JP2014186026A - Method for analyzing trace impurity, and plasma torch for use in the analysis - Google Patents
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Abstract
Description
本発明は、有機金属化合物を不活性な有機溶媒で希釈した試料液体に含まれる微量不純物を分析する方法、及び当該分析に用いるプラズマトーチに関する。 The present invention relates to a method for analyzing trace impurities contained in a sample liquid obtained by diluting an organometallic compound with an inert organic solvent, and a plasma torch used for the analysis.
従来、有機金属化合物の不純物の分析方法としては、例えば、有機金属化合物を炭化水素などで希釈させた後、酸を用いて有機金属化合物を分解させた上で、誘導結合型プラズマ発光分析法により分析する方法が知られている（例えば、特許文献１〜２参照）。 Conventionally, as a method for analyzing impurities in an organometallic compound, for example, after diluting the organometallic compound with a hydrocarbon or the like, the organometallic compound is decomposed with an acid and then inductively coupled plasma emission spectrometry is used. Methods for analysis are known (see, for example, Patent Documents 1 and 2).
ところで、誘導結合型プラズマ発光分析法により、有機溶媒を含む試料を分析する場合には、キャリアガス管の先端部分に不純物（例えば、黒鉛など）が付着して目詰まりを起こしてしまうなどの不具合が生じていた。
これを解決するために、プラズマガスの流量を調節することにより、プラズマ炎によりキャリアガス管先端部の黒鉛を燃焼させる方法（例えば、特許文献３参照）、脱溶媒機能を備えたプラズマトーチを使用する方法（例えば、特許文献４参照）やプラズマ炎に接する部分又はその近傍を保護具で覆う方法（例えば、特許文献５参照）が提案されている。
By the way, when analyzing a sample containing an organic solvent by inductively coupled plasma optical emission spectrometry, impurities (for example, graphite, etc.) adhere to the tip of the carrier gas tube and cause clogging. Has occurred.
In order to solve this, a method of burning the graphite at the tip of the carrier gas pipe with a plasma flame by adjusting the flow rate of the plasma gas (see, for example, Patent Document 3), a plasma torch having a desolvation function is used. And a method of covering a portion in contact with a plasma flame or the vicinity thereof with a protective device (for example, see Patent Literature 5).
しかしながら、特許文献３の方法では、プラズマ炎とキャリアガス管先端部とが近づくことによりキャリアガス管先端部が融解、燃焼などしてしまうという問題があった。
また、特許文献４の方法では、脱溶媒機能として透過材を使用しているものの、溶媒に含まれる有機金属化合物の分解物が目詰まりを起こす恐れがあった。
また、特許文献５の方法では、改めて保護具を装着・脱着しなければならず、煩雑な操作が生じていた。
However, the method of Patent Document 3 has a problem that the carrier gas tube tip is melted and burned when the plasma flame approaches the carrier gas tube tip.
Further, in the method of Patent Document 4, although a permeable material is used as a solvent removal function, the decomposition product of the organometallic compound contained in the solvent may cause clogging.
Moreover, in the method of Patent Document 5, the protective equipment has to be attached / removed again, and a complicated operation has occurred.
以上のように、有機溶媒を含む試料を誘導結合型プラズマ発光分析法により分析する際の問題は完全には解決されておらず、より簡易な方法が求められていた。また、有機金属化合物を不活性な有機溶媒で希釈した試料液体の誘導結合型プラズマ発光分析法を用いた分析に関しては、何ら開示がなされていなかった。 As described above, the problem in analyzing a sample containing an organic solvent by inductively coupled plasma optical emission spectrometry has not been completely solved, and a simpler method has been demanded. In addition, no disclosure has been made regarding the analysis of a sample liquid obtained by diluting an organometallic compound with an inert organic solvent using an inductively coupled plasma emission spectrometry.
