JP2000258310A - Free-carbon analyzer - Google Patents

Free-carbon analyzer

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Publication number
JP2000258310A
JP2000258310A JP11066770A JP6677099A JP2000258310A JP 2000258310 A JP2000258310 A JP 2000258310A JP 11066770 A JP11066770 A JP 11066770A JP 6677099 A JP6677099 A JP 6677099A JP 2000258310 A JP2000258310 A JP 2000258310A
Authority
JP
Japan
Prior art keywords
detector
free carbon
burned
furnace
adsorbed
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
Application number
JP11066770A
Other languages
Japanese (ja)
Inventor
Hiroshi Uchihara
博 内原
Junji Okayama
順二 岡山
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Horiba Ltd
Original Assignee
Horiba Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Horiba Ltd filed Critical Horiba Ltd
Priority to JP11066770A priority Critical patent/JP2000258310A/en
Publication of JP2000258310A publication Critical patent/JP2000258310A/en
Pending legal-status Critical Current

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  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

PROBLEM TO BE SOLVED: To reduce an error due to the drift, the noise or the like of a detector by a method wherein only free carbon in a sample is burned, generated CO is oxidized into CO2 and the CO2 is adsorbed and desorbed so as to be detected. SOLUTION: Only free carbon in a sample S which is introduced into a burning furnace 1 is burned by a temperature regulator 2. A burned and generated gas (CO+CO2) is sent to an oxidizing furnace 3 from the exit of the burning furnace 1 by means of O2 in a carrier gas K. In the oxidizing furnace 3, CO in the bruned and generated gas (CO+CO2) is changed into CO2 by an oxidizing agent, the burned and generated gas is changed wholly into CO2, and the CO2 is adsorbed by an adsorbent at room temperature, which is filled into a CO2 adsorption part 4. After it is adsorbed, the adsorbent is heated by a heater 4 from the outside of the CO2 adsorption part 4. The burned and generated gas CO2 which is adsorbed is desorbed without stopping. A flow-rate regulator 5 is adjusted, and the carrier gas K is made to flow from a branch passage. Then, the burned and generated gas CO2 is sent to a CO2 detector 6 in a set amount. The analyzed value of the CO2 detected by the CO2 detector 6 is integrated by a CPU 8.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【０００１】[0001]

【発明の属する技術分野】本発明は、燃焼法を用いた遊
離炭素分析装置に関する。[0001] The present invention relates to a free carbon analyzer using a combustion method.

【０００２】[0002]

【従来の技術】図３は、従来の遊離炭素分析装置Ｄ’の
構成を概略的に示す図である。１は燃焼炉であり、その
下流には、流量調整器５、ＣＯ検出器６’、ＣＯ2 検出
器６がこの順に設けられている。そして、前記遊離炭素
分析装置Ｄ’による分析は、試料Ｓ中の遊離炭素のみを
燃焼させる温度に温度調整された燃焼炉１に試料Ｓを投
入し、キャリアガスＫ（例えば酸素）を流しながら試料
Ｓ中の遊離炭素の全てが燃焼生成ガスＣＯ＋ＣＯ 2 とな
るまで燃焼させ、キャリアガスＫにて燃焼生成ガスＣＯ
＋ＣＯ2 をＣＯ検出器６’およびＣＯ2 検出器６に送
り、ＣＯ＋ＣＯ2 の分析値を積算していた。FIG. 3 shows a conventional free carbon analyzer D '.
It is a figure which shows a structure schematically. 1 is a combustion furnace, of which
Downstream, the flow regulator 5, CO detector 6 ', COTwodetection
The vessels 6 are provided in this order. And the free carbon
The analysis by the analyzer D 'is performed only for the free carbon in the sample S.
The sample S is thrown into the combustion furnace 1 whose temperature has been adjusted to the temperature at which combustion takes place.
Sample while flowing carrier gas K (eg, oxygen)
All of the free carbon in S is combustion gas CO + CO TwoTona
Until the combustion gas reaches the combustion gas CO
+ COTwoWith CO detector 6 'and COTwoSend to detector 6
CO, COTwoWere integrated.

