験装置を稼働させ
る。試験開始前に高真空バルブ６を開き、四重極
質量分析計の分析管３を収納しているエンベロー
プ４の中を真空排気する。そして、エンベロープ
４の中が高真空（１×10-6torr以下）に達したら
四重極質量分析計を稼働させ、質量分析が可能な
状態に分析管３を制御する。次いで直線導入機１
８を引いて前部のベローズ１１を縮め、直線運動
伝達部１９を介してＯリング２０がはめ込まれて
いるエンベロープ４の前面を回転式オリフイス板
１３との接触部のシールが損わない程度に離す。
そして閉止の状態である回転式オリフイス板１３
を回転導入機１６によつて回転させ、試料室２側
のガスの流入によつて分析管３側の圧力が１×
10-4torr以上にならないように適切な径のオリフ
イス１５を分析管３の前面に位置させ、真線導入
機１８を押して直線運動伝達部１９を介してＯリ
ング２０がはめ込まれているエンベロープ４の前
面を回転式オリフイス板１３に押付け、エンベロ
ープ４の前面と回転式オリフイス板１３の接触部
のシールおよび回転式オリフイス板１３の固定を
行う。そして耐環境性評価試験を開始し、試料室
２内のガスの質量分析を行う。 Next, the operation will be explained. First, the operation at a pressure higher than 1×10 −4 torr in the sample chamber 2 of the environmental resistance evaluation test device will be explained. Normally, the rotary orifice plate 13 and the high vacuum valve 6 are in a closed state before the environment resistance evaluation test device is operated, so the vacuum evacuation device 5 is operated first. Next, sample 1 is attached and the environment resistance evaluation test device is operated. Before starting the test, the high vacuum valve 6 is opened to evacuate the inside of the envelope 4 housing the analysis tube 3 of the quadrupole mass spectrometer. When the inside of the envelope 4 reaches a high vacuum (below 1×10 -6 torr), the quadrupole mass spectrometer is operated and the analysis tube 3 is controlled to a state where mass spectrometry is possible. Next, straight introduction machine 1
8 to retract the front bellows 11, and the front surface of the envelope 4, into which the O-ring 20 is fitted, is moved through the linear motion transmission part 19 to the extent that the seal at the contact part with the rotary orifice plate 13 is not damaged. Let go.
And the rotary orifice plate 13 is in a closed state.
is rotated by the rotation introducer 16, and the pressure on the analysis tube 3 side increases to 1× due to the inflow of gas from the sample chamber 2 side.
An orifice 15 with an appropriate diameter so as not to exceed 10 -4 torr is positioned in front of the analysis tube 3, and the straight line introducing device 18 is pushed to insert the envelope 4 into which the O-ring 20 is fitted via the linear motion transmission part 19. The front surface of the envelope 4 is pressed against the rotary orifice plate 13, and the contact portion between the front surface of the envelope 4 and the rotary orifice plate 13 is sealed and the rotary orifice plate 13 is fixed. Then, an environmental resistance evaluation test is started, and mass spectrometry of the gas in the sample chamber 2 is performed.
次に耐環境性評価試験時において、試験装置の
試料室２の中が１×10-4torrよりも低い圧力にお
ける動作について説明する。まず真空排気装置５
を稼働させ、次いで試料１を取付け、耐環境性評
価試験装置を稼働させる。試験開始前に高真空バ
ルブ６を開き、分析管３を収納しているエンベロ
ープ４の中を真空排気する。そして試料室２およ
びエンベロープ４の中が高真空（１×10-6torr以
下）に達したら高真空バルブ６を閉じて、閉止の
状態にある回転式オリフイス板１３を回転導入機
１６によつて回転させ、全開となる径のオリフイ
ス（直径62mmφ）１５を分析管３の前面に位置さ
せて直線導入機１８を押して直線運動伝達部１９
を介してＯリング２０がはめ込まれているエンベ
ロープ４の前面を回転式オリフイス板１３に押付
けて固定する。次に四重極質量分析計を稼働さ
せ、質量分析が可能な状態に分析管３を制御す
る。そして耐環境性評価試験を開始し、試料室２
内のガスの質量分析を行う。 Next, the operation at a pressure lower than 1×10 −4 torr in the sample chamber 2 of the test device during the environmental resistance evaluation test will be described. First, vacuum exhaust device 5
Then, sample 1 is attached and the environmental resistance evaluation test device is operated. Before starting the test, the high vacuum valve 6 is opened to evacuate the inside of the envelope 4 housing the analysis tube 3. When the inside of the sample chamber 2 and the envelope 4 reach a high vacuum (below 1×10 -6 torr), the high vacuum valve 6 is closed, and the rotary orifice plate 13 in the closed state is inserted by the rotary introduction device 16. Rotate the orifice (diameter 62 mmφ) 15 to be fully opened and position it in front of the analysis tube 3 and push the linear introduction device 18 to open the linear motion transmission section 19.
The front surface of the envelope 4, into which the O-ring 20 is fitted, is pressed against the rotary orifice plate 13 and fixed. Next, the quadrupole mass spectrometer is operated and the analysis tube 3 is controlled to a state where mass spectrometry is possible. Then, we started the environmental resistance evaluation test, and
Perform mass spectrometry of the gas within.
試料１から放出されるガスが微量ないし吸着性
の場合は、エンベロープ４の後部のベローズ１２
を縮めて分析管３を試料１側へ移動させ、分析管
３の前部を試料１に近づけて、試料１から放出さ
れたガスを質量分析する。 If the gas released from the sample 1 is small or adsorbent, the bellows 12 at the rear of the envelope 4
The analysis tube 3 is moved to the sample 1 side by contracting, the front part of the analysis tube 3 is brought close to the sample 1, and the gas released from the sample 1 is subjected to mass spectrometry.
