JPS6183958A - Method for calibrating mass of mass spectrometer - Google Patents

Method for calibrating mass of mass spectrometer

Info

Publication number
JPS6183958A
JPS6183958A JP59205161A JP20516184A JPS6183958A JP S6183958 A JPS6183958 A JP S6183958A JP 59205161 A JP59205161 A JP 59205161A JP 20516184 A JP20516184 A JP 20516184A JP S6183958 A JPS6183958 A JP S6183958A
Authority
JP
Japan
Prior art keywords
mass
condition
calibration
perform
ionization
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
Application number
JP59205161A
Other languages
Japanese (ja)
Inventor
Tsunezo Takeda
武田　常蔵
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shimadzu Corp
Original Assignee
Shimadzu Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shimadzu Corp filed Critical Shimadzu Corp
Priority to JP59205161A priority Critical patent/JPS6183958A/en
Publication of JPS6183958A publication Critical patent/JPS6183958A/en
Pending legal-status Critical Current

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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/022—Circuit arrangements, e.g. for generating deviation currents or voltages ; Components associated with high voltage supply

Landscapes

  • 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)

Abstract

PURPOSE:To make it possible to use a fluorine org. compound and to perform the accurate and highly reliable calibration of mass, in adapting a chemical ionization method (CI method), by changing over an analytical condition to a negative ion analytical condition at the time of the calibration of mass. CONSTITUTION:A computer 8 takes in the output signal of an ion detector 6 through a data interface 9 and sends a control signal to a power source apparatus 7 through a control interface 10 to control the voltage applied to a specimen ionization chamber 1 and an ion lens system 2. When an automatic adjusting mode is selected in performing mass analysis by using a CI method, the computer 8 introduces a standard specimen (fluorine org. compound) and reaction gas into the ionization chamber 1 at first to perform chemical ionization and performs the measurement of sensitivity under a positive ion analysis condition and subsequently performs the measurement of resolving power under the same condition and, thereafter, changes over an analytical condition to a negative ion analysis condition to perform the calibration of mass and again return said condition to a positive ion analysis condition to perform other adjustment. By this method, the accurate and highly reliable calibration of mass can be performed.

Description

【発明の詳細な説明】 イ・　産業上の利用分野 本発明は質量分析装置における質量較正方法に関し、特
にＣＩイオン化法を用いる場合の質量較正方法に関する
。DETAILED DESCRIPTION OF THE INVENTION A. Field of Industrial Application The present invention relates to a mass calibration method in a mass spectrometer, and particularly to a mass calibration method when using the CI ionization method.

口・　従来技術 弗 質量分析装置の質量較正には沸素系有機化合物耶 を標準試料として用いる。標準試料として沸素系有機化
合物を用いるのは、分子量が大きくて、しかも沸点が低
いので、一度に広範囲の質量較正ができ、容易に気体状
態で質量分析装置に導入することができるからである。- Conventional technology For mass calibration of fluoro mass spectrometers, a fluorine-based organic compound, i.e., is used as a standard sample. The reason why fluorine-based organic compounds are used as standard samples is that they have large molecular weights and low boiling points, so mass calibration can be performed over a wide range at once, and they can be easily introduced into the mass spectrometer in a gaseous state. .

質量分析装置において試料をイオン化する方法には１１
４法（電子衝撃法）、Ｃ工法（化学イオン化法）等があ
り、質量分析装置のイオン加速電圧を同じに設定した場
合でも、イオン化室内のガス圧力がＥ工法とｐ２工法と
で大きく異ること等のために、Ｅ工法とＣ工法とでは実
効的なイオン加速電圧が異っている。このためＥ工法、
Ｃ工法夫々に対して質量較正を行うのが弗 望ましいのであるが、沸素系有機化合物はＥ工法の場合
イオン化効率も良く、また多種のイオンを生ずるので質
量較正にとって甚だ都合が良いのであるが、Ｃ工法では
正イオンのイオン化効率が低くまたイオン種も少いので
、質量較正は困難である。このため従来はＣＩイオン化
法を用いて分析を行う場合でも質量較正にはＥエイオン
化法における質量較正結果を用いている。There are 11 methods for ionizing a sample in a mass spectrometer.
There are 4 methods (electron impact method), C method (chemical ionization method), etc., and even if the ion acceleration voltage of the mass spectrometer is set to the same, the gas pressure in the ionization chamber is significantly different between E method and P2 method. For this reason, the effective ion accelerating voltage is different between the E construction method and the C construction method. For this reason, E method,
It is desirable to perform mass calibration for each method, but fluorine-based organic compounds have good ionization efficiency in method E and produce a wide variety of ions, which is extremely convenient for mass calibration. In method C, the ionization efficiency of positive ions is low and the number of ion species is small, so mass calibration is difficult. For this reason, conventionally, even when analysis is performed using the CI ionization method, mass calibration results using the E-ionization method are used for mass calibration.

