JPS5837548A - Analysis of ca in ge-ga alloy - Google Patents

Analysis of ca in ge-ga alloy

Info

Publication number
JPS5837548A
JPS5837548A JP13557081A JP13557081A JPS5837548A JP S5837548 A JPS5837548 A JP S5837548A JP 13557081 A JP13557081 A JP 13557081A JP 13557081 A JP13557081 A JP 13557081A JP S5837548 A JPS5837548 A JP S5837548A
Authority
JP
Japan
Prior art keywords
sample
solution
alloy
sample solution
plasma emission
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP13557081A
Other languages
Japanese (ja)
Other versions
JPS622259B2 (en
Inventor
Ikuo Hayashi
郁夫 林
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Meidensha Corp
Meidensha Electric Manufacturing Co Ltd
Original Assignee
Meidensha Corp
Meidensha Electric Manufacturing Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Meidensha Corp, Meidensha Electric Manufacturing Co Ltd filed Critical Meidensha Corp
Priority to JP13557081A priority Critical patent/JPS5837548A/en
Publication of JPS5837548A publication Critical patent/JPS5837548A/en
Publication of JPS622259B2 publication Critical patent/JPS622259B2/ja
Granted legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/73Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches

Landscapes

  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Plasma & Fusion (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (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)
  • Sampling And Sample Adjustment (AREA)

Abstract

PURPOSE:To analyze Ga quantitatively in a sample quickly and highly accurately, by treating a Ge-Ga alloy sample with an aqueous solution of sodium hydroxide, aqueous hydrogen peroxide and hydrochloric acid. CONSTITUTION:After a Ge-Ga alloy sample is pulverized, an acidic sample solution is prepared by adding a NaOH and H2O2 solution to said sample and dissolving by heating and then, boiling and cooling and moreover, adding HCl. The reason why HCl is added is that mixing a trace quantity component from a glass wave is prevented and sensitivity is improved by protecting a glass nebulizer at the time of using a plasma emission spectroscopic anlyzing apparatus and lowering the viscosity of the sample solution. Water is added to the sample solution thus obtained and said solution is radiated by the plasma emission spectroscopic analyzing apparatus and then, a quantitative analysis of Ga is made by measuring 2944Angstrom luminous intensity.

Description

【発明の詳細な説明】 本発明は、Ge(ケルマニウム)−Ga(ガリウム)合
金中のGmの分析方法に関するものである。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for analyzing Gm in a Ge (kermanium)-Ga (gallium) alloy.

半導体素子の製造工程中においては、半導体素子の原料
のひとつでおるG @−Ga合金中の01の正確且つ迅
速な分析が必要とされる。従来、Go−Ga合金中のG
aの分析方法として、一般的な比色法が用いられていた
が、共存成分から01の分離が必要であるため、操作が
煩雑になるうえに分析時間も多くを要していた。
During the manufacturing process of semiconductor devices, accurate and rapid analysis of 01 in G@-Ga alloy, which is one of the raw materials for semiconductor devices, is required. Conventionally, G in Go-Ga alloy
A general colorimetric method has been used as an analysis method for a, but since it is necessary to separate 01 from coexisting components, the operation is complicated and the analysis takes a long time.

ここにおいて、本発明は、G・−01合金中C)Gaの
分析を迅速に、且つ精度臭く定量分析することが可能な
分析方法を提供しようとするものである。
Here, the present invention seeks to provide an analysis method that enables quick and highly accurate quantitative analysis of C) Ga in the G-01 alloy.

本発明に係る分析方法は、微粉砕した試料(G・−Ga
合金)に、水酸化ナトIJウム水溶液及び過酸化水素水
を加え、加温溶解後煮沸して放冷し、さらに塩酸を加え
て酸性とした後、水で希釈して容量−足の試料溶液をつ
(p、この試料溶液中のGaをプラズマ発光分析法によ
って定量分析することを%做としている。また、検量線
用標準溶液には、水酸化ナトIJウム水溶液及び塩酸を
試料溶液と同濃度となるように添加したものを使用する
The analysis method according to the present invention uses a finely ground sample (G・-Ga
Add a sodium hydroxide aqueous solution and a hydrogen peroxide solution to the alloy), heat and dissolve, boil and let cool, then add hydrochloric acid to make it acidic, dilute with water and make a volumetric sample solution. It is assumed that Ga in this sample solution is quantitatively analyzed by plasma emission spectrometry.In addition, the standard solution for the calibration curve contains sodium hydroxide aqueous solution and hydrochloric acid in the same manner as the sample solution. Use the one added to the desired concentration.

