JP2000241404A - Carbon fractionation analysis device - Google Patents
Carbon fractionation analysis deviceInfo
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- JP2000241404A JP2000241404A JP11351067A JP35106799A JP2000241404A JP 2000241404 A JP2000241404 A JP 2000241404A JP 11351067 A JP11351067 A JP 11351067A JP 35106799 A JP35106799 A JP 35106799A JP 2000241404 A JP2000241404 A JP 2000241404A
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- carbon
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- temperature heating
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- temperature
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】この発明は、試料中の有機炭
素と元素状炭素とを分別分析する装置に関する。The present invention relates to an apparatus for separating and analyzing organic carbon and elemental carbon in a sample.
【０００２】[0002]
【従来の技術】大気中の全浮遊粒子状物質（ＴＳＰ）中
に含まれる炭素成分の１つである元素状炭素はＳＯ2 の
ＳＯ4 2-への酸化に関与し、その濃度によっては気候変
動をひき起こす可能性がある。この元素状炭素を分析す
る手法の一つに、元素状炭素とＴＳＰ中に含まれる他の
炭素成分である有機炭素とを熱的に分離して分析する手
法がある。Is one elemental carbon BACKGROUND ART carbon component contained in the total suspended particulate matter in the air (TSP) is involved in the oxidation of SO 2 SO 4 to 2, climate by its concentration It can cause fluctuations. As one of the methods for analyzing elemental carbon, there is a method for thermally separating and analyzing elemental carbon and organic carbon which is another carbon component contained in TSP.
【０００３】図６は、従来の炭素分別分析を行う装置の
構成を概略的に示すもので、この図において、６１は熱
分解用管で、その一端側には試料Ｓを挿入するための開
閉自在な蓋を有する試料入口６２が形成され、他端側に
はガス出口６３が形成されている。そして、この熱分解
用管６１の試料入口６２側（以下、上流側という）には
キャリアガスＣＧの導入口６４が形成されている。そし
て、６５は熱分解用管６１のキャリアガス導入口６４よ
り下流側の外周に巻設されるヒータで、低温および高温
に温度設定できるようにしてある。また、６６はガス出
口６３に適宜の流路（図示していない）を介して接続さ
れるＣＯ2 分析計である。さらに、６７は試料Ｓを載せ
るための試料ボートである。FIG. 6 schematically shows the structure of a conventional apparatus for performing carbon separation analysis. In FIG. 6, reference numeral 61 denotes a pyrolysis tube, which is opened and closed at one end thereof for inserting a sample S. A sample inlet 62 having a free lid is formed, and a gas outlet 63 is formed at the other end. An inlet 64 for the carrier gas CG is formed on the sample inlet 62 side (hereinafter, referred to as an upstream side) of the pyrolysis tube 61. Reference numeral 65 denotes a heater wound around the outer periphery of the pyrolysis tube 61 on the downstream side of the carrier gas inlet 64 so that the temperature can be set to a low temperature and a high temperature. Reference numeral 66 denotes a CO 2 analyzer connected to the gas outlet 63 via an appropriate flow path (not shown). Reference numeral 67 denotes a sample boat on which the sample S is placed.
【０００４】上記構成の炭素分別分析装置の動作につい
て説明すると、まず、熱分解用管６１内の所定位置に試
料Ｓを載置した試料ボート６７を設け、その状態でヒー
タ６５を低温（例えば４００℃程度）に設定して試料Ｓ
を加熱すると、試料Ｓ中に含まれる有機炭素が揮発しＣ
Ｏ2 となった後、キャリアガスＣＧによってＣＯ2 分析
計６６に運ばれ、ＣＯ2 濃度が測定される。次に、ヒー
タ６５を高温（例えば１０００℃程度に設定し、試料Ｓ
をさらに加熱すると、試料Ｓ中に含まれる元素状炭素が
熱分解されＣＯ2 となった後、キャリアガスＣＧによっ
てＣＯ2 分析計６６に運ばれ、ＣＯ2 濃度が測定され
る。そして、上記各測定によって得られたＣＯ2 濃度に
基づいて、試料Ｓ中の有機炭素および元素状炭素の量を
それぞれ求めることができる。The operation of the carbon separation analyzer having the above structure will be described. First, a sample boat 67 on which a sample S is placed is provided at a predetermined position in a pyrolysis tube 61, and the heater 65 is cooled to a low temperature (for example, 400 ℃) and set the sample S
Is heated, the organic carbon contained in the sample S volatilizes and C
After being turned into O 2 , it is transferred to the CO 2 analyzer 66 by the carrier gas CG, and the CO 2 concentration is measured. Next, the heater 65 is set to a high temperature (for example, about 1000 ° C., and the sample S
Is further heated, the elemental carbon contained in the sample S is thermally decomposed into CO 2, and then transferred to the CO 2 analyzer 66 by the carrier gas CG to measure the CO 2 concentration. Then, the amounts of the organic carbon and the elemental carbon in the sample S can be obtained based on the CO 2 concentration obtained by each of the above measurements.
