CN107202861A - A kind of method of COD contents in detection High Cl- water sample - Google Patents
A kind of method of COD contents in detection High Cl- water sample Download PDFInfo
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- CN107202861A CN107202861A CN201710540374.6A CN201710540374A CN107202861A CN 107202861 A CN107202861 A CN 107202861A CN 201710540374 A CN201710540374 A CN 201710540374A CN 107202861 A CN107202861 A CN 107202861A
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- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
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- G—PHYSICS
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Abstract
The invention discloses a kind of method for detecting COD contents in High Cl- water sample, it can fast and accurately detect the COD contents in Water Sample Containing High Concentration of Cl, and favorable reproducibility.This method is applied to monitoring water quality on line apparatus field, can solve the problem that in national standard because chloride ion content is high and can not Accurate Determining COD value present situation.Particularly it is used for special industry（Leather and fur products, waste incineration）The laboratory manual inspection or monitoring water quality on line equipment of waste water.
Description
Technical field
The invention belongs to analytical chemistry field, more particularly to a kind of method for detecting COD contents in High Cl- water sample.
Background technology
COD, that is, COD, refer under certain condition, handle through potassium dichromate oxidation, the dissolving in water sample
The mass concentration of the property material oxygen corresponding with the potassium bichromate that suspension is consumed, 1mol potassium bichromate (1/6K2Cr2O7)
Equivalent to 1mol oxygen (1/2O).It is used to react the degree that water body is polluted by reducing substances, can be used as organic matter relative amount
Overall target；Meanwhile, we are national to have been carried out overall control for environmental protection to COD, is water quality prison
Survey one of project that industry must be surveyed.At present, it is national standard method COD to be determined using potassium dichromate method, is being determined
During COD, silver sulfate is added as catalyst, in sulfuric acid medium, clears up and will have in water sample in heating under certain temperature
Machine thing is aoxidized, and then determines the amount of remaining potassium bichromate by corresponding method again, and calculates COD value.Existing measure side
The method that method all uses dilution for the water sample of high chloride ion, then adds mercury salt with chlorion formation complex compound to eliminate
The interference of chlorion, but the COD value in water sample is also diluted while dilution Chloride Ion In Water, cause COD concentration relatively low,
During detection, measuring result error is larger, and reappearance is poor.
The content of the invention
Present invention seek to address that the water sample detection resultant error that COD contents are relatively low and chlorine ion concentration is higher is larger, reappear
The poor method of property.Described method passes through m [HgSO in mass ratio4]：m[Cl]≥20：1 ratio adds appropriate mercuric sulfate
The chlorion in water sample is sheltered, while debita spissitudo and the potassium bichromate and silver sulfate-sulfuric acid solution of respective volume are added, heating
Back flow reaction is to detect the COD value in Water Sample Containing High Concentration of Cl.The inventive method degree of accuracy is high, favorable reproducibility, mark-on reclaims
Rate meets the requirements.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of method of COD contents in detection High Cl- water sample, it is characterised in that comprise the following steps：
(1) preparation of COD=5000mg/L standard reserving solutions
It is accurate to weigh 4.2510g Potassium Hydrogen Phthalates and be put into clean beaker, add ultra-pure water and stir to being completely dissolved,
It is then transferred in 1000ml volumetric flask, beaker is cleaned with pure water three times, cleaning fluid is also poured into above-mentioned volumetric flask, Ran Houding
Hold to scale, shake up stand-by；
(2) preparation of different type water sample
A, preparation blank sample a：Electrical conductivity >=18.25M Ω cm and ultraviolet-sterilization ultra-pure water；
B, take High Cl- water sample b；
(3) a, b water sample described in step (2) are respectively taken in 20ml to 250ml conical flask, add 10 a diameter of 3mm
Bead；Heating reflux reaction naturally cools to room temperature after 2 hours at ambient pressure, adds ultra-pure water 80ml, shakes up, quiet
Put, it is to be measured；Add 3 to drip after ferroin indicator, titrated with iron ammonium sulfate, the body then consumed according to iron ammonium sulfate
Product calculates the COD value of each water sample.
The method of COD contents in a kind of described detection High Cl- water sample, it is characterised in that：Described Potassium Hydrogen Phthalate
For top pure grade, need to dry 2~2.5 hours at 100~105 DEG C before use.
