JPH02296143A - Method for measuring dissolved chlorine dioxide - Google Patents
Method for measuring dissolved chlorine dioxideInfo
- Publication number
- JPH02296143A JPH02296143A JP1116288A JP11628889A JPH02296143A JP H02296143 A JPH02296143 A JP H02296143A JP 1116288 A JP1116288 A JP 1116288A JP 11628889 A JP11628889 A JP 11628889A JP H02296143 A JPH02296143 A JP H02296143A
- Authority
- JP
- Japan
- Prior art keywords
- electrode
- chlorine dioxide
- electrodes
- current
- working electrode
- 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.)
- Granted
Links
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000004155 Chlorine dioxide Substances 0.000 title claims abstract description 29
- 235000019398 chlorine dioxide Nutrition 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 4
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 4
- 239000012488 sample solution Substances 0.000 claims description 17
- 239000010931 gold Substances 0.000 claims description 6
- 229910052709 silver Inorganic materials 0.000 claims description 5
- 239000004332 silver Substances 0.000 claims description 5
- 229910052737 gold Inorganic materials 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910021607 Silver chloride Inorganic materials 0.000 claims 1
- 229910021397 glassy carbon Inorganic materials 0.000 claims 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 11
- 238000005259 measurement Methods 0.000 abstract description 10
- 239000003792 electrolyte Substances 0.000 abstract description 7
- 238000005868 electrolysis reaction Methods 0.000 abstract description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052801 chlorine Inorganic materials 0.000 abstract description 3
- 239000000460 chlorine Substances 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
- 229910052740 iodine Inorganic materials 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 230000009182 swimming Effects 0.000 description 2
- 239000008399 tap water Substances 0.000 description 2
- 235000020679 tap water Nutrition 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 239000011324 bead Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野〕
本発明は、試料液中に溶存している二酸化塩素（ａｔＯ
）を連続的に測定する方法に関する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention is directed to the treatment of chlorine dioxide (atO
).
従来から上水やプールの殺菌に塩素が使用されているが
、塩素から発癌性のトリハロメタンが生成することが判
り問題となっている。Chlorine has traditionally been used to disinfect tap water and swimming pools, but it has become a problem as it has been found that chlorine produces carcinogenic trihalomethanes.
そこで最近では、トリハロメタンを生成しない二酸化塩
素による上水やプールの殺菌が検討されている。又、二
酸化塩素は強い酸化力を有するので、繊維の漂白にも利
用されている。Therefore, recently, sterilization of tap water and swimming pools using chlorine dioxide, which does not produce trihalomethane, is being considered. In addition, since chlorine dioxide has strong oxidizing power, it is also used for bleaching textiles.
従って、これらの分野においては、液中に溶解した二酸
化塩素の濃度を適切に管理することが極めて重要である
。Therefore, in these fields, it is extremely important to appropriately control the concentration of chlorine dioxide dissolved in the liquid.
一方、溶存二酸化塩素の測定法としては、ヨウ素滴定法
（化学防災指針（７））と、隔膜形ポーラログラフ電極
法（特開昭５４−１２５０９５号公報）が知られている
。On the other hand, as methods for measuring dissolved chlorine dioxide, the iodine titration method (Chemical Disaster Prevention Guidelines (7)) and the diaphragm polarographic electrode method (Japanese Patent Laid-Open No. 125095/1982) are known.
しかしながら、上記のヨウ素滴定法は間欠測定であって
、連続的な濃彦管理には不適当である。However, the above-mentioned iodine titration method is an intermittent measurement, and is not suitable for continuous control.