【０００５】[0005]
【発明が解決しようとする課題】しかしながら、上記従
来の炭素分別分析装置では、単一のヒータ６５しか用い
てないため、これを低温から高温に設定するには時間が
かかり、高温から低温に設定するにはさらに時間がかか
る。そして、低温で揮発するＨＣ成分はＣＯ2 分析計２
による検出は困難なためＨＣガス検知器が必要となり、
また、温度不足により酸化不十分になればＣＯが発生し
誤差が生じることになる。However, in the above-mentioned conventional carbon separation analyzer, since only a single heater 65 is used, it takes time to set the temperature from a low temperature to a high temperature. It takes more time to do so. The HC component that evaporates at low temperature is the CO 2 analyzer 2
Is difficult to detect by using an HC gas detector,
In addition, if oxidation is insufficient due to insufficient temperature, CO is generated and an error occurs.
【０００６】この発明は、上述の事柄に留意してなされ
たもので、その目的は、試料中の有機炭素および元素状
炭素を分別して精度よく分析することができるととも
に、その分析に要する時間を短縮し、短時間で所定の分
析を高精度に行うことができる炭素分別分析装置を提供
することである。The present invention has been made in consideration of the above-mentioned matters, and has as its object to separate and accurately analyze organic carbon and elemental carbon in a sample and to reduce the time required for the analysis. An object of the present invention is to provide a carbon separation analyzer capable of shortening and performing a predetermined analysis with high accuracy in a short time.
【０００７】[0007]
【課題を解決するための手段】上記目的を達成するた
め、この発明では、一端に試料入口が形成され、他端に
ガス出口が形成された熱分解用管と、前記ガス出口側に
接続されるＣＯ2 分析計を備えた炭素分別分析装置にお
いて、前記熱分解用管に、その上流側から順にキャリア
ガス導入口、試料中の有機炭素を揮発・熱分解させるた
めの低温加熱部および試料中の元素状炭素を熱分解させ
るための高温加熱部を設け、前記低温加熱部で有機炭素
を分離し、前記高温加熱部で元素状炭素を分離するよう
にしている（請求項１）。In order to achieve the above object, according to the present invention, there is provided a pyrolysis tube having a sample inlet formed at one end and a gas outlet formed at the other end, and connected to the gas outlet side. In the carbon separation analyzer equipped with a CO 2 analyzer, the pyrolysis tube is provided with a carrier gas inlet in order from the upstream side, a low-temperature heating section for volatilizing and pyrolyzing organic carbon in the sample, and a A high-temperature heating section for thermally decomposing elemental carbon is provided, organic carbon is separated by the low-temperature heating section, and elemental carbon is separated by the high-temperature heating section (claim 1).
【０００８】上記炭素分別分析装置においては、炭素分
別分析における昇温および冷却に要する時間が不要とな
る。[0008] In the above carbon separation analyzer, the time required for heating and cooling in the carbon separation analysis is not required.
【０００９】そして、高温加熱部とガス出口との間に、
発生したＨＣやＣＯなどの炭素化合物をＣＯ2 に酸化さ
せるための高温酸化部を設けた場合（請求項２）、ＨＣ
やＣＯがそのままＣＯ2 分析計に流れることがなくな
る。Then, between the high-temperature heating section and the gas outlet,
When a high-temperature oxidizing section for oxidizing generated carbon compounds such as HC and CO into CO 2 is provided (claim 2),
And CO does not flow to the CO 2 analyzer as it is.
【００１０】また、熱分解用管の高温加熱部と高温酸化
部との間に酸素または空気を導入する管を接続した場合
（請求項３）、酸素存在下での低温におけるＣＯも完全
にＣＯ2 に変換するためＣＯ発生に起因するＣＯ2 分析
計の誤差を無くすことができる。When a tube for introducing oxygen or air is connected between the high-temperature heating section and the high-temperature oxidizing section of the pyrolysis tube (claim 3), CO at low temperature in the presence of oxygen is completely reduced to CO. Conversion to 2 eliminates errors in the CO 2 analyzer due to CO generation.
【００１１】さらに、酸素または空気を導入する管およ
びこの管と熱分解用管との接続部近傍を加熱するように
した場合（請求項４）、酸素や空気の導入によって発生
したガスの温度が低下させることがなくなり、ＣＯ2 濃
度をより高精度に測定できる。Further, in the case where the pipe for introducing oxygen or air and the vicinity of the connection between the pipe and the pyrolysis pipe are heated (claim 4), the temperature of the gas generated by the introduction of oxygen or air is reduced. Therefore, the CO 2 concentration can be measured with higher accuracy.
