JPH07225226A - Pre-processing method and device for in-steel intervening material analysis sample - Google Patents
Pre-processing method and device for in-steel intervening material analysis sampleInfo
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- JPH07225226A JPH07225226A JP6018169A JP1816994A JPH07225226A JP H07225226 A JPH07225226 A JP H07225226A JP 6018169 A JP6018169 A JP 6018169A JP 1816994 A JP1816994 A JP 1816994A JP H07225226 A JPH07225226 A JP H07225226A
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は、鋼中介在物の測定技
術に係り、微量に含まれる介在物を濃縮分離することに
よって迅速且つ高精度に分析を行う技術に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a technique for measuring inclusions in steel, and more particularly to a technique for performing a quick and highly accurate analysis by concentrating and separating a small amount of inclusions.
【０００２】[0002]
【従来の技術】鋼中介在物は鋼材の性質に大きな影響を
与え、酸化物系介在物を減少させた極低酸素鋼が品質特
性や加工性を向上させることがよく知られている。この
観点から、鋼の清浄化が進み介在物は減少の一途を辿っ
ているが、これに伴い残存する微量の介在物を精度よく
分析する技術が求められている。2. Description of the Related Art It is well known that inclusions in steel have a great influence on the properties of steel materials, and ultra-low oxygen steel containing reduced oxide inclusions improves quality characteristics and workability. From this viewpoint, the cleaning of steel is progressing and the amount of inclusions is steadily decreasing. Along with this, a technique for accurately analyzing a small amount of inclusions remaining is required.
【０００３】一般に、鋼中の介在物を測定する方法とし
て、鋼試料を溶解して介在物を抽出して測定する方法
と、溶解せずに断面を顕微鏡で観察する方法とがある。
介在物を抽出する方法は、かって鋼材加工時に直接欠陥
の原因となる粒径数十μｍの大型の介在物を抽出するた
めに開発された方法で、介在物が溶解しない条件で鋼試
料を溶解するため溶解に長時間を費やさねばならず、又
鋼の清浄化が進み介在物が微量になる程多量の鋼試料を
必要とする。Generally, as a method of measuring inclusions in steel, there are a method of melting a steel sample and extracting and measuring inclusions, and a method of observing a cross section without melting with a microscope.
The method of extracting inclusions was developed to extract large inclusions with a grain size of several tens of μm that directly cause defects during steel processing, and melts steel samples under conditions where inclusions do not dissolve. Therefore, a long time must be spent for melting, and a large amount of steel sample is required as the cleaning of the steel progresses and the amount of inclusions becomes small.
【０００４】一方、顕微鏡観察では、視野が平面に限定
されるので数の少ない大型介在物を捉える事は困難で、
観察できる粒径２乃至３μｍ以上の粒を観察しこれらの
粒度分布から清浄度を判定する。この方法でも鋼の清浄
化に従い視野数を増やさねばならず、その限界から正確
な判定が困難となっている。On the other hand, in a microscope observation, since the field of view is limited to a plane, it is difficult to capture a large number of large inclusions.
The observable particles having a particle size of 2 to 3 μm or more are observed, and the cleanliness is judged from these particle size distributions. Even with this method, the number of fields of view must be increased as the steel is cleaned, and its limitations make accurate determination difficult.
【０００５】従来、このような状況にあって、鋼試料を
一度溶解して介在物を浮上させ試料上部に濃化させる前
処理方法が提案されている。例えば、特開昭６４−７０
１３４号公報には電子ビームを用いて介在物試料の一部
を溶解して介在物を試料表面に浮上させ、これを顕微鏡
観察により定量する方法が開示されている。又、特開平
５−３２２７２０号公報には、介在物試料を電子ビーム
を用いて溶解し、特定の温度に特定時間試料を保ちこの
間に介在物を浮上させる溶解方法が開示されている。更
に、特開平４−３１０８５４号公報には、介在物試料を
坩堝で溶解し、凝固させる際に底部から上方に向けて一
方向に凝固させることによって、介在物を上面に集積さ
せる方法が開示されている。Under such circumstances, a pretreatment method has heretofore been proposed in which a steel sample is once melted to float inclusions and concentrate on the upper part of the sample. For example, JP-A-64-70
JP-A-134 discloses a method of melting a part of a sample of inclusions by using an electron beam to float the inclusions on the surface of the sample and quantifying the inclusions by microscopic observation. Further, Japanese Patent Application Laid-Open No. 5-322720 discloses a melting method in which a sample of inclusions is melted by using an electron beam, and the sample is kept at a specific temperature for a specific time during which the inclusions are floated. Further, Japanese Patent Laid-Open No. 4-310854 discloses a method of melting inclusions in a crucible and solidifying the inclusions in one direction from the bottom to the top when solidifying the inclusions on the upper surface. ing.
