Determination of Low-content Cadmium in Sn-rich Geological Samples by Inductively Coupled Plasma-Mass Spectrometry

YU Lian-ling; GUO Bin; LIU Zhao; ZHAO Xin; DAI Chang-wen; PENG Jun

doi:10.15898/j.cnki.11-2131/td.201906270094

Rock and Mineral Analysis > 2020 > 39(1): 77-84. > DOI: 10.15898/j.cnki.11-2131/td.201906270094

YU Lian-ling, GUO Bin, LIU Zhao, ZHAO Xin, DAI Chang-wen, PENG Jun. Determination of Low-content Cadmium in Sn-rich Geological Samples by Inductively Coupled Plasma-Mass Spectrometry[J]. Rock and Mineral Analysis, 2020, 39(1): 77-84. DOI: 10.15898/j.cnki.11-2131/td.201906270094

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Determination of Low-content Cadmium in Sn-rich Geological Samples by Inductively Coupled Plasma-Mass Spectrometry

Hunan Province Geological Testing Institute, Changsha 410007, China

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Received Date: June 26, 2019
Revised Date: August 18, 2019
Accepted Date: October 20, 2019
Published Date: December 31, 2019

Abstract

HIGHLIGHTS
(1) The open digestion system of three acids and nitric acid extraction were established, which was beneficial to the determination of low-content cadmium by ICP-MS.

(2) On-line equation correction was realized based on the relationship between cadmium and interference elements such as tin, indium, zirconium and molybdenum.

(3) Simultaneous determination of ¹¹¹Cd, ¹¹³Cd and ¹¹⁴Cd isotopes made the analytical results of cadmium more accurate and reliable.

ABSTRACT

BACKGROUNDThere are many kinds of mass spectral interferences when inductively coupled plasma-mass spectrometry (ICP-MS) is used to determine trace amounts of cadmium in geological samples. Usually, on-line or off-line equations are used for correction. When the sample has high tin content, traditional fixed coefficient correction equations can easily lead to significant deviations in the results, and even negative results.
OBJECTIVESTo develop a method for the determination of low-level Cd in high-Sn samples.
METHODSThe system of hydrofluoric acid-perchloric acid-nitric acid digestion and nitric acid compound solvent were applied to analyze the cadmium isotopes, ¹¹¹Cd, ¹¹³Cd and ¹¹⁴Cd for high-tin samples. The influence of interference elements, Sn, In, Zr and Mo on the determination of cadmium was studied.
RESULTSResults showed that there was a non-simple positive correlation between cadmium concentration and the concentration variations of interference sources. The interference increment value increased gradually with the concentration of interference elements. The interference coefficient of ¹¹⁴Sn on ¹¹⁴Cd ranges from 0.0272 to 0.0222, and that of ¹¹³In on ¹¹³Cd was 0.0670 to 0.0412. Cadmium suffers from different degrees of Zr and Mo based oxide/hydroxide mass spectrometry interferences. By measuring the cadmium interference value produced by a single standard solution close to the concentration of the interference source in the sample, the interference coefficient (γ) was corrected on-line to establish an accurate correction equation. The method has been verified by a series of certified standard substances with high accuracy and precision of 6.57%-9.94% (n=7). The method had the Cd detection limit of 0.03mg/kg, which met the requirements of geological sample analysis.
CONCLUSIONSThe method provides a feasible basis for the determination of low-content cadmium in high-Sn geological samples.

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