JP7303513B2 - Hydrogen peroxide concentration detector - Google Patents

Hydrogen peroxide concentration detector Download PDF

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JP7303513B2
JP7303513B2 JP2019214250A JP2019214250A JP7303513B2 JP 7303513 B2 JP7303513 B2 JP 7303513B2 JP 2019214250 A JP2019214250 A JP 2019214250A JP 2019214250 A JP2019214250 A JP 2019214250A JP 7303513 B2 JP7303513 B2 JP 7303513B2
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hydrogen peroxide
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platinum
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貴治 大神田
聡樹 平方
哲也 山本
宏昭 松浦
千尋 島村
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Fuji Electric Co Ltd
Chikoji Gakuen Educational Foundation
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Description

本発明は、過酸化水素濃度検出装置に関するものである。 The present invention relates to a hydrogen peroxide concentration detection device .

従来、過酸化水素の濃度検出を行う装置（過酸化水素濃度検出装置）が特許文献１に提案されている。この特許文献１に提案されている過酸化水素濃度検出装置では、過酸化水素を含有する電解質溶液に浸漬された複数の電極に電圧を印加させることにより、一部の電極にて下記式（１）に示されるような過酸化水素の酸化反応を発生させる。そして、かかる過酸化水素濃度検出装置では、上記酸化反応の酸化電流値を計測して過酸化水素の濃度検出を行っている。 Conventionally, Patent Document 1 proposes a device for detecting the concentration of hydrogen peroxide (hydrogen peroxide concentration detection device). In the hydrogen peroxide concentration detection device proposed in Patent Document 1, by applying a voltage to a plurality of electrodes immersed in an electrolyte solution containing hydrogen peroxide, some of the electrodes are immersed in the following formula (1 ) to generate an oxidation reaction of hydrogen peroxide as shown in FIG. In such a hydrogen peroxide concentration detection device, the concentration of hydrogen peroxide is detected by measuring the oxidation current value of the oxidation reaction.

式（１） Ｈ２Ｏ２→２Ｈ＋＋Ｏ２＋２ｅ－ Formula (1) H 2 O 2 →2H + +O 2 +2e −

特開平９－１２７０５３号公報JP-A-9-127053

ところで、上記過酸化水素濃度検出装置では、一部の電極で過酸化水素の酸化反応を発生させて該酸化反応の酸化電流値を計測しているので、該電極での電流値が比較的高いものとなり、該電極を構成する触媒の劣化の早期化を招来し、結果的に、使用寿命の低減化を招いていた。 By the way, in the above-described hydrogen peroxide concentration detection device, the oxidation reaction of hydrogen peroxide is generated at some electrodes and the oxidation current value of the oxidation reaction is measured, so the current value at the electrodes is relatively high. As a result, the deterioration of the catalyst constituting the electrode is accelerated, and as a result, the service life is shortened.

本発明は、上記実情に鑑みて、使用寿命の長大化を図ることができる過酸化水素濃度検出装置を提供することを目的とする。 SUMMARY OF THE INVENTION It is an object of the present invention to provide a hydrogen peroxide concentration detection device capable of extending the service life.

上記目的を達成するために、本発明に係る過酸化水素濃度検出装置は、過酸化水素を含有する溶液に少なくとも一部が浸漬された作用極を備え、前記作用極に電圧を印加させて該作用極の電解反応の電流値を計測することにより、過酸化水素の濃度検出を行う装置であって、前記作用極は、表面に白金原子を有する触媒金属がコーティングされて構成され、前記作用極に０．９Ｖ以下の電圧を印加させて前記過酸化水素の還元反応を発生させ、該還元反応の還元電流値を計測して過酸化水素の濃度検出を行うことを特徴とする。 In order to achieve the above object, a hydrogen peroxide concentration detection device according to the present invention comprises a working electrode at least partially immersed in a solution containing hydrogen peroxide, and a voltage is applied to the working electrode to A device for detecting the concentration of hydrogen peroxide by measuring the current value of the electrolytic reaction of the working electrode, wherein the working electrode is coated with a catalyst metal having platinum atoms on the surface, and the working electrode is is applied with a voltage of 0.9 V or less to generate a reduction reaction of the hydrogen peroxide, and the reduction current value of the reduction reaction is measured to detect the concentration of the hydrogen peroxide.

