JPH0339631B2 - - Google Patents
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- JPH0339631B2 JPH0339631B2 JP59263002A JP26300284A JPH0339631B2 JP H0339631 B2 JPH0339631 B2 JP H0339631B2 JP 59263002 A JP59263002 A JP 59263002A JP 26300284 A JP26300284 A JP 26300284A JP H0339631 B2 JPH0339631 B2 JP H0339631B2
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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
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/718—Laser microanalysis, i.e. with formation of sample plasma
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- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
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- General Health & Medical Sciences (AREA)
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Description
〔産業上の利用分野〕
本発明は、溶銑、溶鋼、スラグ、ガラス、半導
体などをはじめとする各種の流動状態にある金属
または絶縁物の多成分元素を、これらに接触する
ことなくレーザーにより連続的にオンライン分析
する装置に関する。
〔従来の技術〕
溶融物の分析には従来
試料をるつぼ等の閉容器内に静置して分析す
る。
試料を溶融物の流れから採取して分析する。
励起源や測定系の一部を溶融物の流れの中に
浸漬して分析する。
のいずれか、もしくはこれらを組み合わせた方法
が用いられてきた。
しかし、上記のるつぼ等の閉容器内に試料を
静置して分析する方法は製造工程の分析に直ちに
適用することが困難であり、また上記の試料
の流れから取り出したり、溶融物の流れ中に分析
具を浸漬する方法は被測定物の流れを乱したり、
汚染するという短所を有していた。
このような短所を改善するためにレーザー発光
分光分析を溶融物に適用した例として例えば、
１） 特開昭52−72285、
２） 実用新案昭51−6147、
３） ルンゲ、ボンフイリイオ、ブライアン：ス
ペクトロキム、アクタ22（E.F.Runge，S.
Bonfiglio and E.R.Bryan：Spectrochim，
Acta，22（1965）1678、）
４） 尾崎、高橋、岩井、郡司、須藤；鉄と鋼68
（1982）863）
があるが、これらはいずれも試料をるつぼ等の閉
容器内に静置して行うレーザー分光分析方法であ
る。従つて、
(1) 被測定物表面の上下動
(2) 被測定物中および表面上の不純物
(3) 被測定物からの熱放射
等の問題の生じる製造工程における分析に関する
ものではない。
本発明者らは上記問題点(1)を解決し、流動状態
にある金属や絶縁物に接触することなくその成分
分析をオンラインで実施する方法として、流動状
態の被測定溶融物に大出力パルスレーザー光を照
射し、その時得られる発光スペクトルを分光する
ことにより、被測定物に励起源、測定系を接触さ
せずに、連続的にオンライン分析する方法を提案
した。（特願昭58−108456）
〔発明が解決しようとする問題点〕
上記提案は、流動状態にある金属や絶縁物をオ
ンライン分析することができるので極めて好まし
いが、上記(2)、(3)の問題が依然としてあり、
ａ） 被測定物の表面に浮遊している不純物また
は被測定物中に溶け込んでいる不純物にレーザ
ー光が照射されたときに測定精度が著しく害さ
れ、ータのばらつきを生じること、
ｂ） 装置的に被測定物からの放射熱によつてレ
ーザー発振器光軸のずれまたは光導入系、分光
器等の光学系のずれが生じ、分析値が不正確と
なること、
ｃ） ランス先端部は時々とりかえを要するが、
全体を取替えると取付部の取付精度等の問題か
ら光軸系の再調整を要するので先端部のみを取
替え可能な耐熱構造とする工夫がある。
本発明はこのような問題を解決し、上記オンラ
イン分析方法を好適に実施することのできる連続
測定装置を提供することを目的とする。
〔問題点を解決するための手段〕
本発明は、溶融状態の金属、絶縁物の成分分析
装置において、
１） 被測定物の連続流路を設けること、
２） この流路内の被測定物までの距離ｌとレー
ザー光の集光レンズの焦点距離ｆが被測定物の
表面の変動範囲内で常に
0.95f≦ｌ≦1.05f
の関係を有するレーザー発光分光分析装置を配
設すること、
３） 被測定物中の不純物等にレーザー光が照射
された時の信号を除外して測定値を平均化する
手段を揃えること、すなわち、被測定物のレー
ザー光照射信号測定値６〜10個のデータを平均
した後、該平均値の95〜105％内の測定値を再
平均する手段を備えること、
４） 装置本体の少なくとも被測定物からの放射
熱のある部分に熱反射率の高い材質からなる反
射板あるいは耐火物を取り付けたこと、
５） 少なくともランス先端部が被測定物からの
温度に耐える取替可能な耐熱材からなるランス
を装着したこと、
６） ランス中に不活性ガス吹込口を設けたこ
と、
を特徴とする。
以下、本発明を詳細に説明する。
まずレーザー発光分光分析手法を実際に現場分
析に適用する装置においては、被測定物の上下動
の影響が最大の問題となる。本発明者らはこの問
題点を解明するために第２図に示す装置を用い
て、その調査を行つた。レーザーとしては、パル
ス幅15nsec、出力2J、波長1.06μmの赤外線パル
スレーザーを用いた。
第２図について説明するとレーザー発振器１よ
り発生したレーザー光は、プリズム２で下方に曲
げられ、集光レンズ３により被測定物４の表面に
集光されるようになつている。被測定物４として
ここではFe−0.3％Mn合金を用い、この合金をタ
ンマン炉５により溶解した。この時被測定物４の
表面に酸化膜が生成される事が予想されたので、
アルゴンガス導入部６よりアルゴンガスを吹き込
み、アルゴンガス排出部７より系外に放出させ、
