JPS6041746A - Ci ion source - Google Patents
Ci ion sourceInfo
- Publication number
- JPS6041746A JPS6041746A JP58150825A JP15082583A JPS6041746A JP S6041746 A JPS6041746 A JP S6041746A JP 58150825 A JP58150825 A JP 58150825A JP 15082583 A JP15082583 A JP 15082583A JP S6041746 A JPS6041746 A JP S6041746A
- Authority
- JP
- Japan
- Prior art keywords
- ionization chamber
- ionization
- ion source
- exhaust port
- reaction
- 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
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
- H01J49/14—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers
- H01J49/145—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers using chemical ionisation
Landscapes
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Electron Tubes For Measurement (AREA)
Abstract
Description
本発明は、質量分析装置に用い−Ｃθｆ適なイオン源の
改良に関し、特に化学イオン化（Ｃｈｅｍｉｃａｌｌ
ｏｎｉｚａＬｉｏ＋＋ ： Ｃｌ ）イオン源の改良に
関１Ｊるものである。
第１図に従来のＣｌイΔン源の概略図を示Ｊ。
図において１はイオン源ハウジングで、その内部は油拡
散ポンプ２にＪ、って真空排気され、イオン化室３か配
置されている。該イオン化室３の側壁には試料導入口４
、反応カス専大口５、電子導入口６、及びイＡン出射１
−１７が段（）られ−Ｃいる。８は試料導入管、９は二
一ドルフ゛？、１０は反応カス供給管、１１は電子を発
生づるノイラメン１−１１２はイオン集束電極である。
上）本の如き構成にＪ３い−Ｃ，導入１」５からイオン
化室３内へ導入された反応カスは、導入１］ ６から導
入されｌこ電子にｊ、つＣイオン化される。イし４次に
、尋人口４から導入されｔこ試料が、その反応万スイＡ
ンどのブｌ−１トン移行反応によつＣイオン化される。
かかる従来例ては、イオン化室３内をイオン化に最適な
例えば１王旧゛１゛程１良の月力に保ら、１−１つイオ
ン源ハウジング内を十分な高真空に保つため、反応ガス
が漏れ１ｊしＪ°１ハＴ−導入口６及びイ調ン出ｑ・ｊ
Ｉｊ ７ ｆ／）径を例工＊ｒ１Ｅ）ＯＯ＋□ｍφ桿庶
ニ１儲定しくリ−り■を極めて少なくシ（いる。イの為
、イオン１ヒ室３内へ供給りる反応カスの量は０．１〜
０．／１１ｌｌｌ／分）１′度と）Φめ′Ｃ微少となり
、ニー１きル弁９どしＵ ｆ（７） 、、Ｉ、うな微少
岱の調整が可能な高精度のものが必要であく〉し、ニー
ドル弁９の：ｊンダクタンスの僅かな変化によってイオ
ン化室３内の圧力が大幅に変化しＣしようので、その調
整作業も細心の注意を必要とした。
本発明１；Ｊ −１−： ｉホした従来の問題点に鑑み
てなされたちの（゛、イオン化室に新たにｎ＋気口を設
The present invention relates to the improvement of an ion source suitable for -Cθf used in a mass spectrometer, and in particular to chemical ionization (Chemical ionization).
onizaLio++: 1J related to improvement of Cl) ion source. FIG. 1 shows a schematic diagram of a conventional Cl ion source. In the figure, 1 is an ion source housing, the inside of which is evacuated by an oil diffusion pump 2, and an ionization chamber 3 is arranged therein. A sample introduction port 4 is provided on the side wall of the ionization chamber 3.
, reaction scum exclusive large port 5, electron inlet 6, and ionic output 1
-17 is staged () and -C is there. 8 is the sample introduction tube, 9 is 21 dolphins? , 10 is a reaction waste supply pipe, and 11 is an ion focusing electrode 1-112 which generates electrons. Above) In a structure like a book, the reaction residue introduced into the ionization chamber 3 from introduction 1] 5 is introduced from introduction 1] 6 and is ionized into 1 electrons. 4 Next, the sample introduced from the population 4 is
C is ionized by a blue ton transfer reaction. In such a conventional example, the inside of the ionization chamber 3 is kept at the optimum power for ionization, for example, about 1000 yen, and the inside of the ion source housing is kept at a sufficiently high vacuum. Gas leaks 1j and J°1c T-inlet 6 and A-key outlet q・j
Ij 7 f/) diameter as an example *r1E) OO+ The amount is 0.1~
0. /11lll/min) 1' degrees and) Φ'C is minute, so a high-precision one is required that can adjust the minute height of the knee 1 kill valve 9. However, since a slight change in the inductance of the needle valve 9 would cause a significant change in the pressure within the ionization chamber 3, the adjustment work also required great care. Present invention 1; J-1-: This invention was made in view of the conventional problems mentioned above.