また本発明は、上記過酸化水素濃度検出装置において、前記作用極の触媒金属は、白金原子、白金黒、白金担持カーボン、白金合金、窒素含有炭素電析白金の少なくとも１つを含有することを特徴とする。 Further, according to the present invention, in the hydrogen peroxide concentration detection device described above, the catalyst metal of the working electrode contains at least one of platinum atoms, platinum black, platinum-carrying carbon, platinum alloy, and nitrogen-containing carbon-electrodeposited platinum. Characterized by

また本発明は、上記過酸化水素濃度検出装置において、前記作用極に０．２～０．９Ｖの電圧を印加させることを特徴とする。 Further, according to the present invention, in the hydrogen peroxide concentration detection device, a voltage of 0.2 to 0.9 V is applied to the working electrode.

また、本発明に係る過酸化水素濃度検出方法は、過酸化水素を含有する溶液に少なくとも一部が浸漬された作用極に対して、電圧を印加させて該作用極の電解反応の電流値を計測することにより、過酸化水素の濃度検出を行う方法であって、表面に白金原子を有する触媒金属がコーティングされて構成された作用極に対して、０．９Ｖ以下の電圧を印加させて前記過酸化水素の還元反応を発生させ、該還元反応の還元電流値を計測して過酸化水素の濃度検出を行う工程を含むことを特徴とする。 Further, in the hydrogen peroxide concentration detection method according to the present invention, a voltage is applied to a working electrode at least partially immersed in a solution containing hydrogen peroxide, and the current value of the electrolytic reaction of the working electrode is measured. A method for detecting the concentration of hydrogen peroxide by measuring the The method is characterized by including a step of generating a reduction reaction of hydrogen peroxide and measuring a reduction current value of the reduction reaction to detect the concentration of hydrogen peroxide.

本発明によれば、表面に白金原子を有する触媒金属がコーティングされて構成された作用極に０．９Ｖ以下の電圧を印加させて過酸化水素の還元反応を発生させ、該還元反応の還元電流値を計測して過酸化水素の濃度検出を行うので、作用極での電位を相対的に低減させることができる。これにより、作用極を構成する触媒の経年劣化を抑制させることができ、使用寿命の長大化を図ることができるという効果を奏する。 According to the present invention, a reduction reaction of hydrogen peroxide is generated by applying a voltage of 0.9 V or less to a working electrode having a surface coated with a catalyst metal having platinum atoms, and a reduction current of the reduction reaction is generated. Since the concentration of hydrogen peroxide is detected by measuring the value, the potential at the working electrode can be relatively reduced. As a result, it is possible to suppress deterioration over time of the catalyst that constitutes the working electrode, and it is possible to extend the service life of the catalyst.

また本発明によれば、表面に白金原子を有する触媒金属がコーティングされて構成された作用極に対して、０．９Ｖ以下の電圧を印加させて前記過酸化水素の還元反応を発生させ、該還元反応の還元電流値を計測して過酸化水素の濃度検出を行う工程を含むので、作用極での電位を相対的に低減させることができる。これにより、作用極を構成する触媒の経年劣化を抑制させることができ、使用寿命の長大化を図ることができるという効果を奏する。 Further, according to the present invention, a voltage of 0.9 V or less is applied to the working electrode, the surface of which is coated with a catalyst metal having platinum atoms, to cause the reduction reaction of the hydrogen peroxide. Since the method includes the step of detecting the concentration of hydrogen peroxide by measuring the reduction current value of the reduction reaction, the potential at the working electrode can be relatively reduced. As a result, it is possible to suppress deterioration over time of the catalyst that constitutes the working electrode, and it is possible to extend the service life of the catalyst.

図１は、本発明の実施の形態である過酸化水素濃度検出装置の構成を模式的に示す模式図である。FIG. 1 is a schematic diagram schematically showing the configuration of a hydrogen peroxide concentration detection device that is an embodiment of the present invention. 図２は、図１に示した作用極の構成を模式的に示す断面図である。2 is a cross-sectional view schematically showing the configuration of the working electrode shown in FIG. 1. FIG. 図３は、実施例１、比較例１及び比較例２の作用極での電解電流値を示す図表である。FIG. 3 is a chart showing electrolysis current values in the working electrodes of Example 1, Comparative Examples 1 and 2;

以下に添付図面を参照して、本発明に係る過酸化水素濃度検出装置の好適な実施の形態について詳細に説明する。 Preferred embodiments of the hydrogen peroxide concentration detection device according to the present invention will be described in detail below with reference to the accompanying drawings.

