JP3631919B2 - Mass spectrometry method and apparatus for sample, and mass spectrometry method for analyzing water quality - Google Patents

Description

【００７６】
測定しようとする目的の元素に、同じ質量数の分子イオンのスペクトルが重なり、測定を妨害する。記憶装置１０５は、このような干渉分子イオンを記憶している。表２に、Ａｒガスの分子イオンの例を示す。
【００７７】
【表２】

【００７８】
コントローラ１０２は、ＣＰＵ１０３の演算処理に基づき、同位体元素表示１０６を行い、干渉元素イオンすなわち同一質量数元素の削除１０７および／または干渉分子イオンの削除１０８を行って、測定イオンの質量数決定１０９を行う。
【００７９】
モニター１０４に画面表示しながら分子イオンを除外して測定イオンのみを残す方法について説明する。
【００８０】
（１）親イオンの決定、およびイオン導入
図１３に示すように、親イオンの質量数もしくは、測定金属である元素を選択すると、重なる分子イオンの表示を行う。
【００８１】
５６Ｆｅ を選択した場合は、 ＡｒＯ
８０Ｓｅ を選択した場合は、 ＡｒＡｒ
等を表示する。
【００８２】
反対に、測定試料の内容について、ユーザが判っている場合、分子イオンの構造式を入力することで、重なる親イオンを表示する。
【００８３】
ＡｒＯ を入力すると、 ５６Ｆｅ
ＡｒＡｒ を入力すると、 ８０Ｓｅ
等を表示する。
【００８４】
（２）アイソレーションの実施
図１４に示すように、アイソレーションの実施を行う。
【００８５】
（３）ＣＩＤを行い、親イオンを分解する。
【００８６】
図１５に示すように、親イオンを分解し、分解イオンおよび目的イオンの表示を行う。これらを画面に表示し、ユーザにパラメータを入力させ、ＦＮＦおよびＣＩＤのパラメータを決定する。
【００８７】
前述したプラズマは、Ａｒで生成させるため、非常に多くのＡｒ起因のイオンがプラズマ中に存在する。このＡｒ起因のイオンは、測定元素には無関係のため、妨害ピークになる。
【００８８】
３ＤＱＭＳでは、ナチュラルなデクラスタ反応が、３ＤＱＭＳ内部で起こるため、測定元素の分析の際、Ａｒ起因の分子イオン（ＡｒＡｒなどの分子イオン）を解裂させることができるので、分子イオンの妨害の発生を防止することができる。
【００８９】
次に、これらの装置によって画面上に測定元素の設定を行う方法について説明する。
【００９０】
例１：同位体の存在比を棒グラフで表示して測定元素を選択する例。
【００９１】
図１６は、起動時の画面であり、また、感度調整画面である。画面は、アイコン項目部１３１、条件設定部１３２、画面部１３３および状態表示部１３４から構成される。アイコン項目部１３１には、ファイル、表示、装置制御、条件編集、感度チューニング、データ、ツール、ウインドウ、ヘルプの各項目が設けられている。条件設定部１３２には、各種の条件設定ボタンが設けられている。画面部１３３には、その上部に、時間と信号強度の関係を表示する画面部と、その下部で、装置構成を表示する画面部が設けられている。状態表示部１３４は、検知項目表示を行うものである。
【００９２】
▲１▼周期律表
・フォーカスがある元素（選択元素）の原子番号、元素名、干渉元素を表示する。また、その元素の測定質量数に対応した同位体情報、干渉イオン情報を表示する。測定質量数なしのときは、推奨質量数を選択状態とする。
・左クリックまたはキーで元素を選択すると、指定された元素は、測定元素、測定可能な未選択元素、既知元素の順にエンドレスに選択状態が変更される。
・分析時に測定元素にしたときは、推奨質量数すべてを測定質量数とする。
・調整、診断時に測定元素にしたときは、推奨質量数の中の優先順位が最も高い質量数を測定質量数とする。
・右クリックで元素を選択すると、元素固有の情報画面を表示する。
【００９３】
▲２▼同位体情報テーブル
・単一行の選択となっている。選択した質量数に対応した干渉イオン情報を表示する。
・測定質量数のセルで左のクリックで、測定質量数の選択状態を変更する。
【００９４】
▲３▼干渉元素イオン（干渉分子イオン）情報テーブル
・単一行の選択とする。
【００９５】
▲４▼干渉イオン情報の指定
・干渉分子イオン情報テーブルに表示する干渉分子イオン情報を指定する。
【００９６】
▲５▼測定質量数テーブル
・複数行の選択とする。
・「削除」：選択中の測定質量数を測定しない質量数とする。
・「全削除」：すべての測定質量数を測定しない質量数とする。
・「質量数設定」：測定質量数設定画面を表示する。
・「分子名設定」：測定分子名設定画面を表示する。
【００９７】
▲６▼その他
・「ＯＫ」：設定内容を確認後、ダイアログを閉じ、記憶装置に保存する。
・「キャンセル」：設定内容を無効にし、ダイアログを閉じる。
【００９８】
デスクトップ上のＰｌａｓｍａ ３ＤＱのアイコン１３５をクリックすると、ソフトが起動し、感度調整画面である図１３が表示される。この画面を介して感度調整を行う。
【００９９】
条件設定部１３２の条件設定のボタン１３６をクリックすると、図１７に示す条件設定画面になる。画面部１３３には、分析モード、オペレータ、コメント、元素および元素選択ボタン１３７が表示される。元素選択ボタン１３７をクリックすると、図１８に示す元素選択画面になる。元素選択画面は、左上方の周期律表表示部１４１、その下方の干渉イオン情報表示部１４２、その下方の干渉分子イオン情報表示部１４３、右上方の同位体情報表示部１４４、その下方の測定元素名表示部１４５および右端の測定範囲設定部１４６から構成される。
【０１００】
今回は、質量数５０〜５８の元素を測定するものとする。測定範囲設定部１４６の測定範囲設定ボタン１４７をクリックすると、図１９に示す測定範囲設定画面となり、測定範囲設定画面１４８が表示される。この画面で、測定開始質量数５０、測定終了質量数５８と入力し、追加ボタン１４９を押す。
【０１０１】
図２０に示すように、測定範囲設定画面１４８には、質量数５０〜５８の同位対比が色別で示される。表示部分を拡大すると図２１に示すようになっており、測定イオンの強度が最大の質量数との干渉の度合いがすぐに確認できる。
【０１０２】
図２０におけるＯＫボタン１５０をクリックすると図２２に示す測定元素画面に戻る。周期律表で、選択された質量数にあたる元素が緑色表示される。また、右下の元素名表示部１４５に、測定元素とその質量数および重なった元素が表示される。
【０１０３】
図２３は、測定質量数が重なっている場合の重なりの削除を行うための画面である。すなわち、５８Ｆｅ、５８Ｎｉが重なっているためにこれを選択し、削除しようとする画面である。５８Ｆｅと５８Ｎｉとが質量数が重なっているので、右下の測定元素の質量数をマウスで選択し、削除ボタン１５１を押すことで、５８Ｆｅと５８Ｎｉを測定しないことを指定する。このようにして、他の重なっている元素についても測定しないことを指定する。
【０１０４】
次に、ＯＫボタン１５０をクリックすると、測定元素および測定質量数が決定される。
【０１０５】
例２：周期律表から測定元素を選択する例
起動画面としての感度調整画面および条件設定画面は、例１に示す図１６、図１７と同じ画面である。
【０１０６】
次に、例１に示す図１８が画面表示される。これを図２４として示す。
【０１０７】
今回は、５４Ｃｒと５４Ｆｅとを測定するものとする。
【０１０８】
Ｃｒは、質量数５０、５２、５３、５４に存在する。一般的には感度面で有利なことから、最も存在比の高い質量数を選択する。Ｃｒの場合は５２である。
【０１０９】
Ｆｅは、質量数５４、５６、５７、５８に存在する。Ｆｅの存在比が最も高い質量数は５６である。
【０１１０】
分子イオンが重なり、どうしても存在比の高い質量数を測定できない場合がある。その場合、他の質量数を測定することになる。
【０１１１】
今回は、前述のように質量数の重なるＦｅの５４とＣｒの５４とを測定する場合について説明する。
【０１１２】
図２５はＣｒをクリックした状態を示す図である。周期律表でＣｒのボタンをクリックする。画面右上の同位体情報表示部１４４にＣｒの存在する質量数と、その存在比が表示される。
【０１１３】
同時に質量数の重なる元素が、周期律表にピンク色で示される。Ｃｒの場合は、Ｔｉ、Ｖ、Ｆｅが重なるが、これらは色表示されることによって一目で識別される。
【０１１４】
図２６は５４Ｃｒを選択した状態を示す図である。
【０１１５】
同位体情報表示部１４４に示される同位体情報で質量数５４をクリックする。
【０１１６】
そうすると、画面右下の測定元素名表示部１４５に測定元素として５４Ｃｒが表示される。
【０１１７】
図２７はＦｅをクリックした状態を示す画面である。
【０１１８】
周期律表でＦｅをクリックすると、同位体情報表示部１４４にＦｅの同位体である５４Ｆｅ、５６Ｆｅ、５７Ｆｅ、５８Ｆｅがその存在比と共に表示される。同時に質量数の重なる元素が周期律表にピンク色で表示される。Ｆｅの場合は、Ｃｒ、Ｎｉが重なるが、これらは色表示されることによって一目で識別される。
【０１１９】
図２８は５４Ｆｅを選択した状態を示す画面である。
【０１２０】
同位体情報表示部１４４に表示される同位体情報で、質量数５４をクリックする。
【０１２１】
そうすると、既に表示されている５４Ｃｒに合わせて５４Ｃｒ５４Ｆｅが表示される。この状態で測定を行うと質量数５４でＦｅとＣｒの両方について測定することになる。従って、この状態では、質量数５４はＣｒの測定結果なのかＦｅの測定結果なのかが判らない。使用者は、質量数の重なりを判定し、図２３に示すように、削除ボタン１５１を押し、５４Ｃｒ５４Ｆｅを測定から除外する。
【０１２２】
このようにして質量数の重なりを判定した後に、ＯＫボタン１５２をクリックすると、測定元素および測定質量数が決定される。
【０１２３】
次に、この例における干渉イオン情報表示部１４２に表示される干渉イオン情報および干渉分子イオン情報部１４３に表示される干渉分子イオン情報について説明する。
【０１２４】
干渉イオン情報として、図２５あるいは図２６に示すように、干渉元素イオンが適切な範囲で記憶装置１０４から引き出されて表示されるようになっている。
【０１２５】
使用者は、干渉イオン情報を見て同位体情報の重なりを見ることができ、同位体情報の表示と測定元素の指示および測定元素の重なりから測定元素名表示部１４５において前述のように測定元素を決めることができ、これに伴なって測定質量数が決まる。
【０１２６】
干渉分子イオン情報として、塩素イオン、硝酸イオン、硫酸イオン、環境水およびユーザの任意に指定するユーザ１、ユーザ２、ユーザ３、ユーザ４の干渉イオンを指定し、これらを測定元素から削除することができる。
【０１２７】
例３：質量数から測定元素を選択する例
起動画面としての感度調整画面、条件設定画面および元素選択画面は、例１に示す図１６、図１７、図１８と同じ画面である。
【０１２８】
図１８において、測定範囲設定ボタン１４７をクリックすると、図２９に示す測定範囲設定画面が表示される。
【０１２９】
図３０は、測定質量数の決定のための画面である。
【０１３０】
今回は質量数５０〜７０を測定するものとする。図２７において、測定開始質量数５０、測定終了質量数７０を入力し、追加ボタン１６０を押す。当該グラフを利用して、マウスのドラッグ操作でも、質量数を選択できる。
【０１３１】
図３１は、測定元素画面である。
【０１３２】
図３０において、ＯＫボタン１５０をクリックすると図２８の画面になる。すなわち、測定元素画面に戻り、選択された質量数にあたる元素が緑色になる。また、右下の測定元素名表示部１４５に測定元素と、質量数およびその重なりが表示される。
【０１３３】
図３２は、測定質量数が重なっている場合の削除を行うための画面である。
【０１３４】
測定質量数が重なっている場合、その重なりの元素、例えば５８Ｆｅ５８Ｎｉをマウスで選択し、削除ボタン１５１を押すことで、この元素を測定しないよう指定できる。図２９は、５８Ｆｅ、５８Ｎｉが重なっているため、選択し、削除しようとしている画面である。
【０１３５】
