CN102998266A - Method for analyzing total phosphorus in industrial sewage sample - Google Patents
Method for analyzing total phosphorus in industrial sewage sample Download PDFInfo
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- CN102998266A CN102998266A CN2012104769926A CN201210476992A CN102998266A CN 102998266 A CN102998266 A CN 102998266A CN 2012104769926 A CN2012104769926 A CN 2012104769926A CN 201210476992 A CN201210476992 A CN 201210476992A CN 102998266 A CN102998266 A CN 102998266A
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Abstract
The invention discloses a method for analyzing total phosphorus in an industrial sewage sample, which comprises the following steps of: diluting a sewage sample to a proper concentration; fetching 8ml of the diluted sample, adding 1ml of potassium persulfate solution, and shaking uniformly; covering with a cover under normal pressure at 120 DEG C and heating for 30 minutes; taking out the product and performing water cooling to room temperature; adding 0.3ml of 10% ascorbic acid solution, and adding 0.3ml of molybdate solution; shaking uniformly, and standing for 15 minutes; pouring the product into a cuvette; measuring the absorbance by taking water as a reference in a wavelength of 710nm; and inquiring the content of phosphorus on a working curve after deducting the absorbance of a blank test, wherein the content of phosphate is the phosphorus content inquired from the working curve divided by the volume of the water sample. The method disclosed by the invention overcomes the shortcomings of the prior art, and measures the content of total phosphorus through ultraviolet visible spectrophotometer equipment under normal pressure according to the principle of an ammonium molybdate spectrophotometric method for measuring total phosphorus; and moreover, the operation process of the method is simple, the inspection cost is lowered, the safety is improved, and the result is reliable.
Description
Technical field
The present invention relates to the analytic sample technical field, specifically belong to the method for total phosphorus in a kind of analytical industry sewage sample.
Background technology
The determination and analysis of total phosphorus acts on great in industry, such as the efficient that can rationally control industrial circulating water treatment effect, monitoring wastewater treatment by total phosphorus.In the commercial production, treated sewage needs high frequency time to detect its total phosphorus content, reaches emission standard to control it.Existing method or complicated operation, security has much room for improvement or it is simple and easy not to operate.All need to clear up under the high temperature and high pressure condition, and digestion condition, time and reagent all has a significant impact measurement result, operating process is more loaded down with trivial details, to measuring the industrial sewage sample brings very large inconvenience in batches.The consumptive material of special-purpose instrument and equipment is difficult for buying, testing cost is high.
Summary of the invention
The method that the purpose of this invention is to provide total phosphorus in a kind of analytical industry sewage sample, the deficiencies in the prior art have been overcome, utilize the ammonium molybdate spectrophotometric principles of total phosphorus determination, under normal pressure, by UV, visible light spectrophotometer measuring apparatus total phosphorus content, the operating process of this method is simple, reduce inspection cost and improve security, reliable results.
The technical solution used in the present invention is as follows:
The method of total phosphorus in a kind of analytical industry sewage sample, described the method,
The first step is diluted to suitable concn with sewage sample, pipettes dilute sample 8ml,
Second step adds the 1ml potassium persulfate solution, shakes up, and the cover lid heating is 30 minutes under 120 ℃ of lower normal pressures, takes out water-cooled to room temperature,
The 3rd step added 10% ascorbic acid solution of 0.3ml, added the 0.3ml molybdate solution again, after shaking up, leave standstill 15 minutes after, pour cuvette into, under the 710nm wavelength, do reference with water, measure absorbance;
After the absorbance of deduction blank test, check in the content of phosphorus from working curve, phosphorus amount/volume of water sample that phosphate content=working curve checks in, phosphorus amount and volume of water sample unit are respectively μ g/mL, mL.
The described potassium persulfate solution of second step with 5g potassium persulfate dissolving solid carbon dioxide, and is diluted to 100mL.
Described ascorbic acid of the 3rd step will dissolve the 10g ascorbic acid in water, and be diluted to 100mL.
Described molybdate solution of the 3rd step will dissolve the 13g ammonium molybdate in 100mL water; Dissolving 0.35g potassium antimony tartrate is being added to ammonium molybdate solution in the 300mL sulfuric acid under constantly stirring in 100mL water slowly, tartarize antimony potassium solution and mixing.
Compared with the prior art, beneficial effect of the present invention is as follows:
The present invention utilizes the ammonium molybdate spectrophotometric principles of total phosphorus determination, and under normal pressure, by UV, visible light spectrophotometer measuring apparatus total phosphorus content, the operating process of this method is simple, reduces inspection cost and improves security, reliable results.
Description of drawings
Fig. 1 is total phosphorus working curve diagram of the present invention.
Fig. 2 is that the present invention and National Standard Method are measured as a result comparison diagram of total phosphorus.
