JPS5923381B2 - Glow discharge device for emission spectrometry - Google Patents
Glow discharge device for emission spectrometryInfo
- Publication number
- JPS5923381B2 JPS5923381B2 JP7444778A JP7444778A JPS5923381B2 JP S5923381 B2 JPS5923381 B2 JP S5923381B2 JP 7444778 A JP7444778 A JP 7444778A JP 7444778 A JP7444778 A JP 7444778A JP S5923381 B2 JPS5923381 B2 JP S5923381B2
- Authority
- JP
- Japan
- Prior art keywords
- sample
- glow discharge
- anode
- discharge device
- discharge
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 238000004993 emission spectroscopy Methods 0.000 title description 2
- 238000004611 spectroscopical analysis Methods 0.000 claims description 3
- 239000000523 sample Substances 0.000 description 30
- 239000007789 gas Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 238000000295 emission spectrum Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000011810 insulating material Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000010891 electric arc Methods 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 125000006850 spacer group Chemical group 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000000538 analytical sample Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/67—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using electric arcs or discharges
Landscapes
- Health & Medical Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Description
【発明の詳細な説明】
本発明はアルゴンガスなどによる低気圧雰囲気中でグロ
ー放電を起させ、被分析試料からなる陰極面をスパッタ
させて生じた試料原子の発光スペクトルを測定して分析
する発光分光分析用グロー放電装置に関するものである
。DETAILED DESCRIPTION OF THE INVENTION The present invention is a method for analyzing luminescence by causing a glow discharge in a low-pressure atmosphere such as argon gas, and sputtering a cathode surface consisting of a sample to be analyzed, and measuring the emission spectrum of the sample atoms generated. This invention relates to a glow discharge device for spectroscopic analysis.
通常、発光分光分析用の発光源としては、スパーク放電
、アーク放電などがある。Typically, light sources for emission spectroscopy include spark discharge, arc discharge, and the like.
これらの場合被分析試料を直接電極として、あるいは、
被分析試料が充填されたカップ状のカーボンなどを補助
電極に用いて、試料を熱的に蒸発励起させ、生じた発光
スペクトルを測定する。この場合、ガラスセラミックな
どの不導体物質でも補助電極を使用することにより分析
することができる。これに対して、グロー放電では放電
管を真空にした後、アルゴンなどの希ガスを導入して数
Ｔｏｒｒの低気圧にし、分析試料自体を陰極面として、
対向する陽極電極間でグロー放電を行なわせ、陰極スパ
ッタリング現象を利用して試料物質を蒸発させ、試料成
分による発光スペクトルを得るものである。In these cases, the sample to be analyzed can be used directly as an electrode, or
A cup-shaped carbon filled with the sample to be analyzed is used as an auxiliary electrode to thermally evaporate and excite the sample, and the resulting emission spectrum is measured. In this case, even nonconducting materials such as glass ceramics can be analyzed by using auxiliary electrodes. In contrast, in glow discharge, after the discharge tube is evacuated, a rare gas such as argon is introduced to create a low pressure of several Torr, and the analysis sample itself is used as a cathode surface.
Glow discharge is caused between opposing anode electrodes, and the sample material is evaporated using the cathode sputtering phenomenon to obtain the emission spectrum of the sample components.
この方法は前記熱的方法に比べ、極めて安定な放電が得
られるため定量性が高く、かつ、試料表面層だけの分析
が可能である。しかしながら、分析試料を陰極面とする
ため、ガラスなどの絶縁物の分析は不可能である。本発
明は上記のようなスパーク放電、アーク放電およびグロ
ー放電における問題点を無くし、板状のガラス、セラミ
ックなどの絶縁物質の分析をグロー放電によつて可能と
なしたものである。Compared to the thermal method, this method provides highly stable discharge and is therefore highly quantitative, and allows analysis of only the surface layer of the sample. However, since the analysis sample is the cathode surface, it is impossible to analyze insulators such as glass. The present invention eliminates the problems associated with spark discharge, arc discharge, and glow discharge as described above, and makes it possible to analyze insulating materials such as plate-shaped glass and ceramics using glow discharge.
以下、本発明を実施例に基き図面とともに説明する。第
１図は金属などの導伝性試料を測定する場合のグロー放
電装置の構成図である。Hereinafter, the present invention will be explained based on examples and together with drawings. FIG. 1 is a block diagram of a glow discharge device for measuring conductive samples such as metals.
放電管本体はアノードフランジ１、アノードボテイ２、
カソードフランジ３からなり、アノードとカソード間は
スペーサ６を介して絶縁されておわ、セラミックなどの
絶縁物質からなるボルト１１を用いて本体全部材が固定
されるとともに、被分析試料４および試料おさえ５を用
いて、装置の真空系が保持される。陽極円筒部１はアノ
ード本体内部に装置され、その陽極円筒部Ｔに対向する
位置に被分析試料４が試料おさえ５によりカソードフラ
ンジ３に取りつけられる。The discharge tube body includes an anode flange 1, an anode body 2,
Consisting of a cathode flange 3, the anode and cathode are insulated via a spacer 6, and all parts of the main body are fixed using bolts 11 made of an insulating material such as ceramic. 5 is used to maintain the vacuum system of the apparatus. The anode cylindrical part 1 is installed inside the anode main body, and the sample to be analyzed 4 is attached to the cathode flange 3 by a sample holder 5 at a position facing the anode cylindrical part T.