このようにして、重なった元素を削除した後、ＯＫボタンをクリックすると、測定元素および測定質量数が決定する。
【０１３６】
例４：上水に含まれる測定元素を選択する応用例
水質分析するに当って分析上の留意点として、測定元素はμｇ／Ｌレベルの濃度である、Ｎａ、Ｃａ、Ｍｇなどの共雑物が多く含まれる、スペクトル干渉物として酸化物があることが挙げられる。また、規制強化による測定対象元素の増加として、Ｕ（ウラン）を測定対象とすることが挙げられる。
【０１３７】
前者に対しては、スプレーチャンバーの冷却、材料導入量の抑制、プラズマ温度の高温化、Ａｒに起因する分子イオンの低減を行うなどの対策を実施することにより、そして前述した例１〜例３を採用することにより水質分析を行うことができる。
【０１３８】
図３３は、水質分析のために、周期律表で１５個の元素とＵを指定し、同一質量の５４Ｃｒ５４Ｆｅ、５６Ｆｅ４０Ａｒ１６Ｏを削除した状態を示す。これによって干渉イオンを排除して水質分析を行う。
【０１３９】
次に、質量分析装置においてイオンが動作している状態を画面表示する例について説明する。画面に表示される状態図は、実際のイオンの動作状態を模擬し、かつ拡大して電子的に示すものであるので、ここでは画面上では「イオン子」として表現する。
【０１４０】
図３４は、プラズマが消えていて、真空系のみが動いている状態を示す。この状態が装置の停止状態である。真空系は常に動作している。
【０１４１】
画面上には、図１２に示す装置の本体部１０１の構成が表示される。同一の表示としてもよいが、投入するＡｒあるいはＨｅの存在、その使用状態を示すために加えて表示するのがよい。
【０１４２】
図にあっては、プラズマは点灯前であり、イオンがイオン取込み部１１２への取り込みが行われていないので、イオン子の躍動はない。
【０１４３】
図３５は、プラズマを点灯し、ゲートバルブ部１１３を閉じている状態を示す。プラズマが点灯し、点灯のためのＲＦが出力される。また、イオン取込み部１１２に冷却水も導入される。イオンはゲートバルブ部１１３が閉じているため、ゲートバルブ部１１３の前までにしか導入されない。また、真空系のゲートバルブ部１１３下流側も、まだ動作していない状態にある。
【０１４４】
画像処理装置は、イオン取り込みが行われ、かつゲートバルブ部１１３が閉鎖されているので、取り込まれたイオンを表示するイオン子をゲートバルブ部１１３までの通路で躍動せしめ、ゲートバルブ部１１３下流側ではイオン子の躍動は表示しない。
【０１４５】
図３６は、詳細ボタン１６０をクリックしてその下方に図に示す検査項目の表示を行う。例えば、それらは検知器、ＲＦ出力、プラズマガス、キャリアガス、補助ガス等についての状態を示す出力値である。
【０１４６】
図３７では、ゲートバルブ部１１３が開いていて３ＤＱＭＳ１１７が停止している状態を示す。プラズマは引き続き点灯状態にあり、点灯のためのＲＦも出力される状態にある。また、イオン取込み部１１２に冷却水も導入されている。イオンはゲートバルブ部１１３を開いたため、真空系後段まで導入される。しかし、３ＤＱＭＳ１１７がＯＦＦのため、イオンは３ＤＱＭＳを素通りする。
【０１４７】
画像処理装置は、イオン取り込みが行われ、かつゲートバルブ部１１３が開放されているので、取り込まれたイオンを表示するイオン子をゲートバルブ部１１３までの通路で、また３ＤＱＭＳを素通りするように動作させ、表示する。
【０１４８】
図３８は、ゲートバルブ部１１３が開いていて３ＤＱＭＳ１１７が動作している状態を示す。プラズマは引き続き点灯状態にあり、点灯のためのＲＦも出力される状態にある。また、イオン取込み部１１２に冷却水も導入されている。イオンは、ゲートバルブ部１１３が開いているために、真空系後段まで導入され、３ＤＱＭＳ１１７がＯＮとなったので、イオンは３ＤＱＭＳに導入される。
【０１４９】
画像処理装置は、イオン取り込みが行われ、ゲートバルブ部１１３が開放され、また３ＤＱＭＳ１１７が動作しているので、イオン子をイオン取込み部、ゲートバルブ部、収束レンズ部、および３ＤＱＭＳ部で躍動せしめる。特に、３ＤＱＭＳ部ではイオン子を８の字を描くようにして躍動させ、表示する。分析装置にＱＭＳを採用した場合も同様であり、この場合、画像処理装置は、イオン取り込みが行われ、かつ前記ゲートバルブ部が閉鎖されているときには、取り込まれたイオンを表示するイオン子を前記ゲートバルブ部までの通路で躍動せしめ、前記ゲートバルブ部が開放され、質量分析部への通路が閉鎖されているときには、イオン子をイオン偏向部までの通路で躍動せしめて表示し、質量分析部における分析が行われているときには、イオン子を質量分析部まで躍動せしめて表示することになる。
【０１５０】
前述のように、質量分析装置は、試料をプラズマ化してイオンを生成するイオン源と、該イオン源から生成したイオンを取り込むイオン取込み部と、該イオン取込み部から取り込まれたイオンを引き出して収束する収束レンズ部と、該収束レンズ部で収束されたイオンを偏向レンズにより偏向して質量分析部に導入するイオン偏向部からなり、前記イオン取込み部の入口に小孔を有するスキマーを設け、前記イオン源にアルゴン（Ａｒ）ガスを、そして質量分析部にヘリウム（Ｈｅ）ガスを導入する。
【０１５１】
画像処理装置は、アルゴンガスおよびヘリウムガスの導入が行われていることを表示し、かつ該表示が行われていることを前提として前記イオン源から前記スキマーの小孔にその先端部が達するプラズマ画を模擬燃焼表示することになる。
【０１５２】
前記画像処理装置は、アルゴンガスのためのアルゴンガスボンベを表示し、該アルゴンガスボンベをアルゴンガス導入時、欠乏時および消費時に分けて識別表示し、モニター表示された画像に隣接して、各種検知状態、イオン引き出し状態、イオンシールド状態、イオン源に使用するトーチの使用状態および試料投入のためのペリスタルポンプ状態を表示することになる。
以上のように本実施例によれば、イオントラップを利用し、複数の測定元素を指定して分析を行う質量分析方法において、元素の同位体情報とその元素のイオン質量数に干渉するイオン質量数の元素イオンとを記憶し、一画面に、周期律表を表示し、該周期律表に示される元素を指定することによって該元素の同位体およびそれらのイオン質量数を含む同位体情報を表示し、該イオン質量数に干渉するイオン質量数の元素イオンを質量数と共に干渉イオン情報として表示し、さらに、該イオン質量数に干渉するイオン質量数の分子イオンを質量数と共に干渉イオン情報として表示し、前記同位体情報から測定候補となる同位体元素を表示し、質量数の同じ同位体元素の削除および干渉分子イオンの削除を行って、当該画面上で測定元素の設定を行うことを特徴とする試料の質量分析方法が構成される。
また、本実施例によれば、イオントラップを利用し、複数の測定元素を指定して分析を行う質量分析方法において、元素の同位体情報とその元素のイオン質量数に干渉するイオン質量数の元素イオンとを記憶し、イオン質量数測定範囲を画面上に設定し、該画面上に設定されたイオン質量数測定範囲にある元素の同位体元素をそのイオンを質量数と共に同位体情報として画面に表示し、該イオン質量数に干渉するイオン質量数の元素イオンを質量数と共に干渉イオン情報として表示し、さらに、該イオン質量数に干渉するイオン質量数の分子イオンを質量数と共に干渉イオン情報として表示し、前記同位体情報から測定候補となる同位体元素を表示し、質量数の同じ同位体元素の削除および干渉分子イオンの削除を行って当該画面上で測定元素の設定を行う試料の質量分析方法が構成される。
また、本実施例によれば、イオントラップを利用し、複数の測定元素を指定して分析を行う質量分析装置において、元素の同位体情報とその元素のイオン質量数に干渉するイオン質量数の元素イオンとを記憶する記憶装置を備え、一画面に、周期律表を表示し、周期律表に示される元素を指定することによって該元素の同位体およびそれらのイオン質量数を含む同位体情報を表示し、該イオン質量数に干渉するイオン質量数の元素イオンを質量数と共に干渉イオン情報として表示し、さらに、該イオン質量数に干渉するイオン質量数の分子イオンを質量数と共に干渉イオン情報として表示し、前記同位体情報から測定候補となる同位体元素を表示し、質量数の同じ同位体元素の削除および干渉分子イオンの削除を行って、当該画面上で測定元素の設定を行う画面処理装置とを備えた試料の質量分析装置が構成される。
また、本実施例によればイオントラップを利用し、複数の測定元素を指定して分析を行う質量分析装置において、元素の同位体情報とその元素のイオン質量数に干渉するイオン質量数の元素イオンとを記憶する記憶装置を備え、イオン質量測定範囲を画面上に設定し、該画面上に設定されたイオン質量数測定範囲にある元素の同位体元素をそのイオン質量数と共に同位体情報として画面に表示し、該イオン質量数に干渉するイオン質量数の元素イオンを質量数と共に干渉イオン情報として表示し、さらに、該イオン質量数に干渉するイオン質量数の分子イオンを質量数と共に干渉イオン情報として表示し、前記同位体情報から測定候補となる同位体元素を表示し、質量数の同じ同位体元素の削除および干渉分子イオンの削除を行って、当該画面上で測定元素の設定を行う画面処理装置とを備えた試料の質量分析装置を構成する。
【０１５３】
【発明の効果】
本発明によれば、測定しようとする元素イオンの同位体情報および同位体と同じ質量数の干渉イオンを同一画面に表示し、干渉イオンの存在する同位体元素を削除する操作を同一画面で行えるようにしているので、多数の元素を測定元素として設定することができ、測定可能元素の中から１つずつ選択するのではなく、画面上で上述のように測定元素を設定するので、誤操作を誘発することがなく、測定精度の向上を図ることができる。また、本発明によれば、測定元素の設定を上述のように容易に行うことができるため、どの質量数が測定されるのかが一目で確認できるため、測定結果の確認作業が容易になるばかりでなく、複数の元素を選択する場合でも手間を要しないので汎用性が向上し、各種試料に対する分析に対する応用性が期待できる。
【０１５４】
また、本発明によれば、分析条件設定を多様化することができ、周期律表を使用した元素を指定しての測定元素の設定、質量数の範囲を指定しての測定元素の設定、同位体の存在比をグラフ表示しての測定元素の設定など測定元素の設定の仕方を拡大することが容易になる。
【０１５５】
本発明によれば、イオン取り込み、ゲートバルブ部の開閉、質量分析部の動作に連動して画面上にイオン子の動作を躍動せしめているので、一目瞭然に画面上で操作の状況を判別することができるから、測定手順を間違えると言うことを避け易くなり、ユーザが使い易くなるメリットがある。
【０１５６】
以上のように、ユーザが使用し易くなるに伴なって、水質の分析などのように多元素を含む資料についても含有元素の分析がやり易くなり、汎用性が向上した。
【図面の簡単な説明】
【図１】装置本体の横平面を中心とした構成図。
【図２】装置本体の縦平面を中心とした構成図。
【図３】部品構成図。
【図４】装置本体の平面配置図。
【図５】装置本体の正面配置図。
【図６】装置本体の側面配置図。
【図７】装置本体の外観図。
【図８】扉部を主に説明するための図。
【図９】図８について他側から見た図。
【図１０】図８について他の例に関する構成図。
【図１１】変形例を示す例図。
【図１２】本発明の実施例のブロック図。
【図１３】親イオンの決定、およびイオン導入を説明するための図。
【図１４】親イオンの決定、およびイオン導入を説明するための図。
【図１５】起動時の画面図。
【図１６】感度調整画面（起動時の画面）図。
【図１７】条件設定画面図。
【図１８】元素選択画面図。
【図１９】測定範囲設定画面図。
【図２０】測定質量数の決定を行うための画面図。
【図２１】図２０の一部拡大図。
【図２２】測定元素画面図。
【図２３】選択元素の削除を行うための画面図。
【図２４】元素選択画面図。
【図２５】Ｃｒをクリックした状態図。
【図２６】５４Ｃｒを選択した状態図。
【図２７】Ｆｅをクリックした状態図。
【図２８】５４Ｆｅを選択した状態図。
【図２９】測定範囲設定画面図。
【図３０】測定質量数の決定を行うための画面図。
【図３１】測定元素画面図。