酸化膜の生成を抑制した。レーザー光照射によつ
て生じた光は凹面鏡８、平面鏡９ａ，９ｂからな
る光導入系により分光器１０に導いた。分光器１
０の内部では、通常の方法により波長分離し、
271.4nmのFeスペクトル、293.3nmのMnスペク
トルの強度を二つの光検出器１１により測定し
た。被測定物４とレーザー分光器光学系の距離を
変えるためにタンマン炉５をリフト１２の上に載
せ、溶解炉全体を上下させた。この際アルゴンガ
スの流れが乱れぬよう、光導入系とタンマン炉５
の間にすり合せ１３を設けた。レーザーの集光レ
ンズ３としてはそれぞれ焦点距離20、50、100、
150、200cmの５種類を取り替えて用いた。なお集
光レンズ３を交換した場合には、被測定物表面が
その焦点にある時に励起発光した光が分光器入口
スリツト１４に結像するように凹面鏡８の半径を
選び、平面鏡９ａ，９ｂの角度を調整した。
第３図に焦点距離100cmの集光レンズを用いた
時の被測定物４の上下動によるFe、Mnスペクト
ル強度およびその比の変化を示す。被測定物表面
が集光レンズ３の焦点からずれるに従つて、スペ
クトル強度が次第に減少しているが、分析に使用
するスペクトル強度の比は、被測定物表面が集光
レンズ３の焦点より上下５cmほどずれても変化し
ない。同様の測定を集光レンズ３を換えて行つた
結果をまとめると第４図のようになり、集光レン
ズ３と被測定物表面の間の距離ｌが、集光レンズ
３の焦点距離ｆに対し、
0.95f≦ｌ≦1.05f ……(1)
であれば、スペクトル強度比は不変であり、被測
定物の上下動にかかわらず、安定した分析値が得
られることが判明した。
次に被測定物４として絶縁物系のSiO2・Al2O3
を用い、Si（288.2nm）、Al（309.3nm）の線スペク
トルについて、第２図と同様の測定を行つた。そ
の結果を第５図に示す。この場合にも、被測定物
表面が集光レンズ３の焦点より５cmずれても、ス
ペクトル強度比はほぼ一定となつている。さら
に、集光レンズ３を換えて行つた測定結果も第４
図とほぼ同様であり、上記(1)式が満たされれば、
被測定物表面の上下動の影響を受けないことが明
らかとなつた。
実際の製造工程分析で起こる第２番目の問題と
して被測定物中および表面上の不純物の影響があ
る。被測定物表面上に浮いている軽量の不純物
は、ランスからアルゴンあるいは窒素等のガスを
吹きつければ除去できるが、被測定物中に入つた
不純物にレーザーが照射された場合に問題とな
り、分析値が正確に得られない。そこで本発明で
は、被測定物中の不純物にレーザーが照射され異
常値が得られた場合その値を除外して６〜10回の
値の平均値を求める手段として論理回路１９を備
える。
論理回路１９は具体的には、次の演算を行う。
被測定物のレーザー光照射信号を平均し、次い
でこの平均値の95％未満の測定データおよび105
％を越える測定データを除外し、95〜105％内の
測定値を再平均することにより異常値を除外す
る。この演算は論理回路１９内にて行い、その結
果は表示装置２０に表示される。この手法によつ
て同時にレーザーの発振不良、ばらつき、被測定
物の励起発光不良による異常値も除外することが
可能であり、分析精度が向上する
第７図に論理回路１９のフローチヤートを示
す。装置が始動されると、論理回路１９は、レー
ザー発振器にレーザーの発振を指示するととも
に、光電子増倍管１８により電気信号に変換され
た各元素のスペクトル強度を読み取り、これをデ
ータとして記憶する。このレーザー発振データの
読み込み、およびデータの記憶を10回繰り返し、
この10回のデータの平均値を計算する。
次に、この10回のデータのうち、平均値±５
％以内のデータで再度平均値ａを求める。この
Ｘａと予め標準試料により求めておいた検量線に
より、元素濃度の算出を行い、この結果を表示装
置１０に転送し、表示する。これにより、異常値
を除外した精度の高い測定値を得ることができ
る。
次に問題とされる被測定物からの放射熱である
が、これは、レーザー発振器光軸のずれまたは光
導入系・分光器の光学系のズレ等が生じ、分析値
が不正確になる。そこで本発明では、装置の前部
および下部の被測定物に対する面に熱反射率の高
いジユラルミン製の反射板２１または耐熱物等の
熱遮蔽板を取り付け、被測定物からの反射熱を遮
断している。また、装置本体と反射板２１の間に
水、あるいはガス等を流して冷却してもよい。
光導入系ランスは、被測定物の飛散による付着
等があり、ある期間で交換が必要である。ランス
全体を耐火物製とすると、その接合部が弱く、装
置本体からランスを脱着するたびに再現性がない
ために、光軸系の再調整が必要となる。そこで本
発明は、ランス本体はステンレスまたはジユラル
ミン製等の固い材質にして、先端部のみを耐火物
２２にして、本体との結合の再現性を良くするこ
ととした。またランス内に不活性ガスを導入する
吹込口１７を設け、被測定物表面を清浄化し前記
障害を防止するようにした。
〔実施例〕
本発明の装置は被測定物表面の上下動の範囲の
変動幅の10倍以上の長さの焦点距離をもつ集光レ
ンズを用いる。そうすれば上記(1)式が常に成立す
るようになる。次いでこの焦点距離から放出され
た光が分光器入口スリツトに結像するように光導
入系を調整する。レーザーとしては赤外線パルス
レーザーが適しているが、可視光の得られるルビ
ーレーザーも使用することができる。レーザー照
射によつて放出された光の分光、特定スペクトル
強度の測定装置は、公知の装置を用いる。
被測定物表面に酸化膜等の別の物質が存在する
時は、アルゴンあるいは窒素等のガスを吹きつけ
除去するか、被測定物と分離する適当な障害物等
を設けるが、レーザー光導入系がガス、粉塵で汚
染されないようアルゴンガスを吹き込む導入部６
を設ける。さらに安全を期するために、光導入系
ランス１６上部にさらにアルゴンガスを追加導入
する吹込口１７を設けた。
分光器１０は、焦点距離200cmで、2400l／mmの
回折格子を備えスペクトル強度を求める光電子増
倍管１８を備え、その測定値を入力する論理回路
１９を備えている。
本発明装置により連続分析を行つた結果の一例
を第６図に示す。図中、丸で囲んだ点は異常値で
あり、点線の丸は、被測定物中に入つた不純物の
影響、実線の丸は、励起不良による異常値であ
る。分析した元素、スペクトル線の波長、分析結
果を第１表に示す。この表には、試料を流動状態
から採取して湿式で分析した値、被測定値までの
距離ｌとレーザー光の集光レンズの焦点距離ｆ
を、
0.95f≦ｌ≦1.05f
の関係にして10回測定した平均値より求めた分
析値(1)、および10回測定してその平均値を計算
し、その平均値の±５％以内の測定値を使つて
