CN104515769B - A kind of quick measure high-chloride wastewater COD method - Google Patents
A kind of quick measure high-chloride wastewater COD method Download PDFInfo
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Abstract
The invention discloses a kind of quick measure high-chloride wastewater COD method, comprise the following steps：1st, the chlorine ion concentration of water sample is tested；2nd, distilled water diluting is added to water sample according to chlorinity, control chlorinity is in below 2000mg/l；3rd, COD digestion solutions are prepared：Take 2.65 grammes per square metre potassium chromates to be dissolved in 30 milliliters of concentrated sulfuric acids and 60 milliliters of distillation water mixed liquids and 100 milliliters are titrated to distilled water, then mix and store for future use with the silver-colored solution of 500 milliliter of 1% sulfate sulfatase；4th, take after dilution 5 milliliters of water sample to add 5 milliliters of COD digestion solutions and take after dilution water sample to add 5ml distilled water and COD is respectively adopted clears up instrument and clear up 12 25 minutes, be cooled to room temperature；5th, rear solution will be cleared up and be respectively charged into the ferrous indicator of the drop of addition 23 Phen in titration bottle, the existing rufous of solution is titrated to 0.05 mole every liter of l ferrous ammonium sulfate solution, titration volumes V0, V1 is recorded, this method faster accurately can measure COD.
Description
Technical field
The invention belongs to waste water COD detection technique field, specifically a kind of quick measure high-chloride wastewater COD method.
Background technology
Prior art is mainly the measure rapid-digestion AAS of traditional potassium dichromate method and water chemical oxygen demand.
Traditional potassium dichromate method, i.e.,：The potassium bichromate solution of known quantity is added in the sample, in strong acid medium, is made with silver sulfate
For catalyst, after High-temperature Digestion, titrated with l ferrous ammonium sulfate solution.The measure rapid-digestion light splitting light of water chemical oxygen demand
Colorimetric method for determining COD is used after being cleared up unlike degree method.It is not enough：The concentration of chlorion is higher in industrial wastewater, to experimental result
Make a big impact, although add a certain amount of screening agent, but effect is not very good；Sulfuric acid has compared with extensive chemical corrosion
Property, easily spilt or skin ambustion during addition；Need gradually to add sample, dichromic acid when potassium dichromate method is cleared up
Potassium, mercuric sulfate, sulfuric acid-silver sulfate solution, distilled water, step is comparatively laborious, and mercuric sulfate is poisonous；Carried out using hot plate
Clear up, digestion time is longer.Titrated using buret, it is necessary to l ferrous ammonium sulfate solution repeatedly be added, while whole experiment
During chemical reagent consumption it is all more, cause certain waste.Using the measure rapid-digestion of water chemical oxygen demand
AAS overcomes the problem of Traditional Method digestion time is long, and the influence of halogen is solved to a certain degree, but when in waste water
Chlorinity and COD in finite concentration, test data measured accuracy it is very low, such as table 1, table 2.
Table 1：Sample COD is constant（750mg/l）When, influence of the chlorion to sample experiments data measured.
Table 2. is diluted to chlorinity for 2000mg/l, samples different COD, the influence of instrument test result.
The conclusion of table 1：When chloride ion content reaches 3000mg/l in waste water, COD is measured to experiment and had an impact.The conclusion of table 2：
Chloride ion content measures COD to experiment in 2000mg/l, when COD is less than 100 and had a significant effect in waste water.Experimental result is not
It is highly desirable, precipitation can be produced after clearing up and muddy, take supernatant to carry out test experiments result error after centrifugation very big.
The content of the invention
The present invention is in view of the shortcomings of the prior art, a kind of quick measure high-chloride wastewater COD method of offer, is overcoming halogen pair
On the basis of the influence of experimental result, the operability of experiment is improved, the security of experiment is improved；Shorten the time of experiment, carry
High workload efficiency；Avoid the waste of chemical reagent.
