JPH0626108B2 - Ion source for mass spectrometer - Google Patents
Ion source for mass spectrometerInfo
- Publication number
- JPH0626108B2 JPH0626108B2 JP62192097A JP19209787A JPH0626108B2 JP H0626108 B2 JPH0626108 B2 JP H0626108B2 JP 62192097 A JP62192097 A JP 62192097A JP 19209787 A JP19209787 A JP 19209787A JP H0626108 B2 JPH0626108 B2 JP H0626108B2
- Authority
- JP
- Japan
- Prior art keywords
- porous member
- ion source
- opening
- sample
- mass spectrometer
- 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 - Lifetime
Links
- 239000000523 sample Substances 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 27
- 239000012488 sample solution Substances 0.000 claims description 10
- 230000002093 peripheral effect Effects 0.000 claims description 9
- 150000002500 ions Chemical class 0.000 description 13
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 239000011164 primary particle Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
Landscapes
- Electron Sources, Ion Sources (AREA)
- Electron Tubes For Measurement (AREA)
Description
【発明の詳細な説明】 ［産業上の利用分野］ 本発明は、一次ビームを試料に照射し、その衝撃で試料
をイオン化する方式の質量分析装置用イオン源に関し、
特に液体クロマトグラフからの試料液をイオン化室に直
接導入してイオン化する場合に使用して好適なイオン源
に関する。TECHNICAL FIELD The present invention relates to an ion source for a mass spectrometer, in which a sample is irradiated with a primary beam and the sample is ionized by the impact of the sample.
In particular, it relates to an ion source suitable for use when a sample liquid from a liquid chromatograph is directly introduced into an ionization chamber for ionization.
［従来の技術］ 液体クロマトグラフで分離した試料液を質量分析装置に
直接導入する方式のイオン源として、第３図に示す構造
のものが実開昭６１−１１６０６５号に記載されてい
る。[Prior Art] An ion source of the type in which a sample liquid separated by a liquid chromatograph is directly introduced into a mass spectrometer is described in Japanese Utility Model Publication No. 61-116065, which has a structure shown in FIG.
第３図において、１は質量分析装置の質量分析部、２は
イオン源、３はイオン化室、４はイオン化室内で生成さ
れたイオンの加速と集束を行うスリット群、５は一次粒
子ビーム発生器、６は液体クロマトグラフ、７は液体ク
ロマトグラフ６で分離された試料液をイオン化室３内へ
導入するための導入管である。この導入管としてはフュ
ーズドシリカ管が用いられる。また、イオン化室内に挿
入された導入管７の先端部には、拡大断面図を第４図に
示すように、ステンレス管が８が被せられ、さらにその
外側にガラス管（ステンレス等の金属管でも良い）９が
被せられている。そして、導入管の開口部を塞ぐように
円板状の多孔性部材１０が取付けられている。この多孔
性部材としては、例えばステンレスの粉末を焼結して作
成したフィルタ（フリット）が使用される。なお、前記
ステンレス管８にはリペラ電源１１から適宜な電圧が印
加される。In FIG. 3, 1 is a mass analyzer of the mass spectrometer, 2 is an ion source, 3 is an ionization chamber, 4 is a slit group for accelerating and focusing the ions generated in the ionization chamber, and 5 is a primary particle beam generator. , 6 is a liquid chromatograph, and 7 is an introduction pipe for introducing the sample liquid separated by the liquid chromatograph 6 into the ionization chamber 3. A fused silica tube is used as the introduction tube. Further, as shown in an enlarged cross-sectional view of FIG. 4, a distal end portion of the introduction tube 7 inserted into the ionization chamber is covered with a stainless steel tube 8, and a glass tube (a metal tube such as stainless steel or the like is provided on the outer side thereof). Good) 9 is covered. A disk-shaped porous member 10 is attached so as to close the opening of the introduction tube. As this porous member, for example, a filter (frit) made by sintering stainless powder is used. An appropriate voltage is applied to the stainless steel tube 8 from a repeller power supply 11.
