CN104777113A - Improved spectrophotometry for phosphorus pentoxide ammonium molybdate - Google Patents
Improved spectrophotometry for phosphorus pentoxide ammonium molybdate Download PDFInfo
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- CN104777113A CN104777113A CN201510167045.2A CN201510167045A CN104777113A CN 104777113 A CN104777113 A CN 104777113A CN 201510167045 A CN201510167045 A CN 201510167045A CN 104777113 A CN104777113 A CN 104777113A
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- phosphorus pentoxide
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Abstract
The invention relates to an improved spectrophotometry for phosphorus pentoxide ammonium molybdate. With the adoption of the improved spectrophotometry, the problem of low sensitivity of the existing determination method for the phosphorus pentoxide is mainly solved. The improved spectrophotometry is characterized by comprising the following measures: firstly, preparing standard phosphorus-pentoxide solution; secondly, taking six 50ml color-comparison tubes with stoppers, respectively adding the standard phosphorus pentoxide solution into the color-comparison tubes by 0.0ml, 2.5ml, 5.0ml, 10.0ml, 15.0ml and 20.0ml, adding 0.5ml sulfuric acid solution, 0.5ml ammonium molybdate solution and 2.0ml hydrazine sulfate solution, putting in a boiling water bath for 10 minutes, then taking out, and cooling to the room temperature; measuring the absorbancy under the 680nm wavelength, drawing a standard curve, and calculating a linear regression equation thereof; and then determining the absorbancy of the sample and calculating the recovery rate of standard addition. The improved spectrophotometry has the advantages of wide application range, simple steps, high sensitivity and good reproducibility.
Description
Technical field
The present invention relates to a kind of assay method of phosphorus pentoxide, be specifically related to a kind of phosphorus pentoxide ammonium molybdate spectrophotometric method of improvement.
Background technology
Phosphorus pentoxide is that phosphorus burns generation in oxygen, chemical formula P
2o
5, white amorphous powder or hexagonal, very easily moisture absorption, 360 DEG C of distillations, do not burn, the large calorimetric of water-soluble generation also generates phosphoric acid, to the reaction of ethanol and aqueous phase seemingly, for acidic oxide is corrosive, unavailable hand directly touches or edible, also not directly smelling, these product according to "
safety management of dangerous chemical products regulations" by public security department's control.
The various ways such as route of entry has suction, eats, percutaneous absorbtion.
Health hazard: poisoning manifestations with
white phosphorusidentical., there is Nausea and vomiting, stomachache, diarrhoea, in a few days, occur jaundice and hepatomegaly in acute poisoning: per os: poisonous substance enters in a few hours, or there is acute hepatic necrosis, the most serious case, in a few hours, patient is proceeded to suppression by excitement, is gone into a coma, circulatory failure, thus dead.Suck: patient with slight symptoms has headache, dizziness, vomiting, general weakness, and moderate patient above-mentioned symptom is heavier, Upper abdominal pain, and arteries and veins is fast, blood pressure is on the low side; Severe intoxication causes acute hepatic necrosis and stupor.Slow poisoning: have respiratory tract symptom, gastritis,
hepatitis,
anaemia, osteoporosis and necrosis etc.
The harm of phosphorus pentoxide to practitioner and the pollution problem to surrounding environment, attract attention, and the monitoring of phosphorus pentoxide in air, must ensure Monitoring Data accurately and reliably.
At present, original standard GBZT160.30-2004 utilizes the phosphorus pentoxide absorbing liquid in Ammonium Molybdate Spectrophotometric Method for Determination air, and in real operation, often there is sample can not detect, the problem that sensitivity is low.
Summary of the invention
In order to overcome the deficiency of background technology, the invention provides a kind of phosphorus pentoxide ammonium molybdate spectrophotometric method of improvement, mainly solve the problem that the sensitivity of existing phosphorus pentoxide assay method is low, it is wide that the phosphorus pentoxide ammonium molybdate spectrophotometric method of this improvement has the scope of application, step is simple, highly sensitive, high repeatability and other advantages.
