Advanced Experimental Inorganic Chemistry

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Advanced Experimental Inorganic Chemistry
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Brief Contents
Preface
Part I. Qualitative Inorganic Analysis
	1. Qualitative Inorganic Analysis Contents
	1. Qualitative Inorganic Analysis
		1.1 Introduction
		1.2 Systematic Procedure for Qualitative Inorganic Analysis
			Colour
			Odour
			Flame Test
			Procedure
			Charcoal Cavity Test
			Procedure
			Borax Bead Test
		1.3 Anion Analysis
			1.3.1 Group A (Dilute H2SO4 group)
			1.3.2 Group B (Dilute H2SO4 + KMnO4 Solution Group)
			1.3.3 Group C (Conc. H2SO4 Group)
			1.3.4 Group D – Special Group
			1.3.5 Scheme II
			1.3.6 Conformatory tests for individual anions
			1.3.7 Tests for anions which interfere in presence of each other
		1.4 Cation Analysis
			1.4.1 Systematic qualitative analysis of cation using hydrogen sulphide
				1.4.1.1 Analysis of Group Zero Cations
				1.4.1.2 Analysis of Group I Cations (Pb2+, Ag+, Hg22+)
				1.4.1.3 Analyses of Group II Cations
				1.4.1.4 Analysis of Group III Cations
				1.4.1.5 Analysis of Group IV Cations
				1.4.1.6 Analysis of Group V Cations
				1.4.1.7 Analysis of Group VI Cations (Mg2+ and K+)
		1.5 Analysis of cations using potassium thiocarbonate reagent
			Preparation of Solution of the Mixture
			Analysis of group I cations (Pb2+, Ag+, Hg22+)
			Analyses of group II cation
			Analysis of group II (A) cations
			Analysis of group II (B) cations
			Analysis of group III cations
			Removal of phosphate
			Analysis of group IV cations
			Analysis of group V cations
			Analysis of group VI cations
		1.6 Greener Alternative to Qualitative Analysis of Cations
			Division of Cations in Different Groups
			Separation of cations in different groups
			1.6.1 Analysis of group zero cations
			1.6.2 Analysis of group I cations
			1.6.3 Analysis of group II cations
			1.6.4 Analysis of group III cations
			1.6.5 Analysis of Group IV Cations
		1.7 Spot Tests for Cations
			1. Aluminium (Al3+)
			2. Ammonium (NH4+)
			3. Antimony (Sb3+)
			4. Arsenic (As3+)
			5. Barium (Ba2+)
			6. Bismuth (Bi3+)
			7. Cadmium (Cd2+)
			8. Calcium (Ca2+)
			9. Chromium (Cr3+)
			10. Cobalt (Co2+)
			11. Copper (Cu2+)
			12. Iron (Fe3+)
			13. Lead (Pb2+)
			14. Magnesium (Mg2+)
			15. Manganese (Mn2+)
			16. Mercury (Hg22+)
			17. Nickel (Ni2+)
			18. Potassium
			19. Silver (Ag+)
			20. Strontium (Sr2+)
			21. Tin (Sn2+)
			22. Zinc (Zn2+)
		1.8 Detection of Metals (Cations) by Flame Photometry
		1.9 Detection of Metals (Cations) by Atomic Absorption Spectroscopy
		1.10 Chromatographic Separation and Identification of Cations
			Principle of Chromatographic Separation
			Types of Chromatography
			Paper Chromatography
			Ascending Paper Chromatography
			Thin Layer Chromatography
			Principle of TLC Separation
			Preparation of TLC Plate
			Procedure for TLC Separation
			Column Chromatography
			Principle of Column Chromatography
			Procedure of Column Chromatography
			1.10.1 Separation and identified of group I cations (Pb+, Ag+, Hg+) by paper chromatography
			1.10.2 Separation and identification of group II A cations (Hg2+, Cu2+, Cd2+ and Bi3+) by paper chromatography
			1.10.3 Separation and identification of group II A cations (Hg2+, Cu2+, Cd2+ and Bi3+) by column chromatography
			1.10.4 Separation and identification of Cu2+ and Cd2+ by paper chromatography