【）、該排気口を真空１１１気手段に接続し−ＣＣイン
タ化室内強制的に排気できるようにしたことを特徴どし
ている。以下、図面を用いＣ本発明を詳説覆る。
第２図は本発明の一実施例の構成を示づ概略図であり、
第１図の従来例と同一の構成要素には同一番目が付され
ている。第２図において、第１図と異なるのはイオン化
室３の側壁に新たに比較的太きな二】ンダクタンスを０
りるＪＪＩ気Ｄ Ｉ ３を設り、耕気管１４を介しく真
空ポンプ例えば１」−タリーポンプ１５に接続した＜−
＞、ｒある。
かかる構成となせば、υ１気口１３を介してイオン化室
３内がロータリーポンプ１５にＪ、すＩＪＩ気されるノ
こめ、ニードルづ１ゝりを介しくインン化至３内＋；二
＋ｔｔ給りる反応カスｔｉをＩ ＯｉｒＸあるいはイれ
以上に増してし、イオン化室３内はイオン化に最）凶な
Ｌｆ力に保たれ、旧−）イオン源ハウジング内を−１分
な高真空に保つことがＣ′さる。そのため、ニードル弁
０にＪ、る反応カス流量の設定に幅がぐさ、操作性は極
めて向下りる。
又、そのように反応ガスの流量を増せは、ニードル弁９
のコンダクタンスの変化（例えば振動あるいは湿度変化
等に起因した）がイオン化室３内のＬ１力に！うえる影
ν＾５も極端に小さくむり、そのＩｆ力変動にＪ、っ（
派４（弓る化成・インタ（いの変動（これが質量分析装
置から胃られるビーク強庶の変動に結び一つく）をｌｊ
、＋ｌｌペイことが＋ｉＪ自旨となる１゜本発明では上
述の如くイオン化室を強制的に排気Ｊるため、イオン化
室内に多量のカスを）９人りることができ、例えばｌＰ
ｉ吊分（１７装置（〜＋Ｓ）どｅイ＊ ’ｙ ｕ マｌ
−’ｊ ”ｔ ’） （１，Ｃ） 全結合し／、：ＩＣ
−ＭＳに用いることか（きる。第３図は本発明にががる
インタ源を１ｃｆｖｌｓに適用した実施例のｊｉ、：成
を示し、第２図と同一の構成要素には同一番号がイ」さ
れている。灸′；３図においで１６は高速液体りｌ］ン
トグラノ、′１７は液イ木り［１７Ｉ−グラノとインタ
源を結ぶインタフ■−）（゛ある。該インタフェース１
６内は真空ポンプ１８にｊ、ってｉｌｌ気されており、
液体り（］７１〜グラフ１６からの流出液はスプリッタ
′１９を介しＣインタフ１−ス１６内のノズル２０へ供
給される。該ノズルから小さな液滴のジ■ツトどし【１
噴出した流出液は、ス・１向配置べされた受りノズル２
１へ入則し、途中ヒータ２２による加熱を受０（気化さ
れつつイオン化’、＋ｉ＊ ３内へ送られる。
かかる構成に、１３いＣ、イオン化室内（は、液１小ク
ロマ１〜グフノ１Ｇからの流出液中の溶媒を反応カスと
してイオン化が行われる。即ら、導入に１４を介しく溶
媒を含む流出液がイオン化室内へ導入されると、導入口
６から入用した電子にＪ：つて溶媒（反応カス）が先ず
イオン化され、次いで該溶媒インタどのゾ１−１１〜ン
移行反応によつ−（流出液（気化しでいる）がイオン化
され、インン出剣ロアを（ｌしＵ貿量分析部へ送られる
。 。
本実施例Ｃは、イオン化に必要な反応カスが液体クロマ
ｊ・グラノからｊスられるため、試料）９人口４が反応
カス導入１１を兼ねる形と’ｔＩ：っ（いる。ぞしＣ、
イオン化芋へ導入され／ζ成分はｌｊ空ポンプにＪ、っ
てＪみやかに除去びれるため、？ｌ々１ホク１」７トグ
ラフから多量の流出液が供給され（も、イオン化室内を
イオン化に最適なｊ］］力に保つことができる。イれと
同時に、イオン化室へ導入されｊこ成分がいつまでもそ
の中に留まることが１１（（いのＣ１り［ｊ７１−グフ
ムの応答１’ｌか良好ど＜ｊる。
尚、本発明は一１述しｌこ実施例（Ｊ限定されることな
く低形がｉｉＪ能である。例えば、上記実施例のＪ”）
４ｉ： ＣＩ Ｎｊ 用−１’ Ａ ン１ｌＮｉ ニ
１ｉＪＪ ラ、ｌ’、’ｆｉ−ｉ ”ｆ Ｅｌｌ！撃イ
Ａンイン［ｌ）をＶ（けで行うことのζ゛きる所謂Ｃ１
／′ＥｌイＡン源にｔ）通用でいる。
又、イオン化室内に聞Ｌ１する１１Ｉ気口１３と反応ガ
ス導入［１５（ｕバ３図の実施例Ｃ（よムＩｃ Ｉ’ｊ
１カスン！２人口４）は対向配置ｒ１りるのが最ちＩＪ
Ｉ気効５（″か良いと考えられるが、揚台にＪ、っ′Ｃ
【。Ｌ適宜イｉ ／”Ｉ磨を成りｊ、うに配置）／、１
りることも考えられる。
又、ＩＪＩ気Ｉｉ−、＋ １３に接続される真空ポンプ
と（）（は、【」−タリーポンプに限らず、適当４ｊ流
路抵抗をＩＪＩ気管１７１に勺えることにまり油拡散ポ
ンプ等他の真空ポンプを用いることもできる。その場合
、真空ポンプとして油拡散ポンプ２を兼用りることｂ考
えられる。
又、ニードル弁９は、第３図の例のＪ、うにυｊ気管１
４に設ｉ」で如インン化室３内の圧力を調節りることが
可能ｅあるし、反応ガス供給包１０と排気管１／Ｉの双
方に設（〕るＪ、うにしＣも良い。[) is characterized in that the exhaust port is connected to a vacuum 111 means to forcibly exhaust air from the -CC interior chamber. Hereinafter, the present invention will be explained in detail with reference to the drawings. FIG. 2 is a schematic diagram showing the configuration of an embodiment of the present invention,
