JP2007263814A - Combustion type water quality measuring instrument - Google Patents

Combustion type water quality measuring instrument Download PDF

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JP2007263814A
JP2007263814A JP2006090510A JP2006090510A JP2007263814A JP 2007263814 A JP2007263814 A JP 2007263814A JP 2006090510 A JP2006090510 A JP 2006090510A JP 2006090510 A JP2006090510 A JP 2006090510A JP 2007263814 A JP2007263814 A JP 2007263814A
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sample water
combustion
catalyst
water quality
sample
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Koji Yamada
浩司 山田
Yoko Hayashi
陽子 林
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DKK TOA Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a combustion type water quality analyzer which prevents not only the scattering of sample water to the internal wall surface of a combustion part when sample water is introduced into the combustion part but also the imperfect combustion of a target component caused by the local sudden temperature fall in the combustion part. <P>SOLUTION: The combustion type water quality analyzer is configured in such a way that it includes the combustion part 10, which has a catalyst protecting material filling bed 18 and a catalyst filling bed 16 provided therein in this order and combusts sample water therein, and a sample water introducing nozzle 30 and constituted so as not only to introduce the sample water into the combustion part from the leading end of the sample water introducing nozzle but also to measure the component in the gas obtained by combusting the sample water. In the analyzer, the leading end of the sample water introducing nozzle is brought into contact with the catalyst protecting material filling bed. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

本発明は、試料水を燃焼部内で燃焼させて得られるガス中の成分を測定する燃焼式水質分析装置に関する。   The present invention relates to a combustion-type water quality analyzer that measures components in a gas obtained by burning sample water in a combustion section.

従来、内部で試料水を燃焼させる燃焼部と、試料水の滴下ノズルとを備え、前記滴下ノズルから試料水の液滴を燃焼部内に落下させるとともに、この落下させた液滴を燃焼部内で燃焼させて得られるガス中の成分を測定する燃焼式水質分析装置が知られている。このような燃焼式水質分析装置としては、例えば、排水や河川の汚濁度を測定するために試料水中に含まれる有機物量を測定する全有機炭素測定装置(TOC計)や、同様の目的で窒素量を測定する全窒素測定装置、あるいはこれらを組み合わせた装置などがある(例えば、特許文献1参照)。   Conventionally, a combustion section for burning sample water inside and a dropping nozzle for sample water are provided, and a droplet of sample water is dropped into the combustion section from the dropping nozzle, and the dropped droplet is burned in the combustion section. Combustion-type water quality analyzers that measure the components in the gas obtained by the above process are known. Examples of such combustion-type water quality analyzers include, for example, a total organic carbon measuring device (TOC meter) that measures the amount of organic matter contained in sample water in order to measure the pollution of drainage and rivers, and nitrogen for the same purpose. There is a total nitrogen measuring device that measures the amount, or a device that combines these devices (for example, see Patent Document 1).

この場合、上記燃焼式水質分析装置の燃焼部および滴下ノズルとして、従来、図3に示す構造のものが使用されている。図3において、10は燃焼部、12は滴下ノズルを示す。燃焼部10は、石英ガラスなどからなる燃焼管14の内部に触媒を充填した触媒充填層16を配置するとともに、触媒充填層16の上方に触媒保護材料を充填した触媒保護材料充填層18を配置し、燃焼管14の周囲に燃焼管14内を加熱するための加熱部20を設けたものである。この場合、触媒としては白金触媒等の酸化触媒が使用され、触媒保護材料としてはセラミックビーズ、石英ウール等が使用される。また、加熱部20はヒータや断熱材によって構成される。   In this case, the structure shown in FIG. 3 is conventionally used as the combustion section and the dropping nozzle of the combustion-type water quality analyzer. In FIG. 3, 10 is a combustion part, 12 shows a dripping nozzle. In the combustion unit 10, a catalyst packed layer 16 filled with a catalyst is disposed inside a combustion tube 14 made of quartz glass or the like, and a catalyst protective material packed layer 18 filled with a catalyst protective material is disposed above the catalyst packed layer 16. In addition, a heating unit 20 for heating the inside of the combustion tube 14 is provided around the combustion tube 14. In this case, an oxidation catalyst such as a platinum catalyst is used as the catalyst, and ceramic beads, quartz wool, or the like is used as the catalyst protection material. Moreover, the heating part 20 is comprised with a heater and a heat insulating material.