In order to solve the above-mentioned technical problem, the present invention is addressed by following technical proposals：One kind quickly determines high chlorine
The method of waste water COD, comprises the following steps：（1）, test water sample chlorine ion concentration；（2）, steaming added to water sample according to chlorinity
Distilled water dilutes, and control chlorinity is in below 2000mg/l；（3）, prepare COD digestion solutions：2.65 grammes per square metre potassium chromates are taken to be dissolved in 30 millis
Rise in the concentrated sulfuric acid and 60 milliliters of distillation water mixed liquids and 100 milliliters are titrated to distilled water, then with 500 milliliters of 1% sulfuric acid-sulfuric acid
Silver-colored solution mixing is stored for future use；（4）, take 5 milliliters of water sample after dilution to add 5 milliliters of COD digestion solutions and take water sample after dilution to add
Enter 5ml distilled water and COD is respectively adopted clears up instrument to clear up 12-25 minutes, be cooled to room temperature；（5）, rear solution will be cleared up fill respectively
Enter and 2-3 drops Phen-ferrous iron indicator is added in titration bottle, be titrated to 0.05 mole every liter of l ferrous ammonium sulfate solution molten
The existing rufous of liquid, record titration volumes V0, V1；（6）, calculate COD：COD=[（V0-V1）× C × 8 × 1000] ÷ V, wherein C--
The concentration of iron ammonium sulfate standard liquid, mol/L, iron ammonium sulfate standard liquid volume, ml, V1-- drops during V0-- titration blank
Determine iron ammonium sulfate standard liquid volume during water sample, ml, the volume of V-- water samples, ml, 8--1/2 oxygen molal weights, g/mol,
COD-- water sample COD values, O2, mg/L, this method be applied to COD contents more than 200mg/L high-chloride wastewater measure.Using
This method improves the operability of experiment on the basis of influence of the halogen to experimental result is overcome, and improves the safety of experiment
Property；Shorten the time of experiment, improve operating efficiency；Avoid the waste of chemical reagent.
In above-mentioned technical method, it is preferred that the method for the chlorine ion concentration of the test water sample is to take 2 milliliters of water samples, plus
50 milliliters of distilled water, indicator titration is made with potassium chromate, to terminal afterwards record silver nitrate volume V3, chlorinity=0.1 ×
35.45 × V3/2=1.77 × V3, V3-- silver nitrate titration volumes, milliliter, the concentration of 0.1-- silver nitrates, 35.45-- chlorine rubs
That quality, g/mol, the volume of 2-- water samples, ml.
The present invention compared with prior art, has the advantages that：Halogen is being overcome to tie experiment in this way
On the basis of the influence of fruit, the operability of experiment is improved, the security of experiment is improved；Shorten the time of experiment, improve work
Efficiency；Avoid the waste of chemical reagent.
Embodiment
The present invention is described in further detail with reference to embodiment：A kind of quick measure high-chloride wastewater COD
Method, comprise the following steps：（1）, test water sample chlorine ion concentration；（2）, according to chlorinity add distilled water dilute water sample
Release, control chlorinity is in below 2000mg/l；（3）, prepare COD digestion solutions：2.65 grammes per square metre potassium chromates are taken to be dissolved in 30 milliliters of dense sulphur
100 milliliters are titrated to distilled water in acid and 60 milliliters of distillation water mixed liquids, then with 500 milliliters of 1% sulfuric acid-silver sulfate solutions
Mixing is stored for future use；（4）, take after dilution 5 milliliters of water sample to add 5 milliliters of COD digestion solutions and take after dilution water sample to add 5ml and steam
COD, which is respectively adopted, in distilled water clears up instrument and clears up 12-25 minutes, is cooled to room temperature；（5）, rear solution will be cleared up be respectively charged into titration bottle
Middle addition 2-3 drops Phen-ferrous iron indicator, solution is titrated to 0.05 mole every liter of l ferrous ammonium sulfate solution existing reddish brown
Color, record titration volumes V0, V1；（6）, calculate COD：COD=[（V0-V1）× C × 8 × 1000] ÷ V, wherein C-- ferrous sulfate
The concentration of ammonium standard liquid, mol/L, iron ammonium sulfate standard liquid volume, ml, during V1-- Titration Water Samples during V0-- titration blank
Iron ammonium sulfate standard liquid volume, ml, the volume of V-- water samples, ml, 8--1/2 oxygen molal weights, g/mol, COD-- water samples
COD value, O2, mg/L, this method be applied to COD contents more than 200mg/L high-chloride wastewater measure.Exist in this way
On the basis of overcoming halogen to the influence of experimental result, the operability of experiment is improved, the security of experiment is improved；Shorten experiment
Time, improve operating efficiency；Avoid the waste of chemical reagent.
