JPS63148162A - Gaseous argon control device - Google Patents
Gaseous argon control deviceInfo
- Publication number
- JPS63148162A JPS63148162A JP29541386A JP29541386A JPS63148162A JP S63148162 A JPS63148162 A JP S63148162A JP 29541386 A JP29541386 A JP 29541386A JP 29541386 A JP29541386 A JP 29541386A JP S63148162 A JPS63148162 A JP S63148162A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- oxygen
- argon
- control device
- gaseous
- 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.)
- Pending
Links
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052786 argon Inorganic materials 0.000 title claims abstract description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000001301 oxygen Substances 0.000 claims abstract description 20
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 20
- 239000007789 gas Substances 0.000 claims description 12
- 238000001514 detection method Methods 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052802 copper Inorganic materials 0.000 abstract description 4
- 239000010949 copper Substances 0.000 abstract description 4
- 239000003507 refrigerant Substances 0.000 abstract description 4
- 239000012159 carrier gas Substances 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 abstract description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 abstract 1
- 239000005751 Copper oxide Substances 0.000 abstract 1
- 238000010276 construction Methods 0.000 abstract 1
- 229910000431 copper oxide Inorganic materials 0.000 abstract 1
- 239000013618 particulate matter Substances 0.000 abstract 1
- 210000003323 beak Anatomy 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 6
- 230000014759 maintenance of location Effects 0.000 description 5
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 239000002808 molecular sieve Substances 0.000 description 4
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
Description
【発明の詳細な説明】
（技術分野）
本発明は、アルゴンガス中の不純成分を検出するのに適
したガスクロマトグラフ装置に関する。DETAILED DESCRIPTION OF THE INVENTION (Technical Field) The present invention relates to a gas chromatograph apparatus suitable for detecting impurity components in argon gas.
（従来技術）
例えば、半導体製造工程において使用されるアルゴンガ
スの品質管理は、これに含まれている徴ｊｌな酸素や窒
素の有無を検出することにより行なわれているが、通常
のカラムではアルゴンと酸素を分離することが不可能で
あるため、モレキュラーシーブカラムをマイナス１００
℃程度に冷却したガスクロマトグラフを使用する必要が
ある。(Prior art) For example, quality control of argon gas used in semiconductor manufacturing processes is performed by detecting the presence or absence of characteristic oxygen and nitrogen contained in the gas. Because it is impossible to separate oxygen from
It is necessary to use a gas chromatograph cooled to about ℃.
このため、カラムを低温に保持するための冷却製雪や冷
媒を必要として分析製雪の構造が複雑化や、冷媒の補給
を必要として保守に手間を要するという問題があった。For this reason, there have been problems in that the structure of analytical snow making is complicated because it requires cooling snow making and a refrigerant to keep the column at a low temperature, and it requires replenishment of refrigerant, which requires time and effort for maintenance.
（目的）
本発明はこのような問題に鏡でなされたものであって、
その目的とするところは簡単な構造で、しかも冷媒を不
要とした新規なアルゴンガス管理装置を提供すること（
こある。(Purpose) The present invention has been made to solve these problems,
The purpose is to provide a new argon gas management device that has a simple structure and does not require a refrigerant.
There it is.
（発明の概要）
すなわち、本発明が特徴とするところは、試料自体のク
ロマトグラムと酸化反応炉を通過させたときのクロマト
グラムを得るようにした点にある。(Summary of the Invention) That is, the present invention is characterized in that a chromatogram of the sample itself and a chromatogram of the sample when it passes through an oxidation reactor are obtained.
（実施例）
そこで、以下に本発明の詳細を図示した実施例に基づい
て説明する。(Example) The details of the present invention will be described below based on illustrated examples.
第１図は、本発明の一実施例を示すものであって、図中
符号１は、酸化反応炉で、ヒータ１ａにより加熱を受け
る容器］ｂに還元銅粒子１ｃを収容して構成され、一端
は分岐管２を介して試料注入口３に、他端はダミーカラ
ム４を介して切換弁５に接続されでいる。６は、モレキ
ュラシーブ力ラムからなるメインカラムで、一端は切換
弁５に、他端は検出器８に接続されでいる。一方、試料
注入口３側の分岐管２の他方の排出口にはプレカラム９
を介して切換弁５に、ざらに抵抗管１０を経由して大気
開放口１］に接続されている。この切換弁５は、第１の
位置に設定されたとき、反応炉１− ダミーカラム４−
メインカラム６に至る第１分析流路と、プレカラム９
− 抵抗管１０に至る排気流路を形成し、また第２の位
置に設定されたときには反応炉］ −抵抗管１０に至る
排気流路と、プレカラム９− メインカラム６に至る第
２分析流路を形成するよう（こ管路接続されている。FIG. 1 shows an embodiment of the present invention, in which reference numeral 1 denotes an oxidation reactor, which is constructed by accommodating reduced copper particles 1c in a container]b which is heated by a heater 1a. One end is connected to a sample injection port 3 via a branch pipe 2, and the other end is connected to a switching valve 5 via a dummy column 4. 6 is a main column consisting of a molecular sieve force ram, one end of which is connected to the switching valve 5, and the other end connected to the detector 8. On the other hand, the other outlet of the branch pipe 2 on the side of the sample injection port 3 has a precolumn 9.