本例の燃焼式水質分析装置を用いて水質分析を行う場合、加熱部20によって燃焼管14内を加熱するとともに、燃焼管14内に上方からキャリヤガスを流した状態で、滴下ノズル12により試料水の液滴22を燃焼管14内に上方から落下させる。なお、試料水は、例えばスライドバルブやシリンジポンプにより計量され、ポンプやエアによって滴下ノズル12から滴下される。上記液滴22は、燃焼管14内で加熱されて気化し、この気化したガス中の所定成分が触媒充填層16の触媒の作用により酸化される。そして、上記ガス成分がキャリヤガスにより検出器24に導入され、ガス中の成分が測定されるものである。   When water quality analysis is performed using the combustion-type water quality analyzer of the present example, the inside of the combustion pipe 14 is heated by the heating unit 20 and a carrier gas is flowed into the combustion pipe 14 from above, and the sample is dropped by the dropping nozzle 12. A water droplet 22 is dropped into the combustion tube 14 from above. In addition, sample water is measured with a slide valve or a syringe pump, for example, and is dripped from the dripping nozzle 12 with a pump or air. The droplets 22 are heated and vaporized in the combustion tube 14, and predetermined components in the vaporized gas are oxidized by the action of the catalyst in the catalyst packed bed 16. The gas component is introduced into the detector 24 by the carrier gas, and the component in the gas is measured.

上述した燃焼式水質分析装置では、試料水を高温で燃焼させ、燃焼ガス中の所定の成分を非分散型赤外分析計(NDIR)等の検出器で測定し、測定対象物の濃度換算を行っている。例えば、TOC計においては、試料水の液滴を燃焼部内に滴下して燃焼させるとともに、試料水中の有機物を酸化させて二酸化炭素(CO)に変換し、燃焼ガス中のCO濃度をNDIRで測定することにより、試料水中の有機体炭素濃度を求めている。 In the combustion type water quality analyzer described above, the sample water is burned at a high temperature, a predetermined component in the combustion gas is measured with a detector such as a non-dispersive infrared analyzer (NDIR), and the concentration of the measurement object is converted. Is going. For example, in a TOC meter, droplets of sample water are dropped into the combustion section and burned, and organic substances in the sample water are oxidized and converted to carbon dioxide (CO 2 ), and the CO 2 concentration in the combustion gas is changed to NDIR. The organic carbon concentration in the sample water is obtained by measuring with.

特開昭56−74634号公報JP-A-56-74634

上述した燃焼式水質分析装置において、試料水は、希釈等の前処理後にスライドバルブやシリンジポンプ等によって一定量が滴下ノズルの内部に導入され、ポンプやエアにより圧送されて燃焼部の上方から触媒保護材料充填層上に滴下される。しかし、このときポンプの圧力変動やエアの流量変動、ノズルの向き、試料水の量などにより、燃焼部の内部壁面に試料水が飛散することがあり、その結果測定精度に影響を及ぼすことがあった。   In the above-described combustion-type water quality analyzer, a predetermined amount of sample water is introduced into the inside of the dropping nozzle by a slide valve, a syringe pump or the like after pretreatment such as dilution, and pumped by a pump or air to be catalyst from above the combustion section It is dripped on the protective material packed layer. However, at this time, sample water may be scattered on the inner wall of the combustion section due to fluctuations in pump pressure, air flow rate, nozzle orientation, sample water volume, etc., which may affect measurement accuracy. there were.