【０００６】[0006]
【発明が解決しようとする課題】しかしながら、これら
の溶解方法によって介在物は浮上するが、浮上効率が不
充分である。大きな介在物は浮上しやすいが、小さな介
在物は浮上し難い。試料を溶解した状態で小さな介在物
が上面に浮上してくるまでには莫大な時間が必要であ
る。浮上を速めるために粘性を下げようとして試料温度
を高めるのにも限界がある。凝固時に一方向に凝固させ
る方法を付け加えても浮上に長時間を要することは変わ
らない。勢い介在物を充分に捕捉し得ないままに分析試
料が作られることが多くなる。However, although the inclusions are floated by these melting methods, the floating efficiency is insufficient. Large inclusions are easy to float, but small inclusions are hard to float. It takes an enormous amount of time for small inclusions to rise to the upper surface in the state where the sample is dissolved. There is also a limit to increasing the sample temperature in order to reduce the viscosity in order to accelerate the levitation. Even if a method of solidifying in one direction at the time of solidification is added, it does not change that it takes a long time to float. Often, analytical samples are made without sufficient capture of momentum inclusions.
【０００７】又、電子ビームのように高密度のエネルギ
ーを投入する溶解法では、投入エネルギーが小さくても
局所的に高温部を生じ、試料組成によっては介在物が溶
解してしまうことがある。例えば、高温になり過ぎた局
所では鋼中の炭素が酸化物系介在物を還元してしまうこ
とや、低融点介在物が溶解してしまうことがある。Further, in the melting method in which a high density of energy such as an electron beam is applied, a high temperature portion is locally generated even if the applied energy is small, and inclusions may be dissolved depending on the sample composition. For example, carbon in the steel may reduce the oxide-based inclusions or the low-melting inclusions may be melted locally at an excessively high temperature.
【０００８】このような点から、従来の前処理法では介
在物の測定に際し母試料中の介在物が充分に捕捉され
ず、介在物分析の精度が不充分であるとの問題があっ
た。この発明は、このような問題を解決するために行わ
れたもので、鋼中の介在物を損なうことなくこれらを充
分な精度で捕捉する前処理技術の提供を目的とする。From such a point, the conventional pretreatment method has a problem that the inclusions in the mother sample are not sufficiently captured during the measurement of the inclusions and the accuracy of the inclusion analysis is insufficient. The present invention has been made in order to solve such a problem, and an object thereof is to provide a pretreatment technique for capturing inclusions in steel with sufficient accuracy without damaging them.
