Method for detecting iodine content in phosphate ore

A technology of iodine content and phosphate rock, applied in the field of detection, can solve the problems of large influence on the environment and analysis operators, long time consumption, etc., and achieve the effects of accurate results, high accuracy and tightness of results, and time saving.

Active Publication Date: 2012-07-18
YUNNAN PHOSPHATE CHEM GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the determination of iodine content in phosphate rock - iodine blue spectrophotometry generally uses phosphoric acid and perchloric acid as solvents for decomposing sampl

Method used

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  • Method for detecting iodine content in phosphate ore
  • Method for detecting iodine content in phosphate ore
  • Method for detecting iodine content in phosphate ore

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] First prepare the main reagents:

[0018] ①Sodium bicarbonate-zinc oxide mixed flux: Weigh 70g of anhydrous sodium bicarbonate and 30g of zinc oxide, put them in a mortar and grind and mix evenly. ②The volume concentration of phosphoric acid solution is: 1+1, 1+2; the volume concentration of sulfuric acid solution is: 1+9. ③ Sodium chloride saturated solution; sodium formate solution: 100 g / L, 200 g / L, 300 g / L; potassium iodide solution: 9 g / L, 10 g / L, 11 g / L; bromine water saturated solution; starch solution prepared before use: 4 g / L, 5g / L, 6g / L. ④Iodine standard solution: 100ug / mL. Weigh 0.1308g of high-grade pure potassium iodide pre-dried at 105-110°C to a constant amount, dissolve in water, transfer it to a 1000mL volumetric flask, dilute to the mark with water, and shake well. 1mL of this solution contains 100ug of iodine. ⑤ Iodine standard solution: 5ug / mL. Pipette 25.0mL of iodine standard solution into a 500mL volumetric flask, dilute to the mark with wa...

Embodiment 2

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

[0028] Weigh about 0.8g of the sample to the nearest 0.0001g and place it in a porcelain crucible; add 6g of sodium bicarbonate-zinc oxide mixed flux, mix well, and then cover with 2g of mixed solvent. Put it in a high temperature furnace from low temperature to 750 °C and keep it for 40min, then take it out and cool it; pour the semi-melt in the crucible into a 100mL beaker, after leaching with water, heat it in a boiling water bath for 30min, cool it, and move it together with the precipitate into a 50mL stopper colorimetric tube, shake well. Put it into a multi-tube rack automatic balancing centrifuge, adjust the parameters at 4000 rpm, and rotate for 4 min to achieve liquid-solid separation. Draw 5.0mL of the clear solution, put it into a 25mL colorimetric tube with a stopper, neutralize it with (1+9) sulfuric acid until the Congo red test paper turns blue, and make up the volume to 8mL with water. Then opera...

Embodiment 3

[0035] On the basis of the experimental method of Example 1,

[0036] Weigh about 1 g of the sample to the nearest 0.0001 g, and place it in a porcelain crucible; add 8 g of sodium bicarbonate-zinc oxide mixed flux, mix well, and then cover with 3 g of mixed solvent. Put it in a high temperature furnace from low temperature to 800 ℃ and keep it for 50min, then take it out and cool it; pour the semi-melt in the crucible into a 100mL beaker, after leaching with water, heat it in a boiling water bath for 30min, cool it, and move it together with the precipitate into a 50mL stopper colorimetric tube, shake well. Put it into a multi-tube rack automatic balancing centrifuge, adjust the parameters at 5000 rpm, and rotate for 5 minutes to achieve liquid-solid separation. Draw 5.0mL of the clear solution, put it into a 25mL colorimetric tube with a stopper, neutralize it with (1+9) sulfuric acid until the Congo red test paper turns blue, and make up the volume to 8mL with water. Then...

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Abstract

A method for detecting iodine content in phosphate ore relates to a detecting method, in particular to a method for detecting the iodine content in deposition phosphorite ore. The method includes the steps: a. placing 0.5-1.0g of a phosphate ore sample into a porcelain crucible, adding mixed fusing agent, mixing evenly, and covering a layer of mixed fusing agent; b. placing the porcelain crucible in a high temperature furnace, rising temperature to 700 to 800 DEG C, taking out, cooling, crushing clinker, pouring the clinker into a centrifugal tube, washing the crucible with hot water, diluting to 50mL, mixing evenly; c. rotating the centrifugal tube through a multi-pipe frame automatic balancing centrifugal machine to separate liquid and solid; d. sucking 5-10mL of supernatant liquor in the centrifugal tube, keeping pH in a range of 2.0-2.5, adding an oxidation agent, enabling potassium iodide to react with starch to generate blue compound, measuring absorbance at a corresponding wavelength position by a spectrophotometer, and calculating the iodine content by working curve method. The method is simple, fast, low in cost and good in reproducibility.

Description

technical field [0001] The invention relates to a detection method, in particular to a method for measuring iodine content in sedimentary phosphorite ore. Background technique [0002] At present, the determination of iodine content in phosphate rock - iodine blue spectrophotometry generally uses phosphoric acid and perchloric acid as solvents for decomposing samples. These solvents have a great impact on the environment and analysis operators. Using cation exchange resin to separate other interfering ions requires strict operation and takes a long time. Contents of the invention [0003] The purpose of the present invention is to overcome the defects of the prior art and provide a simple, fast, environmentally friendly and low-cost method for determining iodine in phosphate rock. [0004] A kind of method of measuring iodine content in the phosphate rock of the present invention is realized by following scheme: [0005] a. Put 0.5-1.0g of phosphate rock sample in a porc...

Claims

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Application Information

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IPC IPC(8): G01N21/31G01N1/44G01N1/38
Inventor 冯晓军陈丹红王云华胡莲珍陈晶亮姜威梅连平卢美莲李翠华周玲芬华瑞娟余惠茹
Owner YUNNAN PHOSPHATE CHEM GROUP CORP
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