【図３２】選択元素の削除を行うための画面図。
【図３３】水質分析のための元素選択画面図。
【図３４】装置停止状態図。
【図３５】ゲートバルブが閉じている状態図。
【図３６】図３５に示す状態で、かつ検知項目を表示する状態図。
【図３７】ゲートバルブが開いて３ＤＱＭＳが停止している状態図。
【図３８】ゲートバルブが開いて３ＤＱＭＳが動作している状態図。
【符号の説明】
１００…イオン源質量分析装置、１０１…本体部、１０２…コントローラ、１０３…演算装置（ＣＰＵ）、１０４…モニター、１０５…記憶装置、１０６…同位体元素表示、１０７…同一質量数元素の削除、１０８…干渉イオンの削除、１０９…測定イオンの質量数決定、１１１…イオン源、１１２…イオン取込み部、１１３…ゲートバルブ部、１１４…収束レンズ部、１１５…偏向部、１１６…質量分析部、１１７…３ＤＱＭＳ部、１１８…検知部、１３１…アイコン項目部、１３２…条件設定部、１３３…画面部、１３４…状態表示部、１４１…同期律表表示部、１４２…干渉イオン情報表示部、１４３…干渉分子イオン情報表示部、１４４…同位体情報表示部、１４５…測定元素名表示部、１４６…測定範囲設定部。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a mass spectrometer using a plasma ion source.
[0002]
[Prior art]
In the field of environmental measurement and semiconductors, plasma ion source mass spectrometry has been put into practical use as a multi-element simultaneous analyzer and is becoming widespread. Plasma ion sources use inductively coupled plasma using argon gas or microwave induced plasma using nitrogen gas, and devices that can measure extremely small samples by combining these with a mass spectrometer have been commercialized. Yes.
[0003]
JP-A-7-78590 discloses a plasma ion source for ionizing the sample in plasma for the purpose of identifying and quantifying trace impurities in the sample, a sampling interface for guiding the generated ions into a vacuum vessel, In the plasma ion source mass spectrometer having an ion lens, a mass filter and a detector installed in the vacuum vessel, the axis of the sampling interface and the axis of the mass filter are arranged at an angle of 90 degrees, and the ion lens There is described a plasma ion source mass spectrometer having a 90-degree deflector that deflects the beam of ions that has passed through the sampling interface by 90 degrees, and the 90-degree deflector has an opening on the opposite side of the sampling interface.
[0004]
Recently, an ion trap mass spectrometer has been proposed as a mass spectrometer instead of a quadrupole mass spectrometer. An ion trap mass spectrometer can temporarily store ions to be measured continuously introduced into an electrode by operating a high-frequency electric field. Further, the trapped ions can be extracted and detected according to the mass number. For this reason, it is possible to expect highly sensitive measurement as compared with a mass spectrometer that cannot accumulate ions and can detect only specific ions among ions introduced continuously.
[0005]
ICP-MS is an abbreviation for Inductively Coupled Plasma-Mass Spectrometer (ICP Mass Spectrometer), and trace amounts of elements on the earth up to U (uranium) of m / z 238 are measured in the concentration range mg / L to Analyzes with high sensitivity at ng / L.
[0006]
The principle is that a solution sample is made into a fine mist with a nebulizer and the elements in the sample are ionized. The ionized elements are sorted by the difference in mass, and the content of the element is determined by the amount of ions.
[0007]
Usually, the concentration unit of analysis is expressed in mg / L, μg / L, ng / L, and the like.
[0008]
1 mg / L = 1 × 10^-6g / L
1 μg / L = 1 × 10^-9g / L
1 ng / L = 1 × 10^-12g / L
The structure of ICP-3DQMS is well known, and a solution sample is atomized by a nebulizer, sorted into a fine mist-like uniform particle size in a spray chamber, and introduced into a plasma together with a carrier gas. ICP is a very ideal ion source, and most elements are ionized by 90% or more.
[0009]
Ions generated by ICP pass through the interface section and are introduced into the 3DQMS section. The interface section is composed of a sampling cone and a skimmer cone section, and this section is maintained at about 100 Pa by a rotary pump. After the skimmer cone, there are an extraction electrode and an ion lens. The ion lens unit and the 3DQMS unit are 10 by a turbo molecular pump.^-2-10^-4Exhaust to Pa.
[0010]
Ions subjected to mass selection by 3DQMS are detected by an ion detector.
[0011]
The characteristics of the general ICP-MS method are as follows.
[0012]
O The sensitivity is very high.
Ar plasma is an ideal ion source, and a detection limit of ng / L level can be obtained.
[0013]
〇 Qualitative analysis is easy.
Mass spectra of all elements can be measured in a short time.
Since the spectrum is simple, qualitative peak identification is easy.
[0014]
○ Multi-element simultaneous quantitative analysis is possible.
Multi-element simultaneous analysis of elements of mg / L to ng / L is possible.
[0015]
O There is little spectrum interference.
[0016]
〇Analysis of isotopic contrast is possible.
Since a mass spectrometer is used as a detector, an isotope dilution method that is difficult to measure with other elemental analyzers can be performed, so that highly accurate analysis can be performed.
It can be used as a stable isotope tracer.
[0017]
[Problems to be solved by the invention]
As a problem of conventional ICP-MS,
O Price is high.
○ Received by molecular ions. ArO, ArCl, ArAr and the like.
O There is matrix interference. Therefore, the sensitivity is lowered.
○ High concentration range cannot be measured. There are restrictions on environmental samples.
○ Higher sensitivity. I want to further dilute the sample.
O Operation is complicated. Operation and maintenance are poor.
○ The equipment is large. A dedicated room is required.
Etc. are mentioned.