また、燃焼部内は通常約600〜950℃程度に加熱されているが、試料水の滴下量が多い場合には、試料水を滴下したときに滴下ポイント(燃焼部内の試料水の液滴が当たった箇所)の局部的な急激な温度低下が起こり、試料水中の目的成分が完全に燃焼しないことがあった。   In addition, the inside of the combustion section is usually heated to about 600 to 950 ° C., but when the amount of sample water dripped is large, when the sample water is dripped, the dripping point (the sample water droplet in the combustion section hits). In some cases, the target component in the sample water does not completely burn.

本発明は、前述した事情に鑑みてなされてもので、燃焼部内に試料水を導入したときに燃焼部の内部壁面に試料水が飛散することがないとともに、燃焼部内の局部的な急激な温度低下よって生じる目的成分の不完全燃焼を防止することができる燃焼式水質分析装置を提供することを目的とする。   Although the present invention has been made in view of the above-described circumstances, when sample water is introduced into the combustion part, the sample water does not scatter on the inner wall surface of the combustion part, and a local rapid temperature in the combustion part. An object of the present invention is to provide a combustion-type water quality analyzer that can prevent incomplete combustion of a target component caused by a decrease.

本発明は、前記目的を達成するため、内部に触媒保護材料充填層およびその下方に触媒充填層が設けられ、内部で試料水を燃焼させる燃焼部と、試料水導入ノズルとを備え、前記試料水導入ノズルの先端から試料水を燃焼部内に導入し、この試料水を燃焼部内で燃焼させて得られるガス中の成分を測定する燃焼式水質分析装置であって、前記試料水導入ノズルの先端を前記触媒保護材料充填層に接触させたことを特徴とする燃焼式水質測定装置を提供する。   In order to achieve the above-mentioned object, the present invention comprises a catalyst protection material packed layer inside and a catalyst packed layer below it, a combustion section for burning sample water inside, and a sample water introduction nozzle, A combustion-type water quality analyzer that introduces sample water into a combustion part from the tip of a water introduction nozzle and measures a component in a gas obtained by burning the sample water in the combustion part, the tip of the sample water introduction nozzle A combustion-type water quality measuring apparatus is provided in which the catalyst protection material packed layer is brought into contact with the catalyst protection material packed bed.

本発明の燃焼式水質分析装置は、試料水導入ノズルの先端を触媒保護材料充填層に接触させたので、試料水は直接触媒保護材料充填層内に導入される。したがって、燃焼部の内部壁面に試料水が飛散することがなく、高精度の測定を行うことができる。また、本発明の燃焼式水質分析装置は、試料水導入ノズルの先端を延ばして触媒保護材料充填層に接触させたので、試料水は試料水導入ノズル内で加熱され、高温の液状あるいは既に気化した状態で触媒保護材料充填層内に導入される。したがって、燃焼部内の試料水導入ノズルから試料水が流出した箇所に局部的な急激な温度低下が生じず、その結果燃焼部内での試料水の燃焼効率が向上して目的成分の不完全燃焼が防止される。   In the combustion-type water quality analyzer of the present invention, the tip of the sample water introduction nozzle is brought into contact with the catalyst protective material packed bed, so that the sample water is directly introduced into the catalyst protective material packed bed. Therefore, the sample water does not scatter on the inner wall surface of the combustion unit, and high-precision measurement can be performed. In the combustion-type water quality analyzer of the present invention, since the tip of the sample water introduction nozzle is extended and brought into contact with the catalyst protective material packed layer, the sample water is heated in the sample water introduction nozzle and is heated to a high temperature or already vaporized. In this state, the catalyst protective material is introduced into the packed bed. Therefore, the local rapid temperature drop does not occur at the location where the sample water flows out from the sample water introduction nozzle in the combustion section, and as a result, the combustion efficiency of the sample water in the combustion section is improved and incomplete combustion of the target component occurs. Is prevented.

