CN104515769A - High chloride wastewater COD (chemical oxygen demand) rapid determination method - Google Patents
High chloride wastewater COD (chemical oxygen demand) rapid determination method Download PDFInfo
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Abstract
The invention discloses a high chloride wastewater COD (chemical oxygen demand) rapid determination method which comprises the following steps: 1, chloride ion concentration in a water sample is tested; 2, according to the chlorine content, distilled water is added for dilution of the water sample for controlling the chlorine content below 2000mg / L; 3, a COD digestion solution is prepared, to be more specific, 2.65 grams of potassium dichromate is dissolved in a mixed solution of 30 ml of concentrated sulfuric acid and 60 ml of distilled water, the distilled water is added for titrating to 100 ml, and the mixture is mixed with 500 ml of 1% sulfuric acid-silver sulfate solution for storing and standby use; 4, 5 ml of COD the digestion solution is added into the 5 ml of the diluted water sample, or 5ml of the distilled water is added into the 5 ml of the diluted water sample, the diluted water samples are respectively digested by a COD digestion device for 12-25 minutes, and the diluted water samples are cooled to room temperature; and 5, the digested solutions are filled into titration flasks, 2-3 drops of a phenanthroline-iron(II) indicator are added, the digested solutions are titrated by use of 0.05 mol per liter of ammonium ferrous sulfate solution until the solution turns red brown, titration volumes V0 and V1 are recorded, and the method can more fast and accurately detect COD.
Description
Technical field
The invention belongs to waste water COD detection technique field, specifically a kind of method of Fast Measurement high-chloride wastewater COD.
Background technology
The mensuration rapid-digestion spectrophotometric method of prior art mainly traditional potassium dichromate method and water chemical oxygen demand.Tradition potassium dichromate method, that is: add the potassium bichromate solution of known quantity in the sample, in strong acid medium, using silver sulfate as catalyzer, after High-temperature Digestion, use l ferrous ammonium sulfate solution titration.The mensuration rapid-digestion spectrophotometric method of water chemical oxygen demand is unlike clearing up rear colorimetric method for determining COD.Not enough: in industrial waste water, the concentration of chlorion is higher, makes a big impact to experimental result, although add a certain amount of screening agent, effect is not very good; Sulfuric acid has comparatively extensive chemical corrosivity, easily spills or skin ambustion in the process added; Need when potassium dichromate method is cleared up successively to add sample, potassium dichromate, mercuric sulfate, sulfuric acid-silver sulfate solution, distilled water, step is more loaded down with trivial details, and mercuric sulfate is poisonous; Adopt hot plate to clear up, digestion time is longer.Adopt buret to carry out titration, need repeatedly to add l ferrous ammonium sulfate solution, in whole experimentation, the consumption of chemical reagent is all more simultaneously, causes certain waste.The mensuration rapid-digestion spectrophotometric method of water chemical oxygen demand is adopted to overcome the long problem of Traditional Method digestion time, to a certain degree solve the impact of halogen, but when the chlorinity in waste water and COD are at finite concentration, the accuracy of experiment data measured is very low, as table 1, table 2.
Table 1: time sample COD constant (750mg/l), chlorion is on the impact of sample experiments data measured.
Table 2. is diluted to the impact that chlorinity is the sample that 2000mg/l, COD are different, instrument test result.
Table 1 conclusion: when chloride ion content reaches 3000mg/l in waste water, recording COD to experiment has impact.Table 2 conclusion: in waste water, chloride ion content is when 2000mg/l, records COD to experiment when COD is less than 100 and has a significant effect.Experimental result is not very desirable, can produce precipitation and muddy after clearing up, and getting supernatant after centrifugal, to carry out test experiments result error very large.
Summary of the invention
The present invention is directed to prior art deficiency, a kind of method of Fast Measurement high-chloride wastewater COD is provided, overcoming halogen on the basis of the impact of experimental result, improve the operability of experiment, improve the security of experiment; Shorten the time of experiment, increase work efficiency; Avoid the waste of chemical reagent.
