JPH07287001A - Method and apparatus for analyzing impurity gas in fluorine gas - Google Patents
Method and apparatus for analyzing impurity gas in fluorine gasInfo
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- JPH07287001A JPH07287001A JP7867094A JP7867094A JPH07287001A JP H07287001 A JPH07287001 A JP H07287001A JP 7867094 A JP7867094 A JP 7867094A JP 7867094 A JP7867094 A JP 7867094A JP H07287001 A JPH07287001 A JP H07287001A
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- Prior art keywords
- gas
- fluorine
- impurity
- metal fluoride
- packed
- 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.)
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、フッ素ガス中の不純物
ガスの分析方法に係わり、更に詳しくはフッ素ガス中の
水素、酸素、窒素、一酸化炭素、二酸化炭素、その他の
不純物ガスを簡便かつ精度よく分析する方法およびその
装置に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for analyzing an impurity gas in fluorine gas, and more particularly to a method for easily measuring hydrogen, oxygen, nitrogen, carbon monoxide, carbon dioxide and other impurity gases in fluorine gas. The present invention relates to a method and an apparatus for analyzing accurately.
【０００２】[0002]
【従来の技術及び発明が解決しようとする課題】フッ素
ガス中の不純物ガスの分析方法としては、従来より、
（１）フッ素ガスが接触する部分に、ニッケル、モネ
ル、フッ素樹脂、フッ素油等の耐食性の材質を使用した
ガスクロマトグラフにより分析する方法、および（２）
フッ素を塩化物充填層に通してフッ素を保持容量の大き
い塩素に変換し、ガスクロマトグラフにより分離分析す
る方法等が知られている。しかし、（１）の方法におい
ては、フッ素を酸素等の他成分と分離するための適当な
充填剤がないため、分離できない成分については分析で
きないという問題がある。また、（２）の方法において
は、反応で生じた塩素も腐食性があるため、配管等も耐
蝕性の材料を用いなくてはならず、更に塩素と他の不純
物ガスを分離するガスクロ充填剤に制限があり、分析目
的に合った分離物を得るためには塩素の除去あるいはバ
ルブ操作によるガスクロ系外への排気などの煩雑な操作
が必要である。本発明の目的は、上記従来法の欠点を排
除し、簡便かつ精度良くフッ素ガス中の不純物ガスの分
析を行う方法を提供することにある。2. Description of the Related Art As a method for analyzing impurity gas in fluorine gas, there have been conventionally used
(1) A method of analyzing by a gas chromatograph using a corrosion-resistant material such as nickel, monel, fluororesin, or fluorine oil in a portion in contact with fluorine gas, and (2)
There is known a method in which fluorine is passed through a chloride packed bed to convert the fluorine into chlorine having a large retention capacity, and the gas is separated and analyzed by a gas chromatograph. However, the method (1) has a problem that a component that cannot be separated cannot be analyzed because there is no appropriate filler for separating fluorine from other components such as oxygen. Further, in the method (2), since chlorine generated by the reaction is also corrosive, it is necessary to use a corrosion-resistant material for the piping and the like, and a gas chromatographic filler for separating chlorine and other impurity gases. However, in order to obtain a separated product suitable for the purpose of analysis, it is necessary to perform a complicated operation such as chlorine removal or valve operation to exhaust the gas outside the gas chromatography system. An object of the present invention is to eliminate the above-mentioned drawbacks of the conventional method and to provide a method for simply and accurately analyzing an impurity gas in fluorine gas.
【０００３】[0003]
【課題を解決するための手段】本発明者等は、かかる目
的を達成すべく鋭意検討した結果、本発明に到達した。
即ち本発明は、不純物ガスを含有するフッ素ガスを金属
フッ化物充填層に通し、フッ素ガスを固定化除去した
後、ガスクロマトグラフにより分析することを特徴とす
るフッ素ガス中の不純物ガスの分析方法、およびキャリ
アーガスの流路を切り替えることが可能な六方切換バル
ブに一定容量のサンプルが分取できる試料計量管が付い
たガスサンプラー、金属フッ化物が充填された管、およ
びガスクロマトグラフが順次配管により連結され、キャ
リアーガスがガスサンプラー、金属フッ化物が充填され
た管、ガスクロマトグラフの順で流れるよう配管された
フッ素ガス中の不純物ガスの分析装置に関するものであ
る。The inventors of the present invention have arrived at the present invention as a result of extensive studies to achieve such an object.