かかる構成において、液体クロマトグラフ６で分離され
た試料液は導入管７を介して順次イオン化室３内に導入
され、導入管先端に取付けられている多孔性部材１０の
中を通って表面へ滲出する。表面に滲出した試料液は、
粒子ビーム発生器５からの一次ビームＢの衝撃を受けて
イオン化され、生成されたイオンは質量分析部１へ導入
されて質量分析される。In such a configuration, the sample liquid separated by the liquid chromatograph 6 is sequentially introduced into the ionization chamber 3 through the introduction pipe 7, and exudes to the surface through the porous member 10 attached to the tip of the introduction pipe. To do. The sample liquid oozing on the surface is
The primary beam B from the particle beam generator 5 is impacted to be ionized, and the generated ions are introduced into the mass spectrometric unit 1 for mass spectrometric analysis.
このような装置では、多孔性部材に送られる試料液が順
次完全にイオン化されて多孔性部材表面に残らないよう
な送液速度で試料液を多孔性部材へ供給する必要がある
が、上記構成の装置ではこの適正な送液量が現在の技術
レベルでは正確な制御が困難なほどわずかであるため、
適正な送液速度を越えて多量の試料液が多孔性部材へ送
られてしまうことは避けられない。そうすると、先に送
られた試料成分がイオン化されずに残り、後に送られた
試料成分と一緒にイオンされる所謂メモリ現象が発生し
てしまい、分析に悪影響が出てしまう。In such an apparatus, it is necessary to supply the sample solution to the porous member at a solution sending rate such that the sample solution sent to the porous member is not completely ionized in order and remains on the surface of the porous member. With this device, the appropriate amount of liquid to be delivered is so small that it is difficult to control it accurately at the current technical level.
It is unavoidable that a large amount of sample liquid is sent to the porous member beyond the appropriate liquid sending speed. Then, the sample component sent earlier remains unionized, and a so-called memory phenomenon occurs in which the sample component sent later is ionized together with the sample component sent later, which adversely affects the analysis.
そこで、多孔性部材の部分に包囲体を被せることによ
り、上記問題点を解決したイオン源が特願昭６２−２０
１８４号として提案されている。Therefore, an ion source that solves the above problems by covering the porous member with an envelope is disclosed in Japanese Patent Application No. 62-20.
No. 184 has been proposed.
このイオン源においては、第５図に示すように多孔性部
材１０の表面における試料液の滲出領域を規定する開口
１２を有する包囲体（キャップ）１３を該多孔性部材に
密接して被せ、該開口部に滲出した試料液を一次ビーム
照射によりイオン化するようにしている。１４は導入管
をキャップ１３内に固定する位置決め部材である。In this ion source, as shown in FIG. 5, an envelope (cap) 13 having an opening 12 that defines a leaching area of the sample liquid on the surface of the porous member 10 is closely covered with the porous member, The sample solution that has exuded into the opening is ionized by irradiation with the primary beam. Reference numeral 14 is a positioning member for fixing the introduction pipe in the cap 13.
このようにすれば、多孔性部材に送られた試料液は開口
部とそれ以外の部分に分けて滲出し、開口部以外の面か
ら滲出する試料液はキャップ内部に取出される。そのた
め、多量の試料液を多孔性部材に送っても一次ビームが
照射される開口部の領域に滲出する試料量を抑えること
ができ、メモリ現象の発生を防止することができる。By doing so, the sample liquid sent to the porous member is exuded separately in the opening and the other portion, and the sample liquid exuding from the surface other than the opening is taken out into the cap. Therefore, even if a large amount of the sample liquid is sent to the porous member, the amount of the sample exuded in the area of the opening irradiated with the primary beam can be suppressed, and the occurrence of the memory phenomenon can be prevented.
［発明を解決しようとする問題点］ ところが、このような提案方式を採用してもメモリ現象
を完全に防止することができなかった。本発明者はその
原因を追及すべく試料液に着色して試料液の流れを観察
するなどして検討を重ねた結果、以下のような知見を得
た。即ち、第６図は導入管７から多孔性部材１０内に流
入した試料液の流れの様子を示し、実線は開口部へ滲出
する部分、破線はその他の部分へ排出される部分を示
す。開口部の中央部に滲出した試料液は表面を伝わって
放射状に周囲へ広がり、開口の周縁部分ａにたまった
後、再び多孔性部材内部へ流入してキャップ内部に排出
される。一次ビームは開口の中央部分の試料液にも、開
口の周縁部分ａにたまった試料液にも照射されるため、
前述したメモリ現象が発生していたのである。[Problems to Solve the Invention] However, even if such a proposed method is adopted, the memory phenomenon cannot be completely prevented. The present inventor has obtained the following findings as a result of repeated examinations such as coloring the sample liquid and observing the flow of the sample liquid in order to investigate the cause. That is, FIG. 6 shows the state of the flow of the sample liquid flowing into the porous member 10 from the introduction pipe 7, the solid line shows the portion exuding to the opening, and the broken line shows the portion discharged to other portions. The sample liquid that has exuded to the central portion of the opening spreads radially to the periphery along the surface, accumulates in the peripheral edge portion a of the opening, then flows into the porous member again and is discharged into the cap. Since the primary beam irradiates both the sample solution in the central part of the opening and the sample solution accumulated in the peripheral part a of the opening,
The memory phenomenon described above had occurred.