The technical solution adopted in the present invention is: a kind of phosphorus pentoxide ammonium molybdate spectrophotometric method of improvement, it comprises the steps:
(1) phosphorus pentoxide standard solution preparation:
Accurately take the dipotassium hydrogen phosphate (K that 0.2454g is dried
2hPO
4), soluble in water, be quantitatively transferred in 1000ml volumetric flask, then be diluted to scale, this solution is 100 μ g/ml Standard Reserving Solution.Before use, 10.0 μ g/ml phosphorus pentoxide standard solution are diluted with water to;
(2) drafting of phosphorus pentoxide typical curve
Get 6 50ml color-comparison tubes, add 0.0 respectively, 2.5,5.0,10.0,15.0, the phosphorus pentoxide standard solution of 20.0ml, add distilled water to 10.0ml, be made into 0.0,25.0,50.0,100.0,150.0,200.0 μ g phosphorus pentoxide standard series; In each standard pipe, add 0.5ml sulfuric acid solution, shake up; Add 0.5ml ammonium molybdate solution, mixing; Add 2.0 ml hydrazine sulfate solution, shake up; Add water to 50.0ml, take out after being placed in boiling water bath 10min and be cooled to room temperature; Absorbance is measured, each concentration replication 3 times, with phosphorus pentoxide content x(μ g under 680nm wavelength) for horizontal ordinate, absorbency Y is ordinate, drawing standard curve, and calculates its equation of linear regression.
(3) precision test
Measure each 6 parts of the standard solution containing phosphorus pentoxide 25.0,150.0 μ g respectively.
(4) sample determination
Each 5.0 ml of extracting sample solution add in two 50 ml color-comparison tubes, 1 by all means in add phosphorus pentoxide solution 5.0 ml that normal concentration is 10.0 μ g/ml, another pipe adds water 5.0 ml, measures absorbance, calculate recovery of standard addition according to the operating conditions of standard series.
Sulfuric acid solution preparation in described step (2): concentration is 2.5 mol/ L, measures ρ=1.84 g/ ml sulfuric acid 14.4ml with graduated cylinder, and slow (limit stirring) pours in about 50 ml water, is transferred in 100 ml volumetric flasks, is diluted with water to graticule;
Ammonium molybdate solution preparation in described step (2): concentration is 50g/L, takes 2.5 g ammonium molybdates, is dissolved in the 2.5 mol/ L sulfuric acid of 50 ml;
Hydrazine sulfate solution preparation in described step (2): concentration 15g/L, takes 1.5g hydrazine sulfate and be dissolved in 100 ml distilled water;
Absorbance replicate determination 3 times in described step (2).
The invention has the beneficial effects as follows: owing to taking technique scheme, it is wide that the phosphorus pentoxide ammonium molybdate spectrophotometric method of this improvement has the scope of application, and step is simple, highly sensitive, high repeatability and other advantages.
Accompanying drawing explanation
Fig. 1 is typical curve of the present invention and regression equation schematic diagram.
Embodiment
Below in conjunction with accompanying drawing, embodiments of the present invention is further illustrated:
As shown in Figure 1, a kind of phosphorus pentoxide ammonium molybdate spectrophotometric method of improvement, it comprises the following steps:
(1) sulfuric acid solution preparation: 2.5 mol/ L
Measure ρ=1.84 g/ ml sulfuric acid 14.4ml with graduated cylinder, slow (limit stirring) pours in about 50 ml water, is transferred in 100 ml volumetric flasks, is diluted with water to graticule;
(2) ammonium molybdate solution preparation: 50g/L
Take 2.5 g ammonium molybdates, be dissolved in the 2.5 mol/ L sulfuric acid of 50 ml;
(3) hydrazine sulfate solution preparation: 15g/L
Taking 1.5g hydrazine sulfate is dissolved in 100 ml distilled water;
(4) phosphorus pentoxide standard solution preparation:
Accurately take the dipotassium hydrogen phosphate (K that 0.2454g is dried
2hPO
4), soluble in water, be quantitatively transferred in 1000ml volumetric flask, then be diluted to scale, this solution is 100 μ g/ml Standard Reserving Solution.Before use, 10.0 μ g/ml phosphorus pentoxide standard solution are diluted with water to;
(5) drafting of phosphorus pentoxide typical curve
Get 6 50ml color-comparison tubes, add 0.0 respectively, 2.5,5.0,10.0,15.0, the phosphorus pentoxide standard solution of 20.0ml, add distilled water to 10.0ml, be made into 0.0,25.0,50.0,100,150.0,200.0 μ g phosphorus pentoxide standard series; In each standard pipe, add 0.5ml sulfuric acid solution, shake up; Add 0.5ml ammonium molybdate solution, mixing; Add 2.0 ml hydrazine sulfate solution, shake up; Add water to 50.0ml, take out after being placed in boiling water bath 10min and be cooled to room temperature; Absorbance is measured, each concentration replication 3 times, with phosphorus pentoxide content x(μ g under 680nm wavelength) for horizontal ordinate, absorbency Y is ordinate, drawing standard curve, and calculates its equation of linear regression.