The method of COD contents in a kind of described detection High Cl- water sample, it is characterised in that：Mercuric sulfate addition is 1.2g；
Potassium bichromate concentration is 0.272mol/L, and volume is 10ml；Silver sulfate-sulfuric acid concentration is 6.7g/L, and volume is 30ml；Sulfuric acid is sub-
Iron ammonium concentration is 0.1mol/L.
A kind of method of COD contents in detection high-chloride wastewater, it is characterized in that：
(1) preparation (COD=5000mg/L) of standard reserving solution
The accurate 4.2510g Potassium Hydrogen Phthalates (top pure grade, 100~105 DEG C drying 2 hours) that weigh are put into clean beaker
In, ultra-pure water (ultra-pure water of electrical conductivity >=18.25M Ω cm and ultraviolet-sterilization) stirring is added to being completely dissolved, and is then shifted
Into 1000ml volumetric flask, scale is dissolved to, is shaken up stand-by；
(2) preparation of different type water sample
A, blank sample：Electrical conductivity ＞ 18.25M Ω cm and ultraviolet-sterilization ultra-pure water；
B, high chlorine actual water sample：
High Cl- water sample (garbage burning factory Sewage outlet water sample) is taken, chloride ion content is more than 15000mg/L；
C, High Cl- water sample mark-on COD=25mg/L actual water sample：
2.5ml COD=5000mg/L standard reserving solution is accurately pipetted with pipette, 500ml volumetric flask is poured into
In, scale then is settled to high chlorine actual water sample described in b, shakes up stand-by, the mark-on COD=25mg/L of High Cl- water sample is obtained
Actual water sample.
D, high chlorine actual water sample：
High Cl- water sample (Leather Goods Factory's Sewage outlet water sample) is taken, chloride ion content is more than 18000mg/L；
E, High Cl- water sample mark-on COD=100mg/L actual water sample：
10.0ml COD=5000mg/L standard reserving solution is accurately pipetted with pipette, 500ml volumetric flask is poured into
In, scale then is settled to high chlorine actual water sample described in d, shakes up stand-by, the mark-on COD=100mg/ of High Cl- water sample is obtained
L actual water sample.
(3) different type volume of water sample is 20ml；
(4) mercuric sulfate addition is 1.2g；
(5) potassium bichromate concentration is 0.272mol/L, and volume is 10ml；
(6) silver sulfate-sulfuric acid concentration is 6.7g/L, and volume is 30ml；
(7) ferrous ammonium sulfate concentration is 0.1mol/L；
The different types of water sample of a, b, c, d, e described in step (2) is respectively taken in 20ml to 250ml conical flask, is added
10 a diameter of 3mm bead；Heating reflux reaction is naturally cooled to after room temperature after 2 hours at ambient pressure, adds ultra-pure water
80ml, shakes up, stands, to be measured；Acid buret is used after adding the real ferroin of 3 drops, is titrated with iron ammonium sulfate, Ran Houyi
The volume consumed according to iron ammonium sulfate calculates the COD value of each water sample.
Beneficial effects of the present invention：
A kind of method for detecting COD contents in High Cl- water sample of the present invention can fast and accurately detect highly concentrated
The COD contents spent in chlorion water sample, and favorable reproducibility.This method is applied to monitoring water quality on line apparatus field, can be solved
Certainly in national standard because chloride ion content is high and can not Accurate Determining COD value present situation.Particularly it is used for special industry (leather
Product, waste incineration) waste water laboratory manual inspection or monitoring water quality on line equipment.