また、漠然とキャリアガス管の先端部がプラズマガス管の先端部に対して下部に位置するプラズマトーチが記載されている図面を有する公報が存在するものの、プラズマガス管の内径やプラズマガス管の先端部とキャリアガス管の先端部の長さに着目して、その比率を詳細に制御することは一切なされていなかった。 Further, although there is a publication having a drawing in which a plasma torch is described in which the tip of the carrier gas tube is positioned below the tip of the plasma gas tube, the inside diameter of the plasma gas tube or the tip of the plasma gas tube exists. Focusing on the length of the tip of the carrier gas pipe and the carrier gas pipe, the ratio has not been controlled in detail.
本発明の課題は、即ち、誘導結合型プラズマ発光分析法により、プラズマ炎の位置やキャリアガスの流速の微調整をすることなく、簡便な操作にて、有機金属化合物を不活性な有機溶媒で希釈した試料液体に含まれる微量不純物を感度良く分析する方法、及び当該分析に用いるプラズマトーチを提供することにある。 An object of the present invention is that an organometallic compound can be removed from an inert organic solvent by a simple operation without fine adjustment of the position of the plasma flame or the flow rate of the carrier gas by inductively coupled plasma optical emission spectrometry. It is an object to provide a method for analyzing trace impurities contained in a diluted sample liquid with high sensitivity, and a plasma torch used for the analysis.
本発明の課題は、又、本発明の分析方法によって、有機金属化合物の品質を管理することにもある。 Another object of the present invention is to control the quality of the organometallic compound by the analysis method of the present invention.
本発明の課題は、有機金属化合物を不活性な有機溶媒で希釈した試料液体を霧化させた後、
プラズマガス管、及びその内側にキャリアガス管を備え、キャリアガス管の先端部がプラズマガス管の先端部に対して下部に位置するプラズマトーチであって、
プラズマガス管の内径をＲ（ｍｍ）、
プラズマガス管の先端部とキャリアガス管の先端部の長さをＬ（ｍｍ）
とした場合において、
（Ｒ／Ｌ）×１００
が２０％〜４０％であるプラズマトーチに、
前記霧化させた試料をキャリアガスとともにキャリアガス管を通じてプラズマトーチに導入して、誘導結合型プラズマ発光分析法により試料液体中の微量不純物を分析する方法によって解決される。
An object of the present invention is to atomize a sample liquid obtained by diluting an organometallic compound with an inert organic solvent,
A plasma torch comprising a plasma gas tube and a carrier gas tube inside thereof, the tip of the carrier gas tube being located below the tip of the plasma gas tube,
The inner diameter of the plasma gas tube is R (mm),
The length of the tip of the plasma gas tube and the tip of the carrier gas tube is L (mm)
If
(R / L) × 100
Is a plasma torch with 20% to 40%,
This is solved by introducing the atomized sample together with a carrier gas into a plasma torch through a carrier gas tube, and analyzing trace impurities in the sample liquid by inductively coupled plasma emission spectrometry.
本発明により、プラズマ炎の位置やキャリアガスの流速の微調整をすることなく、簡便な操作にて、有機金属化合物を不活性な有機溶媒で希釈した試料液体に含まれる微量不純物を感度良く分析する方法を提供することができる。 According to the present invention, a small amount of impurities contained in a sample liquid obtained by diluting an organometallic compound with an inert organic solvent can be analyzed with high sensitivity by a simple operation without fine adjustment of the position of the plasma flame or the flow rate of the carrier gas. A method can be provided.
（プラズマトーチ）
本発明において使用するプラズマトーチは、プラズマガス管、及びその内側にキャリアガス管を備え、キャリアガス管の先端部がプラズマガス管の先端部に対して下部に位置するプラズマトーチであって、
プラズマガス管の内径をＲ（ｍｍ）、
プラズマガス管の先端部とキャリアガス管の先端部の長さをＬ（ｍｍ）
とした場合において、
（Ｒ／Ｌ）×１００
が２０％〜４０％であるプラズマトーチである（図１）。
即ち、プラズマガス管の内径に対して２０〜４０％の長さ分だけキャリアガス管の先端部がプラズマガス管の先端部に対して下部に位置するプラズマトーチである。
(Plasma torch)
The plasma torch used in the present invention is a plasma torch comprising a plasma gas tube and a carrier gas tube inside thereof, the tip of the carrier gas tube being located below the tip of the plasma gas tube,
The inner diameter of the plasma gas tube is R (mm),
The length of the tip of the plasma gas tube and the tip of the carrier gas tube is L (mm)
If
(R / L) × 100
Is a plasma torch with 20% to 40% (FIG. 1).
