CN109781644A - A kind of COD of sewage rapid detection method - Google Patents
A kind of COD of sewage rapid detection method Download PDFInfo
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Abstract
The invention discloses a kind of COD of sewage rapid detection methods, specifically includes the following steps: S1: preparation COD rapid-digestion liquid；S2: preparing the COD standard solution of 20ppm, 40ppm, 80ppm, 150ppm, and 2.00ml is taken to be added in the colorimetric cylinder containing 3.00mlCOD rapid-digestion liquid respectively, cooling after heating, does standard curve with absorbance method；S3: it takes a certain amount of sample to be tested to be diluted to a certain concentration, and does blank assay with pure water；S4: the prepare liquid after taking 2.00ml to dilute is added in the colorimetric cylinder containing 3.00mlCOD rapid-digestion liquid, and does blank assay with pure water, and heating cooling is stood；S5: sewage to be measured is surveyed using Hash ultra-violet and visible spectrophotometer, and combines the standard curve in step S2, sewage CDO to be measured can be measured, further calculate actual sewage COD.Beneficial effects of the present invention: measurement is easy, time-consuming short, and precision accuracy is high.
Description
Technical field
The present invention relates to a kind of COD measuring methods, it particularly relates to a kind of COD of sewage rapid detection method.
Background technique
COD (COD) be evaluate water body organic contamination degree one of important overall target, refer to strong acid simultaneously
The amount of consumed oxidant when using potassium bichromate under heating condition as oxidizer treatment water sample.
The standard method of COD in Wastewater is with China standard GB 11914-1989 and international standard ISO
6060 be representative, and this method oxygenation efficiency is high, and reproducibility is good, accurately and reliably, becomes universally recognized classical standard side, international community
Method.But there is also obvious shortcomings for the classical standard method: reflux unit occupy lab space it is big, water, electric consumption compared with
Greatly, reagent dosage is big, inconvenient, it is difficult to high-volume quickly measurement.
It is further improved on the basis of traditional National Standard Method, proposes decrement National Standard Method.Although reducing reagent consumption,
The generation for reducing the pollutants such as spent acid and heavy metal, reduces costs, but time-consuming longer, cumbersome drawback is still deposited
?.
Summary of the invention
For above-mentioned technical problem in the related technology, the present invention proposes a kind of COD of sewage rapid detection method, solves existing
There is National Standard Method to survey the COD bring problem that time-consuming, cumbersome.
To realize the above-mentioned technical purpose, the technical scheme of the present invention is realized as follows:
A kind of COD of sewage rapid detection method, specifically includes the following steps:
S1: it preparation COD rapid-digestion liquid: silver sulfate, sulfuric acid, chromic acid, mercuric sulfate is weighed by mass fraction is sufficiently mixed and shake up；
S2: different volumes each 100ml of COD standard solution of four kinds of concentration of preparation: are separately added into the volumetric flask of four 100ml
1000ppmCOD standard solution, constant volume simultaneously shakes up, and stands；
S3: the COD standard solution of be prepared in step S2 four kinds of various concentrations is taken and is quantitatively added separately to four and contains
In the colorimetric cylinder of COD rapid-digestion liquid, separately takes a colorimetric cylinder to do blank assay, shake up heating, cooling and standings；
S4: four kind are distinguished made from measuring process S3 on Hash ultra-violet and visible spectrophotometer with unicast regular way (420nm)
Absorbance-concentration values are carried out linear fit, obtain COD solution standard curve by the absorbance of standard coloration liquid；
S5: being taken to sample to volumetric flask with pipette, be diluted with water to a certain concentration, shaken up, and is stood；
S6: it takes the quantitative sewage to be measured in step S5 to be put into the colorimetric cylinder containing COD rapid-digestion liquid, separately takes a colorimetric
Pipe is added pure water and does blank assay, shakes up heating, cooling and standings；
S7: sewage absorbance to be measured is measured with Hash ultra-violet and visible spectrophotometer, in conjunction with absorbance-concentration in step S4
Numerical curve obtains COD of sewage to be measured, is further calculated according to formula and obtains actual sewage COD, actual sewage COD=dirt to be measured
Water COD* extension rate.
Further, the mass fraction of silver sulfate, sulfuric acid, chromic acid, mercuric sulfate is taken to be respectively as follows: silver sulfate 0.6- in step S1
0.7%, sulfuric acid 80-85%, chromic acid 0.05%, mercuric sulfate 0.8-0.9%.
Further, the specific preparation method of 1000ppmCOD standard solution described in step S2 are as follows: weigh dry neighbour
Potassium hydrogen phthalate 0.4251g is in small beaker, after being dissolved with water, is transferred in 500.00 ml volumetric flasks, is diluted with water to quarter
Degree, shakes up, and is made into the standard solution that COD is 1000ppm.
