JPH06260134A - Heat vaporization inductively coupled plasma mass-spectrographic device - Google Patents
Heat vaporization inductively coupled plasma mass-spectrographic deviceInfo
- Publication number
- JPH06260134A JPH06260134A JP5045444A JP4544493A JPH06260134A JP H06260134 A JPH06260134 A JP H06260134A JP 5045444 A JP5045444 A JP 5045444A JP 4544493 A JP4544493 A JP 4544493A JP H06260134 A JPH06260134 A JP H06260134A
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- Japan
- Prior art keywords
- heating furnace
- furnace
- inductively coupled
- coupled plasma
- mass
- Prior art date
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は、試料溶液中の微量不
純物の分析を行う誘導結合プラズマ質量分析装置に関
し、特に微少試料量の分析を行う加熱気化誘導結合プラ
ズマ質量分析装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an inductively coupled plasma mass spectrometer for analyzing trace impurities in a sample solution, and more particularly to a heating vaporization inductively coupled plasma mass spectrometer for analyzing a minute amount of sample.
【０００２】[0002]
【従来の技術】従来技術の例を模式図を用いて説明す
る。図２において、１はボンベ、２はレギュレーター、
３は流量制御部、４は加熱炉、６および７は電極、８は
輸送管、９はプラズマトーチ、１０はワークコイル、１
１は誘導結合プラズマ、１２はサンプリングオリフィ
ス、１３は質量分析部である。加熱炉４は上部に試料溶
液を注入するための孔５が開いた円筒状の構造で、電極
６及び７をとおして通電することにより加熱される。キ
ャリアガスはボンベ１中のガスをレギュレーター２によ
り一定の圧力に減圧された後、１から１．５ｌ／ｍｉｎ
程度に流量制御部３で制御され、加熱炉４及び輸送管８
を通してプラズマトーチ９に流される。ここでキャリア
ガスは例えばアルゴンガスが使用される。2. Description of the Related Art An example of prior art will be described with reference to schematic diagrams. In FIG. 2, 1 is a cylinder, 2 is a regulator,
3 is a flow rate control unit, 4 is a heating furnace, 6 and 7 are electrodes, 8 is a transport tube, 9 is a plasma torch, 10 is a work coil, 1
Reference numeral 1 is an inductively coupled plasma, 12 is a sampling orifice, and 13 is a mass spectrometric section. The heating furnace 4 has a cylindrical structure in which a hole 5 for injecting a sample solution is opened in the upper portion, and is heated by supplying electricity through the electrodes 6 and 7. As the carrier gas, the gas in the cylinder 1 was depressurized to a constant pressure by the regulator 2 and then 1 to 1.5 l / min.
The flow rate control unit 3 controls the heating furnace 4 and the transport pipe 8 to some extent.
Through the plasma torch 9. Here, for example, argon gas is used as the carrier gas.
【０００３】試料溶液は５から５０ｍｌ程度加熱炉４に
滴下されて１００℃前後で脱溶媒されたのち３００から
１０００℃で灰化される。測定すべき試料溶液中の不純
物元素は、その後１５００から３０００℃に加熱されて
原子蒸気化され、キャリアガスとともに輸送管８を通し
てプラズマトーチ９にいたる。プラズマトーチ９の先端
ではワークコイル１０により例えば２７．１２ＭＨｚの
高周波が印加されており、キャリアガス及び原子化蒸気
は誘導結合して誘導結合プラズマ１１となる。質量分析
部１３の誘導結合プラズマ１１の軸上にはサンプリング
オリフィスと呼ばれる径１ｍｍ程度の孔１２が開いてい
る。原子化蒸気は、誘導結合プラズマ１１内でイオン化
されてサンプリングオリフィス１２を通して質量分析部
１３に入り、質量分析されて元素同定あるいは定量され
る。About 5 to 50 ml of the sample solution is dropped into the heating furnace 4, desolvated at around 100 ° C., and then ashed at 300 to 1000 ° C. The impurity element in the sample solution to be measured is then heated to 1500 to 3000 ° C. to be atomized and reaches the plasma torch 9 through the transport tube 8 together with the carrier gas. A high frequency of, for example, 27.12 MHz is applied by the work coil 10 at the tip of the plasma torch 9, and the carrier gas and atomized vapor are inductively coupled to form an inductively coupled plasma 11. On the axis of the inductively coupled plasma 11 of the mass spectrometric section 13, a hole 12 having a diameter of about 1 mm called a sampling orifice is opened. The atomized vapor is ionized in the inductively coupled plasma 11 and enters the mass spectrometric section 13 through the sampling orifice 12 and is mass spectrometrically identified or quantified.
