CN101852732A - Rapid determining method of COD by photocatalytic digestion - Google Patents
Rapid determining method of COD by photocatalytic digestion Download PDFInfo
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- CN101852732A CN101852732A CN 201010180037 CN201010180037A CN101852732A CN 101852732 A CN101852732 A CN 101852732A CN 201010180037 CN201010180037 CN 201010180037 CN 201010180037 A CN201010180037 A CN 201010180037A CN 101852732 A CN101852732 A CN 101852732A
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Abstract
The invention provides a novel rapid determining method of COD by photocatalytic digestion, which adopts a compound system combined by colored oxidant and nano-photocatalyst in acidic medium to carrying out illuminating oxidation digestion for water samples, and realizes the determination of COD by optically detecting the consumption of the colored oxidant, wherein the colored oxidant is of an oxidation substance which has absorption and good optical stability in an ultraviolet visible range, and the nano-photocatalyst is of a nano-size semi-conductor material which can absorb light energy and generate electron-hole pairs. In the process of photocatalytic digestion, the colored oxidant not only oxidizes reducing substances in water and receives photo-induced electrons, and the consumption of the colored oxidant corresponds to the amount of COD. The colored oxidant and the nano-photocatalyst are combined to generate extremely strong oxidation efficiency, and can oxidize a plurality of reducing substances, so that the oxidation digestion is quickly and efficiently carried out at room temperature under non-concentrated acid conditions. The invention can solve the problems that the existing determining method of COD has complicated process, time and energy consumption, requirement for high temperature and concentrated acid conditions, and can not realize rapid field determination.
Description
Technical field
The present invention relates to the environmental monitoring technology field, be specifically related to the method for a kind of mensuration chemical oxygen demand (COD) (COD).
Background technology
Chemical oxygen demand (COD) (Chemical Oxygen Damand, COD) be meant under certain conditions, when adopting certain strong oxidizer to handle water sample, the oxidant content that is consumed, be converted into the mass concentration of oxygen, having reflected that water body is subjected to the degree that reducing substances pollutes, is one of important indicator of comprehensive evaluation water pollution degree.
The mensuration of COD needs that at first reducing substances in the sample is carried out oxidation and clears up, and adds that most of organism are difficult to oxidation and clear up, and is emphasis and the difficult point that COD measures so oxidation is cleared up.Existing COD assay method mainly is a dichromate titration, and this method is present China and international accepted standard method.Dichromate titration is in the concentrated sulphuric acid, is oxygenant with the potassium dichromate, Ag
2SO
4Be catalyzer, oxidation was cleared up 2 hours under the boiling reflux condition; This method oxygenation efficiency can reach about 90%, is applicable to the mensuration of high concentration water sample, but during consumption energy consumption, a large amount of concentrated sulphuric acid brings serious secondary pollution, chlorion has serious interference in addition, is difficult to satisfy the requirement of fast-field evaluation.
In recent years, need the deficiency of concentrated acid and high temperature heating to develop a kind of new method that turns to the basis with photocatalytic-oxidation for overcoming existing COD assay method.This method excites by UV-irradiation, makes the photocatalyst surface electronic transition produce electron-hole pair, and wherein photohole is oxidable is adsorbed on surperficial reducing substances, thereby the realization oxidation is cleared up under normal condition.At present, the photocatalyst of photocatalytic oxidation employing has powder and two kinds of forms of film.Powder is that photocatalyst granular is dispersed in the solution, and film is that photocatalyst is loaded on other solid matter; The former influences optical detection because of powder, need filter during mensuration or the centrifuging photocatalyst, and the latter prepares that difficulty is big, oxidation efficiency is low, and these all are unsuitable for fast-field evaluation.
Summary of the invention
Given this, the objective of the invention is the problems referred to above at existing COD photocatalysis assay method existence, the COD assay method that provide a kind of oxidation efficiency height, need not separate is realized the oxidation of water sample is cleared up and optical detection at short notice, makes the fast-field evaluation of COD become possibility.