Further, COD standard solution described in step S2 is configured using Potassium Hydrogen Phthalate and ultrapure water.
Further, the theoretical concentration value of the four kinds of concentration C OD standard solution prepared in step S2 be respectively as follows: 20ppm,
40ppm、80ppm、150ppm。
Further, the COD rapid-digestion liquid being added in step S3 and S6 is 3.00ml, the COD being added in step S3
The amount for the sewage to be measured being added in standard solution and step S6 is 2.00ml.
Further, heating time is 15-25 minutes in step S3 and S6, and heating temperature is 150-170 DEG C
Further, step S4 standard curve correction coefficient of determination is greater than 0.99, it is preferred that correction coefficient of determination is more than or equal to
0.995。
Further, the multiple being diluted with water in step S5 is 1-10 times.
Beneficial effects of the present invention: clearing up organic matter in water sample using high temperature, and Hash ultraviolet-visible is divided light
Degree meter measurement COD of sewage concentration.It is compared with the traditional method, this method can be with mass detection, and easy to operate, analysis time is significantly
Shorten, and preci-sion and accuracy is also higher, realizes the unification of reliability and high efficiency.
Detailed description of the invention
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only some implementations of the invention
Example, for those of ordinary skill in the art, without creative efforts, can also obtain according to these attached drawings
Obtain other attached drawings.
Fig. 1 is the according to embodiments of the present invention 1 COD solution standard curve；
Fig. 2 is the according to embodiments of the present invention 2 COD solution standard curves；
Fig. 3 is the according to embodiments of the present invention 3 COD solution standard curves.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with specific embodiment, it is clear that described
Embodiment be only a part of the embodiment of the present invention, instead of all the embodiments.The embodiment is only used for explaining this hair
It is bright, it is not used in the limitation present invention.
Preparing experiment 1: heating
Heater power source is plugged, button is turned on the switch, sets the time 20 minutes, 165 DEG C of temperature, is started to warm up.
Preparing experiment 2:COD titer is prepared
Dry Potassium Hydrogen Phthalate 0.4251g is weighed in small beaker, after being dissolved with water, is transferred to 500.00 ml capacity
In bottle, it is diluted with water to scale, is shaken up.It is made into 1000ppmCOD standard solution.
Embodiment 1:
S1: taking the volumetric flask of four 100.00ml, is separately added into the 1000ppmCOD standard solution of different volumes, additional amount difference
For 2.00ml, 4.00ml, 8.00ml, 15.00ml.Configured concentration is respectively 20ppm, 40ppm, 80ppm, 150ppm；
S2: the titer and 3.00mlCOD rapid-digestion liquid for taking 2.00ml above-mentioned steps to prepare respectively, which are added in COD colorimetric cylinder, to be shaken
It is even, while the configured RO water of 5ml separately being taken to be added in COD colorimetric cylinder blank pipe as blank, 165 DEG C of heating 20min, after having heated
It is cooled to room temperature；
S3: the suction of each standard coloration liquid is measured respectively on Hash ultra-violet and visible spectrophotometer with unicast regular way (420nm)
Luminosity is first zeroed with blank before measurement.Absorbance-concentration values are inputted into instrument, carry out linear fit, obtain COD solution mark
Directrix curve.Curvature correction coefficient of determination is 0.9969, and linear relationship is fine, and description standard curve is qualified, the standard of acquisition
Curve graph is as shown in Figure 1；
S4: sewage 20.00ml is taken with pipette, 100.00ml volumetric flask is transferred to, is diluted with water to scale, shake up；
S5: take the sewage 2.00ml after diluting in step S4, self-control COD rapid-digestion liquid 3.00ml that COD ratio is added with pipette
It in colour tube pipe, shakes up, while 5.00ml pure water being taken to do blank assay；It will be cold after 165 DEG C of heating 20min of sewage to be measured and blank
But to room temperature；
S6: COD of sewage concentration is measured with Hash ultra-violet and visible spectrophotometer, is first zeroed with blank sample, then survey in prepare liquid
COD, reading is 16.5, COD of sewage actual value CIt is practicalIt can be according to COD value C in prepare liquidIt is to be measuredIt is calculated with following formula:, after abbreviation:, calculating actual sewage COD accordingly is 82.5ppm.