隔膜形ポーラログラフ電極法は連続測定が可能であるが
、試料液の他に電解液を必要とするため、電極反応の進
行に伴なって電解液の消耗が起るので、電解液の補充や
交換の必要から連続使用出来る期間に限界があった。The diaphragm polarographic electrode method allows continuous measurement, but since it requires an electrolyte in addition to the sample solution, the electrolyte is consumed as the electrode reaction progresses, so it is difficult to replenish or replace the electrolyte. There was a limit to how long it could be used continuously due to the need for
本発明はかかる従来の事情に鑑み、連続測定が可能であ
り、補充や交換の必要がある特別な電解液などを用いる
ことのない、溶存二酸化塩素の測定方法を提供すること
を目的とする。In view of the conventional circumstances, it is an object of the present invention to provide a method for measuring dissolved chlorine dioxide, which allows continuous measurement and does not require the use of a special electrolytic solution that requires replenishment or replacement.
（課題を解決するための手段）
上記目的を達成するため、本発明の溶存二酸化塩素の測
定方法では、試料液中に作用電極と対極の２極又は作用
電極と参照電極と対極の３極を浸漬し、貴金属又は炭素
からなる作用電極を試料液に対し相対的に動かしながら
、２極の場合は対極を基準に又３極の場合は参照電極を
基準にして溶存二酸化塩素の還元電流を生じる電圧を作
用′ｒｔ極に印加して発生する還元電流を測定するか、
又は作用電極と対極の短絡電流を測定して試料液中の二
酸化塩素濃度を求めることを特徴とする。(Means for Solving the Problems) In order to achieve the above object, in the method for measuring dissolved chlorine dioxide of the present invention, two electrodes, a working electrode and a counter electrode, or three electrodes, a working electrode, a reference electrode and a counter electrode, are provided in the sample solution. While moving the working electrode made of noble metal or carbon relative to the sample solution, a reduction current of dissolved chlorine dioxide is generated based on the counter electrode in the case of two electrodes or the reference electrode in the case of three electrodes. Apply a voltage to the working 'rt electrode and measure the resulting reduction current, or
Alternatively, the short circuit current between the working electrode and the counter electrode is measured to determine the chlorine dioxide concentration in the sample solution.
（作用）
本発明は、試料液中の溶存二酸化塩素が印加電圧の如何
によっては電解され、電解電流を発生するとの発見に基
づきなされたものである。(Function) The present invention was made based on the discovery that dissolved chlorine dioxide in a sample solution is electrolyzed depending on the applied voltage and generates an electrolytic current.
即ち、本発明方法は試料液自体を電解液として直接電解
し、二酸化塩素の電解により発生する電流を測定するも
のであって、二酸化塩素の電解の場合には還元電流が発
生する。That is, the method of the present invention directly electrolyzes the sample solution itself as an electrolyte and measures the current generated by electrolysis of chlorine dioxide, and in the case of electrolysis of chlorine dioxide, a reduction current is generated.
この還元電流は試料液中に溶存する二酸化塩素の濃度に
比例するので、溶存二酸化塩緊濃度と還元電流の値との
関係を予め求めておけば、供給した試料液における還元
電流を測定することによって溶存二酸化塩素の濃度を知
ることが出来る。Since this reduction current is proportional to the concentration of chlorine dioxide dissolved in the sample solution, it is possible to measure the reduction current in the supplied sample solution by determining the relationship between the dissolved salt dioxide concentration and the reduction current value in advance. The concentration of dissolved chlorine dioxide can be determined by
本発明方法は上記の如く電解を利用した方法であるから
、長期間測定を続けると作用電極の表面に酸化物の生成
による汚れが付着して発生電流値の低下をもたらすので
、このような場合には作用電極表面をブラシやガラスピ
ーズ等でこすって、新しい表面を保つようにする必要が
ある。Since the method of the present invention utilizes electrolysis as described above, if measurements are continued for a long period of time, dirt due to the formation of oxides will adhere to the surface of the working electrode, resulting in a decrease in the generated current value. It is necessary to scrub the surface of the working electrode with a brush or glass beads to keep it fresh.
