CN219935667U - Device for continuously testing COD (chemical oxygen demand) of chlorine-containing wastewater by mercury-free method - Google Patents
Device for continuously testing COD (chemical oxygen demand) of chlorine-containing wastewater by mercury-free method Download PDFInfo
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- CN219935667U CN219935667U CN202223278966.0U CN202223278966U CN219935667U CN 219935667 U CN219935667 U CN 219935667U CN 202223278966 U CN202223278966 U CN 202223278966U CN 219935667 U CN219935667 U CN 219935667U
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- 238000012360 testing method Methods 0.000 title claims abstract description 23
- 239000002351 wastewater Substances 0.000 title claims abstract description 14
- 239000000460 chlorine Substances 0.000 title abstract description 28
- 238000000034 method Methods 0.000 title abstract description 18
- 229910052801 chlorine Inorganic materials 0.000 title abstract description 13
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title description 4
- 239000001301 oxygen Substances 0.000 title description 4
- 229910052760 oxygen Inorganic materials 0.000 title description 4
- 239000000126 substance Substances 0.000 title description 4
- 238000000926 separation method Methods 0.000 claims abstract description 42
- 239000005416 organic matter Substances 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 230000029087 digestion Effects 0.000 claims abstract description 19
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 10
- 239000002699 waste material Substances 0.000 claims abstract description 9
- 238000012545 processing Methods 0.000 claims abstract description 7
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 11
- 238000001179 sorption measurement Methods 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- YUVLVONHNMXKBW-UHFFFAOYSA-L [Ag+2].OS(O)(=O)=O.[O-]S([O-])(=O)=O Chemical compound [Ag+2].OS(O)(=O)=O.[O-]S([O-])(=O)=O YUVLVONHNMXKBW-UHFFFAOYSA-L 0.000 claims description 3
- 238000004891 communication Methods 0.000 claims description 3
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims 1
- 239000007924 injection Substances 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 11
- 150000002894 organic compounds Chemical class 0.000 abstract description 5
- 239000011651 chromium Substances 0.000 description 13
- 238000002835 absorbance Methods 0.000 description 9
- 239000007789 gas Substances 0.000 description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 230000000873 masking effect Effects 0.000 description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 5
- 229910052804 chromium Inorganic materials 0.000 description 5
- IWZKICVEHNUQTL-UHFFFAOYSA-M potassium hydrogen phthalate Chemical compound [K+].OC(=O)C1=CC=CC=C1C([O-])=O IWZKICVEHNUQTL-UHFFFAOYSA-M 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- 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 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 2
- 238000012937 correction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 150000002730 mercury Chemical class 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- -1 silver ions Chemical class 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 238000011410 subtraction method Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- SPFMQWBKVUQXJV-BTVCFUMJSA-N (2r,3s,4r,5r)-2,3,4,5,6-pentahydroxyhexanal;hydrate Chemical compound O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O SPFMQWBKVUQXJV-BTVCFUMJSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The utility model discloses a device for continuously testing chlorine-containing wastewater COD by a mercury-free method, which comprises an automatic sampler, an organic matter separation column, an air pump, a reagent adding module, a high-temperature digestion module, a bubble removal device, a detector, a waste liquid collection module and a data processing module, wherein the device utilizes the organic matter separation column to carry out the reaction on organic compounds and Cl in a water sample – Selective separation; by testing the COD value of the water sample and the COD value of the water sample which does not contain organic matters after separation, the COD value is subtractedThe method calculates the COD value generated by the organic compound in the water sample, thereby fundamentally overcoming the influence of chloride ions on the COD detection result and ensuring the accuracy of the COD detection value.
Description
Technical Field
The utility model relates to a device for testing COD in wastewater, in particular to a device for continuously testing COD in chlorine-containing wastewater by a mercury-free method, and belongs to the technical field of detection and analysis.
Background
Chemical oxygen demand (Chemical Oxygen Demand, COD for short) is a core index of organic pollution in water environment monitoring and is also the most important execution index for industrial wastewater pollution control in China. The national standard test method of COD is potassium dichromate method, because of Cl in water sample – The method can be oxidized by potassium dichromate to generate a contribution value, and further the measurement result is larger, so that the influence of chloride ions on COD measurement is eliminated by adopting a mercury salt masking method and a chlorine correction method in the national standard method for solving the problem. The mercury salt masking method not only can generate mercury-containing waste liquid in the measuring process, but also has little significance on the detection result of high-chlorine low-COD waste water, and the chlorine correction method has complicated operation process and long time consumption.
