Student Projects for B.Sc. Chemistry
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Transcript of Student Projects for B.Sc. Chemistry
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Student Projects for B.Sc. Chemistry
Dr. R. RajeevVSSC, Thiruvananthapuram
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Project
• Introduction Relevance Applications Literature survey• Scope of work• Experimental Procedure• Materials• Instrumentation for experiments and characterization• Results & Discussion• Conclusions• Acknowledgements• References
Feasibility
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Where to find a topic / subject• Inorganic Chemistry Synthesis of metal oxides• Applications metallurgy, catalysts, fillers in composites, ceramics, pigments,
paints• PropertiesInertness, catalytic activity, stability, purity, colourThermal , electrical , magnetic and spectral propertiesParticle characteristics like size (macro, micro, nano), shape,
surface area, porosity• Properties varies with method of preparation, heat
treatment, precursor
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Iron oxide• Oxides of Iron• iron(II) oxide, wüstite (FeO)• iron(II,III) oxide, magnetite (Fe3O4)• iron(III) oxide (Fe2O3)
– alpha phase, hematite (α-Fe2O3) beta phase, (β-Fe2O3)– gamma phase, maghemite (γ-Fe2O3)– epsilon phase, (ε-Fe2O3)
• Hydroxides• iron(II) hydroxide (Fe(OH)2)• iron(III) hydroxide (Fe(OH)3), (bernalite)• Oxide/hydroxides• goethite (α-FeOOH),• akaganéite (β-FeOOH),• lepidocrocite (γ-FeOOH),• feroxyhyte (δ-FeOOH),• ferrihydrite (Fe5HO8·4H2O approx.), or 5Fe2O3•9H2O, better recast as FeOOH•0.4H2O• high-pressure FeOOH• schwertmannite (ideally Fe8O8(OH)6(SO)·nH2O or Fe3+
16O16(OH,SO4)12-13·10-12H2O)• green rust (FeIII
xFeIIy(OH)3x+2y-z(A-)z; where A- is Cl- or 0.5SO4
2-)
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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
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Synthesis of Nano Iron oxide particles
• Combustion technique• Vapour deposition• Sol-Gel method• Template method• Homogeneous precipitation• Powdering- ball milling, Fluid energy milling
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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)
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X-ray Diffraction Spectrometer (XRD)
Nano ferric oxide by sucrose method
Colour Pattern Compound Name FormulaPDF 04-006-6579
Ferric Oxide Fe2O3
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Colour Pattern Compound Name Formula
PDF 00-005-0151 Ammonium Copper Chromium Oxide Hydroxide
NH4 CuCrO4(OH)
PDF 00-041-0625 Ammonium Copper Ammine Chromium Oxide
(NH4)2Cu4(NH3)3Cr5O20
Copper Ammonium Chromate
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Colour Pattern Compound Name Formula
PDF 01-080-8761 Copper Hydrogen Chromium Oxide
Cu0.41 Cu0.24 H1.1 Cr2O4
PDF 00-048-1548 Tenorite, syn CuO
PDF 00-021-0874 Copper Chromium Oxid CuCr2O4
Copper chromite
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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 I0/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
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Ion Chromatograph
PrincipleIon exchange , retention and elution
ApplicationsAnions and cations from ppm to percentage
levels
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Thermogravimetric Analyser (TG) and Differential Thermal Analyser (DTA)
ComponentsBalance assemblies
FurnaceCabinet
Software
Temperature Range: Ambient to 1500°CHeating Rate : 0.1°C/min to100°C/minAccuracy : 1%Balance sensitivity : 0.1gDTA sensitivity : 0. 001°C
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TG /DTG and DTA of FeSO4.7H20
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TG /DTG of Fe(NH4)2.(SO4)2.6H20 – Mohrs. salt
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TG /DTG of FeNH4.(SO4)2.12H20 – Ferric alum
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Differential Scanning Calorimeter (DSC)
Temperature Range: -150°C to 725°CHeating Rate : 0.1°C/min to 100°C/minCalorimetric Precision : 1 %
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UV-Visible Spectrophotometer
SpecificationsRange : 190-900nm Resolution : 1 nm
Principle
Beer-Lambert law
A = log I0/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
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UV-visible spectra of metal complexes
λmax of NiCl2 760 nm, λmax of NiOA is below 650 nm
λmax of CuCl2 754 nm, λmax of CuOA is 650 nm
400 450 500 550
0
1
2
3
Ferric chloride
ferric chloride- Oleyl amine complex
Abso
rban
ce
Wavelength, nm
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Analysis of Titanium by UV-visible Spectrophotometer•In acid medium Titanium ions give an yellow orange
complex with H2O2 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 Spectrophotometermax = 410nm, Band width = 0.5nmQuartz cell with optical path length 10mm
0 5 10 15 20
0.00
0.05
0.10
0.15
0.20
0.25
0.30
0.35
slope 0.01591
Calibration graph for Titanium
Abs
orba
nce
Concentration of Titanium (mg/L)400 450 500 550
0
1
2
3
T-H2O2 complex
Abs
orba
nce
Wavelength, nm
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Fourier Transform Infra red Spectrometer
Wavelength range : 400 - 4000 cm-1 Sa Samples in KBr pellets used for measuring spectrum
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FTIR spectra of OA and CuOA complexes
3300 cm-1 – broadened due to metal oleyl amine complexes
2854 and 2922 cm-1 Oleyl group
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Topics for ProjectsStudies on water crystallization of compoundsSulphate, Double sulphates, alumsNitrates, chlorides, complexesPreparation of crystalsTG, DTA studies, XRD, IR
Catalytic activity studiesAmmonium perchlorate, ammonium nitrate, potassium nitrate, potassium chlorate
Catalysts: Metal oxides, mixed metal oxidesPreparation and characterizationTG, DTA, DSC, particle size, surface area, XRD, IR, SEM, TEM
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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-analysisRemoval of minor and trace contaminants -As, Hg, Cr, Fe, Ni, Fluoride, perchlorate, etc-Adsorption, Ion exchange, chromatography, solvent extraction, precipitation, evaporation, volatilization Regeneration, analysisType of additives / by productsNatural, synthetic reagents, corrosive, ecofriendly
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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)
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Advanced Projects
Mars atmosphere contains >95% CO2 and also as dry ice in soilTechnologies are required for producing oxygen from this CO2 and from iron oxide
Splitting of water to hydrogen and oxygen by low cost / energy methodStorage of hydrogen