図１は、本発明の実施の形態である過酸化水素濃度検出装置の構成を模式的に示す模式図である。ここで例示する過酸化水素濃度検出装置１は、反応容器１０を備えている。 FIG. 1 is a schematic diagram schematically showing the configuration of a hydrogen peroxide concentration detection device that is an embodiment of the present invention. The hydrogen peroxide concentration detection device 1 exemplified here includes a reaction vessel 10 .

反応容器１０は、上面が開口した箱状の形態を成し、電解質溶液１１が貯留されている。電解質溶液１１は、希硫酸に過酸化水素水を添加して構成され、過酸化水素を含有するものである。このような反応容器１０の電解質溶液１１には、外部電源装置２０にリード線Ｒを通じて電気的に接続された作用極２１及び対極２２がそれぞれ一部が浸漬された状態で配置されている。 The reaction container 10 has a box-like shape with an open top, and stores an electrolyte solution 11 . The electrolyte solution 11 is formed by adding hydrogen peroxide solution to dilute sulfuric acid, and contains hydrogen peroxide. A working electrode 21 and a counter electrode 22 electrically connected to an external power source 20 through a lead wire R are partially immersed in the electrolyte solution 11 of the reaction vessel 10 .

作用極２１は、図２に示すように、電極基材２１１及び触媒金属２１２を備えている。電極基材２１１は、例えばガラス状炭素（グラッシーカーボン）や金等の過酸化水素と反応しない金属により構成されている。触媒金属２１２は、作用極２１の表面を構成し、電極基材２１１の下面にコーティングされている。この触媒金属２１２は、白金原子を有するものであり、より詳細には、白金原子、白金黒、白金担持カーボン、白金合金、窒素含有炭素電析白金の少なくとも１つを含有することが好ましい。尚、図２中の符号２１３は、リード線Ｒを被覆する樹脂である。対極２２は、図には明示しないが、例えば銅により構成される棒状体に白金からなるワイヤー状物が巻回して構成されている。 The working electrode 21 includes an electrode base material 211 and a catalyst metal 212, as shown in FIG. The electrode base material 211 is made of metal such as glassy carbon or gold that does not react with hydrogen peroxide. The catalytic metal 212 constitutes the surface of the working electrode 21 and is coated on the lower surface of the electrode substrate 211 . This catalyst metal 212 contains platinum atoms, and more specifically, preferably contains at least one of platinum atoms, platinum black, platinum-carrying carbon, platinum alloys, and nitrogen-containing carbon-electrodeposited platinum. Reference numeral 213 in FIG. 2 denotes a resin covering the lead wire R. As shown in FIG. Although not shown, the counter electrode 22 is formed by winding a platinum wire around a rod made of copper, for example.

外部電源装置２０は、例えばポテンショスタットにより構成されており、作用極２１の電気化学反応を制御して、その電位・電流を測定するものである。より詳細に説明すると、外部電源装置２０は、作用極２１と対極２２との２電極間に０．９Ｖ以下の電圧を印加し、作用極２１と、電解質溶液１１に浸漬された参照極２３との間の電位が所望の電位になるように制御するものである。この外部電源装置２０による測定結果等は、電気的に接続された上位機器３０に送出される。 The external power supply device 20 is composed of, for example, a potentiostat, controls the electrochemical reaction of the working electrode 21, and measures its potential and current. More specifically, the external power supply device 20 applies a voltage of 0.9 V or less between the working electrode 21 and the counter electrode 22 to separate the working electrode 21 and the reference electrode 23 immersed in the electrolyte solution 11. is controlled so that the potential between is a desired potential. The measurement results and the like by the external power supply device 20 are sent to the electrically connected host device 30 .

以上のような構成を有する過酸化水素濃度検出装置１の動作について説明する。 The operation of the hydrogen peroxide concentration detection device 1 having the configuration as described above will be described.