【００１２】さらにまた、熱分解用管のガス出口とＣＯ
2 分析計との間に切替え弁を設けた場合（請求項５）、
外部から流入する空気や熱分解用管内をパージするため
に流すガスなどＣＯ2 分析計に流したくないガスを排出
することができる。Furthermore, the gas outlet of the pyrolysis tube and the CO
When a switching valve is provided between the two analyzers (claim 5),
It is possible to discharge a gas that does not need to flow into the CO 2 analyzer, such as air flowing in from the outside or a gas flowing to purge the inside of the pyrolysis tube.
【００１３】[0013]
【発明の実施の形態】この発明の実施の形態を、図面を
参照しながら説明する。図１は、この発明の炭素分別分
析装置の構成の一例を概略的に示す図で、この図におい
て、１は熱分解用管で、例えば大径部１ａと細径部１ｂ
とからなり、石英または耐熱セラミックスなど耐熱性を
有する素材で形成され、その耐熱温度は１２００℃以上
である。２は熱分解用管の一端側（大径部１ａ側）に形
成される試料入口で、試料Ｓを挿入するための開閉自在
な蓋１ａが設けられている。３は蓋１ａの近傍に設けら
れるキャリアガス導入口で、キャリアガス導入路４が接
続されている。このキャリアガス導入路４の上流側に
は、図示してないが、ＨｅまたはＮ2 などの不活性ガス
源およびＯ2 または空気などの助燃ガス源が設けられ、
不活性ガスまた助燃ガスのいずれかを択一的にキャリア
ガスＣＧとして熱分解用管１内に導入できるように構成
されている。Embodiments of the present invention will be described with reference to the drawings. FIG. 1 is a view schematically showing an example of the configuration of a carbon separation analyzer according to the present invention. In this figure, reference numeral 1 denotes a pyrolysis tube, for example, a large diameter portion 1a and a small diameter portion 1b.
And is formed of a heat-resistant material such as quartz or heat-resistant ceramic, and has a heat-resistant temperature of 1200 ° C. or more. Reference numeral 2 denotes a sample inlet formed on one end side (the large-diameter portion 1a side) of the pyrolysis tube, which is provided with an openable and closable lid 1a for inserting the sample S. Reference numeral 3 denotes a carrier gas inlet provided near the lid 1a, and a carrier gas inlet 4 is connected to the carrier gas inlet. Although not shown, an inert gas source such as He or N 2 and an auxiliary gas source such as O 2 or air are provided on the upstream side of the carrier gas introduction path 4.
It is configured such that either an inert gas or an auxiliary gas can be selectively introduced into the pyrolysis tube 1 as a carrier gas CG.
【００１４】５，６は前記熱分解用管の大径部１ａに適
宜の間隔をおいて設けられる低温加熱部、高温加熱部
で、いずれも室温から１２００°付近まで任意の温度に
設定できるヒータ５ａ，６ａを例えば大径部１ａに巻設
して形成されており、低温加熱部５では試料Ｓ中の有機
炭素が揮発・熱分解され、高温加熱部６では試料Ｓ中の
元素状炭素が熱分解される。Reference numerals 5 and 6 denote a low-temperature heating section and a high-temperature heating section provided at appropriate intervals in the large-diameter section 1a of the pyrolysis tube, and each of the heaters can be set to any temperature from room temperature to about 1200 °. The organic carbon in the sample S is volatilized and thermally decomposed in the low-temperature heating unit 5, and the elemental carbon in the sample S is evaporated in the high-temperature heating unit 6. Pyrolyzed.
【００１５】７は前記大径部１ａに連なる細径部１ｂに
設けられる高温酸化部で、細径部１ｂの外周に巻設され
るヒータ８と、酸化銅または白金などを層状に設けた酸
化触媒９とからなる。Reference numeral 7 denotes a high-temperature oxidizing portion provided on the small-diameter portion 1b connected to the large-diameter portion 1a, and a heater 8 wound around the outer periphery of the small-diameter portion 1b, and an oxidized member provided with copper oxide or platinum in a layered manner. And a catalyst 9.
【００１６】１０は前記細径部１ｂの下流側に形成され
るガス出口で、このガス出口１０には流路１１を介して
例えば非分散型赤外線ガス分析計（ＮＤＩＲ）などより
なるＣＯ2 分析計１２が設けられている。１３は流路１
１に介装される切替え弁としての三方電磁弁で、その第
１のポート１３ａがガス出口１０に、第２のポート１３
ｂがＣＯ2 分析計１２側にそれぞれ接続され、第３のポ
ート１３ｃには排気流路１４が接続されており、通常時
（電源オフ時）、ガス出口１０側とＣＯ2 分析計１２と
が連通するように構成されている。なお、１５はＣＯ2
分析計１２の下流側に設けられるガス排出路である。Reference numeral 10 denotes a gas outlet formed on the downstream side of the small-diameter portion 1b. The gas outlet 10 is connected through a flow path 11 to a CO 2 analysis device such as a non-dispersive infrared gas analyzer (NDIR). A total of 12 are provided. 13 is the channel 1
1 is a three-way solenoid valve as a switching valve, the first port 13a of which is connected to the gas outlet 10 and the second port 13
b is connected to the CO 2 analyzer 12 side, and an exhaust passage 14 is connected to the third port 13c. In a normal state (when the power is off), the gas outlet 10 side and the CO 2 analyzer 12 are connected. It is configured to communicate. In addition, 15 is CO 2
This is a gas discharge path provided downstream of the analyzer 12.
