Determination of Gallium in Coal Fly Ash by Inductively Coupled Plasma-Optical Emission Spectrometry with Microwave Digestion

HUANG Jing; WANG Ying-bin; ZHOU Guan-xuan; MA Zhen-qian

doi:10.15898/j.cnki.11-2131/td.201905190065

Rock and Mineral Analysis > 2020 > 39(1): 92-98. > DOI: 10.15898/j.cnki.11-2131/td.201905190065

HUANG Jing, WANG Ying-bin, ZHOU Guan-xuan, MA Zhen-qian. Determination of Gallium in Coal Fly Ash by Inductively Coupled Plasma-Optical Emission Spectrometry with Microwave Digestion[J]. Rock and Mineral Analysis, 2020, 39(1): 92-98. DOI: 10.15898/j.cnki.11-2131/td.201905190065

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Determination of Gallium in Coal Fly Ash by Inductively Coupled Plasma-Optical Emission Spectrometry with Microwave Digestion

School of Science, China University of Geosciences(Beijing), Beijing 100083, China

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Received Date: May 18, 2019
Revised Date: August 31, 2019
Accepted Date: October 19, 2019
Published Date: December 31, 2019

Abstract

HIGHLIGHTS
(1) A coal fly ash sample with unknown gallium content and a standard reference were selected for experiments.

(2) The influence of the amount of nitric acid, hydrochloric acid and hydrofluoric acid on the leaching effect was investigated.

(3) The method introduces hydrochloric acid and reduces the amount of hydrofluoric acid, greatly shortening the time of removing fluoride.

ABSTRACT

BACKGROUNDThe content of gallium in coal fly ash is 12-230μg/g. The determination of gallium in coal fly ash is crucial to realize the high-value-added utilization of coal fly ash. As a sample pretreatment method, the conventional open wet digestion method has limitations including a large amount of hydrofluoric acid, corrosion of analytical instruments, long dissolution time, the loss of elements, and environmental pollution. Microwave digestion has the advantages of complete digestion, minimal loss, and short digestion time, which can effectively solve the shortcomings of the open wet digestion method.
OBJECTIVESTo develop a good method for the determination of gallium in coal fly ash.
METHODSThe coal fly ash was collected from a power plant in Inner Mongolia. The sample was digested with nitric acid (5.0mL), hydrofluoric acid (1.0mL), hydrochloric acid (5.0mL) and perchloric acid (1.0mL) by microwave digestion and then determined by inductively coupled plasma-optical emission spectrometry (ICP-OES).
RESULTSThe results showed that gallium could be leached totally using HNO₃-HF-HCl-HClO₄ (5:1:5:1, V/V) when the temperature was 190℃, the time 30 minutes and the microwave power 1400W. The limit of detection was 0.004mg/L. The relative standard deviation (RSD) was 1.7% with the recoveries ranging from 95.1% to 100.9%.
CONCLUSIONSICP-OES with microwave digestion method adds hydrochloric acid and reduces the amount of hydrofluoric acid, thus shortening the time of removing fluoride and reducing the damage to instruments. The method is easy to be used for the determination of trace gallium in coal fly ash.

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Determination of Gallium in Coal Fly Ash by Inductively Coupled Plasma-Optical Emission Spectrometry with Microwave Digestion