JPH02136743A - Method and apparatus for analyzing trace element in metallic material - Google Patents
Method and apparatus for analyzing trace element in metallic materialInfo
- Publication number
- JPH02136743A JPH02136743A JP29004788A JP29004788A JPH02136743A JP H02136743 A JPH02136743 A JP H02136743A JP 29004788 A JP29004788 A JP 29004788A JP 29004788 A JP29004788 A JP 29004788A JP H02136743 A JPH02136743 A JP H02136743A
- Authority
- JP
- Japan
- Prior art keywords
- crucible
- heating
- temp
- sample
- temperature
- 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.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000007769 metal material Substances 0.000 title claims description 7
- 235000013619 trace mineral Nutrition 0.000 title claims description 5
- 239000011573 trace mineral Substances 0.000 title claims description 5
- 238000002485 combustion reaction Methods 0.000 claims abstract description 36
- 238000010438 heat treatment Methods 0.000 claims abstract description 30
- 238000004458 analytical method Methods 0.000 claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 18
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 10
- 239000001569 carbon dioxide Substances 0.000 claims description 9
- 150000001247 metal acetylides Chemical class 0.000 claims description 7
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 238000000921 elemental analysis Methods 0.000 claims 1
- 230000001590 oxidative effect Effects 0.000 claims 1
- 238000011109 contamination Methods 0.000 abstract description 17
- 239000007789 gas Substances 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 3
- 230000006698 induction Effects 0.000 abstract description 3
- 229910000831 Steel Inorganic materials 0.000 description 12
- 239000010959 steel Substances 0.000 description 12
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 11
- 229910001882 dioxygen Inorganic materials 0.000 description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 10
- 229960004424 carbon dioxide Drugs 0.000 description 8
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 6
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 6
- 229910052697 platinum Inorganic materials 0.000 description 5
- 238000010411 cooking Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000004445 quantitative analysis Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 238000005202 decontamination Methods 0.000 description 2
- 230000003588 decontaminative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002436 steel type Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000010960 cold rolled steel Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005443 coulometric titration Methods 0.000 description 1
- 238000005261 decarburization Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、鋼材中の炭素を分析する、金属材料中の極微
最元素の分析方法及び装置に関するものである。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method and apparatus for analyzing carbon in steel materials, and for analyzing extremely fine elements in metal materials.
（従来の技術）
近年、自動車、電気部品、色材料として深絞り性の高い
冷延鋼板のニーズが」１常に高くなってきている。これ
にともなって鋼の高純度化が進み、１ｏｐｐｍ前後の極
低酸素鋼の製造が行われている。(Prior Art) In recent years, the need for cold-rolled steel sheets with high deep drawability for use in automobiles, electrical parts, and color materials has been constantly increasing. Along with this, the purity of steel has progressed, and ultra-low oxygen steel of around 1 oppm is being manufactured.
この極低炭素鋼の製造を行う際の工程管理、品質管理を
行う分析では主として、鋼試料を加熱、燃焼させて発生
した二酸化炭素（一部、一酸化炭素は完全に酸化されて
二酸化炭素となる）の測定に赤外線吸収法、又は電信滴
定法などが用いられている。ところが、前記した極低炭
素鋼の炭素の分析精度は、鋼試料表面の吸着あるいは付
着している炭化物及び助燃剤、ルツボ表面あるいは内部
に付着あるいは混入している炭化物により特に大きな影
響を受けることがわかっている。従って十分な分析精度
を達成するためには、上記した炭化物の除去が必要であ
ることから手作業によって鋼試料の酸洗、加熱処理、助
燃剤、ルツボの加熱処理を行って炭化物を除去した上で
鋼中の炭素を定量している。Analysis for process control and quality control when manufacturing this ultra-low carbon steel mainly focuses on carbon dioxide (some carbon monoxide is completely oxidized to carbon dioxide) generated by heating and burning steel samples. Infrared absorption method or telegraph titration method is used to measure However, the accuracy of carbon analysis of the above-mentioned ultra-low carbon steel can be particularly affected by carbides and combustion improvers that are adsorbed or attached to the steel sample surface, and carbides that are attached or mixed on the crucible surface or inside. know. Therefore, in order to achieve sufficient analysis accuracy, it is necessary to remove the carbides mentioned above, so we manually pickled the steel sample, heat-treated it, added a combustion improver, and heat-treated the crucible to remove the carbide. The amount of carbon in steel is quantified.
