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Student Projects for B.Sc. Chemistry Dr. R. Rajeev VSSC, Thiruvananthapuram.

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Presentation on theme: "Student Projects for B.Sc. Chemistry Dr. R. Rajeev VSSC, Thiruvananthapuram."— Presentation transcript:

1 Student Projects for B.Sc. Chemistry Dr. R. Rajeev VSSC, Thiruvananthapuram

2 Project Introduction Relevance Applications Literature survey Scope of work Experimental Procedure Materials Instrumentation for experiments and characterization Results & Discussion Conclusions Acknowledgements References Feasibility

3 Where to find a topic / subject Inorganic Chemistry Synthesis of metal oxides Applications metallurgy, catalysts, fillers in composites, ceramics, pigments, paints Properties Inertness, catalytic activity, stability, purity, colour Thermal, electrical, magnetic and spectral properties Particle characteristics like size (macro, micro, nano), shape, surface area, porosity Properties varies with method of preparation, heat treatment, precursor

4 Iron oxide Oxides of Iron iron(II) oxide, wüstite (FeO) iron(II) oxidewüstite iron(II,III) oxide, magnetite (Fe 3 O 4 ) iron(II,III) oxidemagnetite iron(III) oxide (Fe 2 O 3 ) iron(III) oxide – alpha phase, hematite (α-Fe 2 O 3 ) beta phase, (β-Fe 2 O 3 ) alpha phasehematitebeta phase – gamma phase, maghemite (γ-Fe 2 O 3 ) gamma phasemaghemite – epsilon phase, (ε-Fe 2 O 3 ) epsilon phase Hydroxides iron(II) hydroxide (Fe(OH) 2 ) iron(II) hydroxide iron(III) hydroxide (Fe(OH) 3 ), (bernalite) iron(III) hydroxidebernalite Oxide/hydroxides goethite (α-FeOOH), goethite akaganéite (β-FeOOH), akaganéite lepidocrocite (γ-FeOOH), lepidocrocite feroxyhyte (δ-FeOOH), feroxyhyte ferrihydrite (Fe 5 HO 8 ·4H 2 O approx.), or 5Fe 2 O 3 9H 2 O, better recast as FeOOH0.4H 2 O ferrihydrite high-pressure FeOOH schwertmannite (ideally Fe 8 O 8 (OH) 6 (SO)·nH 2 O or Fe O 16 (OH,SO 4 ) ·10-12H 2 O) schwertmannite green rust (Fe III x Fe II y (OH) 3x+2y-z (A - ) z ; where A - is Cl - or 0.5SO 4 2- ) green rust

5 Synthesis Precipitation of from an aqueous solution of iron compound Precipitating agent,, ammonia, NaOH, KOH, amines Temperature- RT, Hydrothermal, autoclave, microwave Homogeneous precipitation- urea, hexamine Thermal decomposition of Iron compounds Iron salts – inorganic / organic Nitrate, carbonate, sulphate, perchlorate / oxalate, citrate, tartrate Iron complexes- Atmosphere - oxidizing, reducing, inert

6 Synthesis of Nano Iron oxide particles Combustion technique Vapour deposition Sol-Gel method Template method Homogeneous precipitation Powdering- ball milling, Fluid energy milling

7 Characterization techniques Elemental analysis CHNS Analyser UV-Visible Spectrophotometry Ion Chromatography (IC) Atomic Absorption Spectrometry (AAS) Inductively Coupled Plasma Atomic Emission Spectrometry (ICPAES) X-ray Fluorescence Spectrometry (XRF) Structural Analysis Fourier Transform Infra Red Spectrometry (FTIR) X-ray Diffraction Spectrometry (XRD) Particle Characterization Surface area analyser Particle Size analysis by light scattering Scanning Electron Microscope (SEM) Transmission Electron Microscope (TEM) Atomic Force Microscope (AFM) Thermal Analysis Thermogravimetric Analyser (TGA) Differential Thermal Analyser (DTA) Differential Scanning Calorimeter (DSC)

8 X-ray Diffraction Spectrometer (XRD) Nano ferric oxide by sucrose method ColourPatternCompound NameFormula PDF Ferric OxideFe2O3

9 ColourPatternCompound NameFormula PDF Ammonium Copper Chromium Oxide Hydroxide NH4 CuCrO4(OH) PDF Ammonium Copper Ammine Chromium Oxide (NH4)2Cu4(NH3)3Cr5O20 Copper Ammonium Chromate

10 ColourPatternCompound NameFormula PDF Copper Hydrogen Chromium Oxide Cu0.41 Cu0.24 H1.1 Cr2O4 PDF Tenorite, synCuO PDF Copper Chromium OxidCuCr2O4 Copper chromite