For reaching above-mentioned purpose, the present invention proposes a kind of COD photocatalysis and clears up method for measuring, it adopts coloured oxygenant to combine with nano-photocatalyst, under illumination and acid medium condition reducing substances being carried out oxidation clears up, by the consumption of the coloured oxygenant of optical detection, realize the mensuration of COD then.
Wherein, coloured oxygenant is that the oxidizing substance that absorbs and have good light stability is arranged in the UV, visible light scope, comprises Ce (SO
4)
2, K
2Cr
2O
7, KMnO
4Deng.
Nano-photocatalyst is the nanometer size, can absorbs the semiconductor material that luminous energy produces electron-hole pair, comprises various simplification compounds, doped compound or binary or the multiple element compound, for example TiO
2, ZnS, N-TiO
2, Ag-TiO
2-, Fe-TiO
2, Pt-TiO
2, Ag-S-C-TiO
2, TiO
2-ZnS, TiO
2-CdS, TiO
2-Fe
3O
4Deng.
The amount of coloured oxygenant is a key factor of the oxidation efficiency of decision compound system, its amount is big more, and oxidation efficiency is strong more, but content is too big, can make the background absorbance of optical detection too high, therefore the concentration range of coloured oxygenant is preferably 0.1～15mmol/L.The amount of nano-photocatalyst also is one of factor of decision compound system oxidation efficiency simultaneously, measure big more, oxidation efficiency is high more, thereby but the too high meeting of content significantly increases the turbidity interference optical detection of solution, so the concentration range of nano-photocatalyst is preferably 0.0003～0.15g/L.
Acid medium comprises that all have the mineral acid of irreducibility, as H
2SO
4, H
3PO
4Deng.The acidity decision nano-photocatalyst surface charge and the absorption property of medium, thus photocatalysis efficiency influenced, so acidity of medium should be higher than the isoelectric point of nano-photocatalyst.The concentration of acid medium should be greater than the critical hydrolytic acidity of coloured oxygenant in the compound system, and acidity must guarantee PH≤4.
The principle that combines the compound system mensuration COD that forms for coloured oxygenant with nano-photocatalyst is, when nano-photocatalyst is subjected to greater than the irradiation of the light (hv) of energy gap (Eg) energy, the electronic transition of nano-photocatalyst valence band (VB) is to conduction band (CB), so it is right to have produced light induced electron-hole, photocatalyst part light induced electron-hole inner and surface takes place compound, not compound photohole oxidation is adsorbed on a part of reducing substances of photocatalyst surface, its corresponding electronics is attracted to coloured oxygenant of photocatalyst surface and accepts, in addition, oxygenant itself is also wanted oxidation part reducing substances, therefore, the amount of the coloured oxygenant that is consumed is corresponding to the total amount of COD.
The present invention compares with existing COD assay method, has following advantage and effect:
At first, in the oxidation digestion process, coloured oxygenant and photohole can both the oxidation-reduction quality materials, and coloured oxygenant is also accepted light induced electron, stop the compound of electronics-hole, and the nano-photocatalyst specific surface area is bigger, the more reducing substances of easy more absorption and coloured oxygenant are on its surface, accelerate the carrying out of light-catalyzed reaction, this three aspect has all improved oxidation efficiency, the oxidation of COD is cleared up under normal temperature, non-concentrated acid condition carried out; Photocatalyst is the nanometer size, is colloidal and evenly disperses in solution, need not to separate to carry out optical detection, and therefore, the present invention measures water sample more fast, efficiently.
Secondly, compare the many reagent of traditional standard method and add respectively, compound system of the present invention is homogeneously dispersed state, can regularly preserve, and reagent once adds, and makes the method operation easier.
Once more, the present invention is used for water determination and is not subjected to the noisy Cl of dichromate titration
-Influence, and reaction sensitivity height, detection limit are low, therefore have the wideer scope of application than National Standard Method.
The present invention is used for the mensuration of ambient water quality COD, has above-mentioned unique advantage, is easy to apply.
