JP3220791B2 - Organometallic compound detector - Google Patents
Organometallic compound detectorInfo
- Publication number
- JP3220791B2 JP3220791B2 JP06738998A JP6738998A JP3220791B2 JP 3220791 B2 JP3220791 B2 JP 3220791B2 JP 06738998 A JP06738998 A JP 06738998A JP 6738998 A JP6738998 A JP 6738998A JP 3220791 B2 JP3220791 B2 JP 3220791B2
- Authority
- JP
- Japan
- Prior art keywords
- organometallic compound
- color
- agent
- phenosafuranine
- detecting agent
- 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 - Lifetime
Links
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、有機金属化合物の
検知剤に関し、詳しくは、半導体製造工場等で使用され
ている有機金属化合物の漏洩の検知や、除害剤の破過の
検知、あるいは、除害装置の運転状況の確認等を行うた
めに用いる検知剤に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an organometallic compound detection agent, and more particularly, to the detection of leakage of an organometallic compound used in a semiconductor manufacturing plant or the like, the detection of breakthrough of an abatement agent, or The present invention relates to a detection agent used for confirming an operation state of an abatement apparatus.
【０００２】[0002]
【従来の技術及び発明が解決しようとする課題】有機金
属化合物は、悪臭や燃焼性だけでなく、毒性も有してい
るため、装置等からの漏洩の有無や排ガスの除害処理の
状況等を確認する必要がある。有機金属化合物の検知方
法として、例えば、除害処理後の排ガスを硝酸等の水溶
液中にバブリングさせて排ガス中の金属分を水溶液中に
捕捉し、この金属分の濃度をプラズマ発光分光分析計
（ＩＣＰ）で定量する方法が一般的に行われている。こ
の方法は、有機金属化合物の濃度を正確に測定すること
ができるが、ＩＣＰ分析は、非常に手間と時間とを要す
るという問題がある。2. Description of the Related Art Since organometallic compounds have not only bad smell and flammability but also toxicity, the presence or absence of leakage from equipment or the like and the status of detoxification treatment of exhaust gas are required. Need to check. As a method for detecting an organic metal compound, for example, the exhaust gas after the detoxification treatment is bubbled into an aqueous solution of nitric acid or the like to capture the metal component in the exhaust gas in the aqueous solution, and the concentration of the metal component is measured by a plasma emission spectrometer ( A method of quantification by ICP) is generally used. Although this method can accurately measure the concentration of the organometallic compound, there is a problem that the ICP analysis requires much labor and time.
【０００３】一方、各種有害ガスの有無を簡便に検知す
る一手段として、特定のガスに接触すると変色する検知
剤が使用されてきている。例えば、特許第２５９６８１
５号公報には、第二銅塩と金塩との混合物を変色成分と
し、テトラメチル錫等の金属アルキル化合物に接触する
と、レモン色から紫色乃至黒色に変色する検知剤が記載
されている。この検知剤は、他に、一酸化炭素や金属カ
ルボニル化合物、シラン，アルシン，ホスフィン等の揮
発性無機水素化物等と接触しても、レモン色から紫色乃
至黒色に変色する。[0003] On the other hand, as one means for easily detecting the presence or absence of various harmful gases, a detection agent that changes color when it comes into contact with a specific gas has been used. For example, Japanese Patent No. 259681
No. 5 describes a detection agent which uses a mixture of a cupric salt and a gold salt as a color-changing component and changes color from lemon to purple to black when contacted with a metal alkyl compound such as tetramethyltin. In addition, this detecting agent changes its color from lemon to purple or black even when it comes into contact with carbon monoxide, metal carbonyl compounds, volatile inorganic hydrides such as silane, arsine, and phosphine.
