CN103257107A - Preparation and application method of detection sheet for measuring phosphate content of water quality - Google Patents
Preparation and application method of detection sheet for measuring phosphate content of water quality Download PDFInfo
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- CN103257107A CN103257107A CN2013101659308A CN201310165930A CN103257107A CN 103257107 A CN103257107 A CN 103257107A CN 2013101659308 A CN2013101659308 A CN 2013101659308A CN 201310165930 A CN201310165930 A CN 201310165930A CN 103257107 A CN103257107 A CN 103257107A
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Abstract
The invention relates to a preparation and application method of a detection sheet for measuring the phosphate content of water quality. The method comprises the following steps of: firstly mixing concentrated sulfuric acid, sodium sulfate and sulfamic acid to obtain mixed powder I; uniformly mixing sodium ascorbate, polyethylene glycol 6000 and polyvinylpyrrolidone K-30 to obtain mixed powder II; uniformly mixing ammonium molybdate, polyethylene glycol 6000 and polyvinylpyrrolidone K-30 to obtain mixed powder III; and pressing the mixed powder I, the mixed powder II and the mixed powder III into a three-layer tablet to form a detection sheet for measuring the phosphate content of water quality. When in use, the detection sheet is directly immersed in 10ml of water sample which is then slightly shaken for 5-10 minutes until the detection sheet is dissolved; and then reaction lasts for 5-20 minutes, and a portable spectrophotometer is adopted for measurement. The detection sheet prepared by the method provided by the invention is convenient to carry and easy to store; when in use, any reagent is not required, and the result is accurate and reliable; and the detection sheet is suitable for the field detection of phosphate of water bodies such as surface water, domestic sewage, industrial wastewater and the like.
Description
Technical field
The present invention relates to a kind of preparation and using method of measuring the detection lug of water quality phosphate content, belong to the environmental monitoring technology field.
Background technology
In natural water and waste water, phosphorus nearly all exists with various phosphatic forms, and they are divided into orthophosphate, condensed phosphate (pyrophosphate, metaphosphate and polyphosphate) and the phosphorus that organically combines.Do not having under anthropogenic influence's the natural conditions, the compound concentrations of the phosphorus that calculates with hydrogen phosphate is generally less than 0.1mg/L.Because the result of mankind's activity, phosphorus concentration often is higher than this value in underground water and the superficial water (river and lake), plays an important role in the eutrophication of stagnant water.Often contain a large amount of phosphorus in the industrial waste water of industries such as chemical fertilizer, smelting, synthetic detergent and the sanitary sewage.Though one of phosphorus element that to be biological growth essential, phosphorus content is too high in the water body, can cause the excessive multiplication of algae, reaches harmful degree until quantitatively, is called eutrophication, and water quality is degenerated.In recent years, China's water pollution is the trend that increases the weight of, and its main cause is because a large amount of phosphorus-containing wastewaters enters water body, causes a large amount of breedings of algae, water environment degradation.Phosphate radical is as an important parameter of water quality supervision, and measuring its content fast, accurately and timely has very important meaning.
Phosphatic detection method mainly contains the chromatography of ions, the anti-photometry of molybdenum antimony, stannous chloride reduction molybdenum blue method, peacock green-phosphato-molybdic heteropolyacid method etc. in the water body.Have great importance for realizing that phosphatic scene is detected in real time in the Environmental Water and develop detection technique highly sensitive, high selectivity.Wang Qingxia etc. utilize flowing injecting analysis technology and improve the compound method of ascorbic acid reagent, have set up the rapid analysis of measuring orthophosphate in the water.By to optimization of experimental conditions, analyze speed and reach 72 samples/h, detect and be limited to 0.01mg/L, the relative standard deviation of 0.5mg/L phosphorus standard solution being measured 11 times is 0.9%.Be applied to the mensuration of industrial waste water sample, the result satisfactory (Wang Qingxia, Su Ling, Haitao Zhang. orthophosphate [J] in the flow injection spectrophotometry industrial waste water. Chemical Engineer, 2006, (11): 31-36).Wang Ping etc. have set up Flow Injection Chemiluminescence Method and have injected phosphatic method in a crystal violet one phosphato-molybdic heteropolyacid ionic association system mensuration seawater, have established optimum test condition, efficiently solve the salinity interference problem of seawater.This method linear relationship is good, and detection limit is low, and precision and accuracy meet the requirements, and stream is simple, and is easy to operate, can be used for the on-the-spot (Wang Ping that analyzes automatically, Zhang Xinshen. the Flow Injection Chemiluminescence Method injection is measured phosphate [J] in the seawater. environmental monitoring management and technology, 2006,18 (2): 26-30).
