Applied Complexometry

Chapter 1 Volumetric Reagents in Complexometry


1.1 The Properties of EDTA


1.2 The Stability of EDTA Complexes


1.3 EDTA as a Volumetric reagent

Chapter 2 Detection of the Titration End-point


2.1 Complexometric Indicators


2.1.1 Introduction


2.1.2 Metallochromic Indicators


2.1.3 The Properties of Metallochromic Indicators


2.1.4 The Sensitivity of the Indicator and Accuracy of the Titration


2.1.5 A Brief Survey of Metallochromic Indicators


2.1.6 Metallofluorescent Indicators


2.1.7 Redox Indicators


2.1.8 Chemiluminescent Indicators


2.1.9 Blocking of Indicators


2.2 Instrumental Methods in Complexometry

Chapter 3 Masking (Screening) Reagents


3.1 Classification of Masking Agents


3.2 Masking Agents for Alkaline Media


3.2.1 Potassium Cyanide


3.2.2 Triethanolamine (TEA)


3.2.3 Thioglycollic Acid (TGA)


3.2.4 3-Mercaptopropionic Acid (MPA)


3.2.5 2,3-Dimercaptopropan-1-o1 (BAL)


3.2.6 Unithiol


3.2.7 Dimercaptosuccinic Acid


3.2.8 Ammonium Fluoride


3.2.9 Hydrogen Peroxide


3.2.10 Sodium or Potassium Hydroxide


3.3 Masking Reagents for Acid Solutions


3.3.1 Sodium or Ammonium Sulphate


3.3.2 Potassium Iodide


3.3.3 Sodium Thiosulphate


3.3.4 Thiourea


3.3.5 Thiosemicarbazide


3.3.6 1,10-Phenanthroline (Phen)


