JP4767864B2 - 質量分析方法と装置 - Google Patents
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Images
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
- H01J49/16—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission
- H01J49/168—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission field ionisation, e.g. corona discharge
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/0013—Miniaturised spectrometers, e.g. having smaller than usual scale, integrated conventional components
- H01J49/0018—Microminiaturised spectrometers, e.g. chip-integrated devices, Micro-Electro-Mechanical Systems [MEMS]
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0431—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for liquid samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
- G01N30/6095—Micromachined or nanomachined, e.g. micro- or nanosize
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7233—Mass spectrometers interfaced to liquid or supercritical fluid chromatograph
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Electron Tubes For Measurement (AREA)
Description
XH++M → X+MH+ (I)
(X−H)―+M → X+(M−H)―(II)
M+e− → M− (III)
http://www. microchem.com/products/su eight. htm
試料の流速:1μl/分
霧状ガスの流速:1.04l/分(理論設定値)
カーテンガスの流速:0.95l/分
コロナ放電電流:0.1μA
ヒーターの電圧:12/24V(水平モデルの温度、約70℃/195℃に対応)
他の値は測定プログラムの初期値である。
Claims (28)
- 調査すべき試料を含む溶液を気化器内で気化し、気化した試料溶液を気体流を用いてコロナ放電帯内に噴霧し、ここで調査すべき試料をコロナ放電を用いてイオン化して気相イオンを発生させ、該イオンを分離し、検出器に指向させて試料を質量分析により調べるに当たり、
マイクロメカニカル構造として製造され、
溶液用流路網及び該溶液の供給に使用し得るキャリアガス用流路網並びにヒーターを備え、これらすべてをモノリシック構造内に含め、
気化帯及びコロナ放電帯を備え、これらを単一のマイクロメカニカル構造中に一体化してなる気化器を使用することを特徴とする質量分析により試料を調査する方法。 - 前記流路網を、それらを通過する液体の流量が100μl/分未満、より好適には10μl/分未満であるような大きさにする請求項1記載の方法。
- 1つ以上のウエファ用に設計した流路網と、ヒーターとを備えるマイクロメカニカル構造を使用する請求項1または2記載の方法。
- 気体及び液体用流路網を形成する基板ウエファ及び該基板ウエファに付着し、試料溶液を気化させるためのヒーターをパターン化したカバーウエファとを備える構造を使用する
請求項3記載の方法。 - 気化した試料溶液を、空気の存在下通常の大気圧でコロナ放電によってイオン化する請求項1〜4のいずれかに記載の方法。
- コロナ放電帯が、少なくとも先端の近傍における電界強度が空気のコロナ放電閾値を超えるように質量分析器のカーテンプレートに対して高い電圧に接続した針状電極を備える請求項1〜5のいずれかに記載の方法。
- カーテンプレートに対する針状電極の電位が少なくとも1kV以上で、電極の先端近傍における最大の電界強度が約50kV/mmである請求項6記載の方法。
- 極性化合物、非極性化合物、中性化合物又はイオン化合物を調査し、調査すべき試料を溶離液として用いる極性又は非極性溶媒に溶解して試料溶液を形成する請求項1〜7のいずれかに記載の方法。
- 前記化合物を調査し、そのモル質量が大きくても2000Da、最も好適には大きくても1000Daである請求項8に記載の方法。
- 調査すべき試料の液体流量を約10μl/分未満の値に設定し、試料の供給に用いるキャリアガスの流量を少なくとも約50μl/分の値に設定する請求項1〜9のいずれかに記載の方法。
- 試料を大気圧化学イオン化(APCI)法を用いてイオン化する請求項1〜10のいずれかに記載の方法。
- インジェクションに用いる気体の流れを試料の流れ方向と実質的に直交に供給する請求項1〜11のいずれかに記載の方法。
- 気体の流れを、液体の流れの方向で該液体の供給開口前で装置に供給する請求項1〜12のいずれかに記載の方法。
- 気体の流れを一つの供給開口を介して供給して、該気体流を試料を含む液体の流れの周りに分配して均質な混合物を形成する請求項12又は13に記載の方法。
- 調査すべき試料を含む溶液を気化するための気化器と、該気化器に接続し、調査すべき試料を大気圧化学イオン化(APCI)法によってイオン化して荷電粒子を発生させるコロナ放電装置と、該コロナ放電装置に接続して荷電粒子を検出するための検出装置と、電界及び/又は磁界を用いて荷電粒子をコロナ放電装置から検出器に指向させるための手段とを備える質量分析により試料を調べる装置において、
前記気化器をマイクロメカニカル構造として製造するとともに、