Embodiment 2:
S1: taking the volumetric flask of four 100.00ml, is separately added into the 1000ppmCOD standard solution of different volumes, additional amount difference
For 2.00ml, 4.00ml, 8.00ml, 15.00ml.Configured concentration is respectively 20ppm, 40ppm, 80ppm, 150ppm；
S2: the titer and 3.00mlCOD rapid-digestion liquid for taking 2.00ml above-mentioned steps to prepare respectively, which are added in COD colorimetric cylinder, to be shaken
It is even, while the configured RO water of 5ml separately being taken to be added in COD colorimetric cylinder blank pipe as blank, 165 DEG C of heating 20min, after having heated
It is cooled to room temperature；
S3: the suction of each standard coloration liquid is measured respectively on Hash ultra-violet and visible spectrophotometer with unicast regular way (420nm)
Luminosity is first zeroed with blank before measurement.Absorbance-concentration values are inputted into instrument, carry out linear fit, obtain COD solution mark
Directrix curve.Curvature correction coefficient of determination is 0.9975, and linear relationship is fine, and description standard curve is qualified, the standard of acquisition
Curve graph is as shown in Figure 2；
S4: sewage 50.00ml is taken with pipette, 100.00ml volumetric flask is transferred to, is diluted with water to scale, shake up；
S5: take the sewage 2.00ml after diluting in step S4, self-control COD rapid-digestion liquid 3.00ml that COD ratio is added with pipette
It in colour tube pipe, shakes up, while 5.00ml pure water being taken to do blank assay；It will be cold after 165 DEG C of heating 20min of sewage to be measured and blank
But to room temperature；
S6: COD of sewage concentration is measured with Hash ultra-violet and visible spectrophotometer, is first zeroed with blank sample, then survey in prepare liquid
COD, reading is 40, COD of sewage actual value CIt is practicalIt can be according to COD value C in prepare liquidIt is to be measuredIt is calculated with following formula:, after abbreviation:, calculating actual sewage COD accordingly is 80ppm.
Embodiment 3:
S1: taking the volumetric flask of four 100.00ml, is separately added into the 1000ppmCOD standard solution of different volumes, additional amount difference
For 2.00ml, 4.00ml, 8.00ml, 15.00ml.Configured concentration is respectively 20ppm, 40ppm, 80ppm, 150ppm；
S2: the titer and 3.00mlCOD rapid-digestion liquid for taking 2.00ml above-mentioned steps to prepare respectively, which are added in COD colorimetric cylinder, to be shaken
It is even, while the configured RO water of 5ml separately being taken to be added in COD colorimetric cylinder blank pipe as blank, 165 DEG C of heating 20min, after having heated
It is cooled to room temperature；
S3: the suction of each standard coloration liquid is measured respectively on Hash ultra-violet and visible spectrophotometer with unicast regular way (420nm)
Luminosity is first zeroed with blank before measurement.Absorbance-concentration values are inputted into instrument, carry out linear fit, obtain standard curve.
Curvature correction coefficient of determination be 0.9977, linear relationship is fine, description standard curve be it is qualified, the canonical plotting of acquisition is such as
Shown in Fig. 3；
S4: sewage 25.00ml is taken with pipette, 100.00ml volumetric flask is transferred to, is diluted with water to scale, shake up；
S5: take the sewage 2.00ml after diluting in step S4, self-control COD rapid-digestion liquid 3.00ml that COD ratio is added with pipette
It in colour tube pipe, shakes up, while 5.00ml pure water being taken to do blank assay；It will be cold after 165 DEG C of heating 20min of sewage to be measured and blank
But to room temperature；
S6: COD of sewage concentration is measured with Hash ultra-violet and visible spectrophotometer, is first zeroed with blank sample, then survey in prepare liquid
COD, reading is 19.5, COD of sewage actual value CIt is practicalIt can be according to COD value C in prepare liquidIt is to be measuredIt is calculated with following formula:, after abbreviation:, calculating actual sewage COD accordingly is 78ppm.
The existing process using National Standard Method GB11914-1989 measurement is illustrated below:
Embodiment 4:(potassium bichromate National Standard Method experiment)
Agents useful for same is analytical reagents that meet national standards when experiment, and test water is distilled water or comparable purity
Water.
Silver sulfate (Ag2SO4), chemistry is pure.
Mercuric sulfate (Hg SO4), chemistry is pure.
Sulfuric acid (H2SO4), ρ=1.84g/ml.
Silver sulfate-sulphate reagent: 10.0g silver sulfate being added into 1L sulfuric acid, places 1~2 day and is allowed to dissolve, and mixes,
Use preceding careful shake.
Potassium bichromate standard solution: concentration C(1/6K2Cr2O7The potassium bichromate standard solution of)=0.250mol/L: will
Potassium bichromate of the 12.258g after 105 DEG C of dry 2h is soluble in water, is diluted to 1000mL.
