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Critical evaluation of sequential leaching procedures for the determination of Ni and Mn species in welding fumes.

In this work, welding fume samples were collected in a welding plant, where corrosion-resistant steel and unalloyed structural steel were welded by gas metal arc welding (GMAW) and manual metal arc welding (MMAW) techniques. The welding fumes were sampled with a fixed-point sampling strategy applying Higgins-Dewell cyclones. The following solutions were used to dissolve the different species of Ni and Mn: ammonium citrate solution [1.7% (m/v) diammonium hydrogen citrate and 0.5% (m/v) citric acid monohydrate] for 'soluble' Ni, 50:1 methanol-bromine solution for metallic Ni, 0.01 M ammonium acetate for soluble Mn, 25% acetic acid for Mn(0) and Mn(2+) and 0.5% hydroxylammonium chloride in 25% acetic acid for Mn(3+) and Mn(4+). 'Insoluble' Ni and Mn contents of the samples were determined after microwave-assisted digestion with the mixture of concentrated (cc). HNO(3), cc. HCl and cc. HF. The sample solutions were analysed by inductively coupled plasma quadrupole mass spectrometry and inductively coupled plasma atomic emission spectrometry. The levels of total Ni and Mn measured in the workplace air were different because of significant differences of the fume generation rates and the distributions of the components in the welding fumes between the welding processes. For quality control of the leaching process, dissolution of the pure stoichiometric Mn and Ni compounds and their mixtures weighing was investigated using the optimized leaching conditions. The results showed the adequacy of the procedure for the pure metal compounds. Based on the extraction procedures, the predominant oxidation states of Ni and Mn proved to be very different depending on the welding techniques and type of the welded steels. The largest amount of Mn in GMAW fumes were found as insoluble Mn (46 and 35% in case of corrosion-resistant steel and unalloyed structural steel, respectively), while MMAW fumes contain mainly soluble Mn, Mn(0) and Mn(2+) (78%) and Mn(3+) and Mn(4+) (54%) in case of corrosion-resistant steel and unalloyed structural steel, respectively. According to the results of the leaching procedures, GMAW fumes are rich in oxidic Ni (79%), while Ni compounds in welding fumes generated during MMAW are mainly in easily soluble form (44%). The crystalline phases were identified in each welding fume by X-ray powder diffraction (XRPD) technique as well. From the XRPD spectra, it is clear that GMAW fumes contain predominantly magnetite (FeFe(2)O(4)). In case of structural steel welding, there was a little amount of ferrite (alpha-Fe) also found. Welding fume generated during MMAW of structural steel contained a complex alkali-alkali earth fluoride phase (KCaF(3)-CaF(2)) and some magnetite and jakobsite (MnFe(2)O(4)). The XRPD results did not fully confirm the ones obtained from the extraction experiments. However, some results, for example the rate of soluble Ni and Mn compounds compared to the total, can be useful for further investigations of welding fumes.