本発明方法を実施するための測定装置の具体例を第１図
及び第４図から第６図に示した。A specific example of a measuring device for implementing the method of the present invention is shown in FIG. 1 and FIGS. 4 to 6.
第１図は測定槽１に供給される試料液２に作用１極３と
対極４を浸漬した２極による測定装置であり、作用電極
３を回転させることにより試料液２に対して動かしなが
ら、作用電極３に印加した電圧により発生する還元電流
を電流計６でＮＯ定するようになっている。第４図は対
極４として市販の参照電極を用いた２極による測定装置
である。FIG. 1 shows a two-pole measuring device in which a working electrode 3 and a counter electrode 4 are immersed in a sample liquid 2 supplied to a measuring tank 1. While moving the working electrode 3 relative to the sample liquid 2 by rotating the working electrode 3, The reduction current generated by the voltage applied to the working electrode 3 is determined by an ammeter 6. FIG. 4 shows a two-pole measuring device using a commercially available reference electrode as the counter electrode 4.
第５図は電流を流す電極と電位を規制する電極を分離し
た３極による測定装置の例であり、通常は電位を規制す
る′ＦＬ極として市販の参照電極５を使用し且つ電流を
流す作用ｉ極３には貴金属を使用する。又、第５図の測
定装置では、電圧の印加と発生する還元電流の測定をポ
テンショスタット７を用いて行なっている。更に、第６
図は第１図と同様の２極による測定装置であるが、作用
電極３と試料液２との相対的な動きをスターラーによる
試料液２の攪拌により得る例であり、回転するスターラ
ーバ−８を作用電極３に接触させることにより、作用電
極３の表面を常時こすって新しい表面を保つようにした
ものである。Figure 5 is an example of a three-electrode measurement device in which the electrode for flowing current and the electrode for regulating potential are separated.Usually, a commercially available reference electrode 5 is used as the 'FL pole for regulating potential, and the current flows. A noble metal is used for the i-pole 3. Further, in the measuring device shown in FIG. 5, a potentiostat 7 is used to apply voltage and measure the generated reduction current. Furthermore, the sixth
The figure shows a measuring device with two poles similar to that in Figure 1, but this is an example in which the relative movement between the working electrode 3 and the sample liquid 2 is obtained by stirring the sample liquid 2 with a stirrer, and a rotating stirrer bar 8 is used. By bringing it into contact with the working electrode 3, the surface of the working electrode 3 is constantly rubbed to maintain a fresh surface.
第１図の測定装置において、作用電極３として金（Ａｕ
） 、白金（Ｐｔ）又はブラシシーカーボン（ＧＣりを
用い、及び対極４として銀又は銀／環化銀（ＡｇＯ／）
を使用して、約５ ｐｐｍの溶存二酸化塩素を含む試料
液（ｐ Ｈ６）に対して作用ｉ！＃ｉｉ３への印加電圧
を変化させた場合の加電圧電流特性を第２図に示した。In the measuring device of FIG. 1, the working electrode 3 is made of gold (Au).
), platinum (Pt) or brushy carbon (GC), and silver or silver/silver cyclide (AgO/) as the counter electrode 4.
was used to act on a sample solution (pH 6) containing approximately 5 ppm of dissolved chlorine dioxide. FIG. 2 shows the applied voltage and current characteristics when the applied voltage to #ii3 was changed.
この場合、作用電極の種類により多少異なるが印加電圧
が＋０．５ｖよりも小さくなると拡散律速に基づく安定
した還元電流が発生し、特に作用電極３がＡｕ又はＱＣ
の場合には印加電圧子０．４Ｖ〜−〇、４ｖの範囲で二
酸化塩素の安定した還元電流が発生し残余電流も小さい
ことが判る。In this case, although it differs somewhat depending on the type of working electrode, when the applied voltage becomes smaller than +0.5V, a stable reduction current based on diffusion control is generated, especially when the working electrode 3 is made of Au or QC.