［問題点を解決するための手段］ 本発明は上述した諸点に鑑みてなされたものであり、外
部からイオン源内へ試料液を導入するための導入管と、
該導入管の先端に取付けられる多孔性部材と、該多孔性
部材を通りその表面に滲出した試料液に照射する一次ビ
ームを発生する手段とを備えた質量分析装置用イオン源
において、前記多孔性部材の表面における試料液の滲出
領域を規定する開口を有する包囲体を該多孔性部材に密
接して被せると共に、該開口の前記多孔性部材表面と接
する周縁部分の近傍に前記一次ビームが照射されるのを
防止する遮蔽体を設けたことを特徴としている。[Means for Solving Problems] The present invention has been made in view of the above-mentioned points, and an introduction tube for introducing a sample solution into the ion source from the outside,
An ion source for a mass spectrometer, comprising: a porous member attached to the tip of the introduction tube; and a means for generating a primary beam that irradiates a sample liquid that has passed through the porous member and exudes on its surface, The porous member is closely covered with an enclosure having an opening defining the exudation region of the sample liquid on the surface of the member, and the primary beam is irradiated in the vicinity of a peripheral portion of the opening in contact with the surface of the porous member. It is characterized by the provision of a shield to prevent it from falling.
［作用］ 本発明においては、開口の前記多孔性部材表面と接する
周縁部分の近傍に前記一次ビームが照射されるのを防止
する遮蔽体を設けたため、この周縁部分のたまった試料
液に一次ビームいが照射されず、この部分の試料液はイ
オン化されない。そのため、メモリ現象を完全に防止す
ることが可能となる。[Operation] In the present invention, since the shield for preventing the irradiation of the primary beam is provided in the vicinity of the peripheral edge portion of the opening which is in contact with the surface of the porous member, the sample beam accumulated in the peripheral edge portion is not exposed to the primary beam. Is not irradiated, and the sample liquid in this portion is not ionized. Therefore, it is possible to completely prevent the memory phenomenon.
以下、図面を用いて本発明の一実施例を詳説する。An embodiment of the present invention will be described in detail below with reference to the drawings.
［実施例］ 第１図は本発明を実施した質量分析装置用イオン源の一
例を示す要部拡大断面図であり、第５図と同一符号は同
一構成要素を示している。[Examples] FIG. 1 is an enlarged cross-sectional view of an essential part showing an example of an ion source for a mass spectrometer according to the present invention, and the same reference numerals as those in FIG. 5 denote the same components.
第１図の実施例が第５図の提案装置と相違するのは、キ
ャップ１３の先端に開口１２より小さな開口を有する絞
り板１５を取付けた点である。The embodiment shown in FIG. 1 is different from the proposed device shown in FIG. 5 in that a cap plate 13 having an opening smaller than the opening 12 is attached to the tip of the cap 13.
このようにすれば、前述したキャップ１３の開口１２の
周縁部分ａに試料液がたまっても、この部分には絞り板
15により遮られて一次ビームは照射されず、イオン化さ
れない。従って、メモリ現象を完全に防止することがで
きる。尚、絞り板１５に開ける開口の形状は円形に限ら
ず、周縁部分ａに一次ビームが照射されるのを防げれば
楕円形や矩形など任意の形を選択できる。又、絞り板と
キャップを一体構造で作成しても良い。By doing so, even if the sample liquid collects on the peripheral edge portion a of the opening 12 of the cap 13 described above, the diaphragm plate is not formed on this portion.
