JPH01146242A - Mass spectrometer - Google Patents
Mass spectrometerInfo
- Publication number
- JPH01146242A JPH01146242A JP62303158A JP30315887A JPH01146242A JP H01146242 A JPH01146242 A JP H01146242A JP 62303158 A JP62303158 A JP 62303158A JP 30315887 A JP30315887 A JP 30315887A JP H01146242 A JPH01146242 A JP H01146242A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- heater block
- leading pipe
- sample leading
- sample introduction
- 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
- 238000000889 atomisation Methods 0.000 claims abstract description 11
- 239000000945 filler Substances 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 2
- 230000035515 penetration Effects 0.000 claims description 2
- 125000006850 spacer group Chemical group 0.000 abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 4
- 229910002804 graphite Inorganic materials 0.000 abstract description 4
- 239000010439 graphite Substances 0.000 abstract description 4
- 238000012423 maintenance Methods 0.000 abstract description 2
- 238000010079 rubber tapping Methods 0.000 abstract description 2
- 238000002347 injection Methods 0.000 abstract 1
- 239000007924 injection Substances 0.000 abstract 1
- 230000000149 penetrating effect Effects 0.000 abstract 1
- 239000008186 active pharmaceutical agent Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000012951 Remeasurement Methods 0.000 description 1
- 150000001793 charged compounds Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000000752 ionisation method Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Electron Sources, Ion Sources (AREA)
- Electron Tubes For Measurement (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は大気圧イオン化質量分析計に係り、特に試料導
入管とヒータブロックからなる霧化部の改良に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to an atmospheric pressure ionization mass spectrometer, and particularly to an improvement of an atomization section consisting of a sample introduction tube and a heater block.
大気圧イオン化を利用した液体クロマトグラフ直結形質
量分析計（以下ＬＣ／ＡＰＩ質量分析計と称す）は、従
来の電子１ｒｆｖｅ形イオン化を利用したガスクロマト
グラフ直結形質量分析計（以下ＧＣ質量分析計と称す）
に比べ、そのイオン化機構において衝撃の少ない穏やか
なイオン化手段を用いているため、試料をイオン化する
際分解することが少なく、分子イオンが観測し易い特徴
を有し、ＧＣ質量分析計では得られない多くの知見を有
している。A liquid chromatograph directly coupled mass spectrometer (hereinafter referred to as an LC/API mass spectrometer) that utilizes atmospheric pressure ionization is different from a gas chromatograph directly coupled mass spectrometer (hereinafter referred to as a GC mass spectrometer) that utilizes conventional electron 1rfve type ionization. )
Compared to GC mass spectrometers, the ionization mechanism uses a gentle ionization method with less impact, so there is less decomposition during ionization of the sample, making it easier to observe molecular ions, which cannot be obtained with a GC mass spectrometer. He has a lot of knowledge.
第１図にＬＣ／ＡＰＩ質量分析計の概略を示す。Figure 1 shows an outline of the LC/API mass spectrometer.
液体クロマトグラフ１（以下ＬＣと称す）より溶出する
試料および移動相はテフロンパイプ２を通して霧化部３
に送られ、ここで熱を加えられることにより霧化される
。霧化された試料および移動相は分子状態となり、イオ
ン化室４において針電極５より発生するコロナ放電によ
ってイオン化される。イオン化された移動相分子は試料
分子と分子反応を起こし、イオン化がまだされていない
試料分子へプロトンを移すことによって試料分子をイオ
ン化する。この分子反応によって試料分子は穏やかに、
且つほぼすべての分子がイオン化される。イオン化され
た試料分子は第１細孔６を通り、更に第２細孔７を通っ
て質量分析部８に送られ。The sample and mobile phase eluted from the liquid chromatograph 1 (hereinafter referred to as LC) are passed through the Teflon pipe 2 to the atomization section 3.
where it is heated and atomized. The atomized sample and mobile phase are in a molecular state and are ionized by corona discharge generated from the needle electrode 5 in the ionization chamber 4 . The ionized mobile phase molecules cause a molecular reaction with the sample molecules and ionize the sample molecules by transferring protons to the sample molecules that have not yet been ionized. This molecular reaction gently causes the sample molecules to
Moreover, almost all molecules are ionized. The ionized sample molecules pass through the first pore 6 and further pass through the second pore 7 to be sent to the mass spectrometer 8.