[0018]
In the present invention, the isotope information and interference ion information of the element ion to be measured can be processed and displayed on the screen, so that a large number of elements can be easily set as measurement elements with ease and systematically. An object of the present invention is to provide a mass spectrometry method and apparatus.
[0019]
The present invention also provides a water quality analysis method for quickly analyzing water containing U (uranium).
[0020]
[Means for Solving the Problems]
The present invention designates a plurality of measurement elements and performs an analysis.
-The element to be measured is determined by the mass number range or the element specification in the periodic table.
・ By specifying a specific element, detailed information specific to that element is displayed.
-When displaying the mass number range of the measurement element in a graph, displaying a mark in the mass number range of the specified element,
Like to do.
[0021]
By doing in this way, the element selection can be selected from the range of mass number, there is no omission in the selection, and no trouble is required even when selecting a plurality of elements. Since a detailed display can be instantly displayed by selecting a specific element, it is possible to immediately and easily know interference with other elements for each selected element. Moreover, since it is possible to confirm at a glance which mass number range is measured, operations such as confirmation of the measurement result can be easily performed.
[0022]
Specifically, the present invention provides the following methods and apparatuses.
[0023]
The present invention stores an isotope information of an element and ions having an ion mass number that interferes with the ion mass number of the element in a mass spectrometry method that performs analysis by specifying a plurality of measurement elements using an ion trap. , By displaying the isotope information of the element and its ion mass number by designating the element or mass number on one screen, and the ions of the ion mass number interfering with the ion mass number together with the mass number A sample mass analysis method that displays as interference ion information, displays isotope elements as measurement candidates from the isotope information, deletes isotope elements having the same mass number, and sets the measurement element on the screen And providing equipment.
[0024]
The present invention stores an isotope information of an element and an element ion of an ion mass number that interferes with the ion mass number of the element in a mass spectrometry method that performs analysis by specifying a plurality of measurement elements using an ion trap. Then, a periodic table is displayed on one screen, and isotope information including the isotopes of the elements and their ion mass numbers is displayed by designating the elements shown in the periodic table, and the ion mass numbers The element ion of the ion mass number that interferes with the mass number is displayed as interference ion information together with the mass number, the isotope element that is the measurement candidate is displayed from the isotope information, and the isotope element having the same mass number is deleted. Provided is a sample mass spectrometry method and apparatus for setting the measurement element.
[0025]
The present invention stores an isotope information of an element and an element ion of an ion mass number that interferes with the ion mass number of the element in a mass spectrometry method that performs analysis by specifying a plurality of measurement elements using an ion trap. Then, a periodic table is displayed on one screen, and isotope information including the isotopes of the elements and their ion mass numbers is displayed by designating the elements shown in the periodic table, and the ion mass numbers The element ion of the ion mass number that interferes with the ion mass number is displayed as interference ion information together with the mass number, and the molecular ion of the ion mass number that interferes with the ion mass number is displayed together with the mass number as interference ion information, and the isotope information Display the isotope element that is a candidate for measurement, delete the isotope element with the same mass number, delete the interfering molecule ion, and set the measurement element on the screen. To provide a legal and devices.
[0026]
The present invention stores an isotope information of an element and an element ion of an ion mass number that interferes with the ion mass number of the element in a mass spectrometry method that performs analysis by specifying a plurality of measurement elements using an ion trap. The ion mass number measurement range is set on the screen, the isotope element of the element in the ion mass number measurement range set on the screen is displayed on the screen as the isotope information together with the mass number, Element ions with an ion mass number that interferes with the ion mass number are displayed as interference ion information together with the mass number, and isotope elements that are measurement candidates are displayed from the isotope information, and isotope elements having the same mass number are deleted. A sample mass analysis method and apparatus for setting a measurement element on the screen are provided.
[0027]
The present invention stores an isotope information of an element and an element ion of an ion mass number that interferes with the ion mass number of the element in a mass spectrometry method that performs analysis by specifying a plurality of measurement elements using an ion trap. The ion mass number measurement range is set on the screen, the isotope element of the element in the ion mass number measurement range set on the screen is displayed on the screen as the isotope information together with the mass number, The element ion of the ion mass number that interferes with the ion mass number is displayed as interference ion information together with the mass number, and the molecular ion of the ion mass number that interferes with the ion mass number is displayed as interference ion information together with the mass number, Display the isotope elements that are measurement candidates from the isotope information, delete the isotope elements with the same mass number, delete the interfering molecular ions, and set the measurement elements on the screen. It provides a mass spectrometer method and apparatus for fees.
[0028]
The present invention provides a mass spectrometry method for analyzing a water quality by specifying a plurality of measurement elements using an ion trap, and setting a plurality of ion mass number measurement ranges including a uranium (U) mass number range on a screen. , Display isotope information including isotope elements in the ion mass number measurement range, and display interference ion information including element ions of the ion mass number that interfere with the ion mass number of the isotope element and the mass number Further, molecular ions having an ion mass number that interferes with the ion mass number are displayed as interference ion information together with the mass number, and on the screen displaying the isotope information and the interference ion information, the measurement element including the uranium isotope is displayed. A mass spectrometry method for analyzing water quality is provided.
[0029]
DETAILED DESCRIPTION OF THE INVENTION
Embodiments of the present invention will be described below with reference to the drawings.
[0030]
1 and 2 show the structure of the apparatus main body used in the embodiment of the present invention. FIG. 1 shows the arrangement of components and components by cross-sectionally showing the apparatus. FIG. The arrangement status of each part and each component is shown below.
[0031]
In the plasma ion source analyzer, an L-shaped casing 1 and a front cover 2 combined therewith form a casing body, and the interior of the casing body is composed of an upper layer portion 18 and a lower layer portion 19, and the upper layer portion 18 is viewed from the right side. The combustion chamber container 3, the slide valve container 5, and the deflection / analysis container 4 are arranged in a row on the horizontal plane 21.
[0032]
As shown in FIG. 2, a sample portion including a combustion chamber container 3, a peristaltic pump 31, a sample cup 32, and a tray 33 thereof is arranged on a vertical plane 22 in a right side portion of the housing body.
[0033]
Each component will be described in more detail using the component configuration diagram of FIG. The combustion chamber container 3, which is configured by the L-shaped casing 1 and the surface cover 2, includes a torch 7 and a nebulizer 8. The deflection / analysis container 4 has two chambers communicating with each other. A parallel electrode 12 is disposed in one of the deflection chambers, and an analyzer 14 is disposed in the confining chamber 13 for the other. A slide valve container 5 is disposed between the combustion chamber container 3 and the deflection / analysis container 4.
[0034]
These components are mounted on the matching boxes 40 and 41, the detector unit 42, the RF power source unit 43, and the device base unit 44, or are arranged in the casing while being held laterally. In this case, it is positioned and arranged as described above by using such a matching box.
[0035]
The combustion chamber container 3 is open on the front side and the upper side, and a window 10 in which the torch 7 is disposed is provided on the slide valve container 5 side. A chimney 45 is provided in the L-shaped housing 1 in accordance with the opening on the upper side, and combustion exhaust gas is discharged from the chimney 45 to the outside. A power source is disposed in the matching box 43.
[0036]
An opening 15 is formed in the front cover 2 in accordance with the front opening of the combustion chamber container 3, and a pump opening 34 is formed immediately below the opening 15. A peristaltic pump 31 is provided in the pump opening 34.
[0037]
A protective wall 16 is provided above the opening 15, and a protective wall 17 is provided below the pump opening 34.
[0038]
The open portion 15 is provided with a left outer door 51 and a right outer door 53, and the large left outer door 51 is provided with a combustion confirmation window 52. A gas meter 65 and a gas adjustment knob 66 described with reference to FIG. 7 are provided on the entire surface of the device substrate 44, and a panel 54 covering them is fitted.
[0039]
A tray 33 is provided below the pump opening 34, and a sample cup 32 is placed thereon.
[0040]
In FIG. 2, a peristaltic pump 31 sucks a sample from a sample cup 32 through a tube and supplies the sample to the nebulizer 8 directly above.
[0041]
In FIG. 1, the sample supplied to the nebulizer 8 is burned by the torch 7 and turned into plasma. The plasmaized sample is sent to the parallel electrode 12 through the slide valve in the slide valve container 5, deflected there, and sent to the storage chamber 13. Accordingly, a sample flow is formed as shown by the thick lines 24 and 20 in FIGS. That is, the flow of the sample is characterized by flowing on two surfaces along the vertical plane 22 and the horizontal plane 21.
[0042]
The sample that has been turned into ions by being turned into plasma is deflected by the parallel electrode 12, stored in the analyzer 14 for a certain period of time, and subjected to mass analysis by scanning a high-frequency electric field. This ion trap mass spectrometry is well known and does not require further explanation.
[0043]
4 shows a planar arrangement of the apparatus configuration, FIG. 5 shows a cross section from the front, and FIG. 6 shows a cross section from the side.
[0044]
A combustion chamber 6 for generating plasma, a deflection unit 11 having a deflection electrode (parallel electrode 12) for deflecting ions, and a confinement chamber 13 for performing mass separation of the deflected ions are arranged in a horizontal plane. A sample installation section such as a tray 33 for setting a sample serving as an ion source, a peristaltic pump 31 for sucking the sample, and a combustion chamber 6 for introducing the sucked sample and burning it are arranged in a plane in the vertical direction with respect to the plane. ing. As a result, the sample can be supplied from the lower side to the upper combustion chamber 6 and ions generated by the plasma can flow on the horizontal plane. The generated ions reach the slide valve through the interface part 23 which is a disk-shaped metal part having a pore in the center placed beside the torch 7. A combustion chamber vessel 3 having a torch 7 and a nebulizer 8, a deflection electrode (for example, parallel electrode 12) for deflecting ions, and a deflection / analysis vessel 4 having a confinement chamber 13 for mass separation of the deflected ions ( In addition, this includes that it is a separate body), and the interface portion and the slide valve container 5 arranged between the combustion container 3 and the deflection electrode are arranged in a plane in the lateral direction, and these containers are accommodated. The casing is formed with an open portion 15 for observing the combustion state and allowing the interface portion to be taken in and out of the operation side. The open portion is closed by the left outer door 51 and the right outer door 53 to confirm the combustion. The combustion state is confirmed through the window 52.