			1.10.5 Separation and identification of group III cations (Fe3+, Al3+, Cr3+) by paper chromatography
			1.10.6 Separation and identification of Fe3+ and Al3+ by paper chromatography
			1.10.7 Separation and identification of group IV cations (Ni2+, Co2+, Mn2+ and Zn2+) by paper chromatography
			1.10.8 Separation and identification of Ni2+ and Co2+ by paper chromatography
			1.10.9 Separation and identification of cations by thin layer chromatography (TLC)
		1.11 Analysis of Insolubles
			Analysis of Single Salt
			Analysis of a Mixture of Insoluble Salts
		1.12 Analysis of a Metal or an Alloy
		1.13 Analysis of Some Rare Elements
			Confirmatory Tests of Tl and W
			1.13.1 Separation, identification of group I cations (Pb2+, Ag+, Hg2), Ti and W
			1.13.2 Separation, identification of group II A cations (Hg2+, Pb2+, Bi3+, Cu2+ and Cd2+), Pt, Au and Pd
			1.13.3 Separation, identification of group II B cations (Ag, Sb, Sn), Pt, Au, Se, Te and Mo
			1.13.4 Separation, identification of group III cations (Fe, Al, Cr), Ti, Zr, Ce, Th and U
			1.13.5 Separation, Identification of Group IV Cation (Ni, Co, Zn, Mn) and Thorium
Part II. Volumetric Analysis, Instrumental Methods of Volumetric Analysis
	2. Volumetric Analysis Contents
	2. Volumetric Analysis
		2.1 Introduction
			Law of Equivalence
			Terms Used in Volumetric Analysis
			Apparatus used in Volumetric Analysis
			Titration Process
			Chemical Balance
			Single Pan Electrical Balance
			Applications of Volumetric Analysis
		2.2 Acidimetry and Alkalimetry
			2.2.1 Determine the Strength of Hydrochloric Acid using
			2.2.2 Determine the Strength of Oxalic Acid Solution Using
			2.2.3 Determine the Amount of Sodium Carbonate and Sodium Hydroxide in the given solution using N/20 hydrochloric acid
			2.2.4 Determine the Amount of Sodium Carbonate and Sodium Bicarbonate Present in the given solution using N/20 hydrochloric acid
		2.3 Redox Titrations
			Introduction
			Indicators
			Determination of Equivalent Weight
			2.3.1 Determine the Strength of given Oxalic Acid Solution by Titrating against about N/20 solution of potassium permanganate
			2.3.2 Dtermine the Strength of a given Mohr’s Salt Solution (Ferrous Ammonium Sulphate) by titrating against approximately N/20 solution of potassium permanganate
			2.3.3 Determine the Strength of Mohr’s Salt Solution Using About N/20 potassium dichromate solution and using diphenyl amine as internal indicator
			2.3.4 Determine the amount of Mohr’s Salt Solution using Approximately N/20 potassium dichromate solution and potassium ferricyanide as the external indicator
			2.3.5 Determine the Strength of a given Copper Sulphate Solution iodometrically using approximately N/20 sodium thiosulphate solution
			2.3.6 Determine the Strength of Potassium Dichromate Solution using approximately N/20 solution of sodium thiosulphate
			2.3.7 Determine the Strength of the given Tartar Emetic Solution iodometrically using approximately N/20 iodine solution
			2.3.8 Determine the Strength of the given Arsenious Oxide Solution iodometrically using approximately N/20 iodine solution
		2.4 Precipitation Titrations
			Introduction
			Indicators
			Determination Equivalent Weight
			2.4.1 Determine the Strength of the given Solution of Sodium Chloride using N/20 silver nitrate solution and fluorescein as indicator
			2.4.2 Determine the Strength of a given Solution of Silver Nitrate by Volhard’s Method
