CN108088977A - The detection method of organic cod in a kind of high concentration sodium sulfite water sample - Google Patents
The detection method of organic cod in a kind of high concentration sodium sulfite water sample Download PDFInfo
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- CN108088977A CN108088977A CN201810060398.6A CN201810060398A CN108088977A CN 108088977 A CN108088977 A CN 108088977A CN 201810060398 A CN201810060398 A CN 201810060398A CN 108088977 A CN108088977 A CN 108088977A
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- cod
- water sample
- sodium sulfite
- high concentration
- organic
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- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 title claims abstract description 138
- 235000010265 sodium sulphite Nutrition 0.000 title claims abstract description 82
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000001514 detection method Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 51
- 239000005416 organic matter Substances 0.000 claims abstract description 40
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000004364 calculation method Methods 0.000 claims abstract description 10
- 239000002351 wastewater Substances 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 10
- 238000006477 desulfuration reaction Methods 0.000 claims description 7
- 230000023556 desulfurization Effects 0.000 claims description 7
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 abstract description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 abstract description 2
- 235000011152 sodium sulphate Nutrition 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 23
- 241000196324 Embryophyta Species 0.000 description 13
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 9
- 235000019441 ethanol Nutrition 0.000 description 9
- 239000001632 sodium acetate Substances 0.000 description 9
- 235000017281 sodium acetate Nutrition 0.000 description 9
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 8
- 239000008103 glucose Substances 0.000 description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 238000004939 coking Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 2
- 241000276457 Gadidae Species 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
- G01N33/1806—Biological oxygen demand [BOD] or chemical oxygen demand [COD]
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Engineering & Computer Science (AREA)
- Pathology (AREA)
- Immunology (AREA)
- Molecular Biology (AREA)
- General Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biomedical Technology (AREA)
- Medicinal Chemistry (AREA)
- Food Science & Technology (AREA)
- Emergency Medicine (AREA)
- Biodiversity & Conservation Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a kind of detection method of organic cod in high concentration sodium sulfite water sample, this method is oxidized to sodium sulphate theoretical calculation COD COD according to sodium sulfite(Na2SO3), water sample by permanganimetric method or potassium dichromate method detection draw COD(Total), draw COD (organic matter)=COD(Total)‑COD(Na2SO3), the present invention provides one it is simple, accurately and rapidly detect COD in high concentration sodium sulfite water sample(organic matter)Method.
Description
Technical field
The present invention relates to organic cods in field of industrial waste water treatment more particularly to a kind of high concentration sodium sulfite water sample
Detection method.
Background technology
COD (COD) refers to the method for expressing of the oxygen equivalent for the organic matter that can be chemically aoxidized in water.Change
It learns oxygen demand (COD) to have reacted in water by the pollution level of reducing substances, reducing substances includes organic matter, sulfurous acid in water
Sodium, Fe2+、S2-, nitrite etc..Water is very universal by organic pollution, and COD is that current measure organic matter is opposite
One of important indicator of content.
In the prior art measure COD method can chemically (such as permanganimetric method, potassium dichromate method), but
Organic matter, sodium sulfite, Fe are included in desulfurization wastewater2+、S2-, in the water bodys such as nitrite, it is very big to measure content of organics presence
Error, therefore can not comprehensive and accurate reaction COD value by permanganimetric method, potassium dichromate method.And the numerical relation of this COD arrives
During its evaporative crystallization whether the shaping of crystal, joined when being desulfurization wastewater zero-emission using the important operation and control of evaporative crystallization
Number.
In addition, current chemical plant generates organic wastewater with high salt and high, for eliminating sulphite interference, COD inspections are improved
The accuracy of survey is made that substantial amounts of work, it is proposed that sulphite is such as converted by many methods by hydrogen peroxide oxidation
Sulfate, remaining hydrogen peroxide are removed by the method for heating, but the method there are it is certain the defects of, hydrogen peroxide removal is not thorough
Bottom introduces new interfering material instead, and there are apparent deviations for detection of the existing method to COD in water sample, it is therefore necessary to
Establish a kind of detection method for meeting COD in the high sodium sulfite discharge water in existing coke-oven plant and related chemical plant.
Therefore, those skilled in the art be directed to developing it is a kind of detect coke-oven plant and related factories discharge containing high sulfurous
Organic cod in hydrochlorate desulfurization wastewater.
