Abstract
High precision and accuracy make Pb-Fire assay the method of choice for gold analysis in mineralogical samples. The second stage of this method, called cupellation, leaves the used container (cupel) highly contaminated with PbO. Since tons of cupel waste are generated annually from gold analysis worldwide, the disposal of such material constitutes a serious risk to the environment. In the present paper the recovery of the lead from cupel waste by means of an alkaline fusion in the presence of sulfur was evaluated considering the effects of the following variables: amount of NaOH and sulfur, time, and temperature. Gravimetric analyses indicated 81.3% (w/w) recovery of lead in the form of metallic lead from 5.00 g of cupel waste using 3.00 g of NaOH, 0.5 g of S8, after 15 min at 650 °C. During the process, sulfur promoted the reduction of lead oxide. After the process, both the cupel wastes and the resulting secondary wastes presented lead concentrations below the maximum limits determined by both Brazilian legislation and that followed by US Environmental Protection Agency, and can be considered safe for disposal. Furthermore, the proposed method allows cupel wastes to be converted from an environmental liability to a raw material for the production of metallic Pb.
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DNPM—National Department of Mineral Production, Sumário Mineral 2001. http://www.dnpm.gov.br/dnpm/paginas/balanco-mineral/arquivos/balanco-mineral-brasileiro-2001-ouro (2001). Accessed 6 June 2018
WGC—World Gold Council, Gold History and Facts (2018). https://www.gold.org/about-gold/gold-demand (2018). Accessed 6 June 2018
Barefoot, R.R., Van Loon, J.C.: Recent advances in the determination of the platinum group elements and gold. Talanta 49, 1–14 (1999). https://doi.org/10.1016/S0039-9140(98)00347-6
Klemm, D., Klemm, R., Murr, A.: Gold of the Pharaohs—6000 years of gold mining in Egypt and Nubia. J. Afr. Earth Sci. 33, 643–659 (2001). https://doi.org/10.1016/s0899-5362(01)00094-x
Marsden, J.O., House, C.L.: The chemistry of gold extraction. Littleton, Colorado (2006)
Tully, E., Lucey, B.M.: A power GARCH examination of the gold market. Res. Int. Bus. Financ. 21, 316–325 (2007). https://doi.org/10.1016/j.ribaf.2006.07.001
Juvonen, R., Lakomaa, T., Soikkeli, L.: Determination of gold and the platinum group elements in geological samples by ICP-MS after nickel sulphide fire assay: difficulties encountered with different types of geological samples. Talanta 58, 595–603 (2002). https://doi.org/10.1016/S0039-9140(02)00330-2
Vanhaecke, F., Resano, M., Koch, J., McIntosh, K., Günther, D.: Femtosecond laser ablation-ICP-mass spectrometry analysis of a heavy metallic matrix: determination of platinum group metals and gold in lead fire-assay buttons as a case study. J. Anal. At. Spectrom. 25, 1259–1267 (2010). https://doi.org/10.1039/c002746d
Figueiredo, A.M.G., Oliveira, V.X., Jr., Melfi, A.J.: Determination of gold at trace level in samples of weathered itabirite from the iron quadrilateral by analysis by neutron activation. Geochim. Bras. 11, 113–120 (1996). https://doi.org/10.21715/gb.v11i1.122
Anderson, C., Moreno, F., Geurts, F., Wreesmann, C., Ghomshei, M.: A comparative analysis of gold-rich plant material using various analytical methods. Microchem. J. 81, 81–85 (2005). https://doi.org/10.1016/j.microc.2005.01.004
Wall, S.G., Chow, A.: The determination of losses in the fire assay of gold part II. Losses in the complete assay and application of optimal procedures. Anal. Chim. Acta 70, 425–438 (1974). https://doi.org/10.1016/S0003-2670(01)85197-7
Bugbee, E.E.: A textbook of fire assaying. Colorado School of Mines Press, Colorado (1981)
Hall, G.E., Bonham-Carte, G.F., Maclaurin, A.I., Ballantyne, S.B.: Comparison of instrumental neutron activation analysis of geological materials with other multielement techniques. Talanta 37, 135–155 (1990). https://doi.org/10.1016/0039-9140(90)80054-j
Rao, C.R.M., Reddi, G.S.: Platinum group metals (PGM); occurrence, use and recent trends in their determination. Trends Anal. Chem. 19, 565–586 (2000). https://doi.org/10.1016/S0165-9936(00)00031-5
Laurus, K.A., Fletcher, W.K.: Gold distribution in glacial sediments and soils at Boston property, Nunavut, Canada. J. Geochem. Explor. 67, 271–285 (1999). https://doi.org/10.1016/S0375-6742(99)00070-9
