JPH03295449A - Emission spectrochemical analysis - Google Patents
Emission spectrochemical analysisInfo
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- JPH03295449A JPH03295449A JP9815690A JP9815690A JPH03295449A JP H03295449 A JPH03295449 A JP H03295449A JP 9815690 A JP9815690 A JP 9815690A JP 9815690 A JP9815690 A JP 9815690A JP H03295449 A JPH03295449 A JP H03295449A
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- 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
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、導電性試料と電極との間に高電圧を印加し、
この時生じた火花放電のスペクトルから試料中の微量成
分を検出する発光分光分析方法に関する。Detailed Description of the Invention (Industrial Application Field) The present invention applies a high voltage between a conductive sample and an electrode,
This invention relates to an emission spectroscopic analysis method for detecting trace components in a sample from the spectrum of the spark discharge generated at this time.
（従来の技術）
ペースとなる金属、例えば鉄に含まれでいる微量成分、
例えばアルミニウムや炭素の含有量の分析には、発光分
光分析が使用されている６発光分光分析は、真空中や不
活性ガス中に配置された試料と、これに対向させて設け
た針状電極との間にパルス状の高電圧を印加して火花放
電を行なわせ、この時に放射される光を分光して目的成
分に一致するスペクトルを検出し、このスペクトル光の
強度を積算して濃度を測定するようにしたもので、火花
放電を生じる面積が極めて小さいため、試料表面を構成
している成分の微視的な情報を得ることができるという
利点がある。(Conventional technology) Trace elements contained in metals that serve as a paste, such as iron,
For example, emission spectroscopy is used to analyze the content of aluminum and carbon. 6 Emission spectroscopy uses a sample placed in a vacuum or inert gas, and a needle-like electrode placed opposite it. A pulsed high voltage is applied between the Since the area where spark discharge occurs is extremely small, it has the advantage of being able to obtain microscopic information about the components that make up the sample surface.
（発明が解決しようとする課題）
ところで、目的成分のスペクトル強度は、濃度が同じで
あっても、放電位冨によって異なるため、通常ベース金
属のスペクトル強度をモニタし、これの強度によって目
的成分のスペクトル強度を補正した後、積算を行うよう
にしでいる。しかし、７７電位フにピンホールや酸化物
などの介在物か存在すると、その位百に存在するベース
金属か少ないため、上記のような補正を行うと、誤差の
大きなスペクトル強度が積算され、分析結果に大きな誤
差を含むという問題がある。(Problem to be Solved by the Invention) By the way, even if the concentration is the same, the spectral intensity of the target component differs depending on the discharge potential. Therefore, the spectral intensity of the base metal is usually monitored, and the spectral intensity of the target component is determined based on this intensity. After correcting the spectral intensity, the integration is performed. However, if there are inclusions such as pinholes or oxides in the 77 potential band, the base metal present in the 77 potential band is that much smaller, so if the above correction is performed, a spectral intensity with a large error will be integrated, and the analysis will be difficult. The problem is that the results include large errors.
本発明はこのような問題に鑑みてなされたものであって
、その目的とするところは、どンホールや酸化物等の介
在物に関わりなく、精度の高い分析結果を得ることがで
きる新規な発光分光分析方法を提案することにある。The present invention has been made in view of these problems, and its purpose is to provide a novel luminescent method that allows highly accurate analysis results to be obtained regardless of inclusions such as holes and oxides. The objective is to propose a spectroscopic analysis method.
