Elemental Concentrations of Natural Graphite and Steelmaking Slag: Development of Microwave-Assisted Acid Digestion

Abstract

To develop more sustainable purification and recovery processes, it is critical to accurately determine inorganic impurities of natural graphite (NG) and valuable elements present in low concentrations in steelmaking slag. This study applied three microwave-assisted acid digestion methods for basic oxygen furnace (BOF) slag, NG, and NG ash. Nitric acid (HNO3), hydrochloric acid (HCl), and hydrogen fluoride (HF) were used in method 1. In method 2, method 1 was followed by microwave-assisted boric acid (H3BO3) digestion. In method 3, acids (HNO3, HCl, HF, and H3BO3) were added simultaneously. Concentrations were measured using inductively coupled plasma–optical emission spectrometry. Analytical performance was evaluated using spiking recovery tests (NG) and certified reference (slag) material (CRM). Spiking recoveries for Al, Ca, Fe, K, Mg, Na, and Si were between 5% and 116% (method 1) and 94%–116% (methods 2 and 3). CRM recoveries for Al, Ca, Fe, Mg, Mn, P, Si, Ti, and V were between 2% and 102% (method 1) and 92%–103% (methods 2 and 3). The unsuitability of method 1 was evident due to the low recoveries. Methods 2 and 3 digested Ca- and Si-containing BOF slag completely without visible residue. The sufficient recoveries verified the adequacy of the methods. The suitability of method 3 probably depended on the phases of samples, as quartz was not completely digested from the NG. Method 2 completely digested the inorganic material of NG, and the spiking test showed no loss of volatile silicon compounds. These methods have not been published for NG or NG ash and validated for slag before.