			2.4.3 Determine the Strength of a given Solution of Sodium Chloride by Mohr’s method using potassium chromate as the indicator
		2.5 Complexometric titrations
			Introduction
			Advantages of using of EDTA
			Types of EDTA Titrations
			Indicators
			2.5.1 Determine the Strength of a given Solution of Magnesium Sulphate using EDTA (N/40) and eriochrome black T as indicator
			2.5.2 Determine the Strength of a given Solution of Zinc Sulphate using EDTA (N/40) and eriochrome black T as indicator
			2.5.3 Determine the Amount of a given Solution of Calcium Carbonate using N/40 EDTA and eriochrome black T as indicator
	3. Instrumental Methods of Volumetric Analysis Contents
	3. Instrumental Methods of Volumetric Analysis
		Introduction
		3.1 Potentiometric Titrations
			Principal of Potentiometric Titration
			The Indicator Electrode
			Reference Electrodes
			Apparatus used for Potentiometric Titrations
			Applications of Potentiometric Titrations
			Acidimetry and Alkalimetry
			Redox Titrations
			Precipitation Titrations
			Complexometric Titrations
			Automatic Potentiometric Titrations
			Advantages of Potentiometric Titrations
		3.2 Conductometric titrations
			Introduction
			Terms used in Conductometric Titrations
			Applications of Conductivity
			Types of Conductometric Titrations
			Acidimetry-Alkalimetry
			Strong Acid vs Strong Base
			Weak Acid vs a Strong Base
			Strong Acid vs Weak Base
			Weak Acid vs Weak Base
			Precipitation Titrations
			Advantages of Conductometric Titrations
		3.3 Spectrophotometric Titrations
			Introduction
			Procedure of Titration
			Applications
		3.4 pH-Metric Titrations
			Introduction
			pH-Metric Titration of a Strong Acid with a Strong Base
Part III. Gravimetric Analysis Estimation of More than one Constituent Present Together in a Solution Instrumental Methods of Quantitative Analysis
	4. Gravimetric Analysis Contents
	4. Gravimetric Analysis
		4.1 Introduction
			Steps Involved in Gravimetric Estimations
			Cleaning of the Crucible
			Heating the crucible to constant weight
			Precipitation
			Digestion of the Precipitate
			Filtering and Washing of the Precipitate
			Drying of the Precipitate
			Incineration and Heating of the Precipitate
			Calculation
		4.2 Estimation of copper
			4.2.1 Estimation of Copper as Cuprous Thiocyanate
			4.2.2 Estimation of Copper as Copper Oxide (CuO)
		4.3 Estimation of Iron
		4.4 Estimation of Barium
		4.5 Estimation of Sulphate
		4.6 Estimation of Silver
		4.7 Estimation of Chloride
		4.8 Estimation of Zinc
		4.9 Estimation of Lead
			4.9.1 Estimation of Lead as Lead Sulphate
			4.9.2 Estimation of Lead as Lead Chromate
		4.10 Estimation of Nickel
		4.11 Estimation of Chromium
		4.12 Estimation of Aluminium
		4.13 Estimation of Magnesium
			4.13.1 Estimation of Magnesium as Pyrophosphate (Mg2P2O7) or as Magnesium Ammonium phosphate hexahydrate (MgNH4PO4.6H2O)
			4.13.2 Estimation of Magnesium as Oxinate (8-hydroxyquinolate) (C9H6NO)2Mg.2H2O or Mg(C9H6ON)2
	5. Estimation of more than one Constituent Present Together in a Solution Contents
	5. Estimation of more than one Constituent Present Together in a Solution
		5.1 Introduction
		5.2 Estimation of Copper and Nickel in a Given Solution
		5.3 Estimation of Copper and Zinc in a Given Solution
		5.4 Estimation of Copper and Magnesium in a Given Solution
		5.5 Estimation of Copper and Barium in the Given Solution