Components that are the same as those of the conventional example shown in FIG. 1 are numbered the same. In Fig. 2, the difference from Fig. 1 is that a relatively thick inductance has been added to the side wall of the ionization chamber 3.
A vacuum pump, e.g.
>, there are r. With this configuration, the inside of the ionization chamber 3 is supplied to the rotary pump 15 through the υ1 air port 13, and the inside of the ionization chamber 3 is supplied through the needles. The reaction mass is increased to IOirX or above, and the inside of the ionization chamber 3 is maintained at the Lf force that is most harmful to ionization, and the inside of the ion source housing is kept at a high vacuum of -1 minute. That's C'. Therefore, the setting of the reaction mass flow rate for the needle valve 0 is difficult, and the operability is extremely deteriorated. Also, to increase the flow rate of the reaction gas, use the needle valve 9.
Changes in the conductance (due to vibrations or humidity changes, for example) cause the L1 force in the ionization chamber 3! The rising shadow ν^5 is also extremely small, and due to the fluctuation of the If force, J...
Faction 4 (Yumiru Kasei/Inter (internal fluctuation) (this is connected to the fluctuation of the beak strength detected by the mass spectrometer) is lj
In the present invention, as described above, the ionization chamber is forcibly evacuated, so a large amount of waste can be left inside the ionization chamber.
i hanging (17 devices (~+S))
-'j ``t') (1, C) Fully connected /, :IC
- Can it be used in MS? Figure 3 shows the configuration of an embodiment in which the interface according to the present invention is applied to 1cfvls, and the same components as in Figure 2 are designated by the same numbers. In Figure 3, 16 is the high-speed liquid l]tograno, '17 is the liquid tree [17I-interface connecting the grano and the interface source -) (' is there. The interface 1
6 is illuminated by the vacuum pump 18,
The effluent from the liquid reservoir 71 to graph 16 is supplied via a splitter '19 to a nozzle 20 in the C interface 16. From the nozzle, a jet of small droplets [1
The ejected effluent is transferred to a receiving nozzle 2 arranged in one direction.