（課題を解決するための手段）
このような問題を解決するために本発明においでは、試
料と針状電極を対向配設して高電圧パルスにより間欠的
に火花放電を起こさせて、目的成分の第１のスペクトル
光の強度と、同時点における介在物の菓２のスペクトル
光の強度を検出する工程と、第２のスペクトル光の強度
が所定強度以上であるか否かを判定し、笥２のスペクト
ル光の強度が所定強度以上である場合には同時点におけ
る第１のスペクトル光の強度を積算データから除外し、
また所定強度以下である場合には同時点における第１の
スペクトル光の強度を積算データとして取込む工程とを
備えるように（）た。(Means for Solving the Problems) In order to solve such problems, in the present invention, a sample and a needle-like electrode are disposed facing each other, and a spark discharge is caused intermittently by high voltage pulses to remove the target component. Detecting the intensity of the first spectral light and the intensity of the spectral light of the inclusion 2 at the same time, determining whether the intensity of the second spectral light is equal to or higher than a predetermined intensity, If the intensity of the second spectrum light is equal to or higher than a predetermined intensity, the intensity of the first spectrum light at the same time is excluded from the integrated data,
Further, if the intensity is below a predetermined intensity, the intensity of the first spectrum light at the same time point is taken in as integrated data.
（作用）
介在物やピンホールが放電箇所になると、酸化物等の介
在物やピンホールを構成している元素のスペクトル光の
強度が大きくなる。したがって同時点て測定された目的
成分のスペクトル光のデータを排除することにより、異
常部の分析データの取込みを防止して、目的成分の濃度
を高い精度で測定することができる。(Function) When an inclusion or pinhole becomes a discharge location, the intensity of the spectral light of the element constituting the inclusion or pinhole, such as an oxide, increases. Therefore, by excluding the data of the spectrum light of the target component measured at the same time, it is possible to prevent the analysis data of the abnormal part from being taken in and measure the concentration of the target component with high accuracy.
（実施例）
そこで、以下に本発明の詳細を実施例に基づいて説明す
る。(Example) Therefore, the details of the present invention will be explained below based on an example.
第１図は、本発明に使用する装フの一実施例を示すもの
であって、図中符号１は、不活性ガスの充填が可能な発
光スタンドで、イグナイタ２から数百ヘルツ程度の繰り
返し周波数の高電圧パルスが印加される試料台３と、針
状電極４が収容され、試料Ｔと針状電極４との間に生じ
た火花放電の光を外部に取り出し可能に構成されでいる
。FIG. 1 shows an embodiment of the equipment used in the present invention, and reference numeral 1 in the figure is a light emitting stand that can be filled with inert gas. A sample stage 3 to which a high-frequency voltage pulse is applied and a needle-like electrode 4 are housed, and the light of the spark discharge generated between the sample T and the needle-like electrode 4 can be taken out to the outside.
５は、分光部で、スリット６を介して発光スタンド１か
ら出射した光を分光する回折格子７と、回折格子７から
の光をスリット８．９．１０を介して受ける複数の光電
子増倍管等の光検出器１１．１２．１３を１冒して構成
されている。各検出器１］、１２．１３には、単一パル
ス積分器１４．１５．１６が接続されており、積分結果
を信号切替器１７によりアナログ−ディジタル変換器１
８に入力してディジタル信号に変換後、メモリに格納す
るようになっている。２０は、レベルメモリで、排除す
べきデータを選別するためのしベルＳを格納して、マイ
クロコンピュータ２１によりデータ処理を行なう際に、
データの取捨選択基準データを提供するものである。Reference numeral 5 denotes a spectroscopic section, which includes a diffraction grating 7 that separates the light emitted from the light emitting stand 1 through a slit 6, and a plurality of photomultiplier tubes that receive the light from the diffraction grating 7 through slits 8, 9, and 10. It is constructed by including one photodetector 11, 12, 13, etc. A single pulse integrator 14, 15, 16 is connected to each detector 1], 12, 13, and the integration result is transferred to an analog-to-digital converter 1 by a signal switch 17.
8, and after converting it into a digital signal, it is stored in memory. Reference numeral 20 denotes a level memory which stores a level S for selecting data to be excluded, and when data is processed by the microcomputer 21.
It provides data selection criteria.
次にこのように構成した装冨の動作を第２図に示したフ
ローチャートに基づいて説明する。Next, the operation of the loading device configured as described above will be explained based on the flowchart shown in FIG.