【００１７】そして、１６は試料Ｓを載置する試料ボー
トで、試料入口２を経て大径部１ａ内に挿入または取り
出しできるとともに、大径部１ａ内を自由にスライドで
きる程度の大きさに形成されている。Reference numeral 16 denotes a sample boat on which the sample S is placed. The sample boat 16 can be inserted into or taken out of the large-diameter portion 1a through the sample inlet 2 and formed so as to be freely slidable in the large-diameter portion 1a. Have been.
【００１８】次に、上記構成の炭素分別分析装置の動作
について、図２をも参照しながら説明する。まず、蓋２
ａを開けて、有機炭素の揮発・熱分解に必要な温度、例
えばＨｅ雰囲気下では５００℃程度、空気雰囲気下では
３００℃程度に保たれている低温加熱部５に達するよう
熱分解管４内に試料Ｓを試料ボート１６に載せた状態で
挿入し、例えば３〜５分間、揮発または熱分解させる。
なお、ＨｅまたはＮ2雰囲気で揮発または熱分解を行う
ときはキャリアガス入口４からＨｅまたはＮ2の導入を
行い、空気またはＯ2 雰囲気で揮発または熱分解を行う
ときも同様にキャリアガス入口４から導入を行う。Next, the operation of the carbon separation analyzer having the above configuration will be described with reference to FIG. First, lid 2
a is opened, and the temperature required for the volatilization and thermal decomposition of organic carbon, for example, about 500 ° C. in a He atmosphere, and about 300 ° C. in an air atmosphere, reach a low-temperature heating unit 5 inside the pyrolysis tube 4. The sample S is inserted on the sample boat 16 in a state where the sample S is placed on the sample boat 16 and, for example, is volatilized or thermally decomposed for 3 to 5 minutes.
When volatilization or thermal decomposition is performed in a He or N 2 atmosphere, He or N 2 is introduced from the carrier gas inlet 4. Similarly, when volatilization or thermal decomposition is performed in an air or O 2 atmosphere, the carrier gas inlet 4 is also used. Introduce from.
【００１９】前記低温加熱部５における試料Ｓの低温加
熱によって揮発または熱分解した有機炭素は、キャリア
ガスＣＧによって高温酸化部７に送られる。この高温酸
化部７は、ヒータ８によって例えば１０００℃といった
高温に保持されているので、前記有機炭素に含まれるＨ
ＣやＣＯなどが酸化されてＣＯ2 となる。このＣＯ2は
キャリアガスＣＧによって三方電磁弁１３を経てＣＯ2
分析計１２に送られ、その濃度が測定される。The organic carbon volatilized or thermally decomposed by the low-temperature heating of the sample S in the low-temperature heating section 5 is sent to the high-temperature oxidizing section 7 by the carrier gas CG. Since the high-temperature oxidizing section 7 is maintained at a high temperature of, for example, 1000 ° C. by the heater 8, H contained in the organic carbon is used.
C and CO are oxidized to CO 2 . The CO 2 is through the three-way solenoid valve 13 by the carrier gas CG CO 2
It is sent to the analyzer 12 and its concentration is measured.
【００２０】前記有機炭素の揮発または熱分解を所定時
間行った後、試料Ｓを元素状炭素の熱分解に必要な温度
（例えば８５０°Ｃ程度）に保たれている高温加熱部６
に試料ボート１６ごと移動させる。この移動に際して
は、試料入口２の蓋２ａを開けなければならないが、こ
のとき、蓋２ａ側から空気が熱分解用管１内に流入し、
空気中のＣＯ2 がＣＯ2 分析計１２側に流れるのを防ぐ
ため、三方電磁弁１３を切り換えて、ガス出口１０と排
気流路１４とを連通させておく必要がある。After the organic carbon is volatilized or thermally decomposed for a predetermined time, the sample S is heated to a high temperature heating unit 6 at a temperature (for example, about 850 ° C.) required for the thermal decomposition of elemental carbon.
Is moved together with the sample boat 16. During this movement, the lid 2a of the sample inlet 2 must be opened. At this time, air flows into the pyrolysis tube 1 from the lid 2a side,
In order to prevent CO 2 in the air from flowing to the CO 2 analyzer 12, it is necessary to switch the three-way solenoid valve 13 so that the gas outlet 10 and the exhaust passage 14 are communicated.