【０００３】[0003]

【発明が解決しようとする課題】しかし、上記の方法で
は、遊離炭素を低温で燃焼させるため時間がかかり、検
出器に送られるＣＯおよびＣＯ2 の濃度が低くなるとと
もに、ＣＯ検出器６’およびＣＯ2 検出器６を用いる時
間が長くなることから、得られた分析結果に与えるＣＯ
検出器６’およびＣＯ2 検出器６のドリフトやノイズな
どの影響が大きくなり、分析精度が低下していた。However, in the above method, it takes a long time to burn free carbon at low temperature, the concentration of CO and CO 2 sent to the detector becomes low, and the CO detector 6 ′ and Since the time for using the CO 2 detector 6 is prolonged, the CO
The influence of the drift and noise of the detector 6 ′ and the CO 2 detector 6 was increased, and the analysis accuracy was reduced.

【０００４】本発明は上述の事柄に留意してなされたも
ので、その目的は、分析計のドリフトやノイズなどによ
る誤差を減少させることが可能な遊離炭素分析装置を提
供することである。[0004] The present invention has been made in view of the above, and an object of the present invention is to provide a free carbon analyzer capable of reducing errors due to drift or noise of an analyzer.

【０００５】[0005]

【課題を解決するための手段】上記目的を達成するため
に、本発明の遊離炭素分析装置は、試料中の遊離炭素の
みを燃焼させる燃焼炉と、遊離炭素の燃焼により生じた
ＣＯをＣＯ2 に酸化する酸化炉と、ＣＯ2 を吸着すると
ともに、加熱されると吸着したＣＯ2 を一気に脱着させ
るＣＯ2 吸着部と、ＣＯ2 検出器とを、この順に接続し
た。To achieve the above object, according to the Invention The free carbon analyzer of the present invention includes a combustion furnace for combusting the only free carbon in the sample, the CO produced by the combustion of free carbon CO 2 An oxidation furnace for oxidizing CO 2 , a CO 2 adsorbing section for adsorbing CO 2 and desorbing the adsorbed CO 2 at a stretch when heated, and a CO 2 detector were connected in this order.

【０００６】上記の構成により、検出器の使用時間を短
縮し、検出器のドリフトやノイズなどによる誤差を減少
させることが可能な遊離炭素分析装置を提供できる。According to the above configuration, it is possible to provide a free carbon analyzer capable of shortening the use time of the detector and reducing errors due to drift or noise of the detector.

【０００７】[0007]

【発明の実施の形態】以下、この発明の実施例を、図を
参照しながら説明する。図１は、本発明の一実施例にお
ける遊離炭素分析装置Ｄの構造を概略的に示す図であ
る。１は、ヒーター１’を備えた電気燃焼炉（燃焼炉の
一例）であり、温度調整器２によって、燃焼炉１内の温
度が調整される。そして、燃焼炉１の下流には、酸化炉
３、ＣＯ2 吸着部４、流量調整器５、ＣＯ2 検出器６が
この順に接続されている。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be described below with reference to the drawings. FIG. 1 is a diagram schematically showing the structure of a free carbon analyzer D according to one embodiment of the present invention. Reference numeral 1 denotes an electric combustion furnace (an example of a combustion furnace) provided with a heater 1 ′, and the temperature in the combustion furnace 1 is adjusted by a temperature controller 2. Then, downstream of the combustion furnace 1, an oxidation furnace 3, a CO 2 adsorption unit 4, a flow regulator 5, and a CO 2 detector 6 are connected in this order.

