JPH0743320B2 - Method for measuring chemical oxygen demand of water - Google Patents
Method for measuring chemical oxygen demand of waterInfo
- Publication number
- JPH0743320B2 JPH0743320B2 JP20450292A JP20450292A JPH0743320B2 JP H0743320 B2 JPH0743320 B2 JP H0743320B2 JP 20450292 A JP20450292 A JP 20450292A JP 20450292 A JP20450292 A JP 20450292A JP H0743320 B2 JPH0743320 B2 JP H0743320B2
- Authority
- JP
- Japan
- Prior art keywords
- water
- sample
- reaction
- reaction tube
- tube
- 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 - Fee Related
Links
- 238000000034 method Methods 0.000 title claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims description 8
- 239000000126 substance Substances 0.000 title claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims description 5
- 229910052760 oxygen Inorganic materials 0.000 title claims description 5
- 239000001301 oxygen Substances 0.000 title claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 27
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 18
- 239000012286 potassium permanganate Substances 0.000 claims description 8
- 239000007800 oxidant agent Substances 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 7
- 238000002835 absorbance Methods 0.000 claims description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 4
- 239000012498 ultrapure water Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims 1
- 239000003153 chemical reaction reagent Substances 0.000 description 13
- 239000000243 solution Substances 0.000 description 9
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 6
- 238000005259 measurement Methods 0.000 description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 4
- 230000009257 reactivity Effects 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- QNGVNLMMEQUVQK-UHFFFAOYSA-N 4-n,4-n-diethylbenzene-1,4-diamine Chemical compound CCN(CC)C1=CC=C(N)C=C1 QNGVNLMMEQUVQK-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004401 flow injection analysis Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910001437 manganese ion Inorganic materials 0.000 description 1
- 229940099596 manganese sulfate Drugs 0.000 description 1
- 235000007079 manganese sulphate Nutrition 0.000 description 1
- 239000011702 manganese sulphate Substances 0.000 description 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 description 1
- 229940039790 sodium oxalate Drugs 0.000 description 1
Landscapes
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、水の化学的酸素要求量
（以下ＣＯＤと記す）を測定する方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for measuring the chemical oxygen demand (hereinafter referred to as COD) of water.
【０００２】[0002]
【従来の技術】従来、ＣＯＤの測定は、図５に示す如き
フローインジェクション装置によって行われている。同
図において、１はサンプル流路、２は試薬流路、３は両
流路中を送液するダブルレシプロ型マイクロポンプ、４
はサンプルインジェクター、５は恒温槽６内に通した反
応チューブ、７は分光光度計、８は記録計、９は背圧ホ
イルである。2. Description of the Related Art Conventionally, COD is measured by a flow injection device as shown in FIG. In the figure, 1 is a sample flow channel, 2 is a reagent flow channel, 3 is a double reciprocating micropump that feeds both channels, 4
Is a sample injector, 5 is a reaction tube passed through a constant temperature bath 6, 7 is a spectrophotometer, 8 is a recorder, and 9 is a back pressure foil.
【０００３】この装置を使用し、サンプル流路１にはキ
ャリヤーとして超純水を、試薬流路２には過マンガン酸
カリウムや２クロム酸カリウム等の酸化剤を試薬として
送り、サンプルインジェクター４によりキャリヤー送液
中に廃水等のサンプルを注入し、試薬と合流させる。こ
れを１００〜１２０℃に保った恒温槽６内のポリテトラ
フルオロエチレンからなる反応チューブ５内に通して反
応させ、分光光度計７によって吸光度を測定することに
よってＣＯＤを測定している。Using this device, ultrapure water is sent to the sample flow path 1 as a carrier, and an oxidizing agent such as potassium permanganate or potassium dichromate is sent to the reagent flow path 2 as a reagent. A sample of wastewater or the like is injected into the carrier solution to merge with the reagent. The COD is measured by passing this through a reaction tube 5 made of polytetrafluoroethylene in a constant temperature bath 6 kept at 100 to 120 ° C. for reaction, and measuring the absorbance with a spectrophotometer 7.
【０００４】[0004]
【発明が解決しようとする課題】このような従来のＣＯ
Ｄ測定方法においては、試薬として過マンガン酸カリウ
ムを使用した場合、沸騰水中に１〜２時間、２クロム酸
カリウムでも５０ｍもの反応チューブを使用する必要が
あった。[Problems to be Solved by the Invention] Such a conventional CO
In the D measurement method, when potassium permanganate was used as a reagent, it was necessary to use a reaction tube of 50 m even in potassium dichromate for 1 to 2 hours in boiling water.