【００２１】そして、前記高温加熱部６において試料Ｓ
を前記温度で所定の時間例えば３〜５分間高温加熱して
熱分解を行わせる。熱分解された元素状炭素は、有機炭
素の場合と同様に、キャリアガスＣＧにより高温酸化部
７を経てＣＯ2 分析計１２に送られ、ここでＣＯ2 濃度
を測定された後、ガス排出路１５に排出される。Then, in the high-temperature heating section 6, the sample S
At a high temperature for a predetermined time, for example, 3 to 5 minutes to cause thermal decomposition. The thermally decomposed elemental carbon is sent to the CO 2 analyzer 12 through the high-temperature oxidizing unit 7 by the carrier gas CG as in the case of the organic carbon, where the CO 2 concentration is measured. It is discharged to 15.
【００２２】図２（Ａ）は、前記炭素分別分析装置の熱
分解用管１内の温度分布を概略的に示すグラフであり、
横軸は試料入口１からの距離、縦軸は熱分解用管１内の
温度である。FIG. 2A is a graph schematically showing the temperature distribution in the pyrolysis tube 1 of the above-mentioned carbon separation analyzer.
The horizontal axis is the distance from the sample inlet 1 and the vertical axis is the temperature inside the pyrolysis tube 1.
【００２３】そして、同図（Ｂ）は、前記炭素分別分析
装置よって得られたＣＯ2 発生量を概略的に示すグラフ
であり、横軸は分析開始時からの経過時間、縦軸はＣＯ
2 発生量である。このグラフの最初の山（１）は、有機
炭素を揮発・熱分解したことによるＣＯ2 の発生量を示
し、次の山（２）は、元素状炭素を熱分解したことによ
るＣＯ2 の発生量を示している。このように有機炭素と
元素状炭素にそれぞれ対応したＣＯ2 発生量が得られる
ので、この結果から試料Ｓ中に含まれていた有機炭素と
元素状炭素の量を分別して分析することができる。FIG. 3B is a graph schematically showing the amount of CO 2 generated by the above-mentioned carbon separation analyzer. The horizontal axis represents the elapsed time from the start of the analysis, and the vertical axis represents the amount of CO 2.
2 is the amount generated. The first peak (1) of this graph shows the amount of CO 2 generated by volatilization and pyrolysis of organic carbon, and the second peak (2) shows the generation of CO 2 by pyrolysis of elemental carbon. Indicates the amount. As described above, the amounts of CO 2 generated respectively corresponding to the organic carbon and the elemental carbon are obtained, so that the amounts of the organic carbon and the elemental carbon contained in the sample S can be separated and analyzed from the results.
【００２４】上述したように、この発明の炭素分別分析
装置は、一つの熱分解用管１内に、キャリアガス導入口
４、試料Ｓ中の有機炭素を揮発・熱分解させるための低
温加熱部５および試料Ｓ中の元素状炭素を熱分解させる
ための高温加熱部５をこの順で設けてなるものであるの
で、低温加熱部５および高温加熱部６を同時に動作さ
せ、これらをそれぞれ所定の温度になるようにしておく
ことができるので、炭素分別分析における昇温や冷却に
要する時間が不要となり、それだけ、分析時間に要する
時間が短縮される。As described above, the carbon separation analyzer according to the present invention includes a carrier gas inlet 4 and a low-temperature heating section for volatilizing and pyrolyzing organic carbon in the sample S in one pyrolysis tube 1. 5 and a high-temperature heating unit 5 for thermally decomposing elemental carbon in the sample S are provided in this order, so that the low-temperature heating unit 5 and the high-temperature heating unit 6 are operated simultaneously, Since the temperature can be maintained, the time required for heating and cooling in the carbon separation analysis is not required, and the time required for the analysis time is shortened accordingly.
【００２５】そして、熱分解用管１の高温加熱部６の下
流側に、発生したＨＣやＣＯなどの炭素化合物をＣＯ2
に酸化させるための高温酸化部７を設けているので、低
温加熱部５および高温加熱部６において試料Ｓをそし
て、低温加熱および高温加熱した際発生したガスにＨＣ
やＣＯなどの炭素化合物が混入していても、前記高温酸
化部７においてこれらの炭素化合物が確実に酸化されて
ＣＯ2 となるので、ＣＯ 2 分析計１２における測定に誤
差が生ずるといったことがなくなる。Then, under the high temperature heating section 6 of the pyrolysis tube 1
The generated carbon compounds such as HC and COTwo
The high temperature oxidizing section 7 for oxidizing
The sample S is heated in the heating unit 5 and the heating unit 6.
Gas generated during heating at low and high temperatures
Even if carbon compounds such as CO and CO are mixed,
These carbon compounds are reliably oxidized in the
COTwoSo CO TwoIncorrect measurement in analyzer 12
The difference does not occur.