Iron ammonium sulfate standard titration solution: concentration is C ((NH4)2Fe(SO4)2·6H2O) ≈ 0.10mol/L sulfuric acid it is sub-
Iron ammonium standard titration solution: dissolution 39g iron ammonium sulfate ((NH4)2Fe(SO4)2·6H2O) Yu Shuizhong, 20.00ml sulfuric acid is added,
1000ml is diluted to after its solution is cooling.
Ferroin indicator: 1,10- phenanthroline (1,10-phenathroline monohy drate) indicator is molten
Liquid: dissolution 0.7g green vitriol (FeSO4·7H2O) in the water of 50mL, 1.5g1 is added, 10- phenanthroline, agitation is extremely
Dissolution, is diluted with water to 100mL.
S1: taking 20.00ml sewage sample in conical flask, and 10.00mL potassium bichromate standard solution, 0.4g mercuric sulfate is added
It is shaken up with several anti-bumping beades；
S2: conical flask is connected to reflux unit condenser pipe lower end, connects condensed water.30.00mL is slowly added to from condenser pipe upper end
Silver sulfate-sulphate reagent, to prevent the evolution of low-boiling-point organic compound, continuous turn conical flask is allowed to uniformly mixed.It is opened from solution
Beginning, which has boiled, flows back two hours；
S3: after cooling, after rinsing condenser pipe with 20.00~30.00mL water autocondensation pipe upper end, conical flask is removed, then dilute with water
Release to 140.00mL or so；
S4: after solution is cooled to room temperature, 3 drop 1,10- phenanthroline indicator solution are added, with iron ammonium sulfate standard titration solution
Titration, it is terminal that the color of solution, which has yellow to become bronzing through blue-green,.Write down iron ammonium sulfate standard titration solution
Consume ml V2=23.00ml；
S5: it blank test: repeats above-mentioned S1-S4 step and replaces sewage sample to carry out blank test with 20ml water, record blank
Ml V of iron ammonium sulfate standard solution is consumed when titration1=25.00ml, COD of sewage calculation formula:,
In formula: C-iron ammonium sulfate standard titration solution concentration, mol/L；
V1The volume of consumption iron ammonium sulfate standard titration solution, mL consumed by-blank test；
V2The volume of consumption iron ammonium sulfate standard titration solution, mL consumed by-sampling test；
V0--- the volume of sewage sample, mL； 8000——1/4 O2Molal weight using mg/L as unit scaled value.
Calculating COD of sewage accordingly is 80.0ppm.
It in summary it can be seen, the application spectrophotometric rapid test method embodiment 1-3 measures embodiment 4 compared to National Standard Method
For, organic matter in water sample to be cleared up using high temperature, Hash ultra-violet and visible spectrophotometer measures COD of sewage concentration,
Operation is more easy, while reducing the generation of the pollutants such as spent acid and heavy metal, time-consuming short, and preci-sion and accuracy
It is higher, realize the unification of reliability and high efficiency.
Claims (9)
1. a kind of COD of sewage rapid detection method, which is characterized in that specifically includes the following steps:
S1: it preparation COD rapid-digestion liquid: silver sulfate, sulfuric acid, chromic acid, mercuric sulfate is weighed by mass fraction is sufficiently mixed and shake up；
S2: different volumes each 100ml of COD standard solution of four kinds of concentration of preparation: are separately added into the volumetric flask of four 100ml
1000ppmCOD standard solution, constant volume simultaneously shakes up, and stands；
S3: the COD standard solution of be prepared in step S2 four kinds of various concentrations is taken and is quantitatively added separately to four and contains
In the colorimetric cylinder of COD rapid-digestion liquid, separately takes a colorimetric cylinder to do blank assay, shake up heating, cooling and standings；
S4: four kind are distinguished made from measuring process S3 on Hash ultra-violet and visible spectrophotometer with unicast regular way (420nm)
Absorbance-concentration values are carried out linear fit, obtain COD solution standard curve by the absorbance of standard coloration liquid；
S5: being taken to sample to volumetric flask with pipette, be diluted with water to a certain concentration, shaken up, and is stood；
S6: it takes the quantitative sewage to be measured in step S5 to be put into the colorimetric cylinder containing COD rapid-digestion liquid, separately takes a colorimetric
Pipe is added pure water and does blank assay, shakes up heating, cooling and standings；
S7: sewage absorbance to be measured is measured with Hash ultra-violet and visible spectrophotometer, in conjunction with absorbance-concentration in step S4
Numerical curve obtains COD of sewage to be measured, is further calculated according to formula and obtains actual sewage COD, actual sewage COD=dirt to be measured
Water COD* extension rate.
