CN112611725A - Method for detecting ammonia nitrogen content in printing and dyeing wastewater - Google Patents
Method for detecting ammonia nitrogen content in printing and dyeing wastewater Download PDFInfo
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- 239000002351 wastewater Substances 0.000 title claims abstract description 45
- 238000004043 dyeing Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 24
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 title claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 53
- 238000001179 sorption measurement Methods 0.000 claims abstract description 19
- 239000006228 supernatant Substances 0.000 claims abstract description 16
- 238000005189 flocculation Methods 0.000 claims abstract description 11
- 230000016615 flocculation Effects 0.000 claims abstract description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002835 absorbance Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 10
- -1 sodium nitroferricyanide Chemical compound 0.000 claims abstract description 10
- 239000005708 Sodium hypochlorite Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 9
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000011161 development Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000001556 precipitation Methods 0.000 claims abstract description 8
- 239000012528 membrane Substances 0.000 claims abstract description 5
- 230000010355 oscillation Effects 0.000 claims abstract description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 5
- 238000005119 centrifugation Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 6
- 239000011790 ferrous sulphate Substances 0.000 claims description 6
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 6
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 6
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 6
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 6
- 229910021536 Zeolite Inorganic materials 0.000 claims description 5
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 5
- 239000000835 fiber Substances 0.000 claims description 5
- 238000005342 ion exchange Methods 0.000 claims description 5
- 150000002500 ions Chemical class 0.000 claims description 5
- 239000002808 molecular sieve Substances 0.000 claims description 5
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 claims description 5
- 229940074439 potassium sodium tartrate Drugs 0.000 claims description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 5
- 235000011006 sodium potassium tartrate Nutrition 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 239000010457 zeolite Substances 0.000 claims description 5
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 5
- 229960001763 zinc sulfate Drugs 0.000 claims description 5
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 5
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical class O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 4
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 4
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 238000011088 calibration curve Methods 0.000 claims description 3
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 3
- 229960004889 salicylic acid Drugs 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000002834 transmittance Methods 0.000 claims description 3
- RGJFLQSCKQTTRF-UHFFFAOYSA-L C(=O)([O-])C(O)C(O)C(=O)[O-].[Na+].[K+].C(C=1C(O)=CC=CC1)(=O)O Chemical compound C(=O)([O-])C(O)C(O)C(=O)[O-].[Na+].[K+].C(C=1C(O)=CC=CC1)(=O)O RGJFLQSCKQTTRF-UHFFFAOYSA-L 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
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- Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
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Abstract
The invention discloses a method for detecting the content of ammonia nitrogen in printing and dyeing wastewater, which comprises the following steps: s1, taking a printing and dyeing wastewater sample, and adjusting the pH value of the water sample to be less than 2 by using sulfuric acid for later use; s2, carrying out flocculation precipitation pretreatment on the printing and dyeing wastewater sample, transferring the supernatant into a centrifuge tube, adding an adsorption decolorizing material, carrying out ultrasonic oscillation, putting the centrifuge tube into a high-speed centrifuge for centrifugation, taking the centrifuged supernatant, and passing the supernatant through a 0.22-micron PTFE filter membrane for later use; s3, putting the water sample treated in the step S2 into a colorimetric tube, adding 1mL of color development liquid and 0.1mL of sodium nitroferricyanide solution, and uniformly mixing; then 0.1mL of sodium hypochlorite solution is dripped to dilute the solution to the marked line and fully and uniformly mixed; after the mixture is placed for 1-2 hours, measuring the absorbance of a water sample at a wavelength of 697nm by using a spectrophotometer; and comparing with the standard curve to obtain the ammonia nitrogen content in the wastewater sample. The method for detecting the content of ammonia nitrogen in the printing and dyeing wastewater has high sensitivity and no secondary pollution, and can be applied to online monitoring of the printing and dyeing wastewater.
Description
Technical Field
The invention relates to the technical field of environmental detection, in particular to a method for detecting the content of ammonia nitrogen in printing and dyeing wastewater.
Background
China is the biggest textile garment production and export country in the world, so the printing and dyeing industry is closely related to the China, the waste water discharge of the printing and dyeing industry is one of the key industries causing water pollution in China, and compared with other industries, the printing and dyeing waste water has the characteristics of large waste water discharge amount, deep color, high content of organic matters difficult to degrade, unstable water quality and the like.
