CN101713741A - Method for determining content of magnesia in phosphorus ore - Google Patents
Method for determining content of magnesia in phosphorus ore Download PDFInfo
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- CN101713741A CN101713741A CN200910272717A CN200910272717A CN101713741A CN 101713741 A CN101713741 A CN 101713741A CN 200910272717 A CN200910272717 A CN 200910272717A CN 200910272717 A CN200910272717 A CN 200910272717A CN 101713741 A CN101713741 A CN 101713741A
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Abstract
The invention relates to a method for determining the content of magnesia in phosphorus ore, which comprises the steps of: when the content of the magnesia in the phosphorus ore is determined, directly placing filter paper together with a precipitate into a beaker after solution forms the precipitate and is filtered, dissolving the precipitate in 20mL of solution of hot hydrochloric acid, then performing subsequent titration step and blank experiment to calculate the content of the magnesia in the phosphorus ore, but not adopting hot hydrochloric acid and hot water to wash the precipitate on the filter paper. The method can effectively reduce analytical error and improve analysis precision.
Description
Technical field
The present invention relates to a kind of method of measuring content of magnesia in the rock phosphate in powder.
Background technology
The principle of at present domestic assay method for content of magnesia in the rock phosphate in powder is: sample solution adds EGTA and triethanolamine is sheltered interfering ions such as calcium, iron, aluminium, in the alkaline solution of pH＞12, generate magnesium hydrate precipitate, after the filtration, be precipitated as dissolving with hydrochloric acid, in the solution of pH=10, be indicator with acid chromium blue k-naphthol green B, with the titration of EDTA standard titration solution, can obtain magnesian content.
Concrete operation method is: take by weighing sample 1g (accurate to 0.0002g) and place the 300mL beaker, add the molten sample of chloroazotic acid, filter behind the constant volume, accurately pipette part filtrate, add ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA) EGTA solution 12mL and triethanolamine 30mL, stir a moment, add 2 peacock green indicator, it is colourless being neutralized to solution with sodium hydroxide solution, after amount 2～5mL, be heated to about 80 ℃, insulation 30min precipitates at this moment and is condensed into piece, uses quick filter paper filtering (being equipped with a small amount of absorbent cotton in the filter paper) while hot, sodium hydroxide solution with heat washs beaker and precipitates each 3～4 times, with hot hydrochloric acid solution 20mL gradation with resolution of precipitate in former beaker, reusable heat water washing filter paper 6～8 times, and be diluted to 150mL; Add a little ascorbic acid, 5mL triethanolamine, being neutralized to pH with ammonia spirit is 7～8 (with the check of pH test paper), ammoniacal liquor-chloride buffer the solution that adds 10ml ph=10, stir a moment, add an amount of K-B indicator, becoming pure blue look to solution by redness with the titration of EDTA standard titration solution is terminal point, does blank test simultaneously.
The magnesium oxide accuracy rate that the method is chemically examined out is low, and the result does not on average wait than the low 0.7%-0.4% of standard specimen, exceed much than the test permissible error, and this result of laboratory test on the low side on the lower sample of content of magnesia, show more obvious.Be because the fibre structure of filter paper can make magnesium hydrate precipitate not wash fully, and can show without any phenomenon whether magnesium hydroxide has been rinsed fully.Error can be bigger so operate.
Summary of the invention
The object of the present invention is to provide a kind of method of measuring content of magnesia in the rock phosphate in powder more accurately, can reduce analytical error.