第1図は、本発明の分析方法における試料層液作成の一
例を示すフローシート、第2図は検量線用標準溶液作成
の一力を示すフローシートである。
FIG. 1 is a flow sheet showing an example of preparing a sample layer solution in the analysis method of the present invention, and FIG. 2 is a flow sheet showing an example of preparing a standard solution for a calibration curve.

G・−Ga合金を粒状試料のtま溶解するには、従来よ
シ、フッ化水素酸及び硝酸で処通する方法がある。しか
しながら、フッ化水素酸はガラスを溶解する性質がある
ために、ガラス製の実験器具あるいは部品を使用する場
合は、このフッ化水素酸を除去するための何んらかの処
理をする必要があ如、その為の操作が増え、時間も多く
必要とする。それ故に、本発明においては、第1図フロ
ーシートに示すように、微粉砕した試料を秤量後、これ
に5 % NaOH10s/  及び305k H*O
x 3 mを加えて加温溶解し、煮沸、放冷して(1+
1)HCt4gjを加え、酸性の試料溶液をつくる方法
とした。ここで、 HClの添加は、ガラス器具からの
微量成分の混入の防止と、プラズマ発光分析装置の使用
に際し、ガクス製ネブライザーの採暖及び試料溶液の粘
性を低下させて感度を向上させることを目的としている
。最後に水を加えて希釈し、100WLl一定とし、こ
の試料溶液について、2944′kにおけるGaの発光
強度をプラズマ発光分析装置によって測定し、定量分析
を行う。
A conventional method for dissolving the G.--Ga alloy in a granular sample is treatment with hydrofluoric acid and nitric acid. However, since hydrofluoric acid has the property of dissolving glass, it is necessary to perform some kind of treatment to remove this hydrofluoric acid when using glass laboratory equipment or parts. Unfortunately, this requires more operations and more time. Therefore, in the present invention, as shown in the flow sheet of FIG. 1, after weighing a finely ground sample, 5% NaOH 10s/
Add 3 m of
1) HCt4gj was added to create an acidic sample solution. Here, the addition of HCl is intended to prevent trace components from being mixed in from glassware, and to improve sensitivity by reducing the heating of the GAX nebulizer and the viscosity of the sample solution when using the plasma emission spectrometer. There is. Finally, water is added to dilute the sample solution to a constant value of 100 WLl, and the luminescence intensity of Ga at 2944'k is measured using a plasma emission spectrometer for this sample solution to perform quantitative analysis.

また、検量線用標準溶液は、第2図フローシートに示す
ようにGa O〜511fを標準溶液よυ分堆し、これ
に5%NaOH1ON1. (1+ 1 )HCt4I
IJ(試料溶液と同濃度)添加し、ル0を加えて希釈し
100wJ一定としたものを使用する。
The standard solution for the calibration curve was prepared by depositing GaO~511f in υ minutes on the standard solution as shown in the flow sheet of Figure 2, and adding 5% NaOH1ON1. (1+1)HCt4I
Add IJ (same concentration as the sample solution) and dilute it by adding Lu 0 to make it constant at 100 wJ.

第1表は、本発明の分析方法において、溶解条件の検討
結果をフッカ水素酸と硝酸で処理する方法(イ参照)と
比較して示したものである。
Table 1 shows the results of examining the dissolution conditions in the analysis method of the present invention in comparison with the method of treatment with hydrofluoric acid and nitric acid (see A).

第  1  表 いずれの条件においても、試料の溶解が可能であること
がわかった。
It was found that the sample could be dissolved under any of the conditions shown in Table 1.