In order to overcome the defects of the COD detection method of the high-chlorine wastewater, a great deal of researches are carried out by a plurality of students. One direction is the removal or masking of chloride ions before testing, and silver ions are used for replacing mercury ions for precipitation in the removal of the chloride ions, so that heavy metal silver can be consumed, meanwhile, part of organic matters can be flocculated to influence the detection value, and the applicability of the chloride ion masking to high-chlorine wastewater is not great. The second direction is the substitution or improvement of digestion mode, digestion agent and catalyst. On the other hand, the research on the COD related device is carried out, the research direction is to combine the assembly and improvement of the digestion function and the testing function, and the interference of chloride ions is not fundamentally solved.
Disclosure of Invention
Aiming at the defects of the existing detection method for COD in the high-chlorine wastewater, the utility model provides a device for continuously testing the COD in the chlorine-containing wastewater by a mercury-free method.
The technical scheme for solving the technical problems is as follows:
the device comprises an automatic sampler, an organic matter separation column, an air pump, a reagent feeding module, a high-temperature digestion module, an air bubble removing device, a detector, a waste liquid collecting module and a data processing module, wherein a sample outlet of the automatic sampler is communicated with a sample inlet of the organic matter separation column, the organic matter separation column extends along the flowing direction of waste water, an adsorption material is filled in the organic matter separation column, a water sample testing branch connected with the organic matter separation column in parallel is arranged above or below the organic matter separation column, the sample outlet of the organic matter separation column and the water sample testing branch are combined through a pipeline and then are communicated with the sample inlet of the high-temperature digestion module, the air pump and the reagent feeding module are sequentially arranged on the pipeline between the organic matter separation column and the water sample testing branch and the high-temperature digestion module, the high-temperature digestion module comprises a heatable cylinder aluminum block and a liquid pipeline wound on the outer side of the aluminum block, the liquid pipeline outlet of the high-temperature digestion module is communicated with the sample inlet of the air bubble removing device, the organic matter separation device is of a middle fine-head coarse structure, and the air bubble removing device is positioned at the upper middle part of the gas inlet of the high-temperature separation device, and the air bubble removing device is further arranged at the upper part of the gas inlet of the liquid separating device; the liquid sample outlet at the lower part of the bubble removal device is communicated with the sample inlet of the detector, the sample outlet of the detector is communicated with the waste liquid collection module, and the automatic sample injector and the detector are in communication connection with the data processing module.
Further, the reagent adding module comprises a dropping supply device of potassium dichromate solution and silver sulfate-sulfuric acid solution.
The device has the beneficial effects that:
(1) Organic compounds and Cl in water sample by utilizing organic matter separation column – Selective separation; the COD value of the water sample and the COD value of the water sample which does not contain the organic matters after adsorption separation are tested, and the COD value generated by the organic compounds in the water sample is calculated by a subtraction method, so that the influence of chloride ions on the COD detection result is fundamentally overcome, and the accuracy of the COD detection value is ensured;
(2) Air bubbles are introduced into the pipeline through the air pump, liquid to be tested is separated, detection is carried out in a mode of air bubble interval-continuous flow, interference among samples is reduced, and time is saved;
(3) The device can ensure that the detection of COD does not contain secondary pollution of mercury waste liquid, has simple and safe operation and saves time;
further, the organic matter separation column contains an amphiphilic adsorption material, and the surface of the amphiphilic adsorption material contains hydrophilic groups and hydrophobic groups.
The technical scheme has the beneficial effects that the amphiphilic adsorption material has broad spectrum and high efficiency on the adsorption of organic pollutants, ensures the separation of the organic pollutants and chloride ions, and can be recycled.
Further, the detector is an ultraviolet-visible spectrophotometer.