		5.6 Estimation of Copper and Silver in the Given Solution
		5.7 Estimation of Silver and Nickel in the Given Solution
		5.8 Estimation of Silver and Zinc in the Given Solution
		5.9 Estimation of Silver and Magnesium in the Given Solution
		5.10 Estimation of Iron and Nickel in the Given Solution
		5.11 Estimation of Iron and Magnesium in the Given Solution
		5.12 Estimation of Copper Nickel, and Zinc in the Given Solution
		5.13 Estimation of Copper, Nickel and Magnesium in the Given Solution
		5.14 Estimation of Silver, Copper and Nickel in the Given Solution
		5.15 Estimation of Copper, Silver and Zinc in the Given Solution
		5.16 Estimation of Siliver, Nickel and Zinc in the Given Solution
		5.17 Estimation of Silver, Nickel and Magnesium in the Given Solution
		5.18 Estimation of Iron, Nickel and Zinc in a Given Solution
	6. Instrumental Methods of Quantitative Analysis Contents
	6. Instrumental Methods of Quantitative Analysis
		6.1 Flame Atomic Emission Spectrometry (FAES)
			Introduction
			Simple FAES Spectrometer
			Interferences in Flame Atomic Emission Spectrometry
			Limitations of Flame Atomic Emission Spectrometry
			Applications of FAES
		6.2 Atomic Absorption Spectroscopy (AAS)
			Introduction
			Instrumentation
			Determination of the Concentration of elements in ppm
			Estimation of Various Elements
Part IV. Inorganic Preparations
	7. Inorganic Preparations Contents
	7. Inorganic Preparations
		7.1 Simple Salts
			7.1.1 Cuprous Chloride, Cu2Cl2
			7.1.2 Cuprous Oxide, Cu2O
			7.1.3 Ferrous Sulphate, FeSO4.7H2O
			7.1.4 Lead Chromate, PbCrO4
			7.1.5 Lead Tetra-acetate, Pb(CH3COO)4
			7.1.6 Magnesium Sulphate MgSO4.7H2O
			7.1.7 Manganese Dioxide (Active), MnO2
			7.1.8 Mercuric Oxide, HgO
			7.1.9 Potassium Dichromate, K2Cr2O7
			7.1.10 Potassium Permanganate, KMnO4
			7.1.11 Silver Oxide, Ag2O
			7.1.12 Sodium Chloride
			7.1.13 Sodium Perborate, BNaO3
			7.1.14 Sodium Sulphite, Na2SO3.7H2O
			7.1.15 Sodium Thiosulphate, Na2S2O3.5H2O
		7.2 Double Salts
			7.2.1 Chrome Alum, K2SO4.Cr2(SO4)3.24H2O
			7.2.2 Chrome Red, PbCrO4.PbO
			7.2.3 Ferric Alum, [(NH4)2SO4.Fe2(SO4)3.24H2O]
			7.2.4 Ferrous Ammonium Sulphate [FeSO4.(NH4)2SO4.6H2O]
			7.2.5 Potash Alum, [K2SO4.Al2(SO4)3.24H2O]
		7.3 Complex Salts
			7.3.1 Aluminium Isopropoxide, Al[OCH(CH3)2]3
			7.3.2 Ammonium Tetrathiocyanato Diamine Chromate [NH4.(NH2)2 Cr (CNS)4]
			7.3.3 Copper Phthalocyanine
			7.3.4 Cuprammonium Sulphate [Cu(NH3)4SO4.H2O]
			7.3.5 Cuprous Mercuric Iodide, Cu2HgI4
			7.3.6 Ferrocene
			7.3.7 Potassium Trioxalatochromate, [K3[Cr(C2O4)3]]
			7.3.8 Prussian Blue [Fe4[Fe(CN)6]3]
			7.3.9 Sodium Ammonium Hydrogen Phosphate [Na(NH4) HPO4.4H2O]
			7.3.10 Sodium Ferric Oxalate, [Na3[Fe(C2O4)3].9H2O
		7.4 Amalgams
			7.4.1 Aluminium-mercury Couple (Al-Hg) (Aluminium Amalgam)
			7.4.2 Sodium Amalgam, Na-Hg
			7.4.3 Zinc Amalgam, Zn-Hg
		7.5 Activated Metals
			7.5.1 Copper Activated
			7.5.2 Potassium Very Fine Particles
			7.5.3 Zinc Activated
		7.6 Organometallics
			7.6.1 Alkyl Lithium
			7.6.2 Methyl Magnesium Bromide, CH3MgBr
		7.7 Miscellaneous Inorganic Preparations
			7.7.1 Sodium Cobaltinitrite, [Na3Co(NO2)6]
			7.7.2 Tetrabutyl Ammonium Hydrogen Sulphate, Bu4N+HSO4–
			7.7.3 Tetrabutylammonium Chromate
			7.7.4 Tetrabutylammonium Permanganate, Bu4NMnO4
			7.7.5 Polystyrene-aluminium Chloride
			7.7.6 Urea Hydrogen Peroxide Adduct
Index