【０００９】[0009]
【課題を解決するための手段】この目的を達成するため
の手段は、鋼中介在物の分析に先立って、介在物試料を
縦長の坩堝を用いて局所加熱を避けて不活性ガス雰囲気
で溶解し、この溶鋼に不活性ガスを所定の時間吹き込み
続けた後、溶鋼を下部から上部に向かって順次冷却し、
下部の溶鋼が凝固し始めた時点で不活性ガスの吹き込み
を中止するとともに雰囲気を減圧し鋼中ガスを脱気しな
がら下部から上部に向かって順に凝固させる鋼中介在物
分析用試料の前処理方法と、その一態様である縦長の坩
堝が逆円錐台状である前記の鋼中介在物分析用試料の前
処理方法、及びこれらの前処理を実用するのに適した坩
堝中の鋼材を溶解する加熱炉であって、個別に出力を調
整できる複数本の高周波コイルを備え、排気口と不活性
ガスの導入孔を備えるとともに坩堝設置後は炉内を少な
くとも十分の一気圧まで減圧できる気密性を有する鋼中
介在物分析用試料の前処理装置である。[Means for Solving the Problems] The means for achieving this object is to melt inclusion samples in an inert gas atmosphere prior to analysis of inclusions in steel, avoiding local heating using a vertically long crucible. Then, after continuing to blow an inert gas into the molten steel for a predetermined time, the molten steel is sequentially cooled from the lower part to the upper part,
When the molten steel in the lower part begins to solidify, the blowing of the inert gas is stopped, and the atmosphere is decompressed and the gas in the steel is degassed. Method, a pretreatment method for the sample for inclusion inclusion analysis in steel, wherein the vertically long crucible, which is one aspect thereof, has an inverted truncated cone shape, and a steel material in the crucible suitable for practicing these pretreatments is melted A heating furnace equipped with a plurality of high-frequency coils that can individually adjust the output, an exhaust port and an inert gas introduction hole, and at the same time, the furnace can be decompressed to at least 1/10 atmospheric pressure after the crucible is installed. Is a pretreatment device for a sample for analyzing inclusions in steel having
【００１０】[0010]
【作用】介在物試料の溶解は不活性ガス雰囲気で行い、
溶解時に雰囲気との反応による介在物の消滅或いは生成
を防ぐ。不活性ガスとしては、アルゴン、窒素、ヘリウ
ム等が用いられるが、介在物として窒化物を問題にする
場合は、窒素ガスは避けた方がよい。[Function] The inclusion sample is dissolved in an inert gas atmosphere,
Prevents disappearance or formation of inclusions due to reaction with the atmosphere during melting. Argon, nitrogen, helium, etc. are used as the inert gas, but nitrogen gas should be avoided when nitride is a problem as an inclusion.
【００１１】試料を縦長の坩堝で溶解するが、試料凝固
後は介在物が上方に濃化されているので、縦長の試料の
方が横長の試料よりもこの濃化部を適切に分離すること
ができる。The sample is melted in the vertically long crucible, but since the inclusions are concentrated upward after the sample is solidified, the vertically long sample should be separated from the thickened portion more appropriately than the horizontally long sample. You can
【００１２】局所加熱を避けて加熱するのは、前述した
局所的に過度に高温になることを防ぐためであって、例
えば、高周波加熱炉や放射加熱炉等を用いて加熱するこ
とができる。高周波加熱炉や電気抵抗体や赤外線ランプ
による放射加熱炉は、坩堝の上方と下方との温度制御が
容易で取扱い易い。The purpose of avoiding local heating is to prevent the above-mentioned excessively high temperature locally, and heating can be performed using, for example, a high frequency heating furnace or a radiant heating furnace. In a high-frequency heating furnace, a radiant heating furnace using an electric resistor or an infrared lamp, the temperature control above and below the crucible is easy and easy to handle.
【００１３】坩堝は、炉の中央部に設置されるが、底に
ランスを設け炉の不活性ガス導入孔から突き出させてお
くとよい。介在物試料を溶解しながら、この溶鋼に不活
性ガスを吹き込む。この吹き込みにより溶鋼中に上昇ガ
ス流が生じ介在物の浮上を促進する。上昇ガス流の効果
歯大きく、この段階で数十分のうちに殆どの介在物は浮
上する。The crucible is installed in the central part of the furnace, but it is preferable to provide a lance on the bottom so that the crucible protrudes from the inert gas introduction hole of the furnace. An inert gas is blown into this molten steel while melting the inclusion sample. This blowing causes a rising gas flow in the molten steel to promote the floating of inclusions. The effect of rising gas flow is large, and most of the inclusions float within tens of minutes at this stage.
【００１４】その後、溶鋼を下部から上部に向かって一
方向に順次冷却するが、この冷却は下部の方から加熱を
止めていけばよい。この場合、高周波加熱では溶鋼のみ
が加熱されるので、高周波コイルを複数に分割し各コイ
ルの出力を個別に調整できる炉ではコイルが位置する箇
所の溶鋼が直ちに冷却し始めるので、冷却制御が特に容
易である。Thereafter, the molten steel is sequentially cooled in one direction from the lower part to the upper part, but this cooling may be carried out by stopping the heating from the lower part. In this case, since only the molten steel is heated in the high frequency heating, in a furnace in which the high frequency coil is divided into multiple parts and the output of each coil can be adjusted individually, the molten steel at the location of the coil immediately begins to cool, so cooling control is particularly important. It's easy.