Description of drawings
Fig. 1 is a nano-TiO
2-Ce (SO
4)
2System is measured the spectrogram of COD
Fig. 2 is the schematic diagram that nano-photo catalytic is cleared up COD
Embodiment
Below, more in conjunction with the embodiments and accompanying drawing the present invention is further described.
Embodiment 1
The mensuration that relatively reaches actual water sample and simulated water sample of the inventive method and GB dichromate titration oxygenation efficiency:
To select concentration for use be that the particle diameter of 0.003g/L is the TiO of 5nm to nano-photocatalyst in the present embodiment
2It is the Ce (SO of 2.4mmol/L that powder, coloured oxygenant are selected concentration for use
4)
2, it is the H of 1mol/L that acid medium is selected concentration for use
2SO
4, the three forms compound system, at ambient temperature, use the miniwatt UV illumination of 3W, oxidation is carried out spectral detection after clearing up 10min to water sample, and the scan light spectrogram is seen accompanying drawing 1, as standard solution, set up typical curve with 1～20mg/L Potassium Hydrogen Phthalate solution, working sample COD value.
The oxygenation efficiency of oxidizing digestion method is high more, the oxidation of water sample is cleared up complete more, and measurement result is more near actual value.With COD concentration is that the simulated water sample of 15mg/L is an object, adopting this law and dichromate titration that it is carried out oxidation respectively clears up, with the amount of residue Potassium Hydrogen Phthalate in the high-performance liquid chromatogram determination reactant liquor, the oxygenation efficiency that draws Potassium Hydrogen Phthalate is respectively 97% and 95% then; The result shows that this law oxygenation efficiency is a little more than dichromate titration, and the result is more near actual value.
Chlorion (Cl
-) some COD assay method there is obvious interference, as the GB dichromate titration, need to add screening agent and eliminate Cl
-Disturb.Adopt body series to Cl
-The simulated water sample of the 15mg/L of concentration in 0～2000mg/L scope is measured, and the relative deviation of measurement result shows in this scope Cl all less than 5%
-Existence this law is not had remarkable interference, can be used for high Cl
-The mensuration of concentration water sample.
Set up typical curve with standard solution, as accompanying drawing 1, the slope of standard equation is 0.0383, and blank solution is measured the detection limit 0.4mg/L (detection limit=(3 * blank standard deviation)/slope of standard curve) that tries to achieve this law for 5 times, and (COD≤15mg/L) detects requirement can to satisfy I class water quality.
Adopt this law and standard method that actual water sample (lake water sample) is measured, the results are shown in Table 1:
COD Determination on content result (n=5) in table 1 sample
This law dichromate titration
Sample COD (mg/L
Rec(％) RSD(％)?COD(mg/L)?Rec(％)?RSD(％)
)
River sample 1
#6.83 97.5 2.56 6.59 102.1 1.22
River sample 2
#9.72 103.5 1.47 9.83 99.4 3.56
Lake water sample 1
#18.3 100.6 3.75 19.1 98.7 2.95
By table 1 as seen, the body series measured value conforms to substantially with standard weight chromate process measured value, and body series can be used for the mensuration of 1～20mg/L water sample.
The limit of identification 0.4mg/L of present embodiment can once finish in 10 minutes the oxidation of sample is cleared up and mensuration, both can be used for the water determination that COD is 1～20mg/L concentration range, can be used for the mensuration of high cl concn water sample in the 2000mg/L scope again.
Embodiment 2
Present embodiment is measured actual water sample and simulated water sample:
To select concentration for use be that the particle diameter of 0.030g/L is the TiO of 5nm to nano-photocatalyst in the present embodiment
2It is the KMnO of 0.4mmol/L that powder, coloured oxygenant are selected concentration for use
4, it is the H of 1mol/L that acid medium is selected concentration for use
2SO
4, the three forms compound system, at ambient temperature, use the miniwatt UV illumination of 3W, oxidation is carried out spectral detection after clearing up 10min to water sample, with 1～60mg/L Potassium Hydrogen Phthalate solution as standard solution, set up typical curve, working sample COD value.
