CN104089957A - Method for determining phosphorus pentoxide in phosphorite by molybdenum blue colorimetric method - Google Patents
Method for determining phosphorus pentoxide in phosphorite by molybdenum blue colorimetric method Download PDFInfo
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Abstract
The invention provides a method for determining phosphorus pentoxide in phosphorite by a molybdenum blue colorimetric method. The method comprises the following steps: firstly dissolving an ore sample by sulfuric acid; putting a solution into a 100mL volumetric flask and making up to volume; after diluting by 10 times, adjusting the pH (Potential of Hydrogen) and adding ammonium molybdate tetrahydrate and ascorbic acid; making up to volume and uniformly shaking; and carrying out colorimetry by using a spectrophotometer. According to the method, in an analyzing process of a test sample, the cost of a reagent is greatly reduced and the testing time is shortened; the damages to operators and the environment are reduced; the recycling rate of phosphorus pentoxide which is determined by the method is 97.5%-101.1%; the relative standard deviation (RSD) is 0.29%-0.89%; verified by using phosphorite samples with different grades, the method has the characteristics of accurate result, high precision degree, simplicity, rapidness, low cost and the like.
Description
Technical field
The present invention relates to the analyzing detecting method of rock phosphate in powder composition, particularly a kind of method of phosphorus pentoxide in molybdenum blue colorimetric estimation phosphorus ore.
Background technology
In phosphorus ore, phosphorus pentoxide content is an important indicator of flotation of phosphate rock, conventional method is according to GB/T 1871.1-1995 phosphomolybdic acid quinoline gravimetric method and volumetric determination, complex operation step, spended time is longer, and the reagent consuming is more, quinoline molybdenum lemon ketone is also larger on environment and analysis operation personnel impact, with the present invention, can greatly reduce experiment reagent cost, fund input is few, and analysis speed is fast.
Summary of the invention
The technical matters of solution of the present invention is the deficiency that the existing prior art of pin exists, and provides a kind of procedure of test simple, and fund input is few, the method for phosphorus pentoxide in the phosphorus ore of molybdenum blue colorimetric estimation fast and accurately.
The technical matters of solution of the present invention is to realize by following technical scheme.The present invention is the method for phosphorus pentoxide content in a kind of molybdenum blue colorimetric estimation phosphorus ore, is characterized in, its step is as follows:
(1) take phosphorus ore sample 0.1g-0.2g, be placed in 150mL glass beaker, add 1:2 sulfuric acid (volume ratio that refers to the concentrated sulphuric acid and distilled water is 1:2) 6mL;
(2) glass beaker is placed on electric hot plate, temperature is increased to 300 ℃ gradually, covers surface plate, keep temperature again continuous heating to emitting Bai Yanhou to take off;
(3) by the solution of step (2) gained, with a small amount of water, rinse walls of beaker, and move in 100mL volumetric flask, constant volume, shakes up;
(4) step (3) solution that accurately pipettes 10mL enters into 100mL volumetric flask, adds a small amount of distilled water, flush volume bottle wall;
(5) 1% phenolphthalein indicator is dropped in the 100mL volumetric flask of step (4), with the NaOH of 8N, be neutralized to micro-redly, then add 6 mL1:2 sulfuric acid, the ammonium molybdate acid solution that adds again 5 mL2%, the ascorbic acid solution that adds again 5 mL, is diluted to scale, shakes up;
(6) volumetric flask of step (5) is placed on the thermostat water bath of 70 ℃ and is incubated 20 minutes, after developing the color completely, take off, be cooled to room temperature; With the cuvette of 1cm, using water as reference solution, in spectrophotometer 640nm place, measure its absorbance, on working curve, check in the quality of phosphorus, calculate its percentage composition.
In molybdenum blue colorimetric estimation phosphorus ore of the present invention in the method for phosphorus pentoxide content: the preparation method of described ammonium molybdate acid solution is preferably: first take ammonium molybdate 20g in 1000mL beaker, add 500mL distilled water heating for dissolving, cooling, measuring the 15mL level concentrated sulphuric acid slowly adds in above-mentioned solution again, stir while adding, add again 485mL distilled water, stir, obtain.
In molybdenum blue colorimetric estimation phosphorus ore of the present invention in the method for phosphorus pentoxide content: the preparation method of described ascorbic acid solution is preferably: take 2g solid ascorbic acid and be dissolved in 100mL distilled water, constant volume, shakes up, standby after filtering.
