CN102914539A - Method and kit for utilizing Mo-Sb antiluminosity method to detect content of orthophosphate in water - Google Patents
Method and kit for utilizing Mo-Sb antiluminosity method to detect content of orthophosphate in water Download PDFInfo
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- CN102914539A CN102914539A CN2012104591478A CN201210459147A CN102914539A CN 102914539 A CN102914539 A CN 102914539A CN 2012104591478 A CN2012104591478 A CN 2012104591478A CN 201210459147 A CN201210459147 A CN 201210459147A CN 102914539 A CN102914539 A CN 102914539A
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Abstract
The invention discloses a method and kit for utilizing a Mo-Sb antiluminosity method to detect a content of orthophosphate in water. The method comprises blending ammonium molybdate, antimony potassium tartrate and ascorbic acid to make a color developing agent, adding the color developing agent into a to-be-measured water sample to blend the color developing agent, then adding benzene sulfonic acid to enable the pH to be 0-1, fully blending and standing for over 3min, utilizing a spectrophotometer to measure the absorbance at the position of 880nm, and obtaining the content of orthophosphate in the to-be-measured water sample through an absorbance value according to a pre-measured standard curve. According to the method, by improving a strong acid medium, operation in measuring orthophosphate in the Mo-Sb antiluminosity method is simplified, danger is lowered, the detection speed is improved, and field operation is facilitated.
Description
Technical field
The present invention relates to the method for testing of orthophosphate in the water body, be specifically related to a kind of method of utilizing orthophosphate content in the molybdenum-antimony anti-spectrophotometric method test water body.
Background technology
Phosphorus is the important indicator of evaluating water quality, and the common method of measuring at present orthophosphate content in the water body has following several:
Bismuth phosphorus molybdenum orchid-sulfuric acid photometry: in sulfuric acid medium, orthophosphate and ammonium molybdate reaction, after in the presence of bismuth nitrate, generating phosphato-molybdic heteropolyacid, be reduced into complex compound by ascorbic acid, at the 750nm place with spectrophotometric method measure (Chu Zhishan etc. the method for bismuth phosphorus molybdenum orchid-sulfuric acid Photometric Determination of Phosphorus amount. China, CN201010107255.X[P] .2010-01-29).
Molybdenum-antimony anti-spectrophotometric method: be in sulfuric acid medium, orthophosphate and ammonium molybdate reaction behind the generation phosphato-molybdic heteropolyacid, are reduced by ascorbic acid in the presence of potassium antimony tartrate immediately, generate blue complex compound, measure by spectrophotometric method.The method is the method (GB11893-89 " the mensuration ammonium molybdate spectrophotometric method of water quality total phosphorus ") that national standard adopts.
The Reduction with Stannous Chloride photometry: be in sulfuric acid medium, orthophosphate and ammonium molybdate reaction are reduced into blue complex compound behind the adding stannous chloride, measure (" method for monitoring and analyzing of water and the waste water " third edition) by spectrophotometric method.Wherein, the preparation of Reduction with Stannous Chloride agent need to be used hydrochloric acid and metallic tin, and the dissolving of stannous chloride is slower, need to spend the night or heat
Above method can align exactly phosphatic content and measure, but carry out acidifying owing to all need prepare sulfuric acid solution, have following inconvenience in actual mechanical process: at first, sulfuric acid is the liquid acid with strong oxidizing property, is not suitable for long-distance transportation and carries; Secondly, the preparation of all solution all need to be finished in fuming cupboard in the above method, is not suitable for field work.So, for water body to be detected, need behind the field acquisition water sample sample to be delivered to the laboratory, just can finish the work that detects orthophosphate content.
Summary of the invention
The detection method that the purpose of this invention is to provide orthophosphate in a kind of quickly and easily water body makes things convenient for the on-the-spot mensuration of finishing orthophosphate content in the water sample behind the field acquisition water sample, and need not sample is delivered to the laboratory.
Technical scheme of the present invention is to improve on the basis of existing molybdenum-antimony anti-spectrophotometric method to obtain, at first according to a certain ratio ammonium molybdate, potassium antimony tartrate and ascorbic acid mixing are made developer, getting a certain amount of this developer mixes with water sample to be measured, then add a certain amount of benzene sulfonic acid, the system pH of making remains on 0-1, with the abundant mixing of reagent and leave standstill more than 3 minutes, use spectrophotometer to measure absorbance at 880nm, obtain the content of orthophosphate in the water sample to be measured according to the typical curve of measuring with same method in advance by absorbance.