Embodiment:
The method of total phosphorus in a kind of analytical industry sewage sample, described the method,
The first step is diluted to suitable concn with sewage sample, pipettes dilute sample 8ml,
Second step adds the 1ml potassium persulfate solution, shakes up, and the cover lid heating is 30 minutes under 120 ℃ of lower normal pressures, takes out water-cooled to room temperature,
The 3rd step added 10% ascorbic acid solution of 0.3ml, added the 0.3ml molybdate solution again, after shaking up, leave standstill 15 minutes after, pour cuvette into, under the 710nm wavelength, do reference with water, measure absorbance;
After the absorbance of deduction blank test, check in the content of phosphorus from working curve, phosphorus amount/volume of water sample that phosphate content=working curve checks in, phosphorus amount and volume of water sample unit are respectively μ g/mL, mL.
The described potassium persulfate solution of second step with 5g potassium persulfate dissolving solid carbon dioxide, and is diluted to 100mL.
Described ascorbic acid of the 3rd step will dissolve the 10g ascorbic acid in water, and be diluted to 100mL.
Described molybdate solution of the 3rd step will dissolve the 13g ammonium molybdate in 100mL water; Dissolving 0.35g potassium antimony tartrate is being added to ammonium molybdate solution in the 300mL sulfuric acid under constantly stirring in 100mL water slowly, tartarize antimony potassium solution and mixing.
The phosphorus standard is used solution: the phosphorus standard solution of 10.0mL is transferred in the 250mL volumetric flask, is diluted with water to graticule and mixing.1.00mL this standard solution contains 2.0 μ g phosphorus;
The drafting of working curve: the test tube with cover of getting 10 heatable 15ml adds respectively 0.0,0.50,1.00,1.50,2.00,3.00,4.00,6.00,8.00mL phosphate standard solution, corresponding phosphorus content is 0,1,2,3,4,6,8,12,16mg/L adds water to 8ml.
Then the assay method that Clicking here provides is processed, and does reference with water, measures absorbance.After the absorbance of deduction blank test, and the content drawing curve of corresponding phosphorus.
A total phosphorus is surpassed 25 times of the dilutions of sewage of 100mg/L, pipette 8ml dilution water sample to the heatable glass test tube of 15ml, add the potassium persulfate solution of 1ml, cover lid shakes up.Then be placed in 120 ℃ the constent temperature heater heating 30 minutes, and heated complete taking-up water cooling.10% ascorbic acid solution that adds again 0.3ml in the glass test tube shakes up and placed 30 seconds; Add again the 0.3ml molybdate solution and fully shake up, left standstill 15 minutes.Do simultaneously blank assay, replace water sample with distilled water.Water sample after will processing is again poured into respectively in the cuvette of different 1mm with blank sample.Under the 710nm wavelength, do reference with water, measure absorbance.After the absorbance of deduction blank test, check in the content of phosphorus from working curve, the unit of end value be milligram every liter.
1, the result of mensuration different volumes standard phosphorus content
2, identical water sample uses GB11893-89 prescriptive procedure (National Standard Method) and uses result's contrast of new method
Claims (4)
1. the method for total phosphorus in the analytical industry sewage sample is characterized in that: described the method,
The first step is diluted to suitable concn with sewage sample, and about 0.1-0.6mg/L pipettes dilute sample 8ml,
Second step adds the 1ml potassium persulfate solution, shakes up, and the cover lid heating is 30 minutes under 120 ℃ of lower normal pressures, takes out water-cooled to room temperature,
The 3rd step added 10% ascorbic acid solution of 0.3ml, added the 0.3ml molybdate solution again, after shaking up, leave standstill 15 minutes after, pour cuvette into, under the 710nm wavelength, do reference with water, measure absorbance;
After the absorbance of deduction blank test, check in the content of phosphorus from working curve, phosphorus amount/volume of water sample that phosphate content=working curve checks in, phosphorus amount and volume of water sample unit are respectively μ g/mL, mL.
2. the method for total phosphorus in a kind of analytical industry sewage sample according to claim 1 is characterized in that: the described potassium persulfate solution of second step with 5g potassium persulfate dissolving solid carbon dioxide, and is diluted to 100mL.
3. the method for total phosphorus in a kind of analytical industry sewage sample according to claim 1 is characterized in that: described ascorbic acid of the 3rd step, will dissolve the 10g ascorbic acid in water, and be diluted to 100mL.