試料台３に試料Ｔを載冒して装Ｍを作動させると、試料
Ｔと針状電極４との間にイグナイタ２からの高電圧パル
スが印加されて試料Ｔの特定領域との間に放電柱が生じ
、試料の放電領域を構成している各種元素のスペクトル
光が放射される。この光は、回折格子７により分光され
て、検出すべきスペクトルに対応させて配冒されている
光検出器１］、１２．１３に入射する。いうまでもなく
、各光検出器１］、１２．１３からのパルス状出力のピ
ーク高さは、放電箇所における元素の濃度を表すことに
なる。When the sample T is placed on the sample stage 3 and the mount M is activated, a high voltage pulse from the igniter 2 is applied between the sample T and the needle electrode 4, and a discharge column is created between the sample T and a specific area of the sample T. occurs, and spectral light of various elements making up the discharge region of the sample is emitted. This light is separated by the diffraction grating 7 and enters the photodetectors 1, 12 and 13, which are arranged in accordance with the spectrum to be detected. Needless to say, the peak height of the pulsed output from each photodetector 1], 12.13 represents the concentration of the element at the discharge location.
このようにして、針状電極４からの火花柱は、試料１面
での位言を確率的に変えながら高電圧パルスの繰り返し
周波数で火花放電を継続する。このとき、火花柱が試料
面の酸化物等の介在物が存在する領域に移動すると、正
常な箇所に比較して酸素等の酸化物を構成している元素
のスペクトル光の強度が異常に大きくなる。In this way, the spark column from the needle electrode 4 continues to discharge sparks at the repetition frequency of the high voltage pulse while stochastically changing the position on the surface of the sample 1. At this time, when the spark column moves to an area on the sample surface where inclusions such as oxides exist, the intensity of the spectral light of elements constituting oxides such as oxygen becomes abnormally large compared to normal locations. Become.
すなわち、介在物が存在しない領域では、ベースを構成
している成分に目的成分や酸素、窒素がほぼ均等に分散
されでいるが、介在物にあっては殆どが介在物を構成す
る元素で占められているため、正常な領域における成分
分布とは大きく異なリ、少なくとも酸化物を構成してい
る酸素のスペクトル光が異常に強くなり、第３図工に示
したように一パルス積分器］４．１５、］６のデータが
異常に大きな値（図中記号○印を付けたもの）となる。In other words, in a region where there are no inclusions, the target components, oxygen, and nitrogen are almost evenly distributed in the components that make up the base, but when there are inclusions, the elements that make up the inclusions account for most of the elements. As a result, the component distribution is greatly different from the normal region, and at least the spectral light of oxygen constituting the oxide becomes abnormally strong, and as shown in Figure 3, the one-pulse integrator]4. 15, ]6 has an abnormally large value (marked with a symbol ○ in the figure).
このようにして所定時間の分析か終了した段階で、酸素
や窒素等の介在物に含まれている元素のスペクトル光強
度の…現分布を求める。When the analysis for a predetermined period of time is completed in this manner, the current distribution of the spectral light intensity of elements contained in inclusions such as oxygen and nitrogen is determined.
すなわち、このような測定においでは正常な箇所、つま
りとンホールや酸化物等が存在しない箇所であっても、
介在物と同じような成分が含まれているから、介在物に
含まれている元素のスペクトル光は、第４図に示したよ
うに正規分布（Ｉ）に示すようにばらつきを持つことに
はなるが、介在物が放電領域となった場合（こは介在物
を構成している元素の濃度が極めて高いため、介在物の
元素に起因するスペクトル光の強度が大きくなり、正規
分布から外れた領域（ＩＩ）にデータが集中することに
なる。したがって、正規分布から外れた介在物の発光ス
ペクトル光の強度Ｓａ求めておくと、放電箇所が正常領
域か介在物領域かの判定ができることになる。In other words, in such measurements, even if there is a normal location, that is, a location where there are no holes or oxides,
Since it contains the same components as the inclusions, the spectrum light of the elements contained in the inclusions does not have variations as shown in the normal distribution (I) shown in Figure 4. However, if the inclusion becomes a discharge region (in this case, the concentration of the elements that make up the inclusion is extremely high, the intensity of the spectral light caused by the element in the inclusion increases and deviates from the normal distribution). Data will be concentrated in region (II). Therefore, by determining the intensity Sa of the emission spectrum light of inclusions that deviate from the normal distribution, it will be possible to determine whether the discharge location is a normal region or an inclusion region. .