Aiming at the treatment problem of the printing and dyeing wastewater, the existing treatment technology mainly treats the printing and dyeing wastewater through physicochemical treatment and biochemical treatment in sequence, so that harmful substances are degraded and the emission standard is reached. Aiming at the physical and chemical treatment of the prior printing and dyeing wastewater, the prior physical and chemical treatment process is basically completed by manual operation of an operator. The printing and dyeing wastewater is firstly introduced into a pool, and because the pH value of the printing and dyeing wastewater is uncertain, the pH value is generally adjusted to be alkaline by lime, and then the wastewater is subjected to flocculation precipitation treatment by adding ferrous sulfate. At present, whether full flocculation occurs or not is judged according to naked eyes in the early treatment of the printing and dyeing wastewater, if the full flocculation does not occur, the problem of the addition amount of the traditional Chinese medicine in the treatment process is shown, and the adjustment is not in place. In general, the flocculation can be carried out sufficiently by adjusting the pH to 9 to 11, and the supernatant can be separated by passing through a sedimentation tank.
At present, the most common method for measuring ammonia nitrogen is a Nashin reagent colorimetric method, but the configuration of the Nashin reagent in the method is complex, the used reagent contains toxic compounds, secondary pollution is caused to the environment, meanwhile, printing and dyeing wastewater is generally dark, the color and the turbidity of the printing and dyeing wastewater interfere with measurement, and the accuracy of the measurement is influenced. Corresponding pretreatment is needed, and the operation is complicated. The printing and dyeing wastewater with higher chroma and turbidity is pretreated by a flocculation precipitation method and is still interfered by chroma when being measured by a Navier reagent method.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for detecting the content of ammonia nitrogen in printing and dyeing wastewater, which has high sensitivity and no secondary pollution and can be applied to the online monitoring of the printing and dyeing wastewater.
In order to solve the technical problem, the invention provides a method for detecting the content of ammonia nitrogen in printing and dyeing wastewater, which comprises the following steps:
s1, taking a printing and dyeing wastewater sample, and adjusting the pH value of the water sample to be less than 2 by using sulfuric acid for later use;
s2, carrying out flocculation precipitation pretreatment on the printing and dyeing wastewater sample, transferring the supernatant into a centrifuge tube, adding an adsorption decolorizing material, carrying out ultrasonic oscillation, putting the centrifuge tube into a high-speed centrifuge for centrifugation, taking the centrifuged supernatant, and passing the supernatant through a 0.22-micron PTFE filter membrane for later use;
s3, putting the water sample treated in the step S2 into a colorimetric tube, adding 1mL of color development liquid and 0.1mL of sodium nitroferricyanide solution, and uniformly mixing; then 0.1mL of sodium hypochlorite solution is dripped to dilute the solution to the marked line and fully and uniformly mixed; after the mixture is placed for 1-2 hours, measuring the absorbance of a water sample at a wavelength of 697nm by using a spectrophotometer; and comparing with the standard curve to obtain the ammonia nitrogen content in the wastewater sample.
Further, in step S2, the flocculation pretreatment specifically includes: and (4) respectively adding sodium hydroxide and at least one of magnesium sulfate, zinc sulfate and ferrous sulfate into the water sample obtained in the step S1 to enable the pH of the water sample to be more than 10.5, and generating hydroxide flocculent precipitate.
Further, in step S2, the adsorptive decoloring material is selected from one or more of graphitized carbon black, zeolite molecular sieve, ion exchange fiber, ion adsorption resin, and modified bentonite. The graphitized carbon black and the zeolite molecular sieve remove colored suspended matters in a water sample through physical adsorption, and the ion exchange fiber, the ion adsorption resin and the modified bentonite can remove the colored suspended matters in the water sample through double actions of physical adsorption and chemical action.
Furthermore, the addition amount of the adsorption decoloration material is 0.1-0.5 wt% of the mass of the water sample, and the granularity of the adsorption decoloration material is preferably 100-350 meshes.
Further, in step S3, the color developing solution is a salicylic acid-potassium sodium tartrate solution, and the preparation method thereof is: weighing 50g of salicylic acid, adding 100mL of water, then adding 160mL of 2mol/L sodium hydroxide solution, and stirring to completely dissolve; then 50g of potassium sodium tartrate is weighed, dissolved in water, combined with the solution and transferred into a 1000mL volumetric flask, and diluted to the marked line by adding water.