なお、上記実施例では、質量分析に四重極質量
分析計を用いたが、セクター型質量分析計等の他
の質量分析計でもよい。またエンベロープ４およ
び回転式オリフイス板１３の構造、駆動機構等は
変更可能である。 In the above embodiment, a quadrupole mass spectrometer was used for mass spectrometry, but other mass spectrometers such as a sector type mass spectrometer may be used. Further, the structure, drive mechanism, etc. of the envelope 4 and the rotary orifice plate 13 can be changed.
以上のように、この発明によれば、耐環境性評
価試験装置の外部からガス分析システムのオリフ
イス径を変換できるようにしたので、分析管を外
してオリフイス板を取換えることなく、試験装置
内の圧力が大気圧から高真空に至るまでのガス分
析が可能になり、質量分析計の分析管を試験装置
内の試料に近づけることができるので、高真空の
試験装置内において試料から放出される微量ガス
や吸着性ガスの分析が可能になるなどの効果があ
る。
As described above, according to the present invention, it is possible to change the orifice diameter of the gas analysis system from outside the environment resistance evaluation test equipment, so there is no need to remove the analysis tube and replace the orifice plate. It is now possible to analyze gases at pressures ranging from atmospheric pressure to high vacuum, and the analysis tube of the mass spectrometer can be brought close to the sample in the test equipment, so that the gas released from the sample in the high vacuum test equipment can be analyzed. This has the effect of making it possible to analyze trace gases and adsorptive gases.
第１図はこの発明の一実施例を示す断面図、第
２図はＡ方向矢視図、第３図は従来のガス分析シ
ステムを示す断面図である。
各図中、同一符号は同一または相当部分を示
し、１は試料、２は試料室、３は分析管、４はエ
ンベロープ、５は真空排気装置、６は高真空バル
ブ、１１，１２はベローズ、１３は回転式オリフ
イス板、１５はオリフイス、１６は回転導入機、
１７は回転運動伝達部、１８は直線導入機、１９
は直線運動伝達部である。
FIG. 1 is a sectional view showing an embodiment of the present invention, FIG. 2 is a view taken in the direction of arrow A, and FIG. 3 is a sectional view showing a conventional gas analysis system. In each figure, the same reference numerals indicate the same or equivalent parts, 1 is the sample, 2 is the sample chamber, 3 is the analysis tube, 4 is the envelope, 5 is the vacuum exhaust device, 6 is the high vacuum valve, 11 and 12 are the bellows, 13 is a rotating orifice plate, 15 is an orifice, 16 is a rotating introduction machine,
17 is a rotational motion transmission section, 18 is a linear introduction machine, 19
is a linear motion transmission part.
Claims (1)
かつ前後にベローズを有するエンベロープと、こ
のエンベロープ内の圧力を高真空に保つ真空排気
装置と、耐環境性評価試験装置の試料室側から質
量分析計の分析管側へのガス流入量を制御するた
めのコンダクタンス可変の回転式オリフイス板
と、この回転式オリフイス板を回転させるための
回転導入機と、前記回転式オリフイス板に接触す
るエンベロープ前面を前後に移動させる直線導入
機とを備えたことを特徴とする耐環境性評価試験
用ガス分析システム。 ２ 回転式オリフイス板が同一円周上に異なる径
の複数のオリフイスを有するものであることを特
徴とする特許請求の範囲第１項記載の耐環境性評
価試験用ガス分析システム。[Claims] 1. An analysis tube of a mass spectrometer, an envelope that houses the analysis tube and has bellows at the front and rear, a vacuum evacuation device that maintains the pressure inside the envelope at a high vacuum, and an environmental resistance evaluation test. a rotary orifice plate with variable conductance for controlling the amount of gas flowing from the sample chamber side of the device to the analysis tube side of the mass spectrometer; a rotation introduction machine for rotating the rotary orifice plate; A gas analysis system for environmental resistance evaluation testing, which is equipped with a linear introduction device that moves the front surface of the envelope back and forth in contact with the orifice plate. 2. The gas analysis system for environmental resistance evaluation test according to claim 1, wherein the rotary orifice plate has a plurality of orifices with different diameters on the same circumference.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61209560A JPS6366839A (en) | 1986-09-08 | 1986-09-08 | Gas analyzing system for environmental resistance evaluation test |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61209560A JPS6366839A (en) | 1986-09-08 | 1986-09-08 | Gas analyzing system for environmental resistance evaluation test |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6366839A JPS6366839A (en) | 1988-03-25 |
| JPH043062B2 true JPH043062B2 (en) | 1992-01-21 |
Family
ID=16574848
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61209560A Granted JPS6366839A (en) | 1986-09-08 | 1986-09-08 | Gas analyzing system for environmental resistance evaluation test |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6366839A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103364304B (en) * | 2013-06-21 | 2015-08-12 | 浙江工业大学 | Hydrogen release proving installation in material deformation process and method of testing |
| KR101529608B1 (en) * | 2013-11-21 | 2015-06-18 | 한국표준과학연구원 | Small Punch Testing Apparatus under Gas Environment, Testing Method, Analysis Method and Recording Medium using the same |
-
1986
- 1986-09-08 JP JP61209560A patent/JPS6366839A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6366839A (en) | 1988-03-25 |
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| Date | Code | Title | Description |
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| EXPY | Cancellation because of completion of term |