【００２６】この発明の炭素分別分析装置は、上記実施
の形態に限られるものではなく、種々に変形して実施す
ることができ、例えば、試料Ｓを載せた試料ボート１２
を、低温加熱部５から高温加熱部６に移動する際、試料
入口２の蓋２ａを開けるのに代えて、図３に示すよう
に、試料ボート１６に鉄製の支持具１７を連設するとと
もに、熱分解用管１の外部下方に熱分解用管１と平行に
ガイド１８を設け、このガイド１８に磁石よりなる駆動
部１９を移動自在に設け、この磁石駆動部１９の磁力に
より熱分解用管１の外側から支持具１７を、図中の矢印
ＸまたはＹ方向に移動させるようにしてもよい。この構
成の炭素分別分析装置においては、蓋２ａを開けること
なく、外気遮断状態で試料Ｓを移動させることができ
る。The carbon separation analyzer of the present invention is not limited to the above embodiment, but can be modified in various ways, for example, a sample boat 12 on which a sample S is placed.
When moving from the low-temperature heating unit 5 to the high-temperature heating unit 6, instead of opening the lid 2a of the sample inlet 2, an iron support 17 is connected to the sample boat 16 as shown in FIG. A guide 18 is provided below the pyrolysis tube 1 in parallel with the pyrolysis tube 1, and a drive unit 19 made of a magnet is movably provided on the guide 18, and the magnet drive unit 19 uses the magnet force of the magnet drive unit 19 for thermal decomposition. The support 17 may be moved from the outside of the tube 1 in the arrow X or Y direction in the figure. In the carbon separation analyzer having such a configuration, the sample S can be moved in a state where the outside air is shut off without opening the lid 2a.
【００２７】また、図４に示すように、熱分解用管１の
高温加熱部６と高温酸化部７との間に、酸素または空気
などの助燃ガスＪを導入するための助燃ガス導入管２０
を接続し、熱分解用管１内に助燃ガスＪを導入するよう
にしてもよく、このようにした場合、試料Ｓの燃焼（酸
化）をより円滑かつ完全に行うことができ、所望のＣＯ
2 を発生することができる。なお、２１は助燃ガス導入
管２０に介装される開閉弁としての二方電磁弁である。As shown in FIG. 4, between the high-temperature heating section 6 and the high-temperature oxidizing section 7 of the pyrolysis tube 1, a supporting gas introducing pipe 20 for introducing a supporting gas J such as oxygen or air.
And the auxiliary combustion gas J may be introduced into the pyrolysis tube 1. In this case, the combustion (oxidation) of the sample S can be performed more smoothly and completely, and the desired CO
2 can occur. In addition, 21 is a two-way solenoid valve as an on-off valve interposed in the auxiliary combustion gas introduction pipe 20.
【００２８】さらに、図５に示すように、助燃ガス導入
管２０と熱分解用管１との接続部近傍、すなわち、助燃
ガス導入管２０の熱分解用管１に近い部分および熱分解
用管１における接続部分にヒータ２２を設け、熱分解用
管１内に導入される助燃ガスＪを予め加熱するようにし
てもよい。このようにした場合、低温加熱部５または高
温加熱部６において生じたガスが、助燃ガスＪの添加に
よって冷却されることがなく、所望のＣＯ2 を発生させ
ることができる。Further, as shown in FIG. 5, the vicinity of the connection between the auxiliary combustion gas introduction pipe 20 and the thermal decomposition pipe 1, that is, the portion of the auxiliary combustion gas introduction pipe 20 close to the thermal decomposition pipe 1 and the thermal decomposition pipe 1 may be provided with a heater 22 at the connection portion, and the auxiliary combustion gas J introduced into the pyrolysis tube 1 may be heated in advance. In such a case, the gas generated in the low-temperature heating section 5 or the high-temperature heating section 6 is not cooled by the addition of the auxiliary combustion gas J, and desired CO 2 can be generated.
【００２９】[0029]
【発明の効果】以上説明したように、この発明によれ
ば、試料中の有機炭素と元素状炭素とを分別して分析す
ることができる。そして、低温加熱部および高温加熱部
を同時に動作させ、これらをそれぞれ所定の温度になる
ようにしておくことができるので、炭素分別分析におけ
る昇温や冷却に要する時間が不要となり、それだけ、分
析時間に要する時間が短縮される。As described above, according to the present invention, it is possible to separate and analyze organic carbon and elemental carbon in a sample. Then, since the low-temperature heating unit and the high-temperature heating unit can be operated at the same time and each of them can be kept at a predetermined temperature, the time required for heating and cooling in the carbon separation analysis becomes unnecessary, and the analysis time is accordingly reduced. The time required for is reduced.
