JPH03220447A - Tg-gc/ms apparatus - Google Patents
Tg-gc/ms apparatusInfo
- Publication number
- JPH03220447A JPH03220447A JP1480290A JP1480290A JPH03220447A JP H03220447 A JPH03220447 A JP H03220447A JP 1480290 A JP1480290 A JP 1480290A JP 1480290 A JP1480290 A JP 1480290A JP H03220447 A JPH03220447 A JP H03220447A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- trapping
- gas
- generated
- trap
- 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
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000003463 adsorbent Substances 0.000 claims abstract description 4
- 239000013585 weight reducing agent Substances 0.000 claims description 3
- 238000003795 desorption Methods 0.000 claims description 2
- 102100039339 Atrial natriuretic peptide receptor 1 Human genes 0.000 claims 1
- 101710102163 Atrial natriuretic peptide receptor 1 Proteins 0.000 claims 1
- 238000004817 gas chromatography Methods 0.000 claims 1
- 238000000892 gravimetry Methods 0.000 claims 1
- 239000007789 gas Substances 0.000 abstract description 31
- 238000002411 thermogravimetry Methods 0.000 abstract description 16
- 230000000704 physical effect Effects 0.000 abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 3
- 239000012159 carrier gas Substances 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract description 2
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- 230000007423 decrease Effects 0.000 description 6
- 238000005259 measurement Methods 0.000 description 5
- MWEXRLZUDANQDZ-RPENNLSWSA-N (2s)-3-hydroxy-n-[11-[4-[4-[4-[11-[[2-[4-[(2r)-2-hydroxypropyl]triazol-1-yl]acetyl]amino]undecanoyl]piperazin-1-yl]-6-[2-[2-(2-prop-2-ynoxyethoxy)ethoxy]ethylamino]-1,3,5-triazin-2-yl]piperazin-1-yl]-11-oxoundecyl]-2-[4-(3-methylsulfanylpropyl)triazol-1-y Chemical compound N1=NC(CCCSC)=CN1[C@@H](CO)C(=O)NCCCCCCCCCCC(=O)N1CCN(C=2N=C(N=C(NCCOCCOCCOCC#C)N=2)N2CCN(CC2)C(=O)CCCCCCCCCCNC(=O)CN2N=NC(C[C@@H](C)O)=C2)CC1 MWEXRLZUDANQDZ-RPENNLSWSA-N 0.000 description 3
- 238000004949 mass spectrometry Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000001107 thermogravimetry coupled to mass spectrometry Methods 0.000 description 3
- 230000004580 weight loss Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
Landscapes
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明はＴＧ−ＧＣ／ＭＳ装置に関し、さらに詳しくは
、物質の温度変化および化学反応の進行に伴う熱力学的
性質・物理的性質の変化を測定し、かつ温度変化により
その物質から発生したガス成分を分析する装置に関する
。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a TG-GC/MS device, and more specifically, the present invention relates to a TG-GC/MS device, and more specifically, changes in thermodynamic properties and physical properties of substances due to temperature changes and progress of chemical reactions. The present invention relates to a device that measures gas components and analyzes gas components generated from the substance due to temperature changes.
［従来の技術］
従来、ＴＧ （Ｔｈｅｒｍｏ ｇｒａｖｉｍｅｔｒｙ）
測定では、物質の重量を調整された速度で加熱または冷
却される環境中で、時間または温度の関数として記録す
る技法がとられていた。この方法では、試料から発生し
たガス成分の情報を得ることはたいへんむずかしかった
。そこで近年、ＴＧにＭＳ（Ｍａｓｓ ｓｐｅｃｔｒｏ
ｍｅｔｅｒ）やＧＣ（Ｇａｓ ｃｈｒｏｍａｔｏ−ｇｒ
ａｐｈ ） ／ＭＳＭＳ装置続した丁Ｇ−ＭＳ、丁ＧＧ
Ｃ／ＭＳ装置が開発されている。[Conventional technology] Conventionally, TG (Thermo gravimetry)
Measurements have involved recording the weight of a substance as a function of time or temperature in an environment that is heated or cooled at a controlled rate. With this method, it was extremely difficult to obtain information on the gas components generated from the sample. Therefore, in recent years, TG has been using MS (Mass spectro).
meter) and GC (Gas chromato-gr)
aph)/MSMS device connected Ding G-MS, Ding GG
C/MS equipment has been developed.