In order to solve the problems of the technologies described above, the present invention is solved by following technical proposals: a kind of method of Fast Measurement high-chloride wastewater COD, comprises the following steps: the chlorine ion concentration 1, testing water sample; 2, according to chlorinity, water sample adding distil water is diluted, control chlorinity at below 2000mg/l; 3, COD digestion solution is prepared: get 2.65 grammes per square metre potassium chromates and be dissolved in 30 milliliters of concentrated sulphuric acids and 60 ml distilled water mixed liquors and be titrated to 100 milliliters with distilled water, then mix with 500 milliliters of 1% sulfuric acid-silver sulfate solutions and store for future use; 4, after getting dilution water sample 5 milliliters add 5 milliliters of COD digestion solutions and get dilution after water sample add 5ml distilled water and adopt COD counteract appearance to clear up 12-25 minute respectively, be cooled to room temperature; 5, rear solution will be cleared up be respectively charged in titration bottle and add 2-3 and drip Phen-ferrous indicator, be titrated to the existing rufous of solution by the l ferrous ammonium sulfate solution of 0.05 mole often liter, record titration volumes V0, V1; 6, COD:COD (O2 is calculated, mg/L)=(V0-V1) × C × 8 × 1000 ÷ V, the wherein concentration of C--iron ammonium sulfate standard solution, iron ammonium sulfate standard solution volume when mol/L, V0--titration is blank, ml, iron ammonium sulfate standard solution volume during V1--Titration Water Sample, the volume of ml, V--water sample, ml, 8g/mol--oxygen (1/2O) molal weight.Adopt and overcoming halogen on the basis of the impact of experimental result in this way, improve the operability of experiment, improve the security of experiment; Shorten the time of experiment, increase work efficiency; Avoid the waste of chemical reagent.
In above-mentioned technical method, preferably, the method of the chlorine ion concentration of described test water sample is for getting 2 milliliters of water samples, add 50 ml distilled waters, indicator titration is made with potassium chromate, record the volume V3 of silver nitrate to terminal afterwards, chlorinity=0.1 × 35.45 × V3/2=1.77 V 3, V3--silver nitrate titration number milliliter.
The present invention compared with prior art, has following beneficial effect: adopt and overcoming halogen on the basis of the impact of experimental result in this way, improves the operability of experiment, improves the security of experiment; Shorten the time of experiment, increase work efficiency; Avoid the waste of chemical reagent.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail: a kind of method of Fast Measurement high-chloride wastewater COD, comprises the following steps: the chlorine ion concentration 1, testing water sample; 2, according to chlorinity, water sample adding distil water is diluted, control chlorinity at below 2000mg/l; 3, COD digestion solution is prepared: get 2.65 grammes per square metre potassium chromates and be dissolved in 30 milliliters of concentrated sulphuric acids and 60 ml distilled water mixed liquors and be titrated to 100 milliliters with distilled water, then mix with 500 milliliters of 1% sulfuric acid-silver sulfate solutions and store for future use; 4, after getting dilution water sample 5 milliliters add 5 milliliters of COD digestion solutions and get dilution after water sample add 5ml distilled water and adopt COD counteract appearance to clear up 12-25 minute respectively, be cooled to room temperature; 5, rear solution will be cleared up be respectively charged in titration bottle and add 2-3 and drip Phen-ferrous indicator, be titrated to the existing rufous of solution by the l ferrous ammonium sulfate solution of 0.05 mole often liter, record titration volumes V0, V1; 6, COD:COD (O2 is calculated, mg/L)=(V0-V1) × C × 8 × 1000 ÷ V, the wherein concentration of C--iron ammonium sulfate standard solution, iron ammonium sulfate standard solution volume when mol/L, V0--titration is blank, ml, iron ammonium sulfate standard solution volume during V1--Titration Water Sample, the volume of ml, V--water sample, ml, 8g/mol--oxygen (1/2O) molal weight.Adopt and overcoming halogen on the basis of the impact of experimental result in this way, improve the operability of experiment, improve the security of experiment; Shorten the time of experiment, increase work efficiency; Avoid the waste of chemical reagent.
The method of the chlorine ion concentration of described test water sample is for getting 2 milliliters of water samples, add 50 ml distilled waters, make indicator titration with potassium chromate, record the volume V3 of silver nitrate to terminal afterwards, chlorinity=0.1 × 35.45 × V3/2=1.77 V 3, V3--silver nitrate titration number milliliter.