1, and is heated by the heater 22 on the way and is sent to the 0 (ionized while being vaporized) and +i*3. Ionization is performed using the solvent in the effluent from the ionization chamber as reaction residue.That is, when the effluent containing the solvent is introduced into the ionization chamber through the inlet 14, the electrons introduced from the inlet 6 are subjected to J: The solvent (reaction scum) is first ionized, and then the effluent (vaporized) is ionized by the solvent interzone transfer reaction, and the solvent (reaction residue) is ionized. In this Example C, since the reaction residue necessary for ionization is removed from the liquid chromatography, the sample) 9 population 4 also serves as the reaction residue introduction 11. (There it is. Zoshi C,
The ζ component introduced into the ionized potato is removed gracefully by the empty pump, so ? A large amount of effluent is supplied from the tograph to maintain the inside of the ionization chamber at the optimum power for ionization.At the same time as the ionization, it is introduced into the ionization chamber and the components are It is possible to stay there forever. The lower form is iiJ function (for example, J" in the above example)
4i: For CI Nj -1' A n1lNi Ni1iJJ La, l', 'fi-i "f Ell! Shoot A in [l] is performed with V (ke), so-called C1
/'El iA source t) It is common. In addition, the 11I air port 13 connected to L1 in the ionization chamber and the reaction gas introduced [15 (U
1 cassun! 2 population 4) facing arrangement r1 is the most IJ
5('' is considered to be good, but there is a J, t'C on the platform)
[. L appropriate i /"I polish it, place it in a sea urchin)/, 1
It is also possible that the In addition, the vacuum pump connected to the IJI trachea 171 and the vacuum pump connected to the IJI trachea 171 are not limited to the tally pump. It is also possible to use a vacuum pump.In that case, it is conceivable that the oil diffusion pump 2 can also be used as the vacuum pump.Also, the needle valve 9 can be used as the trachea 1 of the example shown in FIG.
It is possible to adjust the pressure inside the incubation chamber 3 by setting it in 4, and it is also good to set it in both the reaction gas supply chamber 10 and the exhaust pipe 1/I. .
第１図は従来のＣ１イＡン源の概略を示り図、第２図は
本発明によるＣ１イオン諒の一例を示す概略図、第３図
はり、 Ｃ−Ｍ Ｓに本発明を）＾出した例を示″ｔＪ
蹴略図である。
３：イオン化空、４：試料心入口、
５：反応ガス導入口、６：電子導入に１．７：インン出
用［１，８：試料導入管、９：二一ドルブ？、１Ｃ）：
反応ガス供給管、１１：ノイラメン１〜、′ド３１月気
１−１．１４：１ノ１気釣、コ５）゛日−クリーボン１
゜特許出願人
ト１木゛宙子株式会着
代表名 （Ｊｌ藤 −夫Figure 1 is a schematic diagram showing a conventional C1 ion source, Figure 2 is a schematic diagram showing an example of a C1 ion source according to the present invention, and Figure 3 is a diagram showing an example of a C1 ion source according to the present invention. Here is an example of "tJ"
This is a schematic diagram. 3: Ionization space, 4: Sample core inlet, 5: Reaction gas inlet, 6: For electron introduction 1.7: For in/out [1, 8: Sample introduction tube, 9: 21 Dorb? , 1C):
Reaction gas supply pipe, 11: Noiramen 1~, 'do 31 month air 1-1.
゜Patent Applicant To 1 Tree Chuko Co., Ltd. Representative Name (Jl Fuji - Husband)
Claims (1)
の試料導入口と、該イオン化某へ反応カスを導入りるＩ
こめの反応カス導入ＩＺＩと、該イオン化室内へ電子線
を入ｑ」させるための電子導入口と、該イオン化室内で
生成されたイＡンか取出されるイオン出射口とを備えた
ＣｌイＡン河１にＪ′ｉいて、前記イオン化室に聞１」
づる排気口を設り、該１１＋気［１を真空排気手段に接
続したことを特徴とりるＣｌイオン源。An ionization chamber, a sample introduction port for introducing a sample (81) into the ionization chamber, and an I for introducing reaction waste into the ionization chamber.
A Cl-I A is equipped with a reaction sludge introduction IZI, an electron introduction port for introducing an electron beam into the ionization chamber, and an ion exit port for taking out the ions generated in the ionization chamber. J'i is in the river 1, and 1 is in the ionization chamber.
A Cl ion source characterized in that an exhaust port is provided, and the 11+ gas [1] is connected to a vacuum evacuation means.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58150825A JPS6041746A (en) | 1983-08-18 | 1983-08-18 | Ci ion source |
| GB08419588A GB2146170B (en) | 1983-08-18 | 1984-08-01 | Ion source for mass spectrometer or the like |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58150825A JPS6041746A (en) | 1983-08-18 | 1983-08-18 | Ci ion source |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6041746A true JPS6041746A (en) | 1985-03-05 |
| JPS61705B2 JPS61705B2 (en) | 1986-01-10 |
Family
ID=15505222
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58150825A Granted JPS6041746A (en) | 1983-08-18 | 1983-08-18 | Ci ion source |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6041746A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS647466A (en) * | 1987-06-30 | 1989-01-11 | Shimadzu Corp | Ci ionization mass analyzer |
-
1983
- 1983-08-18 JP JP58150825A patent/JPS6041746A/en active Granted
Non-Patent Citations (1)
| Title |
|---|
| ANALYTICAL CHEMISTRY=1979 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS647466A (en) * | 1987-06-30 | 1989-01-11 | Shimadzu Corp | Ci ionization mass analyzer |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61705B2 (en) | 1986-01-10 |
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