JPH063342A - Instrument for analyzing gas generated from organic material - Google Patents
Instrument for analyzing gas generated from organic materialInfo
- Publication number
- JPH063342A JPH063342A JP18312292A JP18312292A JPH063342A JP H063342 A JPH063342 A JP H063342A JP 18312292 A JP18312292 A JP 18312292A JP 18312292 A JP18312292 A JP 18312292A JP H063342 A JPH063342 A JP H063342A
- Authority
- JP
- Japan
- Prior art keywords
- gas
- heating
- sample
- gas chromatography
- generated
- 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
Landscapes
- Sampling And Sample Adjustment (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
(57)【要約】
【目的】加熱によって有機材料から発生する微量ガスを
分析する、いわゆる発生気体分析法を適用した場合に
は、目的の材料を外部の専用加熱炉にセットして測定し
ていたため、微量な発生ガスの分析の際には、装置のデ
ッドボリューム、試料の充填量、加熱の不均一性等に左
右され、必ずしも十分な精度での測定ができない点を改
良するものである。
【構成】有機材料を加熱して、熱劣化させるる際に発生
するガスをガスクロマトグラフィーにて分析する装置に
おいて、材料の加熱装置にガスクロマトグラフィー用オ
ーブンを用い、材料をガスクロマトグラフィー充填カラ
ムに充填して分析することにある。
(57) [Summary] [Purpose] When the so-called evolved gas analysis method, which analyzes trace gases generated from organic materials by heating, is applied, the target material is set in an external dedicated heating furnace for measurement. Therefore, in the analysis of a small amount of generated gas, the problem is that the measurement cannot be performed with sufficient accuracy due to the influence of the dead volume of the device, the filling amount of the sample, the nonuniformity of heating, and the like. [Composition] In an apparatus for analyzing a gas generated when an organic material is heated and thermally deteriorated by gas chromatography, an oven for gas chromatography is used as a heating apparatus for the material, and the material is packed in a gas chromatography column. It is to fill and analyze.
Description
【０００１】[0001]
【産業上の利用分野】本発明は、加熱によって有機材料
から発生する微量な発生ガスを、再現性よくかつ高精度
で測定する発生ガス分析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 an evolved gas analyzer for measuring a minute amount of evolved gas produced from an organic material by heating with good reproducibility and high accuracy.
【従来の技術】従来より、加熱によって有機材料から発
生するガスを分析する手段として、ＧＣ法、ＧＣ−ＭＳ
法、赤外線分析法等の各種の方法が知られている。中で
も、ＧＣ法による発生ガス分析法は、装置が廉価であ
り、測定精度もよく各種の気体分析に応用できる事か
ら、もっとも汎用的に用いられている分析装置である。
そのＧＣ法を用いた発生ガス分析装置は、図３に示され
るようなシステム構成によって分析を行う。図３におい
て、11は試料の加熱炉、12は試料ガス切り替えコック、
13はガスクロマトグラフィー本体、14は検出器、15はデ
ータ処理装置で、試料を加熱炉にセットする事により、
ガスボンベを変更する事によって各種雰囲気における試
料からの発生ガスを分析できるような構成になってい
る。2. Description of the Related Art Conventionally, as a means for analyzing a gas generated from an organic material by heating, a GC method or a GC-MS has been used.
Various methods such as a method and an infrared analysis method are known. Among them, the generated gas analysis method by the GC method is the most widely used analyzer because it is inexpensive and can be applied to various gas analyzes with good measurement accuracy.
The evolved gas analyzer using the GC method analyzes with the system configuration as shown in FIG. In FIG. 3, 11 is a sample heating furnace, 12 is a sample gas switching cock,
13 is a gas chromatography main body, 14 is a detector, 15 is a data processing device, and by setting the sample in a heating furnace,
By changing the gas cylinder, the gas generated from the sample in various atmospheres can be analyzed.
【０００２】[0002]
【発明が解決しようとする課題】しかしながら、加熱に
よって有機材料から発生する微量ガスを分析する、いわ
ゆる発生気体分析法を適用した場合には、目的の材料を
外部の専用加熱炉にセットして測定していたため、微量
な発生ガスの分析の際には、装置のデッドボリューム、
試料の充填量、加熱の不均一性等に左右され、必ずしも
十分な精度での測定ができないという問題点があった。However, when a so-called evolved gas analysis method for analyzing a trace gas generated from an organic material by heating is applied, the target material is set in an external dedicated heating furnace for measurement. Therefore, when analyzing a small amount of generated gas, the dead volume of the device,
There is a problem that the measurement cannot be performed with sufficient accuracy due to the filling amount of the sample, the nonuniformity of heating, and the like.