【００１５】そして、下部の溶鋼が凝固し始めた時点で
不活性ガスの吹き込みを中止するとともに雰囲気を減圧
する。減圧することによって残留していたガスが脱気さ
れるとともに僅かに残っていた小さな介在物も浮上す
る。この間、下部から順に凝固が進むので、下部に残っ
ていた介在物は未凝固状態の上方へと押し上げられ、凝
固が終了したときには全ての介在物が最上部に押しやら
れている。Then, when the molten steel at the bottom starts to solidify, the blowing of the inert gas is stopped and the atmosphere is depressurized. By reducing the pressure, the remaining gas is degassed, and the small remaining small inclusions also float up. During this time, solidification proceeds from the lower part in order, so that the inclusions remaining in the lower part are pushed upward to the unsolidified state, and when the solidification is completed, all the inclusions are pushed to the uppermost part.
【００１６】この介在物が濃化された上部は試料全体の
１〜５％で、この部分を切り離すと介在物を分離するこ
とができる。分離された上部だけを溶解すれば、介在物
試料が大重量であっても、溶解量は少なくて済み短時間
で全介在物を抽出することができる。溶解する坩堝は、
円筒状でもよいが逆円錐台状であると、減圧時に脱気し
易い利点がある。The upper part where the inclusions are concentrated is 1 to 5% of the whole sample, and the inclusions can be separated by separating this part. If only the separated upper part is dissolved, even if the inclusion sample has a large weight, the amount of dissolution is small and all inclusions can be extracted in a short time. The melting crucible is
A cylindrical shape may be used, but an inverted frustoconical shape has an advantage that degassing is easily performed during depressurization.
【００１７】[0017]
【実施例】鋼種の異なるＡ，Ｂ，Ｃ材の試料各１０kgに
ついて、前処理を施し凝固試料の上部１％乃至５％を分
析し介在物量を調べた。前処理では、この発明による実
施例の他に、比較例として溶鋼下部からの一方向冷却を
行わず無方向に溶鋼全体を冷却した例と一方向ではある
が定圧下で冷却した例、及び従来の方法による従来例に
ついても行った。これらの前処理法を、１０kg全量を溶
解した場合に捕捉された介在物量を基準量とし、各々の
前処理後測定した介在物量を基準量と比較し、各々の方
法で捕捉されなかった率を求めて評価した。介在物量は
粒度別に、＜５μｍ、５〜１０μｍ及び＞１０μｍの三
つの範囲で測定した。基準量は、＜５μｍではＡ：３５
ppm 、Ｂ：１１ppm 、Ｃ：１９ppm 、５〜１０μｍでは
Ａ：１０ppm 、Ｂ：２ppm 、Ｃ：４ppm 、＞１０μｍで
はＡ：１０ppm 、Ｂ：２ppm 、Ｃ：４ppm であった。EXAMPLE For each 10 kg of A, B, and C materials having different steel types, pretreatment was performed and the upper 1% to 5% of the solidified sample was analyzed to examine the amount of inclusions. In the pretreatment, in addition to the example according to the present invention, as a comparative example, an example of cooling the entire molten steel in one direction without performing unidirectional cooling from the molten steel lower part and an example of cooling under constant pressure in one direction, and a conventional method The conventional example by the above method was also performed. In these pretreatment methods, the amount of inclusions captured when the total amount of 10 kg was dissolved was used as a reference amount, and the amount of inclusions measured after each pretreatment was compared with the reference amount. Seek and evaluate. The amount of inclusions was measured in three ranges of <5 μm, 5 to 10 μm and> 10 μm depending on the particle size. The standard amount is A: 35 when <5 μm.
ppm, B: 11 ppm, C: 19 ppm, A: 10 ppm, B: 2 ppm, C: 4 ppm at 5 to 10 μm, and A: 10 ppm, B: 2 ppm, C: 4 ppm at> 10 μm.