（発明が解決しようとする課題）
ルツボに付着している炭化物を除去するために従来は別
炉中で加熱除去するので終了後−旦か外にルツボを取り
出すことになり、この時、ルツボと閥み具との接触汚染
及びルツボが大気に触れることによる再汚染がある。(Problem to be solved by the invention) Conventionally, in order to remove carbides attached to the crucible, the crucible is removed by heating in a separate furnace. There is contamination due to contact with the curing tool and re-contamination due to the crucible coming into contact with the atmosphere.
（３題を解決するための手段）
（１）本発明ではルツボを始めから反応室内に入れ、酸
素雰囲気中で所定温度（第１設定）で加熱する。(Means for Solving the Three Problems) (1) In the present invention, the crucible is placed in a reaction chamber from the beginning and heated at a predetermined temperature (first setting) in an oxygen atmosphere.
所定温度（第１設定）はルツボの汚染を取除くための温
度でありルツボの材質製造方法によって汚染状況が異な
るため予め汚染状況を確認する実験を行って、処理時間
も８慮して、最適温度を決定する。The predetermined temperature (first setting) is the temperature to remove contamination from the crucible.Contamination conditions vary depending on the material and manufacturing method of the crucible, so we conducted an experiment to confirm the contamination status in advance and took the processing time into account to determine the optimum temperature. Determine the temperature.
（２）前項処理後、ルツボを反応管内で移動し、助燃剤
投入口よりルツボ内に助燃剤を投入し、酸素雰囲気中で
所定温度（第２設定）で加熱する。(2) After the above process, the crucible is moved within the reaction tube, a combustion improver is introduced into the crucible from the combustion improver inlet, and heated at a predetermined temperature (second setting) in an oxygen atmosphere.
所定温度（第２設定）は助燃剤の汚染を取り除くための
温度であり、助燃剤の材質、形状、製造方法によって汚
染状況が異なるため所定温度（第１設定）と同様に予め
汚染状況を確認する実験を行って、処理時間も考慮して
最適温度を決定する。The predetermined temperature (second setting) is a temperature to remove contamination from the combustion improver, and since the contamination status varies depending on the material, shape, and manufacturing method of the combustion improver, check the contamination status in advance like the predetermined temperature (first setting). Conduct experiments to determine the optimal temperature, taking into account the processing time.
（３）前項処理後、ルツボを反応管内で移動し、試料投
入口よりルツボ内に試料を投入し、所定温度（第３設定
）で加熱する。(3) After the above treatment, move the crucible within the reaction tube, introduce the sample into the crucible from the sample input port, and heat it at a predetermined temperature (third setting).
所定温度（第３設定）は鋼の汚染を取り除くための温度
であり、鋼種、試料調整方法により決められるものであ
り、予め各鋼種、試料調整方法により汚染状況を確認す
る実験を行って、処理時間も考慮して最適温度を決定す
る。The predetermined temperature (third setting) is the temperature for removing contamination from the steel, and is determined by the steel type and sample preparation method. Determine the optimal temperature by taking time into account.
（４）前項迄の処理後ルツボを反ｌｌ′ｉ５管内で燃焼
位置に移動し、試料を酸素雰囲気中で所定温度（第４設
定）で加熱し燃焼させる。(4) After the processing up to the previous section, the crucible is moved to the combustion position in the 11'i5 tube, and the sample is heated and burned at a predetermined temperature (fourth setting) in an oxygen atmosphere.
所定温度（第４設定）は鋼を完全に溶融させ、鋼中の炭
素をすべて酸化するために必要な温度である。The predetermined temperature (fourth setting) is the temperature required to completely melt the steel and oxidize all the carbon in the steel.
（５）以上の一連の工程を自動的に実行できる１構、及
び各所定温度に設定できる度自動温度プログラム制御に
よる自動化分析装置となっている。(5) It is an automated analysis device that can automatically execute the series of steps described above, and has automatic temperature program control that allows each predetermined temperature to be set.
本発明は上述の通りの属材料中の微量元素の分析方法及
び５Ａ置である。The present invention is a method and a 5A device for analyzing trace elements in metal materials as described above.
