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Vanadium-titanium magnetite microwave digestion and polarographic determination of vanadium

Author: LiangQingXun
Tutor: ZhuXiaPing
School: Chengdu University of Technology
Course: Analytical Chemistry
Keywords: Vanadium-titanium magnetite Microwave digestion Vanadium Polarographic analysis Electrode reaction mechanism
CLC: P618.31
Type: Master's thesis
Year: 2011
Downloads: 72
Quote: 0
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Abstract


Iron ore is the nation-building process in the large-scale use of resources, as well as the large number of mining iron ore imports to bring the quality of the problems can not be ignored. Vanadium-titanium magnetite' dissertation">Vanadium-titanium magnetite is a country to import large quantities of iron ore, but also a relatively insoluble minerals, therefore representative. This topic by using vanadium-titanium magnetite standard as research subjects, were the main elements of microwave digestion and determination of the specific research content and results are as follows: 1. Establish the following four microwave digestion system: (1) parathion mixed acid digestion System: 0.2000g sample, a small amount of water wetting, 9.00mL concentrated phosphoric acid, 3.00mL of concentrated sulfuric acid and a small amount of concentrated nitric acid in the microwave power 350 W continuous 2 min, 560 W continuous 6 min, 350 W continuous for 2 min digestion procedures carried out under sample digestion. (2) hydrofluoric acid and phosphoric acid digestion system: 0.1000g sample, a small amount of water wetting, 2.00mL hydrofluoric acid, 8.00mL concentrated phosphoric acid, the microwave power 280W continuous 6min, 350W continuous digestion procedure under 2min sample digestion. (3) adding the complex digestion system: 0.1000g sample, 0.0400g 8 - hydroxyquinoline, a small amount of water to wet, 10.00 1 2.00mL of concentrated hydrochloric acid under microwave power 385W Digestion 10 1 2min. (4) alkali fusion system: 0.1000g sample was added to the alumina crucible, 3.000g Solvent (m NaOH : m Na2O2 = 1:2), the microwave power 385W sample digestion under 10min. System (1) System (2) using titanium continuous measurement method to determine in which iron and titanium content, system (3) and the system (4) using the measured iron potassium dichromate, titanium in the sample by , Determination of iron content to determine the full extent of digestion. The results show that the establishment of the four microwave digestion system on the vanadium-titanium magnetite can complete digestion, the results meet the requirements of analytical chemistry. (2) established acetic acid - sodium acetate - phenanthroline determination of trace vanadium in vanadium-titanium magnetite new method. After experimental optimization, optimum reagent conditions: 5.00mL pH ≈ 4.5 acetic acid - sodium acetate buffer solution, 3.00mL 1.00g / L phenanthroline, distilled water to volume 25.00mL; optimum conditions: The test waveform is a derivative wave, the initial potential of-0.20V, scan rate of 1.00V / s, the scan times to 4, still time is 14s. In the preferred reagent and the measurement conditions, the vanadium (V) concentration of 0.050 5 .0μg/mL range, the peak height and peak current proportional to the concentration of vanadium, the linear regression equation Ip ' (× 10 4 nA) = 13.631-1.7678c (μg / mL) (n = 7, R 2 = 0.9953), and the detection limit was 0.0042μg / mL. The method is highly sensitive, wide measurement range, easy to operate faster. The method was applied to the newly created real samples of vanadium vanadium-titanium magnetite determination of the accuracy and precision of the analysis of analytical chemistry to meet the requirements. In this paper, the reaction mechanism of the electrode reaction, the results show that the main electrode reactant is protonated phenanthroline, the polarographic wave is irreversible adsorptive wave.

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CLC: > Astronomy,Earth Sciences > Geology > Of ore deposits > Deposit classification > Ferrous metals > Iron
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