再度平均値ａを求め、その値より求めた分析値
(2)を示す。分析値(1)よりも分析値(2)の方が、湿式
で分析した値に近い値となつている。
[Industrial Application Field] The present invention continuously processes multi-component elements of metals or insulators in various fluid states, including hot metal, molten steel, slag, glass, semiconductors, etc., using a laser without coming into contact with them. The present invention relates to a device for online analysis. [Prior Art] Conventionally, a sample is placed in a closed container such as a crucible for analysis of a molten material. A sample is taken from the melt stream and analyzed. The excitation source and part of the measurement system are immersed in the melt flow for analysis. Either method or a combination of these methods have been used. However, the above-mentioned method of analysis by leaving the sample in a closed container such as a crucible is difficult to apply immediately to analysis during the manufacturing process, and it is difficult to immediately apply the method of analysis by leaving the sample in a closed container such as a crucible. The method of immersing the analyzer in water may disturb the flow of the object to be measured,
It had the disadvantage of being contaminated. Examples of applying laser emission spectrometry to molten materials to improve these shortcomings include: 1) Japanese Patent Application Laid-open No. 52-72285, 2) Utility Model No. 51-6147, 3) Runge, Bonfigurio, Brian: Spectro. Kim, Acta 22 (EF Runge, S.
Bonfiglio and ERBryan: Spectrochim,
Acta, 22 (1965) 1678, ) 4) Ozaki, Takahashi, Iwai, Gunji, Sudo; Tetsu to Hagane 68
(1982) 863), but these are all laser spectroscopic analysis methods in which the sample is placed in a closed container such as a crucible. Therefore, it does not concern analysis in the manufacturing process where problems such as (1) vertical movement of the surface of the object to be measured, (2) impurities in and on the surface of the object to be measured, and (3) heat radiation from the object to be measured occur. The present inventors have solved the above problem (1) by applying a high-output pulse to the melt to be measured in a fluid state as a method for online component analysis without coming into contact with metals or insulators in a fluid state. We proposed a method for continuous online analysis without bringing the excitation source or measurement system into contact with the object to be measured, by irradiating it with laser light and analyzing the resulting emission spectrum. (Patent Application No. 58-108456) [Problems to be Solved by the Invention] The above proposal is extremely preferable because it allows online analysis of metals and insulators in a fluid state, but the above (2) and (3) There are still problems: a) When impurities floating on the surface of the object to be measured or impurities dissolved in the object to be measured are irradiated with laser light, the measurement accuracy is significantly impaired, causing data variations. (b) Radiant heat from the measured object may cause deviations in the optical axis of the laser oscillator or in optical systems such as the light introduction system and spectrometer, resulting in inaccurate analytical values; c) ) The tip of the lance sometimes needs to be replaced, but