The method of the present invention is to be oxidized to the corresponding COD of sodium sulphate according to sodium sulfite, and proposition one is simple, has
Effect detection high concentration sodium sulfite discharge Organic substance in water COD assay methods, detect water sample sulfite sodium content, pass through theory
The corresponding COD of sodium sulfite is calculated, water sample chemical oxygen demand is drawn by permanganimetric method or potassium dichromate method detection
Amount, the corresponding COD of organic matter subtract the corresponding COD of sodium sulfite for water sample COD, and the above method is for containing
High-salt wastewater coke-oven plant and related chemical plant detect the corresponding COD of organic matter, production run and week for enterprise
The protection for enclosing ecology has great importance.
The content of the invention
In view of the drawbacks described above of the prior art, the technical problems to be solved by the invention are how to detect containing concentration sulphuric acid
Organic cod in sodium water sample.
To achieve the above object, the present invention provides a kind of detection sides of organic cod in high concentration sodium sulfite water sample
Method, which is characterized in that comprise the following steps
The first step：The concentration of water sample sulfite sodium is detected, sodium sulfite correspondenceization is drawn by the method for theoretical calculation
Learn oxygen demand COD(Na2SO3)；
Second step：Measure total COD COD in water sample(Total)；
3rd step：Pass through formula COD(organic matter)=COD(Total)-COD(Na2SO3)Calculate the chemical oxygen demand of organic matter in water sample
Measure COD(organic matter)。
Further, the concentration of the high concentration sodium sulfite water sample sulfite sodium is more than 1000ppm.
Further, the high concentration sodium sulfite water sample is a kind of desulfurization wastewater in chemical plant.
Further, the high concentration sodium sulfite water sample is the high-salt wastewater of coke-oven plant's discharge.
Further, the high-salt wastewater of coke-oven plant's discharge can contain Fe2+、S2-And nitrite.
Further, the first step sulfite acid sodium corresponds to COD COD(Na2SO3)Theoretical calculation method
For：COD(Na2SO3)=32/252* ρ(Na2SO3), wherein ρ(Na2SO3)Represent the concentration of sodium sulfite.
Further, total COD COD in water sample in the second step(Total)It can be carried out by Strong oxdiative method
It measures.
Further, the Strong oxdiative method is permanganimetric method or potassium dichromate method.
Further, the water sample sulfite na concn can be measured by oxidimetry.
Further, the high concentration sodium sulfite water sample sulfite na concn and COD(organic matter)And COD(Total)Value is used
Mg/mL is represented.
In the preferred embodiment of the present invention, coke-oven plant's discharge is measured containing high-salt wastewater using TOC methods
The organic matter TOC that measures of numerical value and this method there is good correlation, COD(organic matter)With the R square value convergences of TOC Trendline
In 1, COD(organic matter)/ TOC ratios maintain 4 or so.
The technique effect is described further below with reference to specific embodiment, to be fully understood from the mesh of the present invention
, feature and effect.
Description of the drawings
Fig. 1 be a preferred embodiment of the invention desulfurization wastewater in COD detection method flow chart.
Specific embodiment
Multiple preferred embodiments of the present invention are introduced below with reference to Figure of description, make its technology contents more clear and just
In understanding.The present invention can be emerged from by many various forms of embodiments, and protection scope of the present invention not only limits
The embodiment that Yu Wenzhong is mentioned.
