JPH0259429B2 - - Google Patents
Info
- Publication number
- JPH0259429B2 JPH0259429B2 JP57181983A JP18198382A JPH0259429B2 JP H0259429 B2 JPH0259429 B2 JP H0259429B2 JP 57181983 A JP57181983 A JP 57181983A JP 18198382 A JP18198382 A JP 18198382A JP H0259429 B2 JPH0259429 B2 JP H0259429B2
- Authority
- JP
- Japan
- Prior art keywords
- tube
- carbon
- supply pipe
- pipe
- gas supply
- 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.)
- Expired - Lifetime
Links
- 229910052799 carbon Inorganic materials 0.000 claims description 39
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 38
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 28
- 239000012495 reaction gas Substances 0.000 claims description 27
- 238000007254 oxidation reaction Methods 0.000 claims description 22
- 230000003647 oxidation Effects 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 16
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 14
- 150000001722 carbon compounds Chemical class 0.000 claims description 14
- 239000001569 carbon dioxide Substances 0.000 claims description 14
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 14
- 229910001882 dioxygen Inorganic materials 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 14
- 238000003780 insertion Methods 0.000 claims description 12
- 230000037431 insertion Effects 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 10
- 238000000197 pyrolysis Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000011144 upstream manufacturing Methods 0.000 description 2
- FMMWHPNWAFZXNH-UHFFFAOYSA-N Benz[a]pyrene Chemical compound C1=C2C3=CC=CC=C3C=C(C=C3)C2=C2C3=CC=CC2=C1 FMMWHPNWAFZXNH-UHFFFAOYSA-N 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 238000010420 art technique Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Description
【発明の詳細な説明】
本発明は、試料中に含まれる元素状炭素と有機
性炭素とを分離して分析する炭素および炭素化合
物の分析装置に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a carbon and carbon compound analysis device that separates and analyzes elemental carbon and organic carbon contained in a sample.
大気中に浮遊する粒子状炭素および粒子状炭素
化合物の混合物は、元素状炭素と、有機性炭素と
に分類される。この元素状炭素は、たとえばデイ
ーゼル排出ガスの黒煙として知られ、種々の燃料
の消費に伴なつて発生される。大気中にこの元素
状炭素が浮遊していると、光散乱が行なわれると
同時に光吸収も行なわれるので、視程障害ならび
に下層大気の熱的バランスをくずし気象変化を引
き起す可能性がある。さらにこの元素状炭素は、
大気中におけるSO2→SO4 2-反応の重要な触媒と
成る。また有機性炭素は、ベンツピレンなどに代
表されるように発ガン性を持つ場合もあり、健康
上有害である。このため大気中に含まれる前記混
合物の濃度を元素状炭素と有機性炭素とに分離し
て定量する必要が生じる。 Particulate carbon and mixtures of particulate carbon compounds floating in the atmosphere are classified as elemental carbon and organic carbon. This elemental carbon is known, for example, as black smoke from diesel exhaust gases, and is generated as a result of the consumption of various fuels. When elemental carbon is suspended in the atmosphere, it both scatters and absorbs light, which can impair visibility and disrupt the thermal balance of the lower atmosphere, causing weather changes. Furthermore, this elemental carbon is
It is an important catalyst for the SO 2 →SO 4 2- reaction in the atmosphere. Furthermore, organic carbon can be carcinogenic, as exemplified by benzpyrene, and is harmful to health. Therefore, it is necessary to separate and quantify the concentration of the mixture contained in the atmosphere into elemental carbon and organic carbon.
或る先行技術では、このような粒子状炭素およ
び粒子状炭素化合物の混合物の濃度の測定方法と
して、有機溶媒抽出による装置があるけれども、
抽出溶媒による抽出量の差が大きく、しかも抽出
操作が煩雑である欠点があつた。 Some prior art methods for measuring the concentration of particulate carbon and particulate carbon compound mixtures include devices using organic solvent extraction;
The disadvantages were that there was a large difference in the amount of extraction depending on the extraction solvent, and the extraction operation was complicated.