【００１８】溶解に用いた装置及び坩堝の概要を図１に
示す。炉１には溶鋼を加熱するための高周波コイル２を
設置し、上部に排気口３を設けて真空ポンプ４に接続し
た。高周波コイル２は三分割し溶鋼の下部、中部、上部
と分けて加熱制御が出来るようにした。又、下部には排
気ガス導入孔５を設け、坩堝６の底に設けられたランス
７が炉の壁を突き抜けられるようにした。ランス７と排
気ガス導入孔５との間には銅リング８を使用し気密が保
てるようにした。The outline of the apparatus and crucible used for melting is shown in FIG. A high frequency coil 2 for heating molten steel was installed in a furnace 1, an exhaust port 3 was provided in the upper part, and a vacuum pump 4 was connected. The high frequency coil 2 is divided into three parts, and the heating control can be performed by dividing the molten steel into the lower part, the middle part and the upper part. Further, an exhaust gas introduction hole 5 was provided in the lower part so that a lance 7 provided at the bottom of the crucible 6 could penetrate the wall of the furnace. A copper ring 8 is used between the lance 7 and the exhaust gas introduction hole 5 so that airtightness can be maintained.
【００１９】坩堝には、鋼種Ａでは窒化ホウ素製を使用
し、鋼Ｂ及びＣでは硼化チタン製のものを使用した。不
活性ガスには鋼種Ａでは窒素ガスを、鋼種Ｂ及びＣでは
アルゴンガスを各々使用した。その他の前処理条件及び
調査結果を表１に示す。For the crucible, boron nitride was used for steel type A and titanium boride was used for steels B and C. As the inert gas, nitrogen gas was used for steel type A, and argon gas was used for steel types B and C, respectively. Table 1 shows other pretreatment conditions and survey results.
【００２０】[0020]
【表１】 [Table 1]
【００２１】この発明の実施例では、５μｍ以上の介在
物は全て捕捉され、５μｍ未満の小さな介在物でも捕捉
されなかった率は５％以下であった。これに対して、比
較例では一律に冷却した試験No. ４、５、冷却時に減圧
しなかった試験No. ６共に３０％前後の捕捉漏れがあっ
た。又、溶解中のガス吹きが行われない従来例では捕捉
漏れは３６％（試験No. ８）から６５％（試験No. ７）
に達した。In the examples of the present invention, all the inclusions having a size of 5 μm or more were captured, and the rate of not capturing even the inclusions having a size of less than 5 μm was 5% or less. On the other hand, in the comparative example, there was trap leakage of about 30% in both test Nos. 4 and 5 uniformly cooled and test No. 6 not depressurized during cooling. Also, in the conventional example in which gas blowing during melting is not performed, trapping leakage is 36% (test No. 8) to 65% (test No. 7).
Reached
【００２２】[0022]
【発明の効果】以上述べてきたように、この発明によれ
ば、大重量の介在物試料中の介在物を、ガス吹き及び脱
ガス気流に巻き込まれての浮上と一方向の凝固との効果
によって試料の上部１〜５％に全て濃化させてしまう。
このため、大重量の介在物試料でもその上部のみを溶解
して分析すれば、介在物の全てを捕捉することができ、
短時間で高精度の分析ができるようになった。このよう
に、鋼材介在物の迅速で正確な評価を可能としたこの発
明は、鋼材の品質向上に大きな効果をもたらす。As described above, according to the present invention, the effect of floating and unidirectional solidification of inclusions in a large amount of inclusions in a gas blown and degassed gas stream is obtained. Causes the sample to be fully concentrated in the upper 1% to 5%.
Therefore, even in the case of a large-weight inclusion sample, if only the upper part is dissolved and analyzed, all the inclusions can be captured,
High-precision analysis has become possible in a short time. As described above, the present invention, which enables quick and accurate evaluation of steel inclusions, has a great effect on improving the quality of steel.