In the case of , it can be seen that a stable reduction current of chlorine dioxide occurs in the applied voltage range of 0.4 V to -0.4 V, and the residual current is small.
作用電極３と対極、４による２極の測定の場合、両者の
短絡電流を測定しても良く、この場合は第２図における
印加電圧ゼロと同じ意味である。In the case of two-pole measurement using the working electrode 3 and the counter electrode 4, the short-circuit current between both may be measured, and in this case, the meaning is the same as the applied voltage of zero in FIG. 2.
又、第３図は、上記と同じ測定装置と試料液で印加電圧
を＋０．２５Ｖに設定し、試料液のｐＨを変化させた場
合の電流変化を示す。作用ｉＩＥ極としてｐｔを用いた
場合には残余電流や還元電流が大きく変動し、ｐＨの影
響が大きいことが判る。一方、作用電極としてＡｕ又は
ａＣを用いるとｐＨの影響が少ないことが判り、安定し
て精度のよい測定が出来るので好ましい。尚、作用電極
にＡｕ又はａＣを使用した場合でもｐＨの影響を無視で
きないので、試料液のｐＨが変動する場合にはｐＨを測
定し、測定値を補正することが測定精度を上げるうえで
望ましい。Moreover, FIG. 3 shows the current change when the applied voltage is set to +0.25 V using the same measuring device and sample liquid as described above, and the pH of the sample liquid is changed. It can be seen that when PT is used as the working iIE electrode, the residual current and reduction current fluctuate greatly, indicating that the influence of pH is large. On the other hand, it has been found that the use of Au or aC as the working electrode is less affected by pH and allows for stable and accurate measurements, which is preferable. Note that even when Au or aC is used for the working electrode, the influence of pH cannot be ignored, so it is desirable to measure the pH and correct the measured value when the pH of the sample solution fluctuates in order to improve measurement accuracy. .
本発明によれば、二酸化塩素の溶解した試料液自体を電
解液として電解電流を測定するので、補充や交換が必要
な特別な電解液などを要せず、従って長期間に亘る連続
測定が可能な溶存二酸化塩素の測定方法を提供すること
が出来る。According to the present invention, since the electrolytic current is measured using the sample solution in which chlorine dioxide is dissolved as an electrolyte, there is no need for a special electrolyte that needs to be replenished or replaced, and therefore continuous measurement over a long period of time is possible. A method for measuring dissolved chlorine dioxide can be provided.
第１図は本発明方法の実施に用いる測定装置の一例を示
す概略の断面図であり、第２図は一定濃度の溶存二酸化
塩素を含む試料液の加電圧電流特性を示すグラフであり
、第３図は同じ試料液での還元電流及び残余電流とｐＨ
の関係を示すグラフである。第４図から第６図は本発明
方法の実施に用いる別の測定装置を示す概略の断面図で
ある。
１・・測定槽 ２・・試料液
３・・作用電極 ４・・対極
５・・参照電極 ６・・電流計
７・・ポテンショスタット
８・・スターラーパー
漉１図
第４図
第２図
第３図FIG. 1 is a schematic cross-sectional view showing an example of a measuring device used in carrying out the method of the present invention, and FIG. 2 is a graph showing applied voltage and current characteristics of a sample solution containing a fixed concentration of dissolved chlorine dioxide. Figure 3 shows reduction current, residual current, and pH for the same sample solution.