質量分析される。Mass spectrometry is performed.
ところで、液体クロマトグラフ１より溶出する試料ある
いは溶媒を霧化するこれまでの霧化部３は、非常に細い
穴径（約０．１ｎｗｎ）を有する試料導入パイプとヒー
タブロックを熱伝導度を良くするため溶接によって一体
化した構造となっており、ヒータブロックを加熱するこ
とによって、試料および移動相を霧化する方法をとって
いた。By the way, the conventional atomizing section 3 that atomizes the sample or solvent eluted from the liquid chromatograph 1 uses a sample introduction pipe and a heater block with a very small hole diameter (approximately 0.1 nwn) to improve thermal conductivity. In order to do this, it has an integrated structure by welding, and the sample and mobile phase are atomized by heating the heater block.
〔発明が解決しようとする問題点〕
したがって、試料導入パイプが詰まりを起した場合、ヒ
ータブロックまで交換する必要があった。[Problems to be Solved by the Invention] Therefore, when the sample introduction pipe becomes clogged, it is necessary to replace even the heater block.
本発明の目的は、ヒータブロックに試料導入パイプを着
脱可能とすることにより、詰まりを起こした場合、試料
導入パイプのみの交換で再測定を可能とし、安価でしか
も容易に保守が可能なＬＣ／ＡＰＩ質量分析計を提供す
ることにある。An object of the present invention is to make the sample introduction pipe removable to the heater block, so that in the event of clogging, it is possible to perform remeasurement by replacing only the sample introduction pipe, which is inexpensive and easy to maintain. Our objective is to provide an API mass spectrometer.
上記問題点を液体クロマトグラフと、該液体クロマトグ
ラフより試料および移動相を移送する４管と、該導管に
接続し他端が開口した試料導入管を有し、内部に加熱手
段を有するヒータブロックを該試料導入管が貫通して形
成される霧化部と、該霧化部で霧化された前記試料およ
び移動相をコロナ放電によってイオン化するイオン化部
と、該イオン化部より低圧の中間圧力部と、該中間圧力
部より低圧の分析部とに順次導入し、前記試料の質量を
分析する質量分析計において、前記ヒータブロックの前
記試料導入管の貫通部と該試料導入管との間に間隙を設
け、該間隙内に所定の伝熱性を有する充填材を充填する
とともに、前記試料導入管を脱着自在とすることによっ
て解決される。The above problem can be solved by using a heater block that includes a liquid chromatograph, four tubes for transferring the sample and mobile phase from the liquid chromatograph, a sample introduction tube that is connected to the conduits and has the other end open, and has a heating means inside. an atomization section formed through the sample introduction tube; an ionization section that ionizes the sample and mobile phase atomized in the atomization section by corona discharge; and an intermediate pressure section lower than the ionization section. and a mass spectrometer that sequentially introduces the sample from the intermediate pressure section to the low pressure analysis section and analyzes the mass of the sample. This problem can be solved by providing a gap, filling the gap with a filler having a predetermined heat conductivity, and making the sample introduction tube detachable.
移動相および質量分析をする試料を移送する試料導入管
と、ヒータブロックとの間の間隙部に所定の伝熱性を有
する充填材を充填し、ヒータブロック内の加熱手段によ
る加熱が防げられることなく、試料導入管の脱着が自在
にできる。The space between the sample introduction tube for transporting the mobile phase and the sample for mass spectrometry and the heater block is filled with a filler having a specified heat conductivity, so that heating by the heating means in the heater block is not prevented. , the sample introduction tube can be attached and detached freely.
以下本発明の一実施例を第２図により説明する。 An embodiment of the present invention will be described below with reference to FIG.