本発明においては、試料水導入ノズルの先端を触媒保護材料充填層の内部まで延出させることが好ましい。これによって、燃焼部の内部壁面に試料水が飛散することをより確実に防止することができるとともに、試料水導入ノズル内で試料水をより高温にまで加熱することができ、燃焼部内での試料水の燃焼効率をより向上させることができる。   In the present invention, it is preferable to extend the tip of the sample water introduction nozzle to the inside of the catalyst protective material packed layer. As a result, it is possible to more reliably prevent the sample water from splashing on the inner wall surface of the combustion section, and also to heat the sample water to a higher temperature in the sample water introduction nozzle, so that the sample in the combustion section can be heated. Water combustion efficiency can be further improved.

本発明において、試料水導入ノズルは石英ガラス、金属等によって形成することができるが、伝熱性に優れている点で金属で形成することが好ましい。これによって、試料水導入ノズル内で試料水をより高温にまで加熱することができ、燃焼部内での試料水の燃焼効率をより向上させることができる。   In the present invention, the sample water introduction nozzle can be formed of quartz glass, metal or the like, but is preferably formed of metal in terms of excellent heat conductivity. Accordingly, the sample water can be heated to a higher temperature in the sample water introduction nozzle, and the combustion efficiency of the sample water in the combustion section can be further improved.

本発明の燃焼式水質分析装置は、燃焼部内に試料水を導入したときに燃焼部の内部壁面に試料水が飛散することがないとともに、燃焼部内の局部的な急激な温度低下よって生じる目的成分の不完全燃焼を防止することができ。したがって、本発明の燃焼式水質分析装置によれば、高精度の水質分析を行うことが可能である。   The combustion-type water quality analyzer of the present invention is a target component that is generated when a sample water is not scattered on the inner wall surface of the combustion part when the sample water is introduced into the combustion part, and is caused by a local rapid temperature drop in the combustion part. Can prevent incomplete combustion. Therefore, according to the combustion-type water quality analyzer of the present invention, it is possible to perform highly accurate water quality analysis.

以下、図面を参照して本発明を実施するための最良の形態の一例を示す。図1は本発明に係る燃焼式水質分析装置の燃焼部および試料水導入ノズルの一例を示す概略図である。図1において、30は試料水導入ノズル、12は燃焼部を示す。燃焼部10は、図3に示したのと同じものである。すなわち、燃焼管14の内部に触媒保護材料充填層18およびその下方の触媒充填層16を設け、燃焼管14の周囲に加熱部20を設けたものである。燃焼部10は、検出器24に接続されている。   Hereinafter, an example of the best mode for carrying out the present invention will be described with reference to the drawings. FIG. 1 is a schematic view showing an example of a combustion part and a sample water introduction nozzle of a combustion-type water quality analyzer according to the present invention. In FIG. 1, 30 is a sample water introduction nozzle, 12 is a combustion part. The combustion unit 10 is the same as that shown in FIG. That is, the catalyst protection material packed layer 18 and the catalyst packed layer 16 below the catalyst protective material packed layer 18 are provided inside the combustion tube 14, and the heating unit 20 is provided around the combustion tube 14. The combustion unit 10 is connected to the detector 24.