Further, the method also comprises the step of detecting the transmittance of the wastewater before detection, and specifically comprises the following steps: and (3) placing a water sample with a preset amount in a pore plate, testing the absorbance value at a specific wavelength by using an enzyme-labeling instrument, and if the absorbance is greater than a certain preset value, performing the step S2 on the water sample again.
Further, in step S3, the standard curve is drawn by:
taking 7 10mL colorimetric tubes, sucking 0, 1.00, 2.00, 3.00, 5.00, 6.00 and 8.00mL of ammonium standard use solution into the 10mL colorimetric tubes, wherein the concentration of the ammonium standard use solution is 1 mu g/mL; then adding 1.00mL of color development liquid and 0.1mL of sodium nitrosoferricyanide solution, and mixing uniformly; then 0.1mL of sodium hypochlorite solution is dripped, diluted to the marked line and uniformly mixed; and (3) after the mixture is placed for 1-2 hours, measuring the absorbance of the water sample at the wavelength of 697nm by using a spectrophotometer, and drawing a calibration curve.
The invention has the beneficial effects that:
1. according to the method for detecting the content of ammonia nitrogen in the printing and dyeing wastewater, the pH value of a water sample is more than 10.5 by adding sodium hydroxide before detection, so that impurity ions (such as Ca) in the water sample2+) Precipitating to reduce the turbidity of the water sample; in addition, at least one of magnesium sulfate, zinc sulfate and ferrous sulfate is added as a flocculating agent, and the colloid dye and the suspension dye in the water are subjected to adsorption precipitation treatment by utilizing the self electric neutralization, electric double layer compression, adsorption bridging and net catching functions of the compounds of magnesium sulfate, zinc sulfate and ferrous sulfate, so that the decolorizing effect of more than 90 percent is achieved, the color of the water sample is reduced,the detection accuracy is improved.
2. According to the method for detecting the content of ammonia nitrogen in the printing and dyeing wastewater, after the flocculation precipitation pretreatment, an adsorption decoloration material is added for further treatment. The adsorption decoloration material is graphitized carbon black, zeolite molecular sieve, ion exchange fiber, ion adsorption resin or modified bentonite, and the substances have high specific surface area and adsorption capacity, can remove colored suspended matters in a water sample through physical adsorption and chemical action, further improve the decoloration effect and are beneficial to reducing the influence of chromaticity on a detection result.
Detailed Description
The present invention is further described below in conjunction with specific examples to enable those skilled in the art to better understand the present invention and to practice it, but the examples are not intended to limit the present invention.
In the following examples, sodium hypochlorite solution was a commercial reagent, and the available chlorine content was 3.5g/L and the free chlorine content was 0.75 mol/L.
Example 1: preparing standard liquid and drawing standard curve
(1) Preparing a color developing solution: weighing 50g of salicylic acid, adding 100mL of water, then adding 160mL of 2mol/L sodium hydroxide solution, and stirring to completely dissolve; weighing 50g of potassium sodium tartrate, dissolving the potassium sodium tartrate in water, combining the potassium sodium tartrate with the solution, transferring the mixture into a 1000mL volumetric flask, and adding water to dilute the mixture until the mixture is marked;
(2) preparing a sodium nitrosoferricyanide solution: weighing 0.1g of sodium nitroferricyanide, dissolving in a 10mL colorimetric tube, and adding water until the mark line is marked;
(3) drawing a standard curve: taking 7 10mL colorimetric tubes, and respectively sucking 0mL, 1.00mL, 2.00 mL, 3.00 mL, 5.00 mL, 6.00 mL and 8.00mL of ammonium standard use solution into the 10mL colorimetric tubes, wherein the concentration of the ammonium standard use solution is 1 mu g/mL; then adding 1.00mL of color development liquid and 0.1mL of sodium nitrosoferricyanide solution, and mixing uniformly; then 0.1mL of sodium hypochlorite solution is dripped, diluted to the marked line and uniformly mixed; after standing for 1h, measuring the absorbance of the water sample at the wavelength of 697nm by using a spectrophotometer, and drawing a calibration curve.
Example 2
(1) A50 mL sample of the printing and dyeing wastewater was taken in a 100mL beaker and the pH of the water sample was adjusted to < 2 with sulfuric acid for use.