That is, this is a plasma torch in which the tip of the carrier gas tube is positioned below the tip of the plasma gas tube by a length of 20 to 40% with respect to the inner diameter of the plasma gas tube.
なお、本発明においては、前記プラズマトーチを備えた誘導結合型プラズマ発光分析装置を用いて試料液体中の微量不純物の分析を行う。 In the present invention, trace impurities in the sample liquid are analyzed using an inductively coupled plasma emission analyzer equipped with the plasma torch.
（微量不純物の分析）
本発明の分析方法は、有機金属化合物を不活性な有機溶媒で希釈した試料液体を霧化させた後、前記のプラズマトーチを備えた誘導結合型プラズマ発光分析装置を用いて、霧化させた試料をキャリアガスとともにキャリアガス管を通じてプラズマトーチに導入することによって、試料液体中の微量不純物を感度良く分析することができる。このとき、プラズマ炎の位置やキャリアガスの流速の微調整は特段必要としない。
(Analysis of trace impurities)
According to the analysis method of the present invention, a sample liquid obtained by diluting an organometallic compound with an inert organic solvent is atomized, and then atomized using the inductively coupled plasma emission spectrometer equipped with the plasma torch. By introducing the sample together with the carrier gas into the plasma torch through the carrier gas tube, it is possible to analyze trace impurities in the sample liquid with high sensitivity. At this time, fine adjustment of the position of the plasma flame and the flow rate of the carrier gas is not particularly required.
本発明における有機金属化合物とは、金属と炭素とが直接化学結合している化合物（例えば、アルキル金属等）のみならず、酸素やリン等のヘテロ原子を介してできる広義の有機金属化合物（例えば、金属−アセチルアセトナト錯体、金属−アミド錯体、金属−アルコキシ錯体等）を含み、純度が９９．９％以上である、例えば、トリメチルガリウム、トリエチルガリウム等の有機ガリウム化合物；トリメチルアルミニウム、トリエチルアルミニウム等の有機アルミニウム化合物；トリメチルインジウム等の有機インジウム化合物；ジメチル亜鉛、ジエチル亜鉛等の有機亜鉛化合物；ジエチルマグネシウム、ビス（シクロペンタジエニル）マグネシウム、ビス（メチルシクロペンタジエニル）マグネシウム等の有機マグネシウム化合物が好適に適用される。 The organometallic compound in the present invention is not only a compound in which a metal and carbon are directly chemically bonded (for example, an alkyl metal), but also a broadly defined organometallic compound (for example, an oxygen or phosphorus hetero atom) (for example, A metal-acetylacetonato complex, metal-amide complex, metal-alkoxy complex, etc.) and having a purity of 99.9% or more, for example, organic gallium compounds such as trimethylgallium and triethylgallium; trimethylaluminum, triethylaluminum Organo aluminum compounds such as trimethylindium; Organo zinc compounds such as dimethyl zinc and diethyl zinc; Organo magnesium such as diethyl magnesium, bis (cyclopentadienyl) magnesium and bis (methylcyclopentadienyl) magnesium Preferred compound It is applied.
本発明における不活性な有機溶媒としては、例えば、ペンタン、ヘキサン、ヘプタン、オクタン、シクロヘキサン、シクロヘプタン、シクロオクタン等の飽和脂肪族炭化水素類（各種異性体を含む）；ペンテン、ヘキセン、ヘプテン、オクテン、シクロヘキセン、シクロヘプテン、シクロオクテン等の不飽和脂肪族炭化水素類（各種異性体を含む）；ベンゼン、トルエン、キシレン等の芳香族炭化水素類（各種異性体を含む）が使用されるが、好ましくは芳香族炭化水素類、更に好ましくはトルエン、キシレンが使用される。なお、これらの有機溶媒は単独又は二種以上を混合して使用しても良い。 Examples of the inert organic solvent in the present invention include saturated aliphatic hydrocarbons (including various isomers) such as pentane, hexane, heptane, octane, cyclohexane, cycloheptane, and cyclooctane; pentene, hexene, heptene, Unsaturated aliphatic hydrocarbons (including various isomers) such as octene, cyclohexene, cycloheptene, and cyclooctene; aromatic hydrocarbons (including various isomers) such as benzene, toluene, and xylene are used. Preferably aromatic hydrocarbons are used, more preferably toluene and xylene. In addition, you may use these organic solvents individually or in mixture of 2 or more types.