（作用）
本発明を実施するための加熱方法としては抵抗加熱、赤
外線加熱及び高周波誘導加熱などが適用できるが、本発
明の効果を最も発揮できる高周波誘導加熱法での適用例
を下記する。第１図は本発明装置の構成図、第２図は本
体部となる反応管を含む加熱燃焼部の断面図、第５図は
供試１中の炭素を定量分析するまでの温度パターンの一
例。(Function) Resistance heating, infrared heating, high frequency induction heating, etc. can be applied as a heating method for carrying out the present invention, and an example of application of the high frequency induction heating method, which can best exhibit the effects of the present invention, will be described below. Figure 1 is a configuration diagram of the apparatus of the present invention, Figure 2 is a cross-sectional view of the heating and combustion section including the reaction tube that serves as the main body, and Figure 5 is an example of the temperature pattern until quantitative analysis of carbon in sample 1. .
本発明を実施するための装置は、ガス導入部、加熱燃焼
部、分析部、及び制御記録部から成りたっており、これ
等がンイクロコンピューターによって制御されている。The apparatus for implementing the present invention consists of a gas introduction section, a heating combustion section, an analysis section, and a control recording section, all of which are controlled by a microcomputer.
以下で各部の説明を行う。Each part will be explained below.
（ａ）ガス導入部
ガス導入部は、全ての炭化分を燃焼させるための酸素ガ
ス供給系で、酸素ボンベ１から出る酸素ガス中には、例
えばメタンガスのような有機素炭化物が不純物として含
まれているため、酸素ガス清浄器２で完全燃焼させて二
酸化炭素と水に分解し、各々を吸収する吸収剤を用いる
ことによって不純物を除去する。清浄になった酸素ガス
はマイクロコンピュータ−７によって制御される酸素ガ
ス圧入調整器３を介して、加熱燃焼部４へ導かれる。(a) Gas introduction section The gas introduction section is an oxygen gas supply system for burning all carbonized components, and the oxygen gas coming out of the oxygen cylinder 1 contains organic carbonized carbide such as methane gas as an impurity. Therefore, impurities are removed by complete combustion in the oxygen gas purifier 2, decomposing it into carbon dioxide and water, and using an absorbent that absorbs each of them. The purified oxygen gas is guided to the heating combustion section 4 via the oxygen gas injection regulator 3 controlled by the microcomputer 7.
（ｂ）加熱燃焼部
加熱燃焼部は、第２図に示す石英ガラス管１２中の空炊
位置（Ｉ）に白金管台１４上の白金管１３を設け、空炊
用加熱コイル１７によって高周波１３１加熱し、その中
にあるルツボ台１５上のルツボ１１が加熱される（第１
設定温度）。非金属であるセラミック製ルツボを加熱で
きること、酸素雰囲気中で高温に耐えること、及び汚染
の心配のないことなどの条件を満足するものとして白金
材を採用している。(b) Heating and Combustion Section The heating and combustion section includes a platinum tube 13 on a platinum tube stand 14 at the dry heating position (I) in the quartz glass tube 12 shown in FIG. The crucible 11 on the crucible stand 15 inside the crucible is heated (first
Preset temperature). Platinum material was selected because it satisfies the following conditions: it can heat a non-metallic ceramic crucible, it can withstand high temperatures in an oxygen atmosphere, and there is no risk of contamination.
空炊終了後ルツボ１１は、駆動＠１６により投入位置（
ｎ）に移動し、助燃剤室１９内の助燃剤が投入され、空
炊位１Ｗ（Ｉ）に戻って助燃剤が加熱される（第２設定
温度）。After the dry cooking is completed, the crucible 11 is moved to the loading position (
n), the combustion improver in the combustion improver chamber 19 is introduced, and the combustion improver is heated back to the empty heating level 1W (I) (second set temperature).
次にルツボ１１は再び投入位置（ｎ）に移動し、試料室
２１内の試料が投入され、空炊位置（Ｉ）に戻って試料
が加熱される（第３設定温度）。Next, the crucible 11 moves again to the input position (n), the sample in the sample chamber 21 is input, and returns to the empty cooking position (I), where the sample is heated (third set temperature).