他の先行技術では、熱天びんを用いる熱分析装
置があるけれども、測定時間に長時間を要すると
ともに、炭素を含まない揮発性成分を有機性炭素
として誤まつて見積る可能性があり、さらに検出
感度に劣る欠点があつた。 Other prior art techniques include thermal analyzers that use thermal balances; however, they require long measurement times, may incorrectly estimate volatile components that do not contain carbon as organic carbon, and have low detection sensitivity. It had some disadvantages.
さらに他の先行技術では、水素炎イオン化検知
器を用いる分析装置があるけれども、有機性炭素
が検出されるだけであつた。 Still other prior art analyzers use flame ionization detectors, but only detect organic carbon.
本発明の目的は、上述の先行技術の欠点を解決
し、短時間に測定ができ、かつ検出感度が向上
し、しかも操作が容易である炭素および炭素化合
物の分析装置を提供することである。 An object of the present invention is to solve the above-mentioned drawbacks of the prior art and to provide a carbon and carbon compound analyzer that can perform measurements in a short time, has improved detection sensitivity, and is easy to operate.
本発明は、上下に延び、上方に開放し、底を有
する外筒管４と、
外筒管４内に同軸に挿入され、下端部は、外筒
管４の底から上方に間隔をあけて開口９を有する
内筒管５であつて、この内筒管５と外筒管４との
間に反応ガス経路２５が形成され、反応ガス経路
２５の下部は、外筒管４の底付近に連通してお
り、反応ガス経路２５の上部は閉じられている、
そのような内筒管５と、
外筒管４の底に、内筒管５の下端部の開口９よ
りもわずかに上方まで充填される酸化触媒１５
と、
内筒管５の上端部６付近に連通され、窒素ガス
を供給する窒素ガス供給管１１と、
内筒管５内に、その内筒管５の上端部６付近か
ら挿入され、内筒管５の下端部の開口９付近で酸
化触媒１５よりもわずかに上方まで延びて下方に
開口しており、酸素ガスを供給する酸素ガス供給
管１２と、
外筒管４の外方で、外筒管４の上下方向の途中
位置に設けられ、内筒管５内方の熱分解領域２３
を200〜600℃の一定温度に加熱するための第１加
熱器１３と、
外筒管４の底付近に設けられ、内筒管５の下端
部の開口９よりもわずかに上方の酸化領域２４を
600〜900℃の一定温度に加熱する第２加熱器１４
と、
外筒管４の上下方向の途中位置で、反応ガス経
路２５に連通して接続される反応ガス供給管２６
と、
反応ガス供給管２６に接続され、二酸化炭素ガ
スの定量を行う分析計２７と、
内筒管５の上端部６を開閉可能に閉じる蓋７
と、
蓋７を挿通して内筒管５に挿入され、下端部に
試料１０が設けられ、熱分解領域２３から酸化領
域２４まで、上下に変位自在である挿入棒１６と
を含むことを特徴とする炭素および炭素化合物の
分析装置である。 The present invention includes an outer tube 4 that extends vertically, opens upward, and has a bottom; and an outer tube 4 that is inserted coaxially into the outer tube 4 and whose lower end is spaced upwardly from the bottom of the outer tube 4. The inner tube 5 has an opening 9, and a reaction gas path 25 is formed between the inner tube 5 and the outer tube 4, and the lower part of the reaction gas path 25 is located near the bottom of the outer tube 4. are in communication, and the upper part of the reaction gas path 25 is closed.
Such an inner tube 5 and an oxidation catalyst 15 filled at the bottom of the outer tube 4 to a point slightly above the opening 9 at the lower end of the inner tube 5.
a nitrogen gas supply pipe 11 that is connected to the vicinity of the upper end 6 of the inner cylindrical pipe 5 and supplies nitrogen gas; It extends slightly above the oxidation catalyst 15 near the opening 9 at the lower end of the pipe 5 and opens downward, and connects an oxygen gas supply pipe 12 that supplies oxygen gas, and an outer cylinder pipe 4 that extends outward from the outside. A pyrolysis region 23 is provided at a midway position in the vertical direction of the cylindrical tube 4 and is located inside the inner cylindrical tube 5.
a first heater 13 for heating the water to a constant temperature of 200 to 600°C; and an oxidation region 24 provided near the bottom of the outer tube 4 and slightly above the opening 9 at the lower end of the inner tube 5. of
A second heater 14 that heats to a constant temperature of 600 to 900°C
and a reaction gas supply pipe 26 that is connected to the reaction gas path 25 at an intermediate position in the vertical direction of the outer cylindrical pipe 4.