上位機器３０から与えられる指令に応じて、外部電源装置２０は、作用極２１と対極２２との２電極間に０．９Ｖ以下の電圧を印加し、作用極２１と参照極２３との間の電位が所望の電位になるように制御する。これにより、作用極２１では下記式（２）の還元反応が発生し、対極２２では下記式（３）の水の電気分解反応が発生する。 In response to a command given from the host device 30, the external power supply device 20 applies a voltage of 0.9 V or less between the two electrodes, the working electrode 21 and the counter electrode 22, and the voltage between the working electrode 21 and the reference electrode 23. The potential is controlled to a desired potential. As a result, the reduction reaction of formula (2) below occurs at the working electrode 21 , and the electrolysis reaction of water of formula (3) below occurs at the counter electrode 22 .

式（２） Ｈ２Ｏ２＋２Ｈ＋＋２ｅ－→２Ｈ２Ｏ
式（３） Ｈ２Ｏ→１／２Ｏ２＋２Ｈ＋＋２ｅ－ Formula (2) H 2 O 2 +2H + +2e − →2H 2 O
Formula (3) H 2 O→1/2O 2 +2H + +2e −

つまり、上記過酸化水素濃度検出装置１においては、作用極２１にて過酸化水素の還元反応を発生させ、該還元反応の還元電流値を計測して過酸化水素の濃度検出を行うことになる。 In other words, in the hydrogen peroxide concentration detection device 1, the reduction reaction of hydrogen peroxide is generated at the working electrode 21, and the reduction current value of the reduction reaction is measured to detect the concentration of hydrogen peroxide. .

すなわち、本発明の実施の形態である過酸化水素濃度検出方法においては、上記作用極２１に対して、０．９Ｖ以下の電圧を印加させて過酸化水素の還元反応を発生させ、該還元反応の還元電流値を計測して過酸化水素の濃度検出を行う工程を含んでいる。 That is, in the hydrogen peroxide concentration detection method according to the embodiment of the present invention, a voltage of 0.9 V or less is applied to the working electrode 21 to cause a reduction reaction of hydrogen peroxide, and the reduction reaction and detecting the concentration of hydrogen peroxide by measuring the reduction current value.

よって、上記過酸化水素濃度検出装置１によれば、作用極２１にて発生させた過酸化水素の還元反応の還元電流値を計測して該過酸化水素の濃度検出を行うので、従来のように過酸化水素の酸化反応を発生させてその酸化電流値を計測することに比して、作用極２１での電位を相対的に低減させることができる。これにより、作用極２１を構成する触媒の経年劣化を抑制させることができ、使用寿命の長大化を図ることができる。 Therefore, according to the hydrogen peroxide concentration detection device 1, the concentration of hydrogen peroxide is detected by measuring the reduction current value of the reduction reaction of hydrogen peroxide generated at the working electrode 21. The potential at the working electrode 21 can be relatively reduced compared to the case where the oxidation reaction of hydrogen peroxide is generated in the first step and the oxidation current value is measured. As a result, deterioration over time of the catalyst that constitutes the working electrode 21 can be suppressed, and the service life can be extended.

次に、本発明に係る過酸化水素濃度検出装置１の実施例について説明する。 Next, an embodiment of the hydrogen peroxide concentration detection device 1 according to the present invention will be described.

＜実施例１＞
作用極２１は、電極基材２１１としてグラッシーカーボンを用い、触媒金属２１２として白金黒触媒（株式会社徳力本店製）を用いた。この作用極２１を、１Ｎの希硫酸に１ｍｍｏｌ／Ｌの過酸化水素を添加した電解質溶液１１に浸漬させ、外部電源装置２０により０．６Ｖの電圧を印加させた。これによる電解電流値（ｍＡ）を図３に示した。 <Example 1>
The working electrode 21 used glassy carbon as the electrode base material 211 and platinum black catalyst (manufactured by Tokuriki Honten Co., Ltd.) as the catalyst metal 212 . This working electrode 21 was immersed in the electrolyte solution 11 in which 1 mmol/L of hydrogen peroxide was added to 1N dilute sulfuric acid, and a voltage of 0.6 V was applied by the external power supply device 20 . Electrolytic current values (mA) resulting from this are shown in FIG.