That is, the present invention, a fluorine gas containing an impurity gas is passed through a metal fluoride packed layer, after the fluorine gas is fixed and removed, an analysis method of the impurity gas in the fluorine gas, characterized by analyzing by gas chromatography, A gas sampler with a sample metering tube that can collect a fixed amount of sample in a hexagonal switching valve that can switch the flow path of carrier gas, a tube filled with metal fluoride, and a gas chromatograph are connected sequentially by piping. The present invention relates to an analyzer for impurity gas in fluorine gas, in which a carrier gas is piped so as to flow in the order of a gas sampler, a tube filled with metal fluoride, and a gas chromatograph.
【０００４】本発明では、金属フッ化物にてフッ素ガス
を固定化除去した後、ガスクロマトグラフにより分析す
ることにより、簡便かつ精度良くフッ素ガス中の不純物
ガスの分析が行えるものである。ここで用いられる金属
フッ化物としては、フッ素と反応し高次フッ化物と成り
得るものであれば何れのものでもよく、例えば二フッ化
コバルト（CoF2）、二フッ化マンガン（MnF2）、一フッ
化水銀（HgF)、一フッ化銀（AgF)、三フッ化セリウム
（CeF3）、二フッ化鉛（PbF2）、一フッ化タリウム（Tl
F)、三フッ化ビスマス（BiF3）、二フッ化鉄（FeF2）等
の化合物、あるいはアルカリ金属フッ化物（NaF 、KF、
LiF など) とNiF2との反応物（Na3NiF5 、K3NiF5、Li3N
iF5 など）が挙げられる。これらの金属フッ化物充填層
にフッ素が導入された場合の化学的変化を例えば二フッ
化コバルト（CoF2）について反応式で表せば次式のよう
になる。 F2 ＋ ２CoF2 → ２CoF3 上記反応式のようにフッ素は、固体の高次フッ化物とな
り固定され除去される。又、フッ素除去のための金属フ
ッ化物が充填された管は、反応の効率を上げるために、
その温度を高くしてフッ素と金属フッ化物を反応させる
のが好ましい。例えば、二フッ化コバルトの場合は、 1
00〜400 ℃で反応は促進されるが、望ましくは 200〜30
0 ℃の温度にに金属フッ化物が充填された管を保つのが
よい。金属フッ化物が充填された管においては、フッ素
のみが除去され、フッ素ガス中の不純物ガスである水
素、酸素、窒素、一酸化炭素、二酸化炭素、その他のガ
スは、金属フッ化物が充填された管を損失されることな
く通過する。フッ素が除去され不純物ガスのみとなった
試料ガスは、例えばヘリウム等のキャリアーガスによっ
てガスクロマトグラフに導かれ、適当な充填剤が充填さ
れた分離カラムによって分離される。分離に用いる充填
剤は、例えばモレキュラーシーブ５Ａの様な充填剤を用
いれば、水素、酸素、窒素、一酸化炭素を分離すること
ができる。このとき二酸化炭素は吸着されてしまうた
め、他の充填剤、例えば、ポーラスポリマー系のガスク
ロ充填剤であるポラパックＱ（米国ウォータース社製）
等を使用すれば水素、酸素、窒素、一酸化炭素の混合ガ
スと二酸化炭素を分離することができる。本発明におい
て、ガスクロマトグラムの検出器は、熱伝導度検出器が
使用できるが、より高い感度を得たいのであれば、無機
ガスに対し特に感度の高い光イオン化検出器等も使用で
きる。In the present invention, the impurity gas in the fluorine gas can be easily and accurately analyzed by immobilizing and removing the fluorine gas with the metal fluoride and then analyzing by gas chromatography. The metal fluoride used here may be any as long as it can react with fluorine to form a higher order fluoride, for example, cobalt difluoride (CoF 2 ), manganese difluoride (MnF 2 ), Mercury monofluoride (HgF), silver monofluoride (AgF), cerium trifluoride (CeF 3 ), lead difluoride (PbF 2 ), thallium monofluoride (Tl)
F), bismuth trifluoride (BiF 3 ), compounds such as iron difluoride (FeF 2 ), or alkali metal fluorides (NaF, KF,
LiF) and NiF 2 reaction products (Na 3 NiF 5 , K 3 NiF 5 , Li 3 N
iF 5 etc.) can be mentioned. The chemical changes in the case where fluorine is introduced into these metal fluoride filled layers can be expressed by the following equation, for example, using a reaction equation for cobalt difluoride (CoF 2 ). F 2 + 2CoF 2 → 2CoF 3 As shown in the above reaction formula, fluorine becomes a solid higher fluoride and is fixed and removed. Also, the tube filled with metal fluoride for removing fluorine is
It is preferable to raise the temperature to react the fluorine with the metal fluoride. For example, for cobalt difluoride, 1
The reaction is accelerated at 00 ~ 400 ℃, but preferably 200 ~ 30
It is advisable to keep the tube filled with metal fluoride at a temperature of 0 ° C. In the tube filled with metal fluoride, only fluorine was removed, and hydrogen, oxygen, nitrogen, carbon monoxide, carbon dioxide, and other gases, which are impurity gases in the fluorine gas, were filled with metal fluoride. Pass the tube without loss. The sample gas from which the fluorine has been removed and which has become only the impurity gas is guided to a gas chromatograph by a carrier gas such as helium and separated by a separation column filled with an appropriate packing material. Hydrogen, oxygen, nitrogen and carbon monoxide can be separated by using a packing such as molecular sieve 5A as the packing used for the separation. At this time, since carbon dioxide is adsorbed, another filler, for example, Porapak Q (manufactured by US Waters Corporation), which is a porous polymer-based gas chromatography filler, is used.