試料水導入ノズル30は、ステンレススチールによって形成され、その先端は触媒保護材料充填層18の内部まで延出されている。ただし、試料水導入ノズル30の材質に限定はなく、耐熱性、耐酸化性を有する金属、合金、石英ガラスなどを適宜使用することができる。試料水は、希釈等の前処理後にスライドバルブやシリンジポンプ等によって一定量が試料水導入ノズル30の内部に導入され、ポンプやエアにより圧送されて試料水導入ノズル30の先端から触媒保護材料充填層18内に導入される。この場合、試料水導入ノズル30は触媒保護材料充填層18の内部にまで延びているため、燃焼管14の内部壁面に試料水が飛散することがなく、また、試料水は金属製の試料水導入ノズル30内で加熱されるため、気化した状態で触媒保護材料充填層18内に導入される。なお、本例の燃焼式水質分析装置による水質分析方法は、図3の燃焼式水質分析装置と同様である。   The sample water introduction nozzle 30 is made of stainless steel, and the tip thereof extends to the inside of the catalyst protective material packed layer 18. However, the material of the sample water introduction nozzle 30 is not limited, and a metal having heat resistance and oxidation resistance, an alloy, quartz glass, or the like can be used as appropriate. A predetermined amount of sample water is introduced into the sample water introduction nozzle 30 by a slide valve or syringe pump after pretreatment such as dilution, and is pumped by a pump or air and filled with a catalyst protective material from the tip of the sample water introduction nozzle 30. Introduced into layer 18. In this case, since the sample water introduction nozzle 30 extends to the inside of the catalyst protective material packed bed 18, the sample water does not scatter on the inner wall surface of the combustion tube 14, and the sample water is made of metal sample water. Since it is heated in the introduction nozzle 30, it is introduced into the catalyst protective material packed layer 18 in a vaporized state. In addition, the water quality analysis method by the combustion type water quality analyzer of this example is the same as that of the combustion type water quality analyzer of FIG.

上述した実施形態の燃焼部および試料水導入ノズルは、例えば図2に示すような構成の全有機炭素測定装置の燃焼部および試料水導入部に使用することができる。図2において、100は試料水槽、102は希釈水槽、104はIC除去液槽、106は希釈槽、108は試料水導入部、110は燃焼部、112はキャリヤガス供給手段、114は除湿器、116は検出器(NDIR)を示す。   The combustion unit and the sample water introduction nozzle of the above-described embodiment can be used for the combustion unit and the sample water introduction unit of the total organic carbon measuring device configured as shown in FIG. 2, for example. In FIG. 2, 100 is a sample water tank, 102 is a dilution water tank, 104 is an IC removal liquid tank, 106 is a dilution tank, 108 is a sample water introduction part, 110 is a combustion part, 112 is a carrier gas supply means, 114 is a dehumidifier, Reference numeral 116 denotes a detector (NDIR).

本例の全有機炭素測定装置は、希釈槽106において試料水、希釈水およびIC除去液(塩酸等)を混合し、これにより試料水を希釈するとともに、試料水中に含まれる二酸化炭素等のIC(無機体炭素)を除去した後、キャリヤガス供給手段112により燃焼部110内にキャリヤガスを流した状態で、試料水を試料水導入部108から燃焼部110内に導入する。燃焼部110内では、気化した試料水のガス中の有機物が触媒の作用により酸化され、COに変換される。その後、ガスを除湿器114を通して検出器116に導入し、ガス中のCO濃度を測定することにより、試料水中の有機体炭素濃度を求めるものである。前述した実施形態の燃焼部および試料水導入ノズルは、本例の全有機炭素測定装置の燃焼部110および試料水導入部108に使用することができる。 The total organic carbon measuring apparatus of this example mixes sample water, dilution water, and an IC removal solution (hydrochloric acid, etc.) in a dilution tank 106, thereby diluting the sample water and at the same time ICs such as carbon dioxide contained in the sample water. After removing (inorganic carbon), the sample water is introduced from the sample water introduction unit 108 into the combustion unit 110 in a state where the carrier gas is supplied into the combustion unit 110 by the carrier gas supply unit 112. In the combustion unit 110, organic substances in the vaporized sample water gas are oxidized by the action of the catalyst and converted to CO 2 . Then introduced into the detector 116 through the dehumidifier 114 of the gas, by measuring the CO 2 concentration in the gas, and requests organic carbon concentration in the sample water. The combustion section and the sample water introduction nozzle of the above-described embodiment can be used for the combustion section 110 and the sample water introduction section 108 of the total organic carbon measurement device of this example.