【図１】発明の一実施例に用いた坩堝と前処理装置の概
要を示す概念図である。FIG. 1 is a conceptual diagram showing an outline of a crucible and a pretreatment device used in an embodiment of the invention.
１ 炉 ２ 高周波コイル ３ 排気口 ４ 真空ポンプ ５ 排気ガス導入孔 ６ 坩堝 ７ ランス ８ 銅リング 1 Furnace 2 High frequency coil 3 Exhaust port 4 Vacuum pump 5 Exhaust gas introduction hole 6 Crucible 7 Lance 8 Copper ring
フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｇ０１Ｎ 31/00 Ｙ Continuation of the front page (51) Int.Cl. 6 Identification code Office reference number FI Technical display location G01N 31/00 Y
Claims (3)
料を縦長の坩堝を用い局所加熱を避けて不活性ガス雰囲
中で溶解し、この溶鋼に不活性ガスを所定の時間吹き込
み続けた後、溶鋼を下部から上部に向かって順次冷却
し、下部の溶鋼が凝固し始めた時点で不活性ガスの吹き
込みを中止するとともに雰囲気を減圧し、鋼中ガスを脱
気しながらこの溶鋼を下部から上部に向かって順に凝固
させることを特徴とする鋼中介在物分析用試料の前処理
方法。1. Prior to the analysis of inclusions in steel, a sample of inclusions is melted in an inert gas atmosphere while avoiding local heating by using a vertically long crucible, and an inert gas is blown into the molten steel for a predetermined time. After that, the molten steel is sequentially cooled from the lower part to the upper part, and when the molten steel in the lower part begins to solidify, the blowing of the inert gas is stopped and the atmosphere is depressurized, while degassing the gas in the steel. A method for pretreating a sample for analyzing inclusions in steel, which comprises solidifying in sequence from the bottom to the top.
１記載の鋼中介在物分析用試料の前処理方法。2. The pretreatment method for a sample for analyzing inclusions in steel according to claim 1, wherein the vertically long crucible has an inverted truncated cone shape.
て、個別に出力を調整できる複数本の高周波コイルを備
え、排気口と不活性ガスの導入孔を備えるとともに坩堝
設置後は炉内を少なくとも十分の一気圧まで減圧できる
気密性を有することを特徴とする鋼中介在物分析用試料
の前処理装置3. A heating furnace for melting a steel material in a crucible, comprising a plurality of high-frequency coils capable of individually adjusting the output, having an exhaust port and an introduction hole for an inert gas, and after installing the crucible, the inside of the furnace. For pretreatment of sample for inclusions in steel characterized by having airtightness capable of decompressing at least 1/10 atmospheric pressure
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6018169A JPH07225226A (en) | 1994-02-15 | 1994-02-15 | Pre-processing method and device for in-steel intervening material analysis sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6018169A JPH07225226A (en) | 1994-02-15 | 1994-02-15 | Pre-processing method and device for in-steel intervening material analysis sample |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH07225226A true JPH07225226A (en) | 1995-08-22 |
Family
ID=11964115
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6018169A Withdrawn JPH07225226A (en) | 1994-02-15 | 1994-02-15 | Pre-processing method and device for in-steel intervening material analysis sample |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07225226A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103123329A (en) * | 2012-12-31 | 2013-05-29 | 上海大学 | Rapid detection method and rapid detection device of non-metallic inclusions in metal |
| CN111226291A (en) * | 2018-09-25 | 2020-06-02 | 原子能设计股份公司 | Nuclear reactor core melting positioning device |
-
1994
- 1994-02-15 JP JP6018169A patent/JPH07225226A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103123329A (en) * | 2012-12-31 | 2013-05-29 | 上海大学 | Rapid detection method and rapid detection device of non-metallic inclusions in metal |
| CN111226291A (en) * | 2018-09-25 | 2020-06-02 | 原子能设计股份公司 | Nuclear reactor core melting positioning device |
| CN111226291B (en) * | 2018-09-25 | 2023-08-11 | 原子能设计股份公司 | Nuclear reactor core melting positioning device |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A300 | Withdrawal of application because of no request for examination |
Free format text: JAPANESE INTERMEDIATE CODE: A300 Effective date: 20010508 |