If used, etc., carbon dioxide can be separated from a mixed gas of hydrogen, oxygen, nitrogen and carbon monoxide. In the present invention, as the detector of the gas chromatogram, a thermal conductivity detector can be used, but if higher sensitivity is desired, a photoionization detector having a particularly high sensitivity to inorganic gas can also be used.
【０００５】本発明に用いる装置を分かりやすく説明す
るために、試料ガスが各設備を通過する順に説明すれ
ば、以下の通りである。即ち、試料ガスは、まず一定量
分取するためのガスサンプラーに配管によって導かれ
る。ガスサンプラーは、キャリアーガスの流路を切り替
えることが可能な六方切換バルブに一定容量のサンプル
が分取できるサンプリング管が付いたものである。試料
ガスのサンプリング量は、試料の導入圧力を正確に圧力
計によって読み取り決定すればよい。試料計量管内の試
料ガスは、次に六方切換バルブを操作し流路を切り替え
ることによってキャリアーガスで押し流され、金属フッ
化物が充填された管へ導かれる。金属フッ化物が充填さ
れた管は、フッ素を完全に除去するために予めヒーター
によって加熱しておくのが好ましいのは前述の通りであ
る。例えば、フッ化コバルトを充填剤とした場合、200
〜300 ℃程度に保つのが望ましい。フッ素が接触するこ
こまでの流路、即ち試料ガス容器からガスサンプラーを
経由して金属フッ化物が充填された管に至るまでの流路
は、フッ素ガスによる腐蝕を防ぐためニッケル、モネ
ル、フッ素樹脂等の耐蝕材料を使用するのが望ましい。
また、ステンレス等を用いるのであれば操作前にフッ素
で十分に不動態化すべきである。金属フッ化物が充填さ
れた管を通過した試料ガスは、フッ素が完全に除去さ
れ、不純物ガスである水素、酸素、窒素、一酸化炭素、
二酸化炭素等は損失されることなくキャリアーガスで押
し流され、配管によってガスクロマトグラムに導かれ
る。ガスクロマトグラムでは、水素、酸素、窒素、一酸
化炭素を分析目的とした場合であればモレキュラーシー
ブ５Ａを充填したカラムで分離し、二酸化炭素を分析目
的とした場合、ポーラスポリマー系のガスクロ充填剤で
あるポラパックＱ（米国ウォータース社製）を充填した
カラムで分離する。ガスクロカラムで分離された不純物
ガスは、熱伝導度検出器で検出される。In order to explain the apparatus used in the present invention in an easy-to-understand manner, the order in which the sample gas passes through each facility will be described below. That is, the sample gas is first led by a pipe to a gas sampler for collecting a fixed amount. The gas sampler is a hexagonal switching valve that can switch the flow path of carrier gas and a sampling tube that can collect a fixed amount of sample. The sampling amount of the sample gas may be determined by accurately reading the introduction pressure of the sample with a pressure gauge. The sample gas in the sample measuring tube is then swept away by the carrier gas by operating the hexagonal switching valve to switch the flow path, and is guided to the tube filled with the metal fluoride. As described above, the tube filled with the metal fluoride is preferably heated in advance by a heater in order to completely remove the fluorine. For example, when using cobalt fluoride as the filler, 200
It is desirable to keep the temperature at ~ 300 ° C. The flow path up to which fluorine comes into contact, that is, the flow path from the sample gas container to the tube filled with metal fluoride via the gas sampler is nickel, monel, or fluororesin to prevent corrosion by fluorine gas. It is desirable to use a corrosion resistant material such as.