【０００８】前記酸化炉３は、外部にヒーター３’を備
え、内部には、例えば白金触媒などの酸化剤３ａ（図２
（Ａ）参照）がネット（図示せず）により固定された状
態で充填されている。また、前記ＣＯ2 吸着部４は、外
部にヒーター４’を備え、内部には、例えばモレキュラ
ーシーブなどの市販のＣＯ2 吸着剤４ａ（図２（Ａ）参
照）がネット（図示せず）により固定された状態で充填
されている。また、ＣＯ2 吸着部４は、吸着制御器７に
よりＣＯ2 吸着部４内の温度が調整され、吸着剤４ａの
ＣＯ2 の吸着および脱着が制御される。さらに、酸化炉
３とＣＯ2 吸着部４の間には、ＣＯ2 吸着部４へキャリ
アガスＫを導入するための分岐路９が接続されている。
なお、前記ヒーター４’として赤外線ランプを用いても
よい。The oxidizing furnace 3 has a heater 3 'on the outside and an oxidizing agent 3a such as a platinum catalyst (FIG. 2) inside.
(A) is filled in a state fixed by a net (not shown). The CO 2 adsorbing section 4 includes a heater 4 ′ on the outside, and a commercially available CO 2 adsorbent 4 a such as a molecular sieve (see FIG. 2A) is internally provided by a net (not shown). It is filled in a fixed state. Moreover, CO 2 adsorption unit 4, the temperature in the CO 2 adsorption unit 4 is adjusted, adsorption and desorption of CO 2 adsorbents 4a is controlled by the suction controller 7. Further, a branch 9 for introducing the carrier gas K into the CO 2 adsorbing section 4 is connected between the oxidation furnace 3 and the CO 2 adsorbing section 4.
Note that an infrared lamp may be used as the heater 4 '.

【０００９】前記流量調整器５は、例えば酸素からなる
キャリアガスＫにより、ＣＯ2 吸着部４からＣＯ2 検出
器６に運ばれる燃焼生成ガスＣＯ2 の流量を調整するた
めのものであり、また、ＣＯ2 検出器６には、ＣＰＵ８
が接続されている。[0009] The flow controller 5, for example, by the carrier gas K consisting of oxygen, is intended for adjusting the flow rate of the combustion product gases CO 2 carried from the CO 2 adsorption unit 4 to CO 2 detector 6, also , CO 2 detector 6 includes CPU 8
Is connected.

【００１０】次に、試料Ｓの分析方法について図２
（Ａ）、（Ｂ）を用いて説明する。なお、試料Ｓとし
て、本実施例ではＳｉＣを用いるが、これに限るもので
はない。図２（Ａ）は、遊離炭素が燃焼炉１からＣＯ2
吸着部４に送られるまでの状態を概略的に示した図であ
り、まず、試料Ｓが導入された燃焼炉１は、温度調整器
２によって、試料Ｓ中の遊離炭素だけが燃焼する温度と
して例えば８５０°Ｃに調整され、試料Ｓ中の遊離炭素
が燃焼して生じた燃焼生成ガス（ＣＯ＋ＣＯ2 ）は、キ
ャリアガスＫとして用いられるＯ2 により、燃焼炉１の
出口から酸化炉３を経て、ＣＯ2 吸着部４に送られる。Next, a method of analyzing the sample S is shown in FIG.
This will be described using (A) and (B). In this embodiment, SiC is used as the sample S, but the present invention is not limited to this. FIG. 2A shows that free carbon is supplied from the combustion furnace 1 to CO 2.
FIG. 3 is a diagram schematically illustrating a state before the sample is sent to an adsorption unit 4. First, the temperature of a combustion furnace 1 into which a sample S is introduced is set by a temperature controller 2 as a temperature at which only free carbon in the sample S burns. For example, the temperature is adjusted to 850 ° C., and the combustion product gas (CO + CO 2 ) generated by burning the free carbon in the sample S passes through the oxidation furnace 3 from the outlet of the combustion furnace 1 by O 2 used as the carrier gas K. , CO 2 adsorbing section 4.

【００１１】酸化炉３では、酸化剤３ａにより、燃焼生
成ガス（ＣＯ＋ＣＯ2 ）中のＣＯがＣＯ2 に変換され
（ＣＯ2 はそのまま）、燃焼生成ガスは全てＣＯ2 にな
る。このＣＯ2 は、ＣＯ2 吸着部４に充填された常温の
吸着剤４ａに吸着される。In the oxidizing furnace 3, CO in the combustion product gas (CO + CO 2 ) is converted into CO 2 by the oxidizing agent 3a (CO 2 as it is), and all the combustion product gas becomes CO 2 . This CO 2 is adsorbed by the normal temperature adsorbent 4 a filled in the CO 2 adsorption section 4.

【００１２】上記の操作は、燃焼炉１において試料Ｓ中
の全ての遊離炭素が燃焼するまで続けられるため、吸着
剤４ａには、試料Ｓ中の全ての遊離炭素から生じた燃焼
生成ガスＣＯ2 が吸着されることになる。The above operation is continued until all the free carbon in the sample S is burned in the combustion furnace 1. Therefore, the adsorbent 4a includes the combustion product gas CO 2 generated from all the free carbon in the sample S in the adsorbent 4a. Will be adsorbed.