Each pipe absorbance measurement result is as shown in table 1:
| Phosphorus pentoxide content (μ g) | 0.0 | 25.0 | 50.0 | 100.0 | 150.0 | 200.0 |
| Absorbency Y | 0.000 | 0.042 | 0.083 | 0.175 | 0.271 | 0.358 |
(6) precision test
Measure each 6 parts of the standard solution containing phosphorus pentoxide 25.0,150.0 μ g respectively.
Precision test result is in table 2
| Phosphorus pentoxide content (μ g) | 1 | 2 | 3 | 4 | 5 | 6 | On average | Relative standard deviation (%) |
| 25.0 | 0.042 | 0.038 | 0.040 | 0.040 | 0.040 | 0.042 | 0.040 | 3.7 |
| 150.0 | 0.271 | 0.265 | 0.276 | 0.274 | 0.272 | 0.272 | 0.272 | 1.4 |
(7) sample determination
Each 5.0 ml of extracting sample solution add in two 50 ml color-comparison tubes, 1 by all means in add phosphorus pentoxide solution 5.0 ml that normal concentration is 10.0 μ g/ml, another pipe adds water 5.0 ml, measures absorbance, calculate recovery of standard addition according to the operating conditions of standard series.
Recovery of standard addition P (%) calculates with following formula:
P=(mark-on sample measurements-sample measurements) ÷ adds scalar × 100
Sample determination result is as shown in table 3:
Every technician's notice: although the present invention describes according to above-mentioned embodiment, invention thought of the present invention is not limited in this invention, and the repacking of any utilization inventive concept, all will include in this patent scope of patent protection.
Claims (5)
1. the phosphorus pentoxide ammonium molybdate spectrophotometric method improved, is characterized in that comprising the following steps:
(1) phosphorus pentoxide standard solution preparation:
Accurately take the dipotassium hydrogen phosphate (K that 0.2454g is dried
2hPO
4), soluble in water, be quantitatively transferred in 1000ml volumetric flask, then be diluted to scale, this solution is 100 μ g/ml Standard Reserving Solution, before use, is diluted with water to 10.0 μ g/ml phosphorus pentoxide standard solution;
(2) drafting of phosphorus pentoxide typical curve
Get 6 50ml color-comparison tubes, add 0.0 respectively, 2.5,5.0,10.0,15.0, the phosphorus pentoxide standard solution of 20.0ml, add distilled water to 10.0ml, be made into 0.0,25.0,50.0,100.0,150.0,200.0 μ g phosphorus pentoxide standard series; In each standard pipe, add 0.5ml sulfuric acid solution, shake up; Add 0.5ml ammonium molybdate solution, mixing; Add 2.0 ml hydrazine sulfate solution, shake up; Add water to 50.0ml, take out after being placed in boiling water bath 10min and be cooled to room temperature; Absorbance is measured, each concentration replication 3 times, with phosphorus pentoxide content x(μ g under 680nm wavelength) for horizontal ordinate, absorbency Y is ordinate, drawing standard curve, and calculates its equation of linear regression;
(3) precision test
Measure each 6 parts of the standard solution containing phosphorus pentoxide 25.0,150.0 μ g respectively;
(4) sample determination
Each 5.0 ml of extracting sample solution add in two 50 ml color-comparison tubes, 1 by all means in add phosphorus pentoxide solution 5.0 ml that normal concentration is 10.0 μ g/ml, another pipe adds water 5.0 ml, measures absorbance, calculate recovery of standard addition according to the operating conditions of standard series.