その後ルツボ１１は燃焼位置（ＩＩＩ）に移動し、試料
及び助燃剤が燃焼用加熱コイル１８により加熱され〈第
４設定温度）、燃焼する。Thereafter, the crucible 11 moves to the combustion position (III), and the sample and combustion improver are heated by the combustion heating coil 18 (to the fourth set temperature) and combusted.
酸素ガスは入口２３より入り、出口２４より第１図に示
すガス清浄器５に送られる。Oxygen gas enters through the inlet 23 and is sent through the outlet 24 to the gas purifier 5 shown in FIG.
（Ｃ）分析部
加熱燃焼部（ｂ）から送られてきたガス中には一酸化炭
素、二酸化炭素、二酸化硫黄、水分等を含んでおり、こ
のうち−Ｍ化炭素、二酸化硫黄を酸化して二酸化炭素、
二酸化硫黄とする酸化炉と二酸化炭素の定ｍに影響を及
ぼす水分。(C) Analysis section The gas sent from the heating combustion section (b) contains carbon monoxide, carbon dioxide, sulfur dioxide, moisture, etc. Of these, -M carbon and sulfur dioxide are oxidized. carbon dioxide,
Moisture affects the oxidation furnace and the constant m of carbon dioxide to sulfur dioxide.
三酸化硫黄を取除くための吸収剤を有するガス清浄器５
を介して清浄化されたガスは赤外線吸収法あるいは電量
滴定法、電気伝導法を原理とする検出器６へ導入される
。Gas purifier with absorbent for removing sulfur trioxide 5
The purified gas is introduced into a detector 6 based on the infrared absorption method, coulometric titration method, or electrical conduction method.
（ｄ）制御記録部
制御記録部は圧力調整器３とシャッター２０゜２２並び
に加熱燃焼部温度を制御し検出部から送られる二酸化炭
素のデーターを炭素濃度に換算し、記録剤９に記録し、
同時に記憶部８に記憶させるマイクロコンビｌ−ターフ
と分析操作や分析条件をマイクロコンピュータ−７に入
力するためのコントロールコンソール１０とからなる。(d) Control recording unit The control recording unit controls the pressure regulator 3, the shutter 20° 22, and the temperature of the heating and combustion unit, converts the carbon dioxide data sent from the detection unit into carbon concentration, and records it on the recording medium 9,
It consists of a microcombiner Turf to be stored in a storage section 8 at the same time, and a control console 10 for inputting analysis operations and analysis conditions to the microcomputer 7.
（実施例）
次に低炭素鋼の炭素含有１！１（１０１）Ｉ）ＩＩｆＳ
！度）の定追分析と本発明によって行った具体例を以下
に示ず。(Example) Next, the carbon content of low carbon steel is 1!1(101)I)IIfS
! Specific examples of the follow-up analysis of the degree of oxidation and the present invention are shown below.
ルツボ、助燃剤、及び供試料の汚染を除去するための第
１、第２、第３の各設定温度を、それぞれ１２００℃、
８００℃、４００℃と定めた。The first, second, and third set temperatures for removing contamination from the crucible, combustion improver, and sample were set at 1200°C, respectively.
The temperatures were set at 800°C and 400°C.
また供試料中の炭素を酸化し、二酸化炭素あるいは・−
酸素化酸素として抽出する第４設定湿度を１３００℃と
定めた。It also oxidizes carbon in the sample, converting it to carbon dioxide or...
The fourth set humidity for extraction as oxygenated oxygen was set at 1300°C.
ここで上記各設定温度は検討結果を基に定めたものであ
り、例えば助燃剤の場合は第３図に丞すように６００℃
までに汚染が完全に除去されることがわかる。Here, each set temperature mentioned above was determined based on the study results. For example, in the case of combustion improver, it is set at 600℃ as shown in Figure 3.
It can be seen that the contamination is completely removed.
