Council for Mineral Technology reliable results even in field conditions Application of titration techniques for analysis of hydrometallurgical solutions By Volha Bazhko Senior Scientist Titration Advantages of titration methods: Do not require complicated and expensive equipment Simple and fast method Reliable results even under plant conditions
Titration Types of titration: Acid-base titration determination of acidity of solutions determination of alkalinity of solutions neutralisation tests titration of mixtures of acid Precipitation titration determination of Cldetermination of CNdetermination of S2O32- Titration Types of titration: Complexometric titration
determination of base metals with EDTA Redox titration determination of base metals and PGMs dissolved O2, H2O2 and anions determination of the oxidation state of Fe, Mn and other elements in solution Cu/Co processing Milled ore H2SO4 SO2 tails Fe / Fe 2+
Leach Co bleed product 3+ 1 S/L 2 Cu SX 5
4 Cu EW Cu0 1 PLS (Fe2+, Fe3+ and acid titration) 2 SX feed (Fe, Cu2+ and acid titration) 3 SX raffinate (Cu2+, Fe2+, Fe3+ and acid titration) 4 Advanced electrolyte (Cu2+ and acid titration) 5 Spent electrolyte (Cu2+ and acid titration) 3 SO2, Fe2+ and Fe3+ determination
Titration1: Back dichromatometric titration of the amount of Fe2+ and SO32-: 6 Fe2+ + Cr2O72- + 14 H+ = 2 Cr3+ + 6 Fe3+ + 7 H2O 3 SO32-+ Cr2O72- + 8 H+ = 2 Cr3+ + 3 SO42- + 4 H2O Mixed acid (H2SO4+ H3PO4) Indicator: diphenylamine. Titration 2: Fe3+ titration with EDTA. pH < 2 Indicator: sulphosalicylic acid SO2, Fe2+ and Fe3+ determination Titration 3: Total iron determination with EDTA. Pre-oxidation of Fe2+ with H2O2 pH < 2
2 7 Cu and Fe determination 1 Titration: Determination of the amount of copper and iron Fe2+ pre-oxidation Reduction of Fe3+ and Cu2+ with excess of KI Fe2(SO4)3 + 2 KI = 2 FeSO4 + K2SO4 + I2 2 CuSO4 + 4 KI = 2 CuI + 2 K2SO4 + I2 Titration of I2 liberated I2+ 2 Na2S2O3 = Na2S4O6 + 2 NaI Indicator: starch. Fe3+ can be masked by addition of fluoride.
Cu and Fe determination 2 Titration: Determination of copper Masking of Fe3+ with fluoride Reduction of Cu2+ with excess of KI Titration of I2 liberated CCu (mol/L) = CNa S O * V2 / Vsample 2 2 3 CFe (mol/L) = CNa S O * (V1 - V2) / Vsample 2
2 3 Sulphuric acid determination H2SO4 + Na2CO3 = Na2SO4 + H2O + CO2 Mixed indicator Use the solution remaining after the iron and copper titration or mask Fe3+ by addition of excess of KI and Na2S2O3 CH SO (mol/L) = CNa CO * VNa CO / Vsample 2 4
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