It is connected to the switching valve 5 via the directional control valve 5, and to the atmosphere opening 1 via the resistance pipe 10. When this switching valve 5 is set to the first position, the reactor 1 - dummy column 4 -
The first analysis channel leading to the main column 6 and the pre-column 9
- Forming an exhaust flow path leading to the resistance tube 10 and, when set in the second position, the reactor] - An exhaust flow path leading to the resistance tube 10 and the pre-column 9 - A second analysis flow path leading to the main column 6 (This conduit is connected to form a
この実施例においで、切換弁５を第１の位置（図中 実
線）に設定して試料を注入すると、試料は、キャリアガ
スによつ分岐管２に運ばれ、ここで等分に分流して反応
炉１とプレカラム９に流入する０反応炉１に流入した試
料は、ここに収容されでいる還元銅粉粒体１ｃに接触し
て、還元銅１ｃを酸化鋼としつつ酸素だけを選択的に除
去され、ついで切換弁５を通ってメインカラム６に流入
する。言うまでもなく、モレキュラシーブ力ラム６は、
常温においてもアルゴンと窒素を確実に分離するから、
検出器８はアルゴンと窒素をそれぞれ独立のビークとし
て検出することになる。In this example, when the switching valve 5 is set to the first position (solid line in the figure) and the sample is injected, the sample is carried by the carrier gas to the branch pipe 2, where it is divided into equal parts. The sample that has flowed into the reactor 1 and the pre-column 9 comes into contact with the reduced copper powder 1c housed here, and selectively removes only oxygen while converting the reduced copper 1c into oxidized steel. It then flows into the main column 6 through the switching valve 5. Needless to say, Molecular Sieve Power Ram 6,
Because it reliably separates argon and nitrogen even at room temperature,
The detector 8 detects argon and nitrogen as independent beaks.
一方、プレカラム９側に流入した試料は、抵抗管１０を
通って大気開放口］１がら大気中に排気される。On the other hand, the sample that has flowed into the pre-column 9 side passes through the resistance tube 10 and is exhausted into the atmosphere through the atmosphere opening port]1.
このようにして第１分析流路での測定か終了した段階で
切換弁５を第２の位置に切換えると、プレカラム９に流
入している試料は、切換弁５を介してメインカラム６に
流入する。なお、この切換弁５の操作時においでは、第
１分析流路、及び第２分析流路、つまり反応炉１− ダ
ミーカラム４− メインカラム６に至る流路と、プレカ
ラム９− メインカラム６に至る流路は、その流路抵抗
が同一となるように構成されているから、分析に対象と
なる試料量が同一となるばかりでなく、検出器８に対す
る圧力衝撃が小さくなる。When the switching valve 5 is switched to the second position when the measurement in the first analysis channel is completed in this way, the sample flowing into the pre-column 9 flows into the main column 6 via the switching valve 5. do. In addition, when operating this switching valve 5, the first analysis flow path and the second analysis flow path, that is, the flow path leading from the reactor 1 to the dummy column 4 to the main column 6, and from the precolumn 9 to the main column 6. Since the flow paths leading to the detector 8 are configured to have the same flow path resistance, not only the amount of sample to be analyzed becomes the same, but also the pressure impact on the detector 8 is reduced.
この第２分析流路においでは、試料が反応炉１を経由し
ていないため、メインカラム６は、酸素を含んだ試料の
流入を受け、アルゴンと酸素とを未分離成分として排出
することになり、このため検出器８は、アルゴンと酸素
とを共通とするビー−りと、窒素のビークを検出するこ
とになる。In this second analysis channel, since the sample does not pass through the reactor 1, the main column 6 receives the inflow of the sample containing oxygen and discharges argon and oxygen as unseparated components. Therefore, the detector 8 detects a beak that contains argon and oxygen in common, and a beak that contains nitrogen.