【０００４】[0004]
【発明が解決しようとする課題】しかし、従来技術では
加熱によって生成された原子蒸気が加熱炉壁に吸着し、
プラズマトーチ９には原子蒸気の一部しか輸送されない
問題があった。このため測定する不純物元素の検出下限
が２桁ｐｐｔ（ｐｐｔは、１０-12 ）程度であり、例え
ば半導体産業で管理されるべき不純物レベルを測定する
には感度不足であった。さらに従来技術では加熱炉壁へ
の吸着量が変動するため定量分析値のバラツキが大きく
信頼性が乏しいという課題があった。However, in the prior art, the atomic vapor generated by heating is adsorbed on the wall of the heating furnace,
The plasma torch 9 had a problem that only part of the atomic vapor was transported. Therefore, the lower limit of detection of the impurity element to be measured is about two digits ppt (ppt is 10 −12 ), and the sensitivity is insufficient for measuring the impurity level to be controlled in the semiconductor industry, for example. Further, the conventional technique has a problem that the amount of adsorption on the wall of the heating furnace fluctuates and the quantitative analysis value greatly varies, resulting in poor reliability.
【０００５】この発明は、加熱気化誘導結合プラズマ質
量分析装置の感度向上及び安定性向上をさせて、従来の
このような課題を解決することを目的としたものであ
る。An object of the present invention is to improve the sensitivity and stability of a heating vaporization inductively coupled plasma mass spectrometer and solve such a conventional problem.
【０００６】[0006]
【課題を解決するための手段】上記課題を解決するため
に、この発明は試料溶液をグラファイト製の加熱炉に滴
下し、前記加熱炉を高温で加熱することにより前記不純
物を原子蒸気化し、前記原子蒸気を流量制御されたキャ
リアガスにより誘導結合プラスマを発生するプラスマト
ーチに輸送し、前記誘導結合プラズマにより前記原子蒸
気をイオン化して質量分析部で質量分離して検出する加
熱気化誘導結合プラズマ質量分析装置において、前記加
熱炉と前記プラスマトーチをむすぶ輸送路内および、前
記加熱炉のキャリアガス供給路に、少なくとも前記加熱
炉の容積の約５倍以上の容積をもったガスだめを、加熱
炉に近接して設置したことにより、感度向上及び安定性
の向上を図れるようにしたものである。In order to solve the above-mentioned problems, the present invention is to drop the sample solution into a heating furnace made of graphite and heat the heating furnace at a high temperature to atomize the impurities, Heating vaporized inductively coupled plasma mass, which transports atomic vapor to a plasma torch that generates inductively coupled plasma by a carrier gas whose flow rate is controlled, and ionizes the atomic vapor by the inductively coupled plasma and mass-separates and detects it in a mass spectrometric unit. In the analyzer, a gas reservoir having a volume of at least about 5 times or more of the volume of the heating furnace is provided in the transportation path connecting the heating furnace and the plasma torch and in the carrier gas supply path of the heating furnace. By installing it close to, it is possible to improve sensitivity and stability.
【０００７】[0007]
【作用】上記のように構成された加熱気化誘導結合プラ
ズマ質量分析装置においては、加熱炉の加熱によって加
熱炉内のガスが自由に膨張できるので、原子蒸気を含ん
だ加熱炉内のガス圧力が増大しない。このため加熱炉壁
と原子蒸気の相互作用時間が著しく短縮されかつ、原子
蒸気の分圧も低くなり加熱炉壁への吸着量を低減でき
る。さらに、膨張の過程で原子蒸気は急速に冷却され酸
化物分子などに変換されるので、加熱炉壁や輸送管壁と
の相互作用が起こりにくくなり加熱炉壁や輸送管壁への
吸着ロスを低減できる。すなわち、加熱炉壁や輸送管壁
への吸着ロスを減少することにより、プラスマトーチへ
の試料の輸送効率向上させて感度を向上させた。さら
に、吸着ロスの減少は、吸着ロスの絶対量の変動が小さ
いことなので、バラツキがなくて信頼性の高い測定値を
得られるようになった。In the heating vaporization inductively coupled plasma mass spectrometer configured as described above, since the gas in the heating furnace can freely expand by heating the heating furnace, the gas pressure in the heating furnace containing atomic vapor is Does not increase. For this reason, the interaction time between the heating furnace wall and the atomic vapor is remarkably shortened, and the partial pressure of the atomic vapor is lowered, so that the adsorption amount on the heating furnace wall can be reduced. Furthermore, during the expansion process, the atomic vapor is rapidly cooled and converted into oxide molecules, etc., so that the interaction with the heating furnace wall and the transportation tube wall is less likely to occur, and the adsorption loss to the heating furnace wall and the transportation tube wall is reduced. It can be reduced. That is, by reducing the adsorption loss on the wall of the heating furnace and the wall of the transport tube, the efficiency of transporting the sample to the plasma torch was improved and the sensitivity was improved. Further, the decrease of the adsorption loss is small in the variation of the absolute amount of the adsorption loss, so that it is possible to obtain a highly reliable measurement value without variation.