The principle of the device for detecting COD in the sample is as follows:
when the COD value in the sample is 100-1000mg/L, the trivalent chromium (Cr) generated by reducing the potassium dichromate is measured at the wavelength of 600+/-20 nm 3+ ) The COD value in the sample was equal to the absorbance of trivalent chromium (Cr 3+ ) Is in direct proportion to the absorbance increase value of (2) to thereby increase the absorbance of trivalent chromium (Cr 3+ ) Converted to the COD value of the sample. When the COD value in the sample is 15-250mg/L, the non-reduced hexavalent chromium (Cr 6+ ) And trivalent chromium (Cr) 3+ ) Total absorbance of two chromium ions; COD value and hexavalent chromium (Cr) 6+ ) Is proportional to the absorbance decrease value of trivalent chromium (Cr 3+ ) The absorbance increase value of (2) is proportional to the total absorbance decrease value, and the total absorbance value is converted into the COD value of the sample.
Drawings
FIG. 1 is a schematic view of the overall structure of the device of the present utility model;
1, an automatic sampler; 2. an organic matter separation column; 3. a water sample test branch; 4. an air pump; 5. a reagent adding module; 6. a high temperature digestion module; 7. a bubble removal device; 8. a detector; 9. a waste liquid collection module; 10. a data processing module; 11. and (3) an aluminum block.
Detailed Description
The present utility model is further described below with reference to specific examples, which are only for better illustrating the technical solution, but are not to be construed as limiting the scope of the present utility model.
Example 1:
as shown in figure 1, a device for continuously testing chlorine-containing wastewater COD by a mercury-free method comprises an automatic sampler 1, an organic matter separation column 2, a water sample testing branch 3, an air pump 4, a reagent feeding module 5, a high-temperature digestion module 6, a bubble removal device 7, a detector 8, a waste liquid collecting module 9 and a data processing module 10, wherein a sample outlet of the automatic sampler is communicated with a sample inlet of the organic matter separation column, the organic matter separation column extends along the flowing direction of wastewater, an amphiphilic adsorption material is filled in the organic matter separation column, a water sample testing branch connected with the organic matter separation column in parallel is arranged below the organic matter separation column, the sample outlet of the organic matter separation column and the water sample testing branch are communicated with the sample inlet of the high-temperature digestion module after being combined through pipelines, the air pump and the reagent feeding module are sequentially arranged on the pipeline between the organic matter separation column and the water sample testing branch and the high-temperature digestion module, the high-temperature digestion module comprises a heatable cylinder aluminum block 11 and a liquid pipeline wound on the outer side of the aluminum block, the liquid pipeline sample outlet of the high-temperature digestion module is communicated with the sample inlet of the bubble removal device, the removal device is provided with the middle part, the coarse gas inlet of the gas removal device is arranged at the middle part of the coarse gas inlet, and the coarse gas removal device is arranged at the upper part of the gas inlet of the gas removal device, and the coarse gas removal device is realized; the liquid sample outlet at the lower part of the bubble removal device is communicated with the sample inlet of the detector, the sample outlet of the detector is communicated with the waste liquid collection module, and the detector and the automatic sample injector are in communication connection with the data processing module.
The actual use process of the device is as follows:
the sample is injected by an automatic injector, then alternatively enters an organic matter separation column or a water sample testing branch below the organic matter separation column, the sample entering the organic matter separation column is subjected to adsorption removal of organic matters, and then air is regularly introduced into a pipeline by an air pumpThe bubble separates the sample by bubble, the reagent adding module adds potassium dichromate solution and silver sulfate-sulfuric acid solution into the sample, then the sample enters the high temperature digestion module, the aluminum block heats the sample in the pipeline to heat, the potassium dichromate solution oxidizes the organic matters in the sample, cr 6+ Is reduced to Cr 3+ And then removing bubbles by a bubble removing device, detecting absorbance by a detector, calculating the COD value of the water sample and the COD value of the water sample which does not contain organic matters after adsorption separation by a test, and calculating the COD value generated by the organic compounds in the water sample by a subtraction method.
Example 2:
in order to verify the separation effect of the device of the utility model on organic matters and chloride ions, the following simulation experiment is performed for verification.
First, linear verification of the contribution value of chloride ions to COD
Preparing the material into a material containing Cl by using ultrapure water and NaCl – The concentration of the use solution is 0, 500, 1000, 1500, 2000 mg/L. For the above different Cl – COD detection with the concentration use solution without masking agent HgSO 4 The other steps were carried out according to the method described in Standard HJ828-2017, and the results are shown in Table 1.