このようにして得た第１のクロマトグラムと第２のクロ
マトグラムとを比較し、アルゴンのリテンションタイム
に一敗するビークの差分を求めることにより、アルゴン
ガスに含まれている酸素の量を知ることができる。By comparing the first chromatogram and the second chromatogram obtained in this way and finding the difference in the peak that completely exceeds the retention time of argon, the amount of oxygen contained in the argon gas can be determined. be able to.
［実 施 例］
酸素、アルゴン、及び窒素をそれぞれ体積比で１６．６
％、１６．７％、６６．７％ずつ混合してなる試料を用
い、まず切換弁５を第１の位置（第１図中における実線
）においで分析したところ、第２図工に示すようなアル
ゴンのリテンションタイムにおけるビークＰ□と、窒素
のリテンションタイムにおけるビークＰ２のクロマトグ
ラムを得た。ついで切換弁５を第２の位置（第１図中に
おける点線）に切換えて分析したところ第２図ＩＩに示
すようなアルゴンのリテンションタイムにおけるビーク
Ｐ３と、窒素のリテンションタイムにおけるビークＰ４
のクロマトグラムを得た。 この結果、メインカラム６
により分離可能な窒素のビークＰ２とビークＰ４は、そ
の高さび弁５の切換え前後で変化がなく、これにより等
量ずつ試料が注入されていることが判明した。また反応
炉１を通過きせる前のビークＰ□と、反応炉）を通過さ
せた後のビークＰ３との差は、酸素濃度に一敗していた
。[Example] Oxygen, argon, and nitrogen each at a volume ratio of 16.6
%, 16.7%, and 66.7% were analyzed with the switching valve 5 in the first position (solid line in Figure 1), and the result was as shown in Figure 2. Chromatograms of peak P□ at the argon retention time and peak P2 at the nitrogen retention time were obtained. Then, when the switching valve 5 was switched to the second position (dotted line in FIG. 1) and analyzed, a peak P3 at the argon retention time and a peak P4 at the nitrogen retention time were found as shown in FIG. 2 II.
A chromatogram was obtained. As a result, main column 6
It was found that the height of the nitrogen beaks P2 and P4 that can be separated by this method does not change before and after switching the valve 5, and that the same amount of the sample is injected. Moreover, the difference between the beak P□ before passing through the reactor 1 and the beak P3 after passing through the reactor 1 was determined by the oxygen concentration.
なあ、図中符号Ｐ５は、切換弁５の操作に伴なう外乱ピ
ークを示す。Incidentally, the symbol P5 in the figure indicates a disturbance peak accompanying the operation of the switching valve 5.
これらのことから、反応炉を通過ぎせる前後のビークｐ
、 、Ｐ、の差を測定することによりアルボンガス中の
酸素濃度を正確に検出できることが判明した。From these facts, the beak p before and after passing through the reactor
It has been found that the oxygen concentration in arbon gas can be accurately detected by measuring the difference between , , and P.
第３図は、本発明の第２の実施例を示すものであって、
試料注入口３側に切換弁２０を介して酸化反応炉１と、
これと同一の流路抵抗ｍｔ有する抵抗管２１を接続する
一方、これら反応炉１と抵抗管２］の流出口にメインカ
ラム６を接続して流路を形成し、切換弁２０を交互に切
換えて反応炉１を通過させた試料と、酸化反応工程に関
与していない試料をメインカラム６に流入させて、それ
ぞれの流路からの試料を検出器８により検出して、第２
図に示したような２つのクロマトグラムを得るようにし
たもので、この実施例によれば流路構成を簡素化するこ
とが可能となる。FIG. 3 shows a second embodiment of the present invention,
An oxidation reactor 1 via a switching valve 20 on the sample injection port 3 side,
A resistance tube 21 having the same flow path resistance mt is connected to this, while a main column 6 is connected to the outlet of these reactor 1 and resistance tube 2 to form a flow path, and the switching valve 20 is alternately switched. The sample passed through the reactor 1 and the sample not involved in the oxidation reaction process are flowed into the main column 6, and the sample from each flow path is detected by the detector 8, and the second
Two chromatograms as shown in the figure are obtained, and according to this embodiment, it is possible to simplify the channel configuration.
第４図は、本発明の第３実施例を示すもので、試料注入
口３に直接モレキュラシーブ力ラムからなるメインカラ
ム６を接続し、これの流出口には切換弁３０を介して酸
化反応炉］と、これと同一の流体抵抗を有する抵抗管２
１を接続し、ざらに切換弁３１８介して選択的に検出器
８に接続するように構成されている。FIG. 4 shows a third embodiment of the present invention, in which a main column 6 consisting of a molecular sieve force ram is directly connected to the sample injection port 3, and an oxidation reactor is connected to the outlet of the main column 6 through a switching valve 30. ] and a resistance tube 2 having the same fluid resistance as this.