The method of the chlorine ion concentration of the test water sample is made to take 2 milliliters of water samples, plus 50 milliliters of distilled water with potassium chromate
Indicator titration, records the volume V3 of silver nitrate, chlorinity=0.1 × 35.45 × V3/2=1.77 × V3, V3-- nitre afterwards to terminal
Sour silver titration volumes, milliliter, the concentration of 0.1-- silver nitrates, the molal weight of 35.45-- chlorine, g/mol, the volume of 2-- water samples,
ml。
Claims (2)
1. a kind of quick measure high-chloride wastewater COD method, it is characterised in that comprise the following steps：(1), test water sample chlorine from
Sub- concentration；(2) distilled water diluting, is added to water sample according to chlorinity, control chlorinity is in below 2000mg/l；(3) COD, is prepared
Digestion solution：Take 2.65 grammes per square metre potassium chromates to be dissolved in 30 milliliters of concentrated sulfuric acids and 60 milliliters of distillation water mixed liquids to be titrated to distilled water
100 milliliters, then mix and store for future use with 500 milliliters of 1% sulfuric acid-silver sulfate solutions；(4) 5 milliliters of water sample after dilution, is taken to add 5
Milliliter COD digestion solutions and take after dilution water sample to add 5ml distilled water and COD is respectively adopted clears up instrument to clear up 12-25 minute, cooling
To room temperature；(5) rear solution, will be cleared up and be respectively charged into addition 2-3 drops Phen-ferrous iron indicator in titration bottle, rubbed with 0.05
The l ferrous ammonium sulfate solution of every liter of that is titrated to the existing rufous of solution, record titration volumes V0, V1；(6) COD, is calculated：COD=
[（V0-V1）× C × 8 × 1000] ÷ V, wherein C-- iron ammonium sulfates standard liquid concentration, mol/L, V0-- titration blank when
Iron ammonium sulfate standard liquid volume, ml, iron ammonium sulfate standard liquid volume during V1-- Titration Water Samples, ml, the body of V-- water samples
Product, ml, 8--1/2 oxygen molal weights, g/mol, COD-- water sample COD values, O2, mg/L, this method exists suitable for COD contents
The measure of more than 200mg/L high-chloride wastewater.
2. a kind of quick measure high-chloride wastewater COD method as claimed in claim 1, it is characterised in that：The test water sample
Chlorine ion concentration method to take 2 milliliters of water samples, plus 50 milliliters of distilled water, make indicator titration with potassium chromate, to terminal after
The volume V3 of record silver nitrate, chlorinity=0.1 × 35.45 × V3/2=1.77 × V3, V3-- silver nitrate titration volumes, milliliter,
The concentration of 0.1-- silver nitrates, the molal weight of 35.45-- chlorine, g/mol, the volume of 2-- water samples, ml.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105445413A (en) * | 2015-12-04 | 2016-03-30 | 江阴秋毫检测有限公司 | Determination method for chemical oxygen demand in water and wastewater |
| CN105548160A (en) * | 2015-12-10 | 2016-05-04 | 苏州国环环境检测有限公司 | Method for testing chemical oxygen demand of water sample through bichromate method |
| CN105424902A (en) * | 2015-12-14 | 2016-03-23 | 北京伊普国际水务有限公司 | COD (chemical oxygen demand) determination method of high-chlorine wastewater |
| CN106053746A (en) * | 2016-06-30 | 2016-10-26 | 浙江大学苏州工业技术研究院 | Method for determining chemical oxygen demand of electrolyzed high chlorine waste water |
| CN107202861A (en) * | 2017-07-05 | 2017-09-26 | 安徽皖仪科技股份有限公司 | A kind of method of COD contents in detection High Cl- water sample |
| CN107449855A (en) * | 2017-08-24 | 2017-12-08 | 浙江环茂自控科技有限公司 | A kind of on-line monitoring method for high-chloride wastewater COD |
| CN112485099A (en) * | 2020-11-23 | 2021-03-12 | 陕西彩虹新材料有限公司 | Preparation method of COD mixed digesting agent |
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Denomination of invention: High chloride wastewater COD (chemical oxygen demand) rapid determination method Effective date of registration: 20200520 Granted publication date: 20171020 Pledgee: Ningbo Yinzhou Rural Commercial Bank Co., Ltd. Chengxi sub branch Pledgor: NINGBO DADI CHEMICAL ENGINEERING AND ENVIRONMENTAL PROTECTION Co.,Ltd. Registration number: Y2020330000253 |
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Date of cancellation: 20220331 Granted publication date: 20171020 Pledgee: Ningbo Yinzhou Rural Commercial Bank Co.,Ltd. Chengxi sub branch Pledgor: NINGBO DADI CHEMICAL ENGINEERING AND ENVIRONMENTAL PROTECTION CO.,LTD. Registration number: Y2020330000253 |
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