【０００３】[0003]
【課題を解決するための手段】本発明は上述した点に鑑
みて創案されたもので、有機材料をガスクロマトグラフ
ィー用カラムに充填し、さらにこの試料を加熱する加熱
炉に、ガスクロマトグラフィーのカラムオーブンを用い
る事によって、従来困難であった微量発生ガスの分析が
容易に行えるようになる。すなわち、図３での改良を加
えた点は、11の試料加熱炉にある。本発明では、この加
熱炉の代わりに、試料の充填用として、ガスクロ用のカ
ラムを用いる事により、カラムの長さを変える事によっ
て、自由に試料量を変化させる事ができるようになり、
従来の加熱炉では困難であった、試料量の変更を容易に
している。また、加熱炉としてガスクロ用の精密オーブ
ンを用いる事によって、均一で精度の高い加熱が可能と
なる。また、上述のシステムを構成することによって、
ガスの流路に対するデッドボリュームが極めて小さくな
るため、微量発生ガスの分析においても極めて安定な分
析結果が得られるという利点も伴う。The present invention was devised in view of the above-mentioned points, and a column for gas chromatography is filled with an organic material, and a heating furnace for heating this sample is provided with a gas chromatography column. By using a column oven, it becomes possible to easily analyze a trace amount of gas, which was difficult in the past. That is, the point that the improvement in FIG. 3 is added is in the 11 sample heating furnace. In the present invention, instead of this heating furnace, as a sample filling, by using a column for gas chromatography, by changing the length of the column, it becomes possible to freely change the sample amount,
This makes it easy to change the sample amount, which was difficult with conventional heating furnaces. Further, by using a precision oven for gas chromatography as a heating furnace, uniform and highly accurate heating becomes possible. Also, by configuring the above system,
Since the dead volume with respect to the gas flow path is extremely small, there is an advantage that extremely stable analysis results can be obtained even in the analysis of a small amount of generated gas.
【０００４】[0004]
【作用】その作用は、次に述べる実施例と併せて説明す
る。The operation will be described in combination with the embodiment described below.
【実施例】以下、本発明による一実施例を図面に基づい
て詳述する。図１は本発明の一実施例を示す発生ガス分
析装置のシステム構成図であり、１はガスクロ用カラム
オーブン、２は試料充填用カラム、３は試料ガス切り替
えコック、４はガスクロマトグラフィー本体、５は検出
器、６はデータ処理装置である。ここで、２はガスクロ
用カラムであり、このカラムの中に目的の試料を充填す
る。操作は、通常の発生気体分析法と同様であり、試料
を充填したカラムがセットされた、ガスクロ用カラムオ
ーブンを目的の温度にセットし、安定な状態に達した時
点でガスクロマトグラフィーにキャリアガスとともに発
生ガスを導入し、分析を行う。従来装置による発生ガス
分析結果及び、本発明による分析結果を比較を図２に示
す。試料は、熱硬化性樹脂の一種であるエポキシ樹脂硬
化物を粉砕したもので、それぞれの装置を用いて、空気
中での酸化挙動を調べるために空気雰囲気中で加熱し、
測定温度において発生する炭酸ガスを還元装置でメタン
に還元し、ガスクロの検出器としてＦＩＤを用いて分析
を行ったものである。図２によれば、従来法では困難で
あった150℃以下での酸化反応による、炭酸ガスの発生
が明瞭に捕らえられている。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be described in detail below with reference to the drawings. FIG. 1 is a system configuration diagram of an evolved gas analyzer showing an embodiment of the present invention, 1 is a column oven for gas chromatography, 2 is a column for filling a sample, 3 is a cock for switching a sample gas, 4 is a gas chromatography main body, Reference numeral 5 is a detector, and 6 is a data processing device. Here, 2 is a gas chromatography column, and a target sample is packed in this column. The operation is the same as the usual evolved gas analysis method.Set the column filled with the sample, set the column oven for gas chromatography to the target temperature, and when the stable state is reached, use carrier gas for gas chromatography. At the same time, the generated gas is introduced and analyzed. FIG. 2 shows a comparison between the analysis result of the generated gas by the conventional apparatus and the analysis result by the present invention. The sample is a crushed epoxy resin cured product, which is a type of thermosetting resin, and is heated in an air atmosphere to investigate the oxidation behavior in air using each device,
Carbon dioxide gas generated at the measurement temperature was reduced to methane by a reducing device, and FID was used as a detector for gas chromatography to perform analysis. According to FIG. 2, the generation of carbon dioxide gas due to the oxidation reaction at 150 ° C. or lower, which was difficult with the conventional method, is clearly captured.