[0045]
As described above, the horizontal operation from the deflection unit to the combustion chamber 6 and the vertical arrangement from the sample installation unit to the combustion chamber 6 are adopted, so that the normal operation of the storage chamber 13, the deflection unit 11, the slide valve container 5 and the like is performed. The parts that are not to be placed are stabilized by being placed horizontally, while the combustion chamber 6, the peristaltic pump 31, and the sample cup 32 are parts that must be touched once or twice for analysis, and are operated by placing them vertically. It shall be easy to
[0046]
Further, by dividing each component into functions and arranging each component in a horizontal arrangement and a vertical arrangement, it has been possible to reduce the size in the lateral direction of the casing. Therefore, when the apparatus of the present embodiment is used on the mounting table, it is possible to make the mounting table smaller in width than the conventional one, and the space efficiency of the room where the apparatus of the present embodiment is used is improved.
[0047]
Further, when used on a standard mounting table, an empty space is created in the lateral direction of the apparatus of the present invention, so that peripheral devices can be placed as described later.
[0048]
The operator places the sample cup 32 on the tray 33, puts the tube therein, and fixes the tube to the peristaltic pump 31. For this reason, the lock lever is turned on. With such a vertical arrangement, the operator can operate without moving, and the combustion state from the combustion confirmation window 52 can be confirmed together. As described above, it is an operational merit to concentrate the portion that the operator touches and the portion to be noted. That is, the combustion chamber container 3 placed vertically, that is, the combustion confirmation window 52, the peristaltic pump 31, and the sample placement unit are placed in a concentrated manner, so that the operator can change the standing position in one place. Can work without. The line of sight is also concentrated on these three, making it easier to grasp the overall situation. The combustion confirmation window 52 can naturally enter the viewing angle from any position, and it becomes easy to perform pump operations such as removing the tube and locking the tube. The sample cup 32 may be set while standing, or may be performed while controlling a personal computer (PC) placed on the right side of the apparatus. Since the sample cup 32 is installed directly under the peristaltic pump 31 for such an operation, the operation becomes extremely easy.
[0049]
Since the disk-shaped metal part which comprises the interface part 23 is beside the flame (7000-8000K) of the torch 7, it carbonizes and becomes dirty. Since this contamination affects the analysis accuracy, it is necessary to brush with a metal brush before starting the analysis. The metal part, that is, the interface part 23 can be taken out and cleaned through the opening part 15.
[0050]
As shown in FIG. 3, the opening portion 15 is formed on the operation side, that is, the front side, and combustion confirmation is also performed therethrough. The combustion confirmation window 52 is positioned in the upper layer part of the housing, and facilitates confirmation of combustion, and facilitates maintenance cleaning of the combustion chamber container 3. Furthermore, the tube connector is easily operated. Tubes are changed about once every two weeks. Maintenance cleaning is usually performed at least once a month. The inside of the combustion chamber container 3 is very dirty because a strongly acidic sample is used. Therefore, although cleaning is an important operation, this operation can be easily performed by installing the opening portion 15. In the case of this operation, the right outer door 53 is opened and used. The left outer door 51 is opened for each analysis. Both of them are distinguished in purpose, and are divided into frequencies and hierarchies depending on whether they are frequently operated or not. A part of the peristaltic pump 31 is disposed in the housing, a part of the peristaltic pump 31 is disposed outside the housing, and is installed in a pump opening 34 formed in the housing. The metal part such as the shaft part is preferably disposed outside the housing. This is because if it enters the combustion chamber 6, it may corrode with the acid of the sample solvent.
[0051]
As shown in the figure, only the tube mounting part protrudes because it is easy to access and convenient to use, and the sample path is shortened, which is advantageous for shortening the liquid transportation time, that is, shortening the analysis time. is there.
[0052]
An RF power source 43 is disposed below the combustion chamber container 3, and a matching box 41 is disposed on the rear side. Accordingly, the combustion chamber container 3 can be positioned on the upper layer side, and the combustion chamber container 3 can be moved to the right side by a driving device (not shown) of the matching box 41 when cleaning the periphery of the interface unit 23. . Moreover, when measuring a combustion unit, it can be made to be an optimal position.
[0053]
The operation chamber (front side) and the upper side of the combustion chamber container 3 are opened, and a chimney 45 is provided in the housing in a corresponding relationship. The reason for providing the opening is to use it when performing maintenance work. When carrying out maintenance work, the front side and the upper side are opened in order to secure a visual field. The mass spectrometer can be placed on a desktop. Since the height of the laboratory table is usually 800 to 900 mm, it is desirable for the operator with a height of about 1600 mm to open the front side, and it is advantageous to open the upper side when the height is higher. become. The interface unit 23, the nebulizer 8, and the torch 7 are exchanged through the open portion provided in the combustion chamber container 3 and the corresponding open portion 15 provided in the housing, and the combustion chamber container 3 is cleaned. The
[0054]
A double structure of a box of the inner combustion chamber container 3 and an outer casing is adopted. These are opened by the left outer door 51 and the right outer door 53.
[0055]
The plasma for burning the sample with the torch 7 is 7000 to 8000 K and generates a high frequency. In order to eliminate the influence of this high frequency, a double shield is used. Further, since the sample having an oxidizing action is introduced into the combustion chamber container 3, the inside of the combustion chamber container 3 is affected by the oxidizing action. By making the combustion chamber 6 into an inner box called the combustion chamber container 3, the oxidation action can be suppressed only in the inner box.
[0056]
The interface part 23 is a removable metal part that is disposed and fixed between the slide valve container 5 and the combustion chamber container 3 as described above, and has a thin hole at the center thereof. The plasma will be extracted. Since the interface unit 23 is oxidized, it needs to be replaced. When the left outer door 51 is opened, the interface unit 23 is in front of the user and can be taken out immediately. This operation can be performed by opening the left outer door 51. The left outer door 51 is opened during the normal operation of replacing / cleaning the interface unit 23. An inner door 54 is provided to seal the combustion chamber container 3. Two doors are opened during maintenance work, such as once a month or once every two weeks.
[0057]
The apparatus has a width of 1100 to 1150 mm and is made compact. When the experimental table is 1800 mm wide, a space of about 600 mm remains on the experimental table, and a personal computer (PC) can be placed on the experimental table. In this case, the PC is preferably placed on the right side. As described above, the sample cup 32 is placed close to the right side, and the operation is facilitated by placing the PC on the right side.
[0058]
Next, the operation flow will be described. First, turn on the power and start up the PC. Dozens of sample cups 32 are arranged in front of the apparatus. Before passing the sample through the peristaltic pump 31, a test is performed by sucking up water. Next, the sample cup 32 is placed on the tray 33, the tube is attached to the sample, locked to the peristaltic pump 31, the peristaltic pump 31 is operated, and the sample is sent to the torch 7 via the nebulizer 8 to be converted into plasma.
[0059]
Since the sample cup 32 (tray 33), the peristaltic pump 31, and the combustion section are arranged in a substantially straight line in a vertical arrangement, the path of the tube is shortened. As a result, the time for sending the sample can be shortened, and the sample analysis time can be shortened.
[0060]
As shown in the figure, by forming the left outer door 51 and the right outer door 53 in a shape protruding from the housing surface, the sealing surface of the outer door can be brought into close contact with the housing surface, which is desirable for blocking high frequencies. FIG. 7 shows the appearance of the completed device. In the figure, a power switch 61, a power lamp 62, a plasma switch 63, an emergency stop switch 64, a gas meter 65, and a gas adjustment knob 66 are provided on the outer surface of the front cover 2. These functions and control methods are well known and will not be described here.
[0061]
FIG. 8 is a diagram illustrating the relationship between the outer door and the inner door. Reference numeral 55 denotes an inner door for sealing the front opening 56 of the combustion chamber container 3. The opening portion 15 faces the front opening portion 56 and the interface portion 23 so that parts can be easily replaced and cleaned.
[0062]
FIG. 9 is a view seen from the other side, and the description will not be repeated.
[0063]
FIG. 10 is a configuration diagram when the right outer door 53 is connected to the left outer door 51. In the previous embodiment, the outer door is constituted by two doors. However, prevention of high-frequency leakage occurring in the combustion chamber container 3 can be achieved even if the outer door is constituted by one piece.
[0064]
According to this, since the door is not divided | segmented, productivity can be improved.
[0065]
FIG. 11 shows an example in which the external sample stage 81 is arranged on the right side of the apparatus. The external sample stage 81 includes a sample storage box 82, and a number of sample pots 83 are provided therein. The tube 84 is supported by a tube stopper 85 provided on the front cover 2, supported by a tube support 86, and the tip thereof is positioned on each sample pot 83. The other end is wound around a peristaltic pump 31 and connected to the nebulizer 8 in the combustion chamber 6. The tip of the tube 84 is attached to the sample, sucked by the peristaltic pump 31, and sent to the nebulizer 8 and the torch 7, and the sample is turned into plasma as in the previous example.
[0066]
FIG. 12 is a block diagram. In the figure, an ion source mass spectrometer 100 is constituted by a main body 101, a controller 102 including a calculation device (CPU) 103 and a storage device 105, and a monitor 104. If the main body 101 is compared with the above-described components of the apparatus, the ion source 111 corresponds to the combustion chamber container 3, the combustion chamber 6, the torch 7, and the nebulizer 8, and the ion intake unit (interface: I / I F part) 112 corresponds to the interface part 23, and the gate valve part 113 and the converging lens part 114 correspond to the slide valve container 5. That is, in the slide valve container 5, the gate valve portion 113 is disposed at the inlet portion thereof, and the converging lens portion 114 is disposed so as to face the deflection portion 11. The deflection unit 115 corresponds to the deflection unit 11, and the mass analysis unit 116, the 3DQMS unit 117, and the detector 118 correspond to the analysis device 14. That is, the mass analysis unit 116 includes a 3DQMS unit 117 and a detector 118. The configuration itself shown in this block diagram is already well known. Plasma 90 is emitted from the ion source 111.
[0067]
The main body 101 is connected to the CPU 103 of the controller 102, and the CPU 103 extracts information to be described later from the storage device 105 and displays the screen on the monitor 104. As described above, the controller 102 has a function as an image processing apparatus.