If the entire device was replaced, the optical axis system would need to be readjusted due to problems such as the mounting accuracy of the mounting section, so there is an idea to create a heat-resistant structure that allows only the tip to be replaced. An object of the present invention is to solve such problems and provide a continuous measuring device that can suitably implement the online analysis method described above. [Means for Solving the Problems] The present invention provides an apparatus for analyzing components of metals and insulators in a molten state, which includes: 1) providing a continuous flow path for the object to be measured; 2) dissolving the object to be measured in this flow path 3. Installing a laser emission spectrometer in which the distance l to the laser beam and the focal length f of the laser beam condensing lens always have a relationship of 0.95f≦l≦1.05f within the variation range of the surface of the object to be measured; 3. ) Prepare a means to average the measured values by excluding the signal when impurities in the object to be measured are irradiated with the laser beam, that is, to average the measured values of 6 to 10 laser beam irradiation signals of the object to be measured. After averaging the data, it must be equipped with a means for re-averaging the measured values within 95% to 105% of the average value; 4) At least the part of the main body of the device where there is radiant heat from the object to be measured is made of a material with high heat reflectance. 5) At least the tip of the lance is equipped with a replaceable heat-resistant material that can withstand the temperature from the object to be measured; 6) Inert gas is blown into the lance. It is characterized by having a mouth. The present invention will be explained in detail below. First of all, in equipment that actually applies laser emission spectroscopy to on-site analysis, the biggest problem is the effect of vertical movement of the object to be measured. In order to solve this problem, the present inventors conducted an investigation using the apparatus shown in FIG. 2. The laser used was an infrared pulsed laser with a pulse width of 15 ns, an output of 2 J, and a wavelength of 1.06 μm. Referring to FIG. 2, laser light generated by a laser oscillator 1 is bent downward by a prism 2, and is focused onto the surface of an object to be measured 4 by a condenser lens 3. Here, an Fe-0.3%Mn alloy was used as the object to be measured 4, and this alloy was melted in a Tammann furnace 5. At this time, it was expected that an oxide film would be formed on the surface of the object to be measured 4, so