, an analyzer 27 that is connected to the reaction gas supply pipe 26 and performs quantitative determination of carbon dioxide gas, and a lid 7 that opens and closes the upper end 6 of the inner cylinder pipe 5 .
and an insertion rod 16 which is inserted into the inner tube 5 through the lid 7, has the sample 10 provided at its lower end, and is vertically movable from the pyrolysis region 23 to the oxidation region 24. This is an analyzer for carbon and carbon compounds.
以下、図面によつて本発明に従う実施例を説明
する。第１図は、本発明の一実施例の簡略化した
構成図である。炭素分析器１は、反応手段２と分
析手段３とを含む。反応手段２は、有底円筒状の
外筒管４と、外筒管４の内方に外筒管を密栓して
挿入される内筒管５と、内筒管５の上端部６に密
栓される蓋７と、蓋７に形成された孔８から前記
内筒管５の下端部開口９付近まで挿入される試料
１０を釣支する挿入棒１６と、前記内筒管５の上
端部６付近に連通される窒素ガス供給管１１と、
内筒管５の上端部６付近から挿入され下端部開口
９付近まで延びる酸素ガス供給管１２と、前記外
筒管４の上下方向のほぼ中心部で外筒管４を外囲
して設けられる第１加熱器１３と、外筒管４の下
端部付近で外筒管４を外囲して設けられる第２加
熱器１４とを含む。 Embodiments according to the present invention will be described below with reference to the drawings. FIG. 1 is a simplified configuration diagram of one embodiment of the present invention. Carbon analyzer 1 includes reaction means 2 and analysis means 3. The reaction means 2 includes an outer tube 4 having a cylindrical shape with a bottom, an inner tube 5 inserted into the outer tube 4 with the outer tube sealed, and an upper end 6 of the inner tube 5 with a seal. an insertion rod 16 for supporting a sample 10 inserted from a hole 8 formed in the lid 7 to near the lower end opening 9 of the inner cylindrical tube 5; and an upper end 6 of the inner cylindrical tube 5. a nitrogen gas supply pipe 11 connected to the vicinity;
An oxygen gas supply pipe 12 is inserted from near the upper end 6 of the inner cylindrical pipe 5 and extends to near the lower end opening 9, and an oxygen gas supply pipe 12 is provided surrounding the outer cylindrical pipe 4 at approximately the center of the outer cylindrical pipe 4 in the vertical direction. It includes a first heater 13 and a second heater 14 provided near the lower end of the outer tube 4 to surround the outer tube 4 .
前記外筒管４の底部には、前記内筒管５の開口
９よりもわずかに上方までたとえば白金化酸化銅
から成る酸化触媒１５が充填される。内筒管５と
外筒管４との間には、間隔があり、反応ガス経路
２５が形成される。前記試料１０は、挿入棒１６
の先端に釣支され、移動される。挿入棒１６の先
端部には、試料１０の温度を検出するための、た
とえばクロメル・アロメル熱電対１７が付設され
る。試料１０は、分析すべき大気を等速吸引する
エアサンプラに取付けられるたとえば石英繊維
紙などのフイルタに捕集された粒子状炭素および
粒子状炭素化合物の混合物から成る。 The bottom of the outer cylindrical tube 4 is filled with an oxidation catalyst 15 made of, for example, platinized copper oxide, up to a point slightly above the opening 9 of the inner cylindrical tube 5. There is a gap between the inner tube 5 and the outer tube 4, and a reaction gas path 25 is formed. The sample 10 is inserted into the insertion rod 16
A fishing rod is attached to the tip of the rod and the object is moved. For example, a chromel-allomel thermocouple 17 is attached to the tip of the insertion rod 16 to detect the temperature of the sample 10. Sample 10 consists of a mixture of particulate carbon and particulate carbon compounds collected on a filter, such as quartz fiber paper, attached to an air sampler that draws isokinetically the atmosphere to be analyzed.