(2) Adding a proper amount of 1mol/L sodium hydroxide solution into a water sample to ensure that the pH value of the water sample is more than 10.5 and generate hydroxide flocculent precipitate; then adding 5mL of ferrous sulfate with the concentration of 1mol/L into the water sample, oscillating and standing for 30 min; and transferring the supernatant into a 15mL centrifuge tube, adding 50mg of zeolite molecular sieve with the particle size of 200 meshes, carrying out ultrasonic oscillation for 10min, putting the mixture into a high-speed centrifuge, centrifuging for 5min at the rotating speed of 10000rpm, taking the centrifuged supernatant, and filtering the supernatant through a 0.22-micron PTFE filter membrane for later use.
(3) Adding the water sample into a colorimetric tube, adding 1mL of color development liquid and 0.1mL of sodium nitrosoferricyanide solution, and uniformly mixing; then 0.1mL of sodium hypochlorite solution is dripped to dilute the solution to the marked line and fully and uniformly mixed; after standing for 1h, measuring the absorbance of the water sample at a wavelength of 697nm by using a spectrophotometer; and comparing with the standard curve to obtain the ammonia nitrogen content in the wastewater sample.
Example 3
(1) A50 mL sample of the printing and dyeing wastewater was taken in a 100mL beaker and the pH of the water sample was adjusted to < 2 with sulfuric acid for use.
(2) Adding a proper amount of 1mol/L sodium hydroxide solution into a water sample to ensure that the pH value of the water sample is more than 10.5 and generate hydroxide flocculent precipitate; then adding 5mL of zinc sulfate with the concentration of 1mol/L into the water sample, oscillating and standing for 30 min; and transferring the supernatant into a 15mL centrifuge tube, adding 80mg of ion exchange fiber with the particle size of 200 meshes, carrying out ultrasonic oscillation for 10min, putting the centrifuge into a high-speed centrifuge, centrifuging for 5min at the rotating speed of 10000rpm, taking the centrifuged supernatant, and filtering the supernatant through a 0.22-micron PTFE filter membrane for later use.
(3) Adding the water sample into a colorimetric tube, adding 1mL of color development liquid and 0.1mL of sodium nitrosoferricyanide solution, and uniformly mixing; then 0.1mL of sodium hypochlorite solution is dripped to dilute the solution to the marked line and fully and uniformly mixed; after standing for 1h, measuring the absorbance of the water sample at a wavelength of 697nm by using a spectrophotometer; and comparing with the standard curve to obtain the ammonia nitrogen content in the wastewater sample.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (7)
1. A method for detecting the content of ammonia nitrogen in printing and dyeing wastewater is characterized by comprising the following steps:
s1, taking a printing and dyeing wastewater sample, and adjusting the pH value of the water sample to be less than 2 by using sulfuric acid for later use;
s2, carrying out flocculation precipitation pretreatment on the printing and dyeing wastewater sample, transferring the supernatant into a centrifuge tube, adding an adsorption decolorizing material, carrying out ultrasonic oscillation, putting the centrifuge tube into a high-speed centrifuge for centrifugation, taking the centrifuged supernatant, and passing the supernatant through a 0.22-micron PTFE filter membrane for later use;
s3, putting the water sample treated in the step S2 into a colorimetric tube, adding 1mL of color development liquid and 0.1mL of sodium nitroferricyanide solution, and uniformly mixing; then 0.1mL of sodium hypochlorite solution is dripped to dilute the solution to the marked line and fully and uniformly mixed; after the mixture is placed for 1-2 hours, measuring the absorbance of a water sample at a wavelength of 697nm by using a spectrophotometer; and comparing with the standard curve to obtain the ammonia nitrogen content in the wastewater sample.
2. The method for detecting the content of ammonia nitrogen in printing and dyeing wastewater according to claim 1, wherein in step S2, the flocculation precipitation pretreatment specifically comprises: and (4) respectively adding sodium hydroxide and at least one of magnesium sulfate, zinc sulfate and ferrous sulfate into the water sample obtained in the step S1 to enable the pH of the water sample to be more than 10.5, and generating hydroxide flocculent precipitate.
3. The method for detecting the content of ammonia nitrogen in printing and dyeing wastewater according to claim 1, wherein in step S2, the adsorption decoloration material is one or more selected from graphitized carbon black, zeolite molecular sieves, ion exchange fibers, ion adsorption resins, and modified bentonite.
4. The method for detecting the content of ammonia nitrogen in printing and dyeing wastewater as claimed in claim 3, wherein the addition amount of the adsorption decoloration material is 0.1-0.5 wt% of the mass of a water sample.
5. The method for detecting the content of ammonia nitrogen in printing and dyeing wastewater according to claim 1, wherein in step S3, the color developing solution is a salicylic acid-potassium sodium tartrate solution, and the preparation method comprises: weighing 50g of salicylic acid, adding 100mL of water, then adding 160mL of 2mol/L sodium hydroxide solution, and stirring to completely dissolve; then 50g of potassium sodium tartrate is weighed, dissolved in water, combined with the solution and transferred into a 1000mL volumetric flask, and diluted to the marked line by adding water.
6. The method for detecting the content of ammonia nitrogen in printing and dyeing wastewater as claimed in claim 1, further comprising a step of detecting the transmittance of the water sample before detection, wherein if the transmittance of the water sample is less than a predetermined value, the step of S2 is performed again.
7. The method for detecting the content of ammonia nitrogen in printing and dyeing wastewater as claimed in claim 1, wherein in step S3, the standard curve is drawn by a method comprising the following steps:
taking 7 10mL colorimetric tubes, sucking 0, 1.00, 2.00, 3.00, 5.00, 6.00 and 8.00mL of ammonium standard use solution into the 10mL colorimetric tubes, wherein the concentration of the ammonium standard use solution is 1 mu g/mL; then adding 1.00mL of color development liquid and 0.1mL of sodium nitrosoferricyanide solution, and mixing uniformly; then 0.1mL of sodium hypochlorite solution is dripped, diluted to the marked line and uniformly mixed; and (3) after the mixture is placed for 1-2 hours, measuring the absorbance of the water sample at the wavelength of 697nm by using a spectrophotometer, and drawing a calibration curve.
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| CN114088694A (en) * | 2021-10-21 | 2022-02-25 | 包头钢铁（集团）有限责任公司 | Method for rapidly determining content of hydrogen sulfide in wastewater |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101204607B1 (en) * | 2011-07-14 | 2012-11-23 | 서울시립대학교 산학협력단 | Nitrogen ammonia concentration detecting method |
| CN103570110A (en) * | 2012-07-24 | 2014-02-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Efficient composite absorbing and flocculating agent used for printing and dyeing waste water treatment, preparation method thereof and applications thereof |
| CN104034681A (en) * | 2014-06-26 | 2014-09-10 | 南通永康检测技术有限公司 | Method for detecting content of ammonia nitrogen in sewage |
| CN106092939A (en) * | 2016-08-26 | 2016-11-09 | 淮安自来水有限公司 | Ammonia nitrogen salicylate spectrophotometric method for quick in water |
| CN109521007A (en) * | 2018-10-23 | 2019-03-26 | 九江德福科技股份有限公司 | A kind of Quantitative Monitoring method of ammonia nitrogen in waste water |
| CN110902789A (en) * | 2019-11-29 | 2020-03-24 | 安徽子延科技有限公司 | Textile printing and dyeing wastewater decoloration flocculant and preparation method thereof |
-
2020
- 2020-11-25 CN CN202011339261.8A patent/CN112611725A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101204607B1 (en) * | 2011-07-14 | 2012-11-23 | 서울시립대학교 산학협력단 | Nitrogen ammonia concentration detecting method |
| CN103570110A (en) * | 2012-07-24 | 2014-02-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Efficient composite absorbing and flocculating agent used for printing and dyeing waste water treatment, preparation method thereof and applications thereof |
| CN104034681A (en) * | 2014-06-26 | 2014-09-10 | 南通永康检测技术有限公司 | Method for detecting content of ammonia nitrogen in sewage |
| CN106092939A (en) * | 2016-08-26 | 2016-11-09 | 淮安自来水有限公司 | Ammonia nitrogen salicylate spectrophotometric method for quick in water |
| CN109521007A (en) * | 2018-10-23 | 2019-03-26 | 九江德福科技股份有限公司 | A kind of Quantitative Monitoring method of ammonia nitrogen in waste water |
| CN110902789A (en) * | 2019-11-29 | 2020-03-24 | 安徽子延科技有限公司 | Textile printing and dyeing wastewater decoloration flocculant and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 上海市印染工业公司编著, 中国纺织出版社 * |
| 马芮，刘嘉骥，刘永: "水杨酸法检测水质氨氮的改进方法", 《水杨酸法检测水质氨氮的改进方法》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114088694A (en) * | 2021-10-21 | 2022-02-25 | 包头钢铁（集团）有限责任公司 | Method for rapidly determining content of hydrogen sulfide in wastewater |
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