Embodiment
The present invention can be explained in more detail by the following examples：
1st, the detection of the degree of accuracy：
(1) preparation (COD=5000mg/L) of standard reserving solution
The accurate 4.2510g Potassium Hydrogen Phthalates (top pure grade, 100~105 DEG C drying 2 hours) that weigh are put into clean beaker
In, ultra-pure water (ultra-pure water of electrical conductivity ＞ 18.25M Ω cm and ultraviolet-sterilization) stirring is added to being completely dissolved, and is then shifted
Into 1000ml volumetric flask, scale is dissolved to, is shaken up stand-by；
(2) preparation of different type standard liquid or water sample
A, blank sample：Electrical conductivity ＞ 18.25M Ω cm and ultraviolet-sterilization ultra-pure water；
B, COD=50mg/L without chlorion standard liquid：
5.0ml COD=5000mg/L standard reserving solution is accurately pipetted with pipette, 500ml volumetric flask is poured into
In, with pure water dilution be dissolved to scale, shake up it is stand-by, obtain COD=50mg/L without chlorion standard liquid；C, COD=50mg/L
And chloride ion-containing 20000mg/L standard liquid：
It is accurate to weigh 32.9577g sodium chloride (NaCl) and be put into beaker, add pure water and stir to being completely dissolved, Ran Houzhuan
In the volumetric flask for moving to 1000ml；10.0ml COD=5000mg/L standard reserving solution is accurately pipetted with pipette again, is poured into
Into 1000ml volumetric flask, scale is dissolved to pure water dilution, shakes up stand-by, obtains COD=50mg/L chloride ion-containing
20000mg/L standard liquid；
D, high chlorine actual water sample：
High Cl- water sample (garbage burning factory Sewage outlet water sample) is taken, chloride ion content is more than 15000mg/L；
E, High Cl- water sample mark-on COD=25mg/L actual water sample：
2.5ml COD=5000mg/L standard reserving solution is accurately pipetted with pipette, 500ml volumetric flask is poured into
In, scale then is settled to high chlorine actual water sample described in d, shakes up stand-by, the mark-on COD=25mg/L of High Cl- water sample is obtained
Actual water sample.
F, high chlorine actual water sample：
High Cl- water sample (Leather Goods Factory's Sewage outlet water sample) is taken, chloride ion content is more than 18000mg/L；
G, High Cl- water sample mark-on COD=100mg/L actual water sample：
10.0ml COD=5000mg/L standard reserving solution is accurately pipetted with pipette, 500ml volumetric flask is poured into
In, scale then is settled to high chlorine actual water sample described in f, shakes up stand-by, the mark-on COD=100mg/ of High Cl- water sample is obtained
L actual water sample.
(3) different type volume of water sample is 20ml；
(4) mercuric sulfate addition is 1.2g；
(5) potassium bichromate concentration is 0.272mol/L, and volume is 10ml；
(6) silver sulfate-sulfuric acid concentration is 6.7g/L, and volume is 30ml；
(7) ferrous ammonium sulfate concentration is 0.1mol/L；
The different types of standard liquid of a, b, c, d, e, f, g or water sample described in step (2) respectively take 20ml to 250ml taper
In bottle, 10 a diameter of 3mm bead is added；Heating reflux reaction is naturally cooled to after room temperature after 2 hours at ambient pressure,
Ultra-pure water 80ml is added, shakes up, stand, to be measured；Acid buret is used after adding the real ferroin of 3 drops, iron ammonium sulfate is used
Titration, then calculates each standard liquid or the COD value of water sample according to the volume that iron ammonium sulfate is consumed.
Degree of accuracy testing result is shown in Table 1
2nd, the detection of reappearance：
(1) preparation (COD=5000mg/L) of standard reserving solution
The accurate 4.2510g Potassium Hydrogen Phthalates (top pure grade, 105 DEG C drying 2 hours) that weigh are put into clean beaker, plus
Enter pure water to stir to being completely dissolved, be then transferred in 1000ml volumetric flask, be dissolved to scale, shake up stand-by；
(2) preparation of different type standard liquid or water sample
A, blank sample：Electrical conductivity ＞ 18.25M Ω cm and ultraviolet-sterilization ultra-pure water；
B, COD=50mg/L and chloride ion-containing 20000mg/L standard liquid：
It is accurate to weigh 32.9577g sodium chloride (NaCl) and be put into beaker, add pure water and stir to being completely dissolved, Ran Houzhuan
In the volumetric flask for moving to 1000ml；10.0ml COD=5000mg/L standard reserving solution is accurately pipetted with pipette again, is poured into
Into 1000ml volumetric flask, scale is dissolved to pure water dilution, shakes up stand-by, obtains COD=50mg/L chloride ion-containing
20000mg/L standard liquid；
C, high chlorine actual water sample：
High Cl- water sample (garbage burning factory Sewage outlet water sample) is taken, chloride ion content is more than 15000mg/L；
D, high chlorine actual water sample：
High Cl- water sample (Leather Goods Factory's Sewage outlet water sample) is taken, chloride ion content is more than 18000mg/L；
(3) different type volume of water sample is 20ml；
(4) mercuric sulfate addition is 1.2g；
(5) potassium bichromate concentration is 0.272mol/L, and volume is 10ml；
(6) silver sulfate-sulfuric acid concentration is 6.7g/L, and volume is 30ml；
(7) ferrous ammonium sulfate concentration is 0.1mol/L；
Different types of standard liquid or water sample described in step (2) are respectively taken in 20ml to 250ml conical flask, add 10
A diameter of 3mm bead；Heating reflux reaction is naturally cooled to after room temperature after 2 hours at ambient pressure, adds ultra-pure water
80ml, shakes up, stands, to be measured；Acid buret is used after adding the real ferroin of 3 drops, is titrated with iron ammonium sulfate, Ran Houyi
The volume consumed according to iron ammonium sulfate calculates each standard liquid or the COD value of water sample.