前記有機溶媒の使用量は、高純度有機金属化合物を実質的に溶解させる量ならば特に制限されず、有機溶媒の種類により適宜決定する。 The amount of the organic solvent used is not particularly limited as long as it is an amount capable of substantially dissolving the high-purity organometallic compound, and is appropriately determined depending on the type of the organic solvent.
本発明の有機金属化合物を不活性な有機溶媒で希釈した試料液体とは、前記有機金属化合物と、有機金属化合物と不活性な有機溶媒とを混合した試料液体を示すが、有機金属化合物を不活性な有機溶媒で希釈したものに、酸に加えた後に有機金属化合物を分解させたものや、酸で分解した後に分液操作により水層を除いたものをも含むものとする。 The sample liquid obtained by diluting the organometallic compound of the present invention with an inert organic solvent refers to a sample liquid obtained by mixing the organometallic compound, the organometallic compound, and the inert organic solvent. Those diluted with an active organic solvent include those obtained by decomposing an organometallic compound after being added to an acid, and those obtained by decomposing with an acid and removing the aqueous layer by a liquid separation operation.
前記試料液体を霧化させる方法としては、誘導結合型プラズマ発光分析装置に付属している霧化・噴霧手段をそのまま適用できる。また、霧化させた試料はキャリアガスとともにキャリアガス管を通じてプラズマトーチに導入される。この際のキャリアガスの流速は適宜調節するが、好ましくは０．４〜０．７Ｌ／ｍｉｎ．である。 As a method for atomizing the sample liquid, the atomization / spraying means attached to the inductively coupled plasma emission spectrometer can be applied as it is. The atomized sample is introduced into the plasma torch through the carrier gas tube together with the carrier gas. The flow rate of the carrier gas at this time is adjusted as appropriate, but is preferably 0.4 to 0.7 L / min. It is.
更に、誘導結合型プラズマ発光分析法に導入された試料液体はプラズマ炎により発光することにより、試料液体中の微量不純物を分析することができる。 Furthermore, the sample liquid introduced into the inductively coupled plasma optical emission analysis method emits light with a plasma flame, so that trace impurities in the sample liquid can be analyzed.
この方法で分析された有機金属化合物の微量不純物量は、感度良く分析されたものであるため、その分析値をもって有機金属化合物の品質管理が可能である。 Since the trace amount of impurities of the organometallic compound analyzed by this method is analyzed with high sensitivity, the quality control of the organometallic compound can be performed with the analysis value.
以下、実施例及び比較例を挙げて本発明を具体的に説明するが、本発明は以下の実施例に限定されるものではない。 EXAMPLES Hereinafter, although an Example and a comparative example are given and this invention is demonstrated concretely, this invention is not limited to a following example.
実施例１（プラズマトーチの作成、及びトリメチルアルミニウムの分析）
誘導結合型プラズマ発光分析装置からプラズマトーチを取り外すことなく、プラズマガス管の内径を測定したところ１４ｍｍ（Ｌ）であった。次いで、キャリアガス管の先端部が、プラズマガス管の先端部より３ｍｍ（Ｒ）下部となるように、キャリアガス管を設置した（（Ｒ／Ｌ）×１００＝２１％）。
トリメチルアルミニウム５ｇ及びキシレン３０ｍｌを混合した後、窒素雰囲気にて、塩酸６０ｍｌ中にゆるやかに滴下して、トリメチルアルミニウムを分解した。その後、分液してトリメチルアルミニウム中の微量不純物を分析するための試料液体（キシレン層）を調製した。
次いで、この試料液体を前記誘導結合型プラズマ分析装置で分析したところ、キャリアガス管の先端部には何ら付着は観られなかった。
Example 1 (Preparation of plasma torch and analysis of trimethylaluminum)
When the inner diameter of the plasma gas tube was measured without removing the plasma torch from the inductively coupled plasma optical emission spectrometer, it was 14 mm (L). Next, the carrier gas pipe was installed so that the tip of the carrier gas pipe was 3 mm (R) below the tip of the plasma gas pipe ((R / L) × 100 = 21%).