Muir, A., Mitchell, J., Flatman, S.R., Sabbagha, C.: A practical guide to re-treatment of gold processing residues. Miner. Eng. 18, 811–824 (2005). https://doi.org/10.1016/j.mineng.2005.01.027
Magalhães, F.B., Carvalho, C.F., Carvalho, E.L.C.N., Yoshida, M.I., Santos, C.G.: Rendering wastes obtained from gold analysis by the lead-fusion fire-assay method non-hazardous. J. Environ. Manage. 110, 110–115 (2012). https://doi.org/10.1016/j.jenvman.2012.06.028
Rustini, R., Taufik, D., Purnawan, M., Julyana, R., Widjanarko, D.I.A.: Characteristic of cupel based on magnesia and synthetic bone ash. JKGI 27, 94–102 (2019). https://doi.org/10.32537/jkgi.v27i2.4413
Liu, Y.-H., Wan, B., Xue, D.-S.: Sample digestion and combined preconcentration methods for the determination of ultra-low gold levels in rocks. Molecules 24, 1778 (2019). https://doi.org/10.3390/molecules24091778
United States Environmental Protection Agency (US EPA). Rules and regulations, Federal Register, Vol. 80, No. 74, The Code of Federal Regulations, Title 40, Part 261, 80 FR 21301, 2015–00257, 21301–21501. (2015)
ABNT—Brazilian Association of Technical Standards. NBR 10004: solid waste e classification, Rio de Janeiro, p. 61. (2004a)
ABNT—Brazilian Association of Technical Standards. NBR 10005: leaching tests, Rio de Janeiro, p. 10. (2004b)
Townsend, T., Musson, S., Dubey, B., Pearson, B.: Leachability of printed wire boards containing leaded and lead-free solder. J. Environ. Manage. 88, 926–931 (2008). https://doi.org/10.1016/j.jenvman.2007.04.017
Moody, N., Yoon, D., Johnson, A., Wassweiler, E., Nasilowski, M., Bulovic, V., Bawendi, M.G.: Decreased synthesis costs and waste product toxicity for lead sulfide quantum dot ink photovoltaics. Adv. Sustain. Syst. 3, 1900061 (2019). https://doi.org/10.1002/adsu.201900061
Ming Xia, M., Muhammad, F., Zeng, L., Li, S., Huang, X., Binquan Jiao, B., Shiau, Y., Li, D.: Solidification/stabilization of lead-zinc smelting slag in composite based geopolymer. J. Clean. Prod. 209, 1206–1215 (2019)
Intrakamhaeng, V., Clavier, K.A., Townsend, T.G.: Hazardous waste characterization implications of updating the toxicity characteristic list. J. Hazard. Mater. 383, 121171 (2020). https://doi.org/10.1016/j.jhazmat.2019.121171
de Andrade Lima, L.R.P., Bernardez, L.A.: Characterization of the lead smelter slag in Santo Amaro, Bahia, Brazil. J. Hazard. Mater. 189, 692–699 (2011). https://doi.org/10.1016/j.jhazmat.2011.02.091
Cerceau, C.I., Carvalho, C.F., Rabelo, A.C.S., Santos, C.G., Gonçalves, S.M.D., Varejão, E.V.V.: Recovering lead from cupel waste generated in gold analysis by Pb-fire assay. J. Environ. Manage. 183, 771–776 (2016). https://doi.org/10.1016/j.jenvman.2016.08.052
Pan, D., Li, L., Tian, X., Wu, Y., Cheng, N., Yu, H.: A review on lead slag generation, characteristics, and utilization. Resour. Conserv. Recycl. 146, 140–155 (2019). https://doi.org/10.1016/j.resconrec.2019.03.036
U. S. Environmental Protection Agency. EPASAB-EEC-COM-99-002, pp. 1–3. United States Environmental Protection Agency (US EPA). Federal register, Announcement of Final Regulatory Determinations for Contaminants on the Third Drinking Water Contaminant Candidate List, 81 FR 32760 No. 1 (Monday, January 4, 2016). 2015-32760. pp. 13–19. (2016)
COPAM/CERH-MG—Environmental Policy Council/Water Resource Council of The Minas Gerais State, Joint Normative Resolution N° 01-Classification of Water Bodies and Environmental Guidelines for Effluent Discharge, Belo Horizonte. (2008)
Hettipathirana, T.D.: Simultaneous determination of parts-per-million level Cr, As, Cd and Pb, and major elements in low level contaminated soils using borate fusion and energy dispersive X-ray fluorescence spectrometry with polarized excitation. Spectrochim. Acta B 59, 223–229 (2004). https://doi.org/10.1016/j.sab.2003.12.013
DNPM—National Department of Mineral Production, Mineral Summary 2014. http://www.anm.gov.br/dnpm/sumarios/chumbo-sumario-mineral-2014/view (2014). Accessed 06 June 2018
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Cerceau, C.I., de Freitas Carvalho, C., Varejão, E.V.V. et al. Recovery of Metallic Lead of Cupel Wastes from Gold Analysis by Alkaline Fusion in the Presence of Sulfur. Waste Biomass Valor 13, 2705–2715 (2022). https://doi.org/10.1007/s12649-022-01678-0
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DOI: https://doi.org/10.1007/s12649-022-01678-0