試料１０を釣支する挿入棒１６は、内筒管５の
内方で上下移動され、このとき、前記孔８と気密
に保たれる。前記蓋７には、排気口１８が設けら
れる。前記窒素ガス供給管１１の上流側には、電
磁弁１９が介在され、電磁弁１９の直下流には、
供給する窒素ガス流量を制御するロタメータ２０
が介在される。酸素ガス供給管１２にも、窒素ガ
ス供給管１１と同様の構成で、電磁弁２１とロタ
メータ２２とが介在される。 The insertion rod 16 that suspends the sample 10 is moved up and down inside the inner tube 5, and at this time is kept airtight with the hole 8. The lid 7 is provided with an exhaust port 18 . A solenoid valve 19 is interposed on the upstream side of the nitrogen gas supply pipe 11, and immediately downstream of the solenoid valve 19,
Rotameter 20 that controls the flow rate of nitrogen gas to be supplied
is intervened. The oxygen gas supply pipe 12 also has a configuration similar to that of the nitrogen gas supply pipe 11, and a solenoid valve 21 and a rotameter 22 are interposed therebetween.
第１加熱器１３は、第１加熱器１３の内方の内
筒管５内方の熱分解領域２３の温度範囲が200〜
600℃の一定温度に保持されるように設定される。
第２加熱器１４は、内筒管５の開口９よりわずか
に上方の酸化領域２４の温度範囲が600℃を超え
る一定温度に保持されるように設定される。 The first heater 13 has a temperature range of a pyrolysis region 23 inside the inner cylindrical tube 5 of the first heater 13 of
It is set to maintain a constant temperature of 600℃.
The second heater 14 is set so that the temperature range of the oxidized region 24 slightly above the opening 9 of the inner tube 5 is maintained at a constant temperature exceeding 600°C.
分析手段３は大略的には、前記外筒管４の上下
方向のほぼ中心部に前記反応ガス経路２５に連通
される反応ガス供給管２６と、反応ガス供給管２
６に連通される非分散形赤外分析計２７と、反応
ガスを吸引するためのポンプ２８とを含む。非分
散形赤外分析計２７は、反応ガス供給管２６から
供給される反応ガス中の二酸化炭素ガスの定量を
行なう。非分散形赤外分析計２７の直上流側の反
応ガス供給管２６には、二酸化炭素ガスの定量を
妨害する水分を除去するために除湿器２９が設け
られ、窒素ガスが矢符３０に示すように反応ガス
供給管２６の外周を流過する。反応ガスを一定量
非分散形赤外分析計２７に供給するために、非分
散形赤外分析計２７とポンプ２８との間には、臨
界オリフイス３１が介在される。 Roughly speaking, the analysis means 3 includes a reaction gas supply pipe 26 connected to the reaction gas path 25 at approximately the center in the vertical direction of the outer cylindrical tube 4, and a reaction gas supply pipe 2.
6 and a pump 28 for sucking the reaction gas. The non-dispersive infrared analyzer 27 measures carbon dioxide gas in the reaction gas supplied from the reaction gas supply pipe 26. A dehumidifier 29 is installed in the reaction gas supply pipe 26 immediately upstream of the non-dispersive infrared analyzer 27 in order to remove moisture that interferes with the determination of carbon dioxide gas, and nitrogen gas is supplied to the reaction gas supply pipe 26 as shown by the arrow 30. It flows around the outer periphery of the reaction gas supply pipe 26 as shown in FIG. A critical orifice 31 is interposed between the non-dispersive infrared analyzer 27 and the pump 28 in order to supply a constant amount of reaction gas to the non-dispersive infrared analyzer 27 .