In molybdenum blue colorimetric estimation phosphorus ore of the present invention in the method for phosphorus pentoxide content: typical curve preferably adopts following methods to draw: draw respectively 1.0,2.0,5.0,10.0mL phosphorus standard solution is in 100mL volumetric flask, add 1:2 sulfuric acid 5mL, 2% ammonium molybdate 5mL, 2% ascorbic acid 5mL, is diluted with water to scale, shakes up, be placed on the thermostat water bath of 70 ℃ and be incubated 20 minutes, after developing the color completely, take off, be cooled to room temperature; With the cuvette of 1cm, using water as reference solution, in spectrophotometer 640nm place, measure its absorbance.Phosphorus standard solution preparation method is: accurately take through 0.7668 gram of the potassium dihydrogen phosphate standard reagent of 105 ℃ of oven dry, be dissolved in 1000mL volumetric flask, constant volume, shakes up; 1mL solution is equivalent to 0.4mgP
2o
5.
In molybdenum blue colorimetric estimation phosphorus ore of the present invention in the method for phosphorus pentoxide content, agents useful for same is to be analyzed pure or top grade is pure.
In mensuration phosphorus ore of the present invention, the method for phosphorus pentoxide is that molybdenum blue colorimetric method is measured phosphorus pentoxide, in sample analysis process, greatly reduce reagent cost, shortened test period, reduced the harm to operating personnel and environment, the recovery of the phosphorus pentoxide of measuring by the method is 97.5%～101.1%, relative standard deviation (RSD) 0.29%～0.89%, with the phosphorus ore sample of different grades, this invention is verified, result is accurate, precision is higher, has the features such as easy, quick, cost is low.
embodiment:
Below by embodiment, the present invention will be further described, but be not limited to embodiment.
Embodiment 1, a kind of method of phosphorus pentoxide content in molybdenum blue colorimetric estimation phosphorus ore, and its step is as follows:
(1) take phosphorus ore sample 0.1g-0.2g, be placed in 150mL glass beaker, add 1:2 sulfuric acid 6mL;
(2) glass beaker is placed on electric hot plate, temperature is increased to 300 ℃ gradually, covers surface plate, keep temperature again continuous heating to emitting Bai Yanhou to take off;
(3) by the solution of step (2) gained, with a small amount of water, rinse walls of beaker, and move in 100mL volumetric flask, constant volume, shakes up;
(4) step (3) solution that accurately pipettes 10mL enters into 100mL volumetric flask, adds a small amount of distilled water, flush volume bottle wall;
(5) 1% phenolphthalein indicator is dropped in the 100mL volumetric flask of step (4), with the NaOH of 8N, be neutralized to micro-redly, then add 6 mL1:2 sulfuric acid, the ammonium molybdate acid solution that adds again 5 mL2%, the ascorbic acid solution that adds again 5 mL, is diluted to scale, shakes up;
(6) volumetric flask of step (5) is placed on the thermostat water bath of 70 ℃ and is incubated 20 minutes, after developing the color completely, take off, be cooled to room temperature; With the cuvette of 1cm, using water as reference solution, in spectrophotometer 640nm place, measure its absorbance, on working curve, check in the quality of phosphorus, calculate its percentage composition.
Embodiment 2, in molybdenum blue colorimetric estimation phosphorus ore described in embodiment 1 in the method for phosphorus pentoxide content, the preparation method of described ammonium molybdate acid solution is: first take ammonium molybdate 20g in 1000mL beaker, add 500mL distilled water heating for dissolving, cooling, then measure the 15mL level concentrated sulphuric acid and slowly add in above-mentioned solution, stir while adding, add again 485mL distilled water, stir, obtain.
Embodiment 3, and in the molybdenum blue colorimetric estimation phosphorus ore described in embodiment 1 or 2, in the method for phosphorus pentoxide content, the preparation method of described ascorbic acid solution is: take 2g solid ascorbic acid and be dissolved in 100mL distilled water, constant volume, shakes up, standby after filtering.
Embodiment 4, in molybdenum blue colorimetric estimation phosphorus ore described in embodiment 1 or 2 or 3 in the method for phosphorus pentoxide content, typical curve adopts following methods to draw: draw respectively 1.0,2.0,5.0,10.0mL phosphorus standard solution in 100mL volumetric flask, add 1:2 sulfuric acid 5mL, 2% ammonium molybdate 5mL, 2% ascorbic acid 5mL, is diluted with water to scale, shakes up, be placed on the thermostat water bath of 70 ℃ and be incubated 20 minutes, after developing the color completely, take off, be cooled to room temperature.With the cuvette of 1cm, using water as reference solution, in spectrophotometer 640nm place, measure its absorbance; Phosphorus standard solution preparation method is: accurately take through 0.7668 gram of the potassium dihydrogen phosphate standard reagent of 105 ℃ of oven dry, be dissolved in 1000mL volumetric flask, constant volume, shakes up; 1mL solution is equivalent to 0.4mgP
2o
5.