TABLE 1 different concentrations of Cl – COD contribution value of (2)
The linear fitting equation is COD Cl– ＝128.4×C Cl– +11，r 2 ＝0.9986。
Weighing a certain amount of glucose, dissolving in ultrapure water to prepare stock solution with the concentration of 1000mg/L, diluting the stock solution with ultrapure water to prepare a plurality of parts of use solution with the concentration of 50mg/L, and respectively adding Cl with different concentrations – Organic water samples with different chloride ion concentrations are prepared. Potassium hydrogen phthalate (KHP) and methanol were prepared in the same manner. The chlorine-containing organic water sample is used for carrying out organic matters and Cl by using the device – Separation without masking agent HgSO 4 Others of the othersThe procedure was followed as described in Standard HJ828-2017, and the results are shown in Table 2, table 3 and Table 4.
TABLE 2 different Cl – COD value of glucose water sample with concentration
By Cl – Concentration is on the abscissa, cl – Performing linear fitting with the total COD value of the organic matters as an ordinate, wherein the linear fitting equation is COD Cl- +glucose ＝143.29×C Cl– +48.5，r 2 ＝0.9995。
TABLE 3 different Cl – COD value of KHP water sample with concentration
The linear fitting equation is COD Cl–+KHP ＝135.29×C Cl– +65.5，r 2 ＝0.9994。
TABLE 4 different Cl – COD value of methanol water sample with concentration
The linear fitting equation is COD Cl- +methanol ＝133.57×C Cl– +72.5，r 2 ＝0.9999。
As shown by the experiment, the device can well mix organic matters and Cl – Separated and Cl – The contribution value to COD is in linear relation, cl – The contribution to COD remained unchanged in 3 different systems containing one organic matter, and thus it was found that the apparatus of the present utility model was not affected by the kind of organic matter in the system, not before separationThe COD value of the water sample only contains Cl after being subtracted and separated – The COD contribution value of the water sample can accurately obtain the COD value of the organic matters in the water sample.
The foregoing description of the preferred embodiments of the utility model is not intended to limit the utility model to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the utility model are intended to be included within the scope of the utility model.
Claims (3)
1. The device is characterized in that a sample outlet of the automatic sampler is communicated with a sample inlet of the organic matter separation column, the organic matter separation column extends along the flowing direction of wastewater, an adsorption material is filled in the organic matter separation column, a water sample test branch connected with the organic matter separation column in parallel is arranged above or below the organic matter separation column, the sample outlet of the organic matter separation column and the water sample test branch are communicated with the sample inlet of the high-temperature digestion module after being combined through a pipeline, the pipeline between the organic matter separation column and the water sample test branch and the high-temperature digestion module is sequentially provided with the air pump and the reagent injection module, the high-temperature module comprises a cylindrical aluminum block and a liquid pipeline wound on the outer side of the aluminum block, the liquid pipeline of the high-temperature digestion module is communicated with the sample inlet of the air bubble removal device, the air bubble removal device is of a middle fine-head coarse-removal structure, and the air bubble removal device is positioned at the upper part of the middle part of the gas and the lower part of the gas inlet of the gas separation device; the liquid sample outlet at the lower part of the bubble removal device is communicated with the sample inlet of the detector, the sample outlet of the detector is communicated with the waste liquid collection module, and the automatic sample injector and the detector are in communication connection with the data processing module.
2. The apparatus of claim 1, wherein the reagent dosing module comprises a drip supply of potassium dichromate solution and silver sulfate-sulfuric acid solution.
3. The apparatus of claim 1 or 2, wherein the detector is an ultraviolet-visible spectrophotometer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202223278966.0U CN219935667U (en) | 2022-12-08 | 2022-12-08 | Device for continuously testing COD (chemical oxygen demand) of chlorine-containing wastewater by mercury-free method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202223278966.0U CN219935667U (en) | 2022-12-08 | 2022-12-08 | Device for continuously testing COD (chemical oxygen demand) of chlorine-containing wastewater by mercury-free method |
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| Publication Number | Publication Date |
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| CN219935667U true CN219935667U (en) | 2023-10-31 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202223278966.0U Active CN219935667U (en) | 2022-12-08 | 2022-12-08 | Device for continuously testing COD (chemical oxygen demand) of chlorine-containing wastewater by mercury-free method |
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| Country | Link |
|---|---|
| CN (1) | CN219935667U (en) |
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2022
- 2022-12-08 CN CN202223278966.0U patent/CN219935667U/en active Active
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