It is relatively stable that Zhao builds the equal utilization vanadium phosphate, and the characteristics that measurement range is big are listed as the purpose that reaches reactive phosphate in the quick mensuration water by the production standard look.The standard colors row are chosen to be 5d stabilization time, and measurement range is 0.5～5.0mg/L.It is simple for production that this method has standard, measures characteristics fast, be particularly suitable for the engineering debug field monitoring (Zhao Jianping, Feng Huanyin, Weng Yanbo. reactive phosphate is measured [J] fast with standard colors row. Chinese environmental monitoring, 2004,20 (6): 28-29).Qu's oats roses etc. are selected the yellow colorimetric method for determining phosphate of phosphorus vanadium molybdenum color condition, find out best color condition and improve.The measurement range of the back method of improvement is at 0～0.014mg/mL, and related coefficient is 1.000, and phosphate in the recirculated cooling water is measured, and the recovery is 90%～100%.Do the contrast experiment with former molybdenum blue method, illustrate that phosphatic mensuration selects the yellow colourimetry of phosphorus vanadium molybdenum more satisfactory in the recirculated cooling water, have good selectivity and reappearance (Qu Youqiang, Tang Guoping. phosphatic discussion [J] in the yellow colorimetric method for determining recirculated water of phosphorus vanadium molybdenum. big nitrogenous fertilizer, 2001.24 (5): 351-352).Wu's generation is medium to be matrix with the metallic cobalt, forms the cobalt oxide sensitive membrane that dihydric phosphate is had good electrochemical response on its surface, successful preparation the phosphate ion electrodes selective.Different soak times and the linear response range of different activated solutions to the phosphate detection, the influence of response slope and detectability have been discussed in detail.Experimental result shows: should be based on the phosphate ion electrodes selective of cobalt in the end of 0.025mol/L Potassium Hydrogen Phthalate liquid, to dihydric phosphate 10
-4～10
-1Be linear response in the mol/L concentration range, its response slope is-48.27mV/dec to detect and be limited to 2.27 * 10
-5Mol/L, coefficient R
2Be 0.99.This electrode has good stable and reappearance, successfully be used for the reality detection of water sample dihydric phosphate from the beginning, satisfied (the Wu Shijie of result, Zhang Haiyun, the Lu literary composition is brilliant, Yan Lixia, Kang Qi, Pan Dawei etc. based on the phosphate ion electrodes selective research of cobalt. environmental science and technology, 2012,35 (6I): 234-238).But still find no the report that closes the development of phosphate detection lug.
Summary of the invention
The objective of the invention is to disclose a kind of preparation method who is suitable for water systems'phosphorus phosphate content detection lugs such as surface water, sanitary sewage, industrial waste water, another object of the present invention provides a kind of using method of this tablet.
In order to achieve the above object, the present invention uses the phosphorus molybdenum blue spectrophotometric method to prepare the phosphate detection lug, the main pH regulating course that is mixed by the concentrated sulphuric acid, sulfaminic acid and anhydrous sodium sulfate, individual layer quality 0.5～2g, by sodium ascorbate reducing zone and the ammonium molybdate color layer through the Macrogol 6000 parcel, individual layer quality 0.05～0.5g successively adds sheeter with three layers of powder, and compacting forms.Concrete preparation method is as follows:
The first step, measure the concentrated sulphuric acid by mass fraction: anhydrous sodium sulfate: sulfaminic acid=0.7:26:8.01, earlier the concentrated sulphuric acid and anhydrous sodium sulfate are mixed then, place 110 ℃ of baking 1～2h down again, at last they are mixed with sulfaminic acid, obtain the mixed-powder I;
Second step, measure sodium ascorbate by mass fraction: Macrogol 6000: polyvinylpyrrolidone K-30=1:4:1.7, earlier sodium ascorbate and Macrogol 6000 are mixed then, place again under 60 ℃ of water-baths and heat, grind after the cooling, at last they and polyvinylpyrrolidone K-30 are mixed, obtain the mixed-powder II;
The 3rd step, measure ammonium molybdate by mass fraction: Macrogol 6000: polyvinylpyrrolidone K-30=1:6:7, earlier ammonium molybdate and Macrogol 6000 are mixed then, place again under 60 ℃ of water-baths and heat, grind after the cooling, again they and polyvinylpyrrolidone K-30 are mixed, obtain the mixed-powder III;
The 4th step, get 0.4～1.0g mixed-powder I, 0.05～0.12g mixed-powder II and 0.05～0.14g mixed-powder III are put into the sheeter mould of diameter 8～20mm successively, 4～20MPa depresses to tri-layer tablets at pressure, is the detection lug of measuring water quality phosphate content;
The above-mentioned concentrated sulphuric acid, anhydrous sodium sulfate, sulfaminic acid, ammonium molybdate, sodium ascorbate, Macrogol 6000, polyvinylpyrrolidone K-30 are commercially available analysis pure chemistry product.