【０００５】このため、送液速度や恒温槽温度等の条件
を長時間にわたって安定化させることが困難となり、安
定した測定値が得られず、また感度も低い等の問題があ
った。For this reason, it becomes difficult to stabilize the conditions such as the liquid feed rate and the temperature of the constant temperature bath for a long period of time, so that stable measured values cannot be obtained and the sensitivity is low.
【０００６】本発明はこのような問題にかんがみ、反応
が短時間でなされ、従って短い反応チューブで良く、安
定した高感度の測定値が短時間で得られる水のＣＯＤ測
定方法の提供を目的としたものである。In view of the above problems, the present invention aims to provide a method for measuring COD of water in which the reaction is carried out in a short time, and therefore a short reaction tube is sufficient and stable and highly sensitive measured values can be obtained in a short time. It was done.
【０００７】[0007]
【課題を達成するための手段】上述の如き従来の問題を
解決し、所期の目的を達成するための本発明の要旨とす
るところは、超純水をキャリヤー溶液としてサンプルを
送液し、これに過マンガン酸カリウム等の酸化剤を合流
させて恒温槽で温められた反応チューブ内に通した後、
吸光度を測定する水の化学的酸素要求量測定方法におい
て、前記反応チューブに白金製チューブを使用すること
を特徴としてなる水の化学的酸素要求量測定方法に存す
る。Means for Achieving the Object The object of the present invention to solve the above-mentioned conventional problems and achieve the intended purpose is to send a sample using ultrapure water as a carrier solution, After merging this with an oxidizing agent such as potassium permanganate and passing it through a reaction tube heated in a constant temperature bath,
In the method for measuring the chemical oxygen demand of water for measuring the absorbance, a platinum tube is used as the reaction tube, which is a method for measuring the chemical oxygen demand of water.
【０００８】[0008]
【作用】本発明のＣＯＤ測定方法は、過マンガンカリウ
ム等の酸化剤を廃水等のサンプル中に混合して酸化させ
ることにり生じる５２５mmの光吸収減少を測定するもの
であり、サンプルと酸化剤が反応チューブ内を通る間
に、その反応チューブの白金が液中の過マンガン酸カリ
ウムの一部を分解し、実際の触媒である二酸化マンガン
をチューブ内壁面に析出させ、これが反応を促進させ、
反応が数分でなされ、約１時間で測定値が一定の安定し
たものとなる。The COD measuring method of the present invention is for measuring the decrease in light absorption of 525 mm caused by mixing an oxidizing agent such as potassium permanganate with a sample such as wastewater and oxidizing it. While passing through the reaction tube, platinum in the reaction tube decomposes part of potassium permanganate in the liquid, and manganese dioxide that is the actual catalyst is deposited on the inner wall surface of the tube, which accelerates the reaction,
The reaction is carried out in a few minutes, and the measured value becomes constant and stable in about 1 hour.
【０００９】[0009]
【実施例】次に本発明の実施例を図１〜図４について説
明する。EXAMPLE An example of the present invention will be described with reference to FIGS.
【００１０】図１は発明方法を実施する装置のフローダ
イヤグラムを示しており、図において、１１はサンプル
流路、１２は試薬流路、１３は反応検出流路、１４は両
流路中の薬液を送るダブルシレプロ型マイクロポンプ、
１５はサンプルインジェクター、１６は反応検出路１３
に設けた反応チューブ、１７は同じく冷却コイル、１８
は分光光度計、１９は記録計、２０は背圧コイルであ
る。FIG. 1 shows a flow diagram of an apparatus for carrying out the method of the invention. In the figure, 11 is a sample channel, 12 is a reagent channel, 13 is a reaction detection channel, and 14 is a chemical solution in both channels. Double Sile Pro type micro pump,
15 is a sample injector, 16 is a reaction detection path 13
Reaction tube provided in the same, 17 is a cooling coil, 18
Is a spectrophotometer, 19 is a recorder, and 20 is a back pressure coil.
【００１１】反応チューブ１６は内径０．５mm、長さ約
３ｍの白金製の細管が使用され、恒温槽２１内に収容さ
れている。また冷却チューブは長さを約２ｍとしてい
る。The reaction tube 16 is a platinum thin tube having an inner diameter of 0.5 mm and a length of about 3 m, and is housed in a constant temperature bath 21. The cooling tube has a length of about 2 m.