3.3.7 Derivatives of Salicylic Acid


3.3.8 Acetylacetone


3.3.9 Hydrogen Peroxide


3.4 Masking by Precipitation


3.5 Conclusions

Chapter 4 Separation Methods


4.1 Separation during Dissolution


4.2 Separation by Precipitation


4.3 Separation by Electrolysis


4.4 Separation on Ion-Exchangers


4.5 Separation by Liquid-Liquid Extraction

Chapter 5 Apparatus and Solutions


5.1 Glass and Plastic Ware


5.2 Reagents


5.2.1 Ethylenediaminetetra-Acetic Acid - EDTA


5.2.2 The Stability of Standard EDTA Solutions


5.2.3 Standardization of EDTA Solutions


5.2.4 Preparation of Other Standard Solutions


5.2.5 Preparation of Indicators


5.2.6 Buffers

Chapter 6 Classification of EDTA Complexes


6.1 Complexometry of Group I Cations


6.1.1 Zirconium


6.1.2 Hafnium


6.1.3 Thorium


6.1.4 Scandium


6.1.5 Bismuth


6.1.6 Iron


6.1.7 Uranium


6.1.8 Indium


6.1.9 Gallium


6.1.10 Thallium


6.1.11 Chromium


6.1.12 Titanium


6.1.13 Tin


6.1.14 Mercury


6.2 Complexometry of Group II Cations


6.2.1 Copper


6.2.2 Lead


6.2.3 Nickel


6.2.4 Cobalt


6.2.5 Zinc


6.2.6 Cadmium


6.2.7 Aluminum


6.2.8 Manganese


6.2.9 Molybdenum


6.2.10 Vanadium


6.2.11 The Rare-Earth Lanthanides (RE) - The Lanthanides


6.3 Complexometry of Group III Cations


6.3.1 Calcium and Magnesium


6.3.2 Strontium


6.3.3 Barium


6.3.4 Beryllium


6.3.5 Silver


6.3.6 Alkali Metals


6.3.7 Gold and the Platinum Metals

Chapter 7 The Complexometry of Anions


7.1 Fluoride


7.1.1 Determination of Fluoride as CaF2


7.1.2 Determination of Fluoride as PbClF


7.1.3 Determination of Fluoride as PbBrF


7.1.4 Determination of Fluoride as CeFo


7.1.5 Determination of Fluoride as LaF3(H2O)3


7.1.6 Direct Determination of Fluoride by Titration with Thorium Nitrate


7.1.7 Direct Determination of Fluoride with U(SO4)2 Solution


7.2 Determination of Sulphate


7.2.1 Determination of Sulphate as BaSO4


7.2.2 Determination of Sulphate as PbSO4


7·3 Determination of Phosphate


7.3.1 Determination of Phosphate as MgNH4PO4.6H2O


7.3.2 Determination of Phosphate as ZnNH4PO4.6H2O 233


7.3.3 Determination of Phosphate as BiPO4


7.3.4 Determination of Phosphate as Th3(PO4)4


7.3.5 Determination of Phosphate as Zr(HPO4)2 or ZrO(HPO4)


7.3.6 Determination of Phosphate by Precipitation Titration

Chapter 8 Analytical Applications

Chapter 9 Analysis of Alloys


9.1 Aluminum and Aluminum Alloys


9.1.1 Determination of Manganese


9.1.2 Determination of Zinc in Aluminum Alloys


9.1.3 Determinations of Aluminum in Binary Al-Zn Alloys (ALZINOY)


9.1.4 Determination of Lead and Bismuth in Aluminum Alloys


9.1.5 Analysis of Binary Alloys of Aluminum and Titanium


9.1.6 Analysis of Binary Alloys of Aluminum and Lanthanides


9.1.7 Analysis of Some other Aluminum Alloys


9.2 Iron and its Alloys


9.2.1 Analysis of Binary Master Alloys


9.2.2 Analysis of Steels and Cast Iron


9.3 Lead and Lead Alloys


9.3.1 Determination of Lead in the Presence of Other Metals


9.3.2 Determination of Lead in Lead Drosses


9.3.3 Determination of Lead in Accumulator Plates


9.3.4 Analysis of Simple Pb-Sn Alloys


9.3.5 Analysis of White Metals (Pb-Sn-Sb-Cu)


9.3.6 Analysis of Low-Melting Alloys


9.3.7 Analysis of Bi-Pb-Sn Alloys


9.3.8 Analysis of Low-Melting Pb-In Alloys


9·3·9 Analysis of Lead-Silver Alloys


9.3.10 Determination of Lead and Zinc in Brass and Bronzes


9.4 Copper and Copper Alloys


9.4.1 Determination of Tin in Bronze and Gun Metal


9.4.2 Determination of Lead in Brasses and Bronzes


9.4.3 Determination of Zinc and Copper in Cu-Zn Alloys


9.4.4 Determination of Zinc and Lead in Brasses


9.4.5 Determination of Cadmium in Copper Alloys


9.4.6 Determination of Manganese in Copper Alloys


9.4.7 Determination of Aluminum in Copper Alloys


9.4.8 Complete Analysis of Various Copper Alloys

Chapter 10 Analysis of Rocks and Minerals


10.1 Analysis of Limestones, Dolomites and Magnesites


10.1.1 Determination of Calcium in Magnesites


10.1.2 Determination of Magnesium in Dolomites and Limestones


10.1.3 Determination of CaO in Burnt Limestone Fluorspar and Cryolite


10.2.1 Analysis of Fluorite according to Nielsch


10.2.2 Analysis of Fluorite according to Povondra and Vébr


10.2.3 Determination of CaF2 in Fluorite


10.2.4 Analysis of Fluorites according to Steinhauser et Al.


10.2.5 Determination of Fluoride in Cryolite


10.3 Analysis of Phosphates


