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Analysis method of gallium content in tailings of vanadium extraction

A technology for extracting vanadium tailings and analysis methods, applied in the field of analysis and testing, can solve the problems of dark solution, difficult operation, poor reproducibility, etc., and achieve the effects of high accuracy, simple equipment and reliable methods

Active Publication Date: 2017-08-25
南通北外滩建设工程有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method adopted by people such as Long Ping only adopts sulfuric acid to dissolve the ore sample, and the dissolution effect of the vanadium extraction tailings in the present invention is relatively poor, and the extraction agent used is more expensive, the concentration of rhodamine B is larger, and the color of the solution after extraction is darker. The error in the determination of the organic phase is large, the reproducibility is poor, and the steps of filtering with absorbent cotton are cumbersome and difficult to operate

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  • Analysis method of gallium content in tailings of vanadium extraction
  • Analysis method of gallium content in tailings of vanadium extraction
  • Analysis method of gallium content in tailings of vanadium extraction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] 1. Prepare gallium standard solution as usual:

[0047] 1. Preparation of gallium standard solution: gallium standard solution: 1ug / mL;

[0048] Pipette 1ml of the gallium stock solution (1000ug / ml) into a 1000ml volumetric flask and use 6mol / L to make up the volume, the solution is 1ug / ml.

[0049] 2. Preparation of iron-containing standard solution

[0050] Accurately pipette 1ml, 2ml, 3ml, 4ml, 5ml, 6ml, 7ml, 8ml, and 9m gallium standard solution into a 60ml pear-shaped separating funnel, and add ferric chloride solution dropwise (according to the iron content in the sample). Dilute to 10ml with 6mol / l hydrochloric acid. Add 0.60~2.50mLTiCl 3 The solution is purple, 3-5 drops in excess, after standing for 20-30min, add 15mL butyl acetate + toluene (1+1), extract for 1min, discard the water phase after layering, then add 10mL 6mol / L HCl, shake and wash for 30s, Discard the water phase, add 10 mL of water to the organic phase, extract for 1 min, transfer the water ...

Embodiment 2

[0066] Gallium standard working curve is made as shown in the first step of embodiment 1

[0067] Determination of gallium in tailings of vanadium extraction to be tested:

[0068] 1. Weigh 0.1500g of vanadium extraction tailings and add 7g of sodium carbonate + boric acid + borax = 1 + 1 + 1 for fluxing, melt at a high temperature of 950-1000°C for 25 minutes, and take out the molten mass in a beaker;

[0069] 2. Add 40ml (1+1) hydrochloric acid to the fusion beaker, heat and dissolve at 80-120°C, then add 5-6ml concentrated nitric acid, hydrofluoric acid, and perchloric acid to dissolve the sample in smoke, Get 20-30ml test solution, after cooling, use 6mol / L HCl to dilute it in a 200ml volumetric flask;

[0070] 3. Pipette 15ml into a 60mL pear-shaped separating funnel, add 0.60-2.5mL TiCl dropwise 3 , until the solution turns purple, add 3-5 drops in excess, add 15mL butyl acetate + toluene (1+1) after standing for 20-30min, extract for 1min, discard the water phase afte...

Embodiment 3

[0073] Gallium standard working curve is made as shown in the first step of embodiment 1

[0074] Determination of gallium in tailings of vanadium extraction to be tested:

[0075] 1. Weigh 0.2000g of vanadium extraction tailings, add 8g of sodium carbonate + boric acid + borax = 1+1+1 for fluxing, melt at a high temperature of 950-1000°C for 25 minutes, and take out the molten mass in a beaker;

[0076] 2. Add 40ml (1+1) hydrochloric acid to the fusion beaker, heat and dissolve at 80-120°C, then add 5-6ml concentrated nitric acid, hydrofluoric acid, and perchloric acid to dissolve the sample in smoke, Get 20-30ml test solution, after cooling, use 6mol / L HCl to dilute it in a 200ml volumetric flask;

[0077] 3. Pipette 10ml into a 60mL pear-shaped separating funnel, add 0.60mL~2.5mL TiCl dropwise 3 , until the solution turns purple, add 3-5 drops in excess, add 15mL butyl acetate + toluene (1+1) after standing for 20-30min, extract for 1min, discard the water phase after lay...

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Abstract

The invention provides an analysis method for gallium content in vanadium extraction tailings, which belongs to the field of chemical analysis and detection. Add sodium carbonate, boric acid and borax to the vanadium extraction tailings sample to help melting, add hydrochloric acid to dissolve after high-temperature melting, use hydrochloric acid to constant volume, add extraction agent for extraction, and then add an appropriate amount of water for back extraction, so as to obtain a solution of trace gallium , Determination of gallium in the sample liquid by spectrophotometry at a wavelength of 565nm. The invention not only has simple test equipment and low cost, but also has high accuracy rate of measured gallium content, which can completely meet the requirement of routine determination of gallium content in vanadium extraction tailings.

Description

technical field [0001] The invention relates to an analysis method for gallium content in vanadium extraction tailings, belonging to the technical field of analysis and testing. Background technique [0002] Gallium is an important scattered element, which is widely used in the electronics industry and nuclear energy industry. With the rapid development of science and technology in my country, gallium plays an increasingly important role in the national economy. [0003] Gallium is analyzed and determined by spectrophotometry, and ion association extraction method is commonly used, and basic dyes such as butyl rhodamine B are mostly used as chromogenic agents. In recent years, in order to improve the analytical sensitivity and improve the operating conditions, it has been reported that the capsule melting method is used, and more and more types of chromogens are used. [0004] There is no national standard analytical method for the determination of gallium content in vanadi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/31
Inventor 黄平吴恩辉侯静李俊翰杨绍利李军张树立阳雨
Owner 南通北外滩建设工程有限公司
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