【００３０】そして、請求項２に記載の炭素分別分析装
置によれば、ＨＣやＣＯがそのままＣＯ2 分析計に流れ
ることがなくなり、ＣＯ2 の分析精度が向上する。According to the second aspect of the present invention, HC and CO do not flow directly to the CO 2 analyzer, and the accuracy of CO 2 analysis is improved.
【００３１】また、請求項３に記載の炭素分別分析装置
によれば、酸素存在下での低温におけるＣＯも完全にＣ
Ｏ2 に変換できるので、ＣＯ発生に起因するＣＯ2 分析
計の誤差を無くすことができる。According to the third aspect of the present invention, CO at low temperature in the presence of oxygen is completely C
Since it can be converted to O 2 , errors in the CO 2 analyzer due to CO generation can be eliminated.
【００３２】したがって、この発明の炭素分別分析装置
によれば、炭素分別分析をより速くより正確に行うこと
ができる。Therefore, according to the carbon separation analyzer of the present invention, carbon separation analysis can be performed faster and more accurately.
【図１】この発明の炭素分別分析装置の構成の一例を概
略的に示す図である。FIG. 1 is a diagram schematically showing an example of the configuration of a carbon separation analyzer of the present invention.
【図２】（Ａ）は前記炭素分別分析装置の熱分解用管に
おける温度分布を概略的に示すグラフ、（Ｂ）は前記炭
素分別分析装置による分析結果を概略的に示すグラフで
ある。FIG. 2 (A) is a graph schematically showing a temperature distribution in a pyrolysis tube of the carbon separation analyzer, and FIG. 2 (B) is a graph schematically showing an analysis result by the carbon separation analyzer.
【図３】前記炭素分別分析装置の他の実施の形態を概略
的に示す図である。FIG. 3 is a view schematically showing another embodiment of the carbon separation analyzer.
【図４】前記炭素分別分析装置のさらに他の実施の形態
を概略的に示す図である。FIG. 4 is a view schematically showing still another embodiment of the carbon separation analyzer.
【図５】前記炭素分別分析装置のさらに他の実施の形態
を概略的に示す図である。FIG. 5 is a view schematically showing still another embodiment of the carbon separation analyzer.
【図６】従来の炭素分別分析装置の構成を概略的に示す
図である。FIG. 6 is a diagram schematically showing a configuration of a conventional carbon separation analyzer.
１…熱分解用管、２…試料入口、３…キャリアガス導入
口、５…低温加熱部、６…高温加熱部、７…高温酸化
部、１０…ガス出口、１２…ＣＯ2 分析計、１３…切替
え弁、２０…助燃ガス導入管、Ｓ…試料。1 ... thermal cracking tube, 2 ... sample inlet, 3 ... carrier gas inlet, 5 ... low-temperature heating section, 6 ... high temperature heating part, 7 ... high-temperature oxidation unit, 10 ... gas outlet, 12 ... CO 2 analyzer 13 ... switching valve, 20 ... combustion gas introduction pipe, S ... sample.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｇ０１Ｎ 31/12 Ｇ０１Ｎ 1/28 Ｋ (72)発明者 坂東 篤 京都府京都市南区吉祥院宮の東町２番地 株式会社堀場製作所内 (72)発明者 池田 昌彦 京都府京都市南区吉祥院宮の東町２番地 株式会社堀場製作所内 (72)発明者 足立 正之 京都府京都市南区吉祥院宮の東町２番地 株式会社堀場製作所内 Ｆターム(参考） 2G042 AA01 BA03 CB06 DA03 DA05 GA01 HA02 ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification FI FI Theme Court ゛ (Reference) G01N 31/12 G01N 1/28 K (72) Inventor Atsushi Bando 2 Higashicho, Kichijoin-gu, Minami-ku, Kyoto-shi, Kyoto Address: Horiba Seisakusho Co., Ltd. F-term in HORIBA, Ltd. (reference) 2G042 AA01 BA03 CB06 DA03 DA05 GA01 HA02
Claims (5)
出口が形成された熱分解用管と、前記ガス出口側に接続
されるＣＯ2 分析計を備えた炭素分別分析装置におい
て、前記熱分解用管に、その上流側から順にキャリアガ
ス導入口、試料中の有機炭素を揮発・熱分解させるため
の低温加熱部および試料中の元素状炭素を熱分解させる
ための高温加熱部を設け、前記低温加熱部で有機炭素を
分離し、前記高温加熱部で元素状炭素を分離することを
特徴とする炭素分別分析装置。1. A carbon separation / analysis apparatus comprising: a pyrolysis tube having a sample inlet formed at one end and a gas outlet formed at the other end; and a CO 2 analyzer connected to the gas outlet side. The pyrolysis tube is provided with a carrier gas inlet, a low-temperature heating unit for volatilizing and pyrolyzing organic carbon in the sample, and a high-temperature heating unit for pyrolyzing elemental carbon in the sample, starting from the upstream side. An organic carbon separator in the low-temperature heating section and elemental carbon in the high-temperature heating section.
