Method for measuring content of high magnesium in phosphate ore

A phosphate rock, high magnesium technology, applied in the field of detection, can solve the problems of poor accuracy of high magnesium results, cumbersome operation, strict requirements, etc., and achieve high accuracy and precision of results, low cost, accuracy and precision. high effect

Inactive Publication Date: 2013-05-15
YUNNAN PHOSPHATE CHEM GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the magnesium hydroxide flocculent precipitate is easily filtered through filter paper, the accuracy of the determination of high magnesium is poor, and the operation is cumbersome and strict.

Method used

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  • Method for measuring content of high magnesium in phosphate ore
  • Method for measuring content of high magnesium in phosphate ore
  • Method for measuring content of high magnesium in phosphate ore

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] First prepare the main reagents:

[0018] ① 0.02mol / L disodium ethylenediaminetetraacetic acid (EDTA) standard solution: Weigh 8g of AR grade disodium ethylenediaminetetraacetic acid and dissolve it in water, dilute to 1000mL with water, and mix well. Calibration shall be carried out according to GB / T601. ②Sodium hydroxide solution: 200g / L, 20g / L; ethylene glycol diethyl ether diammonium tetraacetic acid (EGTA) solution: 70g / L; phenylglycolic acid solution: 50g / L; triethanolamine solution: 1+4; hydrochloric acid Solution: 1+9; ammonia solution: 2+3. ③Acid chrome blue K-naphthol green B indicator: Weigh 0.1g of AR grade acid chrome blue K, weigh 0.1g of AR grade naphthol green B, weigh 20g of AR grade chlorine Potassium chloride is placed in a mortar, thoroughly ground and mixed. ④ pH=10 ammonia water-ammonium chloride buffer solution: Weigh 67.5g of AR grade ammonium chloride, dissolve it in water, add 570mL of AR grade ammonia water, dilute to 1000 mL with water, an...

Embodiment 2

[0027] On the basis of the experimental method of embodiment 1,

[0028] Weigh about 0.15g sample, weigh to an accuracy of 0.0001g, place it in a 250mL beaker, add 25mL hydrochloric acid-nitric acid (aqua regia), gradually raise the temperature to 250°C, cover with a watch glass, and keep the temperature slightly boiling for 15min. After continuing to heat for 2.5 minutes, take down the glass beaker, rinse the watch glass and the inner wall of the beaker with 18mL water to cool, add 10mL phenylglycolic acid, stir well, add 12mL ethylene glycol diethyl ether diammonium tetraacetic acid (EGTA), add 35mL tris Ethanolamine, stir for a while, add 12mL dextrin, add two drops of malachite green indicator solution, neutralize with sodium hydroxide solution until the solution is colorless, then add 4mL, heat the solution to 85°C, and use Filter the funnel with a sponge ball filter pulp, wash the beaker and the precipitate with 55°C hot sodium hydroxide solution for 3 to 4 times; dissolve...

Embodiment 3

[0036] On the basis of the experimental method of embodiment 1,

[0037] Weigh about 0.2g sample, weigh to an accuracy of 0.0001g, place it in a 250mL beaker, add 25mL hydrochloric acid-nitric acid (aqua regia), gradually raise the temperature to 300°C, cover with a watch glass, and keep the temperature slightly boiling for 15min. After continuing to heat for 3 minutes, take off the glass beaker, rinse the watch glass and the inner wall of the beaker with 20mL water to cool, add 15mL phenylglycolic acid, after stirring well, add 14mL ethylene glycol diethyl ether diammonium tetraacetic acid (EGTA), add 40mL triethanolamine , stir for a while, add 15mL dextrin, add two drops of malachite green indicator solution, neutralize the solution with sodium hydroxide solution until the solution is colorless, then add 5mL in excess, heat the solution to 90°C, and use a pad to Filter the pulp through a funnel with a sponge ball, wash the beaker and the precipitate with 60°C hot sodium hyd...

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Abstract

The invention provides a method for measuring the content of high magnesium in phosphate ore, relates to a measuring method, and in particular relates to a method of detecting more than 4 percent of the content of high magnesium in the phosphorite ore. The method comprises the following steps of: measuring the magnesium in a phosphate sample by hydrochloric acid-nitric acid at certain temperature, and introducing magnesium ions to flow into liquid; adding dihydroxy-phenylacetic acid, glycoletherdiaminetetracetic acid (EGTA) liquid, triethanolamine masked titanium, iron, aluminum, alkaline earth and other metal ions; adding dextrin serving as a protective agent to generate a magnesium hydroxide coarse grain type precipitate in alkaline liquid with the pH of more than 12 to inhibit the interference of phosphate radicals and calcium; and filtering and cleaning by a hopper which is provided sponge balls for filtering paper pulp, dissolving the precipitate by hydrochloric acid, and performing titration on the dissolved precipitate by taking acid chrome blue K-naphthol green B serves as an indicating agent by suing thylene diamine tetraacetic acid (EDTA) standard solution in a solution with 10 pH, so as to obtain the content of magnesium oxide. The method has the characteristics of convenience, quickness, low cost, good repeatability and the like.

Description

technical field [0001] The invention relates to a detection method, in particular to a method for determining that the content of magnesium oxide in sedimentary iron block rock ore is greater than 4%. Background technique [0002] At present, the content of magnesium oxide in phosphate rock is determined by the complexometric titration method, and the decomposition samples are mostly melted with sodium hydroxide and dissolved with aqua regia acid. Add EDTA and triethanolamine to the sample solution to mask interfering ions such as calcium, iron, aluminum, etc., and form magnesium hydroxide flocculent precipitates in alkaline solutions with pH>12. After filtration, the precipitates are dissolved in hydrochloric acid. Chromium blue K-naphthol chloride B is used as an indicator, and the content of magnesium oxide can be obtained by titrating with EDTA standard titration solution. Since the magnesium hydroxide flocculent precipitate is easily filtered through filter paper, t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/22G01N31/16
Inventor 冯晓军薛菁
Owner YUNNAN PHOSPHATE CHEM GROUP CORP
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