Blowing argon gas from the argon gas introduction part 6 and releasing it from the argon gas discharge part 7 to the outside of the system,
Suppressed the formation of oxide film. Light generated by laser beam irradiation was guided to a spectroscope 10 by a light introduction system consisting of a concave mirror 8 and plane mirrors 9a and 9b. Spectrometer 1
0, the wavelength is separated by the usual method,
The intensities of the Fe spectrum at 271.4 nm and the Mn spectrum at 293.3 nm were measured by two photodetectors 11. In order to change the distance between the object to be measured 4 and the laser spectrometer optical system, the Tammann furnace 5 was placed on a lift 12, and the entire melting furnace was moved up and down. At this time, the light introduction system and the Tammann furnace 5 should be
A grinder 13 was provided in between. The focal length of the laser condensing lens 3 is 20, 50, 100, respectively.
Five types of 150 and 200 cm were used interchangeably. Note that when the condenser lens 3 is replaced, the radius of the concave mirror 8 is selected so that the excited and emitted light forms an image on the spectrometer entrance slit 14 when the surface of the object to be measured is at its focal point, and the radius of the plane mirrors 9a and 9b is changed. Adjusted the angle. FIG. 3 shows the changes in the Fe and Mn spectral intensities and their ratios due to the vertical movement of the object to be measured 4 when using a condensing lens with a focal length of 100 cm. The spectral intensity gradually decreases as the surface of the object to be measured shifts from the focal point of the condenser lens 3, but the ratio of spectral intensities used for analysis is as follows: There is no change even if it is shifted by about 5 cm. The results of similar measurements performed by changing the condenser lens 3 are summarized as shown in Figure 4, where the distance l between the condenser lens 3 and the surface of the object to be measured is equal to the focal length f of the condenser lens 3. On the other hand, it was found that when 0.95f≦l≦1.05f (1), the spectral intensity ratio remains unchanged, and a stable analytical value can be obtained regardless of the vertical movement of the object to be measured. Next, as the object to be measured 4, insulator-based SiO 2 Al 2 O 3
The same measurements as shown in Fig. 2 were carried out on the line spectra of Si (288.2 nm) and Al (309.3 nm) using the same method. The results are shown in FIG. In this case as well, even if the surface of the object to be measured is shifted by 5 cm from the focal point of the condenser lens 3, the spectral intensity ratio remains almost constant. Furthermore, the measurement results obtained by changing the condenser lens 3 are also shown in the fourth column.
