JPS61116654A - Mass chromatography apparatus - Google Patents

Mass chromatography apparatus

Info

Publication number
JPS61116654A
JPS61116654A JP59237318A JP23731884A JPS61116654A JP S61116654 A JPS61116654 A JP S61116654A JP 59237318 A JP59237318 A JP 59237318A JP 23731884 A JP23731884 A JP 23731884A JP S61116654 A JPS61116654 A JP S61116654A
Authority
JP
Japan
Prior art keywords
mass
peak
cycle
scanning
chromatogram
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
Application number
JP59237318A
Other languages
Japanese (ja)
Other versions
JPH0574782B2 (en
Inventor
Katsuaki Shirato
白土 勝章
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 JP59237318A priority Critical patent/JPS61116654A/en
Publication of JPS61116654A publication Critical patent/JPS61116654A/en
Publication of JPH0574782B2 publication Critical patent/JPH0574782B2/ja
Granted legal-status Critical Current

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/022Circuit arrangements, e.g. for generating deviation currents or voltages ; Components associated with high voltage supply

Landscapes

  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Electron Tubes For Measurement (AREA)

Abstract

PURPOSE:To enable efficient use of memory capacity, by providing a control system for variable setting the cycle of mass scanning according to the peak range of chromatogram so that the frequency of scanning will be almost the same with respect to any peak. CONSTITUTION:A gas chromatograph 1 is connected to a mass spectrometer (an ion source 3, an ion acceleration electrode 4, a total ion detector 5, a magnetic field 6 for mass spectrograph, an ion detector 7 or the like) through an interface 2. An excitation power source circuit 8 generates a saw-tooth current to run current to the magnetic field 6, where this cycle thereof is controlled with a computer (CP)9 at each one cycle of mass scanning. The CP9 samples the output of the detector 5 at a fixed cycle to obtain a differentiation signal of a chromatogram depending on the difference between adjacent sampling data. The CP9 also has the cycle of mass scanning set for the first peak of the chromatogram and the circuit 8 is controlled by the cycle. On the other hand, the CP9 counts the time from the start to the end of the mass scanning to determine the scanning cycle at the next peak.

Description

【発明の詳細な説明】 イ、産業上の利用分野 本発明はマスクロマトグラフィを行うに適したククマト
グラフ質量分析計に関する。
DETAILED DESCRIPTION OF THE INVENTION A. Field of Industrial Application The present invention relates to a cumatograph mass spectrometer suitable for performing mass chromatography.

口、従来技術 マスクロマトグラフィと云うのは、試料分子を電子衝撃
法等でイオン化すると幾種類かの断片イオン(7yグメ
ントイオン)が生放され、フラグメントイオンのでき方
は匍々の物質を特徴づけるので、質量分析計でぐり返し
走査全行い幾種類かのイオンを選定して出力するようく
し、クロマトグラフで分離された試料成分を質量分析計
に導入し各イオンの時間的な増減を記録するもので、ク
ロマトグラフで分離され九試料成分の同定とか、クロマ
トグラフで分離不充分な成分の弁別が可能となる。
Conventional technology Mass chromatography is a process in which when sample molecules are ionized using an electron impact method, several types of fragment ions (7y fragment ions) are released, and the way these fragment ions are formed characterizes various substances. Therefore, the mass spectrometer performs multiple scans to select and output several types of ions, and the sample components separated by the chromatography are introduced into the mass spectrometer and the increase and decrease of each ion over time is recorded. This makes it possible to identify nine sample components that have been separated by chromatography, or to discriminate components that are insufficiently separated by chromatography.

マスクロマトグラフィを行う場合、質量分析計では磁場
形ては磁場を四重概形では高周波電圧をくり返し走査し
て特定のイオンのみをコンビーータを用いて選択的に出
力して夫鳥のイオンの検出強度を記録する。このとき質
量走査の周期はクロマトグラフの試料成分の一つのピー
クの幅内で何回かの走査が行われるようにしておくこと
が必要である。
When performing mass chromatography, a mass spectrometer repeatedly scans a magnetic field (or quadruple-shaped magnetic field) or a high-frequency voltage and selectively outputs only specific ions using a combeater to determine the detection intensity of the husband ion. Record. At this time, it is necessary to set the period of mass scanning so that several scans are performed within the width of one peak of the sample component on the chromatograph.

所がクロマトグラフでキャピラリカラムを用いたような
場合、始めに出て来る試料成分のピークは非常に幅がせ
まくシャープであるが、後になる程次第くピーク幅が広
がって来る。このような場合、質量分析計の質量走査の
周期は始めに出て来るシャープなピークに合せて短かく
設定されるので、後の方の幅の広(’715たピークに
対しては、一つのピークにおける質量走査の回数が大へ
ん多くなり、イオン検出出力データをコンビ為−タ内の
メモリに格納し、後でデータの解析を行う場合メモリの
必要容量が増大し、記憶容量の無駄使いとなっていた。
However, when a capillary column is used in a chromatograph, the peaks of the sample components that appear at the beginning are very narrow and sharp, but the peak widths gradually become wider later on. In such cases, the mass scanning period of the mass spectrometer is set short to match the sharp peak that appears at the beginning. The number of mass scans for a single peak becomes very large, and if the ion detection output data is stored in the memory of the combinator and the data is analyzed later, the required memory capacity increases and the storage capacity is wasted. It became.

