Determination of Trace Silver in Geological Samples by Inductively Coupled Plasma-Mass Spectrometry with Acid Decomposition and Internal Standard Calibration

LIU Hai-ming; WU Ming-li; CHENG Jing-te

doi:10.15898/j.cnki.11-2131/td.202002190018

Rock and Mineral Analysis > 2021 > 40(3): 444-450. > DOI: 10.15898/j.cnki.11-2131/td.202002190018

LIU Hai-ming, WU Ming-li, CHENG Jing-te. Determination of Trace Silver in Geological Samples by Inductively Coupled Plasma-Mass Spectrometry with Acid Decomposition and Internal Standard Calibration[J]. Rock and Mineral Analysis, 2021, 40(3): 444-450. DOI: 10.15898/j.cnki.11-2131/td.202002190018

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Determination of Trace Silver in Geological Samples by Inductively Coupled Plasma-Mass Spectrometry with Acid Decomposition and Internal Standard Calibration

1.
Key Laboratory of Radioactive and Rare Scattered Mineral, Ministry of Natural Resources, Shaoguan 512026, China
2.
Guangdong Key Laboratory of Radioactive and Rare Resource Utilization, Shaoguan 512026, China

More Information

Received Date: February 18, 2020
Revised Date: September 09, 2020
Accepted Date: November 10, 2020
Published Date: May 27, 2021

Abstract

HIGHLIGHTS
(1) The method of open digestion with three acids, followed by simultaneous extraction of inverse aqua regia and internal standard elements established.

(2) Silver has the characteristics of precipitation before dissolution in excess ammonia aqueous solution, which provides a way to separate mass spectrometry interference elements for the determination of trace silver by ICP-MS.

(3) The internal standard elements coexisted with Ag during the whole process. The internal standard elements were used as the reference system, which resulted in the efficient, fast and accurate determination of trace silver.

ABSTRACT

BACKGROUNDInductively coupled plasma-mass spectrometry (ICP-MS) is used for the determination of trace silver in geological samples. Hydroxides and oxides of Zr, Nb, Mo cause serious overlapping interference on the two mass numbers of ¹⁰⁷Ag and ¹⁰⁹Ag, which can result in a significant deviation of the results.
OBJECTIVESTo develop a method for precise determination of trace Ag in geological samples.
METHODSConsidering that the MS interference of ¹⁰⁷Ag is relatively simple and only ⁹⁰Zr¹⁶OH⁺ and ⁹¹Zr¹⁶O⁺ have interferences on ¹⁰⁷Ag, ¹⁰⁷Ag was selected for the determination of silver in ICP-MS analysis. In the sample pretreatment, hydrofluoric acid, perchloric acid and nitric acid were used for open digestion, and excessive ammonia was added to the extraction solution. The main interference element Zr of ¹⁰⁷Ag was separated by precipitation. Trace silver was determined with Re as the internal standard to complement matrix effect and signal drift.
RESULTSThe content of trace silver in national standard materials of stream sediment, rock and soil was determined by ICP-MS. The test value was consistent with the certified value. The detection limit of the method was 0.0031μg/g, and the relative standard deviation (RSD) was 4.38%.
CONCLUSIONSThe method has the advantages of simple and accurate measurement of trace silver. Moreover, common metal elements can be determined before adding ammonia to the leaching solution, so that the extraction solution can be recycled.
- geological sample,
- trace silver,
- acid dissolution,
- ammonia,
- internal standard method,
- inductively coupled plasma-mass spectrometry

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References (30)

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