It is a graph showing the relationship between. 4 to 6 are schematic cross-sectional views showing another measuring device used for carrying out the method of the invention. 1... Measuring tank 2... Sample solution 3... Working electrode 4... Counter electrode 5... Reference electrode 6... Ammeter 7... Potentiostat 8... Stirrer filter 1 Figure 4 Figure 2 Figure 3 figure
Claims (2)
参照電極と対極の３極を浸漬し、貴金属又は炭素からな
る作用電極を試料液に対し相対的に動かしながら、２極
の場合は対極を基準に又３極の場合は参照電極を基準に
して溶存二酸化塩素の還元電流を生じる電圧を作用電極
に印加して発生する還元電流を測定するか、又は作用電
極と対極の短絡電流を測定して試料液中の二酸化塩素濃
度を求めることを特徴とする溶存二酸化塩素の測定方法
。(1) Immerse two electrodes, a working electrode and a counter electrode, or three electrodes, a working electrode, a reference electrode, and a counter electrode, in the sample solution, and move the working electrode made of noble metal or carbon relative to the sample solution. In the case of three electrodes, a voltage that generates a reduction current of dissolved chlorine dioxide is applied to the working electrode with reference to the counter electrode, or in the case of three electrodes, a voltage that generates a reduction current of dissolved chlorine dioxide is applied to the working electrode and the generated reduction current is measured, or the working electrode and the counter electrode are shorted A method for measuring dissolved chlorine dioxide, characterized by determining the concentration of chlorine dioxide in a sample solution by measuring an electric current.
対極に銀又は銀／塩化銀を使用して、対極を基準にして
作用電極に＋０．４Ｖ〜−０．４Ｖの電圧を印加するこ
とを特徴とする、請求項（１）記載の溶存二酸化塩素の
測定方法。(2) Using gold or glassy carbon for the working electrode,
Dissolved chlorine dioxide according to claim (1), characterized in that silver or silver/silver chloride is used as a counter electrode, and a voltage of +0.4 V to -0.4 V is applied to the working electrode with respect to the counter electrode. How to measure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1116288A JPH0746090B2 (en) | 1989-05-10 | 1989-05-10 | Method for measuring dissolved chlorine dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1116288A JPH0746090B2 (en) | 1989-05-10 | 1989-05-10 | Method for measuring dissolved chlorine dioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02296143A true JPH02296143A (en) | 1990-12-06 |
| JPH0746090B2 JPH0746090B2 (en) | 1995-05-17 |
Family
ID=14683341
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1116288A Expired - Fee Related JPH0746090B2 (en) | 1989-05-10 | 1989-05-10 | Method for measuring dissolved chlorine dioxide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0746090B2 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000298110A (en) * | 1999-02-08 | 2000-10-24 | Toa Electronics Ltd | Oxidation-reduction current measuring device |
| KR20040009344A (en) * | 2002-07-23 | 2004-01-31 | 유일정공 주식회사 | Residual Chlorine Sensor On Electrochemistry And Measurement Equipment Use Thereof |
| CN104459167A (en) * | 2014-09-26 | 2015-03-25 | 浙江工商大学 | Lactose concentration detection device and lactose concentration detection method |
| CN104459168A (en) * | 2014-09-26 | 2015-03-25 | 浙江工商大学 | Device and method for detecting concentration of D-galactose solution |
| KR102090694B1 (en) * | 2019-11-18 | 2020-03-19 | 한국기초과학지원연구원 | Electrochemical cell and system including the same |
-
1989
- 1989-05-10 JP JP1116288A patent/JPH0746090B2/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000298110A (en) * | 1999-02-08 | 2000-10-24 | Toa Electronics Ltd | Oxidation-reduction current measuring device |
| KR20040009344A (en) * | 2002-07-23 | 2004-01-31 | 유일정공 주식회사 | Residual Chlorine Sensor On Electrochemistry And Measurement Equipment Use Thereof |
| CN104459167A (en) * | 2014-09-26 | 2015-03-25 | 浙江工商大学 | Lactose concentration detection device and lactose concentration detection method |
| CN104459168A (en) * | 2014-09-26 | 2015-03-25 | 浙江工商大学 | Device and method for detecting concentration of D-galactose solution |
| KR102090694B1 (en) * | 2019-11-18 | 2020-03-19 | 한국기초과학지원연구원 | Electrochemical cell and system including the same |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0746090B2 (en) | 1995-05-17 |
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