【０００４】しかし、金塩を使用する場合、金塩の混合
量が多いと検知剤自体の色が褐色となり、変色の確認が
困難になる。また、測定対象となるガス、例えば排ガス
中にアンモニアが含まれていると、アンモニアとの接触
によって変色するため、有機金属化合物との接触による
変色の確認が困難になることがある。したがって、Ｇａ
Ｎ半導体基板の製造のように、有機金属化合物とアンモ
ニアとを用いる場合は、有機金属化合物の検知剤として
最適なものであるとはいえなかった。However, when gold salt is used, if the amount of gold salt mixed is large, the color of the detection agent itself becomes brown, making it difficult to confirm discoloration. In addition, if ammonia is contained in a gas to be measured, for example, exhaust gas, the color is changed by contact with ammonia, so that it may be difficult to confirm the color change by contact with the organometallic compound. Therefore, Ga
When an organometallic compound and ammonia are used as in the production of an N-semiconductor substrate, it cannot be said that the composition is optimal as a detecting agent for the organometallic compound.
【０００５】そこで本発明は、単一の成分で金属アルキ
ル化合物や金属アルコキシドのような有機金属化合物を
検知することができ、アンモニアが共存する場合でも変
色の確認を容易に行える検知剤を提供することを目的と
している。Accordingly, the present invention provides a detecting agent which can detect an organometallic compound such as a metal alkyl compound or a metal alkoxide with a single component and can easily confirm discoloration even in the presence of ammonia. It is intended to be.
【０００６】[0006]
【課題を解決するための手段】上記目的を達成するた
め、本発明の有機金属化合物の検知剤は、有機化合物で
あるフェノサフラニンを変色成分とするものであって、
特に、前記フェノサフラニンを、担持量が０．１〜０．
５重量％となるように担体に担持させたことを特徴とし
ている。Means for Solving the Problems To achieve the above object, the organometallic compound detecting agent of the present invention comprises phenosafuranine, an organic compound, as a color-changing component,
In particular, the loading amount of the phenosafuranine is 0.1 to 0.1.
It is characterized in that it is supported on a carrier so as to be 5% by weight.
【０００７】本発明において除害対象となる前記有機金
属化合物としては、トリメチルアルミニウム，トリエチ
ルアルミニウム，トリメチルガリウム，トリエチルガリ
ウム，ジメチル亜鉛，ジエチル亜鉛，トリメチルインジ
ウム，トリエチルインジウム，テトラメチル錫，テトラ
エチル錫，ターシャリーブチルホスフィン，トリメチル
アルシン，トリエチルアルシン，ターシャリーブチルア
ルシン等の金属アルキル化合物や、テトラメトキシシラ
ン，テトラエトキシシラン，トリメトキシホスフィン，
トリエトキシホスフィン，トリメトキシアルシン，トリ
エトキシアルシン，ペンタエトキシタンタル等の金属ア
ルコキシドを挙げることができる。[0007] In the present invention, the organometallic compounds to be harmed include trimethylaluminum, triethylaluminum, trimethylgallium, triethylgallium, dimethylzinc, diethylzinc, trimethylindium, triethylindium, tetramethyltin, tetraethyltin, and tersha. Metal alkyl compounds such as tributyl phosphine, trimethyl arsine, triethyl arsine, and tertiary butyl arsine; tetramethoxysilane, tetraethoxysilane, trimethoxyphosphine,
Examples thereof include metal alkoxides such as triethoxyphosphine, trimethoxyarsine, triethoxyarsine, and pentaethoxytantalum.
【０００８】検知剤の変色成分となるフェノサフラニン
（Ｃ１８Ｈ１５Ｎ４Ｃｌ：３，７−ジアミノ−５−フェ
ニルフェナジニウムクロライド）は、減感色素の一種
で、写真感光材料用乳剤及び処理液添加剤として使用さ
れ、また、生体組織の染色用としても使用されるもので
あって、通常は緑色柱状晶の固体であり、担体に適当量
を担持させるとピンク色の外観となる。このフェノサフ
ラニンは、有機金属化合物に接触すると紫色に変色する
が、アンモニアに接触しても変色することはない。Phenosafranine (C 18 H 15 N 4 Cl: 3,7-diamino-5-phenylphenazinium chloride), which is a discoloring component of the detecting agent, is a kind of desensitizing dye and is used as an emulsion for photographic materials and It is used as a treatment liquid additive, and is also used for staining living tissue. Usually, it is a green columnar solid and has a pink appearance when an appropriate amount is supported on a carrier. This phenosafuranin changes color to purple when it comes into contact with the organometallic compound, but does not change color when it comes into contact with ammonia.