10.4 Analysis of Monazites

Chapter 11 Analysis of Silicates and Rocks


11.1 Partial Analysis of Silicates and Rocks


11.1.1 Aluminum


11.1.2 Calcium and Magnesium


11.1.3 Additional Methods

Chapter 12 Analysis of Slags


12.1 Determination of Individual Components in Slags


12.1.1 Calcium


12.1.2 Magnesium


12.1.3 Calcium and Magnesium


12.1.4 Aluminum


12.1.5 Titanium


12.1.6 Manganese


12.1.7 Metallic Iron


12.1.8 Magnesium and Magnesium oxide in Uranium Slags


12.2 Complete Analysis of Slags


12.2.1 Analysis of Basic Slags according to Wakamatsu


12.2.2 Analysis of Slags according to Endo


12.2.3 Analysis of Basic Slags


12.2.4 Analysis of Slags according to Pribil and Vesely


12.3 Combined Methods for Slag Analysis


12.3.1 Analysis of Cupola Slags


12.3.2 Analysis of Slags with High Manganese and Phosphorus Contents

Chapter 13 Analysis of Cements


13.1 Determination of CaO and MgO


13.2 Determination of Aluminum


13.3 Total Analysis of Cements


13.3.1 Analysis of Cements (Jugovic)


13.3.2 Rapid Analysis of Cements (Stiglitz and Cornet)


13.3.3 Analysis of Aluminosilicates (Debras-Guedon)


13.3.4 Analysis of Cements (Naidu and Sastry)


13.3.5 Complexometric Determination of Sulphate in Cements

Chapter 14 Analysis of Glasses


14.1 Determination of Calcium, Magnesium and Manganese in Glasses


14.2 Determination of Zirconium


14.3 Determination of Thorium


14.4 Determination of Thorium, Lanthanum, Barium and Boron


14.5 Partial Analyses of Glasses

Chapter 15 Analysis of Ores and Concentrates


15.1 Lead Ores and Concentrates


15.1.1 Lead in Galena


15.1.2 Determination of Lead and Sulphur in Galena


15.1.3 Determination of Lead in Ores


15.1.4 Determination of Lead in Ores after Ion-Exchange Separation


15.2 Zinc Ores and Concentrates


15.2.1 Determination of Zinc in Concentrates


15.2.2 Determination of Zinc in Ores


15.2.3 Determination of Sulphur in Zinc Concentrates


15.3 Zinc-lead Ores


15.4 Chromium Ores


15.4.1 Complete Complexometric Analysis of Chromium Ores


15.4.2 Analysis of Chromium ores according to Král


15.5 Manganese Ores


15.5.1 Determination of Manganese (Povondra and Pribil)


15.5.2 Determination of Manganese (Endo and Koroki)


15.5.3 Determination of Manganese after Ion-Exchange Separation


15.6 Analysis of Copper Ores


15.7 Determination of Ca and Mg in ores and Concentrates

Chapter 16 Analysis of Ferrites


16.1 Dissolution of Ferrites


16.2 Separation of Iron


16.3 Analysis of Individual Ferrites


16.3.1 Rapid Determination of Magnesium in Ferrites


16.3.2 Determination of Strontium in Sr-Ferrites


16.3.3 Determination of Zinc in Zn-Mn Ferrites


16.3.4 Analysis of Mn-Zn-Mg Ferrites


16.3.5 Analysis of Mn-Zn Ferrites


16.3.6 Analysis of Co-Mn-Mg Ferrites


16.3.7 Analysis of Co-Ba Ferrites


16.3.8 Analysis of Pb-Ni-Mg Ferrites


16.4 Potentiometric Analysis of Ferrites

Chapter 17 Analysis of Semiconductors

Chapter 18 Analysis of Catalysts

Chapter 19 Analysis of Pigments

Chapter 20 Analysis of Varnish Driers

Chapter 21 Analysis of Electroplating Solutions


21.1 Acid Baths


21.1.1 Analysis of Copper Plating Baths


21.1.2 Analysis of Nickel Plating Baths


21.1.3 Analysis of Zinc Plating Baths


21.1.4 Analysis of Tin Plating Baths


21.1.5 Analysis of Lead Plating Baths


21.2 Alkaline Baths


21.2.1 Analysis of Silver Plating Baths


21.2.2 Analysis of Copper Plating Solutions


21.2.3 Analysis of Zinc Plating Solutions


21.2.4 Analysis of Cadmium Plating Solutions


21.2.5 Analysis of Brass Plating Solutions


21.2.6 Analysis of Nickel Plating Solutions


21.2.7 Determination of Impurities in Brass and Nickel Baths


21.3 Analysis of Chromium Plating Solutions


21.4 Analysis of Special Plating Solutions


21.4.1 Analysis of Gallium-Indium Electrolytes


21.4.2 Analysis of Indium-Tin Electrolytes


21.4.3 Determination of Gallium in Gold Baths


21.4.4 Determination of Indium in Gold Baths


21.4.5 Determination of Indium, Nickel and Zinc in Gold Baths


21.4.6 Determination of indium, Nickel and Aluminum in Gold Baths


21.4.7 Analysis of Cyanide Gold Baths


21.4.8 Determination of Antimony in Gold-Antimony Baths


21.4.9 Determination of NTA and Cadmium in Cadmium Baths


21.4.10 Determination of Rochelle (Segnette) Salt

Chapter 22 Further Applications of Complexometry


22.1 Pharmaceutical Analysis


22.2 Clinical Analysis


22.3 Analysis of Foods

Index