ＬＣＩから溶出する試料あるいは移動相を導くテフロン
パイプ２はスエジロツクネジを用いたジヨイント９でス
テンレス製の試料導入パイプ１ｏに接続される。試料導
入パイプ１０はヒータブロック１１に挿入され、更にヒ
ータブロック１１と試料導入パイプ１０の間にはヒータ
ブロック１１からの熱伝導度を良くするための、例えば
アルミニウムの粉末かグラファイトで作られたスペーサ
１２が充填または挿入される。A Teflon pipe 2 for introducing the sample or mobile phase eluted from the LCI is connected to a stainless steel sample introduction pipe 1o through a joint 9 using a wedge lock screw. The sample introduction pipe 10 is inserted into the heater block 11, and a spacer made of aluminum powder or graphite, for example, is provided between the heater block 11 and the sample introduction pipe 10 to improve the thermal conductivity from the heater block 11. 12 is filled or inserted.
ヒータブロック１１にはヒータブロック１１を加熱する
ヒータ１３と、ヒータブロック１１の温度を検出する温
度検出素子１４が取付けられ試料または移動相が安定に
、しかも良好な霧となって試料導入パイプ１０の先端よ
り噴出するように任意の温度に保持できるようになって
いる。A heater 13 that heats the heater block 11 and a temperature detection element 14 that detects the temperature of the heater block 11 are attached to the heater block 11 so that the sample or mobile phase is stabilized and becomes a good mist, so that the sample introduction pipe 10 is heated. It can be maintained at any temperature so that it can be ejected from the tip.
スペーサ１２は、ネジキャップ１５で試料導入パイプ押
え１６をヒータブロック１１側に押しつけることによっ
て、その圧力で変形し、従ってヒータブロック１１と試
料導入パイプ１０は、スペーサ１２を介して密着した状
態で固定される。これは試料導入パイプ１０に安定に熱
を供給し、しかも試料または移動相を一定に霧化される
には非常に重要なことである。事実、単純にヒータブロ
ック１１に試料導入パイプ１ｏが挿入可能な穴をあけ試
料導入パイプ１０を挿入して固定する方法では、ヒータ
ブロック１１と試料導入パイプ１０との間にすき間が生
じ、試料導入パイプ１０への熱の供給が不十分となり、
試料または移動用を一定に霧化させることが不可能とな
る場合がある。By pressing the sample introduction pipe holder 16 against the heater block 11 side with the screw cap 15, the spacer 12 is deformed by the pressure, so that the heater block 11 and the sample introduction pipe 10 are fixed in close contact via the spacer 12. be done. This is very important in order to stably supply heat to the sample introduction pipe 10 and to ensure constant atomization of the sample or mobile phase. In fact, in the method of simply making a hole in the heater block 11 into which the sample introduction pipe 1o can be inserted, inserting the sample introduction pipe 10, and fixing it, a gap will be created between the heater block 11 and the sample introduction pipe 10, and the sample introduction pipe 1o will not be able to be introduced. Heat supply to the pipe 10 becomes insufficient,
It may not be possible to consistently atomize the sample or transfer material.
従って、スペーサ１２は熱伝導度が良いことと同時に、
適度な圧力を受けることによって変形するものが適して
いる。前述したアルミニウムの粉末、あるいは、グラフ
ァイトの熱伝導率はそれぞれ約２．４Ｊ／σ・Ｓ−Ｋ、
１．７Ｊ／■・Ｓ −’にであり、更にネジキャップ１
５の適度な締め付けの圧力によって変形し試料導入パイ
プ１０とヒータブロック１１を熱的に密若させるために
は最も適している方法といえる。もちろんこの二種類以
外の材料でもアルミニウムの粉末、あるいはグラファイ
トに準するものであれば使用可能であることは言うまで
もない。Therefore, the spacer 12 has good thermal conductivity and at the same time
A material that deforms when subjected to moderate pressure is suitable. The thermal conductivity of the aforementioned aluminum powder or graphite is approximately 2.4 J/σ・S-K, respectively.
