JPS6134686Y2 - - Google Patents
Info
- Publication number
- JPS6134686Y2 JPS6134686Y2 JP19727481U JP19727481U JPS6134686Y2 JP S6134686 Y2 JPS6134686 Y2 JP S6134686Y2 JP 19727481 U JP19727481 U JP 19727481U JP 19727481 U JP19727481 U JP 19727481U JP S6134686 Y2 JPS6134686 Y2 JP S6134686Y2
- Authority
- JP
- Japan
- Prior art keywords
- ionization chamber
- sample
- heater
- ionization
- ion source
- 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
Links
- 238000010438 heat treatment Methods 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 238000000151 deposition Methods 0.000 claims description 2
- 230000005684 electric field Effects 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 description 14
- 238000000034 method Methods 0.000 description 11
- 238000000451 chemical ionisation Methods 0.000 description 5
- 239000000356 contaminant Substances 0.000 description 5
- 239000011888 foil Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000000752 ionisation method Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
Landscapes
- Electron Tubes For Measurement (AREA)
Description
【考案の詳細な説明】
この考案は質量分析装置、特にそのイオン源の
構成に関するものである。[Detailed Description of the Invention] This invention relates to a mass spectrometer, particularly to the configuration of its ion source.
質量分析装置のイオン源、特にそのイオン化室
においては、気化された試料がイオン化室内に取
り残され壁面等に付着してイオン化室を汚染する
ためイオン化効率を低下させたり、絶縁不良など
を生じ、分析の継続が不可能となることが多い。
また、最近とくに難揮発性物質の質量分析におけ
る分析手法の改良がめざましく、これらの物質も
電界脱離イオン化法（FD法）、電子衝撃イオン化
法（EI法）、化学イオン化法（CI法）等によつて
質料分析が可能となつてきたため、イオン源が汚
染される機会が、より増加している。 In the ion source of a mass spectrometer, especially in its ionization chamber, vaporized samples are left behind in the ionization chamber and adhere to walls, etc., contaminating the ionization chamber, reducing ionization efficiency and causing poor insulation. It is often impossible to continue.
In addition, recently there has been a remarkable improvement in analysis methods for mass spectrometry, especially for refractory substances, and these substances can also be analyzed using field desorption ionization (FD), electron impact ionization (EI), chemical ionization (CI), etc. As material analysis has become possible, the chances of contamination of the ion source are increasing.
この考案は上記にかんがみなされたもので、イ
オン化室内への試料導入機構にイオン化室内面に
付着した試料の焼き出し、あるいはイオン化室内
面への金属蒸着用の加熱機構を具備したことを特
徴とする質量分析装置であり、以下図面に従つて
説明する。 This invention is based on the above considerations, and is characterized in that the sample introduction mechanism into the ionization chamber is equipped with a heating mechanism for baking out the sample adhering to the inside of the ionization chamber or for depositing metal onto the inside of the ionization chamber. This is a mass spectrometer, and will be explained below with reference to the drawings.
第１図は一般的な質量分析装置の概略を説明す
る。図において１はイオン源で、これは、イオン
化室２、レンズ電極３、スリツト４等で構成され
ており、試料はFD法では試料導入機構５の先端
のエミツタ６に付着されて直接イオン化室内に導
入される。なお、このFD法ではエミツタに電流
を流して加熱することでイオン生成が促進される
ので、適当な速度でエミツタを昇温しながら質量
分析が行なわれる。 FIG. 1 provides an overview of a general mass spectrometer. In the figure, 1 is an ion source, which is composed of an ionization chamber 2, a lens electrode 3, a slit 4, etc. In the FD method, the sample is attached to the emitter 6 at the tip of the sample introduction mechanism 5 and is directly placed in the ionization chamber. be introduced. Note that in this FD method, ion generation is promoted by heating the emitter by passing a current through it, so mass spectrometry is performed while heating the emitter at an appropriate rate.
ついで、上記のFD法に限らず、EI法、CI法
（これらのイオン化法は周知なのでここではその
説明は省略する）等によつてイオン化されたイオ
ンは磁界、あるいは電界７内で分離され、特定の
質量を有するイオンのみが検出器８で検出されレ
コーダ９に記録される。 Next, ions ionized not only by the above-mentioned FD method but also by the EI method, the CI method (these ionization methods are well known and will not be described here) are separated in a magnetic field or an electric field 7, Only ions having a specific mass are detected by the detector 8 and recorded in the recorder 9.