外筒管４は上下に延び、上方に開放し、底を有
する。内筒管５は外筒管４内に同軸に挿入され、
上端部６が、開閉可能に蓋７によつて閉じられ
る。反応ガス経路２５の上部は閉じられている。
第１加熱器１３は、外筒管４の上下方向の途中位
置に設けられる。第２加熱器１４は、外筒管４の
底付近に設けられる。反応ガス供給管２６は、外
筒管４の上下方向の途中位置で、前述のように反
応ガス経路２５に連通して接続される。挿入棒１
６の下端部である前記先端部には、試料１０が設
けられ、少なくとも、熱分解領域２３から酸化領
域２４まで、上下に変位自在である。 The outer cylindrical tube 4 extends vertically, is open upward, and has a bottom. The inner tube 5 is coaxially inserted into the outer tube 4,
The upper end 6 is closed by a lid 7 in an openable and closable manner. The upper part of the reaction gas path 25 is closed.
The first heater 13 is provided at a midway position in the vertical direction of the outer cylindrical tube 4. The second heater 14 is provided near the bottom of the outer cylindrical tube 4. The reaction gas supply pipe 26 is connected to the reaction gas path 25 at a midway position in the vertical direction of the outer tube 4 as described above. Insertion rod 1
A sample 10 is provided at the tip, which is the lower end of the sample 6, and is vertically movable from at least the pyrolysis region 23 to the oxidation region 24.
捕集された粒子状炭素および粒子状炭素化合物
の混合物を元素状炭素と有機性炭素とに分離して
分析するにあたつては、熱分解領域２３の温度を
たとえば450℃とし、酸化領域２４の温度をたと
えば800℃とする。この熱分解領域の温度を200℃
〜600℃の範囲で適当に選ぶことによつて、比較
的低沸点の有機性炭素成分と比較的高沸点の有機
性炭素成分とに分別することが可能である。酸化
領域２３の温度は、高温になる程酸化反応に要す
る時間が短かくて済むけれども、炭素分析器１の
保護の立場から900℃を超えないように設定され
る。 When separating and analyzing the collected mixture of particulate carbon and particulate carbon compounds into elemental carbon and organic carbon, the temperature of the thermal decomposition zone 23 is set to 450° C., for example, and the temperature of the oxidation zone 24 is set to 450°C. For example, let the temperature be 800℃. The temperature of this pyrolysis area is 200℃
By appropriately selecting the temperature within the range of ~600°C, it is possible to separate the organic carbon component with a relatively low boiling point and the organic carbon component with a relatively high boiling point. The temperature of the oxidation region 23 is set not to exceed 900° C. from the standpoint of protecting the carbon analyzer 1, although the higher the temperature, the shorter the time required for the oxidation reaction.
前記窒素ガス供給管１１の電磁弁１９が開か
れ、ロタメータ２０が調整されることによつて一
定流量の不活性ガスとしての窒素ガスが矢符３２
で示すように内筒管５内を流過する。前記酸素供
給管１２からは、酸化領域２４に酸素ガスが供給
される。ポンプ２８が駆動されてこれらの窒素ガ
スと酸素ガスは、反応ガス経路２５を経由して分
析手段３のポンプ２８から排出される。 The solenoid valve 19 of the nitrogen gas supply pipe 11 is opened and the rotameter 20 is adjusted, so that a constant flow rate of nitrogen gas as an inert gas is supplied to the arrow 32.
The liquid flows through the inner tube 5 as shown in FIG. Oxygen gas is supplied from the oxygen supply pipe 12 to the oxidation region 24 . The pump 28 is driven, and these nitrogen gas and oxygen gas are discharged from the pump 28 of the analysis means 3 via the reaction gas path 25.
粒子状炭素および粒子状炭素化合物の混合物か
ら成る試料１０が仮想線３３で示すように熱分解
領域２３に挿入棒に釣支されて配置される。前記
混合物のうち揮発性成分は、揮発され、窒素ガス
とともに酸化領域２４に流過され、酸化触媒１５
の作用によつて酸素ガスと反応し、第１の二酸化
炭素ガスが生成される。この生成した第１の二酸
化炭素ガスは、反応ガス経路２５、反応ガス供給
管２６を経由して非分散形赤外分析計２７に導入
され、定量される。 A sample 10 consisting of a mixture of particulate carbon and particulate carbon compound is placed in the pyrolysis zone 23 as shown by phantom line 33 and suspended from an insertion rod. Volatile components of the mixture are volatilized and flowed together with nitrogen gas into the oxidation region 24, where they are passed through the oxidation catalyst 15.