【０００９】フェノサフラニンを有機金属化合物の検知
剤として使用する際には、適宜な担体に担持させて使用
することが好ましい。担体としては、シリカゲル，アル
ミナ，珪藻土等、様々なものを使用することができる
が、白色のものが好ましく、中でも、一般に乾燥剤（吸
湿剤）として広く流通しているシリカゲルが最適であ
る。When phenosafuranine is used as a detecting agent for an organometallic compound, it is preferable to use it by supporting it on a suitable carrier. Various carriers such as silica gel, alumina, and diatomaceous earth can be used as the carrier, but white ones are preferred. Among them, silica gel, which is generally widely distributed as a desiccant (hygroscopic agent), is most suitable.
【００１０】フェノサフラニンを担体に担持させる手順
は任意であり、例えば、フェノサフラニンを水に溶解
し、これに担体を浸漬するなどの従来から行われている
方法で行うことができる。[0010] The procedure for supporting phenosafuranine on a carrier is optional. For example, phenosafuranin can be carried out by a conventional method such as dissolving phenosafuranin in water and immersing the carrier in the solution.
【００１１】そして、フェノサフラニンを担体に担持さ
せて使用する場合は、その担持量を０．１〜０．５重量
％にすることが好ましい。担持量が多くなると濃い赤紫
色になり、有機金属化合物に接触した際の紫色への変色
が判別し難くなる。逆に、担持量が少なくなると白に近
いピンク色になり、有機金属化合物に接触してもほとん
ど変色が認められなくなる。When phenosafuranine is supported on a carrier, the amount of phenosafuranin is preferably 0.1 to 0.5% by weight. When the supported amount increases, the color becomes deep reddish purple, and it becomes difficult to distinguish the color change to purple upon contact with the organometallic compound. Conversely, when the supported amount decreases, the color becomes pink close to white, and almost no discoloration is observed even when the organic metal compound is brought into contact.
【００１２】ガス中の有機金属化合物の検知を行う際に
は、従来のこの種の検知剤と同様に、少なくとも一部が
透明な筒体（カラム）内に前記検知剤を充填し、このカ
ラム内に適当な流速で検知対象ガス、例えば除害処理後
の排ガスを流通させればよい。When detecting an organometallic compound in a gas, as in the case of a conventional detection agent of this type, at least a part of the detection agent is filled in a transparent cylinder (column). The gas to be detected, for example, the exhaust gas after the detoxification treatment, may be circulated at an appropriate flow rate.
【００１３】[0013]
【実施例】実施例１ 市販のフェノサフラニン０．０４ｇを水４０ｍｌに溶解
し、シリカゲル（富士シリシア製キャリアクト１００）
４０ｇに浸した後、真空乾燥してピンク色の検知剤を得
た（フェノサフラニンの担持量０．１重量％）。この検
知剤を内径４３ｍｍのガラス製カラムに充填し、カラム
内を窒素ガスでパージした後、以下に示す有機金属化合
物をそれぞれ３０ｐｐｍ含有する窒素ガスを空塔速度５
ｍ／ｓｅｃで導入し、変色状況を観察した。その結果を
以下に示す。Example 1 Commercially available 0.04 g of phenosafranine was dissolved in 40 ml of water, and silica gel (Carrierct 100 manufactured by Fuji Silysia) was dissolved.
After immersion in 40 g, it was vacuum-dried to obtain a pink detecting agent (amount of fenosafranine supported: 0.1% by weight). This detection agent was packed in a glass column having an inner diameter of 43 mm, and the inside of the column was purged with nitrogen gas.
It was introduced at m / sec, and the discoloration state was observed. The results are shown below.
