Determination of Vanadium, Iron, Aluminum and Phosphorus in Stone Coal Vanadium Ore by ICP-OES with Open Acid Dissolution

DOU Xiangli; ZHANG Wangqiang; HEI Wenlong; YIN Taogang

doi:10.15898/j.cnki.11-2131/td.202002200020

Rock and Mineral Analysis > 2022 > 41(4): 673-679. > DOI: 10.15898/j.cnki.11-2131/td.202002200020

DOU Xiangli, ZHANG Wangqiang, HEI Wenlong, YIN Taogang. Determination of Vanadium, Iron, Aluminum and Phosphorus in Stone Coal Vanadium Ore by ICP-OES with Open Acid Dissolution[J]. Rock and Mineral Analysis, 2022, 41(4): 673-679. DOI: 10.15898/j.cnki.11-2131/td.202002200020

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Determination of Vanadium, Iron, Aluminum and Phosphorus in Stone Coal Vanadium Ore by ICP-OES with Open Acid Dissolution

Lanzhou Testing and Quality Supervision Center for Geological and Mineral Products, Ministry of Land and Resources, Lanzhou 730050, China

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Received Date: February 19, 2020
Revised Date: April 19, 2022
Accepted Date: April 29, 2022
Available Online: September 08, 2022

Abstract

HIGHLIGHTS
(1) A method for the determination of main components in stone coal vanadium ore by inductively coupled plasma atomic emission spectrometry was provided without burning carbon and dissolving samples in five acid mixed systems.

(2) When the sample weight was 0.1g and the amount of concentrated sulfuric acid was 0.30mL, the digestion rate of the sample was more than 99%.

(3) The results of this method are basically consistent with those of traditional methods such as spectrophotometry and titration, with higher sensitivity and precision.

ABSTRACT

BACKGROUND
The exploration, research and utilization of stone coal vanadium ore resources need accurate composition determination, while there is no standard method for the determination of its main components such as vanadium, iron, aluminum and phosphorus. At the same time, every analysis method currently used has its own shortcomings. When the sample of stone coal vanadium ore is treated by alkali fusion and determined by ICP-OES, the high concentration of soluble salt will lead to high background and interference with the determination. The acid dissolution method can avoid the above problems, but when the conventional four acid system composed of HF+HCl+HNO₃+HClO₄ is used to digest the sample, the components to be tested in the sample cannot be completely released, so the sample needs to be burned at high temperature to remove carbon, making the process is cumbersome.
OBJECTIVES
In order to establish a method for the determination of the main components in stone coal vanadium ore samples by ICP-OES using five acid systems to digest samples.
METHODS
A mixed acid system of H₂SO₄+HF+HCl+HNO₃+HClO₄ with electric hot plate heating and hydrochloric acid extraction were used to digest the samples. The contents of vanadium, iron, aluminum and phosphorus in stone coal vanadium were determined by ICP-OES.
RESULTS
Using the strong oxidizing property of sulfuric acid to oxidize a large amount of carbon in the sample into carbon dioxide, eliminated the process of burning carbon removal, eliminated the adsorption and wrapping of carbon-containing substances on the sample, and significantly enhanced the digestion effect. When the sample weight was 0.1g and the concentration of sulfuric acid was 0.30mL, the digestion rate of the sample reached more than 99%. The detection limit was 17-51mg/kg, relative standard deviation (n=11) was between 1.7%-5.1%, and relative error was -4.6%-2.7%.
CONCLUSIONS
The method has the advantages of low background, high efficiency and accuracy, and can meet the detection requirements of stone coal and vanadium ore samples.
- acid dissolution,
- sulfuric acid,
- inductively coupled plasma-optical emission spectrometry,
- stone coal vanadium,
- vanadium,
- iron,
- aluminium,
- phosphorus

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Determination of Vanadium, Iron, Aluminum and Phosphorus in Stone Coal Vanadium Ore by ICP-OES with Open Acid Dissolution

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