It is almost the same as the figure, and if the above equation (1) is satisfied,
It has become clear that this method is not affected by vertical movement of the surface of the object to be measured. The second problem that occurs in actual manufacturing process analysis is the influence of impurities in and on the surface of the object to be measured. Light impurities floating on the surface of the object to be measured can be removed by blowing gas such as argon or nitrogen from a lance, but problems can arise if the laser is irradiated onto impurities that have entered the object to be measured. The value cannot be obtained accurately. Therefore, in the present invention, a logic circuit 19 is provided as a means for calculating an average value of 6 to 10 values by excluding an abnormal value when an impurity in the object to be measured is irradiated with a laser and obtaining an abnormal value. Specifically, the logic circuit 19 performs the following calculation. The laser light irradiation signal of the object to be measured is averaged, and then the measurement data less than 95% of this average value and 105
%, and remove abnormal values by re-averaging the measured values within 95-105%. This calculation is performed within the logic circuit 19, and the result is displayed on the display device 20. By this method, abnormal values due to laser oscillation defects, variations, and excitation/emission defects of the object to be measured can be excluded at the same time, and analysis accuracy is improved. FIG. 7 shows a flowchart of the logic circuit 19. When the apparatus is started, the logic circuit 19 instructs the laser oscillator to oscillate the laser, reads the spectral intensity of each element converted into an electric signal by the photomultiplier tube 18, and stores this as data. Repeat reading this laser oscillation data and storing the data 10 times,
Calculate the average value of these 10 data. Next, among these 10 data, the average value ± 5
Obtain the average value a again using data within %. The element concentration is calculated using this Xa and a calibration curve previously determined using a standard sample, and the result is transferred to the display device 10 and displayed. Thereby, highly accurate measurement values excluding abnormal values can be obtained. The next problem is radiant heat from the object to be measured, which causes misalignment of the optical axis of the laser oscillator or misalignment of the light introduction system/spectroscope optical system, resulting in inaccurate analytical values. Therefore, in the present invention, a reflective plate 21 made of duralumin with high heat reflectance or a heat shielding plate made of heat-resistant material is attached to the front and lower surfaces of the device facing the object to be measured to block the reflected heat from the object to be measured. ing. Alternatively, water, gas, or the like may be allowed to flow between the device main body and the reflecting plate 21 for cooling. The light introduction system lance is prone to adhesion due to scattering of the object to be measured, and needs to be replaced after a certain period of time. If the entire lance is made of refractory material, the joints will be weak and the optical axis system will need to be readjusted each time the lance is attached or detached from the main body of the device, since there is no reproducibility. Therefore, in the present invention, the lance main body is made of a hard material such as stainless steel or duralumin, and only the tip is made of refractory material 22 to improve the reproducibility of the connection with the main body. In addition, an inlet 17 for introducing an inert gas into the lance is provided to clean the surface of the object to be measured and prevent the above-mentioned troubles. [Embodiment] The apparatus of the present invention uses a condenser lens having a focal length that is at least 10 times longer than the range of vertical movement of the surface of the object to be measured. By doing so, the above equation (1) will always hold true. The light introduction system is then adjusted so that the light emitted from this focal length is imaged onto the spectrometer entrance slit. An infrared pulsed laser is suitable as the laser, but a ruby laser that emits visible light can also be used. A known device is used for spectroscopy of the light emitted by laser irradiation and measurement of specific spectral intensity. If there is another substance such as an oxide film on the surface of the object to be measured, remove it by blowing gas such as argon or nitrogen, or install an appropriate obstacle to separate it from the object to be measured, but the laser beam introduction system Introductory part 6 in which argon gas is blown to prevent contamination with gas and dust.
will be established. In order to further ensure safety, an inlet 17 for additionally introducing argon gas was provided above the light introduction system lance 16. The spectrometer 10 has a focal length of 200 cm, a photomultiplier tube 18 equipped with a 2400 l/mm diffraction grating for determining spectral intensity, and a logic circuit 19 for inputting the measured value. FIG. 6 shows an example of the results of continuous analysis performed using the apparatus of the present invention. In the figure, the circled points are abnormal values, the dotted circles are the effects of impurities that have entered the object to be measured, and the solid circles are abnormal values due to poor excitation. Table 1 shows the analyzed elements, wavelengths of spectral lines, and analysis results. This table includes the values obtained when the sample was taken from a flowing state and analyzed using a wet method, the distance l to the measured value, and the focal length f of the laser beam condensing lens.