このレベルＳをレベルメモリ２０に格納した段階で、高
電圧パルスを印加して試料Ｔとの間で火花放電を生じさ
せると（ステップ １）、この放電箇所の成分や性状に
対応してスペクトル光が発生する。この発光光は、回折
格子７により目的成分のスペクトル光と、酸素等の介在
物の成分のスペクトル光に分光されて光検出器１１．１
２．１３に入射し、電気信号に変換され、単一パルス積
分器１４．１５．１６により積分される（ステップ ２
）、この積分値は、信号切替器１７によりディジタル信
号に変換されてメモリ１９に格納される。酸素の発光ス
ペクトル光の強度データは、レベルメモリ２０のレベル
Ｓと比較され、酸素のスペクトル光強度が設定レベル以
下の場合には（ステップ ３）、同時点で検出された目
的成分のスペクトル光をベース全屈のスペクトル強度で
補正した後、積分データとして取込み、これを積算する
（ステップ ４）。When this level S is stored in the level memory 20, a high voltage pulse is applied to generate a spark discharge with the sample T (step 1), and a spectral light is generated corresponding to the components and properties of this discharge location. occurs. This emitted light is separated by a diffraction grating 7 into a spectrum light of the target component and a spectrum light of components of inclusions such as oxygen, and is detected by a photodetector 11.1.
2.13, is converted into an electrical signal and integrated by a single pulse integrator 14.15.16 (step 2
), this integral value is converted into a digital signal by the signal switch 17 and stored in the memory 19. The intensity data of the emission spectrum light of oxygen is compared with the level S of the level memory 20, and if the intensity of the oxygen spectrum light is below the set level (step 3), the spectrum light of the target component detected at the same time is compared with the level S of the level memory 20. After correcting with the spectral intensity of the base total refraction, it is imported as integral data and integrated (step 4).
この段階では、所定の放電回数に到達しないので（ステ
ップ ５）、次の放電パルスが印加されて発光が生じる
（ステップ １）。放電柱が介在物に位置したときには
、介在物を構成している酸素や窒素のスペクトル光の強
度がレベルＳを超えるので（ステップ ３）、同時点て
検出された目的成分のスペクトル光の強度データを積算
データから破棄するか、積算データとしての取込むを阻
止する（ステップ ６）。At this stage, since the predetermined number of discharges has not been reached (step 5), the next discharge pulse is applied and light emission occurs (step 1). When the discharge column is located on the inclusion, the intensity of the spectral light of oxygen and nitrogen constituting the inclusion exceeds level S (step 3), so the intensity data of the spectral light of the target component detected at the same time is is discarded from the integrated data or prevented from being included as integrated data (Step 6).
すなわち、酸素のスペクトル強度が設定値Ｓを超える場
合（第３図ＩＩのＯ印を付けたデータ）を排除していく
。That is, cases where the spectral intensity of oxygen exceeds the set value S (data marked with O in FIG. 3 II) are excluded.
以下、このようにして所定回数の放電が終了した時点で
（ステップ ５）、目的成分のスペクトル光の積算値と
検量データを比較することにより目的成分の濃度を知る
ことができる。Thereafter, when a predetermined number of discharges are completed in this manner (step 5), the concentration of the target component can be determined by comparing the integrated value of the spectrum light of the target component with the calibration data.
