Presentation to [TITLE OF PRESENTATION]

Presentation to [TITLE OF PRESENTATION]

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

Indicator: sulphosalicylic acid CFe III (mol/L) = CEDTA * V2 / Vsample CFe II (mol/L) = CEDTA * (V3 - V2) / Vsample CSO (mol/L) = 3(CK Cr O * VK Cr O - (CFeSO * V1 + CEDTA * (V3 - V2)) / 6 ) / Vsample 2 2 4 2 7 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

2 3 2 3 U ore processing Milled ore H2SO4 oxidant Leach 1

tails S/L 2 SX or IX 1- PLS (U, Fe2+, Fe3+, Cl- and acid titration) 2- feed (U and acid titration) 3- loaded strip liquor (U and acid titration) 3 U determination: redox titration

Step 1: Pre-reduction of Uranium UO22+ + 2 Fe2+ + 4 H+ = U4+ + 2 Fe3+ + 2 H2O Strong phosphoric acid medium Step 2: Destruction of Fe(II) excess 4 Fe2+ + 2 HNO3 + 4 H+ = 4 Fe3+ + NO + NO2 + 3 H2O Catalyst: ammonium molybdate U determination: redox titration Step 3: Destruction of NO or NO2 with sulpham acid 2 (NH2)HSO3 + NO + NO2= 2 H2SO4 + 2 N2+ H2O Step 4: Dilution with H2SO4 Step 5: Oxidation of U(IV) into U(VI)

U4+ + 2VO2+ = UO22+ + 2V3+ or U4+ + 2 Fe3+ + 2 H2O = UO22+ + 2 Fe2+ + 4 H+ U determination: redox titration Step 6: Dichromatometric titration Cr2O72- + 6 V3+ + 2 H+ = 2 Cr3+ + 6 VO2+ + H2O or Cr2O72- + 6 Fe2+ + 14 H+ = 2 Cr3+ + 6 Fe3+ + 7 H2O Indicator: diphenylamine or Potentiometric titration C U (mol/L) = 3 * CK Cr O * VK Cr O / Vsample 2 2 7

2 2 7 Cl determination: precipitation titration Ag+ + Cl = AgCl Indicator: potassium chromate or dichromate 2 Ag+ + CrO42 = Ag2CrO4 Fe2+ pre-oxidation pH from 6.5 and 10 CCl (mol/L) = CAgNO * VAgNO / Vsample 3 3

Thank you www.mintek.co.za

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