The analysis value (1) obtained from the average value of 10 measurements with the relationship 0.95f≦l≦1.05f, and the analysis value (1) calculated from the average value of 10 measurements, and the value within ±5% of the average value. Calculate the average value a again using the measured values, and then calculate the analysis value from that value.
(2) is shown. Analysis value (2) is closer to the wet analysis value than analysis value (1).
本発明により、レーザー分光分析装置を流動被
測定物に対して最も適正な位置に配列すると共に
不可避的な不純物等による不適正データを除外す
る機能を備えることにより精度がすぐれ、信頼度
の高い、流動状態の金属、絶縁物のレーザー発光
分光分析がオンラインで可能となつた。また、熱
影響による光学系のずれ等による精度低下を確実
に防止し、また、ランスの先端部に耐熱材を装着
して結合の再現性を良くしたので光軸系の再調整
が不要となつた。さらにランス内に不活性ガスを
吹込むことにより測定物の清浄化とランス全体の
取替を不要とすることができた。従つて本発明装
置はオンラインの各種の制御や処理に貢献すると
ころが大である。
According to the present invention, the laser spectrometer is arranged at the most appropriate position with respect to the flowing object to be measured, and is equipped with a function to exclude inappropriate data due to unavoidable impurities, etc., resulting in excellent accuracy and high reliability. Laser emission spectroscopic analysis of fluidized metals and insulators is now possible online. In addition, it reliably prevents deterioration in accuracy due to misalignment of the optical system due to heat effects, and a heat-resistant material is attached to the tip of the lance to improve the reproducibility of coupling, eliminating the need for readjustment of the optical axis system. Ta. Furthermore, by blowing inert gas into the lance, it was possible to eliminate the need for cleaning the object to be measured and replacing the entire lance. Therefore, the device of the present invention greatly contributes to various online controls and processes.
第１図は本発明の装置の実施例の側面図、第２
図は被測定物表面の上下動の影響を調査したレー
ザー分光分析装置の模式的側面図、第３図はFe
−0.3％Mnの表面の上下動によるスペクトル強度
の変化を示すグラフ、第４図はスペクトル強度比
が一定となる範囲を示すグラフ、第５図はSiO2
−Al2O3の表面の上下動によるスペクトル強度の
変化を示すグラフ、第６図は本発明の実施例によ
つて測定した各元素のFeに対するスペクトル強
度比を示すグラフ、第７図は論理回路のフローチ
ヤートである。
１……レーザー発振器、２……プリズム、３…
…集光レンズ、４……被測定物、５……タンマン
炉、６……アルゴンガス導入部、７……アルゴン
ガス排出部、８……凹面鏡、９ａ，９ｂ……平面
鏡、１０……分光器、１１……光検出器、１２…
…リフト、１３……すり合せ、１４……分光器入
口スリツト、１５……分析台、１６……ランス、
１７……アルゴンガス追加導入吹込口、１８……
光電子増倍管、１９……反射板。
FIG. 1 is a side view of an embodiment of the device of the invention; FIG.
The figure is a schematic side view of a laser spectrometer used to investigate the effects of vertical movement on the surface of the object to be measured.
A graph showing the change in spectral intensity due to vertical movement of the surface of -0.3%Mn. Figure 4 is a graph showing the range where the spectral intensity ratio is constant. Figure 5 is a graph showing the range where the spectral intensity ratio is constant.
- A graph showing the change in spectral intensity due to vertical movement of the surface of Al 2 O 3. Fig. 6 is a graph showing the spectral intensity ratio of each element to Fe measured by the embodiment of the present invention. Fig. 7 is a graph showing the change in spectral intensity due to vertical movement of the surface of Al 2 O 3. This is a flowchart of the circuit. 1... Laser oscillator, 2... Prism, 3...