In above-described molybdenum blue colorimetric estimation phosphorus ore in the method for phosphorus pentoxide content, agents useful for same is to be analyzed pure or top grade is pure.
Embodiment 5, the methods experiment of phosphorus pentoxide content in molybdenum blue colorimetric estimation phosphorus ore:
Test 1. sample precision tests
Accurately take 8 kinds of phosphorus ore sample 0.1g-0.2g(and look P
2o
5content and determine), 6 parts of every kind of sample replicate determinations, are placed in 150mL glass beaker, add 1:2 sulfuric acid 6mL, and glass beaker is placed on electric hot plate, temperature is increased to 300 ℃ gradually, covers surface plate, keep temperature again continuous heating to emitting Bai Yanhou to take off.With a small amount of water, rinse walls of beaker, and move in 100mL volumetric flask, constant volume, shakes up.Accurately pipette 10mL solution and enter into 100mL volumetric flask, add a small amount of distilled water, flush volume bottle wall.1% phenolphthalein indicator is dropped in above-mentioned 100mL volumetric flask, with the NaOH of 8N, be neutralized to micro-redly, then add 6 mL1:2 sulfuric acid, the ammonium molybdate solution of 5 mL2%, then add the ascorbic acid of 5 mL, and be diluted to scale, shake up.Volumetric flask is placed on the thermostat water bath of 70 ℃ and is incubated 20 minutes, after developing the color completely, take off, be cooled to room temperature.With the cuvette of 1cm, using water as reference solution, in spectrophotometer 640nm place, measure its absorbance, on working curve, check in the quality of phosphorus, calculate its percentage composition.Measurement result is in Table 1.
Table 1 sample determination precision test
As can be seen from Table 1, this assay method precision is good, can meet and measure requirement.
Test 2. sample recovery rate tests
8 kinds of phosphorus ore samples in experiment 1 are done to mark-on recovery test: 8 kinds of phosphorus ore samples that accurately take in experiment 1 are placed in 150mL glass beaker, add 1:2 sulfuric acid 6mL, glass beaker is placed on electric hot plate, temperature is increased to 300 ℃ gradually, cover surface plate, keep temperature again continuous heating to emitting Bai Yanhou to take off.With a small amount of water, rinse walls of beaker, and move in 100mL volumetric flask, constant volume, shakes up.Accurately pipette respectively 10mL solution and enter into A group 100mL volumetric flask and B group 100mL volumetric flask, wherein B group respectively adds 0.8mg mark liquid, and following A group is identical with B group experimental procedure: add a small amount of distilled water, flush volume bottle wall.1% phenolphthalein indicator is dropped in above-mentioned 100mL volumetric flask, with the NaOH of 8N, be neutralized to micro-redly, then add 6 mL1:2 sulfuric acid, the ammonium molybdate solution of 5mL2%, then add the ascorbic acid of 5 mL, and be diluted to scale, shake up.Volumetric flask is placed on the thermostat water bath of 70 ℃ and is incubated 20 minutes, after developing the color completely, take off, be cooled to room temperature.With the cuvette of 1cm, using water as reference solution, in spectrophotometer 640nm place, measure its absorbance, on working curve, check in the quality of phosphorus, calculate its percentage composition.Measurement result is in Table 2.
Table 2 sample mark-on recovery test result
As can be seen from Table 2, this assay method recovery is good, can meet and measure requirement.
Test 3. sample accuracy tests
In 1,8 kinds of sample ores are done to precision test, by this method, record the mean value of each sample, in test 3, these 8 kinds of sample ores are done to parallel experiment by phosphomolybdic acid quinoline gravimetric method (arbitration law), record the percentage composition of each sample, draw gravimetric method mean value, the result of these two kinds of experimental techniques is compared, result is as table 3:
Table 3 sample accuracy test result
This method and phosphomolybdic acid quinoline gravimetric method (arbitration law) have been carried out to contrast test, and two kinds of assay method results, all within permissible error scope, can meet and analyze the requirement of measuring as can be seen from Table 3.As can be seen here, this method is feasible.
Sum up: in above 3 experiments, simple with the method formality of phosphorus pentoxide in molybdenum blue colorimetric estimation phosphorus ore, quick and precisely, cost is low, can be widely used in the mensuration of phosphorus pentoxide in phosphorus ore.
The foregoing is only embodiments of the invention, not thereby limit usable range of the present invention.