【００１３】図２（Ｂ）は、遊離炭素がＣＯ2 吸着部４
からＣＯ2 検出器６に送られるまでの状態を概略的に示
した図であり、燃焼生成ガスＣＯ2 をＣＯ2 吸着部４に
吸着させたあと、ヒータ４’によりＣＯ2 吸着部４の外
側から吸着剤４ａを加熱することで、吸着剤４ａに吸着
されていた燃焼生成ガスＣＯ2 を一気に脱着させるとと
もに、流量調整器５を調整して、分岐路９からキャリア
ガスＫを流すことで、燃焼生成ガスＣＯ2 を一定流量で
ＣＯ2 検出器６に送り、ＣＯ2 検出器６が検知したＣＯ
2 の分析値をＣＰＵ８によって積算して求める。[0013] FIG. 2 (B), free carbon CO 2 adsorption unit 4
From a view state shown schematically to be sent to the CO 2 detector 6, after adsorbing the combustion product gases CO 2 to CO 2 adsorption unit 4, the outer CO 2 adsorption unit 4 by the heater 4 ' By heating the adsorbent 4a from the above, the combustion product gas CO 2 adsorbed on the adsorbent 4a is desorbed at a stretch, and the flow regulator 5 is adjusted to flow the carrier gas K from the branch passage 9, The combustion product gas CO 2 is sent at a constant flow rate to the CO 2 detector 6, and the CO 2 detected by the CO 2 detector 6
The analysis value of 2 is obtained by integration by the CPU 8.

【００１４】なお、上記の構成において、ＣＯ2 吸着部
４に吸着された燃焼生成ガスＣＯ2をＣＯ2 吸着部４か
らＣＯ2 検出器６に送る場合に、キャリアガスＫを、酸
化炉３とＣＯ2 吸着部４の間に設けた分岐路９から流さ
ずに、燃焼炉１の上流側から流してもよい。[0014] In the configuration described above, when sending the combustion product gases CO 2 adsorbed on CO 2 adsorption unit 4 from the CO 2 adsorption unit 4 to CO 2 detector 6, the carrier gas K, the oxidizing furnace 3 The gas may be flowed from the upstream side of the combustion furnace 1 without flowing from the branch passage 9 provided between the CO 2 adsorption sections 4.

【００１５】上記の構成により、遊離炭素の燃焼生成ガ
スＣＯ2 を一気に検出器に送りこむことで、検出器が検
出するＣＯ2 の濃度を高くするとともに、検出器による
検出時間を短縮できることから、検出器のドリフトやノ
イズの影響を小さくし、分析精度を上げることが可能と
なる。According to the above configuration, the concentration of CO 2 detected by the detector can be increased and the time required for detection by the detector can be reduced by sending the combustion product gas CO 2 of free carbon to the detector at a stretch. It is possible to reduce the influence of instrument drift and noise and increase the analysis accuracy.

【００１６】[0016]

【発明の効果】以上説明したように、本発明の遊離炭素
分析装置は、試料中の遊離炭素のみを燃焼させる燃焼炉
と、遊離炭素の燃焼により生じたＣＯをＣＯ2 に酸化す
る酸化炉と、ＣＯ2 を吸着するとともに、加熱されると
吸着したＣＯ2 を一気に脱着させるＣＯ2 吸着部と、Ｃ
Ｏ2 検出器とを、この順に接続したので、検出器のドリ
フトやノイズなどによる誤差を減少させ、分析精度の高
い遊離炭素分析装置を提供できる。As described above, the free carbon analyzer of the present invention comprises a combustion furnace for burning only free carbon in a sample, and an oxidation furnace for oxidizing CO generated by burning free carbon into CO 2. , together with adsorption of CO 2, and CO 2 adsorption unit to once desorb the CO 2 adsorbed when heated, C
Since the O 2 detector and the O 2 detector are connected in this order, errors due to drift and noise of the detector can be reduced, and a free carbon analyzer with high analysis accuracy can be provided.