又、供試料の場合は低炭素鋼中に１２Ｃの同位体である
Ｔ３ Ｃを添加した試料を加熱し、この時に発生するガ
スを質量分析計によって分析した結果、第４図に示すよ
うに４１０〜４３０℃以下では、供試料中の脱炭に起因
する１３ＣＯ１１３ＣＯ２はなかったことがわかる。た
だし、前記した様にこれらの所定−度は、使用するルツ
ボ、助燃剤の材質、供試料ついては鋼種によっても異な
ることから、分析時間も考慮して決定する必要がある。In addition, in the case of the sample, a sample in which T3C, an isotope of 12C, was added to low carbon steel was heated, and the gas generated at this time was analyzed using a mass spectrometer. As a result, as shown in Figure 4, 410 It can be seen that at temperatures below ~430°C, there was no 13CO113CO2 resulting from decarburization in the sample. However, as described above, these predetermined degrees vary depending on the crucible used, the material of the combustion improver, and the steel type of the specimen, so it is necessary to determine the analysis time by taking into account the analysis time.
この様にして決定した、温度箱１．２．３．４を設定し
て本発明装置で低炭素鋼の炭素含有量を定量分析した時
の炉内温度を第５図に、分析結果を表に丞した。Figure 5 shows the analysis results of the furnace temperature determined in this manner when the carbon content of low carbon steel was quantitatively analyzed using the device of the present invention with temperature box 1.2.3.4 set. I was raised.
なお、検出器は赤外線吸収装置とし、低炭素の鉄鋼標準
試料により検量線を作成し供試料中の炭素含有量を測定
したもので、同一試料の単純１０回繰返し測定を行った
結果である。The detector was an infrared absorption device, and a calibration curve was created using a low-carbon steel standard sample to measure the carbon content in the sample.The results were obtained by simply repeating the measurement 10 times on the same sample.
衷
第５図より、本発明法に単一装置でルツボ、助燃剤、試
料表面の汚染除去を行った上での分析値には従来法に比
べ、分析精度の良い結束が得られることが判明した。From Figure 5, it is clear that the method of the present invention provides a higher level of analysis accuracy in analytical values after removing contamination from the crucible, combustion improver, and sample surface using a single device, compared to the conventional method. did.
（発明の効果）
以上のように本発明により鋼中炭素分析を行なえば、単
一装置でルツボ、助燃剤、供試料の熱処理を同時に行い
各々の汚染を除去することにより微量の炭素を精度良く
定量分析、及び自動化することが可能である。(Effects of the Invention) As described above, if carbon analysis in steel is performed according to the present invention, trace amounts of carbon can be accurately analyzed by simultaneously heat-treating the crucible, combustion improver, and sample to remove contamination from each of them using a single device. Quantitative analysis and automation are possible.
第１図は本発明を実施するための装置の構成図、第２図
は反応管を含む加熱燃焼部の断面図、第３図は助燃剤の
汚染除去湿度を決定するための汚染炭素と加熱時間の関
係図、第４図は供試料の汚染除去温度を決定するための
汚染炭素と加熱時間の関係図、第５図は微量炭素の定量
分析を行った時の炉内温度パターン例図である。
１は酸素ボンベ、２は酸素ガス清浄器、３は酸素ガス圧
力調整器、４は加熱燃焼部、５は酸素ガス清浄器、６は
検出器、７はマイクロコンピュータ−１８は記憶部、９
は記録計、１０はコントロールコンソール、１１はルツ
ボ、１２は石英管、１３は白金管、１４は白金管用台、
１５はルツボ台、１６は駆動軸、１７は空炊用加熱コイ
ル、１８は燃焼用加熱コイル、１９は助燃剤至、２０は
助燃剤用シャッター ２１は試料室、２２は試料用シャ
ッター ２３は酸素ガス入口、２７１は酸素ガス出口、
■は空炊位置、■は投入位置、■は燃焼位置。
特許出願人 新日本製鉄株式会社Fig. 1 is a block diagram of an apparatus for carrying out the present invention, Fig. 2 is a sectional view of a heating combustion section including a reaction tube, and Fig. 3 is a diagram showing contaminated carbon and heating for determining the decontamination humidity of a combustion improver. Figure 4 is a diagram showing the relationship between contaminant carbon and heating time to determine the decontamination temperature of the sample. Figure 5 is an example of the temperature pattern in the furnace when quantitative analysis of trace carbon is performed. be. 1 is an oxygen cylinder, 2 is an oxygen gas purifier, 3 is an oxygen gas pressure regulator, 4 is a heating combustion section, 5 is an oxygen gas purifier, 6 is a detector, 7 is a microcomputer, 18 is a storage section, 9
is a recorder, 10 is a control console, 11 is a crucible, 12 is a quartz tube, 13 is a platinum tube, 14 is a stand for platinum tubes,
15 is a crucible stand, 16 is a drive shaft, 17 is a heating coil for dry cooking, 18 is a heating coil for combustion, 19 is a combustion improver, 20 is a shutter for combustion improver, 21 is a sample chamber, 22 is a shutter for a sample, 23 is oxygen Gas inlet, 271 is oxygen gas outlet,
■ is the empty cooking position, ■ is the loading position, and ■ is the combustion position. Patent applicant Nippon Steel Corporation
Claims (5)
たまま、酸素雰囲気中で所定温度（第１設定）に加熱し
、ルツボに付着した炭化物を酸化除去する金属材料中の
極微量元素の分析方法。(1) While the sample container (crucible) is inserted into the analysis chamber (reaction tube), it is heated to a predetermined temperature (first setting) in an oxygen atmosphere to oxidize and remove carbides attached to the crucible. Elemental analysis methods.