Repeated testing result is shown in Table 2, table 3 and table 4
Table 1
Table 2 (high chlorine standard liquid repeatability)
Table 3 (garbage burning factory Sewage outlet water sample repeatability)
Table 4 (Leather Goods Factory's Sewage outlet water sample repeatability)
Claims (3)
1. a kind of method for detecting COD contents in High Cl- water sample, it is characterised in that comprise the following steps：
（1）The preparation of COD=5000mg/L standard reserving solutions
Accurately weigh 4.2510g Potassium Hydrogen Phthalates to be put into clean beaker, add ultra-pure water and stir to being completely dissolved, then
It is transferred in 1000ml volumetric flask, beaker is cleaned with pure water three times, cleaning fluid is also poured into above-mentioned volumetric flask, is then settled to
Scale, shakes up stand-by；
（2）The preparation of different type water sample
A, preparation blank sample a：Electrical conductivity >=18.25M Ω cm and ultraviolet-sterilization ultra-pure water；
B, take High Cl- water sample b；
（3）Step（2）Described in a, b water sample respectively take in 20ml to 250ml conical flask, add 10 a diameter of 3mm glass
Glass pearl；Heating reflux reaction naturally cools to room temperature after 2 hours at ambient pressure, adds ultra-pure water 80ml, shakes up, stands, treats
Survey；Add 3 to drip after ferroin indicator, titrated with iron ammonium sulfate, the stereometer then consumed according to iron ammonium sulfate
Calculate the COD value of each water sample.
2. the method for COD contents in a kind of detection High Cl- water sample according to claims 1, it is characterised in that：Described
Potassium Hydrogen Phthalate is to need before top pure grade, use to dry 2 ~ 2.5 hours at 100 ~ 105 DEG C.
3. the method for COD contents in a kind of detection High Cl- water sample according to claims 1, it is characterised in that：Mercuric sulfate
Addition is 1.2g；Potassium bichromate concentration is 0.272mol/L, and volume is 10ml；Silver sulfate-sulfuric acid concentration is 6.7g/L, volume
For 30ml；Ferrous ammonium sulfate concentration is 0.1mol/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| US11610467B2 (en) | 2020-10-08 | 2023-03-21 | Ecolab Usa Inc. | System and technique for detecting cleaning chemical usage to control cleaning efficacy |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104280384A (en) * | 2014-06-24 | 2015-01-14 | 浙江富春环保新材料有限公司 | Method for accurately measuring COD value of wastewater generated through strip steel hydrochloric acid pickling process |
| CN104515769A (en) * | 2014-11-27 | 2015-04-15 | 宁波大地化工环保有限公司 | High chloride wastewater COD (chemical oxygen demand) rapid determination method |
-
2017
- 2017-07-05 CN CN201710540374.6A patent/CN107202861A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104280384A (en) * | 2014-06-24 | 2015-01-14 | 浙江富春环保新材料有限公司 | Method for accurately measuring COD value of wastewater generated through strip steel hydrochloric acid pickling process |
| CN104515769A (en) * | 2014-11-27 | 2015-04-15 | 宁波大地化工环保有限公司 | High chloride wastewater COD (chemical oxygen demand) rapid determination method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| US11610467B2 (en) | 2020-10-08 | 2023-03-21 | Ecolab Usa Inc. | System and technique for detecting cleaning chemical usage to control cleaning efficacy |
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