第2表は、試料溶解に使用した過酸化水素の影響を調査
した結果である。煮沸の操作によって、過酸化水素の影
響がはとんどなくなることがわかる。
Table 2 shows the results of investigating the influence of hydrogen peroxide used in sample dissolution. It can be seen that the effects of hydrogen peroxide are almost completely eliminated by boiling.

第   2   表 第3f1!は、G・共存の影響を調べた実験結果でおる
Table 2 3f1! These are the results of an experiment investigating the influence of G coexistence.

第   6   表 注1) 試料溶液中では11000ppの濃度となる。Table 6 Note 1) The concentration in the sample solution is 11,000 pp.

この実験結果から、発光分析の際、G・1000 pp
mの共存の影響な(’ Gaの分析ができることを確認
し良。
From this experimental result, G・1000 pp
The effect of the coexistence of m (' It is good to confirm that it is possible to analyze Ga.

以上説明したように、本発明に係る分析方法によれば、
G・−Gm合金中の01を迅速に且つ精度良く定量分析
することができる。分析の精度は、合金中のGa含有率
として0.016%である。また、フッ化水素酸を使用
しないので、使用器具の制限もなく、試料溶液の操作が
簡単である等の特長を工ある0 本発明に係る分析方法は、G・−〇m合金の品質管理や
受入れ検査、半導体素子の製造に際してのGm拡散工程
の管理に利用して、極めて有効である。
As explained above, according to the analysis method according to the present invention,
01 in the G.-Gm alloy can be quantitatively analyzed quickly and accurately. The accuracy of the analysis is 0.016% as the Ga content in the alloy. In addition, since hydrofluoric acid is not used, there are no restrictions on the equipment used, and the analysis method according to the present invention has advantages such as easy manipulation of sample solutions. It is extremely effective when used for control of Gm diffusion process during acceptance inspection and manufacturing of semiconductor devices.

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

第1図は本発明の分析方法における試料溶液作成のフロ
ーシート図、第2医紘検量線用標準溶液作成のフローシ
ート図である。 代理人 弁理士 佐 藤 正 年 第1図 100 rrLt −E 第2図 100rr/ニーに
FIG. 1 is a flow sheet diagram for preparing a sample solution in the analysis method of the present invention, and a flow sheet diagram for preparing a standard solution for a second medical calibration curve. Agent Patent Attorney Tadashi Sato Figure 1 100rrLt -E Figure 2 100rr/knee

Claims (1)

【特許請求の範囲】[Claims] (1)  微粉砕した試料に水酸化ナトリウム水溶液及
び過酸化水素水を加え、加温溶解後煮沸して放冷し、さ
らに塩酸を加えて酸性とした後水で希釈して容量−定の
試料溶液をつ〈シ、この試料溶液中のGaをプラズマ発
光分析法によって定量分析をすることを特徴とするG・
−Ga合金中のGaの分析方法。
(1) Add an aqueous sodium hydroxide solution and a hydrogen peroxide solution to the finely ground sample, heat to dissolve, boil and let cool, then add hydrochloric acid to make it acidic, then dilute with water to prepare a sample with a constant volume. A method for preparing a sample solution, which is characterized in that Ga in the sample solution is quantitatively analyzed by plasma emission spectrometry.
-A method for analyzing Ga in a Ga alloy.
JP13557081A 1981-08-31 1981-08-31 Analysis of ca in ge-ga alloy Granted JPS5837548A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP13557081A JPS5837548A (en) 1981-08-31 1981-08-31 Analysis of ca in ge-ga alloy

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP13557081A JPS5837548A (en) 1981-08-31 1981-08-31 Analysis of ca in ge-ga alloy

Publications (2)

Publication Number Publication Date
JPS5837548A true JPS5837548A (en) 1983-03-04
JPS622259B2 JPS622259B2 (en) 1987-01-19

Family

ID=15154897

Family Applications (1)

Application Number Title Priority Date Filing Date
JP13557081A Granted JPS5837548A (en) 1981-08-31 1981-08-31 Analysis of ca in ge-ga alloy

Country Status (1)