The first carbon dioxide gas is generated by reacting with oxygen gas. The generated first carbon dioxide gas is introduced into a non-dispersive infrared analyzer 27 via a reaction gas path 25 and a reaction gas supply pipe 26, and is quantified.
次いで、挿入棒１６を第１図の下方に移動して
実線で示す位置に試料１０を配置する。試料１０
が酸化領域２４に配置されると、前記混合物のう
ち非揮発性成分は、酸素ガスと酸化触媒１５の作
用によつて反応し、第２の二酸化炭素ガスが生成
される。この生成した第２の二酸化炭素ガスは、
前述の第１の二酸化炭素ガスと同様に、非分散形
赤外分析計２７によつて定量される。 Next, the insertion rod 16 is moved downward in FIG. 1 to place the sample 10 at the position shown by the solid line. Sample 10
is placed in the oxidation region 24, the non-volatile components of the mixture react with oxygen gas under the action of the oxidation catalyst 15, and a second carbon dioxide gas is produced. This generated second carbon dioxide gas is
Similar to the first carbon dioxide gas described above, it is quantified by the non-dispersive infrared analyzer 27.
第２図は、第１図に示した炭素分析器１によつ
て測定された結果を示すグラフである。第２図に
実線で示す曲線３４は、非分散形赤外分析計２７
によつて測定された二酸化炭素ガスの吸収強度曲
線であり、破線で示す曲線３５は試料１０の温度
曲線である。曲線３４のピーク３６は前記第１の
二酸化炭素の吸収を示し、ピーク３７は前記第２
の二酸化炭素ガスの吸収を示す。したがつて曲線
３４を積分して、ピーク３６を含む面積から前記
混合物のうち揮発性成分の有機性炭素が定量さ
れ、ピーク３７を含む面積から前記混合物のうち
非揮発性成分の元素状炭素が定量される。 FIG. 2 is a graph showing the results measured by the carbon analyzer 1 shown in FIG. A curve 34 shown as a solid line in FIG.
The curve 35 shown by the broken line is the temperature curve of the sample 10. The peak 36 of the curve 34 indicates the absorption of the first carbon dioxide, and the peak 37 indicates the absorption of the second carbon dioxide.
shows the absorption of carbon dioxide gas. Therefore, by integrating the curve 34, the organic carbon, which is a volatile component of the mixture, is determined from the area that includes the peak 36, and the elemental carbon, which is a non-volatile component, of the mixture, is determined from the area that includes the peak 37. Quantitated.
この炭素分析器１によれば、たとえば0.1μｇオ
ーダの炭素および炭素化合物を検出することがで
きる。また測定に要する時間は２〜３分程度であ
る。 According to this carbon analyzer 1, carbon and carbon compounds on the order of 0.1 μg can be detected, for example. Further, the time required for measurement is about 2 to 3 minutes.
上述の実施例では、分析手段３に二酸化炭素ガ
スを分析するために非分散形赤外分析計２７が用
いられたけれども、本発明のさらに他の実施例で
は、非分散形赤外分析計２７に限ることはなく、
他の二酸化炭素ガスの分析計が用いられてもよ
い。 In the above embodiment, the non-dispersive infrared analyzer 27 was used as the analysis means 3 to analyze carbon dioxide gas, but in still another embodiment of the present invention, the non-dispersive infrared analyzer 27 Not limited to,
Other carbon dioxide gas analyzers may also be used.
上述の実施例では、大気中に浮遊する粒子状炭
素および粒子状炭素化合物の混合物の分析方法に
ついて述べたけれども、本発明は、大気中に浮遊
する前記混合物の分析方法に限ることはなく、そ
の他の炭素および炭素化合物に関連して実施する
ことができる。たとえば、湖沼水を石英繊維紙
によつて過して、湖沼水中に含まれる前記混合
物を試料１０として分析することができる。 Although the above embodiment describes a method for analyzing a mixture of particulate carbon and particulate carbon compounds floating in the air, the present invention is not limited to a method for analyzing the mixture floating in the air, and may be applied to other methods. carbon and carbon compounds. For example, lake water can be passed through quartz fiber paper and the mixture contained in the lake water can be analyzed as sample 10.