ハ、 目 的 本発明はマスクロマトグラフィを行う(当りて必要メモ
リ容量の不必要な増大を抑制し、メそり容量の効率的使
用を可能にすることを目的とする。
C. Purpose The present invention aims to perform mask chromatography by suppressing unnecessary increases in memory capacity and enabling efficient use of memory capacity.

二、構成 本発明はクロマトグラフによって分離された試料成分ビ
ークの幅に応じて質量分析計の質量走査周期を自動的に
変えシャープなピークでもブロードなピークで4一つの
ピークに対する質量走査の回数が略同じになるようにし
九マスクロマトグラフィ装置を提供する。
2. Configuration The present invention automatically changes the mass scanning period of the mass spectrometer according to the width of the sample component peak separated by chromatography. A nine-mass chromatography apparatus is provided so as to be substantially the same.

ホ、*施例 第1図は本発明の一実施例の構成を示す。1はガスクロ
マトグラフ、2はガスクロマトグラフと質量分析計とを
結合する分子セパレータ等のインター7j−−ス、3は
イオン源、4はイオン加速電極、5は全イオン検出器、
6は貫通分析用磁場、7はイオン検出器で、検出された
イオン強度データハコンビ為−夕9の内部に格納される
。コンビーータ9はまた、装置全体を制御している。
E. *Embodiment FIG. 1 shows the configuration of an embodiment of the present invention. 1 is a gas chromatograph, 2 is an interface such as a molecular separator that connects the gas chromatograph and the mass spectrometer, 3 is an ion source, 4 is an ion accelerating electrode, 5 is a total ion detector,
6 is a magnetic field for penetrating analysis, 7 is an ion detector, and the detected ion intensity data is stored inside the combination unit 9. The combiner 9 also controls the entire device.

10はイオン加速電圧を発生している電源回路8は磁場
に電流を流すための励磁電源回路である。
A power supply circuit 8 generating an ion accelerating voltage is an excitation power supply circuit 10 for causing a current to flow through the magnetic field.

励磁電源回路8は第2図に示すような鋸歯状電流を発生
して磁場6#′C電流を流しておシ、第2図のTが質量
走査の一周期で、コンビーータ9によってこの周期Tが
制御されている。第3図はクロマトグラムの一例で全イ
オン検出@5の出力の記録である。コンビ1−夕9は全
イオン検出器5の出力を一定周期でサンプリングしてお
り、相隣るサシプリングデータの差によってクロマトグ
ラムの微分信号を得ている。もっともこの微分信号を得
る方法は任意である。全イオン検出器を用いないでくり
返し走査を行なって得られた全てのイオンを加算してク
ロマトグラムとし、このクロマトグラムの信号を微分し
てもよい。
The excitation power supply circuit 8 generates a sawtooth current as shown in FIG. 2 to flow a magnetic field 6#'C current, and T in FIG. is controlled. FIG. 3 is an example of a chromatogram, which is a record of the output of total ion detection@5. The combinations 1 to 9 sample the output of the total ion detector 5 at regular intervals, and obtain a differential signal of the chromatogram based on the difference between adjacent sampling data. However, any method can be used to obtain this differential signal. All ions obtained by repeated scanning without using a total ion detector may be added to form a chromatogram, and the signals of this chromatogram may be differentiated.

コンビーータ9にはクロマトグラムの最初のピークに対
する質量走査の周期が設定してあり、最初のピークに対
してはコンビ為−夕9はこの周期によりて励磁電源回路
81!を制御している。他方コンビーータ9は質量走査
の開始から終了までの時間を計数して、その時間管適当
に選択して設定しである整数で割算して得られる値の下
位の桁を切捨チー次回のピークにおける質量走査の周期
とする。
A mass scanning cycle for the first peak of the chromatogram is set in the combiner 9, and the excitation power supply circuit 81! is controlled. On the other hand, the converter 9 counts the time from the start to the end of the mass scan, selects and sets the time tube appropriately, and divides the obtained value by a certain integer, truncating the lower digits and calculating the next peak. Let be the period of mass scanning at .

こ\で上記適当に選択して設定しである整数は一つのピ
ークにおける質量走査の回数であり、4とか5戒は10
と云った整数を設定する。この実施例はクロマトグラム
のピークは相隣るものは余りピーク幅が変らず、かつ次
第にピーク幅が広がると云う傾向に立脚して、一つのピ
ークの幅くよって次のピークにおける走査周期を決める
ものである。
Here, the integer selected and set appropriately above is the number of mass scans for one peak, and 4 or 5 precepts is 10.
Set an integer such as . In this example, the scanning period for the next peak is determined based on the width of one peak, based on the tendency that the width of neighboring peaks in a chromatogram does not change much, and the width of the peak gradually increases. It is something.