八　発明が解決しようとする問題点 上述したように従来はＣＩイオン化法を用いる場合、質
量較正が困難なため、Ｅエイオン化法による質量較正の
結果を援用しており、ＣＩイオン化法を用いて分析を行
った場合、測定される質量には誤差があるっ本発明はＣ
Ｉイオン化法を用いる場合の質量分析装置の調整におい
て、質量較正にもＣＩイオン化法を用い得るようにして
、ＣＩイオン化法による分析の場合の質量測定の精度を
高めようとするものである。8. Problems to be Solved by the Invention As mentioned above, conventionally when using the CI ionization method, mass calibration is difficult, so the results of mass calibration by the E-ionization method are used. When an analysis is performed, there is an error in the measured mass.
In adjusting a mass spectrometer when using the I ionization method, the CI ionization method can also be used for mass calibration, thereby increasing the accuracy of mass measurement in the case of analysis using the CI ionization method.

二８問題解決のだめの手段 弗 廃棄系有機化合物はＣＩイオン化の場合正イオンのイオ
ン化効果は低いが、負イオンの場合は効率良くイオン化
される。本発明はこの点に着眼して、負イオン測定の条
件で質量較正を行うようにしだ。28 Remedies for Solving Problems Fluorous waste organic compounds have a low positive ionization effect when CI ionized, but are efficiently ionized when negative ions are used. The present invention focuses on this point and performs mass calibration under negative ion measurement conditions.

ホ０作用 質量分析装置の分析前の調整項目は、感度１分解能、質
量較正等であるが、ＣＩイオン化法で分境 析を行う場合、感度２分解能の測定は廃棄化合物の正の
ＣＩイオン化で得られる少数のイオンでも充分であるか
ら、正イオン測定条件でも調整は可能である。質量較正
に当っては負イオン測定条件で測定を行うのであるが、
正イオン測定条件と負イオン測定条件とでの測定される
質量数のずれは理論上はＯであり、実際上もきわめて小
さいと認められるので、負イオン測定条件で質量較正を
行っても充分な精度が得られる。Adjustment items before analysis for a zero-effect mass spectrometer include sensitivity 1 resolution, mass calibration, etc. However, when performing differential analysis using the CI ionization method, measurement of sensitivity 2 resolution is performed by positive CI ionization of waste compounds. Since the small number of ions obtained is sufficient, it is possible to adjust the positive ion measurement conditions. During mass calibration, measurements are performed under negative ion measurement conditions.
The difference in mass numbers measured between positive ion measurement conditions and negative ion measurement conditions is theoretically 0, and it is recognized that it is extremely small in practice, so even if mass calibration is performed under negative ion measurement conditions, it is not sufficient Accuracy is obtained.

へ・　実　　施　　例 第１図は本発明の一実施例を示す。１は試料イオン化室
、２はイオンレンズ系、３は質量分析部の入口スリット
、４は質量分析部、５は質量分析部の出口スリット、６
はイオン検出器である。７は電源装置でイオン化室１と
入口スリットとの間及びレンズ系２の夫々に所定の電圧
を印加している。８は質量分析装置全体の動作を制御す
るコンピュータで、イオン検出器６の出力信号をデータ
インターフェース９を介して取込み、また制御インター
フェース１０を介して電源装置７に制御信号を送ってイ
オン化室？レンズ系等に印加する電圧を制御している。Embodiment FIG. 1 shows an embodiment of the present invention. 1 is a sample ionization chamber, 2 is an ion lens system, 3 is an entrance slit of the mass spectrometry section, 4 is a mass spectrometry section, 5 is an exit slit of the mass spectrometry section, 6
is an ion detector. A power supply 7 applies a predetermined voltage between the ionization chamber 1 and the entrance slit and to the lens system 2, respectively. Reference numeral 8 denotes a computer that controls the operation of the entire mass spectrometer, which takes in the output signal of the ion detector 6 via the data interface 9, and sends a control signal to the power supply device 7 via the control interface 10 to control the ionization chamber. It controls the voltage applied to the lens system, etc.