[0068]
FIG. 12 shows an example in which the 3DQMS unit 117 is used. In addition to 3DQMS, QMS can be adopted. Both are mechanisms for separating ions for each target mass. In QMS, DC and AC voltages are applied to a quadrupole in which four hyperbolic cylinders are arranged in parallel, a hyperbolic electric field is generated on the inner surface of the Q pole, and ions are separated for each target mass. In contrast, 3DQMS is composed of a ring electrode having a rotating hyperbolic surface and an end cap electrode sandwiching the ring electrode, and ions are confined in this space, and then a mass spectrum is obtained.
[0069]
When performing metal analysis in a solution by ICP-MS, there are two types of ions that interfere with mass number.
[0070]
(1) Metal ions that exist in the solution and are different from the metal to be measured, for example, 54Fe and 54Cr correspond to this.
When it is desired to measure the concentration of Cr in the Fe ore at a mine or the like, if an attempt is made to measure Cr at a mass number of 54, since Fe exists at a very high concentration, interference occurs and an accurate value cannot be obtained. In this application, this ion is referred to as an element ion.
[0071]
(2) There is a molecular ion that exists in plasma or air and overlaps with the metal whose mass number is measured. In order to generate plasma, 40Ar gas is used. Further, a large amount of 14N (nitrogen) and 16O (oxygen) exist in the atmosphere. With this combination, mass number overlap, that is, interference occurs. For example, molecular ions are generated in plasma from Ar and O, and ArO becomes 40 + 16 = 56 (mass number) and causes interference with 56Fe. Therefore, it is said that ICP-MS using QMS in the MS part cannot measure a very small amount of 56Fe. In this application, such ions are referred to as molecular ions, and ions whose mass numbers overlap are referred to as interfering molecular ions.
[0072]
Thus, interfering element ions are metal ions other than the metal to be measured, and interfering molecular ions are molecular ions generated from molecules such as plasma, air, and solvent of the sample, and so on. Become. In this application, both are collectively referred to as interference ions.
[0073]
In such a configuration, the storage device 105 has interference ion information and interference molecular ion information.
[0074]
In the conventional apparatus, it takes time and effort to remove interference caused by interfering element ions and interfering molecular ions, and interference is inevitable. The storage device 105 stores interference element ions for a certain mass number as shown in Table 1.
[0075]
[Table 1]

[0076]
The spectrum of molecular ions with the same mass number overlaps the target element to be measured, which interferes with the measurement. The storage device 105 stores such interference molecular ions. Table 2 shows examples of molecular ions of Ar gas.
[0077]
[Table 2]

[0078]
Based on the arithmetic processing of the CPU 103, the controller 102 performs the isotope element display 106, performs the deletion 107 of the interference element ions, that is, the same mass number element 107 and / or the deletion 108 of the interference molecular ions, and determines the mass number 109 of the measurement ions I do.
[0079]
A method for excluding molecular ions and leaving only measurement ions while displaying on the monitor 104 will be described.
[0080]
(1) Determination of parent ion and ion introduction
As shown in FIG. 13, when a mass number of a parent ion or an element that is a measurement metal is selected, overlapping molecular ions are displayed.
[0081]
When 56Fe is selected, ArO
If you choose 80Se, ArAr
Etc. are displayed.
[0082]
On the other hand, when the user knows the contents of the measurement sample, overlapping parent ions are displayed by inputting the structural formula of molecular ions.
[0083]
When ArO is entered, 56Fe
When ArAr is entered, 80Se
Etc. are displayed.
[0084]
(2) Implementation of isolation
As shown in FIG. 14, isolation is performed.
[0085]
(3) Perform CID to decompose parent ions.
[0086]
As shown in FIG. 15, the parent ions are decomposed, and the decomposed ions and target ions are displayed. These are displayed on the screen, and the user inputs parameters to determine the parameters of FNF and CID.
[0087]
Since the plasma described above is generated by Ar, a very large number of Ar-derived ions exist in the plasma. Since the ions derived from Ar are irrelevant to the measurement element, they become interference peaks.
[0088]
In 3DQMS, a natural declustering reaction takes place inside 3DQMS. Therefore, when analyzing the measurement element, molecular ions originating from Ar (molecular ions such as ArAr) can be cleaved, preventing the occurrence of molecular ion interference. Can be prevented.
[0089]
Next, a method for setting the measurement element on the screen using these apparatuses will be described.
[0090]
Example 1: An example in which the abundance ratio of isotopes is displayed in a bar graph and a measurement element is selected.
[0091]
FIG. 16 shows a screen at the time of startup and a sensitivity adjustment screen. The screen includes an icon item part 131, a condition setting part 132, a screen part 133, and a status display part 134. The icon item section 131 includes items of file, display, device control, condition editing, sensitivity tuning, data, tool, window, and help. The condition setting unit 132 is provided with various condition setting buttons. The screen part 133 is provided with a screen part for displaying the relationship between time and signal intensity at the upper part and a screen part for displaying the apparatus configuration at the lower part. The status display unit 134 displays detection items.
[0092]
(1) Periodic table
-Display the atomic number, element name, and interfering element of the focused element (selected element). Also, isotope information and interference ion information corresponding to the measured mass number of the element are displayed. When there is no measured mass number, the recommended mass number is selected.
-When an element is selected with a left click or key, the selected element is changed endlessly in the order of the measurement element, the measurable unselected element, and the known element.
・ If the measurement element is used during analysis, all the recommended mass numbers are measured mass numbers.
・ When the measurement element is used during adjustment and diagnosis, the mass number with the highest priority among the recommended mass numbers is taken as the measurement mass number.
・ Selecting an element by right-clicking displays an element-specific information screen.
[0093]
(2) Isotope information table
-Single line selection. The interference ion information corresponding to the selected mass number is displayed.
・ Click the left button on the cell for the measured mass number to change the selected state of the measured mass number.
[0094]
(3) Interfering element ion (interfering molecular ion) information table
・ Select a single line.
[0095]
(4) Interference ion information specification
Specify interference molecule ion information to be displayed in the interference molecule ion information table.
[0096]
(5) Measurement mass number table
・ Select multiple lines.
-“Delete”: The selected mass number is not measured.
-“Delete all”: All measured mass numbers are not measured.
• “Mass number setting”: Displays the measurement mass number setting screen.
• “Molecular name setting”: Displays the measurement molecule name setting screen.
[0097]
▲ 6 ▼ Other
“OK”: After confirming the settings, close the dialog and save to the storage device.
・ "Cancel": Invalidate the settings and close the dialog.
[0098]
When the Plasma 3DQ icon 135 on the desktop is clicked, the software is activated and the sensitivity adjustment screen shown in FIG. 13 is displayed. Sensitivity is adjusted via this screen.
[0099]
When the condition setting button 136 of the condition setting unit 132 is clicked, a condition setting screen shown in FIG. 17 is displayed. On the screen unit 133, an analysis mode, an operator, a comment, an element, and an element selection button 137 are displayed. When the element selection button 137 is clicked, an element selection screen shown in FIG. 18 is displayed. The element selection screen includes a periodic table display unit 141 in the upper left, an interference ion information display unit 142 in the lower part, an interfering molecular ion information display unit 143 in the lower part, an isotope information display unit 144 in the upper right part, and a measurement in the lower part. It consists of an element name display unit 145 and a measurement range setting unit 146 at the right end.
[0100]
This time, an element having a mass number of 50 to 58 is measured. When the measurement range setting button 147 of the measurement range setting unit 146 is clicked, the measurement range setting screen shown in FIG. 19 is displayed, and the measurement range setting screen 148 is displayed. On this screen, enter the measurement start mass number 50 and the measurement end mass number 58 and press the add button 149.
[0101]
As shown in FIG. 20, on the measurement range setting screen 148, the isotopic ratios of mass numbers 50 to 58 are shown by color. When the display portion is enlarged, it is as shown in FIG. 21, and the degree of interference with the mass number where the intensity of the measured ions is maximum can be immediately confirmed.
[0102]
When the OK button 150 in FIG. 20 is clicked, the screen returns to the measurement element screen shown in FIG. In the periodic table, the element corresponding to the selected mass number is displayed in green. Further, the element name display section 145 at the lower right displays the measurement element, its mass number, and the overlapping element.
[0103]
FIG. 23 is a screen for deleting the overlap when the measured mass numbers overlap. That is, since 58Fe and 58Ni overlap, it is a screen which selects and deletes this. Since the mass numbers of 58Fe and 58Ni overlap, the mass number of the lower right measurement element is selected with the mouse and the delete button 151 is pressed to specify that 58Fe and 58Ni are not measured. In this way, it is specified that other overlapping elements are not measured.
[0104]
Next, when the OK button 150 is clicked, the measurement element and the measurement mass number are determined.
[0105]
Example 2: Selecting measurement elements from the periodic table
The sensitivity adjustment screen and the condition setting screen as the startup screen are the same screens as those shown in FIGS.
[0106]
Next, FIG. 18 shown in Example 1 is displayed on the screen. This is shown as FIG.
[0107]
This time, 54Cr and 54Fe are measured.
[0108]
Cr exists in mass numbers 50, 52, 53, and 54. Since it is generally advantageous in terms of sensitivity, the mass number with the highest abundance ratio is selected. In the case of Cr, it is 52.
[0109]
Fe exists in mass numbers 54, 56, 57, and 58. The mass number with the highest abundance ratio of Fe is 56.
[0110]
In some cases, molecular ions overlap, and a mass number with a high abundance ratio cannot be measured. In that case, another mass number is measured.
[0111]
This time, the case where Fe 54 and Cr 54 having the same mass number are measured as described above will be described.
[0112]
FIG. 25 is a diagram showing a state where Cr is clicked. Click the Cr button in the periodic table. The isotope information display unit 144 in the upper right of the screen displays the mass number of Cr and its abundance ratio.
[0113]
At the same time, elements with overlapping mass numbers are shown in pink on the periodic table. In the case of Cr, Ti, V, and Fe overlap, but these are identified at a glance by color display.
[0114]
FIG. 26 is a diagram showing a state in which 54Cr is selected.
[0115]
Click the mass number 54 in the isotope information displayed in the isotope information display unit 144.
[0116]
Then, 54Cr is displayed as the measurement element in the measurement element name display section 145 at the lower right of the screen.
[0117]
FIG. 27 is a screen showing a state in which Fe is clicked.