以上のように本発明によれば、分析すべき粒子
状炭素および粒子状炭素化合物の混合物を熱分解
領域から酸化領域に移動するようにしたので、短
時間に測定ができ、かつ検出感度が向上し、しか
も操作が容易である炭素および炭素化合物の分析
装置が得られる。 As described above, according to the present invention, since the mixture of particulate carbon and particulate carbon compounds to be analyzed is moved from the thermal decomposition region to the oxidation region, measurement can be performed in a short time and detection sensitivity is improved. However, an apparatus for analyzing carbon and carbon compounds that is easy to operate can be obtained.
特に本発明によれば、試料の揮発性成分と非揮
発性成分とを個別的に定量することができるよう
になる。 In particular, according to the present invention, volatile components and non-volatile components of a sample can be individually quantified.
しかも不活性ガスとして、安価な窒素ガスを用
い、酸素ガス供給管１２は、酸化触媒１５よりも
わずかに上方に酸素ガスを供給するので、揮発性
成分を輸送するための窒素ガスが不所望に熱分解
領域２３において酸素と反応することを確実に防
ぐことができ、こうして揮発性成分の定量を高精
度で行うことができる。蓋７には挿入棒１６が挿
通しており、この蓋７は内筒管５の上端部６を開
閉可能であるので、蓋７を内筒管５から取外して
試料１０の装着が容易であり、また挿入棒１６の
操作が容易である。 Moreover, since cheap nitrogen gas is used as the inert gas and the oxygen gas supply pipe 12 supplies oxygen gas slightly above the oxidation catalyst 15, the nitrogen gas used to transport volatile components is undesirably used. Reaction with oxygen in the thermal decomposition region 23 can be reliably prevented, and thus volatile components can be quantified with high precision. An insertion rod 16 is inserted through the lid 7, and since the lid 7 can open and close the upper end 6 of the inner tube 5, it is easy to remove the lid 7 from the inner tube 5 and attach the sample 10. Moreover, the insertion rod 16 is easy to operate.
第１図は本発明の一実施例の簡略化した構成
図、第２図は第１図に示した炭素分析器１によつ
て測定された結果を示すグラフである。
１……炭素分析器、２……反応手段、３……分
析手段、４……外筒管、５……内筒管、１０……
試料、１１……窒素ガス供給管、１２……酸素ガ
ス供給管、１３，１４……加熱器、１５……酸化
触媒、１６……挿入棒、２３……熱分解領域、２
４……酸化領域、２７……非分散形赤外分析計。
FIG. 1 is a simplified configuration diagram of an embodiment of the present invention, and FIG. 2 is a graph showing the results measured by the carbon analyzer 1 shown in FIG. DESCRIPTION OF SYMBOLS 1... Carbon analyzer, 2... Reaction means, 3... Analysis means, 4... Outer tube, 5... Inner tube, 10...
Sample, 11...Nitrogen gas supply pipe, 12...Oxygen gas supply pipe, 13, 14...Heater, 15...Oxidation catalyst, 16...Insertion rod, 23...Pyrolysis region, 2
4...Oxidation region, 27...Non-dispersive infrared analyzer.