生したＨＣやＣＯなどの炭素化合物をＣＯ2 に酸化させ
るための高温酸化部を設けてなる請求項１に記載の炭素
分別分析装置。2. The carbon fractionation apparatus according to claim 1, wherein a high-temperature oxidizing section for oxidizing generated carbon compounds such as HC and CO to CO 2 is provided downstream of the high-temperature heating section of the pyrolysis tube. Analysis equipment.
の間に酸素または空気を導入する管を接続してなる請求
項２に記載の炭素分別分析装置。3. The carbon separation analyzer according to claim 2, wherein a pipe for introducing oxygen or air is connected between the high-temperature heating section and the high-temperature oxidizing section of the pyrolysis tube.
管と熱分解用管と酸素導入管との接続部近傍を加熱する
ようにしてなる請求項３に記載の炭素分別分析装置。4. The apparatus for separating and analyzing carbon according to claim 3, wherein the pipe for introducing oxygen or air and the vicinity of the connection between the pipe, the pyrolysis pipe and the oxygen introducing pipe are heated.
の間に切替え弁を設けてなる請求項１〜４のいずれかに
記載の炭素分別分析装置。5. The carbon separation analyzer according to claim 1, further comprising a switching valve provided between the gas outlet of the pyrolysis tube and the CO 2 analyzer.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35106799A JP3840019B2 (en) | 1998-12-25 | 1999-12-10 | Carbon separation analyzer |
| US09/730,361 US6516654B2 (en) | 1999-12-10 | 2000-12-05 | Apparatus and method for analyzing particulate matter in gas and apparatus and method for carbon differentiating |
| DE60045910T DE60045910D1 (en) | 1999-12-10 | 2000-12-07 | Method and apparatus for analyzing particulate matter in gas. |
| EP00126862A EP1106985B1 (en) | 1999-12-10 | 2000-12-07 | Method and apparatus for analyzing particulate matter in gas. |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP37076698 | 1998-12-25 | ||
| JP10-370766 | 1998-12-25 | ||
| JP35106799A JP3840019B2 (en) | 1998-12-25 | 1999-12-10 | Carbon separation analyzer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2000241404A true JP2000241404A (en) | 2000-09-08 |
| JP3840019B2 JP3840019B2 (en) | 2006-11-01 |
Family
ID=26579317
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP35106799A Expired - Fee Related JP3840019B2 (en) | 1998-12-25 | 1999-12-10 | Carbon separation analyzer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3840019B2 (en) |
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| WO2014064985A1 (en) * | 2012-10-23 | 2014-05-01 | Sato Ayako | System for unified quantitative determination of various forms of carbon and nitrogen which employs calibration curves based on organic compounds |
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- 1999-12-10 JP JP35106799A patent/JP3840019B2/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014064985A1 (en) * | 2012-10-23 | 2014-05-01 | Sato Ayako | System for unified quantitative determination of various forms of carbon and nitrogen which employs calibration curves based on organic compounds |
| JP2014085215A (en) * | 2012-10-23 | 2014-05-12 | Ayako Sato | System for unified analysis and measurement of various forms of carbon and nitrogen which employs calibration curve based on organic compounds |
| JPWO2014064985A1 (en) * | 2012-10-23 | 2016-09-08 | 佐藤 綾子 | Unified quantitative system for carbon and nitrogen using calibration curves with organic compounds |
| WO2014115364A1 (en) * | 2013-01-24 | 2014-07-31 | 株式会社島津製作所 | Sample heating device and elemental analyzer |
| JP5935908B2 (en) * | 2013-01-24 | 2016-06-15 | 株式会社島津製作所 | Sample heating device and element analyzer |
| EP2950094A4 (en) * | 2013-01-24 | 2017-02-22 | Shimadzu Corporation | Sample heating device and elemental analyzer |
| JP5527676B1 (en) * | 2013-04-04 | 2014-06-18 | 綾子 佐藤 | Carbon component measurement system in microparticulate matter |
| CN104181022A (en) * | 2014-08-28 | 2014-12-03 | 中国科学院地质与地球物理研究所 | System and method for preparing carbon dioxide gas needed by carbonate coupled isotope analysis |
| WO2020115946A1 (en) * | 2018-12-04 | 2020-06-11 | 株式会社堀場製作所 | Analysis device and analysis method |
| JPWO2020115946A1 (en) * | 2018-12-04 | 2021-10-28 | 株式会社堀場製作所 | Analytical equipment and analytical method |
| JP7217755B2 (en) | 2018-12-04 | 2023-02-03 | 株式会社堀場製作所 | Analysis device and analysis method |
| WO2023112679A1 (en) * | 2021-12-14 | 2023-06-22 | 株式会社堀場テクノサービス | Elemental analysis method, and elemental analysis device |
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