ＴＧ−ＭＳ装置は、熱重量測定中に時々刻々発生する混
合ガスを直接質量分析計に導き分析する方法で、温度上
昇に伴う試料の重量減少と発生ガス濃度の比較データを
とることができる。また、ＴＧ ＧＣ／ＭＳＩ置は熱
重量測定中の発生ガスを任意の時間トラップして、その
後切り替えバルブを動作すると同時に、トラップ管を急
速加熱してトラップしてあった発生ガスをカラムに導き
、その構成成分を分別して定性・定量するものである。The TG-MS device is a method in which a mixed gas generated from time to time during thermogravimetric measurement is directly guided to a mass spectrometer for analysis, and it is possible to obtain comparative data on the weight loss of a sample due to temperature rise and the concentration of generated gas. In addition, the TG GC/MSI equipment traps the generated gas during thermogravimetric measurement for an arbitrary period of time, then operates the switching valve and at the same time rapidly heats the trap tube to guide the trapped generated gas to the column. It separates its constituent components for qualitative and quantitative analysis.
［発明か解決しようとする課題１
しかし、このようなＴＧ−ＭＳ装置、ＴＧＧＣ／ＭＳ装
置を用いた場合でも、熱重量測定の結果（温度上昇に伴
う試料の重量減少）と発生ガスとの詳細な情報、例えば
分子構造の局所部分までの情報を得ることはむずかしい
という欠点があった。[Problem to be solved by the invention 1 However, even when such a TG-MS device or TGGC/MS device is used, details of the results of thermogravimetric measurement (reduction in sample weight due to temperature rise) and generated gas cannot be obtained. The disadvantage is that it is difficult to obtain detailed information, for example, information on local parts of the molecular structure.
即ち、ＴＧ−ＭＳ装置での測定では、熱重量測定中の発
生ガス成分を連続で質量分析するために、試料の重量減
少と発生ガス濃度の比較はとれるが、個々の発生ガス成
分に対する解析はむずかしいという欠点がある。また、
ＴＧ−ＧＣ／ＭＳ装置では、試料より発生したガス成分
をすべて一つのトラップ管に濃縮し、その後、急速加熱
してカラムに送るため、熱重量減少に伴う発生ガス成分
の変化に関する情報を得ることができない等の欠点があ
った。In other words, in measurements with a TG-MS device, the gas components generated during thermogravimetry are continuously analyzed by mass analysis, so it is possible to compare the weight loss of the sample and the concentration of the gas generated, but it is difficult to analyze individual gas components. It has the disadvantage of being difficult. Also,
In the TG-GC/MS system, all the gas components generated from the sample are concentrated in one trap tube, then rapidly heated and sent to the column, so it is possible to obtain information about changes in the gas components generated due to thermogravimetric reduction. There were drawbacks such as the inability to
本発明の目的は以上述べたような従来の問題点を解消し
、ＴＧ測定時に試料より微量発生した個々のガス成分を
経時的に質量分析することかできる新規なＴＧ−ＧＣ／
ＭＳ装置を提供することにある。The purpose of the present invention is to solve the above-mentioned conventional problems and to develop a new TG-GC/
Our objective is to provide MS devices.