【０００８】[0008]
【実施例】以下に、この発明の実施例を図に基づいて説
明する。図１は本発明の実施例を示す模式図で、ボンベ
１はキャリアガスを貯蔵しする。レギュレーター２は、
ボンベ１のキャリアガスを一定の圧力に減圧するもので
ある。流量制御部３は減圧されたキャリアガスを一定の
流量に制御するものである。流量制御部３により一定の
流量に制御されたキャリアガスは、ガスため１４に導入
される。グラファイト製の加熱炉４は横向きに配置され
た円筒形状をしており、試料溶液を加熱し、試料の不純
物を原子化するものである。加熱炉４の上方には試料を
加熱炉４に注入するための孔５が設けられている。加熱
炉４の両端には電極６が配置されており、電極６、６か
ら電力を加熱炉４に供給し、そして加熱炉４は加熱され
る。Embodiments of the present invention will be described below with reference to the drawings. FIG. 1 is a schematic diagram showing an embodiment of the present invention, in which a cylinder 1 stores a carrier gas. Regulator 2 is
The carrier gas in the cylinder 1 is depressurized to a constant pressure. The flow rate control unit 3 controls the depressurized carrier gas to a constant flow rate. The carrier gas controlled to have a constant flow rate by the flow rate control unit 3 is introduced into the gas reservoir 14. The heating furnace 4 made of graphite has a cylindrical shape arranged horizontally, and heats the sample solution to atomize the impurities in the sample. A hole 5 for injecting a sample into the heating furnace 4 is provided above the heating furnace 4. Electrodes 6 are arranged at both ends of the heating furnace 4, and electric power is supplied to the heating furnace 4 from the electrodes 6, 6 and the heating furnace 4 is heated.
【０００９】輸送管８は、加熱炉４にて原子化された試
料の不純物を加熱炉４からプラズマトーチ９に輸送する
ものであり、輸送管８と加熱炉４との間にガス溜１４が
設けられている。プラズマトーチ９の廻りには、ワーク
コイル１０が配置されており、ワークコイル１０に高周
波電力を供給することにより、プラズマトーチ９の先端
から排出される試料は、誘導結合プラズマ１１になる。
誘導結合プラズマ１１においてイオン化した試料の不純
物の一部は、サンプリングオリフィス１２を通って、質
量分析部１３に到達し、質量分析される。The transport pipe 8 transports the impurities of the sample atomized in the heating furnace 4 from the heating furnace 4 to the plasma torch 9, and a gas reservoir 14 is provided between the transportation pipe 8 and the heating furnace 4. It is provided. A work coil 10 is arranged around the plasma torch 9, and by supplying high-frequency power to the work coil 10, the sample discharged from the tip of the plasma torch 9 becomes the inductively coupled plasma 11.
A part of the impurities of the sample ionized in the inductively coupled plasma 11 reaches the mass spectrometric section 13 through the sampling orifice 12 and undergoes mass spectrometric analysis.
【００１０】ガスだめ１４は、加熱炉４と輸送管８の
間、および流量制御部３と加熱炉４のあいだに設置され
る。ガスだめ１４はいずれも加熱炉４に近接させて設置
される必要がある。ガスだめ１４の容積はそれぞれ加熱
炉の容積の約５倍以上が適当である。ガスだめ４の容積
を小さくすると吸着ロスを減少させる効果が減少する。The gas sump 14 is installed between the heating furnace 4 and the transport pipe 8 and between the flow rate control unit 3 and the heating furnace 4. Each of the gas sumps 14 needs to be installed close to the heating furnace 4. It is suitable that the volume of each gas reservoir 14 is about 5 times or more the volume of the heating furnace. If the volume of the gas reservoir 4 is reduced, the effect of reducing the adsorption loss is reduced.