本発明に係る燃焼式水質分析装置の燃焼部および試料水導入ノズルの一例を示す概略図である。It is the schematic which shows an example of the combustion part of the combustion type water quality analyzer which concerns on this invention, and a sample water introduction nozzle. 全有機炭素測定装置の一例を示す概念図である。It is a conceptual diagram which shows an example of a total organic carbon measuring apparatus. 燃焼式水質分析装置の燃焼部および試料水導入ノズルの従来例を示す概略図である。It is the schematic which shows the prior art example of the combustion part of a combustion type water quality analyzer, and a sample water introduction nozzle.

符号の説明Explanation of symbols

12 燃焼部
14 燃焼管
16 触媒充填層
18 触媒保護材料充填層
20 加熱部
24 検出器
30 試料水導入ノズル
12 Combustion unit 14 Combustion tube 16 Catalyst packed layer 18 Catalyst protective material packed layer 20 Heating unit 24 Detector 30 Sample water introduction nozzle

Claims (3)

内部に触媒保護材料充填層およびその下方に触媒充填層が設けられ、内部で試料水を燃焼させる燃焼部と、試料水導入ノズルとを備え、前記試料水導入ノズルの先端から試料水を燃焼部内に導入し、この試料水を燃焼部内で燃焼させて得られるガス中の成分を測定する燃焼式水質分析装置であって、前記試料水導入ノズルの先端を前記触媒保護材料充填層に接触させたことを特徴とする燃焼式水質測定装置。   A catalyst protection material packed layer is provided inside and a catalyst packed layer is provided therebelow, and includes a combustion section for burning sample water therein and a sample water introduction nozzle, and the sample water is introduced into the combustion section from the tip of the sample water introduction nozzle. Is a combustion-type water quality analyzer that measures the components in the gas obtained by burning the sample water in the combustion section, the tip of the sample water introduction nozzle being brought into contact with the packed layer of the catalyst protection material Combustion-type water quality measuring device characterized by that. 前記試料水導入ノズルの先端を触媒保護材料充填層の内部まで延出させたことを特徴とする請求項1に記載の燃焼式水質測定装置。   The combustion type water quality measuring device according to claim 1, wherein the tip of the sample water introduction nozzle extends to the inside of the catalyst protective material packed bed. 前記試料水導入ノズルを金属で形成したことを特徴とする請求項1または2に記載の燃焼式水質測定装置。
The combustion type water quality measuring apparatus according to claim 1 or 2, wherein the sample water introduction nozzle is made of metal.
JP2006090510A 2006-03-29 2006-03-29 Combustion type water quality measuring instrument Pending JP2007263814A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2016156706A (en) * 2015-02-25 2016-09-01 国立大学法人名古屋大学 Carbon isotope analysis device and carbon isotope analysis method
JP2016156752A (en) * 2015-02-25 2016-09-01 国立大学法人名古屋大学 Carbon isotope analysis device and carbon isotope analysis method
JP2018004656A (en) * 2015-03-04 2018-01-11 国立大学法人名古屋大学 Device and method for analyzing carbon isotopes
CN110508546A (en) * 2019-10-10 2019-11-29 攀钢集团攀枝花钢铁研究院有限公司 Detection probe or electrode stem cleaning device

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2016156706A (en) * 2015-02-25 2016-09-01 国立大学法人名古屋大学 Carbon isotope analysis device and carbon isotope analysis method
JP2016156752A (en) * 2015-02-25 2016-09-01 国立大学法人名古屋大学 Carbon isotope analysis device and carbon isotope analysis method
JP2018004656A (en) * 2015-03-04 2018-01-11 国立大学法人名古屋大学 Device and method for analyzing carbon isotopes
CN110508546A (en) * 2019-10-10 2019-11-29 攀钢集团攀枝花钢铁研究院有限公司 Detection probe or electrode stem cleaning device

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