［課題を解決するための手段］
本発明は、試料を一定の条件で加熱しながら、その重量
減少を連続的に測定すると共に、試料から発生したガス
成分をガスクロマトグラフで分離し質量分析する、ＴＧ
（Ｔｈｅｒｍｏ （］ｒａＶｉｍｅｔｒｙ）装置と該
ＴＧ装置に接続したＧＣ／ＭＳ （Ｇａｓｃｈｒｏｍａ
ｔｏｇｒａｐｈ ／１４ａｓｓ ｓｐｅｃｔｒｏｍｅｔ
ｅｒ ＞装置とからなるＴＧ−ＧＣ／ＭＳ装置において
、丁Ｇ装置とＧＣ／ＭＳ装置との間に、内部に吸着剤が
充填された複数のトラップ管と該トラップ管の加熱装置
とを備えたトラップ装置が配設されてなり、Ｔｌ置から
発生したガス成分は、熱重量減少と連動させて各トラッ
プ管に順次トラップし、かつ各トラップ管ごとに加熱・
脱離するようにしたことを特徴とするＴＧ−ＧＣ／ＭＳ
装置である。[Means for Solving the Problems] The present invention continuously measures the weight loss of a sample while heating it under certain conditions, and also separates gas components generated from the sample using a gas chromatograph and performs mass spectrometry. T.G.
(Thermo (]raVimetry) device and GC/MS (Gaschroma
tograph /14ass spectromet
A TG-GC/MS device consisting of a TG device and a GC/MS device is provided with a plurality of trap tubes filled with adsorbent inside and a heating device for the trap tubes, between the GC device and the GC/MS device. A trap device is installed, and the gas components generated from the Tl placement are sequentially trapped in each trap pipe in conjunction with thermal weight reduction, and heated and heated for each trap pipe.
TG-GC/MS characterized by desorption
It is a device.
本発明のＴＧ−ＧＣ／ＭＳ装置によれば、試料から発生
したガス成分を熱重量減少と連動させて各トラップ管に
トラップするので、試料を入れ直して再度同じ操作を行
うことにより、繰り返して同一成分を同一のトラップ管
に濃縮することが可能であり、その後、各濃縮物をそれ
ぞれ別々に加熱・脱離してＧ Ｃ／ Ｍ Ｓ装置に送る
ことができる。According to the TG-GC/MS device of the present invention, the gas components generated from the sample are trapped in each trap tube in conjunction with the thermogravimetric reduction, so the same operation can be repeated by re-inserting the sample and performing the same operation again. The components can be concentrated in the same trap tube, and each concentrate can then be separately heated and desorbed and sent to a GC/MS device.
本発明による丁Ｇ−ＧＣ／ＭＳ装置を用いれば、試料の
温度変化、および化学反応の進行に伴う試料の分子構造
内局部の熱力学的性質・物理的性質の変化を測定するこ
とが可能である。By using the Ding G-GC/MS device according to the present invention, it is possible to measure temperature changes in a sample and changes in local thermodynamic properties and physical properties within the sample's molecular structure as chemical reactions progress. be.
［作用］
本発明においては、ＴＧ測測定おいて試料の重量減少時
に試料から発生した各ガス成分を熱重量減少に連動させ
て各トラップ管にトラップする。[Function] In the present invention, each gas component generated from the sample when the weight of the sample decreases in TG measurement is trapped in each trap tube in conjunction with the thermal weight decrease.
このため、熱重量減少に伴う発生ガス成分の変化に関゛
する情報が得られ、かつ個々の発生ガス成分の同定も可
能である。Therefore, information regarding changes in generated gas components due to thermogravimetric reduction can be obtained, and individual generated gas components can also be identified.
また、発生ガス量が微量であっても、試料を繰り返し装
填して測定することにより、各成分を濃縮できる。この
ため、試料の重量減少時に試料より発生した極微量成分
を感度よく測定できるようになる。したがって、試料の
分子構造中の局所部分の熱力学的性質・物理的性質の変
化が容易にわかるようになる。Further, even if the amount of gas generated is minute, each component can be concentrated by repeatedly loading and measuring samples. Therefore, it becomes possible to measure with high sensitivity the extremely small amount of components generated from the sample when the weight of the sample decreases. Therefore, changes in thermodynamic properties and physical properties of local parts in the molecular structure of the sample can be easily seen.