以上が質量分析装置の構成の概要であるが、そ
のイオン化室２では、導入された試料が、取り残
されて滞留したりあるいは逆流したりして室内壁
面に付着して、イオン源の絶縁不良、電子電流の
制御不良等の原因となる場合がある。そこで一般
的には第２図のごとくそのイオン化室２の壁面に
ヒータ１０および温度センサ１１を埋設し、セン
サで温度を制御しながらヒータで約350℃以上に
加熱し、付着した試料を焼き出し（ベーキン
グ）、イオン源を正常な状態に復帰させる工夫も
なされている。しかしながら、イオン化室の構造
等によつて壁面からの間接的な加熱では付着した
汚染物の焼き出し効果は少なく、特にCI法にお
けるイオン化室のように密封型となるとその焼き
出し効果は非常に少なかつた。 The above is an overview of the configuration of the mass spectrometer.In the ionization chamber 2, the introduced sample may be left behind and stagnate, or may flow backwards and adhere to the chamber wall, resulting in poor insulation of the ion source. This may cause poor control of electronic current. Therefore, generally, a heater 10 and a temperature sensor 11 are buried in the wall of the ionization chamber 2 as shown in Figure 2, and the temperature is controlled by the sensor and the heater is heated to about 350°C or higher to bake out the attached sample. (baking) and other methods have been devised to restore the ion source to its normal state. However, due to the structure of the ionization chamber, indirect heating from the wall surface has little effect on baking out adhered contaminants, and especially when the ionization chamber is a sealed type such as in the CI method, the baking out effect is very small. Nakatsuta.
本願は上記の壁面からの間接的な加熱に加えて
イオン化室内に直接加熱機構を挿入して付着した
汚染物を焼き出すか、あるいはこの加熱機構によ
り金属箔を蒸発させてイオン化室内を蒸着し絶縁
不良を解消し、イオン源を再生するようにしたも
のである。 In this application, in addition to the indirect heating from the wall surface described above, a heating mechanism is inserted directly into the ionization chamber to burn out the attached contaminants, or metal foil is evaporated by this heating mechanism and deposited inside the ionization chamber to insulate it. This is to eliminate defects and regenerate the ion source.
第３図は、特にFD法、EI法に利用可能なこの
考案の試料導入機構の一実施例であり、試料を付
着させるエミツタの近辺にさらに加熱機構として
の加熱ヒータ１２を装備したものである。 Figure 3 shows an example of the sample introduction mechanism of this invention which can be used particularly for the FD method and the EI method, and is equipped with a heater 12 as a heating mechanism near the emitter to which the sample is attached. .
なお、１３，１４はこれらのエミツタ、あるい
はヒータの電源でスイツチの開閉によつてエミツ
タ、あるいはヒータが使いわけられる。ただし、
場合によれば、エミツタあるいはヒータのどちら
か一方のみを設け、これをヒータ、あるいはエミ
ツタとして使用することも可能で、また電源も共
用することができる。 In addition, 13 and 14 are the power sources for these emitters and heaters, and the emitters and heaters can be used by opening and closing the switches. However,
Depending on the circumstances, it is possible to provide only either the emitter or the heater and use this either as a heater or an emitter, and the power source can also be shared.
第３図の構成においてヒータ１２を1200〜1300
℃程度に加熱してイオン化室壁面に付着した汚染
物の焼き出しを行ない得るが、逆に焼き出し操作
によつても汚染物質の焼き出しが不可能であつた
り、不十分な場合がある。このようなとき本願で
はこのヒータ１２に金属箔、例えば金箔、アルミ
箔等を付着させ、ヒータを加熱することによつて
これらの金属箔を蒸発させ、イオン化室内に蒸着
させることが可能である。この結果、汚染物の表
面に金属薄膜が形成され、導電性が保たれるよう
になり、イオン化室が再生されるのである。 In the configuration shown in Fig. 3, the heater 12 is set at 1200 to 1300
It is possible to bake out contaminants adhering to the wall surface of the ionization chamber by heating the chamber to about 0.degree. C., but conversely, even with the baking operation, it may be impossible or insufficient to bake out the contaminants. In such a case, in the present application, it is possible to attach metal foil, for example, gold foil, aluminum foil, etc. to the heater 12, evaporate the metal foil by heating the heater, and deposit it inside the ionization chamber. As a result, a thin metal film is formed on the surface of the contaminant, maintaining electrical conductivity and regenerating the ionization chamber.