Ammonium molybdate in the above-mentioned developer, potassium antimony tartrate and ascorbic acid powder can come proportioning to mix by the amount of using in the existing molybdenum-antimony anti-spectrophotometric method, preferred in the present invention, above-mentioned developer by the powder of ammonium molybdate, potassium antimony tartrate and ascorbic acid according to 35 ~ 40: 1: 65 ~ 75 mass ratio mixes; Preferred, the mass ratio of ammonium molybdate, potassium antimony tartrate and ascorbic acid powder is 35 ~ 38: 1: 70 ~ 72.
The blending ratio of described developer and water sample to be measured is: preferred 10 ~ 28mg developer that adds in every 10mL water sample to be measured more preferably adds 10 ~ 20mg developer.
The addition of benzene sulfonic acid is preferably every 10mL water sample and adds 0.32 ~ 0.64g benzene sulfonic acid, more preferably 0.45 ~ 0.50g.
After adding benzene sulfonic acid, fully the mixing reaction was finished the mensuration of absorbance more than 3 minutes usually in 24 hours, then can obtain the content of orthophosphate in the water sample according to the typical curve of measuring in advance.
The present invention also provides a kind of kit for fast detecting water body orthophosphate content, comprise two pack of separating of developer and benzene sulfonic acid, the mass ratio of two pack is developer: benzene sulfonic acid=10 ~ 28mg: 0.32 ~ 0.64g, be preferably 10 ~ 20mg: 0.45 ~ 0.50g, wherein developer is mixed by ammonium molybdate, potassium antimony tartrate and three kinds of powder of ascorbic acid, and the mass ratio of ammonium molybdate, potassium antimony tartrate and ascorbic acid is 35 ~ 40: 1: 65 ~ 75, be preferably 35 ~ 38: 1: 70 ~ 72.
Use for convenient, pack in the mentioned reagent box is packed according to disposable use amount, detect as example to get the 10mL water sample at every turn, the developer that has 10 ~ 20mg in each color-developer reagent bag, the benzene sulfonic acid that has 0.45 ~ 0.50g in each benzene sulfonic acid pack with after the 10mL water sample mixes, adds the benzene sulfonic acid in the benzene sulfonic acid pack with the developer in the color-developer reagent bag again, fully mixing leaves standstill after 3 minutes and can use spectrophotometer to measure under 880nm.
The present invention is by the improvement strong acid media, so that molybdenum-antimony anti-spectrophotometric method is measured the simplified control of orthophosphate, the use of solid acid has greatly reduced the danger of operation, reaction conditions requires lower, and the course of reaction heat release is few, and is comparatively gentle, reach stablize consuming time few, detection speed is fast, and reaction product is very stable, longer duration.The inventive method is stable, and is with low cost, not only can improve laboratory work efficient, also makes things convenient for field operation.
Description of drawings
Fig. 1 is the orthophosphate examination criteria curve under the different wave length measured of embodiment;
Fig. 2 is the orthophosphate examination criteria curve (880nm) under the different quality developer condition measured of embodiment;
Fig. 3 is the orthophosphate detection reaction kinetic curve (880nm) under the different acidity condition measured of embodiment.
Embodiment
Below in conjunction with instantiation the present invention is elaborated, but the scope that does not limit the present invention in any way.
1, key instrument and reagent
Instrument: DR2800 visible spectrophotometer, XS105DU 100,000/balance, one of percentage balance, bowl mill, oscillator, heat sealing machine;
Reagent: potassium dihydrogen phosphate, ammonium molybdate, potassium antimony tartrate, ascorbic acid, benzene sulfonic acid, the concentrated sulphuric acid, ultrapure water.Reagent all adopts analyzes pure or chromatographically pure reagent.
2, working curve with mix developer
1) working curve: experimental design water sample phosphorus concentration gradient is 0.00,0.06,0.30 and 0.60mg/L KH
2PO
4(in pure P).
2) mix developer: take by weighing 5.2g ammonium molybdate, 0.14g potassium antimony tartrate and 10g ascorbic acid, use bowl mill that it is ground to about 200 orders, use the oscillator mixing, it is for subsequent use to put into test tube.The ratio of ammonium molybdate, potassium antimony tartrate and ascorbic acid is with reference to national standard (GB11893-89) herein.
Determining of developer quality:
Take by weighing developer that a series of 28mg, 21mg, 14mg prepare in the 10ml color comparison tube, add respectively the phosphorus standard solution of 10ml variable concentrations, slight concussion makes the developer dissolving, and this moment, solution was little yellow.Take by weighing the 0.64g benzene sulfonic acid and join in the color comparison tube that has added developer and phosphorus standard solution, left standstill after the concussion 5 minutes, under 700nm and 880nm, measure respectively its absorbance (see figure 1), and the match typical curve, as shown in Figure 2.Because its absorption is stronger under 880nm, therefore in the test of back, all is chosen under the 880nm wavelength and tests.