...Condensing lens, 4...Measurement object, 5...Tammann furnace, 6...Argon gas inlet, 7...Argon gas exhaust part, 8...Concave mirror, 9a, 9b...Plane mirror, 10...Spectroscopy Device, 11... Photodetector, 12...
... Lift, 13 ... Grinding, 14 ... Spectrometer entrance slit, 15 ... Analysis table, 16 ... Lance,
17...Additional argon gas introduction inlet, 18...
Photomultiplier tube, 19...reflector.
Claims (1)
いて、連続流路内の被測定物表面までの距離ｌと
レーザー光の集光レンズの焦点距離ｆが被測定物
の表面の変動範囲で常に 0.95f≦ｌ≦1.05f の関係を有するレーザー発光分光分析装置を配設
し、被測定物のレーザー光照射信号測定値６〜10
個のデータを平均した後、該平均値の95〜105％
内の測定値を再平均する手段を備え、装置本体の
被測定物から放射熱を受ける部分に熱遮蔽板を取
り付け、ランス先端部を取替可能な耐熱材とし、
該ランスに不活性ガスの吹込み口を設けたことを
特徴とする、流動状態の金属、絶縁物の連続分析
装置。[Claims] 1. In an apparatus for analyzing the components of metals and insulators in a molten state, the distance l to the surface of the object to be measured in a continuous flow path and the focal length f of the condensing lens of the laser beam are equal to the surface of the object to be measured. A laser emission spectrometer is installed that always has a relationship of 0.95f≦l≦1.05f in the variation range of 6 to 10.
After averaging the data, 95-105% of the average value
A heat shield plate is attached to the part of the device body that receives radiant heat from the object to be measured, and the tip of the lance is made of replaceable heat-resistant material.
A continuous analysis device for metals and insulators in a fluid state, characterized in that the lance is provided with an inert gas inlet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26300284A JPS61140842A (en) | 1984-12-14 | 1984-12-14 | Continuous analyzing device for metal and insulator in fluid state |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26300284A JPS61140842A (en) | 1984-12-14 | 1984-12-14 | Continuous analyzing device for metal and insulator in fluid state |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61140842A JPS61140842A (en) | 1986-06-27 |
| JPH0339631B2 true JPH0339631B2 (en) | 1991-06-14 |
Family
ID=17383526
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26300284A Granted JPS61140842A (en) | 1984-12-14 | 1984-12-14 | Continuous analyzing device for metal and insulator in fluid state |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61140842A (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999005511A1 (en) * | 1997-07-28 | 1999-02-04 | Nippon Steel Corporation | Method and device for ascertaining cause of abnormality of surface of material |
| US6060685A (en) * | 1997-10-23 | 2000-05-09 | Trw Inc. | Method for monitoring laser weld quality via plasma light intensity measurements |
| CN102216485B (en) * | 2008-11-14 | 2014-12-31 | 西门子Vai金属科技有限公司 | Method and device for controlling the introduction of several metals into a cavity designed to melt said metals |
| JP5862101B2 (en) * | 2011-08-10 | 2016-02-16 | Ｊｆｅスチール株式会社 | Method and apparatus for analyzing carbon concentration in molten steel |
| JP6671102B2 (en) | 2015-02-20 | 2020-03-25 | 三菱日立パワーシステムズ株式会社 | Fixing device, rotating machine, manufacturing method, assembling method and removing method of rotating machine |
| FI20155549A7 (en) * | 2015-07-10 | 2017-01-11 | Outotec Finland Oy | Method and apparatus for optical emission spectroscopy of fluids |
| JP2020187081A (en) * | 2019-05-17 | 2020-11-19 | パナソニックＩｐマネジメント株式会社 | Gas security device |
| CN118974546A (en) * | 2022-06-21 | 2024-11-15 | 日本制铁株式会社 | Molten metal bath component analysis system, molten metal bath component analysis method, hot-dip galvanizing bath management method, and hot-dip galvanized steel sheet manufacturing method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5347034B2 (en) * | 1973-09-07 | 1978-12-18 |
-
1984
- 1984-12-14 JP JP26300284A patent/JPS61140842A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61140842A (en) | 1986-06-27 |
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