【００１２】本発明はこのような装置を使用し、サンプ
ル流路１１に従来と同様にキャリヤーとして超純水を送
液するとともに、試薬流路に酸化剤としての試薬溶液と
して過マンガン酸カリウムと硫酸の混合水溶液を送液
し、恒温槽２１を１００℃に保たせる。この状態でサン
プルインジェクター１５よりＣＯＤを測定しようと水、
即ちサンプルを注入する。これによってサンプルが反応
検出路１３の入口で酸化剤と混合され、反応チューブ１
６内で１００℃の温度条件下にて反応される。次いで冷
却チューブ１７内で冷却され、分光光度計１８にて吸光
度が測定され、記録計１９に記録される。According to the present invention, using such an apparatus, ultrapure water is sent to the sample channel 11 as a carrier as in the conventional case, and potassium permanganate is used as a reagent solution as an oxidizing agent in the reagent channel. A mixed aqueous solution of sulfuric acid is sent to keep the thermostat 21 at 100 ° C. In this state, water is used to measure COD from the sample injector 15.
That is, the sample is injected. As a result, the sample is mixed with the oxidant at the inlet of the reaction detection path 13, and the reaction tube 1
6 under the temperature condition of 100 ° C. Then, it is cooled in the cooling tube 17, the absorbance is measured by the spectrophotometer 18, and recorded in the recorder 19.
【００１３】次に本発明方法による測定値のピーク高
（感度）及びその再現性の試験例について説明する。Next, a test example of the peak height (sensitivity) of the measured value and its reproducibility by the method of the present invention will be described.
【００１４】本発明方法として、５×１０−５Ｍ硫酸マ
ンガンを試薬溶液に加え、マンガン２価イオンとし、図
１に示すフローチャートの装置により標準サンプルとし
てＤ−グルコースを３０ｐｐｍ注入した。この時の測定
結果は図２に示す如くであった。In the method of the present invention, 5 × 10 −5 M manganese sulfate was added to the reagent solution to form divalent manganese ions, and 30 ppm of D-glucose was injected as a standard sample by the apparatus of the flow chart shown in FIG. The measurement result at this time was as shown in FIG.
【００１５】対象例として、内径０．５mm、長さ３ｍの
ポリテトラフルオロエチレンからなる反応チューブを使
用し、その中に白金線を入れた場合、及びパラジウム線
を入れた場合について、上記本発明方法と同じ条件下に
て測定した。この結果、白金線の場合は図３、パラジウ
ム線の場合は図４の測定結果が得られた。As a target example, a reaction tube made of polytetrafluoroethylene having an inner diameter of 0.5 mm and a length of 3 m is used, and a platinum wire is put therein and a palladium wire is put therein. It measured on the same conditions as the method. As a result, the measurement results of FIG. 3 were obtained for the platinum wire and FIG. 4 were obtained for the palladium wire.
【００１６】白金線を使用した場合は、図３に示すよう
にピーク高が小さく、反応性が悪く、またピーク高は時
間と共に上昇し続け、再現性がない。またパラジウム線
を使用した場合は図４に示すように反応性、再現性とと
もに良くはなっているが、ベースラインがあまり安定し
ていない。When a platinum wire is used, the peak height is small and the reactivity is poor as shown in FIG. 3, and the peak height continues to rise with time and is not reproducible. When the palladium wire is used, the reactivity and reproducibility are improved as shown in FIG. 4, but the baseline is not very stable.
【００１７】これに対し、本発明方法は図２に示すよう
に白金チューブを用いることにより試薬溶液を流し始め
てから約１時間程度で、ピーク高とベースラインが安定
するという結果が得られた。On the other hand, according to the method of the present invention, as shown in FIG. 2, the result that the peak height and the baseline became stable was obtained within about 1 hour after starting the flow of the reagent solution by using the platinum tube.
【００１８】白金チューブの作用は、試薬溶液中の過マ
ンガン酸カリウムの一部を分解し、実際の触媒である二
酸化マンガンを作り、それを触媒表面に付着させ反応を
促進させることであると考えられる。触媒表面の黒褐色
の付着物が二酸化マンガンであると確認したのは、しゅ
う酸ナトリウム溶液につけると溶けなくなり、酸化剤に
対して発色試薬であるN,N −ジエチル−Ｐ−フェニレン
ジアミン溶液につけると、赤色に呈色するところからで
ある。It is considered that the action of the platinum tube is to decompose a part of potassium permanganate in the reagent solution to produce manganese dioxide which is an actual catalyst and to attach it to the catalyst surface to accelerate the reaction. To be It was confirmed that the blackish brown deposits on the catalyst surface were manganese dioxide because they became insoluble when soaked in sodium oxalate solution, and soaked in N, N-diethyl-P-phenylenediamine solution which is a coloring reagent for the oxidizing agent. And from where it turns red.