Claims (1)
管４と、 外筒管４内に同軸に挿入され、下端部は、外筒
管４の底から上方に間隔をあけて開口９を有する
内筒管５であつて、この内筒管５と外筒管４との
間に反応ガス経路２５が形成され、反応ガス経路
２５の下部は、外筒管４の底付近に連通してお
り、反応ガス経路２５の上部は閉じられている、
そのような内筒管５と、 外筒管４の底に、内筒管５の下端部の開口９よ
りもわずかに上方まで充填される酸化触媒１５
と、 内筒管５の上端部６付近に連通され、窒素ガス
を供給する窒素ガス供給管１１と、 内筒管５内に、その内筒管５の上端部６付近か
ら挿入され、内筒管５の下端部の開口９付近で酸
化触媒１５よりもわずかに上方まで延びて下方に
開口しており、酸素ガスを供給する酸素ガス供給
管１２と、 外筒管４の外方で、外筒管４の上下方向の途中
位置に設けられ、内筒管５内方の熱分解領域２３
を200〜600℃の一定温度に加熱するための第１加
熱器１３と、 外筒管４の底付近に設けられ、内筒管５の下端
部の開口９よりもわずかに上方の酸化領域２４を
600〜900℃の一定温度に加熱する第２加熱器１４
と、 外筒管４の上下方向の途中位置で、反応ガス経
路２５に連通して接続される反応ガス供給管２６
と、 反応ガス供給管２６に接続され、二酸化炭素ガ
スの定量を行う分析計２７と、 内筒管５の上端部６を開閉可能に閉じる蓋７
と、 蓋７を挿通して内筒管５に挿入され、下端部に
試料１０が設けられ、熱分解領域２３から酸化領
域２４まで、上下に変位自在である挿入棒１６と
を含むことを特徴とする炭素および炭素化合物の
分析装置。[Scope of Claims] 1. An outer cylindrical tube 4 that extends vertically, is open upward, and has a bottom, and is inserted coaxially into the outer cylindrical tube 4, and the lower end is spaced upward from the bottom of the outer cylindrical tube 4. The inner tube 5 has an opening 9 at a distance, and a reactive gas path 25 is formed between the inner tube 5 and the outer tube 4 . It communicates near the bottom, and the upper part of the reaction gas path 25 is closed.
Such an inner tube 5 and an oxidation catalyst 15 filled at the bottom of the outer tube 4 to a point slightly above the opening 9 at the lower end of the inner tube 5.
a nitrogen gas supply pipe 11 that is connected to the vicinity of the upper end 6 of the inner cylindrical pipe 5 and supplies nitrogen gas; It extends slightly above the oxidation catalyst 15 near the opening 9 at the lower end of the pipe 5 and opens downward, and connects an oxygen gas supply pipe 12 that supplies oxygen gas, and an outer cylinder pipe 4 that extends outward from the outside. A pyrolysis region 23 is provided at a midway position in the vertical direction of the cylindrical tube 4 and is located inside the inner cylindrical tube 5.
a first heater 13 for heating to a constant temperature of 200 to 600°C; and an oxidation region 24 provided near the bottom of the outer tube 4 and slightly above the opening 9 at the lower end of the inner tube 5. of
A second heater 14 that heats to a constant temperature of 600 to 900°C
and a reaction gas supply pipe 26 that is connected to the reaction gas path 25 at an intermediate position in the vertical direction of the outer cylindrical pipe 4.
, an analyzer 27 that is connected to the reaction gas supply pipe 26 and performs quantitative determination of carbon dioxide gas, and a lid 7 that opens and closes the upper end 6 of the inner cylinder pipe 5 .
and an insertion rod 16 which is inserted into the inner tube 5 through the lid 7, has a sample 10 at its lower end, and is vertically movable from the pyrolysis region 23 to the oxidation region 24. Analyzer for carbon and carbon compounds.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18198382A JPS5970964A (en) | 1982-10-15 | 1982-10-15 | Analysis of carbon and carbon compound |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18198382A JPS5970964A (en) | 1982-10-15 | 1982-10-15 | Analysis of carbon and carbon compound |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5970964A JPS5970964A (en) | 1984-04-21 |
| JPH0259429B2 true JPH0259429B2 (en) | 1990-12-12 |
Family
ID=16110267
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP18198382A Granted JPS5970964A (en) | 1982-10-15 | 1982-10-15 | Analysis of carbon and carbon compound |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5970964A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWM579721U (en) * | 2019-02-20 | 2019-06-21 | 總翔企業股份有限公司 | Water sample analyzing apparatus |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5661458U (en) * | 1979-10-16 | 1981-05-25 |
-
1982
- 1982-10-15 JP JP18198382A patent/JPS5970964A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5970964A (en) | 1984-04-21 |
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