＜比較例１＞
作用極は、電極基材としてグラッシーカーボンを用い、触媒金属として白金触媒（株式会社徳力本店製）を用いた。この作用極を、１Ｎの希硫酸に１ｍｍｏｌ／Ｌの過酸化水素を添加した電解質溶液に浸漬させ、外部電源装置により１．０Ｖの電圧を印加させた。これによる電解電流値（ｍＡ）を図３に示した。 <Comparative Example 1>
For the working electrode, glassy carbon was used as the electrode base material, and platinum catalyst (manufactured by Tokuriki Honten Co., Ltd.) was used as the catalyst metal. This working electrode was immersed in an electrolyte solution prepared by adding 1 mmol/L hydrogen peroxide to 1N dilute sulfuric acid, and a voltage of 1.0 V was applied by an external power supply device. Electrolytic current values (mA) resulting from this are shown in FIG.

＜比較例２＞
作用極は、電極基材としてグラッシーカーボンを用い、触媒金属として二酸化イリジウム触媒（株式会社徳力本店製）を用いた。この作用極を、１Ｎの希硫酸に１ｍｍｏｌ／Ｌの過酸化水素を添加した電解質溶液に浸漬させ、外部電源装置により１．０Ｖの電圧を印加させた。これによる電解電流値（ｍＡ）を図３に示した。 <Comparative Example 2>
For the working electrode, glassy carbon was used as the electrode base material, and iridium dioxide catalyst (manufactured by Tokuriki Honten Co., Ltd.) was used as the catalyst metal. This working electrode was immersed in an electrolyte solution prepared by adding 1 mmol/L hydrogen peroxide to 1N dilute sulfuric acid, and a voltage of 1.0 V was applied by an external power supply device. Electrolytic current values (mA) resulting from this are shown in FIG.

図３に示したように、実施例１では電解電流値が－０．３９ｍＡであり、比較例１では電解電流値が０．１６ｍＡであり、比較例２では電解電流値が０．００ｍＡであった。つまり、比較例２では、過酸化水素の電解反応が示されずに電流が流れなかった。比較例１では、作用極で過酸化水素の酸化反応（上記式（１）参照）が発生し、その酸化電流値が示された。一方、実施例１では、作用極２１で過酸化水素の還元反応（上記式（２）参照）が発生し、その還元電流値が示された。 As shown in FIG. 3, in Example 1, the electrolysis current value was −0.39 mA, in Comparative Example 1, the electrolysis current value was 0.16 mA, and in Comparative Example 2, the electrolysis current value was 0.00 mA. rice field. In other words, in Comparative Example 2, no electrolysis reaction of hydrogen peroxide was observed and no current flowed. In Comparative Example 1, the oxidation reaction of hydrogen peroxide (see formula (1) above) occurred at the working electrode, and the oxidation current value was shown. On the other hand, in Example 1, the reduction reaction of hydrogen peroxide (see formula (2) above) occurred at the working electrode 21, and the reduction current value was shown.

従って、作用極２１に対する印加電圧を０．９Ｖ以下にしつつ、作用極２１を構成する触媒金属２１２が白金原子を含むものにすることにより、作用極２１において過酸化水素の還元反応を発生させることができ、その還元電流値で過酸化水素の濃度検出を行うことができる。よって、作用極２１での電位を相対的に低減させることができることが明らかである。 Therefore, by setting the voltage applied to the working electrode 21 to 0.9 V or less and making the catalytic metal 212 constituting the working electrode 21 contain platinum atoms, the reduction reaction of hydrogen peroxide can be generated at the working electrode 21. , and the concentration of hydrogen peroxide can be detected based on the reduction current value. Therefore, it is clear that the potential at the working electrode 21 can be relatively reduced.

以上、本発明の好適な実施の形態について説明したが、かかる実施の形態で図示した各構成は概略的なものであり、必ずしも物理的に図示の構成をされていることを要しない。すなわち、各構成要素の分散・統合の形態は図示のものに限られず、その全部又は一部を各種の使用状況等に応じて、任意の単位で機能的又は物理的に分散・統合して構成することができる。 Although the preferred embodiments of the present invention have been described above, each configuration illustrated in these embodiments is schematic, and does not necessarily need to be physically configured as illustrated. In other words, the form of dispersion/integration of each component is not limited to the one shown in the figure, and all or part of it is functionally or physically distributed/integrated in arbitrary units according to various usage conditions. can do.