［実施例］
酸化アルミニウムを介在物として０．０２パーセント含
むとともに、炭素含有量が異なる複数の鉄を試料として
発光分析を行ない、この分析結果から検量線を求めたと
ころ、第５図（Ｉ）に示したようなものが、また従来法
による酸化物からの放電光に起因するデータを除去しな
い場合には、第５図（ＩＩ）に示したような枝Ｊ１１線
が求められた。[Example] Luminescence analysis was performed using multiple iron samples containing 0.02% aluminum oxide as inclusions and different carbon contents, and a calibration curve was determined from the analysis results, as shown in Figure 5 (I). In addition, when the conventional method did not remove data caused by discharge light from oxides, a branch J11 line as shown in FIG. 5(II) was obtained.
これらの検量線（１）、及び（ＩＩ）を用いて炭素含有
量が既知の鉄を試料として発光分析により得たデータか
ら炭素含有ｊｌを求めたところ、従来法による検量線で
は炭素の含有量が大略１５パーセント程度低目に見積ら
れたものが、はぼ一致するようになった。Using these calibration curves (1) and (II), the carbon content jl was determined from the data obtained by luminescence spectrometry using a sample of iron with a known carbon content. What used to be a low estimate of about 15% has now become a close match.
なお、この実施例においては、発光スペクトル強度が変
化する介在物として酸化物１こ例を採って説明したが、
分析に障害となる物質、例えば窟化物や硫化物について
は、これら元素の発光スペクトルを検出し、これらの強
度が設定レベルを超えるようなデータを排除することに
より同様に適用することができる。In addition, in this example, one example of an oxide was used as an inclusion that changes the intensity of the emission spectrum.
The same method can be applied to substances that impede analysis, such as cavestones and sulfides, by detecting the emission spectra of these elements and excluding data whose intensities exceed a set level.
なお、上述の実施例においては介在物が存在する場合に
ついて説明したが、介在物と同じような異常データを発
生するピンホールのデータに対しでも同様（こ排除でき
ることは明かである。Although the above-described embodiments have been described with reference to the case where inclusions exist, it is clear that pinhole data that generates abnormal data similar to inclusions can also be eliminated in the same way.
（発明の効果）
以上説明したように本発明においては、試料と針状電極
を対向配設して高電圧パルスにより間欠的に火花放電を
起こさせて、目的成分の第１のスペクトル光の強度と、
同時点における介在物の第２のスペクトル光の強度を検
出する工程と、第２のスペクトル光の強度が所定強度以
上であるか杏かを判定し、第２のスペクトル光の強度が
所定強度以上である場合には同時点における第１のスペ
クトル光の強度を積算データから除外（八また所定強度
以下である場合には同時点における第１のスペクトル光
の強度を積算データとしで取込む工程とを備えるように
したので、介在物やピンホールによる発光スペクトル強
度のデータを選択的に排除して導電性物質に含まれる特
定成分の濃度をを高い精度で分析することができる。(Effects of the Invention) As explained above, in the present invention, a sample and a needle-like electrode are disposed facing each other, and a spark discharge is caused intermittently by a high voltage pulse, thereby increasing the intensity of the first spectrum light of the target component. and,
Detecting the intensity of the second spectrum light of the inclusion at the same time, determining whether the intensity of the second spectrum light is equal to or higher than a predetermined intensity, and determining whether the intensity of the second spectrum light is equal to or higher than the predetermined intensity. If the intensity of the first spectral light at the same point in time is excluded from the integrated data (or if the intensity is below a predetermined intensity, the intensity of the first spectral light at the same point in time is taken in as integrated data. Since it is equipped with this, the concentration of a specific component contained in a conductive substance can be analyzed with high accuracy by selectively excluding emission spectrum intensity data due to inclusions and pinholes.
第１図は本発明の一実施例を示す装盲の構成図、第２図
は同上装言の動作を示すフローチャート、第３図（ＩＸ
ＩＩ）は、それぞれ同一試料１５ついての酸素のスペク
トル強度と目的成分のスペクトル強度を時間軸に展開し
１．：図、第４図は第３図のデータをスペクトル強度に
対する頻度で集計した頻度図、及び第５図は本発明によ
る測定結果と従来法による測定結果を示す線図である。FIG. 1 is a block diagram of a blind device showing one embodiment of the present invention, FIG. 2 is a flowchart showing the operation of the same device, and FIG. 3 (IX
In II), the spectral intensity of oxygen and the spectral intensity of the target component for the same sample 15 are developed on the time axis, and 1. 4 is a frequency diagram in which the data in FIG. 3 is summarized by frequency with respect to spectral intensity, and FIG. 5 is a diagram showing the measurement results according to the present invention and the measurement results according to the conventional method.