Embodiment 1：
The sodium acetate solution of 500mg/L is prepared, COD (sodium acetate) is measured by permanganimetric method or potassium dichromate method；
Successively prepare the sodium sulfite and sodium acetate solution of 500mg/L of 1000mg/L, the sodium sulfite of 3000mg/L and 500mg/L
Sodium acetate solution, the sodium acetate solution of the sodium sulfite of 6000mg/L and 500mg/L, 10000mg/L sodium sulfite and
The sodium acetate solution of 500mg/L, theoretical calculation draw COD(Na2SO3), COD(Total)Pass through permanganimetric method or potassium dichromate method
It measures, draws COD (organic matter)=COD(Total)-COD(Na2SO3), by comparing COD(sodium acetate)And COD(organic matter), organic matter correspondence
COD and COD(sodium acetate)Relative error is smaller.Concrete outcome see the table below：
| ρ(Na2SO3) | COD(Na2SO3) | COD(Total) | COD(organic matter) | COD(sodium acetate) | Relative error % |
| 1000 | 127 | 494 | 367 | 381 | 3.81 |
| 3000 | 381 | 758 | 377 | 381 | 1.1 |
| 6000 | 762 | 1141 | 379 | 381 | 0.5 |
| 10000 | 1270 | 1654 | 384 | 381 | 0.8 |
Embodiment 2：
Prepare the glucose solution of 500mg/L, COD(glucose)It is measured by permanganimetric method or potassium dichromate method；Successively
Prepare the sodium sulfite of 1000mg/L and the grape of the glucose solution of 500mg/L, the sodium sulfite of 3000mg/L and 500mg/L
Sugar juice, the glucose solution of the sodium sulfite of 6000mg/L and 500mg/L, the sodium sulfite of 10000mg/L and 500mg/L
Glucose solution, theoretical calculation draw COD(Na2SO3), COD(Total)It is measured, drawn by permanganimetric method or potassium dichromate method
COD(organic matter)=COD(Total)-COD(Na2SO3), by comparing COD(glucose)And COD(organic matter), the corresponding COD of organic matter with
COD(glucose)Relative error is smaller.Concrete outcome see the table below：
| ρ(Na2SO3) | COD(Na2SO3) | COD(Total) | COD(organic matter) | COD(glucose) | Relative error % |
| 1000 | 127 | 634 | 507 | 526 | 3.8 |
| 3000 | 381 | 914 | 533 | 526 | 1.3 |
| 6000 | 762 | 1264 | 502 | 526 | 4.9 |
| 10000 | 1270 | 1787 | 517 | 526 | 1.7 |
Embodiment 3：
Prepare the ethanol solution of 500mg/L, COD(ethyl alcohol)It is measured by permanganimetric method or potassium dichromate method；It prepares successively
The sodium sulfite of 1000mg/L and the ethanol solution of 500mg/L, the sodium sulfite of 3000mg/L and 500mg/L ethanol solution,
The ethanol solution of the sodium sulfite of 6000mg/L and the ethanol solution of 500mg/L, the sodium sulfite of 10000mg/L and 500mg/L,
Theoretical calculation draws COD(Na2SO3), COD(Total)It is measured by permanganimetric method or potassium dichromate method, draws COD(organic matter)=
COD(Total)-COD(Na2SO3), by comparing COD(ethyl alcohol)And COD(organic matter), organic matter corresponds to COD and COD(ethyl alcohol)It is opposite to miss
Difference is smaller.Concrete outcome see the table below：
| ρ(Na2SO3) | COD(Na2SO3) | COD(Total) | COD(organic matter) | COD(ethyl alcohol) | Relative error % |
| 1000 | 127 | 1115 | 988 | 1022 | 3.4 |
| 3000 | 381 | 1388 | 1007 | 1022 | 1.5 |
| 6000 | 762 | 1767 | 1005 | 1022 | 1.7 |
| 10000 | 1270 | 2264 | 994 | 1022 | 2.8 |
Embodiment 4：
As shown in Figure 1, be the present invention a preferred embodiment desulfurization wastewater in COD detection method flow chart.
Shanxi coking plant vapo(u)rization system two is taken to imitate water sample, detection sodium sulfite content ρ(Na2SO3), drawn by theoretical calculation
COD(Na2SO3), COD(Total)It is measured by permanganimetric method or potassium dichromate method, draws COD(organic matter)=COD(Total)-
COD(Na2SO3), TOC pass through Sievers InnovOx (TOC analyzers) detection, COD(organic matter)/ TOC maintains 4 or so,
COD(organic matter)1, COD is leveled off to the R square values of TOC Trendline(organic matter)It is close with two relation of variables of TOC, by this
Theoretical calculation draws COD(Na2SO3), COD(Total)It is measured by permanganimetric method or potassium dichromate method, draws COD(organic matter)=
COD(Total)-COD(Na2SO3)With practical feasibility and representativeness.