1.7J/■・S -', and screw cap 1
It can be said that this is the most suitable method for thermally sealing the sample introduction pipe 10 and the heater block 11 by deforming the sample introduction pipe 10 and the heater block 11 with appropriate tightening pressure. Of course, it goes without saying that materials other than these two types can also be used as long as they are similar to aluminum powder or graphite.
試料導入パイプ１０が詰まりを起こし交換する場合は、
ネジキャップ１５をゆるめ、試料導入パイプ１０を試料
または移動相を噴出する側より軽くたたくことによって
取り外し、新しい試料導入パイプ１０を挿入してネジキ
ャップ１５を再度締め付ければ完了する。If the sample introduction pipe 10 becomes clogged and needs to be replaced,
Loosen the screw cap 15, remove the sample introduction pipe 10 by tapping it from the side from which the sample or mobile phase is ejected, insert a new sample introduction pipe 10, and tighten the screw cap 15 again to complete the process.
本発明によれば、霧化部のヒータブロックと試料導入管
の貫通部との間の間隙部に、所定の伝熱性を有する充填
材を充填できる構造としたので、ヒータブロック内の加
熱手段による加熱が妨げられることなく試料導入管の交
換が可能となり、保守が容易になる。According to the present invention, the gap between the heater block of the atomization part and the penetration part of the sample introduction tube can be filled with a filler having a predetermined heat conductivity. The sample introduction tube can be replaced without interfering with heating, making maintenance easier.
第１図はＬＣ／ＡＰＩ質量分析計の概略図、第２図は本
発明の霧化部の構造を示す図である。
１・・・液体クロマトグラフ、３・・・霧化部、１０・
・・試料導入管、１１・・・ヒータブロック、１２・・
・スペーサ、１３・・・ヒータ。−
代理人 弁理士 小川筋力 乙 ＼、。
（：、FIG. 1 is a schematic diagram of an LC/API mass spectrometer, and FIG. 2 is a diagram showing the structure of the atomization section of the present invention. 1...Liquid chromatograph, 3...Atomization section, 10.
...Sample introduction tube, 11...Heater block, 12...
・Spacer, 13...Heater. − Agent: Patent attorney Ogawa Musume Otsu ＼、. (:,
Claims (1)
試料および移動相を移送する導管と、該導管に接続し他
端が開口した試料導入管を有し、内部に加熱手段を有す
るヒータブロックを該試料導入管が貫通して形成される
霧化部と、該霧化部で霧化された前記試料および移動相
をコロナ放電によつてイオン化するイオン化部と、該イ
オン化部より低圧の中間圧力部と、該中間圧力部より低
圧の分析部とに順次導入し、前記試料の質量を分析する
質量分析計において、前記ヒータブロックの前記試料導
入管の貫通部と該試料導入管との間に間隙を設け、該間
隙内に所定の伝熱性を有する充填材を充填するとともに
、前記試料導入管を脱着自在としたことを特徴とする質
量分析計。1. It has a liquid chromatograph, a conduit for transferring the sample and mobile phase from the liquid chromatograph, and a sample introduction tube connected to the conduit and open at the other end, and a heater block having a heating means inside the sample. an atomization section formed through the introduction tube; an ionization section that ionizes the sample and mobile phase atomized in the atomization section by corona discharge; and an intermediate pressure section having a lower pressure than the ionization section. , in a mass spectrometer that sequentially introduces the sample from the intermediate pressure section to the low pressure analysis section and analyzes the mass of the sample, a gap is provided between the penetration part of the sample introduction tube of the heater block and the sample introduction tube. 1. A mass spectrometer, wherein the gap is filled with a filler having a predetermined heat conductivity, and the sample introduction tube is detachable.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62303158A JPH01146242A (en) | 1987-12-02 | 1987-12-02 | Mass spectrometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62303158A JPH01146242A (en) | 1987-12-02 | 1987-12-02 | Mass spectrometer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01146242A true JPH01146242A (en) | 1989-06-08 |
Family
ID=17917579
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62303158A Pending JPH01146242A (en) | 1987-12-02 | 1987-12-02 | Mass spectrometer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01146242A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5736741A (en) * | 1996-07-30 | 1998-04-07 | Hewlett Packard Company | Ionization chamber and mass spectrometry system containing an easily removable and replaceable capillary |