上述装置においてＣＩイオン化法を用いた質量分析を行
う場合の自動調整モードが選択されだ場合、コンピュー
タ８は第２図に示す順序で調整動作を進行させて行く。When the automatic adjustment mode for performing mass spectrometry using the CI ionization method in the above-mentioned apparatus is selected, the computer 8 proceeds with the adjustment operation in the order shown in FIG.

まずイオン化室に前述した都 標準試料（′ｓ素系有機化合物）及び反応ガスを導入し
、ＣＩイオン化を行うと共に、正イオン分析条件で感度
測定を行い、次いで同条件で分解能測定を行い、その後
負イオン分析条件に切換えて質量較正を行い、再び正イ
オン分析条件に戻してその他の調整を行う。First, the aforementioned Tokyo standard sample ('s elemental organic compound) and reaction gas are introduced into the ionization chamber, CI ionization is performed, and sensitivity measurement is performed under positive ion analysis conditions.Next, resolution measurement is performed under the same conditions. Switch to negative ion analysis conditions and perform mass calibration, then return to positive ion analysis conditions and make other adjustments.

ト、効果 本発明は上述したようにＣＩイオン化法を適用する場合
において質量較正時に負イオン分析条件部 に切換えるので沸素系有機化合物を用いることができ、
Ｅエイオン化法を適用する場合の質量較正と同じ標準試
料が用いられると云う便宜があり、しかもＣＩイオン化
法における質量較正が直接（Ｋ工法の結果の援用でなく
）行われるので、正確で信頼性の高い質量較正ができる
っG. Effect As mentioned above, when applying the CI ionization method, the present invention switches to the negative ion analysis condition section during mass calibration, so fluorine-based organic compounds can be used.
It is convenient that the same standard sample is used for mass calibration when applying the E-A ionization method, and mass calibration for the CI ionization method is performed directly (instead of relying on the results of the K method), making it accurate and reliable. Highly accurate mass calibration is possible.

【図面の簡単な説明】[Brief explanation of the drawing]

第１図は本発明が適用される質量分析装置の構成を示す
ブロツク図、第２図は上記実施例におけるＣＩイオン化
法を用いる場合の自動調整動作のフローを示すフローチ
ャートである。FIG. 1 is a block diagram showing the configuration of a mass spectrometer to which the present invention is applied, and FIG. 2 is a flowchart showing the flow of automatic adjustment operation when using the CI ionization method in the above embodiment.

Claims (1)

【特許請求の範囲】[Claims] ＣＩイオン化法を用いた質量分析における自動調整モー
ドにおいて、標準試料としてＥＩイオン化法の場合の質
量較正に用いるのと同じ弗素系有機化合物を用い、質量
較正の段階において、質量分析装置を負イオン分析条件
に切換えるようにした質量分析装置の質量較正方法。In the automatic adjustment mode for mass spectrometry using the CI ionization method, the same fluorine-based organic compound used for mass calibration in the EI ionization method is used as the standard sample, and the mass spectrometer is set to perform negative ion analysis during the mass calibration stage. A mass calibration method for a mass spectrometer that changes the conditions.
JP59205161A 1984-09-29 1984-09-29 Method for calibrating mass of mass spectrometer Pending JPS6183958A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP59205161A JPS6183958A (en) 1984-09-29 1984-09-29 Method for calibrating mass of mass spectrometer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP59205161A JPS6183958A (en) 1984-09-29 1984-09-29 Method for calibrating mass of mass spectrometer

Publications (1)

Publication Number Publication Date
JPS6183958A true JPS6183958A (en) 1986-04-28

Family

ID=16502432

Family Applications (1)

Application Number Title Priority Date Filing Date
JP59205161A Pending JPS6183958A (en) 1984-09-29 1984-09-29 Method for calibrating mass of mass spectrometer

Country Status (1)

Country Link
JP (1) JPS6183958A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01120755A (en) * 1987-10-31 1989-05-12 Shimadzu Corp Mass spectrometry

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01120755A (en) * 1987-10-31 1989-05-12 Shimadzu Corp Mass spectrometry

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