JPH0264444A - thermal conductivity detector - Google Patents
thermal conductivity detectorInfo
- Publication number
- JPH0264444A JPH0264444A JP21686088A JP21686088A JPH0264444A JP H0264444 A JPH0264444 A JP H0264444A JP 21686088 A JP21686088 A JP 21686088A JP 21686088 A JP21686088 A JP 21686088A JP H0264444 A JPH0264444 A JP H0264444A
- Authority
- JP
- Japan
- Prior art keywords
- tcd
- thermal conductivity
- present
- conductivity detector
- allyl chloride
- 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.)
- Granted
Links
Landscapes
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明はガスクロマトグラフに用いる熱伝導度検出器（
以下ＴＣＤという）に関する。Detailed Description of the Invention (Industrial Application Field) The present invention relates to a thermal conductivity detector (
(hereinafter referred to as TCD).
（従来の技術）
ＴＣＤはステンレススチール製のセル室とタングステン
レニウム合金、白金もしくはタングステンで作られたフ
ィラメントより構成されている。(Prior Art) A TCD consists of a cell chamber made of stainless steel and a filament made of tungsten rhenium alloy, platinum or tungsten.
（発明が解決しようとする課題）
ＴＣＤを用いるＧＣ分析時に、成分の溶出中に分析対象
化合物によってはベースラインが負側に下がり、定量値
に信頼がおけなくなったり、あるいは定量が不可能にな
る、またはノイズレベルが高くなるなどの問題点があっ
た。(Problems to be Solved by the Invention) During GC analysis using TCD, the baseline may drop to the negative side for some target compounds during component elution, making quantitative values unreliable or impossible. , or there were problems such as an increase in the noise level.
本発明の発明者は、空気を含む試料をカラムに導入した
ときに上記の現象が順著であり、有機溶媒溶液試料をカ
ラムに導入したとき上記の現象が少ないこと、また水素
をキャリヤガスとするＧＣ分析時は上記の現象が少ない
ことを注意深く考察した結果この現象がＴＣＤに使用さ
れているフィラメントの酸化に起因することをみいだし
本発明をなすに至った。The inventors of the present invention have found that the above phenomenon occurs more frequently when a sample containing air is introduced into the column, and less when an organic solvent solution sample is introduced into the column, and that hydrogen is used as a carrier gas. As a result of careful consideration of the fact that the above-mentioned phenomenon is rare during GC analysis, it has been discovered that this phenomenon is caused by oxidation of the filament used in the TCD, and the present invention has been completed.
（課題を解決するための手段）
本発明のＴＣＤはシラン化処理したフィラメントを用い
る。(Means for Solving the Problems) The TCD of the present invention uses a silanized filament.
本発明のＴＣＤはフィラメントの材料としてタングステ
ンレニウム合金、白金もしくはタングステンが用いられ
る。また本発明のＴＣＤは直通型、半拡散型、拡散型等
のセル構造のものを含み、さイ
らにシュアルカラム流路に使用するＴ’ＣＤだけでなく
シングル流路に使用するＴＣＤをも包含する。In the TCD of the present invention, tungsten-rhenium alloy, platinum, or tungsten is used as the filament material. Furthermore, the TCD of the present invention includes those with cell structures such as direct type, semi-diffusion type, and diffusion type, and further includes not only T'CD used in a dual column flow path but also TCD used in a single flow path. do.
（作用）
ＴＣＤ動作中はフィラメント表面の温度は３００℃〜３
５０℃になるが、フィラメント表面はシラン化合物によ
り被覆されているために酸化作用を持つ被験成分が通過
してもフィラメントは酸化されることなく安定した状態
を維持することができ検出器出力も正常な出力値を与え
る。(Function) During TCD operation, the temperature of the filament surface is 300℃~3
Although the temperature reaches 50 degrees Celsius, the filament surface is coated with a silane compound, so even if the oxidizing test component passes through, the filament remains stable without being oxidized, and the detector output is also normal. gives an output value.
（実施例）
タングステンレニウム合金製のフィラメントとステンレ
ススチール製のセル室よりなる半拡散型子゛
ツユアル流路のＴＣＤにシラン化処理を行った。(Example) A silanization treatment was performed on the TCD of a semi-diffusion type elementary channel consisting of a filament made of tungsten rhenium alloy and a cell chamber made of stainless steel.
まず室温で行ったシラン化処理の手順を述べる。First, the procedure for silanization treatment performed at room temperature will be described.
■ジメチルジクロルシラン（（ＣＨ３）２ＳｉＣ１）３
０％を含むトルエン溶液をＴＣＤセルの内部に満たし３
分間放置する。■Dimethyldichlorosilane ((CH3)2SiC1)3
Fill the inside of the TCD cell with a toluene solution containing 0%
Leave for a minute.
■ジメチルジクロルシランのトルエン溶液を自然落下さ
せてＴＣＤセルより除く。■ Let the toluene solution of dimethyldichlorosilane fall by gravity to remove it from the TCD cell.
■ＴＣＤセル内部をメタノールで洗浄する。５回洗浄を
縁り返す。■Cleanse the inside of the TCD cell with methanol. Wash and turn over 5 times.
■洗浄廃液のメタノールのｐＨが中性になっていること
を確認する。■ Confirm that the pH of methanol in the cleaning waste liquid is neutral.
０８０℃の恒温乾燥機中で乾燥する。Dry in a constant temperature dryer at 080°C.