Claims (1)
的に火花放電を起こさせて、目的成分の第１のスペクト
ル光の強度と、同時点における介在物の第２のスペクト
ル光の強度を検出する工程と、第２のスペクトル光の強
度が所定強度以上であるか否かを判定し、第２のスペク
トル光の強度が所定強度以上である場合には同時点にお
ける第１のスペクトル光の強度を積算データから除外し
、また所定強度以下である場合には同時点における第１
のスペクトル光の強度を積算データとして取込む工程と
を備えてなる発光分光分析方法。A sample and a needle-like electrode are arranged facing each other, and a spark discharge is caused intermittently by high voltage pulses, and the intensity of the first spectrum light of the target component and the intensity of the second spectrum light of the inclusion at the same time are determined. and determining whether the intensity of the second spectral light is greater than or equal to a predetermined intensity, and if the intensity of the second spectral light is greater than or equal to the predetermined intensity, the first spectral light at the same time point is detected. If the intensity is below the predetermined intensity, the intensity of
An emission spectroscopic analysis method comprising: a step of capturing the intensity of the spectrum light of the spectrum as integrated data.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9815690A JPH0711486B2 (en) | 1990-04-12 | 1990-04-12 | Emission spectroscopy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9815690A JPH0711486B2 (en) | 1990-04-12 | 1990-04-12 | Emission spectroscopy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03295449A true JPH03295449A (en) | 1991-12-26 |
| JPH0711486B2 JPH0711486B2 (en) | 1995-02-08 |
Family
ID=14212280
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9815690A Expired - Fee Related JPH0711486B2 (en) | 1990-04-12 | 1990-04-12 | Emission spectroscopy |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0711486B2 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999056110A1 (en) * | 1998-04-28 | 1999-11-04 | Kawasaki Steel Corporation | Method of analyzing oxygen and oxide in metallic material |
| JP2010071271A (en) * | 2008-09-22 | 2010-04-02 | Imagineering Inc | Fuel concentration measuring device, fuel concentration measuring method, and method of preparing calibration curve therefor |
| CN101819151A (en) * | 2010-04-22 | 2010-09-01 | 复旦大学 | Active fast acquisition system for atmospheric optical spectrum |
| JP2014215113A (en) * | 2013-04-24 | 2014-11-17 | Ｊｆｅスチール株式会社 | Emission spectral analysis method |
| JP2014215100A (en) * | 2013-04-24 | 2014-11-17 | Ｊｆｅスチール株式会社 | Method for refining carbon steel |
-
1990
- 1990-04-12 JP JP9815690A patent/JPH0711486B2/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999056110A1 (en) * | 1998-04-28 | 1999-11-04 | Kawasaki Steel Corporation | Method of analyzing oxygen and oxide in metallic material |
| US6480274B1 (en) | 1998-04-28 | 2002-11-12 | Kawasaki Steel Corporation | Method of analyzing oxygen and oxide in metallic material |
| JP2010071271A (en) * | 2008-09-22 | 2010-04-02 | Imagineering Inc | Fuel concentration measuring device, fuel concentration measuring method, and method of preparing calibration curve therefor |
| CN101819151A (en) * | 2010-04-22 | 2010-09-01 | 复旦大学 | Active fast acquisition system for atmospheric optical spectrum |
| JP2014215113A (en) * | 2013-04-24 | 2014-11-17 | Ｊｆｅスチール株式会社 | Emission spectral analysis method |
| JP2014215100A (en) * | 2013-04-24 | 2014-11-17 | Ｊｆｅスチール株式会社 | Method for refining carbon steel |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0711486B2 (en) | 1995-02-08 |
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