After mixing 5 g of trimethylaluminum and 30 ml of xylene, it was slowly dropped into 60 ml of hydrochloric acid in a nitrogen atmosphere to decompose trimethylaluminum. Thereafter, liquid separation was performed to prepare a sample liquid (xylene layer) for analyzing trace impurities in trimethylaluminum.
Next, when this sample liquid was analyzed by the inductively coupled plasma analyzer, no adhesion was observed at the tip of the carrier gas tube.
比較例１（トリメチルアルミニウムの分析）
実施例１において、プラズマトーチにおけるキャリアガス管の位置を変更せず、キャリアガス管の先端部とプラズマガス管の先端部の位置が同じ高さのプラズマトーチを用いて、実施例１と同様にトリメチルアルミニウムの分析を行った（（Ｒ／Ｌ）×１００＝０％）。その結果、キャリアガス管先端部には黒色の不純物の付着が観られた。
当該不純物を分析した結果を以下に示す。
Comparative Example 1 (analysis of trimethylaluminum)
In the first embodiment, the position of the carrier gas tube in the plasma torch is not changed, and a plasma torch having the same height at the tip of the carrier gas tube and the tip of the plasma gas tube is used as in the first embodiment. Analysis of trimethylaluminum was performed ((R / L) × 100 = 0%). As a result, adhesion of black impurities was observed at the tip of the carrier gas pipe.
The results of analyzing the impurities are shown below.
（分析結果）
炭素；９９．８％
ケイ素；０．２％
以上の結果より、不純物はキシレン由来の黒鉛を主成分とするものであった。また、ケイ素成分が検出されたことから、キシレン中のケイ素成分（分析対象）が分析されずに、黒鉛の発生とともに付着したと考えられる。
(result of analysis)
Carbon; 99.8%
Silicon; 0.2%
From the above results, the impurities were mainly composed of xylene-derived graphite. Moreover, since the silicon component was detected, it is thought that the silicon component (analysis object) in xylene was not analyzed but adhered with the generation of graphite.
比較例２（プラズマトーチの作成、及びトリメチルアルミニウムの分析）
実施例１において、プラズマトーチにおけるプラズマガス管の内径に対するキャリアガス管の先端部の位置を２ｍｍに変えたこと以外、実施例１と同様に分析を行った（（Ｒ／Ｌ）×１００＝１４％）。その結果、キャリアガス管の先端部には黒色の不純物の付着が僅かに観られた。
Comparative Example 2 (Preparation of plasma torch and analysis of trimethylaluminum)
In Example 1, analysis was performed in the same manner as in Example 1 except that the position of the tip of the carrier gas tube with respect to the inner diameter of the plasma gas tube in the plasma torch was changed to 2 mm ((R / L) × 100 = 14). %). As a result, slight adhesion of black impurities was observed at the tip of the carrier gas pipe.
実施例３（プラズマトーチの作成、及びトリメチルアルミニウムの分析）
実施例１において、プラズマトーチにおけるプラズマガス管の内径に対するキャリアガス管の先端部の位置を４ｍｍに変えたこと以外、実施例１と同様に分析を行った（（Ｒ／Ｌ）×１００＝２８％）。その結果、キャリアガス管の先端部には何ら付着は観られなかった。
Example 3 (Preparation of plasma torch and analysis of trimethylaluminum)
In Example 1, analysis was performed in the same manner as in Example 1 except that the position of the tip of the carrier gas tube with respect to the inner diameter of the plasma gas tube in the plasma torch was changed to 4 mm ((R / L) × 100 = 28). %). As a result, no adhesion was observed at the tip of the carrier gas pipe.