【図面の簡単な説明】[Brief description of the drawings]

【図１】本発明の遊離炭素分析装置における一実施例の
構成を概略的に示す図である。FIG. 1 is a diagram schematically showing a configuration of one embodiment of a free carbon analyzer of the present invention.

【図２】（Ａ）は上記実施例における燃焼炉からＣＯ2
吸着部までの遊離炭素の流れを概略的に示す図であり、
（Ｂ）は上記実施例におけるＣＯ2 吸着部からＣＯ2 検
出器までの遊離炭素の流れを概略的に示す図である。FIG. 2 (A) shows CO 2 from the combustion furnace in the above embodiment.
It is a diagram schematically showing the flow of free carbon to the adsorption section,
(B) is a diagram schematically showing the flow of free carbon from CO 2 adsorption unit in the above embodiment to CO 2 detector.

【図３】従来の遊離炭素分析装置の構成を概略的に示す
図である。FIG. 3 is a diagram schematically showing a configuration of a conventional free carbon analyzer.

【符号の説明】[Explanation of symbols]

１…燃焼炉、３…酸化炉、４…ＣＯ2 吸着部、６…ＣＯ
2 検出器、Ｄ…遊離炭素分析装置、Ｓ…試料。1 ... combustion furnace, 3 ... oxidation furnace, 4 ... CO 2 adsorption unit, 6 ... CO
2 detector, D: free carbon analyzer, S: sample.

Claims (1)

【特許請求の範囲】[Claims] 【請求項１】 試料中の遊離炭素のみを燃焼させる燃焼
炉と、遊離炭素の燃焼により生じたＣＯをＣＯ2 に酸化
する酸化炉と、ＣＯ2 を吸着するとともに、加熱される
と吸着したＣＯ2 を一気に脱着させるＣＯ2 吸着部と、
ＣＯ2 検出器とを、この順に接続してなる遊離炭素分析
装置。1. A combustion furnace for burning only free carbon in a sample, an oxidizing furnace for oxidizing CO generated by burning free carbon to CO 2 , and a CO furnace for adsorbing CO 2 and adsorbing CO 2 when heated. A CO 2 adsorbing part for desorbing 2 at a stretch,
A free carbon analyzer connected to a CO 2 detector in this order.
JP11066770A 1999-03-12 1999-03-12 Free-carbon analyzer Pending JP2000258310A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP11066770A JP2000258310A (en) 1999-03-12 1999-03-12 Free-carbon analyzer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP11066770A JP2000258310A (en) 1999-03-12 1999-03-12 Free-carbon analyzer

Publications (1)

Publication Number Publication Date
JP2000258310A true JP2000258310A (en) 2000-09-22

Family

ID=13325453

Family Applications (1)

Application Number Title Priority Date Filing Date
JP11066770A Pending JP2000258310A (en) 1999-03-12 1999-03-12 Free-carbon analyzer

Country Status (1)

Country Link
JP (1) JP2000258310A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008039607A (en) * 2006-08-07 2008-02-21 Horiba Ltd Quantitative analyzing method, quantitative analyzer and program
CN108956259A (en) * 2018-06-20 2018-12-07 攀钢集团西昌钢钒有限公司 The detection method of free carbon in a kind of continuous casting covering slag
WO2022190466A1 (en) * 2021-03-12 2022-09-15 株式会社堀場製作所 Element analysis device, operation method for element analysis device, and work program for element analysis device

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008039607A (en) * 2006-08-07 2008-02-21 Horiba Ltd Quantitative analyzing method, quantitative analyzer and program
JP4733589B2 (en) * 2006-08-07 2011-07-27 株式会社堀場製作所 Quantitative analysis method, quantitative analysis apparatus and program
CN108956259A (en) * 2018-06-20 2018-12-07 攀钢集团西昌钢钒有限公司 The detection method of free carbon in a kind of continuous casting covering slag
WO2022190466A1 (en) * 2021-03-12 2022-09-15 株式会社堀場製作所 Element analysis device, operation method for element analysis device, and work program for element analysis device
JP7458504B2 (en) 2021-03-12 2024-03-29 株式会社堀場製作所 Elemental analyzer, operating method for elemental analyzer, and operation program for elemental analyzer

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