前記気化器が溶液用の流路網および該溶液を供給するのに使用し得るキャリアガス用流路網並びに気化器のヒーターとを備え、これら全てをモノリシック構造内に含ませるものであり、
前記気化器が気化帯及びコロナ放電帯を備え、これらを単一のマイクロメカニカル構造に一体化して気化器とコロナ放電装置との組み合わせ物を形成することを特徴とする質量分析により試料を調査するための装置。 - 前記流路網が、それらを通過する液体の流量が100μl/分未満、より好適には10μl/分未満であるような大きさにする請求項15記載の装置。
- 2つ以上の部品を互いに接続してなるモノリシックブロックを備える請求項15又は16に記載の装置。
- 前記ブロックが、気体及び液体用流路網を形成したシリコンウエファと、試料溶液を気化するためのヒーターを形成したガラスプレートとを備える請求項17記載の装置。
- 前記ブロックが、気体及び液体用流路網を形成したガラスプレートと、試料溶液を気化するためのヒーターを形成したシリコンウエファとを備える請求項17記載の装置。
- 前記コロナ放電装置が、少なくとも電極の先端の近傍における電界強度が空気のコロナ放電閾値を超えるように質量分析器のカーテンプレートに対して高い電圧に接続した針状電極を備える請求項15−19のいずれかに記載の装置。
- 前記カーテンプレートに対する針状電極の電位を少なくとも1kVの値に設定し、電極の先端の近傍の電界の最大強度を少なくとも約50kV/分の値に設定する請求項20記載の装置。
- 全体にガラス構造として製造する請求項15−21のいずれかに記載の装置。
- 溶液を供給するために用いるキャリアガスの流路システムを気体の供給ノズルに接続し、該ノズルを溶液の流れ方向の上流に位置させ、これを通して気体を溶液の流れ方向と実質的に直交して装置に供給する請求項15−22のいずれかに記載の装置。
- 供給開口を経て供給した気体流を溶液の流路システムの周りに分配して均質な混合物にする請求項23記載の装置。
- ヒーターが、加熱抵抗体からなり、その前部を広くして流れ抵抗を減じ、気体と液体の混合帯の近傍のみを狭くし、これにより加熱抵抗体として働き実際の加熱帯を形成する請求項15−24のいずれかに記載の装置。
- 大気圧化学イオン化(APCI)法によってイオン化するために供給する気化試料を生成するためのマイクロメカニカル装置として製造し、
溶液用の流路網及び該溶液を供給に使用し得るキャリアガス用流路網並びに気化器のヒーターとを備え、これら全てをモノリシック構造内に含め、
気化帯及びコロナ放電帯を備え、これらを単一のマイクロメカニカル構造中に一体化した気化器の使用。 - 少なくとも調査すべき試料用の流路網及び該試料を供給するのに使用し得るキャリアガス用流路網並びに試料を気化するためのヒーターを形成したモノリシックブロックを備え、ここで前記流路網を、それらを通過する流量が100μl/分未満であるような大きさにした請求項26記載の気化器の使用。
- 調査すべき試料のモル質量がせいぜい約2000Daである請求項27記載の気化器の使用。
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PCT/FI2004/000683 WO2005047848A2 (en) | 2003-11-14 | 2004-11-15 | Method and apparatus for mass spectrometric analysis |
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US8716655B2 (en) * | 2009-07-02 | 2014-05-06 | Tricorntech Corporation | Integrated ion separation spectrometer |
JP5995643B2 (ja) * | 2012-10-11 | 2016-09-21 | ヒューマン・メタボローム・テクノロジーズ株式会社 | 酸性化合物の検出方法 |
CA2916138C (en) * | 2013-06-21 | 2023-03-21 | Smiths Detection Montreal Inc. | Method and device for a coated corona ionization source |
EP3109612A1 (en) * | 2015-06-26 | 2016-12-28 | Nina Wojtas | Mems deposition trap for vacuum transducer protection |
US11162972B2 (en) * | 2018-05-23 | 2021-11-02 | University Of Central Florida Research Foundation, Inc. | Resonant MEMS piezoelectric sensor |
JP6922961B2 (ja) * | 2018-10-18 | 2021-08-18 | 株式会社村田製作所 | 回転運動検出用微小電気機械デバイス |
US20230024038A1 (en) * | 2020-02-28 | 2023-01-26 | Georgetown University | Apparatus and methods for detection and quantification of elements in molecules |
DE102020214695B4 (de) * | 2020-11-23 | 2022-06-09 | Micro-Sensys Gmbh | Vorrichtung zur Ermittlung eines Füllstands einer Flüssigkeit in einem Behälter |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS60127453A (ja) * | 1983-12-13 | 1985-07-08 | Hitachi Ltd | 大気圧イオン化式試料導入装置 |
JPH042033A (ja) * | 1990-04-18 | 1992-01-07 | Hitachi Ltd | 試料のイオン化および質量分析のための装置 |
JP2000088808A (ja) * | 1999-10-13 | 2000-03-31 | Hitachi Ltd | 質量分析計及びそのイオン源 |