実施例４（プラズマトーチの作成、及びトリメチルアルミニウムの分析）
実施例１において、プラズマトーチにおけるプラズマガス管の内径に対するキャリアガス管の先端部の位置を５ｍｍに変えたこと以外、実施例１と同様に分析を行った（（Ｒ／Ｌ）×１００＝３６％）。その結果、キャリアガス管の先端部には何ら付着は観られなかった。
Example 4 (Preparation of plasma torch and analysis of trimethylaluminum)
In Example 1, analysis was performed in the same manner as in Example 1 except that the position of the tip of the carrier gas tube with respect to the inner diameter of the plasma gas tube in the plasma torch was changed to 5 mm ((R / L) × 100 = 36). %). As a result, no adhesion was observed at the tip of the carrier gas pipe.
比較例３（プラズマトーチの作成、及びトリメチルアルミニウムの分析）
実施例１において、プラズマトーチにおけるプラズマガス管の内径に対するキャリアガス管の先端部の位置を６ｍｍに変えたこと以外、実施例１と同様に分析を行った（（Ｒ／Ｌ）×１００＝４３％）。
その結果、キャリアガス管の先端部には不純物の付着はなかったものの、キャリアガス管の先端部に黒鉛が生じていた。また、霧化した試料がプラズマ炎まで十分に届かなかったため、試料液体中の微量不純物を分析が十分にできなかった（分析感度が低下した）。
Comparative Example 3 (Preparation of plasma torch and analysis of trimethylaluminum)
In Example 1, analysis was performed in the same manner as in Example 1 except that the position of the tip of the carrier gas tube with respect to the inner diameter of the plasma gas tube in the plasma torch was changed to 6 mm ((R / L) × 100 = 43). %).
As a result, although no impurities adhered to the tip of the carrier gas tube, graphite was generated at the tip of the carrier gas tube. Moreover, since the atomized sample did not reach the plasma flame sufficiently, analysis of trace impurities in the sample liquid could not be sufficiently performed (analysis sensitivity was lowered).
以上の結果より、［（Ｒ／Ｌ）×１００］が２１％、２９％、３６％に位置する場合（おおよそプラズマガス管の内径に対して２０〜４０％）には、不純物の付着は観察されなかった。これに対して、０％、１４％（２０％未満）とした場合には、不純物の付着が観察され、４３％（４０％超）とした場合には、分析が十分にできなかった。 From the above results, when [(R / L) × 100] is located at 21%, 29%, and 36% (approximately 20 to 40% with respect to the inner diameter of the plasma gas tube), the adhesion of impurities is observed. Was not. On the other hand, when 0% and 14% (less than 20%), adhesion of impurities was observed, and when 43% (over 40%), analysis could not be performed sufficiently.
実施例及び比較例（プラズマトーチの作成、及び有機金属化合物の分析）
実施例１において、プラズマトーチにおけるプラズマガス管の内径に対するキャリアガス管の先端部の位置と、分析対象物である有機金属化合物に変えたこと以外、実施例１と同様に分析を行った。
なお、記号、略語の意味は以下の通りである。
（記号）
○；不純物の付着なし、分析感度良好
△；不純物の僅かな付着及び／又は分析感度不良
×：不純物の付着及び分析感度不良
（略語）
ＴＭＡ：トリメチルアルミニウム
ＴＥＡ；トリエチルアルミニウム
ＴＭＧ；トリメチルガリウム
ＴＥＧ；トリエチルガリウム
ＴＭＩ；トリメチルインジウム
ＤＭＺ；ジメチル亜鉛
ＤＥＺ；ジエチル亜鉛
Ｃｐ２Ｍｇ；ビス（シクロペンタジエニル）マグネシウム
Ａｌ錯体；トリス（ｔ−ブチルメチルアミド）アルミニウム
Examples and Comparative Examples (Plasma Torch Creation and Analysis of Organometallic Compounds)
In Example 1, the analysis was performed in the same manner as in Example 1 except that the position of the tip of the carrier gas tube relative to the inner diameter of the plasma gas tube in the plasma torch was changed to the organometallic compound as the analysis object.