Experimental data compares, this experimental selection is the sodium sulfite water sample of different gradients and Shanxi coking plant water
Sample, water sample COD are measured by permanganimetric method or potassium dichromate method, the sodium sulfite of experimental formula difference gradient
It show that organic matter corresponds to COD data and do not add in sodium sulfite solution detection with organic solution detection and draws COD numbers
According to be compared, Shanxi coking plant contains different gradient sodium sulfite water sample organic matters and corresponds to COD and TOC and carries out
Compare, data are as follows：
| ρ(Na2SO3) | COD(Na2SO3) | COD(Total) | COD(organic matter) | TOC | COD(organic matter)/TOC |
| 17330 | 2201 | 4800 | 2599 | 649 | 4.01 |
| 20500 | 2601 | 9000 | 6399 | 1640 | 3.9 |
| 140200 | 17800 | 26400 | 8600 | 2195 | 3.92 |
| 165100 | 20960 | 37600 | 16640 | 4220 | 3.94 |
| 119700 | 15200 | 40000 | 24800 | 6280 | 3.95 |
| 137000 | 17397 | 58000 | 40603 | 10200 | 3.98 |
The preferred embodiment of the present invention described in detail above.It should be appreciated that the ordinary skill of this field is without wound
The property made work, which according to the present invention can conceive, makes many modifications and variations.Therefore, all technician in the art
Pass through the available technology of logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea
Scheme, all should be in the protection domain being defined in the patent claims.
Claims (10)
1. the detection method of organic cod in a kind of high concentration sodium sulfite water sample, which is characterized in that comprise the following steps
The first step：The concentration of water sample sulfite sodium is detected, show that sodium sulfite corresponds to chemistry and needs by the method for theoretical calculation
Oxygen amount COD(Na2SO3)；
Second step：Measure total COD COD in water sample(Total)；
3rd step：Pass through formula COD(organic matter)=COD(Total)-COD(Na2SO3)Calculate the COD of organic matter in water sample
COD(organic matter)。
2. the detection method of organic cod in high concentration sodium sulfite water sample as described in claim 1, which is characterized in that institute
The concentration for stating high concentration sodium sulfite water sample sulfite sodium is more than 1000ppm.
3. the detection method of organic cod in high concentration sodium sulfite water sample as described in claim 1, which is characterized in that institute
It is a kind of desulfurization wastewater in chemical plant to state high concentration sodium sulfite water sample.
4. the detection method of organic cod in high concentration sodium sulfite water sample as described in claim 1, which is characterized in that institute
State the high-salt wastewater that high concentration sodium sulfite water sample is coke-oven plant's discharge.
5. the detection method of organic cod in high concentration sodium sulfite water sample as claimed in claim 4, which is characterized in that institute
Fe can be contained by stating the high-salt wastewater of coke-oven plant's discharge2+、S2-And nitrite.
6. the detection method of organic cod in high concentration sodium sulfite water sample as described in claim 1, which is characterized in that institute
It states first step sulfite acid sodium and corresponds to COD COD(Na2SO3)Theoretical calculation method be：COD(Na2SO3)=32/252*
ρ(Na2SO3), wherein ρ(Na2SO3)Represent the concentration of sodium sulfite.
7. the detection method of organic cod in high concentration sodium sulfite water sample as described in claim 1, which is characterized in that institute
State in second step total COD COD in water sample(Total)It can be measured by Strong oxdiative method.
8. the detection method of organic cod in high concentration sodium sulfite water sample as claimed in claim 6, which is characterized in that institute
Strong oxdiative method is stated as permanganimetric method or potassium dichromate method.
9. the detection method of organic cod in high concentration sodium sulfite water sample as described in claim 1, which is characterized in that institute
Water sample sulfite na concn is stated to be measured by oxidimetry.
10. the detection method of organic cod in high concentration sodium sulfite water sample as claimed in claim 4, which is characterized in that institute
State the COD that detection method measures(organic matter)Ratio C OD between the numerical value measured with TOC methods(organic matter)/TOC≈4。
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| CN112255225A (en) * | 2020-09-25 | 2021-01-22 | 斯瑞尔环境科技股份有限公司 | Method for testing COD (chemical oxygen demand) of organic matters in iron-containing waste hydrochloric acid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111380862A (en) * | 2020-03-16 | 2020-07-07 | 佛山市顺德区药品检验所 | Method for detecting concentration of ethanol in alcohol disinfectant product |
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| CN112255225A (en) * | 2020-09-25 | 2021-01-22 | 斯瑞尔环境科技股份有限公司 | Method for testing COD (chemical oxygen demand) of organic matters in iron-containing waste hydrochloric acid |
| CN112255225B (en) * | 2020-09-25 | 2024-02-02 | 斯瑞尔环境科技股份有限公司 | Method for testing COD (chemical oxygen demand) of organic matters in waste hydrochloric acid containing iron |
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