JP2002524755A (ja) * | 1998-09-17 | 2002-08-06 | アドヴィオン バイオサイエンシィズ インコーポレイテッド | 一体化モノリシックマイクロ加工したエレクトロスプレーと液体クロマトグラフィーのシステムおよび方法 |
US6610978B2 (en) * | 2001-03-27 | 2003-08-26 | Agilent Technologies, Inc. | Integrated sample preparation, separation and introduction microdevice for inductively coupled plasma mass spectrometry |
Family Cites Families (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5259254A (en) * | 1991-09-25 | 1993-11-09 | Cetac Technologies, Inc. | Sample introduction system for inductively coupled plasma and other gas-phase, or particle, detectors utilizing ultrasonic nebulization, and method of use |
US5750988A (en) * | 1994-07-11 | 1998-05-12 | Hewlett-Packard Company | Orthogonal ion sampling for APCI mass spectrometry |
EP1155435A4 (en) | 1999-01-08 | 2004-08-11 | Univ Northeastern | ELECTRO-PNEUMATIC DISTRIBUTOR FOR MULTIPLEX ANALYTICAL MICROSYSTEM DEVICES |
US6690004B2 (en) * | 1999-07-21 | 2004-02-10 | The Charles Stark Draper Laboratory, Inc. | Method and apparatus for electrospray-augmented high field asymmetric ion mobility spectrometry |
US6649908B2 (en) * | 2001-09-20 | 2003-11-18 | Agilent Technologies, Inc. | Multiplexing capillary array for atmospheric pressure ionization-mass spectrometry |
GB2391694B (en) * | 2002-08-01 | 2006-03-01 | Microsaic Systems Ltd | Monolithic micro-engineered mass spectrometer |
US7417225B2 (en) * | 2002-09-25 | 2008-08-26 | Thermo Finnigan Llc | Apparatus and method for adjustment of ion separation resolution in FAIMS |
US7057170B2 (en) * | 2004-03-12 | 2006-06-06 | Northrop Grumman Corporation | Compact ion gauge using micromachining and MISOC devices |
GB2422951B (en) * | 2005-02-07 | 2010-07-28 | Microsaic Systems Ltd | Integrated analytical device |
-
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS60127453A (ja) * | 1983-12-13 | 1985-07-08 | Hitachi Ltd | 大気圧イオン化式試料導入装置 |
JPH042033A (ja) * | 1990-04-18 | 1992-01-07 | Hitachi Ltd | 試料のイオン化および質量分析のための装置 |
JP2002524755A (ja) * | 1998-09-17 | 2002-08-06 | アドヴィオン バイオサイエンシィズ インコーポレイテッド | 一体化モノリシックマイクロ加工したエレクトロスプレーと液体クロマトグラフィーのシステムおよび方法 |
JP2000088808A (ja) * | 1999-10-13 | 2000-03-31 | Hitachi Ltd | 質量分析計及びそのイオン源 |
US6610978B2 (en) * | 2001-03-27 | 2003-08-26 | Agilent Technologies, Inc. | Integrated sample preparation, separation and introduction microdevice for inductively coupled plasma mass spectrometry |
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US20090108193A1 (en) | 2009-04-30 |
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WO2005047848A2 (en) | 2005-05-26 |
FI119747B (fi) | 2009-02-27 |
FI20031658A (fi) | 2005-05-15 |
WO2005047848A3 (en) | 2005-08-18 |
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US7863559B2 (en) | 2011-01-04 |
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