【０００５】[0005]
【発明の効果】以上述べたように、本発明における発生
ガス分析装置を用いる事によって、試料から発生する微
量の発生ガスを分析する際においても、容易に精度の高
い測定が実現でき、従来困難であった条件における発生
ガス分析も可能となる。As described above, by using the evolved gas analyzer of the present invention, even when a trace amount of evolved gas generated from a sample is analyzed, highly accurate measurement can be easily realized, which is difficult to achieve in the past. It is also possible to analyze the evolved gas under the above conditions.
【図１】図１は本発明の発生ガス分析装置のシステム構
成図である。FIG. 1 is a system configuration diagram of an evolved gas analyzer of the present invention.
【図２】図２は本発明のものと従来のものとの比較ずで
ある。FIG. 2 is a comparison between the present invention and a conventional one.
【図３】図３は従来の発生ガス分析装置のシステム構成
図である。FIG. 3 is a system configuration diagram of a conventional evolved gas analyzer.
【０００６】[0006]
１ ガスクロ用カラムオーブン ２ 試料充填用カラム ３ 試料ガス切り替えコック ４ ガスクロマトグラフィー本体 ５ 検出器 ６ データ処理装置 11 試料の加熱炉 12 試料ガス切り替えコック 13 ガスクロマトグラフィー本体 14 検出器 15 データ処理装置 1 Gas Chromatographic Column Oven 2 Sample Packing Column 3 Sample Gas Switching Cock 4 Gas Chromatography Main Body 5 Detector 6 Data Processing Device 11 Sample Heating Furnace 12 Sample Gas Switching Cock 13 Gas Chromatography Main Body 14 Detector 15 Data Processing Device
Claims (1)
に発生するガスをガスクロマトグラフィーにて分析する
装置において、材料の加熱装置にガスクロマトグラフィ
ー用オーブンを用い、材料をガスクロマトグラフィー充
填カラムに充填して分析する事を特徴とする有機材料の
発生ガス分析装置。1. An apparatus for analyzing a gas generated when an organic material is heated to be thermally deteriorated by gas chromatography, wherein an oven for gas chromatography is used as a heating apparatus for the material, and the material is gas chromatographed. An evolved gas analyzer for organic materials, characterized by being packed in a packed column for analysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18312292A JPH063342A (en) | 1992-06-17 | 1992-06-17 | Instrument for analyzing gas generated from organic material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18312292A JPH063342A (en) | 1992-06-17 | 1992-06-17 | Instrument for analyzing gas generated from organic material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH063342A true JPH063342A (en) | 1994-01-11 |
Family
ID=16130180
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP18312292A Pending JPH063342A (en) | 1992-06-17 | 1992-06-17 | Instrument for analyzing gas generated from organic material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH063342A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8002860B2 (en) * | 1999-06-18 | 2011-08-23 | Hitachi Chemical Co., Ltd. | CMP abrasive, method for polishing substrate and method for manufacturing semiconductor device using the same, and additive for CMP abrasive |
| WO2016063975A1 (en) * | 2014-10-24 | 2016-04-28 | 横浜ゴム株式会社 | Phosphoric acid-modified polymer |
-
1992
- 1992-06-17 JP JP18312292A patent/JPH063342A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8002860B2 (en) * | 1999-06-18 | 2011-08-23 | Hitachi Chemical Co., Ltd. | CMP abrasive, method for polishing substrate and method for manufacturing semiconductor device using the same, and additive for CMP abrasive |
| WO2016063975A1 (en) * | 2014-10-24 | 2016-04-28 | 横浜ゴム株式会社 | Phosphoric acid-modified polymer |
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