11 Atomic Absorption Spectrophotometry (AAS) Specifications Source : hollow cathode lamp Flame : air/C2H2, N2O/C2H2 Range : 0.1 ppm to 5% Detector : PM tube Sensitivity : 0.01 ppm Sample : aqueous/ non aqueous solutions Principle is Beer-Lambert’s law: log I 0 /I = εcl Measurement of radiation, absorbed by the ground state atoms at specific resonance wavelength, from a hollow cathode lamp Extent of absorption is directly proportional to the number of ground state atoms in the flame, measured by a spectrophotometer 11

12 Ion Chromatograph Principle Ion exchange, retention and elution Applications Anions and cations from ppm to percentage levels

13 Thermogravimetric Analyser (TG) and Differential Thermal Analyser (DTA) Components Balance assemblies Furnace Cabinet Software Temperature Range: Ambient to 1500°C Heating Rate : 0.1°C/min to100°C/min Accuracy :  1% Balance sensitivity : 0.1  g DTA sensitivity : °C

14 TG /DTG and DTA of FeSO 4.7H 2 0

15 TG /DTG of Fe(NH 4 ) 2.(SO 4 ) 2.6H 2 0 – Mohrs. salt

16 TG /DTG of FeNH 4.(SO 4 ) 2.12H 2 0 – Ferric alum

17 Differential Scanning Calorimeter (DSC) Temperature Range: -150°C to 725°C Heating Rate : 0.1°C/min to 100°C/min Calorimetric Precision : 1 %



20 UV-Visible Spectrophotometer Specifications Range : nm Resolution : 1 nm Principle Beer-Lambert law A = log I 0 /I = εcL  UV -Visible spectroscopy involves the absorption of UV or visible light by a molecule causing the promotion of an electron from a ground electronic state to an excited electronic state Applications Estimation of trace level impurities in alloys Estimation of titanium, Iridium in alloys and catalysts Absorption studies of Quantum dots, dyes Fe in Al powder Ammonium dinitramide analysis 20

21 UV-visible spectra of metal complexes λ max of NiCl nm, λ max of NiOA is below 650 nm λ max of CuCl nm, λ max of CuOA is 650 nm

22 Analysis of Titanium by UV-visible Spectrophotometer In acid medium Titanium ions give an yellow orange complex with H 2 O 2 which forms the basis of spectrometric method for determination of Titanium. The interference from other elements can be eliminated by the addition of citric acid / tartaric acid UV-Visible Spectrophotometer max = 410nm, Band width = 0.5nm Quartz cell with optical path length 10mm slope Calibration graph for Titanium Absorbance Concentration of Titanium (mg/L)

23 Fourier Transform Infra red Spectrometer Wavelength range : cm -1 Sa Samples in KBr pellets used for measuring spectrum

24 FTIR spectra of OA and CuOA complexes 3300 cm -1 – broadened due to metal oleyl amine complexes 2854 and 2922 cm -1 Oleyl group

25 Topics for Projects Studies on water crystallization of compounds Sulphate, Double sulphates, alums Nitrates, chlorides, complexes Preparation of crystals TG, DTA studies, XRD, IR Catalytic activity studies Ammonium perchlorate, ammonium nitrate, potassium nitrate, potassium chlorate Catalysts: Metal oxides, mixed metal oxides Preparation and characterization TG, DTA, DSC, particle size, surface area, XRD, IR, SEM, TEM

26 Topics for Projects Pollution control studies Removal of major contaminants -acid, base, sulphate, nitrate, perchlorate, fluoride, iron, etc -Addition of suitable neutralizing /precipitating agents, separation -analysis Removal of minor and trace contaminants -As, Hg, Cr, Fe, Ni, Fluoride, perchlorate, etc -Adsorption, Ion exchange, chromatography, solvent extraction, precipitation, evaporation, volatilization Regeneration, analysis Type of additives / by products Natural, synthetic reagents, corrosive, ecofriendly

27 Topics for Projects Analytical Chemistry Projects Estimation of iron content in soil from different area by spectrophotometry Analysis of Titanium content in beach sand by spectrophotometry Quantitative composition analysis of alloys eg. Chromium / Nickel content in Stainless steel (gravimetry, volumetry, colorimetry, AAS, ICP-AES)

28 Advanced Projects Mars atmosphere contains >95% CO 2 and also as dry ice in soil Technologies are required for producing oxygen from this CO 2 and from iron oxide Splitting of water to hydrogen and oxygen by low cost / energy method Storage of hydrogen

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