Determination of Rhenium in Tungsten and Molybdenum Ore by ICP-MS with Lefort <i>Aqua</i> <i>Regia</i> Microwave Digestion and 8-hydroxyquinoline Precipitation

XIAO Yufang; JI Yiping; REN Xiaorong; CHEN Zhigui; DONG Xuelin; ZHANG Qinfeng

doi:10.15898/j.ykcs.202307310108

2023 Vol. 42, No. 5

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XIAO Yufang, JI Yiping, REN Xiaorong, CHEN Zhigui, DONG Xuelin, ZHANG Qinfeng. Determination of Rhenium in Tungsten and Molybdenum Ore by ICP-MS with Lefort Aqua Regia Microwave Digestion and 8-hydroxyquinoline Precipitation[J]. Rock and Mineral Analysis, 2023, 42(5): 915-922. doi: 10.15898/j.ykcs.202307310108

Citation:

XIAO Yufang, JI Yiping, REN Xiaorong, CHEN Zhigui, DONG Xuelin, ZHANG Qinfeng. Determination of Rhenium in Tungsten and Molybdenum Ore by ICP-MS with Lefort Aqua Regia Microwave Digestion and 8-hydroxyquinoline Precipitation[J]. Rock and Mineral Analysis, 2023, 42(5): 915-922. doi: 10.15898/j.ykcs.202307310108

Determination of Rhenium in Tungsten and Molybdenum Ore by ICP-MS with Lefort Aqua Regia Microwave Digestion and 8-hydroxyquinoline Precipitation

1.
Wuhan Geological Research Laboratory, Wuhan 430034, China
2.
Hubei Key Laboratory of Resources and Eco-Environment Geology, Wuhan 430034, China
3.
Key Laboratory of Rare Mineral, Ministry of Natural Resources, Wuhan 430034, China

More Information

Corresponding author: DONG Xuelin, dongxlin109@126.com

Received Date: 31 July 2023

Revised Date: 21 August 2023

Accepted Date: 08 September 2023

Publish Date: 31 October 2023

Abstract

Abstract

BACKGROUND
Rhenium (Re) is a key mineral resource widely used in the aerospace field. As one of the rarest elements in the earth, Re rarely exists as an independent mineral but is dispersed in various sulfide ores. Due to its low content and dispersed distribution, the highly sensitive and accurate quantification of Re (ng/g) in complex ore is one of the challenges of modern geological analysis. In order to solve the problem of incomplete decomposition and the great interference caused by co-dissolution of high abundance matrix elements, the existing “digestion-separation” method using 8-12h for one sample is complicated, time-consuming and labor-intensive. Therefore, the development of a simple, fast and low-cost method is urgently required.
OBJECTIVES
To establish an analytical method based on Lefort aqua regia microwave digestion, molybdenum and tungsten precipitation, ICP-mass spectrometry for the determination of rhenium in ore.
METHODS
Lefort aqua regia microwave digestion was used to fully decompose ore, and then the organic precipitator 8-hydroxyquinoline (8-HQ) was used to selectively precipitate high-abundance matrix interference elements molybdenum (Mo) and tungsten (W) in the acid-ammonium acetate buffer system (pH 4.5). The organic precipitator 8-HQ was used to precipitate Mo and W to produce stable hydroxyquinoline molybdenum [MoO₂(C₉H₆ON)₂] and tungsten [WO₂(C₉H₆ON)₂], thereby removing the high-abundance Mo and W in the digestion solution and reducing the interference of matrix on the quantitative analysis of Re. The relevant parameters of Lefort aqua regia microwave digestion and 8-HQ precipitation were systematically studied, and the digestion and precipitation properties were deeply studied by using national certified reference materials.
RESULTS
The key parameters that influence ore digestion including volume of Lefort aqua regia and temperature of microwave digestion, were determined as 2.8mL and 130℃ for step 1 and 150℃ for step 2 separately. The addition amount of 8-HQ was also determined as 0.2mL (3%, w%) by comparing precipitation rates of W, Mo and W-Mo solution (25g/mL) under different amounts, and results showed that the precipitation rate was greater than 95% in different ore digestion solutions. In the established method, the detection limit of Re was 6.9ng/g, the relative error was 0.71%-6.07%, and the RSD was less than 5%.
CONCLUTIONS
The method established in this study can effectively eliminate the interference of matrix elements molybdenum and tungsten on Re quantification without introducing new interference elements. Compared with the existing “digestion-separation” process, the method is simpler and faster (shortened from 8-12h for one sample to approximately 1h) and the method has been successfully applied in molybdenum ore, rhenium molybdenum ore and tungsten-tin bismuth ore. This study proves that interfering instead of target element precipitation is feasible and provides a simple, fast and low-cost method for accurate quantification of Re in complex ore.
- Lefort aqua regia microwave digestion /
- 8-hydroxyquinoline precipitation /
- simple and fast /
- tungsten and molybdenum ore /
- rhenium

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