陽極円筒部１と試料である陰極面４間に数１００ボルト
の電圧を印加して行くと放電が開始し、陽極と試料間に
電流が流れ、分析試料４面がスパッタされる。このよう
にして蒸発励起した分析試料による発光スペクトルをア
ノードフランジ１の先端にある石英製の光窓８を通して
取り出し、分光器により光スペクトルを分光して試料成
分を分析する。アノードボデイ２にはガス導入口９およ
び排気口１０が取りつけられ、放電中、ガスを導入する
とともに放電部での圧力を一定に維持させる。第２図は
不導体物質を試料とした場合の電極部の構成を示す。When a voltage of several hundred volts is applied between the anode cylindrical portion 1 and the cathode surface 4, which is a sample, discharge starts, a current flows between the anode and the sample, and the surface of the analysis sample 4 is sputtered. The emission spectrum of the analytical sample evaporated and excited in this way is taken out through the quartz optical window 8 at the tip of the anode flange 1, and the optical spectrum is separated by a spectrometer to analyze the sample components. A gas inlet 9 and an exhaust port 10 are attached to the anode body 2 to introduce gas and maintain a constant pressure in the discharge section during discharge. FIG. 2 shows the structure of the electrode section when a nonconducting material is used as a sample.
カソードフランジ３の内側試料接触部３ａを円盤状に切
削し、純度が高い金属線、ダえばＮｉ線などによるメツ
シユ状の補助電極１２をフランジ３の切削部に固定させ
る。この補助電極１２ＶＣ対し、被分析試料４を平行に
おき、第１図と同様な方法でカソードフランジ３ＶＣ固
定させて、真空系を維持させる。陽極円筒部７と補助電
極１２間に直流電圧を印加して行くとグロー放電が開始
し、その結果、陰極部であると同時に絶縁物である試料
４面の一部もスパツタされる。このようにして得られた
スペクトルより補助電極１２の成分を除去することによ
り、被分析試料４の組成分析が可能となる。とくに、補
助電極１２の形状をメツシユ状とした場合、試料４面全
体に 二わたり安定な放電が得られる。第３図にはガラ
スを試料としてグロー放電を起させた後の表面形状を測
定した結果を示す。The inner sample contacting part 3a of the cathode flange 3 is cut into a disk shape, and a mesh-shaped auxiliary electrode 12 made of a high-purity metal wire, such as a Ni wire, is fixed to the cut part of the flange 3. The sample to be analyzed 4 is placed parallel to the auxiliary electrode 12VC, and the cathode flange 3VC is fixed in the same manner as shown in FIG. 1 to maintain the vacuum system. When a DC voltage is applied between the anode cylindrical part 7 and the auxiliary electrode 12, a glow discharge starts, and as a result, not only the cathode part but also a part of the surface of the sample 4, which is an insulator, is spattered. By removing the components of the auxiliary electrode 12 from the spectrum obtained in this manner, it becomes possible to analyze the composition of the sample to be analyzed 4. In particular, when the auxiliary electrode 12 is shaped like a mesh, a stable discharge can be obtained over the entire four surfaces of the sample. FIG. 3 shows the results of measuring the surface shape after glow discharge was caused using glass as a sample.
陽極部と陰極部との間隙の大きさ，メツシユのあらさ、
印加電圧などにより放電こん跡の形状が異なるが、スパ
ツタによるこん跡がわかる。以上のように本発明によれ
ば、グロー放電を利用して絶縁物質の分析が可能となり
、応用範囲が拡大する。The size of the gap between the anode part and the cathode part, the roughness of the mesh,
The shape of the discharge marks differs depending on the applied voltage, etc., but the marks caused by spatter can be seen. As described above, according to the present invention, it becomes possible to analyze insulating materials using glow discharge, and the range of applications is expanded.
また、補助電極をメツシユ構造とすることにより、試料
面全体にわたり安定な放電が得られる。さらにまた、不
導体粉末試料の場合でも、試料のみ、あるいは、カーボ
ン粉末などをバインダーとして加圧成型することにより
、上記方法で分析することができる。Furthermore, by forming the auxiliary electrode into a mesh structure, stable discharge can be obtained over the entire sample surface. Furthermore, even in the case of a nonconducting powder sample, it can be analyzed by the above method by press-molding the sample alone or using carbon powder or the like as a binder.