If stainless steel or the like is used, it should be sufficiently passivated with fluorine before the operation. The sample gas that has passed through the tube filled with metal fluoride has fluorine completely removed, and hydrogen, oxygen, nitrogen, carbon monoxide, which are impurity gases,
Carbon dioxide and the like is washed away by the carrier gas without being lost, and is guided to the gas chromatogram by a pipe. In the gas chromatogram, when hydrogen, oxygen, nitrogen, and carbon monoxide are used for analysis, they are separated by a column packed with molecular sieve 5A, and when carbon dioxide is used for analysis, a porous polymer-based gas chromatographic filler is used. Separation is performed using a column packed with a certain Polapack Q (manufactured by Waters, USA). The impurity gas separated by the gas chromatography column is detected by the thermal conductivity detector.
【０００６】[0006]
【実施例】以下、本発明の分析方法に用いる装置を示す
図１を用い、本発明の実際の分析方法を更に具体的に説
明する。先ず、試料容器11を接続した後、容器バルブ７
が閉まっていることを確認し、バルブ１〜３を開、４を
閉、六方切換バルブ６を図１の状態とし、バルブ５から
のびる配管からヘリウムガスを流し、フッ素が通る配
管、バルブ等から空気成分その他分析に正の誤差を与え
る成分をヘリウムで置換する。次にバルブ３を閉じ４を
開け、真空ポンプ12で容器バルブ７から真空ポンプ12に
至る配管等を真空にし、バルブ２を閉じ容器バルブ７を
徐々に開き大気圧以下で試料計量管14に試料ガスを導入
する。このとき真空計13で正確に試料導入圧を読み取
り、試料の採取量を決定する。次に、六方切換バルブ６
を切り替え、ガスクロマトグラムのキャリアーガスによ
って試料ガスを押し流し、ヒーター９によって加熱され
いてる二フッ化コバルトが充填された管８に導き、フッ
素を固定化除去する。このとき不純物ガスはキャリアー
ガスによって同伴され、ガスクロマトグラフ10に導入さ
れる。ガスクロマトグラム10に導入された不純物ガスは
ガスクロ充填剤が充填されたカラムで分離され、熱伝導
度検出器で検出される。予め同様な操作で分析した標準
ガスのピーク面積と試料ガスの不純物ガスのピーク面積
を比較することによって不純物ガスの濃度を知ることが
できる。EXAMPLE An actual analysis method of the present invention will be described more specifically below with reference to FIG. 1 showing an apparatus used in the analysis method of the present invention. First, after connecting the sample container 11, the container valve 7
Confirm that the valve is closed, open valves 1 to 3, close 4 and set the hexagonal switching valve 6 to the state shown in FIG. 1, and flow helium gas from the pipe extending from the valve 5 to the pipe through which fluorine passes and the valve. Replace air components and other components that give a positive error in the analysis with helium. Next, the valve 3 is closed and the valve 4 is opened, the pipes from the container valve 7 to the vacuum pump 12 are evacuated by the vacuum pump 12, the valve 2 is closed, and the container valve 7 is gradually opened. Introduce gas. At this time, the sample introduction pressure is accurately read by the vacuum gauge 13 to determine the sampling amount of the sample. Next, the hexagonal switching valve 6
And the sample gas is swept away by the carrier gas of the gas chromatogram and guided to the tube 8 filled with cobalt difluoride heated by the heater 9 to immobilize and remove the fluorine. At this time, the impurity gas is entrained by the carrier gas and introduced into the gas chromatograph 10. The impurity gas introduced into the gas chromatogram 10 is separated by a column filled with a gas chromatographic filler and detected by a thermal conductivity detector. The concentration of the impurity gas can be known by comparing the peak area of the standard gas and the peak area of the impurity gas of the sample gas, which are previously analyzed by the same operation.
【０００７】[0007]
【発明の効果】以上述べた様に、本発明の分析方法およ
び分析装置を用いれば、フッ素ガス中の水素、酸素、窒
素、一酸化炭素、二酸化炭素、その他の不純物ガスの分
析を簡便かつ精度良く行うことが可能である。As described above, by using the analysis method and the analysis apparatus of the present invention, the analysis of hydrogen, oxygen, nitrogen, carbon monoxide, carbon dioxide and other impurity gases in fluorine gas can be carried out easily and accurately. It can be done well.