［実施例］
以下、本発明の実施例について、図面を参照して詳細に
説明する。[Example] Hereinafter, an example of the present invention will be described in detail with reference to the drawings.
第１図は本発明の一実施例を示すＴＧ−ＧＣ／ＭＳ装置
の概略構成図である。本装置はＴＧ装置１およびトラッ
プ装置２およびＧＣ／ＭＳ装置３よりなる。ＴＧ測測定
おいて、試料９をヒータ１０により一定の昇温速度で加
熱していく時に発生したガス成分は、フローコントロー
ラ８によって流量を調節したキャリヤガスにより、温度
コントロルか可能なライン４を通り、トラップ装置２に
導かれる。FIG. 1 is a schematic diagram of a TG-GC/MS device showing an embodiment of the present invention. This device consists of a TG device 1, a trap device 2, and a GC/MS device 3. In the TG measurement, gas components generated when the sample 9 is heated at a constant temperature increase rate by the heater 10 pass through a line 4 whose temperature can be controlled by a carrier gas whose flow rate is adjusted by a flow controller 8. , guided to the trap device 2.
トラップ装置２内には数本のトラップ管５がセットされ
てあり、ＴＧ測測定あける重量減少に伴い、順次可動で
ある。また、トラップ管５は液体窒素により冷やされて
おり、吸着剤が詰められている。ＴＧ測測定終了すると
、加熱装置６によりそれぞれのトラップ管５が加熱され
、吸着された成分が脱離する。発生ガスが微量の場合に
は、トラップ管５を初期状態に戻し、試料を装填して再
度トラップさせることも可能である。Several trap tubes 5 are set in the trap device 2 and are movable in sequence as the weight decreases during TG measurement. Further, the trap pipe 5 is cooled with liquid nitrogen and filled with an adsorbent. When the TG measurement is completed, each trap tube 5 is heated by the heating device 6, and the adsorbed components are desorbed. If the amount of generated gas is small, it is also possible to return the trap tube 5 to its initial state, load the sample, and trap it again.
このようにして脱離した成分は、温度コントロルされた
ライン７を通り、ＧＣ／ＭＳ装置３に送られ、質量分析
される。以上のようにしてＴＧ測測定おける重量減少と
連動してトラップ管を駆動させ、順次発生ガス成分をト
ラップさせることにより、試料の分子構造中の局所部分
の熱力学的性質・物理的性質の変化をとらえることがで
きる。The components desorbed in this manner are sent to the GC/MS device 3 through a temperature-controlled line 7 and subjected to mass spectrometry. As described above, by driving the trap tube in conjunction with weight reduction during TG measurement and sequentially trapping the generated gas components, changes in thermodynamic properties and physical properties of local parts in the molecular structure of the sample are caused. can be captured.
［発明の効果］
以上説明したように、本発明のＴＧ−ＧＣ／ＭＳ装置で
は、ＴＧ測測定おいて試料の重量減少時に発生した各ガ
ス成分を熱重量減少と連動して別々にトラップし、その
後、トラップしたガス成分を個々に急速加熱してガスク
ロマトグラフに導入し、質量分析するため、試料の分子
構造中の局所部分の熱力学的・物理的性質の変化が明確
にわかるという効果を有する。[Effects of the Invention] As explained above, the TG-GC/MS device of the present invention separately traps each gas component generated when the weight of the sample decreases in TG measurement in conjunction with the thermogravimetric decrease. The trapped gas components are then rapidly heated individually and introduced into a gas chromatograph for mass spectrometry analysis, which has the effect of clearly showing changes in the thermodynamic and physical properties of local parts of the sample's molecular structure. .
第１図は本発明の一実施例の概略構成図である。
１・・・ＴＧ装置 ２・・・トラップ装置３
・・・ＧＣ／ＭＳ装置 ４，７・・・ライン５・・
・トラップ管 ６・・・加熱装置８・・・フロ
ーコントローラ ９・・・試料１０・・・ヒータFIG. 1 is a schematic diagram of an embodiment of the present invention. 1...TG device 2...Trap device 3
...GC/MS device 4,7...Line 5...