Chlorion (Cl
-) some COD assay method there is obvious interference, as the GB dichromate titration, need to add screening agent and eliminate Cl
-Disturb.Adopt body series to Cl
-The simulated water sample of the 15mg/L of concentration in 0～2000mg/L scope is measured, and the relative deviation of measurement result shows in this scope Cl all less than 5%
-Existence this law is not had remarkable interference, can be used for high Cl
-The mensuration of concentration water sample.
Set up typical curve with standard solution, the slope of standard equation is 0.0357, blank solution is measured the detection limit 0.75mg/L (detection limit=(3 * blank standard deviation)/slope of standard curve) that tries to achieve this law for 5 times, and (COD≤15mg/L) detects requirement can to satisfy I class water quality.
Adopt this law and standard method that actual water sample (river sample and lake water sample) is measured, the results are shown in Table 2:
COD Determination on content result (n=5) in table 2 sample
This law dichromate titration
Sample COD (mg/L
Rec(％)?RSD(％)?COD(mg/L)?Rec(％)?RSD(％)
)
River sample 1
#3.25 98.1 1.13 3.17 99.5 1.78
Lake water sample 1
#17.4 99.3 0.82 17.8 100.7 2.65
Lake water sample 2
#35.9 97.6 2.57 36.1 96.2 1.43
By table 2 as seen, the body series measured value conforms to substantially with standard weight chromate process measured value, and body series can be used for the mensuration of 1～60mg/L water sample.
The limit of identification 0.75mg/L of present embodiment can once finish in 10 minutes the oxidation of sample is cleared up and mensuration, both can be used for the water determination that COD is 1～60mg/L concentration range, Cl
-Concentration does not make significant difference in 0～2000mg/L scope, and resisting chloride ion penetration disturbs strong.
Embodiment 3
Present embodiment is measured actual water sample and simulated water sample:
To select concentration for use be that the particle diameter of 0.030g/L is the TiO of 5nm to nano-photocatalyst in the present embodiment
2It is the K of 4.8mmol/L that powder, coloured oxygenant are selected concentration for use
2Cr
2O
7, it is the H of 1mol/L that acid medium is selected concentration for use
2SO
4, the three forms compound system, at ambient temperature, use the miniwatt UV illumination of 3W, oxidation is carried out spectral detection after clearing up 10min to water sample, with 1～35mg/L Potassium Hydrogen Phthalate solution as standard solution, set up typical curve, working sample COD value.
Chlorion (Cl
-) some COD assay method there is obvious interference, as the GB dichromate titration, need to add screening agent and eliminate Cl
-Disturb.Adopt body series to Cl
-The simulated water sample of the 15mg/L of concentration in 0～2000mg/L scope is measured, and the relative deviation of measurement result shows in this scope Cl all less than 5%
-Existence this law is not had remarkable interference, can be used for high Cl
-The mensuration of concentration water sample.
Set up typical curve with standard solution, the slope of standard equation is 0.0325, blank solution is measured the detection limit 0.87mg/L (detection limit=(3 * blank standard deviation)/slope of standard curve) that tries to achieve this law for 5 times, and (COD≤15mg/L) detects requirement can to satisfy I class water quality.
Adopt this law and standard method that actual water sample (lake water sample) is measured, the results are shown in Table 4:
COD Determination on content result (n=5) in table 3 sample
This law dichromate titration
Sample COD (mg/L
Rec(％)?RSD(％)?COD(mg/L)?Rec(％) RSD(％)
)
River sample 1
#2.17 97.5 1.83 2.11 100.5 2.37
River sample 2
#16.8 100.4 3.67 16.9 99.5 1.39
Lake water sample 1
#22.6 98.7 0.59 21.3 101.4 3.32
By table 3 as seen, the body series measured value conforms to substantially with standard weight chromate process measured value, and body series can be used for the mensuration of 1～35mg/L water sample.