A kind of using method of measuring the detection lug of water quality phosphate content, get 10ml water sample to be measured in the 10ml color comparison tube, detection lug is directly immersed, shake and reacted again 5～20 minutes after making tablet dissolved in 5～10 minutes, utilize portable spectrophotometer to measure at last, namely get phosphate concn in the water;
Above-mentioned water sample to be measured is surface water, sanitary sewage, industrial waste water.
Advantage of the present invention is:
1, because the detection lug quality of mensuration water quality phosphate content of the present invention 0.5～2g only need not add other any reagent during use, have characteristics such as cheap, easy to carry, the layman can operate.
2, this detection lug detects phosphatic scope: 0～1.0mg/L in the water, is suitable for the fast detecting of water systems'phosphorus phosphate contents such as surface water, sanitary sewage, industrial waste water.
Embodiment
Embodiment 1, measures the preparation of water quality phosphate content detection sheet
The first step, measure the concentrated sulphuric acid by mass fraction: anhydrous sodium sulfate: sulfaminic acid=0.7:26:8.01, earlier the concentrated sulphuric acid and anhydrous sodium sulfate are mixed then, place 110 ℃ of baking 1～2h down again, at last they are mixed with sulfaminic acid, obtain the mixed-powder I;
Second step, get the 12g Macrogol 6000 and place heat fused under 60 ℃ of water-baths, again the 3g sodium ascorbate is added in the Macrogol 6000 of fusing, mix, grind after the cooling again, mix with 5g polyvinylpyrrolidone K-30 again, obtain the mixed-powder II;
The 3rd step, get the 6g Macrogol 6000 and place heat fused under 60 ℃ of water-baths, again the Macrogol 6000 after 1g ammonium molybdate and the fusing is mixed, after cooling grinds, mix obtaining the mixed-powder III again with 7g polyvinylpyrrolidone K-30;
The 4th step, get 0.65g mixed-powder I, 0.1g mixed-powder II, 0.1g mixed-powder III respectively, and successively put into diameter 12mm mould sheeter (model YP-15A) according to above-mentioned order, under 6MPa pressure, be pressed into tri-layer tablets, namely get the detection lug of water quality phosphate content.
The above-mentioned concentrated sulphuric acid, anhydrous sodium sulfate, sulfaminic acid, ammonium molybdate, sodium ascorbate, Macrogol 6000, polyvinylpyrrolidone K-30 are commercially available analysis pure chemistry product.
Embodiment 2, and phosphate concn is measured in certain sanitary sewage
Get the 10ml sanitary sewage in the 10ml color comparison tube, the detection lug of the mensuration water quality phosphate content that embodiment 1 is prepared immerses, shake color comparison tube 8min and make its dissolving, reaction 10min obtains blue solution, utilize portable spectrophotometer (the general company of analysing in the portable spectrometer of PORS-15V Beijing), be that the 710nm place measures solution absorbency at wavelength, phosphate concn is 0.26mg/L in the calculating sanitary sewage, with traditional molybdenum-antimony anti-spectrophotometric method as a result 0.23mg/L be more or less the same, show this detection lug accurately, reliable.