１…過酸化水素濃度検出装置、１０…反応容器、１１…電解質溶液、２０…外部電源装置、２１…作用極、２１１…電極基材、２１２…触媒金属、２１３…樹脂、２２…対極、２３…参照極、３０…上位機器、Ｒ…リード線。 DESCRIPTION OF SYMBOLS 1... Hydrogen peroxide concentration detection apparatus 10... Reaction container 11... Electrolyte solution 20... External power supply device 21... Working electrode 211... Electrode base material 212... Catalyst metal 213... Resin 22... Counter electrode 23 ... reference electrode, 30 ... host device, R ... lead wire.

Claims (3)

過酸化水素を含有する溶液に少なくとも一部が浸漬された作用極を備え、前記作用極に電圧を印加させて該作用極の電解反応の電流値を計測することにより、過酸化水素の濃度検出を行う装置であって、
前記作用極は、
過酸化水素と反応しない金属により構成された電極基材と、
前記電極基材の下面にコーティングされることで表面を構成し、かつ白金原子を有する触媒金属と、
前記触媒金属のみが露出される態様で、前記電極基材及び該電極基材に接続されたリード線を被覆する樹脂と
により構成され、
前記作用極に０．９Ｖ以下の電圧を印加させて前記過酸化水素の還元反応を発生させ、該還元反応の還元電流値を計測して過酸化水素の濃度検出を行うことを特徴とする過酸化水素濃度検出装置。 A concentration of hydrogen peroxide is detected by providing a working electrode at least partially immersed in a solution containing hydrogen peroxide, applying a voltage to the working electrode, and measuring the current value of the electrolytic reaction of the working electrode. A device for performing
The working electrode is
an electrode base made of a metal that does not react with hydrogen peroxide;
a catalyst metal that constitutes the surface by being coated on the lower surface of the electrode substrate and has platinum atoms;
a resin covering the electrode substrate and lead wires connected to the electrode substrate in such a manner that only the catalyst metal is exposed;
is composed of
A hydrogen peroxide concentration is detected by applying a voltage of 0.9 V or less to the working electrode to cause a reduction reaction of the hydrogen peroxide, and measuring a reduction current value of the reduction reaction. Hydrogen oxide concentration detector. 前記作用極の触媒金属は、白金原子、白金黒、白金担持カーボン、白金合金、窒素含有炭素電析白金の少なくとも１つを含有することを特徴とする請求項１に記載の過酸化水素濃度検出装置。 2. The hydrogen peroxide concentration detection according to claim 1, wherein the catalyst metal of the working electrode contains at least one of platinum atoms, platinum black, platinum-carrying carbon, platinum alloy, and nitrogen-containing carbon-electrodeposited platinum. Device. 前記作用極に０．２～０．９Ｖの電圧を印加させることを特徴とする請求項１又は請求項２に記載の過酸化水素濃度検出装置。 3. The hydrogen peroxide concentration detection device according to claim 1, wherein a voltage of 0.2 to 0.9 V is applied to said working electrode.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001013102A (en) 1999-06-30 2001-01-19 Ricoh Kyosan Inc Fractionately measuring method for peracetic acid and hydrogen peroxide
JP2010185136A (en) 2009-01-16 2010-08-26 Institute Of National Colleges Of Technology Japan Catalyst for decomposing hydrogen peroxide, storage method thereof and method for decomposing hydrogen peroxide

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JPS55146035A (en) * 1980-04-07 1980-11-14 Mitsubishi Gas Chem Co Inc Measuring method of concentration of hydrogen peroxide

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001013102A (en) 1999-06-30 2001-01-19 Ricoh Kyosan Inc Fractionately measuring method for peracetic acid and hydrogen peroxide
JP2010185136A (en) 2009-01-16 2010-08-26 Institute Of National Colleges Of Technology Japan Catalyst for decomposing hydrogen peroxide, storage method thereof and method for decomposing hydrogen peroxide

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