【００１４】 [0014]
【００１５】また、トリエチルガリウムやトリエトキシ
ホスフィンでも同様の操作を行ったが、上記同様の変色
が認められた。The same operation was carried out with triethylgallium and triethoxyphosphine, but the same discoloration was observed.
【００１６】実施例２ 実施例１と同じ検知剤を同じガラス製カラム内に充填
し、カラム内を窒素ガスでパージした後、アンモニア１
０％を含む窒素ガスを空塔速度１ｍ／ｓｅｃで導入し
た。その結果、２４時間経過しても検知剤の変色は観察
されなかった。続けて、実施例と同じ条件で有機金属化
合物含有窒素ガスをそれぞれ導入したところ、実施例１
と同様に、約５分でピンク色から紫色にそれぞれ変色し
た。Example 2 The same detecting agent as in Example 1 was filled in the same glass column, and the column was purged with nitrogen gas.
Nitrogen gas containing 0% was introduced at a superficial velocity of 1 m / sec. As a result, no discoloration of the detection agent was observed even after 24 hours. Subsequently, nitrogen gas containing an organometallic compound was introduced under the same conditions as in the example.
Similarly, the color changed from pink to purple in about 5 minutes.
【００１７】実施例３ フェノサフラニンの担持量が０．０２重量％及び１．０
重量％となるように調整したそれぞれの検知剤に、実施
例１と同じ条件でトリメチルインジウムを含有する窒素
ガスを流通させた。その結果、０．０２重量％のもの
は、もともと薄いピンク色であり、変色の確認が困難で
あった。また、１．０重量％のものは、約５分後に赤紫
色から紫色に変色したが、これも変色の確認は困難であ
った。Example 3 The loading amount of phenosafuranine was 0.02% by weight and 1.0%.
Under the same conditions as in Example 1, nitrogen gas containing trimethylindium was allowed to flow through each of the detection agents adjusted to be in% by weight. As a result, the one with 0.02% by weight was originally light pink, and it was difficult to confirm discoloration. In the case of 1.0% by weight, the color changed from reddish purple to purple after about 5 minutes, but it was also difficult to confirm the color change.
【００１８】[0018]
【発明の効果】以上説明したように、本発明の有機金属
化合物の検知剤によれば、アンモニアと共存している場
合であっても、微量の有機金属化合物を確実に検知する
ことができ、除害処理の状況、例えば除害剤の破過を簡
便に確認できる。As described above, according to the organometallic compound detecting agent of the present invention, a trace amount of an organometallic compound can be reliably detected even when coexisting with ammonia. The status of the abatement treatment, for example, breakthrough of the abatement agent can be easily confirmed.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7，ＤＢ名) G01N 31/22 G01N 31/00 ──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int.Cl. 7 , DB name) G01N 31/22 G01N 31/00
Claims (3)
を特徴とする有機金属化合物の検知剤。1. An organometallic compound detecting agent comprising phenosafuranine as a discoloring component.
るとともに、その担持量を０．１〜０．５重量％とした
ことを特徴とする請求項１記載の有機金属化合物の検知
剤。2. The detecting agent for an organometallic compound according to claim 1, wherein the phenosafuranine is supported on a carrier, and the supported amount is 0.1 to 0.5% by weight.
ニアと共存していることを特徴とする請求項１又は２記
載の有機金属化合物の検知剤。3. The organometallic compound detecting agent according to claim 1, wherein the organometallic compound to be detected coexists with ammonia.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP06738998A JP3220791B2 (en) | 1998-03-17 | 1998-03-17 | Organometallic compound detector |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP06738998A JP3220791B2 (en) | 1998-03-17 | 1998-03-17 | Organometallic compound detector |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH11264815A JPH11264815A (en) | 1999-09-28 |
| JP3220791B2 true JP3220791B2 (en) | 2001-10-22 |
Family
ID=13343589
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP06738998A Expired - Lifetime JP3220791B2 (en) | 1998-03-17 | 1998-03-17 | Organometallic compound detector |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3220791B2 (en) |
-
1998
- 1998-03-17 JP JP06738998A patent/JP3220791B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH11264815A (en) | 1999-09-28 |
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