Determining of acidity:
Because acidity all has the concentrated sulphuric acid to provide in the classic method, therefore the quality (0.64g) of benzene sulfonic acid is to obtain by the sulfuric acid mass conversion in the GB (GB11893-89) in preliminary test.For optimizing acidity condition, the inventor draws polymerization kinetics curves under 0.64g, 0.48g and 0.32g benzene sulfonic acid condition, and the kinetic curve in 15min under each acidity is seen Fig. 3.Simultaneously, at the typical curve of doing respectively under the condition of 0.48g and 0.32g benzene sulfonic acid under the different quality developer condition, finding has part solution deposited phenomenon to occur under 0.32g benzene sulfonic acid condition.
Above-mentioned experimental result is the mean value of 3 panel datas.
3. results and analysis
1) as seen from Figure 2, under the condition of 14mg developer linear best (R2=0.9996) of typical curve.And, in 24 hours of leaving standstill, under the 28mg developer condition variation of solution absorbance larger, absorbance is stablized constant under 21mg and the 14mg developer condition.
2) as can see from Figure 3, reaction reaches stable slower under the 0.64g benzene sulfonic acid condition, and phosphorus solution all can reach stable fast under 0.48g and 0.32g benzene sulfonic acid condition, and stable in 24 hours.
Because under 0.32g benzene sulfonic acid condition, precipitation appears in part solution, does not have versatility, determine that therefore optimum condition is: in 10ml water sample system, the quality of mixing developer is 14mg, and the quality of benzene sulfonic acid is 0.48g.
3) use national standard method the phosphorus standard solution to be measured the R of the typical curve of this method (getting above-mentioned optimum condition) and the match of national standard method institute
2Value is respectively 0.9996 and 0.9993, and the concentration value and the relative deviation that use two methods to record see the following form:
The concentration value and the actual concentrations value that calculate according to fitting formula compare, and obtain the relative deviation of method, and the relative deviation that uses this method to calculate is slightly less than national standard method, and the reliable accuracy of having of this method is described.
4. the making of kit
For making things convenient for the orthophosphate content in the fast detecting water sample after the field sampling, can in advance reagent be made into the kit that 14mg mixing color-developer reagent bag and 0.48g benzene sulfonic acid pack form, wherein 14mg mixing color-developer reagent bag is comprised of 4.75mg ammonium molybdate, 0.13mg potassium antimony tartrate and 9.13mg ascorbic acid.Only need weighing in the laboratory is poured into well in the Aluminium Foil Package and is got final product with the heat sealing machine sealing.When needs detect orthophosphate, open first the color-developer reagent bag, reagent is poured in the color comparison tube, add the 10ml water sample, open again the benzene sulfonic acid pack and pour color comparison tube into, shake and left standstill 3 minutes, can use portable spectrophotometer to detect.Pack is easy to make, can making in laboratory also can factory's mass production, convenient to use, not only be fit to the laboratory and use, also be applicable to field condition work.
Claims (10)
1. method that detects orthophosphate content in the water body with molybdenum-antimony anti-spectrophotometric method, at first ammonium molybdate, potassium antimony tartrate and ascorbic acid mixing are made developer, get this developer and add mixing in the water sample to be measured, and then adding benzene sulfonic acid, to make pH be 0-1, abundant mixing also leaves standstill more than 3 minutes, use spectrophotometer to measure absorbance at 880nm, obtain the content of orthophosphate in the water sample to be measured according to the typical curve of measuring with same method in advance by absorbance.
2. the method for claim 1 is characterized in that, described developer by the powder of ammonium molybdate, potassium antimony tartrate and ascorbic acid according to 35 ~ 40: 1: 65 ~ 75 mass ratio mixes.
3. method as claimed in claim 2 is characterized in that, the mass ratio of ammonium molybdate, potassium antimony tartrate and ascorbic acid powder is 35 ~ 38 in the described developer: 1: 70 ~ 72.
4. the method for claim 1 is characterized in that, adds the described developer of 10 ~ 28mg and 0.32 ~ 0.64g benzene sulfonic acid in every 10mL water sample to be measured.
5. method as claimed in claim 4 is characterized in that, adds the described developer of 10 ~ 20mg in every 10mL water sample to be measured.
6. method as claimed in claim 4 is characterized in that, adds 0.45 ~ 0.50g benzene sulfonic acid in every 10mL water sample to be measured.
7. kit that detects orthophosphate content in the water body, comprise two pack of separating of developer and benzene sulfonic acid, the mass ratio of two pack is developer: benzene sulfonic acid=10 ~ 28mg: 0.32 ~ 0.64g, wherein developer is 35 ~ 40 by ammonium molybdate, potassium antimony tartrate and three kinds of powder of ascorbic acid in mass ratio: 1: 65 ~ 75 mix.
8. kit as claimed in claim 7 is characterized in that, the mass ratio of ammonium molybdate, potassium antimony tartrate and ascorbic acid is 35 ~ 38 in the described developer: 1: 70 ~ 72.