4. the method for total phosphorus in a kind of analytical industry sewage sample according to claim 1 is characterized in that: described molybdate solution of the 3rd step, will dissolve the 13g ammonium molybdate in 100mL water; Dissolving 0.35g potassium antimony tartrate is being added to ammonium molybdate solution in the 300mL sulfuric acid under constantly stirring in 100mL water slowly, tartarize antimony potassium solution and mixing.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103969204A (en) * | 2014-05-22 | 2014-08-06 | 江苏省农业科学院 | Method for rapidly detecting phosphorus in forage-grade calcium hydrogen phosphate |
| CN103994996A (en) * | 2014-06-11 | 2014-08-20 | 攀枝花学院 | Analysis method for phosphorus in ferrovanadium |
| CN104034722A (en) * | 2014-06-03 | 2014-09-10 | 江苏永钢集团有限公司 | Method for measuring substance content of composite silicon carbide |
| CN104048964A (en) * | 2014-03-11 | 2014-09-17 | 北京城市排水集团有限责任公司 | Making method and use method of kit for determination of total phosphorus and orthophosphate by all-automatic water quality analyzer |
| CN104502295A (en) * | 2015-01-09 | 2015-04-08 | 成都海兰天澄科技有限公司 | On-line monitoring method for total phosphorus in water |
| CN107367470A (en) * | 2017-05-22 | 2017-11-21 | 安徽宏远职业卫生技术服务有限公司 | A kind of method of Judgment of Determination of Total Phosphorus In Water With Ammonium Molybdate Spectrophotometry |
| CN109142621A (en) * | 2018-08-21 | 2019-01-04 | 深圳市长隆科技有限公司 | Fast check reagent box of phosphorus and preparation method thereof and phosphorus detection method |
| CN109883968A (en) * | 2019-03-07 | 2019-06-14 | 长江水利委员会水文局 | The method for quickly testing and analyzing phosphorus in water using microplate reader microcolorimetry high-volume |
| CN110455794A (en) * | 2019-08-29 | 2019-11-15 | 安徽理工大学 | A kind of Direct Determination of the particle cluster flow based on pollution of area source |
| CN111912797A (en) * | 2019-12-17 | 2020-11-10 | 南开大学 | Method for measuring total phosphorus content in water |
| CN112730288A (en) * | 2020-12-25 | 2021-04-30 | 海南逸盛石化有限公司 | Total phosphorus analysis method |
| CN113029981A (en) * | 2021-03-08 | 2021-06-25 | 长春工程学院 | Method for detecting sludge total phosphorus of urban sewage plant |
| CN113884485A (en) * | 2021-10-22 | 2022-01-04 | 海南大学 | Method for rapidly detecting form and concentration of inorganic arsenic in water |
| CN114295564A (en) * | 2021-12-27 | 2022-04-08 | 辽宁大学 | Method for determining total phosphorus content in sewage by utilizing microplate reader |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104048964A (en) * | 2014-03-11 | 2014-09-17 | 北京城市排水集团有限责任公司 | Making method and use method of kit for determination of total phosphorus and orthophosphate by all-automatic water quality analyzer |
| CN104048964B (en) * | 2014-03-11 | 2016-08-17 | 北京城市排水集团有限责任公司 | Full-automatic water quality analysis-e/or determining total phosphorus and orthophosphate test kit make and usage |
| CN103969204A (en) * | 2014-05-22 | 2014-08-06 | 江苏省农业科学院 | Method for rapidly detecting phosphorus in forage-grade calcium hydrogen phosphate |
| CN104034722A (en) * | 2014-06-03 | 2014-09-10 | 江苏永钢集团有限公司 | Method for measuring substance content of composite silicon carbide |
| CN103994996A (en) * | 2014-06-11 | 2014-08-20 | 攀枝花学院 | Analysis method for phosphorus in ferrovanadium |
| CN104502295A (en) * | 2015-01-09 | 2015-04-08 | 成都海兰天澄科技有限公司 | On-line monitoring method for total phosphorus in water |
| CN104502295B (en) * | 2015-01-09 | 2017-05-17 | 成都海兰天澄科技股份有限公司 | On-line monitoring method for total phosphorus in water |
| CN107367470A (en) * | 2017-05-22 | 2017-11-21 | 安徽宏远职业卫生技术服务有限公司 | A kind of method of Judgment of Determination of Total Phosphorus In Water With Ammonium Molybdate Spectrophotometry |
| CN109142621A (en) * | 2018-08-21 | 2019-01-04 | 深圳市长隆科技有限公司 | Fast check reagent box of phosphorus and preparation method thereof and phosphorus detection method |
| CN109883968A (en) * | 2019-03-07 | 2019-06-14 | 长江水利委员会水文局 | The method for quickly testing and analyzing phosphorus in water using microplate reader microcolorimetry high-volume |
| CN110455794A (en) * | 2019-08-29 | 2019-11-15 | 安徽理工大学 | A kind of Direct Determination of the particle cluster flow based on pollution of area source |
| CN111912797A (en) * | 2019-12-17 | 2020-11-10 | 南开大学 | Method for measuring total phosphorus content in water |
| CN111912797B (en) * | 2019-12-17 | 2022-11-01 | 南开大学 | Method for measuring total phosphorus content in water |
| CN112730288A (en) * | 2020-12-25 | 2021-04-30 | 海南逸盛石化有限公司 | Total phosphorus analysis method |
| CN113029981A (en) * | 2021-03-08 | 2021-06-25 | 长春工程学院 | Method for detecting sludge total phosphorus of urban sewage plant |
| CN113884485A (en) * | 2021-10-22 | 2022-01-04 | 海南大学 | Method for rapidly detecting form and concentration of inorganic arsenic in water |
| CN114295564A (en) * | 2021-12-27 | 2022-04-08 | 辽宁大学 | Method for determining total phosphorus content in sewage by utilizing microplate reader |
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Application publication date: 20130327 |