The present invention realizes in the following manner: a kind of method of measuring content of magnesia in the rock phosphate in powder, carry out according to the following steps: take by weighing rock phosphate in powder sample 1.0000g and place the 300mL beaker, add 40 milliliters of aqua regia dissolution rock phosphate in powder samples, with filtering behind the distilled water constant volume 250mL, accurately pipette 25mL filtrate, add EGTA solution 12mL and triethanolamine 30mL, stir a moment, add 2 peacock green indicator, it is colourless being neutralized to solution with sodium hydroxide solution, after amount 2～5mL; Solution is heated to 80 ℃, insulation 30min, precipitation is condensed into piece, while hot with the filter paper filtering that is equipped with a small amount of absorbent cotton, sodium hydroxide solution with 40 degree heat washs beaker and precipitates each 3～4 times, and filter paper directly is put in the beaker together with precipitation, spends the hydrochloric acid solution 20mL of heat with resolution of precipitate with 40; Spend the distilled water diluting of heat to 150mL with 40 again, add 1 gram ascorbic acid, 5mL triethanolamine, being neutralized to pH with ammonia spirit is 7～8, add 10mL ph=10 ammoniacal liquor-chloride buffer solution, stir a moment, add 3-5 and drip acid chromium blue k-naphthol green B indicator, with volumetric molar concentration be the titration of C mol/L disodium ethylene diamine tetraacetate EDTA standard titration solution to become pure blue look to solution by redness be terminal point, write down the volume V of the disodium ethylene diamine tetraacetate EDTA standard titration solution that is consumed
1ML does blank test simultaneously, the volume V of the disodium ethylene diamine tetraacetate EDTA standard titration solution that record is consumed
0ML, content of magnesia MgO%=C* (V in the rock phosphate in powder sample
1-V
0) * 0.04030*1000, wherein C is the volumetric molar concentration of disodium ethylene diamine tetraacetate.
The present invention compares than existing assay method has following advantage: 1, analytical precision height; 2, analytical error is little; 3, analysis operation is simple, and is easy to operate.
Embodiment
Content of the present invention is described in detail in detail below.
Take by weighing sample rock phosphate in powder table sample (MgO%=1.03) 1.0013g and place the 300mL beaker, add 40 milliliters of aqua regia dissolution rock phosphate in powder samples, with filtering behind the distilled water constant volume 250mL, accurately pipette 25mL filtrate, add EGTA solution 12mL and triethanolamine 30mL, stir a moment, add 2 peacock green indicator, it is colourless being neutralized to solution with sodium hydroxide solution, after amount 3mL; Be heated to about 80 ℃, insulation 30min precipitates at this moment and is condensed into piece, while hot with the filter paper filtering that is equipped with a small amount of absorbent cotton, washs beakers and precipitates each 3～4 times with 40 ℃ sodium hydroxide solutions, with filter paper together with the precipitation directly be put in the beaker, with 40 ℃ of hydrochloric acid solution 20mL with resolution of precipitate; Use 40 ℃ of distilled water dilutings to 150mL again, add 1 gram ascorbic acid, the 5mL triethanolamine, being neutralized to pH with ammonia spirit is 7～8, check with the pH test paper, ammoniacal liquor-chloride buffer the solution that adds 10mL ph=10, stir a moment, add an amount of K-B indicator, with volumetric molar concentration is that to become pure blue look to solution by redness be terminal point to the titration of 0.0102mol/LEDTA standard titration solution, the volume 2.63mL of the disodium ethylene diamine tetraacetate EDTA standard titration solution that record is consumed, do blank test simultaneously, the volume 0.1mL of the disodium ethylene diamine tetraacetate EDTA standard titration solution that consumed of record, calculate in the rock phosphate in powder sample content of magnesia be 1.04%.
In order to verify the accuracy of two kinds of methods, now take three kinds of rock phosphate in powder standard samples that content of magnesia is different, carry out the contrast test of two kinds of methods, the result is as follows:
Magnesium oxide is analyzed the permissible error as a result of parallel sample:
| Magnesium oxide (MgO) % | Permissible error % |
| ??0.10～1.00 | ??0.08 |
| ??5.0 | ??0.12 |
| ??＞5.0 | ??0.20 |
Can obviously find out from analytical table: the content of magnesia of taking out-of-date methods to analyze is much lower than standard sample, the result does not on average wait than standard specimen low 0.7%～0.4%, and the error between the parallel sample is also very big, this result who analyzes is on the low side, and performance is more obvious on the lower sample of content of magnesia.And methods and results of the present invention is little by mistake than standard sample, and the error between the parallel sample is also all in the permissible error scope.