Claims (2)
1. a method of Fast Measurement high-chloride wastewater COD, is characterized in that comprising the following steps: the chlorine ion concentration of (1), test water sample; (2), according to chlorinity to the dilution of water sample adding distil water, chlorinity is controlled at below 2000mg/l; (3), preparation COD digestion solution: get 2.65 grammes per square metre potassium chromates and be dissolved in 30 milliliters of concentrated sulphuric acids and 60 ml distilled water mixed liquors and be titrated to 100 milliliters with distilled water, then mix with 500 milliliters of 1% sulfuric acid-silver sulfate solutions and store for future use; (4), get dilution after water sample 5 milliliters add 5 milliliters of COD digestion solutions and get dilution after water sample add 5ml distilled water and adopt COD counteract appearance to clear up 12-25 minute respectively, be cooled to room temperature; (5), rear solution will be cleared up be respectively charged in titration bottle and add 2-3 and drip Phen-ferrous indicator, be titrated to the existing rufous of solution by the l ferrous ammonium sulfate solution of 0.05 mole often liter, record titration volumes V0, V1; (6), COD:COD (O2 is calculated, mg/L)=(V0-V1) × C × 8 × 1000 ÷ V, the wherein concentration of C--iron ammonium sulfate standard solution, iron ammonium sulfate standard solution volume when mol/L, V0--titration is blank, ml, iron ammonium sulfate standard solution volume during V1--Titration Water Sample, the volume of ml, V--water sample, ml, 8g/mol--oxygen (1/2O) molal weight.
2. the method for a kind of Fast Measurement high-chloride wastewater COD as claimed in claim 1, it is characterized in that: the method for the chlorine ion concentration of described test water sample is for getting 2 milliliters of water samples, add 50 ml distilled waters, indicator titration is made with potassium chromate, record the volume V3 of silver nitrate to terminal afterwards, chlorinity=0.1 × 35.45 × V3/2=1.77 V 3, V3--silver nitrate titration number milliliter.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| 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 |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03144348A (en) * | 1989-10-30 | 1991-06-19 | Shikoku Chem Corp | Measuring method and reagent for chemical oxygen demand |
| JP2001281220A (en) * | 2000-03-29 | 2001-10-10 | Dkk Toa Corp | Automatic cod measuring device |
| CN101713739A (en) * | 2008-12-05 | 2010-05-26 | 江苏工业学院 | Reagent and method for determining chemical oxygen demand of high-chloride wastewater |
| CN102279183A (en) * | 2011-06-02 | 2011-12-14 | 中国科学院青海盐湖研究所 | Method of detecting COD in high chlorine water with chloride oxygen demand calibration curve-sealed digestion method |
| CN203405441U (en) * | 2013-04-07 | 2014-01-22 | 江西怡杉环保有限公司 | Instrument for detecting COD (chemical oxygen demand) of high-chlorine wastewater on line by basic potassium permanganate method |
| CN103645186A (en) * | 2013-12-24 | 2014-03-19 | 南京中锗科技股份有限公司 | Method for analyzing content of COD (chemical oxygen demand) in sewage with high chloride ion concentration |
-
2014
- 2014-11-27 CN CN201410693246.1A patent/CN104515769B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03144348A (en) * | 1989-10-30 | 1991-06-19 | Shikoku Chem Corp | Measuring method and reagent for chemical oxygen demand |
| JP2001281220A (en) * | 2000-03-29 | 2001-10-10 | Dkk Toa Corp | Automatic cod measuring device |
| CN101713739A (en) * | 2008-12-05 | 2010-05-26 | 江苏工业学院 | Reagent and method for determining chemical oxygen demand of high-chloride wastewater |
| CN102279183A (en) * | 2011-06-02 | 2011-12-14 | 中国科学院青海盐湖研究所 | Method of detecting COD in high chlorine water with chloride oxygen demand calibration curve-sealed digestion method |
| CN203405441U (en) * | 2013-04-07 | 2014-01-22 | 江西怡杉环保有限公司 | Instrument for detecting COD (chemical oxygen demand) of high-chlorine wastewater on line by basic potassium permanganate method |
| CN103645186A (en) * | 2013-12-24 | 2014-03-19 | 南京中锗科技股份有限公司 | Method for analyzing content of COD (chemical oxygen demand) in sewage with high chloride ion concentration |
Non-Patent Citations (5)
| Title |
|---|
| 刘子传 等: "高氯有机废水CODCr的快速测定方法研究", 《实验技术与管理》 * |
| 周言凤: "CODCr测定中微波密封消解快速法与标准法的比较", 《中氮肥》 * |
| 国家环境保护局: "《GB/T 11896-89》", 1 July 1990 * |
| 谢萍 等: "高氯采油废水测定的CODCr质量控制方法研究", 《油气田环境保护》 * |
| 陈爽 等: "程序控温石墨消解仪在测定废水中化学需氧量的应用研究", 《能源环境保护》 * |
Cited By (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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