Determination of Rare Earth Elements in Sepiolite by ICP-MS Using Microwave Digestion

Nan ZHANG; Tie-min XU; Liang-ying WU; Shuang WEI; Peng-da FANG; Jia-song WANG

doi:10.15898/j.cnki.11-2131/td.201803160023

Rock and Mineral Analysis > 2018 > 37(6): 644-649. > DOI: 10.15898/j.cnki.11-2131/td.201803160023

Nan ZHANG, Tie-min XU, Liang-ying WU, Shuang WEI, Peng-da FANG, Jia-song WANG. Determination of Rare Earth Elements in Sepiolite by ICP-MS Using Microwave Digestion[J]. Rock and Mineral Analysis, 2018, 37(6): 644-649. DOI: 10.15898/j.cnki.11-2131/td.201803160023

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Determination of Rare Earth Elements in Sepiolite by ICP-MS Using Microwave Digestion

Tianjin Center of Geological Survey, China Geological Survey, Tianjin 300170, China

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Received Date: March 15, 2018
Revised Date: May 02, 2018
Accepted Date: June 10, 2018
Published Date: October 31, 2018

Abstract

HIGHLIGHTS
(1) The contents of 15 rare earth elements in sepiolite were determined by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) using microwave digestion.

(2) Three dissolving systems were compared to evaluate the dissolution effect of nitric acid-hydrofluoric acid-hydrogen peroxide, nitric acid-hydrofluoric acid and nitric acid-hydrogen peroxide.

(3) The method used less acid and had higher dissolution efficiency and the analytical results were in good agreement with those of the closed acid dissolution ICP-MS method.

ABSTRACT

BACKGROUNDSepiolite is a fibrous hydrous magnesium rich silicate clay mineral with the content of rare earth elements between 1×10^-7 and 1×10^-5. There is no national standard method for the determination of rare earth elements in sepiolite. Determination of rare earth elements in rocks commonly uses ICP-MS. Sample pretreatments generally use closed digestion and alkaline fusion, but these two treatments are time consuming and inefficient.
OBJECTIVESTo find an efficient dissolution method for the determination of 15 rare earth elements in sepiolite.
METHODSBy comparing three sample pretreatment methods of nitrate hydrofluoric acid hydrogen peroxide, nitric acid-hydrofluoric acid and nitric-acid hydrogen peroxide, the nitric acid-hydrofluoric acid solution system was selected. Microwave digestion was carried out and the hydrofluoric acid was driven off to avoid the formation of insoluble fluorides from the hydrofluoric acid. The content of 15 rare earth elements was determined by ICP-MS.
RESULTSDue to the high content of magnesium in sepiolite, two internal standards of ¹⁰³Rh and ¹⁸⁵Re are selected to compensate for the drift of analytical signals and to correct matrix effects. The recoveries of the method range from 91.2% to 110.9%. The detection limits are 0.002-0.011 μg/L, and the precisions are 0.81%-2.79%.
CONCLUSIONSThe result of this method is in good agreement with that of the closed acid-digestion ICP-MS method, and with a small amount of acid (7 mL), high digestion efficiency (1 h), and a lower detection limit.
- sepiolite,
- rare earth elements,
- microwave digestion,
- nitric acid-hydrofluoric acid,
- Inductively Coupled Plasma-Mass Spectrometry

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