Claims (1)
1. method of measuring content of magnesia in the rock phosphate in powder, it is characterized in that: carry out according to the following steps: take by weighing rock phosphate in powder sample 1.0000g and place the 300mL beaker, add 40 milliliters of chloroazotic acid heating for dissolving rock phosphate in powder samples, with filtering behind the distilled water constant volume 250mL, accurately pipette 25mL filtrate, add EGTA solution 12mL and triethanolamine 30mL, stir a moment, add 2 peacock green indicator, it is colourless being neutralized to solution with sodium hydroxide solution, after amount 2～5mL; This solution is heated to 80 ℃, insulation 30min, precipitation is condensed into piece, while hot with the filter paper filtering that is equipped with a small amount of absorbent cotton, sodium hydroxide solution with 40 degree heat washs beaker and precipitates each 3～4 times, filter paper directly is put in the beaker together with precipitation, spends the hydrochloric acid solution 20mL of heat with resolution of precipitate with 40; Spend the distilled water diluting of heat to 150mL with 40 again, add 1 gram ascorbic acid, 5mL triethanolamine, being neutralized to pH with ammonia spirit is 7～8, ammoniacal liquor-chloride buffer the solution that adds 10mLph=10, stir a moment, add 3-5 and drip acid chromium blue k-naphthol green B indicator, with volumetric molar concentration be the titration of C mol/L disodium ethylene diamine tetraacetate EDTA standard titration solution to become pure blue look to solution by redness be terminal point, write down the volume V of the disodium ethylene diamine tetraacetate EDTA standard titration solution that is consumed
1ML is the volume V that the disodium ethylene diamine tetraacetate EDTA standard titration solution that is consumed is write down in blank test simultaneously
0ML, content of magnesia MgO%=C* (V in the rock phosphate in powder sample
1-V
0) * 0.04030*1000, wherein C is the volumetric molar concentration of disodium ethylene diamine tetraacetate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910272717A CN101713741A (en) | 2009-11-10 | 2009-11-10 | Method for determining content of magnesia in phosphorus ore |
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| CN200910272717A CN101713741A (en) | 2009-11-10 | 2009-11-10 | Method for determining content of magnesia in phosphorus ore |
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| CN101713741A true CN101713741A (en) | 2010-05-26 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102636617A (en) * | 2012-03-28 | 2012-08-15 | 云南磷化集团有限公司 | Method for measuring content of magnesium oxide in iron ores |
| CN103105456A (en) * | 2013-01-28 | 2013-05-15 | 云南磷化集团有限公司 | Method for measuring content of high magnesium in phosphate ore |
| CN104297246A (en) * | 2014-11-03 | 2015-01-21 | 武汉钢铁(集团)公司 | Method for measuring magnesium content in aluminum magnesium alloy powder |
| CN111257094A (en) * | 2020-02-28 | 2020-06-09 | 武汉科技大学 | Filter paper composite filtering method for precipitation quantitative separation |
| CN113418917A (en) * | 2021-07-06 | 2021-09-21 | 广西博世科环保科技股份有限公司 | Analysis method for measuring aluminum content in aluminum ash by EDTA titration |
-
2009
- 2009-11-10 CN CN200910272717A patent/CN101713741A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102636617A (en) * | 2012-03-28 | 2012-08-15 | 云南磷化集团有限公司 | Method for measuring content of magnesium oxide in iron ores |
| CN102636617B (en) * | 2012-03-28 | 2014-12-24 | 云南磷化集团有限公司 | Method for measuring content of magnesium oxide in iron ores |
| CN103105456A (en) * | 2013-01-28 | 2013-05-15 | 云南磷化集团有限公司 | Method for measuring content of high magnesium in phosphate ore |
| CN104297246A (en) * | 2014-11-03 | 2015-01-21 | 武汉钢铁(集团)公司 | Method for measuring magnesium content in aluminum magnesium alloy powder |
| CN111257094A (en) * | 2020-02-28 | 2020-06-09 | 武汉科技大学 | Filter paper composite filtering method for precipitation quantitative separation |
| CN113418917A (en) * | 2021-07-06 | 2021-09-21 | 广西博世科环保科技股份有限公司 | Analysis method for measuring aluminum content in aluminum ash by EDTA titration |
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Open date: 20100526 |