1 and is configured to be selectively connected to the detector 8 via a switching valve 318.
この実施例において、切換弁３０．３１を一方の位置、
例えば図中実線側に接続した状態で一定量の試料を注入
すると、酸素とアルゴンが未分離な状態のクロマトグラ
ムが、また切換弁を他方の位置（図中 点線）に設定し
て同量の試料を注入すると、メインカラム６では未分離
状態であった酸素とアルゴンを含む試料は、反応炉］に
おいて酸素を除去されてアルゴン単一成分としてのピー
クを持つロマトグラムを示すから、両者のクロマトグラ
ムを比較することによりアルゴン中の酸素や窒素の量を
知ることができる。In this embodiment, the switching valve 30.31 is placed in one position.
For example, if a fixed amount of sample is injected with the connection connected to the solid line in the figure, the chromatogram will show that oxygen and argon are not separated, and if the switching valve is set to the other position (dotted line in the figure), the same amount of sample will be injected. When the sample is injected, the sample containing oxygen and argon, which were unseparated in the main column 6, has oxygen removed in the reactor and shows a chromatogram with a peak as a single component of argon, so the chromatogram of both By comparing , you can find out the amount of oxygen and nitrogen in argon.
なお、上述の実施例においては、酸化反応炉に還元銅を
、またメインカラムとしてモレキュラシーブ力ラムを使
用しているが、酸素吸着剤や、常温以上においてもアル
ゴンと窒素を分離することのできるカラムを使用すれば
同様の作用を奏することは明らかである。In the above example, reduced copper is used in the oxidation reactor and a molecular sieve ram is used as the main column. It is clear that the same effect can be achieved by using .
（効果）
以上、説明したように本発明によれば、試料自体のクロ
マトグラムと、酸化反応炉を通過させたときのクロマト
グラムを得るようにしたので、カラムの冷却を不要とし
て構造と、保守の簡素化を図ったアルゴンガス管理装置
ｌを実現することができる。(Effects) As explained above, according to the present invention, the chromatogram of the sample itself and the chromatogram of the sample when it passes through the oxidation reactor are obtained, so there is no need to cool the column and the structure and maintenance can be improved. It is possible to realize an argon gas management device l that is simplified.
第１図は本発明の一実施例を示す装置の構成図、第２図
は同上製雪による分析結果を示すクロマトグラム、第３
．４図は、それぞれ本発明の他の実施例を示す装置の構
成図である。FIG. 1 is a configuration diagram of an apparatus showing an embodiment of the present invention, FIG. 2 is a chromatogram showing the analysis results obtained by the same snowmaking process, and FIG.
．． FIG. 4 is a block diagram of an apparatus showing other embodiments of the present invention.
Claims (1)
くともアルゴンをガスクロマトグラフ的に分離する第２
の手段、検出手段、及び前記第１の手段と第２の手段を
通過した試料を前記検出器に導く流路と、第１の手段だ
けを通過した試料を前記検出器に導く流路とを切換える
手段を備えてなるアルゴンガス管理装置。a first means for selectively removing oxygen in the sample gas; a second means for gas chromatographically separating at least argon;
means, a detection means, a flow path for guiding the sample that has passed through the first means and the second means to the detector, and a flow path for guiding the sample that has passed only the first means to the detector. An argon gas management device comprising means for switching.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29541386A JPS63148162A (en) | 1986-12-10 | 1986-12-10 | Gaseous argon control device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29541386A JPS63148162A (en) | 1986-12-10 | 1986-12-10 | Gaseous argon control device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63148162A true JPS63148162A (en) | 1988-06-21 |
Family
ID=17820282
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP29541386A Pending JPS63148162A (en) | 1986-12-10 | 1986-12-10 | Gaseous argon control device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63148162A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0688815A (en) * | 1992-09-07 | 1994-03-29 | Taiyo Sanso Co Ltd | Method and instrument for analyzing oxygen gas for impurity with high sensitivity |
| JP2000009734A (en) * | 1998-06-29 | 2000-01-14 | Hitachi Ltd | Analytical equipment and analysis method using the same and reagent vessel and deoxygenation mechanism used for the method |
-
1986
- 1986-12-10 JP JP29541386A patent/JPS63148162A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0688815A (en) * | 1992-09-07 | 1994-03-29 | Taiyo Sanso Co Ltd | Method and instrument for analyzing oxygen gas for impurity with high sensitivity |
| JP2000009734A (en) * | 1998-06-29 | 2000-01-14 | Hitachi Ltd | Analytical equipment and analysis method using the same and reagent vessel and deoxygenation mechanism used for the method |
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