・Trap tube 6... Heating device 8... Flow controller 9... Sample 10... Heater
Claims (1)
を連続的に測定すると共に、試料から発生したガス成分
をガスクロマトグラフで分離し質量分析する、ＴＧ（Ｔ
ｈｅｒｍｏ ｇｒａｖｉｍｅｔｒｙ）装置と該ＴＧ装置
に接続したＧＣ／ＭＳ（Ｇａｓｃｈｒｏｍａｔｏｇｒａ
ｐｈ／Ｍａｓｓ ｓｐｅｃｔｒｏｍｅｔｅｒ）装置とか
らなるＴＧ−ＧＣ／ＭＳ装置において、ＴＧ装置とＧＣ
／ＭＳ装置との間に、内部に吸着剤が充填された複数の
トラップ管と該トラップ管の加熱装置とを備えたトラッ
プ装置が配設されてなり、ＴＧ装置から発生したガス成
分は、熱重量減少と連動させて各トラップ管に順次トラ
ップし、かつ各トラップ管ごとに加熱・脱離するように
したことを特徴とするＴＧ−ＧＣ／ＭＳ装置。(1) TG (T
hermo gravimetry) device and the GC/MS (Gaschromatography) device connected to the TG device.
In a TG-GC/MS device consisting of a ph/Mass spectrometer) device, the TG device and the GC
A trap device including a plurality of trap tubes filled with adsorbent and a heating device for the trap tubes is disposed between the MS device and the gas component generated from the TG device. A TG-GC/MS device characterized by trapping in each trap tube sequentially in conjunction with weight reduction, and heating and desorption for each trap tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1480290A JPH03220447A (en) | 1990-01-26 | 1990-01-26 | Tg-gc/ms apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1480290A JPH03220447A (en) | 1990-01-26 | 1990-01-26 | Tg-gc/ms apparatus |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03220447A true JPH03220447A (en) | 1991-09-27 |
Family
ID=11871176
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1480290A Pending JPH03220447A (en) | 1990-01-26 | 1990-01-26 | Tg-gc/ms apparatus |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03220447A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1993020956A1 (en) * | 1992-04-21 | 1993-10-28 | Glaxo Inc. | Aerosol testing method |
| EP2302372A1 (en) * | 2009-09-18 | 2011-03-30 | Helmholtz Zentrum München Deutsches Forschungszentrum für Gesundheit und Umwelt GmbH | Method and device for repetitive chemical analysis of a gas flow |
| US11543394B2 (en) | 2020-03-05 | 2023-01-03 | Shimadzu Corporation | Combined analyzer and analysis method |
-
1990
- 1990-01-26 JP JP1480290A patent/JPH03220447A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1993020956A1 (en) * | 1992-04-21 | 1993-10-28 | Glaxo Inc. | Aerosol testing method |
| EP2302372A1 (en) * | 2009-09-18 | 2011-03-30 | Helmholtz Zentrum München Deutsches Forschungszentrum für Gesundheit und Umwelt GmbH | Method and device for repetitive chemical analysis of a gas flow |
| WO2011033054A3 (en) * | 2009-09-18 | 2011-05-26 | Helmholtz Zentrum München Deutsches Forschungszentrum Für Gesundheit Und Umwelt (Gmbh) | Method and device for repetitive chemical analysis of a gas flow |
| US8431889B2 (en) | 2009-09-18 | 2013-04-30 | Helmholtz Zentrum Muenchen Deutsches Forschungszentrum Fuer Gesundheit Und Umwelt (Gmbh) | Method and device for repetitive chemical analysis of a gas flow |
| US11543394B2 (en) | 2020-03-05 | 2023-01-03 | Shimadzu Corporation | Combined analyzer and analysis method |
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