【００１９】[0019]
【発明の効果】上述したように本発明のＣＯＤ測定方法
においては、白金製のチューブを反応チューブとして使
用したことにより、３ｍ程度の長さであっても充分な反
応性（感度）が得られ、従って反応チューブを通り抜け
るまでの時間、即ち反応時間が数分程度の短時間で良く
なり、安定した反応条件下にて測定値が得られ、しかも
ピーク高の再現性が良く、正確な測定値が得られること
となったものである。As described above, in the COD measuring method of the present invention, by using a platinum tube as a reaction tube, sufficient reactivity (sensitivity) can be obtained even with a length of about 3 m. Therefore, the time to pass through the reaction tube, that is, the reaction time is improved in a short time of about several minutes, the measured value can be obtained under stable reaction conditions, and the reproducibility of the peak height is good, and the measured value is accurate. Will be obtained.
【図面の簡単な説明】[Brief description of drawings]
【図１】本発明方法を実施するためのフローチャートで
ある。1 is a flow chart for implementing the method of the present invention.
【図２】本発明方法による測定結果のグラフである。FIG. 2 is a graph of measurement results according to the method of the present invention.
【図３】白金線を使用した対象方法による測定結果のグ
ラフである。FIG. 3 is a graph of measurement results by a target method using a platinum wire.
【図４】パラジウム線を使用した対象方法による測定結
果のグラフである。FIG. 4 is a graph of measurement results by a target method using a palladium wire.
【図５】従来方法を実施するためのフローチャートであ
る。FIG. 5 is a flow chart for implementing a conventional method.
１１ サンプル流路 １２ 試薬流路 １３ 反応検出流路 １４ マイクロプンプ １５ サンプルインジェクター １６ 反応チューブ １７ 冷却コイル １８ 分光光度計 １９ 記録計 ２０ 背圧コイル ２１ 恒温槽 11 sample flow path 12 reagent flow path 13 reaction detection flow path 14 micro pump 15 sample injector 16 reaction tube 17 cooling coil 18 spectrophotometer 19 recorder 20 back pressure coil 21 constant temperature bath
Claims (1)
を送液し、これに過マンガン酸カリウム等の酸化剤を合
流させて恒温槽で温められた反応チューブ内に通した
後、吸光度を測定する水の化学的酸素要求量測定方法に
おいて、前記反応チューブに白金製チューブを使用する
ことを特徴としてなる水の化学的酸素要求量測定方法。1. A sample is sent using ultrapure water as a carrier solution, and an oxidizing agent such as potassium permanganate is joined to the sample, and the mixture is passed through a reaction tube heated in a constant temperature bath, and then the absorbance is measured. A method for measuring the chemical oxygen demand of water, characterized in that a platinum tube is used as the reaction tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20450292A JPH0743320B2 (en) | 1992-07-08 | 1992-07-08 | Method for measuring chemical oxygen demand of water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20450292A JPH0743320B2 (en) | 1992-07-08 | 1992-07-08 | Method for measuring chemical oxygen demand of water |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0627100A JPH0627100A (en) | 1994-02-04 |
| JPH0743320B2 true JPH0743320B2 (en) | 1995-05-15 |
Family
ID=16491595
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20450292A Expired - Fee Related JPH0743320B2 (en) | 1992-07-08 | 1992-07-08 | Method for measuring chemical oxygen demand of water |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0743320B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20180135600A (en) * | 2017-06-13 | 2018-12-21 | 서울시립대학교 산학협력단 | Semi-continuos flow method and device for COD determination using coil-reactor under low temperature and high pressure |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113816482A (en) * | 2020-06-18 | 2021-12-21 | 北京博诺安科科技有限公司 | Manganese salt for treating landfill leachate and refractory wastewater in printing, dyeing and papermaking industries |
-
1992
- 1992-07-08 JP JP20450292A patent/JPH0743320B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20180135600A (en) * | 2017-06-13 | 2018-12-21 | 서울시립대학교 산학협력단 | Semi-continuos flow method and device for COD determination using coil-reactor under low temperature and high pressure |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0627100A (en) | 1994-02-04 |
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