【００１１】次ぎに動作について説明する。試料溶液を
孔５からグラファイト製の加熱炉４に滴下し、前記加熱
炉４を高温で加熱することにより前記不純物を原子蒸気
化し、前記原子蒸気を流量制御されたキャリアガスによ
り誘導結合プラスマを発生するプラスマトーチ１に輸送
し、前記誘導結合プラズマ１１により前記原子蒸気をイ
オン化して質量分析部１３で質量分離して検出する。Next, the operation will be described. The sample solution is dropped from a hole 5 into a heating furnace 4 made of graphite, the heating furnace 4 is heated at a high temperature to atomize the impurities, and an inductively coupled plasma is generated by a carrier gas whose flow rate is controlled. The atomic vapor is ionized by the inductively coupled plasma 11 and is mass-separated by the mass spectrometric section 13 for detection.
【００１２】加熱炉４を高温で加熱する過程で加熱炉内
のガスも加熱され、このガスの中に原子蒸気もふくまれ
る。等圧下では約１０倍の体積膨張が見込まれ、このと
きガスだめ１４が加熱炉の前後に設置されているので加
熱炉内の圧力上昇を起こさず、ガスはガスだめに向かっ
て自由に膨張する。一方、従来構成においては、ガスだ
め１４が無いので加熱炉内の圧力が上昇し、ガスの移動
も小さい。このため加熱炉と原子蒸気の接触時間は従来
構成にくらべ１０分の１になる。接触時間が短く、か
つ、原子蒸気の分圧も従来構成に比べ小さいので加熱炉
４の壁への吸着量を著しく減少できる。また、膨張によ
ってガスの温度が下がるので原子蒸気は酸化物分子など
の不活性な形態に変化し、加熱炉壁への吸着量の減少に
効果がある。なお、ゆうまでもなくガスだめ１４は、電
極６、６の内径でつくる容積を大きくすることによって
機能を兼用することもできる。During the process of heating the heating furnace 4 at a high temperature, the gas in the heating furnace is also heated, and atomic vapor is also included in this gas. Under equal pressure, a volume expansion of about 10 times is expected. At this time, since the gas sump 14 is installed before and after the heating furnace, the pressure in the heating furnace does not rise, and the gas expands freely toward the gas sump. . On the other hand, in the conventional configuration, since the gas reservoir 14 is not provided, the pressure in the heating furnace rises and the gas movement is small. Therefore, the contact time between the heating furnace and the atomic vapor is 1/10 of that of the conventional configuration. Since the contact time is short and the partial pressure of atomic vapor is smaller than that of the conventional structure, the amount of adsorption onto the wall of the heating furnace 4 can be significantly reduced. Further, since the temperature of the gas decreases due to the expansion, the atomic vapor changes into an inactive form such as oxide molecules, which is effective in reducing the amount of adsorption on the wall of the heating furnace. Needless to say, the gas sump 14 can also have a function by increasing the volume formed by the inner diameters of the electrodes 6, 6.
【００１３】[0013]
【発明の効果】この発明は、以上説明したように試料溶
液をグラファイト製の加熱炉に滴下し、前記加熱炉を高
温で加熱することにより試料溶液中の不純物元素を不純
物を原子蒸気化し、前記原子蒸気を流量制御されたキャ
リアガスにより誘導結合プラズマを発生するプラスマト
ーチに輸送し、前記誘導結合プラズマにより前記原子蒸
気をイオン化して質量分析部で質量分離して検出する加
熱気化誘導結合プラズマ質量分析装置において、前記加
熱炉と前記プラスマトーチをむすぶ輸送路内および、前
記加熱炉のキャリアガス供給路に、少なくとも前記加熱
炉の容積の約５倍以上の容積をもったガスだめを、加熱
炉に近接して設置したことを特徴とした構成なので、加
熱炉壁への吸着量を著しく減少でき、感度を１桁向上さ
せ、しかも吸着ロス量の絶対量がへるので、吸着ロス量
の変動の割合は小さくなり、その結果安定した測定値を
得ることができる効果がある。As described above, according to the present invention, the sample solution is dropped into a graphite heating furnace, and the heating furnace is heated at a high temperature to atomize the impurity elements in the sample solution into atomic vapors. Heating vaporized inductively coupled plasma mass that transports atomic vapor to a plasma torch that generates inductively coupled plasma by a carrier gas whose flow rate is controlled, and ionizes the atomic vapor by the inductively coupled plasma and mass-separates and detects it in a mass spectrometer In the analyzer, a gas reservoir having a volume of at least about 5 times or more of the volume of the heating furnace is provided in the transportation path connecting the heating furnace and the plasma torch and in the carrier gas supply path of the heating furnace. Since it is installed close to the furnace, the amount of adsorption to the heating furnace wall can be significantly reduced, the sensitivity is improved by one digit, and the adsorption Since the absolute amount of the amount is reduced, the ratio of the variation of the adsorption amount of loss is small, there is an effect that it is possible to obtain the result stable measurement value.