また、本発明のＴＣＤは以下の処理によっても得られる
。ＴＣＤの温度を１５０℃〜３００℃に保ちセルの中に
ビストリメチルアセトアミドの気体を導入してシラン化
反応を行う。その後ＴＣＤを室温まで冷却して前述の■
〜■の処理を行う、この場合洗浄液はメタノールの他に
アセトンも使用できる。Moreover, the TCD of the present invention can also be obtained by the following treatment. The temperature of the TCD is maintained at 150° C. to 300° C., and bistrimethylacetamide gas is introduced into the cell to carry out the silanization reaction. After that, the TCD is cooled to room temperature and the above
Perform the treatment of ~①. In this case, acetone can be used in addition to methanol as the cleaning liquid.
第１図は本発明のＴＣＤ（室温シラン化処ＦＪ）により
塩化アリルを検出したクロマトグラムである。第２図は
従来のＴＣＤにより塩化アリルを検出したクロマトグラ
ムである。従来のＴＣＤでは酸化力を有する塩化アリル
溶出直後はベースラインが負側に下がり塩化アリル自身
とその後に溶出する成分の定量を妨害したが、本発明の
ＴＣＤを使用すれば塩化アリルビーク溶出の前後でベー
スラインは同一レベルであった。第１図第２図のタロマ
ドグラムを得な分析条件は以下の通りであった。FIG. 1 is a chromatogram in which allyl chloride was detected by the TCD (room temperature silanization treatment FJ) of the present invention. FIG. 2 is a chromatogram in which allyl chloride was detected by conventional TCD. In the conventional TCD, immediately after elution of allyl chloride, which has oxidizing power, the baseline fell to the negative side and interfered with the quantification of allyl chloride itself and the components eluted thereafter, but with the TCD of the present invention, it was possible to detect allyl chloride before and after the allyl chloride peak elution. Baseline was at the same level. The analysis conditions for obtaining the taromadograms shown in FIGS. 1 and 2 were as follows.
カラム ：化学結合型メチルシリコン０．５３ｍ
ｍＩＤＸ２５ｍＬ
カラム温度 ：６０℃
注入口温度 ：１５０℃
検出器温度 ：１５０℃
試料 ：塩化アリル
試料注入ｉ ：０．５μｌ（全量注入法）電流値
：１２０ｍＡ
キャリアガス ：ヘリウム ５０ｍ１／ｍ１ｎ（発明の
効果）
本発明のＴＣＤは酸化作用を有する分析対象物が通過し
てもベースラインの変動やベースラインノイズ増大現象
が少ない。従って定量値に信頼のおける信号値を得るこ
とが出来る。Column: Chemically bonded methyl silicone 0.53m
mIDX 25mL Column temperature: 60℃ Inlet temperature: 150℃ Detector temperature: 150℃ Sample: Allyl chloride sample injection i: 0.5μl (whole volume injection method) Current value
: 120 mA Carrier gas: Helium 50 m1/m1n (Effects of the Invention) The TCD of the present invention has little baseline fluctuation and baseline noise increase phenomenon even when an analyte having an oxidizing effect passes through it. Therefore, a reliable signal value can be obtained as a quantitative value.
第１図は本発明のＴＣＤにより塩化アリルを検出したク
ロマトグラムであり、第２図は従来のＴＣＤにより塩化
アリルを検出したクロマトグラムである。
（’ｊ’ｌＡ ＃Ｔｌ−ｔ： Ｅ４ｓｉｉｕｉｊ、、、
’−，；＝、。
第１図
第２図
ｙ】シ、杷アソυ
ノFIG. 1 is a chromatogram in which allyl chloride was detected by the TCD of the present invention, and FIG. 2 is a chromatogram in which allyl chloride was detected by the conventional TCD. ('j'lA #Tl-t: E4siiuij,,,
'−,;=,. Figure 1 Figure 2 y]
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63216860A JP2676810B2 (en) | 1988-08-31 | 1988-08-31 | Thermal conductivity detector |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63216860A JP2676810B2 (en) | 1988-08-31 | 1988-08-31 | Thermal conductivity detector |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0264444A true JPH0264444A (en) | 1990-03-05 |
| JP2676810B2 JP2676810B2 (en) | 1997-11-17 |
Family
ID=16695042
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63216860A Expired - Fee Related JP2676810B2 (en) | 1988-08-31 | 1988-08-31 | Thermal conductivity detector |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2676810B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004107016A3 (en) * | 2003-05-27 | 2005-01-27 | Hentze Lissotschenko Patentver | Device for converting a light beam |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57155386A (en) * | 1981-03-18 | 1982-09-25 | Murata Mfg Co Ltd | Preventing method for oxidation of copper powder |
| JPS61105451A (en) * | 1984-10-30 | 1986-05-23 | Riken Keiki Kk | Heat conduction type gas detecting element |
-
1988
- 1988-08-31 JP JP63216860A patent/JP2676810B2/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57155386A (en) * | 1981-03-18 | 1982-09-25 | Murata Mfg Co Ltd | Preventing method for oxidation of copper powder |
| JPS61105451A (en) * | 1984-10-30 | 1986-05-23 | Riken Keiki Kk | Heat conduction type gas detecting element |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004107016A3 (en) * | 2003-05-27 | 2005-01-27 | Hentze Lissotschenko Patentver | Device for converting a light beam |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2676810B2 (en) | 1997-11-17 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |