CN112595682A - Method for detecting polyphosphate in environment-friendly activated sludge based on hydrogen peroxide as strong oxidant - Google Patents
Method for detecting polyphosphate in environment-friendly activated sludge based on hydrogen peroxide as strong oxidant Download PDFInfo
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- CN112595682A CN112595682A CN202011418314.5A CN202011418314A CN112595682A CN 112595682 A CN112595682 A CN 112595682A CN 202011418314 A CN202011418314 A CN 202011418314A CN 112595682 A CN112595682 A CN 112595682A
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 239000010802 sludge Substances 0.000 title claims abstract description 41
- 229920000388 Polyphosphate Polymers 0.000 title claims abstract description 27
- 239000001205 polyphosphate Substances 0.000 title claims abstract description 27
- 235000011176 polyphosphates Nutrition 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000007800 oxidant agent Substances 0.000 title claims abstract description 9
- 230000001590 oxidative effect Effects 0.000 title claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000006228 supernatant Substances 0.000 claims abstract description 20
- 239000012153 distilled water Substances 0.000 claims abstract description 19
- 238000004140 cleaning Methods 0.000 claims abstract description 12
- 239000000047 product Substances 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000001514 detection method Methods 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 7
- WYWFMUBFNXLFJK-UHFFFAOYSA-N [Mo].[Sb] Chemical compound [Mo].[Sb] WYWFMUBFNXLFJK-UHFFFAOYSA-N 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000002798 spectrophotometry method Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000003556 assay Methods 0.000 claims 1
- 238000005259 measurement Methods 0.000 abstract description 7
- 238000003912 environmental pollution Methods 0.000 abstract 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 12
- 229910052698 phosphorus Inorganic materials 0.000 description 12
- 239000011574 phosphorus Substances 0.000 description 12
- 238000002386 leaching Methods 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 230000010355 oscillation Effects 0.000 description 4
- 241000282414 Homo sapiens Species 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000003321 amplification Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000012851 eutrophication Methods 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 229920000137 polyphosphoric acid Polymers 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- TVBSSDNEJWXWFP-UHFFFAOYSA-N nitric acid perchloric acid Chemical compound O[N+]([O-])=O.OCl(=O)(=O)=O TVBSSDNEJWXWFP-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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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
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- Spectroscopy & Molecular Physics (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for detecting polyphosphate in environment-friendly activated sludge based on hydrogen peroxide as a strong oxidant. The method comprises the following steps: adding hydrogen peroxide with the concentration of 30% into the dried activated sludge residues for pretreatment; cleaning the hydrogen peroxide pretreatment product by using 75% ethanol solution, 95% ethanol solution and absolute ethanol in sequence, adding 35% hydrogen peroxide, oscillating for 8-36h at 20-60 ℃, and centrifuging to obtain supernatant; adding 30% hydrogen peroxide into the residue, shaking and mixing at 90-100 deg.C, centrifuging, and collecting supernatant; and combining the supernatants, fixing the volume by using distilled water, accurately transferring 2ml of constant volume solution, adding concentrated sulfuric acid, heating, and cooling to determine the content of polyphosphate. The method improves the accuracy of measuring the content of the polyphosphate, reduces the environmental pollution and improves the measurement efficiency.
Description
Technical Field
The invention relates to the technical field of treatment of industrial wastewater and domestic sewage, in particular to a method for detecting polyphosphate in environment-friendly activated sludge based on hydrogen peroxide as a strong oxidant.
Background
Human activities cause a large amount of nitrogen, phosphorus and other substances to enter natural water bodies, so that plankton and algae are rapidly bred, water quality is deteriorated, normal photosynthesis of aquatic plants is influenced, and a large amount of fishes and other aquatic organisms die. In recent years, the problem of water eutrophication is receiving more and more attention. The deterioration of water quality seriously affects the normal life of human beings. The phosphorus contained in the sewage is mainly from industrial raw materials, detergents, pesticides, chemical fertilizers and human wastewater. The biological sewage dephosphorization method is an economic and effective technology for reducing the phosphorus content in the wastewater and preventing the eutrophication of water bodies. The process is widely researched at home and abroad, and different treatment processes are developed. The determination of the content of the polyphosphate in the phosphorus removing bacteria cells and the change rule thereof in the activated sludge has important significance for disclosing the biological phosphorus removal mechanism of the wastewater and improving the phosphorus removal efficiency by the prior art. At present, the common measurement methods at home and abroad are classified into chemical, biological, ion spectrum and the like. For the measurement of polyphosphate in activated sludge, potassium persulfate or nitric acid-perchloric acid is generally adopted in China as a strong oxidant, and the strong oxidant has strong corrosivity and can generate other additional products.
Disclosure of Invention
The invention aims to provide a method for detecting the content of polyphosphate in activated sludge, which can control the pollution and influence degree of the activated sludge on the environment. The method improves the accuracy, reduces the damage to the environment and basically does not produce harmful byproducts.
In order to realize the purpose of the invention, the technical scheme adopted by the invention is as follows: the method for detecting the polyphosphate in the environment-friendly activated sludge based on the hydrogen peroxide as the strong oxidant comprises the following steps:
1) washing the activated sludge mixed liquor with distilled water, and drying the obtained activated sludge residues;
2) weighing the dried activated sludge residue, adding 20-30% by mass of hydrogen peroxide for pretreatment, stirring and centrifuging to obtain a hydrogen peroxide pretreatment product;
3) cleaning the hydrogen peroxide pretreatment product obtained in the step 2) by using 75% ethanol solution, 95% ethanol solution and absolute ethanol in sequence, adding 35-45% hydrogen peroxide in mass percentage concentration, oscillating for 8-36h at 20-60 ℃, and centrifuging to obtain supernatant;
4) adding hydrogen peroxide with the mass percentage concentration of 20-30% into the residue obtained by centrifugation in the step 3), oscillating and mixing at 90-100 ℃, and centrifuging to obtain supernatant;
5) and (3) merging the supernatants obtained in the steps 3) and 4), fixing the volume by using distilled water, accurately transferring 2ml of fixed volume liquid, adding concentrated sulfuric acid, heating, and cooling to determine the content of polyphosphate.
Further, in the detection method, in the step 1), the activated sludge mixed solution is washed with distilled water for at least 4 times, and then the activated sludge residue is dried at 110 ℃.
Further, in the detection method, in the step 2), the mass percentage concentration of the hydrogen peroxide is 30%.
Further, in the detection method, in the step 2), the dried activated sludge residue is 20-25mg of hydrogen peroxide with a mass percentage concentration of 30% in 10ml according to the material-to-liquid ratio.
Further, in the detection method, in the step 3), the mass percentage concentration of the hydrogen peroxide is 35%.
Further, in the detection method, step 3), hydrogen peroxide with the mass percentage concentration of 35% is added and oscillated for 24 hours at the temperature of 20-30 ℃.
Further, in the detection method, in the step 4), the mass percentage concentration of the hydrogen peroxide is 30%.
Further, in the above detection method, step 4), shaking and mixing are carried out at 95 ℃ for 15 min.
Further, in the detection method, step 5), the supernatants obtained in the steps 3) and 4) are combined, distilled water is used for fixing the volume to 60ml, 2ml of fixed volume liquid is accurately transferred and added into concentrated sulfuric acid to be heated for 15min at 100 ℃, and the content of polyphosphate is determined after cooling.
Further, in the detection method, step 5), the polyphosphate content is determined by a molybdenum-antimony anti-spectrophotometry method.
The invention has the beneficial effects that: the method can effectively measure the content of the polyphosphate in the activated sludge mixed liquor, thereby mastering the pollution and the influence degree of the polyphosphate on the environment. The method provided by the invention has the advantages that the measurement accuracy is improved, the catalytic oxidation effect is excellent, the measurement time is saved, and the measurement efficiency is improved. Is beneficial to recycling waste experimental materials, basically has no pollution discharge and is environment-friendly.
Drawings
FIG. 1 is a graph showing the effect of reaction temperature on polyphosphate determination in activated sludge in the process of the present invention.
FIG. 2 is a graph showing the effect of shaking time on polyphosphate determination in activated sludge in the method of the present invention.
Detailed Description
The invention is further described below with reference to specific examples.
Example 1
The method for detecting the polyphosphate in the environment-friendly activated sludge based on the hydrogen peroxide as the strong oxidant comprises the following steps:
1) washing the activated sludge mixed liquor with distilled water for at least 4 times, preferably 4 times, centrifuging, and drying the obtained activated sludge residue at 110 ℃ for 12 h;
2) weighing dried activated sludge residues, adding hydrogen peroxide with the mass percentage concentration of 30%, uniformly stirring, centrifuging, taking solids, and repeatedly operating for 4 times; in each operation, according to the material-liquid ratio, 20-25mg:10ml, adding hydrogen peroxide with the mass percentage concentration of 30% into the dried activated sludge residue to obtain a hydrogen peroxide pretreatment product.
3) Cleaning the hydrogen peroxide pretreatment product obtained in the step 2) by using 75% ethanol solution, 95% ethanol solution and absolute ethanol in sequence, adding 35% hydrogen peroxide in mass percentage concentration, oscillating for 8-36h at 20-60 ℃, and centrifuging to obtain supernatant; preferably, shaking is carried out at 20-30 deg.C for 24 h.
4) Adding hydrogen peroxide with the mass percentage concentration of 30% into the residue obtained by centrifugation in the step 3), oscillating and mixing for 15min at 95 ℃, and centrifuging to obtain supernatant;
5) and (3) merging the supernatants obtained in the steps 3) and 4), fixing the volume to 60ml by using distilled water, accurately transferring 2ml of the fixed volume solution, adding concentrated sulfuric acid, heating at 100 ℃ for 15min, cooling, and measuring the content of polyphosphate by adopting a molybdenum-antimony anti-spectrophotometry method. Influence of reaction temperature on detection of polyphosphate in activated sludge
The method comprises the following steps:
1) taking an activated sludge mixed liquid sample of a certain water plant of Shenyang, adding distilled water into the sample by adopting a centrifugal cleaning method, stirring, centrifuging, adding distilled water into solid again, cleaning, centrifuging, repeating the steps, cleaning with distilled water for 4 times totally, and drying the obtained activated sludge residue for 12 hours at 110 ℃.
2) Respectively weighing four parts of 25mg of dried activated sludge residues, adding 10ml of hydrogen peroxide with the mass percentage concentration of 30% into each part for pretreatment, uniformly stirring and centrifuging, adding 10ml of hydrogen peroxide with the mass percentage concentration of 30% into the obtained solid again, and repeatedly carrying out the steps for 4 times to obtain a hydrogen peroxide pretreatment product.
3) Cleaning the hydrogen peroxide pretreatment product obtained in the step 2) by using 75% ethanol solution, 95% ethanol solution and absolute ethanol in sequence, adding 10ml of 35% hydrogen peroxide in mass percentage, oscillating at 0 ℃, 20 ℃, 40 ℃ and 60 ℃ for 24h, centrifuging for 15min, and keeping supernatant to obtain a residue for later use.
4) Adding 10ml of hydrogen peroxide with the mass percentage concentration of 30 percent into the residue obtained by the centrifugation in the step 3), shaking and mixing the mixture at the temperature of 95 ℃ for 15min respectively, and centrifuging the mixture to obtain supernatant.
5) Merging the supernatants obtained in the step 3) and the step 4), fixing the volume to 60ml by using distilled water, accurately transferring 2ml of the fixed volume solution, adding 0.1ml of concentrated sulfuric acid, heating at 100 ℃ for 15min, cooling, measuring the content of polyphosphoric acid in the activated sludge by using a molybdenum-antimony anti-spectrophotometry method, and calculating the leaching rate, wherein the result is shown in figure 1.
As can be seen from FIG. 1, the reaction temperature has a great influence on the leaching rate of polyphosphate. With the increase of the reaction temperature, the leaching speed of phosphorus is increased quickly, then the leaching speed of phosphorus is slowed down, and after the reaction temperature exceeds 30 ℃, even if the reaction temperature is continuously increased, the amplification rate of the leaching rate of phosphorus is reduced, so that the resource waste is caused, and the measurement efficiency is also influenced. Therefore, in the present invention, the reaction temperature is preferably 20 to 30 ℃ with shaking.
(II) influence of reaction time on detection of polyphosphate in activated sludge
The method comprises the following steps:
1) taking an activated sludge mixed liquid sample of a certain water plant of Shenyang, adding distilled water into the sample by adopting a centrifugal cleaning method, stirring, centrifuging, adding distilled water into solid again, cleaning, centrifuging, repeating the steps, cleaning with distilled water for 4 times totally, and drying the obtained activated sludge residue for 12 hours at 110 ℃.
2) Respectively weighing four parts of 25mg of dried activated sludge residues, adding 10ml of hydrogen peroxide with the mass percentage concentration of 30% into each part for pretreatment, uniformly stirring and centrifuging, adding 10ml of hydrogen peroxide with the mass percentage concentration of 30% into the obtained solid again, and repeatedly carrying out the steps for 4 times to obtain a hydrogen peroxide pretreatment product.
3) Cleaning the hydrogen peroxide pretreatment product obtained in the step 2) by using 75% ethanol solution, 95% ethanol solution and absolute ethanol in sequence, adding 10ml of 35% hydrogen peroxide, oscillating for 8 hours, 12 hours, 24 hours and 36 hours at the temperature of 30 ℃, centrifuging for 15min, and reserving supernatant to obtain residues for later use.
4) Adding 10ml of hydrogen peroxide with the mass percentage concentration of 30 percent into the residue obtained by the centrifugation in the step 3), shaking and mixing the mixture at the temperature of 95 ℃ for 15min respectively, and centrifuging the mixture to obtain supernatant.
5) Merging the supernatants obtained in the step 3) and the step 4), fixing the volume to 60ml by using distilled water, accurately transferring 2ml of the fixed volume solution, adding 0.1ml of concentrated sulfuric acid, heating at 100 ℃ for 15min, cooling, measuring the content of polyphosphoric acid in the activated sludge by using a molybdenum-antimony anti-spectrophotometry method, and calculating the leaching rate, wherein the result is shown in figure 2.
As can be seen from FIG. 2, the effect of the oscillation time on the leaching rate of polyphosphate was large. With the increase of the oscillation time, the phosphorus leaching speed is increased quickly, then the phosphorus leaching speed is reduced, and after the oscillation time exceeds 24 hours, even if the oscillation time is continuously prolonged, the amplification rate of the phosphorus leaching rate is reduced, resources are wasted, and the measurement efficiency is influenced. Therefore, the present invention preferably has a shaking time of 24 hours.
Claims (10)
1. The method for detecting the polyphosphate in the environment-friendly activated sludge based on hydrogen peroxide as a strong oxidant is characterized by comprising the following steps of:
1) washing the activated sludge mixed liquor with distilled water, and drying the obtained activated sludge residues;
2) weighing the dried activated sludge residue, adding 20-30% by mass of hydrogen peroxide for pretreatment, stirring and centrifuging to obtain a hydrogen peroxide pretreatment product;
3) cleaning the hydrogen peroxide pretreatment product obtained in the step 2) by using 75% ethanol solution, 95% ethanol solution and absolute ethanol in sequence, adding 35-45% hydrogen peroxide in mass percentage concentration, oscillating for 8-36h at 20-60 ℃, and centrifuging to obtain supernatant;
4) adding hydrogen peroxide with the mass percentage concentration of 20-30% into the residue obtained by centrifugation in the step 3), oscillating and mixing at 90-100 ℃, and centrifuging to obtain supernatant;
5) and (3) merging the supernatants obtained in the steps 3) and 4), fixing the volume by using distilled water, accurately transferring 2ml of fixed volume liquid, adding concentrated sulfuric acid, heating, and cooling to determine the content of polyphosphate.
2. The detection method according to claim 1, wherein in the step 1), the activated sludge mixed solution is washed with distilled water at least 4 times, and then the activated sludge residue is dried at 110 ℃.
3. The detection method according to claim 1, wherein in the step 2), the concentration of hydrogen peroxide is 30% by mass.
4. The detection method as claimed in claim 3, wherein in the step 2), the dried activated sludge residue is 20-25 mg/10 ml of hydrogen peroxide with a mass percentage concentration of 30% according to the material-liquid ratio.
5. The detection method according to claim 1, wherein in the step 3), the concentration of hydrogen peroxide is 35% by mass.
6. The detection method according to claim 5, wherein in the step 3), hydrogen peroxide with the mass percent concentration of 35% is added and the mixture is shaken for 24 hours at the temperature of 20-30 ℃.
7. The detection method according to claim 1, wherein in the step 4), the concentration of hydrogen peroxide is 30% by mass.
8. The assay of claim 1, wherein in step 4), the mixing is performed with shaking at 95 ℃ for 15 min.
9. The detection method according to claim 1, wherein in the step 5), the supernatants obtained in the step 3) and the step 4) are combined, distilled water is used for fixing the volume to 60ml, 2ml of fixed volume liquid is accurately transferred and added with concentrated sulfuric acid to be heated for 15min at 100 ℃, and the polyphosphate content is measured after cooling.
10. The detection method according to claim 1, wherein in step 5), the polyphosphate content is determined by molybdenum-antimony anti-spectrophotometry.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100243571A1 (en) * | 2007-11-12 | 2010-09-30 | Technion Research And Development Foundation Ltd. | Method for adsorption of phosphate contaminants from water solutions and its recovery |
| CN102841089A (en) * | 2011-06-24 | 2012-12-26 | 韩秀梅 | Determining method for total phosphorus in soil |
| CN106841062A (en) * | 2016-12-29 | 2017-06-13 | 贵港市芭田生态有限公司 | The detection method of total phosphorus content in water quality |
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- 2020-12-07 CN CN202011418314.5A patent/CN112595682A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100243571A1 (en) * | 2007-11-12 | 2010-09-30 | Technion Research And Development Foundation Ltd. | Method for adsorption of phosphate contaminants from water solutions and its recovery |
| CN102841089A (en) * | 2011-06-24 | 2012-12-26 | 韩秀梅 | Determining method for total phosphorus in soil |
| CN106841062A (en) * | 2016-12-29 | 2017-06-13 | 贵港市芭田生态有限公司 | The detection method of total phosphorus content in water quality |
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