[0118]
When Fe is clicked on the periodic table, 54 isotopes 54Fe, 56Fe, 57Fe and 58Fe are displayed together with their abundance ratios in the isotope information display section 144. At the same time, elements with overlapping mass numbers are displayed in pink on the periodic table. In the case of Fe, Cr and Ni overlap, but these are identified at a glance by color display.
[0119]
FIG. 28 is a screen showing a state in which 54Fe is selected.
[0120]
Click the mass number 54 in the isotope information displayed in the isotope information display unit 144.
[0121]
If it does so, 54Cr54Fe will be displayed according to 54Cr already displayed. If measurement is performed in this state, both Fe and Cr are measured at a mass number of 54. Therefore, in this state, it is not known whether the mass number 54 is a measurement result of Cr or a measurement result of Fe. The user determines the overlap of the mass numbers and presses the delete button 151 to exclude 54Cr54Fe from the measurement as shown in FIG.
[0122]
If the OK button 152 is clicked after determining the mass number overlap in this way, the measurement element and the measurement mass number are determined.
[0123]
Next, interference ion information displayed on the interference ion information display unit 142 and interference molecule ion information displayed on the interference molecule ion information unit 143 in this example will be described.
[0124]
As interference ion information, as shown in FIG. 25 or FIG. 26, interference element ions are drawn out from the storage device 104 and displayed within an appropriate range.
[0125]
The user can see the overlap of the isotope information by looking at the interference ion information. From the display of the isotope information, the indication of the measurement element, and the overlap of the measurement element, the measurement element name display unit 145 determines the measurement element as described above. And the measurement mass number is determined accordingly.
[0126]
As interference molecule ion information, specify chloride ions, nitrate ions, sulfate ions, environmental water, and user 1, user 2, user 3, and user 4 interference ions that are arbitrarily specified by the user, and delete these from the measurement element. Can do.
[0127]
Example 3: Example of selecting measurement element from mass number
The sensitivity adjustment screen, the condition setting screen, and the element selection screen as the startup screen are the same screens as those shown in FIGS. 16, 17, and 18 shown in Example 1.
[0128]
18, when the measurement range setting button 147 is clicked, the measurement range setting screen shown in FIG. 29 is displayed.
[0129]
FIG. 30 is a screen for determining the measured mass number.
[0130]
This time, mass number 50-70 shall be measured. In FIG. 27, the measurement start mass number 50 and the measurement end mass number 70 are input, and the add button 160 is pressed. Using the graph, the mass number can be selected by dragging the mouse.
[0131]
FIG. 31 is a measurement element screen.
[0132]
In FIG. 30, when the OK button 150 is clicked, the screen shown in FIG. 28 is displayed. That is, returning to the measurement element screen, the element corresponding to the selected mass number becomes green. Further, the measurement element, the mass number, and the overlap thereof are displayed in the measurement element name display section 145 in the lower right.
[0133]
FIG. 32 is a screen for performing deletion when the measured mass numbers overlap.
[0134]
When the measurement mass numbers are overlapped, it is possible to designate not to measure this element by selecting the overlapping element, for example, 58Fe58Ni with the mouse and pressing the delete button 151. FIG. 29 shows a screen to be selected and deleted because 58Fe and 58Ni overlap.
[0135]
In this way, after deleting the overlapped elements, when the OK button is clicked, the measurement element and the measurement mass number are determined.
[0136]
Example 4: Application example for selecting measurement elements contained in tap water
As a point to keep in mind when analyzing water quality, the element to be measured has a concentration of μg / L and contains a lot of contaminants such as Na, Ca and Mg, and there is an oxide as a spectral interference substance. Can be mentioned. In addition, as an increase in elements to be measured due to stricter regulations, U (uranium) can be measured.
[0137]
For the former, by implementing measures such as cooling the spray chamber, suppressing the amount of material introduced, increasing the plasma temperature, reducing molecular ions caused by Ar, and the above-described Examples 1 to 3 Water quality analysis can be performed by adopting.
[0138]
FIG. 33 shows a state where, for water quality analysis, 15 elements and U are specified in the periodic table, and 54Cr54Fe and 56Fe40Ar16O having the same mass are deleted. This eliminates interference ions and performs water quality analysis.
[0139]
Next, an example in which the state in which ions are operating in the mass spectrometer is displayed on the screen will be described. Since the state diagram displayed on the screen simulates the actual operating state of ions and is enlarged and shown electronically, it is expressed herein as “ionons” on the screen.
[0140]
FIG. 34 shows a state where the plasma is extinguished and only the vacuum system is moving. This state is a stop state of the apparatus. The vacuum system is always working.
[0141]
On the screen, the configuration of the main body 101 of the apparatus shown in FIG. 12 is displayed. The display may be the same, but it may be displayed in addition to indicate the presence of Ar or He to be input and its use state.
[0142]
In the figure, the plasma is before lighting, and ions are not taken into the ion take-in part 112, so there is no movement of ion ions.
[0143]
FIG. 35 shows a state in which the plasma is turned on and the gate valve portion 113 is closed. Plasma is lit and RF for lighting is output. Further, cooling water is also introduced into the ion intake unit 112. Since the gate valve portion 113 is closed, ions are introduced only before the gate valve portion 113. In addition, the downstream side of the gate valve portion 113 of the vacuum system is not in operation.
[0144]
In the image processing apparatus, since the ion uptake is performed and the gate valve unit 113 is closed, the ions that display the taken-in ions are moved in the path to the gate valve unit 113, and the downstream side of the gate valve unit 113. Then, Ion's dynamics are not displayed.
[0145]
In FIG. 36, the details button 160 is clicked and the inspection items shown in the figure are displayed below it. For example, they are output values that indicate the state of the detector, RF output, plasma gas, carrier gas, auxiliary gas, etc.
[0146]
FIG. 37 shows a state where the gate valve unit 113 is open and the 3DQMS 117 is stopped. The plasma is still in a lighting state, and RF for lighting is also output. Further, cooling water is also introduced into the ion intake portion 112. Since the gate valve 113 is opened, the ions are introduced to the latter stage of the vacuum system. However, since 3DQMS 117 is OFF, ions pass through 3DQMS.
[0147]
The image processing apparatus operates so that ions are taken in and the gate valve unit 113 is opened, so that the ions that display the taken-in ions pass through the passage to the gate valve unit 113 and the 3DQMS. And display.
[0148]
FIG. 38 shows a state where the gate valve unit 113 is open and the 3DQMS 117 is operating. The plasma is still in a lighting state, and RF for lighting is also output. Further, cooling water is also introduced into the ion intake portion 112. Since the gate valve portion 113 is open, the ions are introduced to the latter stage of the vacuum system, and the 3DQMS 117 is turned on, so that the ions are introduced into the 3DQMS.
[0149]
In the image processing apparatus, ions are taken in, the gate valve unit 113 is opened, and the 3DQMS 117 is in operation. In particular, in the 3DQMS section, the ionons are moved and displayed as if they are 8 characters. The same applies to the case where QMS is adopted as the analyzer, and in this case, the image processing apparatus displays ion ions for displaying captured ions when ions are captured and the gate valve portion is closed. When the gate valve section is opened and the path to the mass analysis section is closed, the ions are moved up and displayed in the path to the ion deflection section. When the analysis in is performed, the ionons are moved to the mass spectrometer and displayed.
[0150]
As described above, the mass spectrometer is configured to ionize a sample to generate ions, generate an ion from the ion source, take in ions taken from the ion source, and extract and focus ions taken from the ion take-in unit. A converging lens unit, and an ion deflecting unit that deflects ions converged by the converging lens unit by a deflecting lens and introduces the ions into a mass analyzing unit, and a skimmer having a small hole is provided at the entrance of the ion capturing unit, Argon (Ar) gas is introduced into the ion source, and helium (He) gas is introduced into the mass spectrometer.
[0151]
The image processing apparatus displays that argon gas and helium gas are being introduced, and plasma that reaches the tip of the skimmer from the ion source on the premise that the indication is being performed. The image will be displayed with simulated combustion.
[0152]
The image processing apparatus displays an argon gas cylinder for argon gas, and displays the argon gas cylinder separately when the argon gas is introduced, when it is deficient, and when it is consumed. The ion extraction state, the ion shield state, the use state of the torch used for the ion source, and the state of the peristaltic pump for loading the sample are displayed.
As described above, according to the present embodiment, in the mass spectrometry method for performing analysis by specifying a plurality of measurement elements using an ion trap, the ion mass that interferes with the isotope information of the element and the ion mass number of the element. The number of element ions is memorized, the periodic table is displayed on one screen, and by specifying the elements shown in the periodic table, the isotopes of the elements and the isotope information including their ion mass numbers are obtained. The element ion of the ion mass number that interferes with the ion mass number is displayed as interference ion information together with the mass number, and the molecular ion of the ion mass number that interferes with the ion mass number is displayed as interference ion information together with the mass number. Display the isotope element that is a candidate for measurement from the isotope information, delete the isotope element with the same mass number, delete the interfering molecular ion, and set the measurement element on the screen. Mass spectrometry of a sample and performing is formed.
Further, according to the present embodiment, in the mass spectrometry method for performing analysis by designating a plurality of measurement elements using an ion trap, the ion mass number that interferes with the isotope information of the element and the ion mass number of the element. Memorizes element ions, sets the ion mass number measurement range on the screen, and displays the isotope elements of the elements in the ion mass number measurement range set on the screen as the isotope information with the ions and the mass number The element ion of the ion mass number that interferes with the ion mass number is displayed as interference ion information together with the mass number, and the molecular ion of the ion mass number that interferes with the ion mass number is also displayed along with the mass number. Display the isotope element as a measurement candidate from the isotope information, delete the isotope element with the same mass number and delete the interfering molecular ion, and Mass spectrometry of a sample for setting is constituted.
Further, according to the present embodiment, in a mass spectrometer that performs analysis by specifying a plurality of measurement elements using an ion trap, the ion mass number that interferes with the isotope information of the element and the ion mass number of the element A storage device that stores element ions, displays a periodic table on one screen, and designates the elements shown in the periodic table to specify the isotopes of the elements and the isotope information including their ion mass numbers , Element ions having an ion mass number that interferes with the ion mass number are displayed as interference ion information together with the mass number, and molecular ions having an ion mass number that interferes with the ion mass number are also displayed along with the mass number. Display the isotope element that is a candidate for measurement from the isotope information, delete the isotope element with the same mass number and delete the interfering molecular ion, and display the measurement source on the screen. Mass spectrometer of samples and a screen processing unit for setting a constitute.