Country Link
JP (1) JPS5837548A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60205586A (en) * 1984-03-30 1985-10-17 日本電気株式会社 Driving system for compound discharge display panel
JPS6161043A (en) * 1984-09-03 1986-03-28 Seiko Instr & Electronics Ltd Analyzing device for plating liquid
JP2009085943A (en) * 2007-09-14 2009-04-23 Sumitomo Electric Ind Ltd Icp emission spectral analysis method
CN102778379A (en) * 2012-08-09 2012-11-14 江苏省产品质量监督检验研究院 Method for preparing ferrovanadium alloy fusing sample for X-ray spectrofluorimetry
CN103308509A (en) * 2013-06-07 2013-09-18 武钢集团昆明钢铁股份有限公司 Method for measuring gallium and scandium contents in blast furnace smoke dust

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60205586A (en) * 1984-03-30 1985-10-17 日本電気株式会社 Driving system for compound discharge display panel
JPS6161043A (en) * 1984-09-03 1986-03-28 Seiko Instr & Electronics Ltd Analyzing device for plating liquid
JP2009085943A (en) * 2007-09-14 2009-04-23 Sumitomo Electric Ind Ltd Icp emission spectral analysis method
CN102778379A (en) * 2012-08-09 2012-11-14 江苏省产品质量监督检验研究院 Method for preparing ferrovanadium alloy fusing sample for X-ray spectrofluorimetry
CN103308509A (en) * 2013-06-07 2013-09-18 武钢集团昆明钢铁股份有限公司 Method for measuring gallium and scandium contents in blast furnace smoke dust

Also Published As

Publication number Publication date
JPS622259B2 (en) 1987-01-19

Similar Documents

Publication Publication Date Title
Tothill et al. Inductively coupled plasma mass spectrometry for the determination of platinum in animal tissues and a comparison with atomic absorption spectrometry
CN108732292B (en) Method and device for rapidly detecting sufentanil in blood plasma
JP2001324427A (en) Method for high accuracy boron analysis in iron and steel
JP3768442B2 (en) Analytical sample preparation method and element quantification method
JPS5837548A (en) Analysis of ca in ge-ga alloy
CN106990098A (en) The method of each element content in simultaneous determination aluminium electrolyte
Langmyhr et al. Atomic absorption spectrometric determination of cadmium and lead in dental material by atomization directly from the solid state
KR100923860B1 (en) Method of making portable analysis kit for rapid measurement of HF concentration in mixed solution
Desesa et al. Spectrophotometric and Polarographic Determinations of Soluble Silicate
Chuparina et al. Analytical control of Mn and Se in synthesized compounds, promising plant-derived medicines, by WDXRF and TXRF methods
CN103558069A (en) Chromium-containing gelatin standard substance and preparation method thereof
CN106525552A (en) Serum sample diluent and detection kit
CN109374394B (en) Method for measuring arsenic and mercury contents in plant sample and sample pretreatment method
da Silva et al. A simple digestion procedure for the determination of cadmium, copper, molybdenium and vanadium in plants by graphite furnace atomic absorption spectrometry and mass inductively coupled plasma spectrometry.
CN104897648B (en) Method for measuring gallium in bauxite by inductively coupled plasma emission spectrometry
CN111323280A (en) Pretreatment method for determination of silicon element in fluorine-containing injection packaged by medicinal glass
Filatova et al. Ruthenium and palladium determination in advanced materials based on tin dioxide by mass spectrometry with inductively coupled plasma and total reflection X-ray fluorescence
Derayea et al. Sensitive spectrofluorimetric determination of the prokinetic drug prucalopride succinate based on supramolecular aggregation approach with evaluation of method greenness: application to content uniformity test
JP2002168855A (en) Method for converting inorganic glass sample into solution and quantitative analysis method for inorganic glass sample
Baharom et al. Certification of Ca, Mg, and K in human plasma reference material using isotope dilution inductively coupled plasma mass spectrometry
Hansen et al. Rapid Polarographic Determination of Tetraethyllead in Gasoline
CN114152661B (en) ICP-MS detection method for elemental impurities in conjugated estrogens bulk drug containing high-salt matrix
US2360644A (en) Method of analyzing steel for copper
Motkosky et al. Characterization of trace amounts of aluminium in biological reference materials by electrothermal atomic absorption spectrometry
JPH03218445A (en) Analysis of glass composition