| US5750988A (en) * | 1994-07-11 | 1998-05-12 | Hewlett-Packard Company | Orthogonal ion sampling for APCI mass spectrometry |
| USRE36892E (en) * | 1994-07-11 | 2000-10-03 | Agilent Technologies | Orthogonal ion sampling for electrospray .[.LC/MS.]. mass spectrometry |
| US6667474B1 (en) | 2000-10-27 | 2003-12-23 | Thermo Finnigan Llc | Capillary tube assembly with replaceable capillary tube |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61256254A (en) * | 1985-05-10 | 1986-11-13 | Hitachi Ltd | Apparatus for coupling liquid chromatograph and mass analyzer |
-
1987
- 1987-12-02 JP JP62303158A patent/JPH01146242A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61256254A (en) * | 1985-05-10 | 1986-11-13 | Hitachi Ltd | Apparatus for coupling liquid chromatograph and mass analyzer |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5750988A (en) * | 1994-07-11 | 1998-05-12 | Hewlett-Packard Company | Orthogonal ion sampling for APCI mass spectrometry |
| USRE36892E (en) * | 1994-07-11 | 2000-10-03 | Agilent Technologies | Orthogonal ion sampling for electrospray .[.LC/MS.]. mass spectrometry |
| US5736741A (en) * | 1996-07-30 | 1998-04-07 | Hewlett Packard Company | Ionization chamber and mass spectrometry system containing an easily removable and replaceable capillary |
| US6667474B1 (en) | 2000-10-27 | 2003-12-23 | Thermo Finnigan Llc | Capillary tube assembly with replaceable capillary tube |
| EP1225616A3 (en) * | 2000-10-27 | 2006-02-15 | Thermo Finnigan LLC | Capillary tube assembly with replaceable capillary tube |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4935624A (en) | Thermal-assisted electrospray interface (TAESI) for LC/MS | |
| US4298795A (en) | Method and apparatus for introducing samples to a mass spectrometer | |
| CN202196744U (en) | Ion source and mass spectrum system | |
| JP5016191B2 (en) | Multimode ionization source, method of generating ions using the same, and multimode ionization mass spectrometer | |
| JPH0943200A (en) | Ion generator and ion generating method | |
| US6794646B2 (en) | Method and apparatus for atmospheric pressure chemical ionization | |
| US20080083873A1 (en) | Device and method for introducing multiple liquid samples at atmospheric pressure for mass spectrometry | |
| JPH01146242A (en) | Mass spectrometer | |
| JPS60127453A (en) | Atmospheric pressure ionizing type specimen introducing apparatus | |
| Hirata et al. | The application of a new sampling technique using an atomizer for chemical ionization mass spectrometry to free amino acids, drug components, higher phthalates and oligomers of styrene and ethyleneglycol | |
| JPH11326302A (en) | Liquid chromatograph mass spectroscope | |
| JP3238450B2 (en) | Mass spectrometer | |
| JP3554732B2 (en) | Mass spectrometer | |
| JP3285550B2 (en) | Mass spectrometer | |
| JP7433477B2 (en) | Ion source and mass spectrometer equipped with it | |
| WO2023047546A1 (en) | Mass spectrometry method and mass spectrometer | |
| JP3242264B2 (en) | Ion source and mass spectrometer using the same | |
| JPH1123554A (en) | Gas chromatograph device | |
| JP3285549B2 (en) | Mass spectrometer | |
| JPH08211020A (en) | Introduction of sample into ionizing part of mass analyser from liquid chromatograph | |
| JP2767135B2 (en) | Method and apparatus for introducing sample into mass spectrometer | |
| JPS6257068B2 (en) | ||
| JPH03285245A (en) | Liquid chromatographic mass spectrometric device | |
| JP3622332B2 (en) | Mass spectrometer | |
| JP2005259400A (en) | Mass spectrometer |