Claims (2)
1. preparation method who measures the detection lug of water quality phosphate content is characterized in that:
The first step, measure the concentrated sulphuric acid by mass fraction: anhydrous sodium sulfate: sulfaminic acid=0.7:26:8.01, earlier the concentrated sulphuric acid and anhydrous sodium sulfate are mixed then, place 110 ℃ of baking 1～2h down again, at last they are mixed with sulfaminic acid, obtain the mixed-powder I;
Second step, measure sodium ascorbate by mass fraction: Macrogol 6000: polyvinylpyrrolidone K-30=1:4:1.7, earlier sodium ascorbate and Macrogol 6000 are mixed then, place again under 60 ℃ of water-baths and heat, grind after the cooling, at last they and polyvinylpyrrolidone K-30 are mixed, obtain the mixed-powder II;
The 3rd step, measure ammonium molybdate by mass fraction: Macrogol 6000: polyvinylpyrrolidone K-30=1:6:7, earlier ammonium molybdate and Macrogol 6000 are mixed then, place again under 60 ℃ of water-baths and heat, grind after the cooling, again they and polyvinylpyrrolidone K-30 are mixed, obtain the mixed-powder III;
The 4th step, get 0.4～1.0g mixed-powder I, 0.05～0.12g mixed-powder II and 0.05～0.14g mixed-powder III are put into the sheeter mould of diameter 8～20mm successively, 4～20MPa depresses to tri-layer tablets at pressure, is the detection lug of measuring water quality phosphate content;
The above-mentioned concentrated sulphuric acid, anhydrous sodium sulfate, sulfaminic acid, ammonium molybdate, sodium ascorbate, Macrogol 6000, polyvinylpyrrolidone K-30 are commercially available analysis pure chemistry product.
2. the using method of the detection lug of a mensuration water quality phosphate content that obtains with the described method of claim 1, it is characterized in that: get 10ml water sample to be measured in the 10ml color comparison tube, detection lug is directly immersed, shake and made the detection lug dissolving in 5～10 minutes, and then reacted 5～20 minutes, utilize portable spectrophotometer to measure at last, namely get phosphate concn in the water;
Above-mentioned water sample to be measured is surface water, sanitary sewage or industrial waste water.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103712980A (en) * | 2013-12-05 | 2014-04-09 | 同济大学 | Preparation and application methods for detection agent for detecting zinc content in water |
| CN105987982A (en) * | 2015-02-16 | 2016-10-05 | 艺康美国股份有限公司 | Composition for measuring concentration of orthophosphoric radicals in water system, measuring method and application of composition |
| CN109142245A (en) * | 2018-06-25 | 2019-01-04 | 聊城煤泗新材料科技有限公司 | A kind of method of phosphate content in measurement hydrogen peroxide |
| CN109827915A (en) * | 2019-03-12 | 2019-05-31 | 闫宏涛 | A kind of bi-component detection agent measuring phosphorus content |
| CN110168377A (en) * | 2016-11-10 | 2019-08-23 | 英国研究与创新组织 | Molybdenum blue for measuring chemical species measures |
Citations (1)
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| CN102879241A (en) * | 2011-07-13 | 2013-01-16 | 上海绿帝环保科技有限公司 | Rapid phosphate detection tablet |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102879241A (en) * | 2011-07-13 | 2013-01-16 | 上海绿帝环保科技有限公司 | Rapid phosphate detection tablet |
Non-Patent Citations (2)
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| 王丽等: "《免试剂离子色谱法检测水产品及其制品中的多聚磷酸盐》", 《中国食品学报》, vol. 11, no. 4, 31 July 2011 (2011-07-31), pages 203 - 210 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103712980A (en) * | 2013-12-05 | 2014-04-09 | 同济大学 | Preparation and application methods for detection agent for detecting zinc content in water |
| CN105987982A (en) * | 2015-02-16 | 2016-10-05 | 艺康美国股份有限公司 | Composition for measuring concentration of orthophosphoric radicals in water system, measuring method and application of composition |
| CN110168377A (en) * | 2016-11-10 | 2019-08-23 | 英国研究与创新组织 | Molybdenum blue for measuring chemical species measures |
| CN109142245A (en) * | 2018-06-25 | 2019-01-04 | 聊城煤泗新材料科技有限公司 | A kind of method of phosphate content in measurement hydrogen peroxide |
| CN109827915A (en) * | 2019-03-12 | 2019-05-31 | 闫宏涛 | A kind of bi-component detection agent measuring phosphorus content |
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