2. the phosphorus pentoxide ammonium molybdate spectrophotometric method of improvement according to claim 1, it is characterized in that: sulfuric acid solution preparation in described step (2): concentration is 2.5 mol/ L, ρ=1.84 g/ ml sulfuric acid 14.4ml is measured with graduated cylinder, slowly (limit stirring) pour in about 50 ml water, be transferred in 100 ml volumetric flasks, be diluted with water to graticule.
3. the phosphorus pentoxide ammonium molybdate spectrophotometric method of improvement according to claim 1, is characterized in that: ammonium molybdate solution preparation in described step (2): concentration is 50g/L, takes 2.5 g ammonium molybdates, is dissolved in the 2.5 mol/ L sulfuric acid of 50 ml.
4. the phosphorus pentoxide ammonium molybdate spectrophotometric method of improvement according to claim 1, is characterized in that: hydrazine sulfate solution preparation in described step (2): concentration 15g/L, takes 1.5g hydrazine sulfate and be dissolved in 100 ml distilled water.
5. the phosphorus pentoxide ammonium molybdate spectrophotometric method of improvement according to claim 1, is characterized in that: absorbance replicate determination 3 times in described step (2).
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106153819A (en) * | 2016-07-27 | 2016-11-23 | 湖北富邦科技股份有限公司 | Phosphorus pentoxide assay method in the phosphorus ore of a kind of improvement |
| CN106248467A (en) * | 2016-08-29 | 2016-12-21 | 河南心连心化肥有限公司 | A kind of ultrafiltration pre-treatment measures the method for Biuret Content in humic acid urea |
| CN107703082A (en) * | 2017-11-24 | 2018-02-16 | 昭通市鼎安科技有限公司 | Using the phosphatic method of Ammonium Molybdate Spectrophotometric Method for Determination |
| CN107894415A (en) * | 2017-11-23 | 2018-04-10 | 上海国齐检测技术有限公司 | The assay method of phosphoric acid in a kind of workplace |
| CN108469417A (en) * | 2017-12-19 | 2018-08-31 | 江苏康达检测技术股份有限公司 | The method for measuring phosphoric acid concentration in workplace |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104089957A (en) * | 2014-07-21 | 2014-10-08 | 中蓝连海设计研究院 | Method for determining phosphorus pentoxide in phosphorite by molybdenum blue colorimetric method |
-
2015
- 2015-04-09 CN CN201510167045.2A patent/CN104777113A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104089957A (en) * | 2014-07-21 | 2014-10-08 | 中蓝连海设计研究院 | Method for determining phosphorus pentoxide in phosphorite by molybdenum blue colorimetric method |
Non-Patent Citations (5)
| Title |
|---|
| 宋新魁等: "工作场所空气中磷酸的测定方法", 《中国职业医学》 * |
| 洪雪花: "工作场所空气中五氧化二磷的两种测定方法的比较", 《职业与健康》 * |
| 王国梅: "磷钼蓝分光光度法测定大气中的五氧化二磷", 《分析化学》 * |
| 董玉莲等: "《水质检验》", 31 October 2014 * |
| 黄志强等: "作业场所空气中五氧化二磷测定方法的改进", 《浙江预防医学》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106153819A (en) * | 2016-07-27 | 2016-11-23 | 湖北富邦科技股份有限公司 | Phosphorus pentoxide assay method in the phosphorus ore of a kind of improvement |
| CN106248467A (en) * | 2016-08-29 | 2016-12-21 | 河南心连心化肥有限公司 | A kind of ultrafiltration pre-treatment measures the method for Biuret Content in humic acid urea |
| CN107894415A (en) * | 2017-11-23 | 2018-04-10 | 上海国齐检测技术有限公司 | The assay method of phosphoric acid in a kind of workplace |
| CN107703082A (en) * | 2017-11-24 | 2018-02-16 | 昭通市鼎安科技有限公司 | Using the phosphatic method of Ammonium Molybdate Spectrophotometric Method for Determination |
| CN108469417A (en) * | 2017-12-19 | 2018-08-31 | 江苏康达检测技术股份有限公司 | The method for measuring phosphoric acid concentration in workplace |
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Application publication date: 20150715 |