The meanings of symbols and abbreviations are as follows.
(symbol)
○: No impurity adhesion, good analysis sensitivity Δ: Slight impurity adhesion and / or poor analysis sensitivity ×: Impurity adhesion and poor analysis sensitivity (abbreviation)
TMA: trimethylaluminum TEA; triethylaluminum TMG; trimethylgallium TEG; triethylgallium TMI; trimethylindium DMZ; dimethylzinc DEZ; diethylzinc Cp 2 Mg; bis (cyclopentadienyl) magnesium Al complex; )aluminum
以上の結果より、本発明のプラズマトーチを用いた分析方法により、不純物の付着を生じさせず、精度良く有機金属化合物の分析ができることが確認された。
また、本発明の分析により、有機金属化合物の品質管理能力が向上し、有機金属化合物を製品として出荷するのに適した態様となった。
From the above results, it was confirmed that the organometallic compound can be analyzed with high accuracy without causing adhesion of impurities by the analysis method using the plasma torch of the present invention.
Further, the analysis of the present invention has improved the quality control ability of the organometallic compound, and has become a mode suitable for shipping the organometallic compound as a product.
本発明は、プラズマ炎の位置やキャリアガスの流速の微調整をすることなく、簡便な操作にて、有機金属化合物を不活性な有機溶媒で希釈した試料液体に含まれる微量不純物を感度良く分析する方法、及び当該分析に用いるプラズマトーチに関する。 The present invention is capable of sensitively analyzing trace impurities contained in a sample liquid obtained by diluting an organometallic compound with an inert organic solvent by a simple operation without fine adjustment of the position of the plasma flame and the flow rate of the carrier gas. And a plasma torch used for the analysis.
１ プラズマガス管
２ キャリアガス管
1
Claims (7)
プラズマガス管、及びその内側にキャリアガス管を備え、キャリアガス管の先端部がプラズマガス管の先端部に対して下部に位置するプラズマトーチであって、
プラズマガス管の内径をＲ（ｍｍ）、
プラズマガス管の先端部とキャリアガス管の先端部の長さをＬ（ｍｍ）
とした場合において、
（Ｒ／Ｌ）×１００
が２０％〜４０％であるプラズマトーチに、
前記霧化させた試料をキャリアガスとともにキャリアガス管を通じてプラズマトーチに導入して、誘導結合型プラズマ発光分析法により試料液体中の微量不純物を分析する方法。 After atomizing a sample liquid in which an organometallic compound is diluted with an inert organic solvent,
A plasma torch comprising a plasma gas tube and a carrier gas tube inside thereof, the tip of the carrier gas tube being located below the tip of the plasma gas tube,
The inner diameter of the plasma gas tube is R (mm),
The length of the tip of the plasma gas tube and the tip of the carrier gas tube is L (mm)
If
(R / L) × 100
Is a plasma torch with 20% to 40%,
A method in which the atomized sample is introduced into a plasma torch together with a carrier gas through a carrier gas tube, and trace impurities in the sample liquid are analyzed by inductively coupled plasma emission spectrometry.
プラズマガス管、及びその内側にキャリアガス管を備え、キャリアガス管の先端部がプラズマガス管の先端部に対して下部に位置するプラズマトーチであって、
プラズマガス管の内径をＲ（ｍｍ）、
プラズマガス管の先端部とキャリアガス管の先端部の長さをＬ（ｍｍ）
とした場合において、
（Ｒ／Ｌ）×１００
が２０％〜４０％であるプラズマトーチ。 A plasma torch used in the analysis method according to claim 1, comprising a plasma gas tube and a carrier gas tube inside thereof, the tip of the carrier gas tube being located below the tip of the plasma gas tube,
The inner diameter of the plasma gas tube is R (mm),
The length of the tip of the plasma gas tube and the tip of the carrier gas tube is L (mm)
If
(R / L) × 100
Is a plasma torch with 20% to 40%.
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