In addition, according to the present embodiment, in a mass spectrometer that performs analysis by specifying a plurality of measurement elements using an ion trap, an element having an ion mass number that interferes with the isotope information of the element and the ion mass number of the element A storage device for storing ions, setting an ion mass measurement range on the screen, and isotopic elements of elements in the ion mass number measurement range set on the screen together with the ion mass number as isotope information Display on the screen, display element ions of the ion mass number that interferes with the ion mass number as interference ion information together with the mass number, and further display molecular ions of the ion mass number that interfere with the ion mass number together with the mass number. Information, displaying isotope elements as measurement candidates from the isotope information, deleting isotope elements having the same mass number, and deleting interfering molecular ions. Constituting the mass spectrometer of the sample and a screen processing unit for setting the measurement element above.
[0153]
【The invention's effect】
According to the present invention, the isotope information of the element ion to be measured and the interference ion having the same mass number as the isotope are displayed on the same screen, and the operation of deleting the isotope element in which the interference ion exists can be performed on the same screen. Therefore, many elements can be set as measurement elements, and instead of selecting one element from each measurable element one by one, the measurement elements are set on the screen as described above. Measurement accuracy can be improved without induction. In addition, according to the present invention, since the measurement element can be easily set as described above, it is possible to confirm at a glance which mass number is measured, so that the confirmation work of the measurement result is facilitated. In addition, even when a plurality of elements are selected, since no labor is required, versatility is improved, and applicability to analysis on various samples can be expected.
[0154]
Further, according to the present invention, the analysis condition setting can be diversified, the measurement element setting by designating the element using the periodic table, the measurement element setting by designating the mass number range, It becomes easy to expand the method of setting the measurement element, such as setting the measurement element by displaying the abundance ratio of the isotope in a graph.
[0155]
According to the present invention, the operation of the ionon is vibrated on the screen in conjunction with the ion intake, opening / closing of the gate valve unit, and the operation of the mass spectrometer unit, so that the operation status can be clearly identified on the screen. Therefore, it is easy to avoid making a mistake in the measurement procedure, and there is an advantage that the user can use it easily.
[0156]
As described above, as the user becomes easy to use, it is easy to analyze the contained elements even for materials containing multiple elements such as water quality analysis, and the versatility is improved.
[Brief description of the drawings]
FIG. 1 is a configuration diagram centering on a horizontal plane of an apparatus main body.
FIG. 2 is a configuration diagram centering on a vertical plane of the apparatus main body.
FIG. 3 is a component configuration diagram.
FIG. 4 is a plan layout view of the apparatus main body.
FIG. 5 is a front layout view of the apparatus main body.
FIG. 6 is a side layout view of the apparatus main body.
FIG. 7 is an external view of the apparatus main body.
FIG. 8 is a diagram for mainly explaining a door portion.
9 is a view from the other side of FIG.
FIG. 10 is a configuration diagram regarding another example of FIG. 8;
FIG. 11 is an example showing a modification.
FIG. 12 is a block diagram of an embodiment of the present invention.
FIG. 13 is a diagram for explaining determination of parent ions and ion introduction.
FIG. 14 is a diagram for explaining determination of parent ions and ion introduction.
FIG. 15 is a screen diagram at startup.
FIG. 16 is a sensitivity adjustment screen (screen at startup).
FIG. 17 is a condition setting screen diagram.
FIG. 18 is an element selection screen diagram.
FIG. 19 is a measurement range setting screen diagram.
FIG. 20 is a screen view for determining the measured mass number.
FIG. 21 is a partially enlarged view of FIG.
FIG. 22 is a measurement element screen view.
FIG. 23 is a screen diagram for deleting a selected element.
FIG. 24 is an element selection screen diagram.
FIG. 25 is a state diagram in which Cr is clicked.
FIG. 26 is a state diagram in which 54Cr is selected.
FIG. 27 is a state diagram in which Fe is clicked.
FIG. 28 is a state diagram in which 54Fe is selected.
FIG. 29 is a measurement range setting screen diagram.
FIG. 30 is a screen view for determining the measured mass number.
FIG. 31 is a measurement element screen view.
FIG. 32 is a screen diagram for deleting a selected element.
FIG. 33 is an element selection screen diagram for water quality analysis.
FIG. 34 is a diagram showing a state where the apparatus is stopped.
FIG. 35 is a state diagram in which the gate valve is closed.
FIG. 36 is a state diagram for displaying detection items in the state shown in FIG. 35;
FIG. 37 is a state diagram in which the gate valve is opened and 3DQMS is stopped.
FIG. 38 is a state diagram in which 3DQMS is operating with the gate valve opened.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 100 ... Ion source mass spectrometer, 101 ... Main part, 102 ... Controller, 103 ... Arithmetic unit (CPU), 104 ... Monitor, 105 ... Memory | storage device, 106 ... Isotope element display, 107 ... Deletion of the same mass element, 108 ... deletion of interference ions, 109 ... determination of mass number of measurement ions, 111 ... ion source, 112 ... ion take-in part, 113 ... gate valve part, 114 ... converging lens part, 115 ... deflection part, 116 ... mass analysis part, 117 ... 3DQMS unit, 118 ... detection unit, 131 ... icon item unit, 132 ... condition setting unit, 133 ... screen unit, 134 ... status display unit, 141 ... synchronization table display unit, 142 ... interference ion information display unit, 143 ... interfering molecule ion information display part, 144 ... isotope information display part, 145 ... measurement element name display part, 146 ... measurement range setting part.

Claims (7)

In a mass spectrometry method that uses an ion trap to perform analysis by specifying multiple measurement elements,
Memorizes the isotope information of an element and the ion of the ion mass number that interferes with the ion mass number of the element,
By specifying the element or mass number on one screen, the isotope information of the element and its ion mass number are displayed, and ions with the ion mass number that interferes with the ion mass number are interfered with the mass number. display as an ion information, the display of the isotope to be measured candidate isotopic information, and delete the same isotope of the mass number from the measuring elements go together display the same isotope of mass number A method for mass spectrometry of a sample, characterized in that a measurement element is set on the screen. In a mass spectrometry method that uses an ion trap to perform analysis by specifying multiple measurement elements,
Memorize element isotopic information and element ions of ion mass number that interferes with ion mass number of the element,
The periodic table is displayed on one screen, and isotope information including the isotopes of the elements and their ion mass numbers is displayed by designating the elements shown in the periodic table, and interferes with the ion mass numbers. Element ions of the mass number of ions to be displayed as interference ion information together with the mass number, isotope elements that are measurement candidates are displayed from the isotope information, and isotope elements having the same mass number are displayed together. A method for mass spectrometry of a sample , wherein the same number of isotope elements are deleted from the measurement element and the measurement element is set on the screen. In a mass spectrometry method that uses an ion trap to perform analysis by specifying multiple measurement elements,
Memorize element isotopic information and element ions of ion mass number that interferes with ion mass number of the element,
Ion mass number measuring range set on the screen,
Display isotopes of an element in the ion mass number measured range set on said screen to screen isotopically information together with its ion Weight number,
The element ion of the ion mass number that interferes with the ion mass number is displayed as interference ion information together with the mass number,
The isotopic information to display the isotope to be measured candidates, and deletes the same isotope of the mass number from the measuring elements go together display the same isotope of mass number, measured on the screen A method for mass spectrometry of a sample, wherein the element is set. In a mass spectrometry method for analyzing water quality by specifying multiple measurement elements using an ion trap,
A plurality of ion mass number measurement ranges including the uranium (U) mass number range are set on the screen, isotope information including isotope elements in the ion mass number measurement range is displayed, and the ion mass of the isotope element is displayed. Interfering ion information including the element ion of the ion mass number interfering with the number and the mass number, and displaying the molecular ion of the ion mass number interfering with the ion mass number together with the mass number as interference ion information, On the screen displaying isotope information and interference ion information, display isotope elements with the same mass number, delete isotope elements with the same mass number from the measurement elements, and set the measurement elements including the uranium isotope A mass spectrometry method for analyzing water quality, characterized in that In a mass spectrometer that performs analysis by specifying multiple measurement elements using an ion trap,
A storage device that stores isotope information of an element and ions having an ion mass number that interferes with the ion mass number of the element;
By specifying the element or mass number on one screen, the isotope information of the element and its ion mass number are displayed, and ions with the ion mass number that interferes with the ion mass number are interfered with the mass number. Display as ion information, display isotope elements as measurement candidates from the isotope information, and display isotope elements with the same mass number and delete the isotope elements with the same mass number from the measured element stomach line, mass spectrometer of the sample, characterized in that it comprises a screen processing unit for setting the measurement element on the screen. In a mass spectrometer that performs analysis by specifying multiple measurement elements using an ion trap,
A storage device for storing element isotopic information and element ions having an ion mass number that interferes with the ion mass number of the element;
By displaying the elements shown in the periodic table on one screen, isotope information including the isotopes of the elements and their ion mass numbers is displayed, and element ions having ion mass numbers that interfere with the ion mass numbers are displayed. It is displayed as interference ion information together with the mass number, isotope elements that are measurement candidates from the isotope information, and isotope elements with the same mass number are displayed together to measure the isotope elements with the same mass number. There line to be removed from elemental mass spectrometer of the sample, characterized in that it comprises a screen processing unit for setting the measurement element on the screen. In a mass spectrometer that performs analysis by specifying multiple measurement elements using an ion trap,
A storage device for storing element isotopic information and element ions having an ion mass number that interferes with the ion mass number of the element;
The ion mass measurement range is set on the screen, and the isotope element of the element in the ion mass number measurement range set on the screen is displayed on the screen as the isotope information together with the ion mass number. The interfering ion mass number element ion is displayed together with the mass number as interference ion information, the isotope element as a measurement candidate is displayed from the isotope information, and the isotope elements having the same mass number are displayed together. remove the same isotope of mass number from the measuring element, the mass spectrometer of the sample, characterized in that it comprises a screen processing unit for setting the measurement element on the screen.

Images