【図１】 本発明のフッ素ガス中の不純物ガスの分析装
置を示す図である。FIG. 1 is a diagram showing an analyzer for impurity gas in fluorine gas according to the present invention.
１〜５ バルブ ６ 六方切換バルブ ７ 容器バルブ ８ 金属フッ化物が充填された管 ９ 加熱ヒーター 10 ガスクロマトグラフ 11 試料容器 12 真空ポンプ 13 真空計 14 試料計量管 1 to 5 valves 6 hexagonal switching valve 7 container valve 8 metal fluoride filled tube 9 heating heater 10 gas chromatograph 11 sample container 12 vacuum pump 13 vacuum gauge 14 sample measuring tube
───────────────────────────────────────────────────── フロントページの続き (72)発明者 武藤 忠彦 群馬県渋川市1497番地 関東電化工業株式 会社渋川工場内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Tadahiko Muto 1497 Shibukawa City Gunma Prefecture Kanto Denka Kogyo Co., Ltd. Shibukawa Factory
Claims (2)
フッ化物充填層に通し、フッ素ガスを固定化除去した
後、ガスクロマトグラフにより分析することを特徴とす
るフッ素ガス中の不純物ガスの分析方法。1. A method for analyzing an impurity gas in a fluorine gas, which comprises passing a fluorine gas containing an impurity gas through a metal fluoride packed layer to fix and remove the fluorine gas, and then analyzing the gas by a gas chromatograph.
が可能な六方切換バルブに一定容量のサンプルが分取で
きる試料計量管が付いたガスサンプラー、金属フッ化物
が充填された管、およびガスクロマトグラフが順次配管
により連結され、キャリアーガスがガスサンプラー、金
属フッ化物が充填された管、ガスクロマトグラフの順で
流れるよう配管されたフッ素ガス中の不純物ガスの分析
装置。2. A gas sampler equipped with a hexagonal switching valve capable of switching a flow path of a carrier gas and a sample measuring tube capable of collecting a fixed volume of sample, a tube filled with metal fluoride, and a gas chromatograph. An analyzer for impurity gas in fluorine gas, which is connected by sequential pipes and in which the carrier gas is piped in the order of a gas sampler, a pipe filled with metal fluoride, and a gas chromatograph.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP07867094A JP3339962B2 (en) | 1994-04-18 | 1994-04-18 | Method and apparatus for analyzing impurity gas in fluorine gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP07867094A JP3339962B2 (en) | 1994-04-18 | 1994-04-18 | Method and apparatus for analyzing impurity gas in fluorine gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07287001A true JPH07287001A (en) | 1995-10-31 |
| JP3339962B2 JP3339962B2 (en) | 2002-10-28 |
Family
ID=13668310
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP07867094A Expired - Lifetime JP3339962B2 (en) | 1994-04-18 | 1994-04-18 | Method and apparatus for analyzing impurity gas in fluorine gas |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3339962B2 (en) |
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| WO2003002454A3 (en) * | 2001-06-29 | 2003-05-30 | Showa Denko Kk | High-purity fluorine gas, production and use thereof, and method for analyzing trace impurities in high-purity fluorine gas |
| JP2007057371A (en) * | 2005-08-24 | 2007-03-08 | Showa Denko Kk | Quantitative analyzing method of gas component contained in fluorine gas and quantitative analyzer used therein |
| KR101025748B1 (en) * | 2009-03-03 | 2011-04-04 | (주)원익머트리얼즈 | Analysis equipment of impurities for fluorine gas |
| WO2011045338A1 (en) * | 2009-10-16 | 2011-04-21 | Solvay Fluor Gmbh | High-purity fluorine gas, the production and use thereof, and a method for monitoring impurities in a fluorine gas |
| JP4699377B2 (en) * | 2004-09-30 | 2011-06-08 | 昭和電工株式会社 | Trace component analysis method and analyzer |
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| CN114814039A (en) * | 2022-05-24 | 2022-07-29 | 福建德尔科技股份有限公司 | Method for analyzing content of impurities in fluorine gas |
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| WO2003002454A3 (en) * | 2001-06-29 | 2003-05-30 | Showa Denko Kk | High-purity fluorine gas, production and use thereof, and method for analyzing trace impurities in high-purity fluorine gas |
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