【図１】本発明の実施例を示した概略模式図である。FIG. 1 is a schematic diagram showing an example of the present invention.
【図２】従来技術を示す概略模式図である。FIG. 2 is a schematic diagram showing a conventional technique.
１ ボンベ ２ レギュレーター ３ 流量制御部 ４ 加熱炉 ５ 孔 ６ 電極 ８ 輸送管 ９ プラズマトーチ １０ ワークコイル １１ 誘導結合プラズマ １２ サンプリングオリフィス １３ 質量分析部 １４ ガスだめ 1 cylinder 2 regulator 3 flow control unit 4 heating furnace 5 hole 6 electrode 8 transport tube 9 plasma torch 10 work coil 11 inductively coupled plasma 12 sampling orifice 13 mass spectrometry unit 14 gas sump
Claims (1)
下し、前記加熱炉を高温で加熱することにより前記不純
物を原子蒸気化し、前記原子蒸気を流量制御されたキャ
リアガスにより誘導結合プラスマを発生するプラスマト
ーチに輸送し、前記誘導結合プラズマにより前記原子蒸
気をイオン化して質量分析部で質量分離して検出する加
熱気化誘導結合プラズマ質量分析装置において、前記加
熱炉と前記プラスマトーチをむすぶ輸送路内および、前
記加熱炉のキャリアガス供給路に、ガスだめを持ち、前
記ガスだめ野容積が、少なくとも前記加熱炉の容積の約
５倍以上であり、前記ガスだめは加熱炉に近接して設置
されることを特徴とする、加熱気化誘導結合プラズマ質
量分析装置。1. A sample solution is dropped into a heating furnace made of graphite, and the heating furnace is heated at a high temperature to atomize the impurities, and an inductively coupled plasma is generated by a carrier gas whose flow rate is controlled. A heating vaporization inductively coupled plasma mass spectrometer, which transports to the plasma torch, ionizes the atomic vapor by the inductively coupled plasma, and mass-separates and detects the mass in a mass spectrometer. A gas reservoir is provided inside and in the carrier gas supply path of the heating furnace, the gas reservoir volume is at least about 5 times the volume of the heating furnace, and the gas reservoir is installed close to the heating furnace. A heating vaporization inductively coupled plasma mass spectrometer, which is characterized in that:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05045444A JP3116151B2 (en) | 1993-03-05 | 1993-03-05 | Heated vaporization inductively coupled plasma mass spectrometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05045444A JP3116151B2 (en) | 1993-03-05 | 1993-03-05 | Heated vaporization inductively coupled plasma mass spectrometer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06260134A true JPH06260134A (en) | 1994-09-16 |
| JP3116151B2 JP3116151B2 (en) | 2000-12-11 |
Family
ID=12719507
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP05045444A Expired - Fee Related JP3116151B2 (en) | 1993-03-05 | 1993-03-05 | Heated vaporization inductively coupled plasma mass spectrometer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3116151B2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008544454A (en) * | 2005-06-17 | 2008-12-04 | パーキンエルマー・インコーポレイテッド | Strengthening device and method of using the same |
| US8786394B2 (en) | 2010-05-05 | 2014-07-22 | Perkinelmer Health Sciences, Inc. | Oxidation resistant induction devices |
| US8829386B2 (en) | 2010-05-05 | 2014-09-09 | Perkinelmer Health Sciences, Inc. | Inductive devices and low flow plasmas using them |
| US8896830B2 (en) | 2005-06-17 | 2014-11-25 | Perkinelmer Health Sciences, Inc. | Devices and systems including a boost device |
-
1993
- 1993-03-05 JP JP05045444A patent/JP3116151B2/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008544454A (en) * | 2005-06-17 | 2008-12-04 | パーキンエルマー・インコーポレイテッド | Strengthening device and method of using the same |
| US8896830B2 (en) | 2005-06-17 | 2014-11-25 | Perkinelmer Health Sciences, Inc. | Devices and systems including a boost device |
| US8786394B2 (en) | 2010-05-05 | 2014-07-22 | Perkinelmer Health Sciences, Inc. | Oxidation resistant induction devices |
| US8829386B2 (en) | 2010-05-05 | 2014-09-09 | Perkinelmer Health Sciences, Inc. | Inductive devices and low flow plasmas using them |
| US10096457B2 (en) | 2010-05-05 | 2018-10-09 | Perkinelmer Health Sciences, Inc. | Oxidation resistant induction devices |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3116151B2 (en) | 2000-12-11 |
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