走査周期を決める他の実施例は全イオン検出器50出力
の微分信号が成る値を超え、次にその値より大きく設定
した別の値を超える迄の時間を計数し、この時間によっ
てそのピークの幅を推定して走査周期を決めるもので、
上記時間に係数を掛算した値を走査周期とする。更に他
の方法としては走査周期をクロマトグラフに試料を導入
した時点からの時間の関数として、周期算定の式を作っ
ておき、プログラムによって走査周期を決定する。
Another example of determining the scanning period is to count the time until the differential signal of the output of the total ion detector 50 exceeds a value and then exceed another value set larger than that value, and use this time to determine the peak of the peak. The scanning period is determined by estimating the width.
The value obtained by multiplying the above time by the coefficient is set as the scanning period. Still another method is to create a period calculation formula in which the scanning period is a function of time from the time when the sample is introduced into the chromatograph, and to determine the scanning period by a program.

へ、効 果 本発明によればマスクロマトグラフィを行プ場合、クロ
マトグラムO各ピークとも大体同回数ずつ質量走査が繰
返されるので、幅の広いピークに対して不易l!に大量
のデータが蓄積されることがなく、メモリの容量の有効
利用が達成される。
Effects According to the present invention, when mass chromatography is performed, mass scanning is repeated approximately the same number of times for each peak in the chromatogram, so it is difficult to scan a wide peak. A large amount of data is not accumulated in the memory, and memory capacity is effectively utilized.

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

第1図は本発明の一5!施例の構成を示すブロック図、
第2図はイオン加速電圧の波形グラフ、第3図はクロマ
トグラムの一例のグラフである。 J・・・ガスクロマトグラフ、2・・・インターフェー
ス、3・・・イオン源、4・・・イオン加速電極、5・
・・全イオン検出器、6・・・質量分析用磁場、7・・
・イオン検出器、10・・・イオン加速電圧電源回路、
8・・・励磁電源回路 第1図
Figure 1 shows part 5 of the present invention! A block diagram showing the configuration of the example,
FIG. 2 is a waveform graph of the ion acceleration voltage, and FIG. 3 is a graph of an example of a chromatogram. J... Gas chromatograph, 2... Interface, 3... Ion source, 4... Ion acceleration electrode, 5...
...All ion detector, 6...Magnetic field for mass spectrometry, 7...
・Ion detector, 10... ion acceleration voltage power supply circuit,
8...Excitation power supply circuit diagram 1

Claims (4)

【特許請求の範囲】[Claims] (1)クロマトグラムのピークの幅に応じて質量走査の
周期を、何れのピークに対しても走査回数が略同程度に
なるように可変設定する制御系を設けたマスクロマトグ
ラフィ装置。
(1) A mass chromatography apparatus equipped with a control system that variably sets the period of mass scanning according to the width of a peak in a chromatogram so that the number of scans is approximately the same for any peak.
(2)一つのピークの幅を検出して次のピークの質量走
査周期を設定することを特徴とする特許請求の範囲第1
項記載のマスクロマトグラフィ装置。
(2) Claim 1, characterized in that the width of one peak is detected to set the mass scanning period of the next peak.
The mass chromatography apparatus described in Section 1.
(3)ピークの立上り速さを検出してそのピークに対す
る質量走査周期を設定することを特徴とする特許請求の
範囲第1項記載のマスクロマトグラフィ装置。
(3) The mass chromatography apparatus according to claim 1, wherein a mass scanning period for the peak is set by detecting the rising speed of the peak.
(4)質量走査周期を時間の関数として予め設定してお
くことを特徴とする特許請求の範囲第1項記載のマスク
ロマトグラフィ装置。
(4) The mass chromatography apparatus according to claim 1, wherein the mass scanning period is set in advance as a function of time.
JP59237318A 1984-11-09 1984-11-09 Mass chromatography apparatus Granted JPS61116654A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP59237318A JPS61116654A (en) 1984-11-09 1984-11-09 Mass chromatography apparatus

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP59237318A JPS61116654A (en) 1984-11-09 1984-11-09 Mass chromatography apparatus

Publications (2)

Publication Number Publication Date
JPS61116654A true JPS61116654A (en) 1986-06-04
JPH0574782B2 JPH0574782B2 (en) 1993-10-19

Family

ID=17013587

Family Applications (1)

Application Number Title Priority Date Filing Date
JP59237318A Granted JPS61116654A (en) 1984-11-09 1984-11-09 Mass chromatography apparatus

Country Status (1)

Country Link
JP (1) JPS61116654A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04326041A (en) * 1991-04-26 1992-11-16 Tokyo Gas Co Ltd Gas concentration measuring method and device
WO2003075308A1 (en) * 2002-03-04 2003-09-12 Mikhail Lvovich Troshkov Multi-collector magnetic mass spectrometer

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04326041A (en) * 1991-04-26 1992-11-16 Tokyo Gas Co Ltd Gas concentration measuring method and device
WO2003075308A1 (en) * 2002-03-04 2003-09-12 Mikhail Lvovich Troshkov Multi-collector magnetic mass spectrometer

Also Published As

Publication number Publication date
JPH0574782B2 (en) 1993-10-19

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