9. kit as claimed in claim 7 is characterized in that, the mass ratio of described two pack is developer: benzene sulfonic acid=10 ~ 20mg: 0.45 ~ 0.50g.
10. kit as claimed in claim 9, it is characterized in that, described pack is according to the disposable use amount packing for 10mL water sample to be measured, and each color-developer reagent bag has the developer of 10 ~ 20mg, and each benzene sulfonic acid pack has the benzene sulfonic acid of 0.45 ~ 0.50g.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104165849A (en) * | 2014-08-01 | 2014-11-26 | 湖北富邦科技股份有限公司 | Method for determining total phosphorous in surfactant |
| 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 |
| CN106442511A (en) * | 2016-11-21 | 2017-02-22 | 广东环凯微生物科技有限公司 | Water quality phosphate rapid detection kit and detection method |
| CN108279232A (en) * | 2018-01-23 | 2018-07-13 | 浙江大学 | Rice phosphorus content rapid screening method |
| 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 |
| 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 |
| CN109187390A (en) * | 2018-09-13 | 2019-01-11 | 重庆欣欣向荣精细化工有限公司 | A method of measuring phosphorus concentration in water body to be checked |
| CN109406513A (en) * | 2018-12-27 | 2019-03-01 | 广州市合信环保科技有限公司 | A kind of method that environomental pollution source is traced to the source |
| CN109827915A (en) * | 2019-03-12 | 2019-05-31 | 闫宏涛 | A kind of bi-component detection agent measuring phosphorus content |
| CN111239126A (en) * | 2020-03-11 | 2020-06-05 | 深圳市朗诚科技股份有限公司 | Detection reagent combination for phosphate molybdenum antimony resistance method determination and preparation method thereof |
| CN112285039A (en) * | 2020-09-15 | 2021-01-29 | 青海西矿同鑫化工有限公司 | Method for determining phosphate radical in fluosilicic acid |
| CN116429759A (en) * | 2023-02-15 | 2023-07-14 | 北京连华永兴科技发展有限公司 | Phosphate colorimetric detection test paper and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1687787A (en) * | 2005-04-08 | 2005-10-26 | 山西大学 | Method for visual detection of inorganic phosphorus in urine and kit thereof |
| CN101297197A (en) * | 2005-10-26 | 2008-10-29 | 通用电气公司 | Material compositions for sensors for determination of chemical species at trace concentrations and method of using sensors |
-
2012
- 2012-11-15 CN CN2012104591478A patent/CN102914539A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1687787A (en) * | 2005-04-08 | 2005-10-26 | 山西大学 | Method for visual detection of inorganic phosphorus in urine and kit thereof |
| CN101297197A (en) * | 2005-10-26 | 2008-10-29 | 通用电气公司 | Material compositions for sensors for determination of chemical species at trace concentrations and method of using sensors |
Non-Patent Citations (1)
| Title |
|---|
| 国家环境保护局: "《GB 11893-89中华人民共和国国家标准》", 1 July 1990, article "水质总磷的测定 钼酸铵分光光度法", pages: 1-3 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104165849A (en) * | 2014-08-01 | 2014-11-26 | 湖北富邦科技股份有限公司 | Method for determining total phosphorous in surfactant |
| 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 |
| CN106442511A (en) * | 2016-11-21 | 2017-02-22 | 广东环凯微生物科技有限公司 | Water quality phosphate rapid detection kit and detection method |
| CN108279232A (en) * | 2018-01-23 | 2018-07-13 | 浙江大学 | Rice phosphorus content rapid screening method |
| 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 |
| 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 |
| CN109187390A (en) * | 2018-09-13 | 2019-01-11 | 重庆欣欣向荣精细化工有限公司 | A method of measuring phosphorus concentration in water body to be checked |
| CN109406513A (en) * | 2018-12-27 | 2019-03-01 | 广州市合信环保科技有限公司 | A kind of method that environomental pollution source is traced to the source |
| CN109827915A (en) * | 2019-03-12 | 2019-05-31 | 闫宏涛 | A kind of bi-component detection agent measuring phosphorus content |
| CN111239126A (en) * | 2020-03-11 | 2020-06-05 | 深圳市朗诚科技股份有限公司 | Detection reagent combination for phosphate molybdenum antimony resistance method determination and preparation method thereof |
| CN112285039A (en) * | 2020-09-15 | 2021-01-29 | 青海西矿同鑫化工有限公司 | Method for determining phosphate radical in fluosilicic acid |
| CN116429759A (en) * | 2023-02-15 | 2023-07-14 | 北京连华永兴科技发展有限公司 | Phosphate colorimetric detection test paper and preparation method and application thereof |
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Application publication date: 20130206 |