2. a kind of COD of sewage rapid detection method according to claim 1, which is characterized in that taken in step S1 silver sulfate,
Sulfuric acid, chromic acid, mercuric sulfate mass fraction be respectively as follows: silver sulfate 0.6-0.7%, sulfuric acid 80-85%, chromic acid 0.05%, mercuric sulfate
0.8-0.9%。
3. a kind of COD of sewage rapid detection method according to claim 1, which is characterized in that described in step S2
The specific preparation method of 1000ppmCOD standard solution are as follows: weigh dry Potassium Hydrogen Phthalate 0.4251g in small beaker
In, it after being dissolved with water, is transferred in 500.00 ml volumetric flasks, is diluted with water to scale, shakes up, being made into COD is 1000ppm's
Standard solution.
4. a kind of COD of sewage rapid detection method according to claim 1, which is characterized in that the mark of COD described in step S2
Quasi- solution is configured using Potassium Hydrogen Phthalate and ultrapure water.
5. a kind of COD of sewage rapid detection method according to claim 1, which is characterized in that four prepared in step S2
The theoretical concentration value of kind concentration C OD standard solution is respectively as follows: 20ppm, 40ppm, 80ppm, 150ppm.
6. a kind of COD of sewage rapid detection method according to claim 1, which is characterized in that be added in step S3 and S6
COD rapid-digestion liquid be 3.00ml, the sewage to be measured being added in the COD standard solution and step S6 being added in step S3
Amount is 2.00ml.
7. a kind of COD of sewage rapid detection method according to claim 1, which is characterized in that heated in step S3 and S6
Time is 15-25 minutes, and heating temperature is 150-170 DEG C.
8. a kind of COD of sewage rapid detection method according to claim 1, which is characterized in that step S4 standard curve
It corrects coefficient of determination and is greater than 0.99.
9. a kind of COD of sewage rapid detection method according to claim 1, which is characterized in that be diluted with water in step S5
Multiple be 1-10 times.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110646413A (en) * | 2019-09-27 | 2020-01-03 | 常州罗盘星检测科技有限公司 | Reagent for rapidly detecting calcium hardness concentration in water and use method thereof |
| CN112051317A (en) * | 2019-08-05 | 2020-12-08 | 广东上智环保科技有限公司 | COD on-line detection method and equipment |
| CN113340827A (en) * | 2021-05-07 | 2021-09-03 | 山东上远环保科技有限公司 | Method for detecting concentration of deoxidant |
| CN114199798A (en) * | 2021-11-12 | 2022-03-18 | 葛洲坝水务温岭有限公司 | Method for rapidly measuring high-range COD |
| CN114199797A (en) * | 2021-11-12 | 2022-03-18 | 葛洲坝水务温岭有限公司 | Method for rapidly measuring low-range COD |
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| CN101539526A (en) * | 2009-04-09 | 2009-09-23 | 同济大学 | Method for preparing prefabricated reagent for fast measuring COD in water body and application thereof |
| CN108318618A (en) * | 2018-01-31 | 2018-07-24 | 天津亿利科能源科技发展股份有限公司 | One kind being suitable for the high chlorine root sanitary sewage COD rapid detection methods of production platform |
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| CN101539526A (en) * | 2009-04-09 | 2009-09-23 | 同济大学 | Method for preparing prefabricated reagent for fast measuring COD in water body and application thereof |
| CN108318618A (en) * | 2018-01-31 | 2018-07-24 | 天津亿利科能源科技发展股份有限公司 | One kind being suitable for the high chlorine root sanitary sewage COD rapid detection methods of production platform |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112051317A (en) * | 2019-08-05 | 2020-12-08 | 广东上智环保科技有限公司 | COD on-line detection method and equipment |
| CN112051317B (en) * | 2019-08-05 | 2022-07-15 | 广东上智环保科技有限公司 | COD on-line detection method and equipment |
| CN110646413A (en) * | 2019-09-27 | 2020-01-03 | 常州罗盘星检测科技有限公司 | Reagent for rapidly detecting calcium hardness concentration in water and use method thereof |
| CN113340827A (en) * | 2021-05-07 | 2021-09-03 | 山东上远环保科技有限公司 | Method for detecting concentration of deoxidant |
| CN114199798A (en) * | 2021-11-12 | 2022-03-18 | 葛洲坝水务温岭有限公司 | Method for rapidly measuring high-range COD |
| CN114199797A (en) * | 2021-11-12 | 2022-03-18 | 葛洲坝水务温岭有限公司 | Method for rapidly measuring low-range COD |
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