Sample Treatment Methods for Determination of Rare Earth Elements in Manganese Ore by High-pressure Closed Digestion-Inductively Coupled Plasma-Mass Spectrometry

Lei WU; Yi-bo LIU; Jia-song WANG; Liang-ying WU; Nan ZHANG; Na WANG

doi:10.15898/j.cnki.11-2131/td.201712060189

Rock and Mineral Analysis > 2018 > 37(6): 637-643. > DOI: 10.15898/j.cnki.11-2131/td.201712060189

Lei WU, Yi-bo LIU, Jia-song WANG, Liang-ying WU, Nan ZHANG, Na WANG. Sample Treatment Methods for Determination of Rare Earth Elements in Manganese Ore by High-pressure Closed Digestion-Inductively Coupled Plasma-Mass Spectrometry[J]. Rock and Mineral Analysis, 2018, 37(6): 637-643. DOI: 10.15898/j.cnki.11-2131/td.201712060189

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Sample Treatment Methods for Determination of Rare Earth Elements in Manganese Ore by High-pressure Closed Digestion-Inductively Coupled Plasma-Mass Spectrometry

1.
Tianjin Center of Geological Survey, China Geological Survey, Tianjin 300170, China
2.
Key Laboratory of Muddy Coast Geo-Environment, China Geological Survey, Tianjin 300170, China

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Received Date: December 05, 2017
Revised Date: May 29, 2018
Accepted Date: June 10, 2018
Published Date: October 31, 2018

Abstract

HIGHLIGHTS
(1) Three manganese ore standard references with different manganese contents and an unknown sample of manganese ore were selected for experiments.

(2) Concentrations of rare-earth elements were determined by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) for comparing the digestion effect of three high-pressure closed digestion methods for manganese ore.

(3) The strong oxidative and catalytic properties of hydrogen peroxide were the key to ensure the digestion effect of manganese ore samples with higher manganese content.

ABSTRACT

BACKGROUNDWith advantages of small sample quantity, less acid, and low blank, high-pressure closed digestion-Inductively Coupled Plasma-Mass Spectrometry became the main method in the determination of rare earth elements. However, the composition of manganese ore is complex with varying manganese contents and different valence states of Mn, often with accompanying (co)producing metals and other impurities. The ore is difficult to digest completely using conventional acid-soluble systems, resulting in inaccurate ICP-MS analytical results.
OBJECTIVESTo optimize the acid-solution system condition of the high-pressure closed digestion method, in order to completely and effectively digest the manganese ore with complex components and improve the accuracy of the results.
METHODSThree standards GBW07261, GBW07263, GBW07266 and an unknown sample of manganese ore were digested using three different acid-solution systems of high-pressure closed digestion:Hydrofluoric acid-nitric acid closed digestion, extracted with nitric acid (Method 1); Hydrofluoric acid-nitric acid-hydrogen peroxide closed digestion, redissolved with nitric acid-hydrogen peroxide, extracted with nitric acid (Method 2); Hydrofluoric acid-nitric acid closed digestion, redissolved with hydrochloric acid, extracted with nitric acid (Method 3). The contents of rare-earth elements were then determined by ICP-MS.
RESULTSMethods 2 and Methods 3 can completely digest manganese ore samples. The results of rare-earth elements by ICP-MS were similar, and were consistent with the results of conventional sodium peroxide fusion. However, during the experimental process, for samples with high manganese content, Method 3 required repeated additions of hydrochloric acid before the samples were completely digested, whereas Method 2 need only one repeat. The precision of Method 2 was 0.96%-2.68%, and the recovery was 95.0%-107.0%.
CONCLUSIONSFor different manganese ore samples, Method 2 can completely digest the samples. The determination of rare earth elements was reliable by ICP-MS. Method 2 was the most suitable sample digestion method for the determination of rare earth elements in manganese ores.
- manganese ore,
- rare earth elements,
- high-pressure closed digestion,
- hydrogen peroxide,
- Inductively Coupled Plasma-Mass Spectrometry

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Sample Treatment Methods for Determination of Rare Earth Elements in Manganese Ore by High-pressure Closed Digestion-Inductively Coupled Plasma-Mass Spectrometry

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