The limit of identification 0.87mg/L of present embodiment can once finish in 10 minutes the oxidation of sample is cleared up and mensuration, both can be used for the water determination that COD is 1～35mg/L concentration range, Cl
-Concentration does not make significant difference in 0～2000mg/L scope, and resisting chloride ion penetration disturbs strong.
Embodiment 4
Present embodiment is measured simulated water sample:
To select concentration for use be Ag, the S of 0.003g/L, the nano-TiO of C codope to nano-photocatalyst in the present embodiment
2It is the Ce (SO of 3mmol/L that powder, coloured oxygenant are selected concentration for use
4)
2, it is the H of 1mol/L that acid medium is selected concentration for use
2SO
4, the three forms compound system, at ambient temperature, use the miniwatt UV illumination of 3W, oxidation is carried out spectral detection after clearing up 10min to water sample, with 1～30mg/L Potassium Hydrogen Phthalate solution as standard solution, set up typical curve, working sample COD value.
Set up typical curve with standard solution, the slope of standard equation is 0.0613, blank solution is measured the detection limit 0.1mg/L (detection limit=(3 * blank standard deviation)/slope of standard curve) that tries to achieve this law for 5 times, and (COD≤15mg/L) detects requirement can to satisfy I class water quality.
Embodiment 5
Present embodiment is measured simulated water sample:
To select concentration for use be the TiO of 0.003g/L to nano-photocatalyst in the present embodiment
2-ZnS, it is the K of 4.8mmol/L that coloured oxygenant is selected concentration for use
2Cr
2O
7, it is the H of 1mol/L that acid medium is selected concentration for use
2SO
4, the three forms compound system, at ambient temperature, use the miniwatt UV illumination of 3W, oxidation is carried out spectral detection after clearing up 10min to water sample, with 1～45mg/L Potassium Hydrogen Phthalate solution as standard solution, set up typical curve, working sample COD value.
Set up typical curve with standard solution, the slope of standard equation is 0.0452, blank solution is measured the detection limit 0.5mg/L (detection limit=(3 * blank standard deviation)/slope of standard curve) that tries to achieve this law for 5 times, and (COD≤15mg/L) detects requirement can to satisfy I class water quality.
Claims (6)
1. rapid assay methods is cleared up in a COD photocatalysis, it is characterized in that, described method is to adopt coloured oxygenant to combine the compound system of forming with nano-photocatalyst in acid medium water sample is carried out the illumination oxidation to clear up, the mensuration of the consumption realization COD by the coloured oxygenant of optical detection;
Described acid medium is chosen all mineral acids with irreducibility, and its acidity should be higher than the isoelectric point of nano-photocatalyst;
Described coloured oxygenant is meant the oxidizing substance that absorbs and have good light stability in the UV, visible light scope, it is selected from Ce (SO
4)
2, K
2Cr
2O
7, KMnO
7
Described nano-photocatalyst is meant the nanometer size, can absorbs the semiconductor material that luminous energy produces electron-hole pair, and it is selected from TiO
2, ZnS, doping TiO
2, binary or polynary compound nano-photocatalyst;
The concentration range of nano-photocatalyst is 0.0003～0.15g/L in the compound system, the concentration range of coloured oxygenant is 0.1～15mmol/L, the concentration of acid medium is to determine according to the character of selected coloured oxygenant, the concentration of acid medium should be greater than the critical hydrolytic acidity of coloured oxygenant in the compound system, and acidity must guarantee PH≤4.
2. rapid assay methods is cleared up in COD photocatalysis according to claim 1, it is characterized in that described acid medium is selected from H
2SO
4, H
3PO
4
3. Rapid Determination Method is cleared up in COD photocatalysis according to claim 1 and 2, it is characterized in that described method is to carry out at ambient temperature.
4. Rapid Determination Method is cleared up in COD photocatalysis according to claim 1 and 2, and the illumination that it is characterized in that described method is that the miniwatt uviol lamp of employing 1～20W is a light source.