第１図は金属など導電性物質を被分析試料とした場合の
グロー放電装置の概略構成図、第２図は本発明の一実施
例を示す要部構成図、第３図は放電後の試料断面図であ
る。
１・・・・・・アノードフランジ、２・・・・・・アノ
ードボデイ、３・・・・・・カソードフランジ、４・・
・・・・被分析試料、５・・・・・・試料おさえ、６・
・・・・・スペーサ、１・・・・・・陽極円筒部、８・
・・・・・光窓、９・・・・・・ガス導入口、１０・・
・・・・排気口、１１・・・・・・ボルト、１２・・・
・・・補助電極。Figure 1 is a schematic configuration diagram of a glow discharge device when a conductive substance such as metal is used as a sample to be analyzed, Figure 2 is a configuration diagram of main parts showing an embodiment of the present invention, and Figure 3 is a sample after discharge. FIG. 1... Anode flange, 2... Anode body, 3... Cathode flange, 4...
... Sample to be analyzed, 5... Sample holding, 6.
... Spacer, 1 ... Anode cylindrical part, 8.
...Light window, 9...Gas inlet, 10...
...Exhaust port, 11...Bolt, 12...
...Auxiliary electrode.
Claims (1)
記陽極部および前記被測定試料の間の前記陰極部に装着
し得る、透孔を有する補助電極とを備えたことを特徴と
する発光分光分析用グロー放電装置。 ２ 補助電極がメッシュ状からなることを特徴とする特
許請求の範囲第１項に記載の発光分光分析用グロー放電
装置。[Claims] 1. An anode comprising: an anode section, a cathode section on which a sample to be measured is attached, and an auxiliary electrode having a through hole that can be attached to the cathode section between the anode section and the sample to be measured. A glow discharge device for emission spectroscopic analysis, characterized in that: 2. The glow discharge device for emission spectroscopic analysis according to claim 1, wherein the auxiliary electrode has a mesh shape.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7444778A JPS5923381B2 (en) | 1978-06-19 | 1978-06-19 | Glow discharge device for emission spectrometry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7444778A JPS5923381B2 (en) | 1978-06-19 | 1978-06-19 | Glow discharge device for emission spectrometry |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS551543A JPS551543A (en) | 1980-01-08 |
| JPS5923381B2 true JPS5923381B2 (en) | 1984-06-01 |
Family
ID=13547492
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7444778A Expired JPS5923381B2 (en) | 1978-06-19 | 1978-06-19 | Glow discharge device for emission spectrometry |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5923381B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5954840U (en) * | 1982-09-21 | 1984-04-10 | セイコーインスツルメンツ株式会社 | Glow discharge device for emission spectrometry |
| US5028133A (en) * | 1989-12-14 | 1991-07-02 | Regie Nationale Des Usines Renault | Process and device for analysis of nonconductive surfaces |
| JP6765328B2 (en) | 2017-03-15 | 2020-10-07 | 株式会社堀場製作所 | Preparation method, glow discharge emission spectrometry method, instrument, and glow discharge emission spectrometer |
| CN113053720A (en) * | 2021-03-13 | 2021-06-29 | 厦门大学 | Glow discharge excitation light source device |
-
1978
- 1978-06-19 JP JP7444778A patent/JPS5923381B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS551543A (en) | 1980-01-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP2530189B2 (en) | Glow discharge lamp | |
| Marcus et al. | rf-Powered Glow Discharges Elemental Analysis across the Solids Spectrum | |
| US5105123A (en) | Hollow electrode plasma excitation source | |
| US5969349A (en) | Ion mobility spectrometer | |
| Hodoroaba et al. | Emission spectra of copper and argon in an argon glow discharge containing small quantities of hydrogen | |
| US4812040A (en) | Hollow cathode plasma plume | |
| Woo et al. | Analysis of aluminium oxide powder by glow discharge mass spectrometry with low mass resolution | |
| JPS5923381B2 (en) | Glow discharge device for emission spectrometry | |
| WO1990004852A1 (en) | Hollow electrode plasma excitation source | |
| Daughtrey et al. | Critical parameters affecting the hollow cathode ion source | |
| KennetháMarcus | Radiofrequency powered glow discharges for emission and mass spectrometry: operating characteristics, figures of merit and future prospects | |
| EP0448061B1 (en) | Glow discharge atomic emission spectroscopy and apparatus thereof | |
| WO1985004015A1 (en) | Glow discharge tube for analysis | |
| Fröhlich | A hollow-cathode ion source in glow discharge mass spectrometry | |
| RU2487434C1 (en) | Mass-spectral device for quick and direct analysis of samples | |
| JPH086288Y2 (en) | Sample holder for glow discharge emission spectroscopy | |
| JPS6311621B2 (en) | ||
| JP2723455B2 (en) | Glow discharge emission spectrometer | |
| JPH0542608Y2 (en) | ||
| JP2723457B2 (en) | Glow discharge optical emission spectrometer and analysis method | |
| JPH06102180A (en) | Glow discharge spectroscopy analyzer | |
| JPS6041731A (en) | Glow discharge device for emission spectral analysis | |
| JP3284186B2 (en) | Glow discharge emission spectroscopy sample, method for producing the same, and glow discharge emission spectrometer | |
| JP2001004548A (en) | Glow discharge analyzer | |
| JPS637891Y2 (en) |