Claims (5)
1. a method for phosphorus pentoxide content in molybdenum blue colorimetric estimation phosphorus ore, is characterized in that, its step is as follows:
(1) take phosphorus ore sample 0.1g-0.2g, be placed in 150mL glass beaker, add 1:2 sulfuric acid 6mL;
(2) glass beaker is placed on electric hot plate, temperature is increased to 300 ℃ gradually, covers surface plate, keep temperature again continuous heating to emitting Bai Yanhou to take off;
(3) by the solution of step (2) gained, with a small amount of water, rinse walls of beaker, and move in 100mL volumetric flask, constant volume, shakes up;
(4) step (3) solution that accurately pipettes 10mL enters into 100mL volumetric flask, adds a small amount of distilled water, flush volume bottle wall;
(5) 1% phenolphthalein indicator is dropped in the 100mL volumetric flask of step (4), with the NaOH of 8N, be neutralized to micro-redly, then add 6 mL1:2 sulfuric acid, the ammonium molybdate acid solution that adds again 5 mL2%, the ascorbic acid solution that adds again 5 mL, is diluted to scale, shakes up;
(6) volumetric flask of step (5) is placed on the thermostat water bath of 70 ℃ and is incubated 20 minutes, after developing the color completely, take off, be cooled to room temperature; With the cuvette of 1cm, using water as reference solution, in spectrophotometer 640nm place, measure its absorbance, on working curve, check in the quality of phosphorus, calculate its percentage composition.
2. the method for phosphorus pentoxide content in molybdenum blue colorimetric estimation phosphorus ore according to claim 1, it is characterized in that: the preparation method of described ammonium molybdate acid solution is: first take ammonium molybdate 20g in 1000mL beaker, add 500mL distilled water heating for dissolving, cooling, measure again the 15mL level concentrated sulphuric acid and slowly add in above-mentioned solution, stir while adding, then add 485mL distilled water, stir, obtain.
3. the method for phosphorus pentoxide content in molybdenum blue colorimetric estimation phosphorus ore according to claim 1, it is characterized in that: the preparation method of described ascorbic acid solution is: take 2g solid ascorbic acid and be dissolved in 100mL distilled water, constant volume, shakes up, standby after filtering.
4. the method for phosphorus pentoxide content in molybdenum blue colorimetric estimation phosphorus ore according to claim 1, it is characterized in that: typical curve adopts following methods to draw: draw respectively 1.0,2.0,5.0,10.0mL phosphorus standard solution is in 100mL volumetric flask, add 1:2 sulfuric acid 5mL, 2% ammonium molybdate 5mL, 2% ascorbic acid 5mL, be diluted with water to scale, shake up, be placed on the thermostat water bath of 70 ℃ and be incubated 20 minutes, after developing the color completely, take off, be cooled to room temperature; With the cuvette of 1cm, using water as reference solution, in spectrophotometer 640nm place, measure its absorbance; Phosphorus standard solution preparation method is: accurately take through 0.7668 gram of the potassium dihydrogen phosphate standard reagent of 105 ℃ of oven dry, be dissolved in 1000mL volumetric flask, constant volume, shakes up; 1mL solution is equivalent to 0.4mgP
2o
5.
5. the method for phosphorus pentoxide content in molybdenum blue colorimetric estimation phosphorus ore according to claim 1, is characterized in that, agents useful for same is to be analyzed pure or top grade is pure.
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| CN104483313A (en) * | 2014-12-19 | 2015-04-01 | 日泰（上海）汽车标准件有限公司 | Detection solvent and detection method of residual phosphorus on surface of bolt |
| CN104777113A (en) * | 2015-04-09 | 2015-07-15 | 浙江正安检测技术有限公司 | Improved spectrophotometry for phosphorus pentoxide ammonium molybdate |
| 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 |
| CN111650194A (en) * | 2020-07-07 | 2020-09-11 | 中冶北方（大连）工程技术有限公司 | Method for determining phosphorus content in iron ore by bismuth-phosphorus-molybdenum blue |
| CN117538314A (en) * | 2023-11-13 | 2024-02-09 | 山东省产品质量检验研究院 | Quick detection device and detection method for ammonium dihydrogen phosphate |
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| CN111650194A (en) * | 2020-07-07 | 2020-09-11 | 中冶北方（大连）工程技术有限公司 | Method for determining phosphorus content in iron ore by bismuth-phosphorus-molybdenum blue |
| CN117538314A (en) * | 2023-11-13 | 2024-02-09 | 山东省产品质量检验研究院 | Quick detection device and detection method for ammonium dihydrogen phosphate |
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