It is blocked by 15 and is not irradiated with the primary beam and is not ionized. Therefore, the memory phenomenon can be completely prevented. The shape of the opening formed in the diaphragm plate 15 is not limited to a circular shape, and an arbitrary shape such as an elliptical shape or a rectangular shape can be selected as long as the peripheral portion a can be prevented from being irradiated with the primary beam. Further, the diaphragm plate and the cap may be formed as an integral structure.
第２図は本発明の他の実施例を示す。本実施例では多孔
性部材１０′が周縁部に円筒状のスカートを持つように
成型されると共に、キャップ先端部分で多孔性部材表面
とキャップとの間に隙間Ｇがあくように配置されてい
る。そのため、キャップと多孔性部材の表面とが接する
境界部分ａがスカート部にまで後退し、この部分ａに試
料液がたまっても一次ビームはキャップ１３によって遮
られて照射されない。FIG. 2 shows another embodiment of the present invention. In this embodiment, the porous member 10 'is molded so as to have a cylindrical skirt in the peripheral portion, and is arranged so that a gap G is formed between the surface of the porous member and the cap at the tip of the cap. . Therefore, the boundary portion a where the cap and the surface of the porous member are in contact with each other recedes to the skirt portion, and even if the sample solution collects on this portion a, the primary beam is blocked by the cap 13 and is not irradiated.
［効果］ 以上詳述した如く、本発明によれば、メモリ現象を完全
に防止することのできる質量分析装置用イオン源が実現
される。[Effect] As described in detail above, according to the present invention, an ion source for a mass spectrometer capable of completely preventing a memory phenomenon is realized.
第１図及び第２図は夫々本発明の一実施例の構成を示す
部分断面図、第３図及び第４図は従来例を説明するため
の図、第５図は特願昭６２−２０１８４号に提案された
装置を説明するための断面図、第６図は多孔性部材中の
試料液の流れを説明するための図である。 ２：イオン源 ５：一次粒子ビーム発生器 ７：導入管 １０，１０′：多孔性部材 １２：開口部 １３：キャップ １５：絞り板1 and 2 are partial cross-sectional views showing the structure of an embodiment of the present invention, FIGS. 3 and 4 are drawings for explaining a conventional example, and FIG. 5 is Japanese Patent Application No. 62-20184. FIG. 6 is a cross-sectional view for explaining the apparatus proposed in No. 6, and FIG. 6 is a view for explaining the flow of the sample liquid in the porous member. 2: Ion source 5: Primary particle beam generator 7: Introduction tube 10, 10 ': Porous member 12: Opening 13: Cap 15: Aperture plate
Claims (1)
めの導入管と、該導入管の先端に取付けられる多孔性部
材と、該多孔性部材を通りその表面に滲出した試料液に
照射する一次ビームを発生する手段とを備えた質量分析
装置用イオン源において、前記多孔性部材の表面におけ
る試料液の滲出領域を規定する開口を有する包囲体を該
多孔性部材に密接して被せると共に、該開口の前記多孔
性部材表面と接する周縁部分の近傍に前記一次ビームが
照射されるのを防止する遮蔽体を設けたことを特徴とす
る質量分析装置用イオン源。1. An introduction tube for introducing a sample solution into the ion source from the outside, a porous member attached to the tip of the introduction tube, and a sample solution exuded on the surface through the porous member to irradiate the sample solution. In an ion source for a mass spectrometer provided with a means for generating a primary beam, while closely covering the porous member with an enclosure having an opening that defines an exudation region of the sample liquid on the surface of the porous member, An ion source for a mass spectrometer, wherein a shield for preventing irradiation of the primary beam is provided in the vicinity of a peripheral portion of the opening in contact with the surface of the porous member.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62192097A JPH0626108B2 (en) | 1987-07-31 | 1987-07-31 | Ion source for mass spectrometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62192097A JPH0626108B2 (en) | 1987-07-31 | 1987-07-31 | Ion source for mass spectrometer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6435846A JPS6435846A (en) | 1989-02-06 |
| JPH0626108B2 true JPH0626108B2 (en) | 1994-04-06 |
Family
ID=16285595
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62192097A Expired - Lifetime JPH0626108B2 (en) | 1987-07-31 | 1987-07-31 | Ion source for mass spectrometer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0626108B2 (en) |
-
1987
- 1987-07-31 JP JP62192097A patent/JPH0626108B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6435846A (en) | 1989-02-06 |
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