さずに助燃剤を投入し、酸素雰囲気中で所定温度（第２
設定）に加熱し、助燃剤に付着した炭化物を酸化除去す
る金属材料中の極微最元素の分析方法。(2) A combustion improver is added to the crucible from which carbides have been removed without taking it out from the reaction tube, and the crucible is heated to a predetermined temperature (second temperature) in an oxygen atmosphere.
A method for analyzing ultra-fine elements in metal materials that involves heating to a certain temperature (setting) to oxidize and remove carbides attached to combustion improvers.
から取り出さずに試料を投入し、酸素雰囲気中で所定温
度（第３設定）に加熱し、試料に付着した炭化物を酸化
除去する金属材料中の極微量元素の分析方法。(3) After the treatment described in claims (1) and (2), the sample is put into the reaction tube without being taken out, and heated to a predetermined temperature (third setting) in an oxygen atmosphere to remove the carbide attached to the sample. A method for analyzing trace elements in metal materials to be removed by oxidation.
から取り出さずに分析位置に移動し、酸素雰囲気中で所
定温度（第４設定）に加熱し試料を燃焼させ、試料中の
炭素を酸化させ、一酸化炭素あるいは二酸化炭素として
抽出する金属材料中の極微量元素の分析方法。(4) After the treatment described in claims (1) to (3), the sample is moved to an analysis position without being removed from the reaction tube, heated to a predetermined temperature (fourth setting) in an oxygen atmosphere, and burned. A method for analyzing trace elements in metal materials by oxidizing the carbon inside and extracting it as carbon monoxide or carbon dioxide.
機構、及び各所定温度に制御することができる金属材料
中の極微量元素の分析装置。(5) A mechanism for carrying out the series of steps of claims (1) to (4) above, and an analyzer for trace elements in a metal material, which can control each temperature to a predetermined temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29004788A JPH02136743A (en) | 1988-11-18 | 1988-11-18 | Method and apparatus for analyzing trace element in metallic material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29004788A JPH02136743A (en) | 1988-11-18 | 1988-11-18 | Method and apparatus for analyzing trace element in metallic material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02136743A true JPH02136743A (en) | 1990-05-25 |
Family
ID=17751098
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP29004788A Pending JPH02136743A (en) | 1988-11-18 | 1988-11-18 | Method and apparatus for analyzing trace element in metallic material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02136743A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100313238B1 (en) * | 1999-08-12 | 2001-11-07 | 김세종 | Buner for analysis of radioactivity 14C and 3H |
| JP2010107379A (en) * | 2008-10-30 | 2010-05-13 | Horiba Ltd | Introduction system used for sample analyzing apparatus |
| WO2023120490A1 (en) * | 2021-12-21 | 2023-06-29 | Ｊｆｅスチール株式会社 | Method for quantifying carbon in carbide |
-
1988
- 1988-11-18 JP JP29004788A patent/JPH02136743A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100313238B1 (en) * | 1999-08-12 | 2001-11-07 | 김세종 | Buner for analysis of radioactivity 14C and 3H |
| JP2010107379A (en) * | 2008-10-30 | 2010-05-13 | Horiba Ltd | Introduction system used for sample analyzing apparatus |
| WO2023120490A1 (en) * | 2021-12-21 | 2023-06-29 | Ｊｆｅスチール株式会社 | Method for quantifying carbon in carbide |
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