5. Rapid Determination Method is cleared up in COD photocatalysis according to claim 1 and 2, it is characterized in that described method is 1～15min to the oxidation digestion time of water sample.
6. Rapid Determination Method is cleared up in COD photocatalysis according to claim 1 and 2, it is characterized in that: described method will be that described compound system joins in the testing sample, after the UV illumination reaction, directly carry out spectral detection; As standard solution, set up typical curve with Potassium Hydrogen Phthalate solution, then the spectroscopic assay value of water sample is brought into the COD value that calculates sample in the equation of typical curve.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102279123A (en) * | 2011-06-14 | 2011-12-14 | 聚光科技(杭州)股份有限公司 | Pretreatment method and device |
| CN102288599A (en) * | 2011-05-13 | 2011-12-21 | 重庆大学 | Associative colorimetric measuring method for total phosphorus and chemical oxygen demand (COD) |
| CN102680461A (en) * | 2012-06-08 | 2012-09-19 | 江南大学 | Chemical oxygen demand (COD) determination method based on chemiluminiscence method of photocatalytic oxidation of nano-TiO2 on (-KMnO4) |
| CN102818778A (en) * | 2012-07-25 | 2012-12-12 | 漳州师范学院 | Method for rapid determination of chemical oxygen demand in environmental water sample |
| CN103105329A (en) * | 2012-11-06 | 2013-05-15 | 苏州聚阳环保科技有限公司 | Permanganate index digestion method and device in on-line water monitoring |
| CN106092719A (en) * | 2016-08-11 | 2016-11-09 | 贵州开磷质量检测中心有限责任公司 | A kind of method measuring COD by rapid-digestion |
| CN109374559A (en) * | 2018-12-24 | 2019-02-22 | 燕山大学 | A kind of water body COD value measuring method based on ultra-violet absorption spectrum |
| CN114904586A (en) * | 2022-05-09 | 2022-08-16 | 洛阳莱博图电子科技有限公司 | COD prefabricated reagent for water quality sample determination and preparation method thereof |
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| CN1412540A (en) * | 2002-11-22 | 2003-04-23 | 华东师范大学 | Method for determining COD of water body by using nano titanium dioxide powder |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102288599A (en) * | 2011-05-13 | 2011-12-21 | 重庆大学 | Associative colorimetric measuring method for total phosphorus and chemical oxygen demand (COD) |
| CN102279123A (en) * | 2011-06-14 | 2011-12-14 | 聚光科技(杭州)股份有限公司 | Pretreatment method and device |
| CN102680461A (en) * | 2012-06-08 | 2012-09-19 | 江南大学 | Chemical oxygen demand (COD) determination method based on chemiluminiscence method of photocatalytic oxidation of nano-TiO2 on (-KMnO4) |
| CN102818778A (en) * | 2012-07-25 | 2012-12-12 | 漳州师范学院 | Method for rapid determination of chemical oxygen demand in environmental water sample |
| CN102818778B (en) * | 2012-07-25 | 2015-08-12 | 闽南师范大学 | A kind of method of Fast Measurement Determination of Chemical Oxygen Demand in Aqueous samples |
| CN103105329A (en) * | 2012-11-06 | 2013-05-15 | 苏州聚阳环保科技有限公司 | Permanganate index digestion method and device in on-line water monitoring |
| CN106092719A (en) * | 2016-08-11 | 2016-11-09 | 贵州开磷质量检测中心有限责任公司 | A kind of method measuring COD by rapid-digestion |
| CN109374559A (en) * | 2018-12-24 | 2019-02-22 | 燕山大学 | A kind of water body COD value measuring method based on ultra-violet absorption spectrum |
| CN109374559B (en) * | 2018-12-24 | 2020-04-07 | 燕山大学 | Water body COD value determination method based on ultraviolet absorption spectrum |
| CN114904586A (en) * | 2022-05-09 | 2022-08-16 | 洛阳莱博图电子科技有限公司 | COD prefabricated reagent for water quality sample determination and preparation method thereof |
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