第４図は、特にEI法、CI法に利用可能な試料
導入機構の他の実施例で、試料は試料導入機構の
先端の金属部分に形成された凹部１５で保持され
イオン化室内に導入される。その後、電源１３を
投入してヒータで試料を保持する金属部分を加熱
して試料を蒸発させ、電子ビームによつてイオン
化するが、一方焼き出しを行なうときはスイツチ
を切り換えて電源１４を投入してヒータをさらに
高温に加熱し、ヒータを囲む試料導入機構を構成
する金属筒体を介してイオン化室内を加熱する。
なおこの場合にも凹部に金箔保持させ急速加熱す
ることによつて、金属箔を蒸発させることが可能
である。 Figure 4 shows another example of a sample introduction mechanism that can be used particularly for the EI method and CI method, in which the sample is held in a recess 15 formed in the metal part at the tip of the sample introduction mechanism and introduced into the ionization chamber. . After that, the power supply 13 is turned on and the metal part that holds the sample is heated by a heater to evaporate the sample and ionized by the electron beam.On the other hand, when baking out, the switch is turned on and the power supply 14 is turned on. The heater is then heated to a higher temperature, and the inside of the ionization chamber is heated via the metal cylinder that constitutes the sample introduction mechanism that surrounds the heater.
In this case as well, the metal foil can be evaporated by holding the gold foil in the recess and rapidly heating it.
以上のようにこの考案によれば、汚染されたイ
オン源が簡単な構成によつて再生できるので、従
来気化した試料が滞留、逆流によつてイオン室内
壁に付着していたことに原因するイオン化効率の
低下、絶縁不良等によるイオン源の崩壊は完全に
解決され、安定な状態での分析が可能となるので
ある。 As described above, according to this invention, a contaminated ion source can be regenerated with a simple configuration, which eliminates ionization caused by conventionally vaporized samples adhering to the walls of the ion chamber due to retention and backflow. This completely eliminates the problem of ion source collapse due to reduced efficiency, poor insulation, etc., and enables analysis in a stable state.
第１図は質量分析装置の概略図、第２図はイオ
ン源部の一部拡大断面図、第３図・第４図（一部
断面）は本考案の試料導入機構の概略説明図であ
る。
５……試料導入機構、１２……加熱ヒータ、１
３，１４……電源。
Figure 1 is a schematic diagram of a mass spectrometer, Figure 2 is a partially enlarged sectional view of the ion source, and Figures 3 and 4 (partially in cross section) are schematic explanatory diagrams of the sample introduction mechanism of the present invention. . 5... Sample introduction mechanism, 12... Heater, 1
3,14...Power supply.
Claims (1)
のもとに分離分析するものにおいてイオン化室内
への試料導入機構にイオン化室内面に付着した試
料の焼き出し、あるいはイオン化室内面への金属
蒸着用の加熱機構を具備したことを特徴とする質
量分析装置。 In devices that separate and analyze ionized samples under the action of a magnetic or electric field, the sample introduction mechanism into the ionization chamber includes a heating mechanism for baking out the sample adhered to the inside of the ionization chamber or for depositing metal on the inside of the ionization chamber. A mass spectrometer characterized by comprising:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19727481U JPS58101458U (en) | 1981-12-29 | 1981-12-29 | mass spectrometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19727481U JPS58101458U (en) | 1981-12-29 | 1981-12-29 | mass spectrometer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58101458U JPS58101458U (en) | 1983-07-09 |
| JPS6134686Y2 true JPS6134686Y2 (en) | 1986-10-08 |
Family
ID=30110486
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19727481U Granted JPS58101458U (en) | 1981-12-29 | 1981-12-29 | mass spectrometer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58101458U (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6066174A (en) * | 1983-09-21 | 1985-04-16 | Hitachi Ltd | Method and device for detecting electron and ion superposed beam |
| JPS61140046A (en) * | 1984-12-12 | 1986-06-27 | Fumio Watanabe | Method of degassing by heating in mass spectrometer type residual gas analyzer |
| JP6045467B2 (en) * | 2013-09-27 | 2016-12-14 | 日本電子株式会社 | Mass spectrometer |
-
1981
- 1981-12-29 JP JP19727481U patent/JPS58101458U/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS58101458U (en) | 1983-07-09 |
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