CH4220 : Advanced Chemistry Laboratory (Spring 2023) | Academic Portal of IISER Kolkata

Details of CH4220 (Spring 2023)

Level: 4

Type: Laboratory

Credits: 4.0

Course Code	Course Name	Instructor(s)
CH4220	Advanced Chemistry Laboratory	Alakesh Bisai, Biplab Maji, Chilla Malla Reddy

Preamble
This laboratory course will focus on advanced level experiments to showcase the applications of various branches of Chemistry that are discovered in the last 1-2 decade/s or so. Students will get the flavour of interdisciplinary aspects of Chemistry, and thus it will help them in choosing their future research based on their interests.

Syllabus
Expt. No. 1 Designing Small Molecules for Enzymatic Studies: Photophysical Studies and DFT Calculations Aim & Objective: Chemidosimetric Probes for Luminescence Response by Hydrolysis of the Phosphoester linkage by Alkaline Phosphatase (ALP) in Living Cells Sub-Objective 1: 2 Weeks (4 days & 2 h each day) Synthesis and Characterization of Chemidosimetric Probe (i) Coupling of 3-(N,N-diethyl)amino phenol with active methylene compound (ii) Synthesis of Chemidosimetric Probe having phosphate linkage (iii) Analysis of results and preparation of reports Sub-Objective 2: 1 Week (2 days & 2 h each day) Photophysical Studies (i) UV-VIS Spectroscopy of Chemidosimetric Probe (ii) Fluorescence Spectroscopy of Chemidosimetric Probe with and without phosphate group (iii) Analysis of results and preparation of reports Sub-Objective 3: 1 Week (2 days & 2 h each day) (i) Studies of Enzymatic Kinetics of Chemidosimetric Probe having phosphate linkage (ii) Analysis of results and preparation of reports Sub-Objective 4: 1 Week (2 days & 2 h each day) (i) Life-Cell Imaging Studies using Chemidosimetric Probe having phosphate linkage (ii) Analysis of results and preparation of reports Sub-Objective 5: 1 Week (2 days & 2 h each day) (i) Theoretical and Computational understanding of the behaviours of Chemidosimetric Probe (ii) Analysis of results and preparation of reports Summary Quiz, Assignments, Lab. Report submission ---------------------------------------------------------------------------------------------------------------- Expt. No. 2 Perovskite Solar Cell/Dye-Sensitive Solar Cell for Energy Application: Detailed Studies with Theoretical Aspects Aim & Objective: Application of Hybrid Perovskites and Organic Dyes in Photovoltaics, Optoelectronics, and Photoelectrocatalysis Sub-Objective 1: 1 Week (2 days & 2 h each day) 1. Fabrication of n-i-p type photovoltaic devices with bulk CH3NH3PbI3-xClx (synthesis of the perovskite, TiO2 coated FTO substrate, Spin Coating, Thermal deposition) 2. Current-Voltage measurements, Electrochemical Impedance Spectroscopy 3. Data plotting - Open-circuit voltage, short-circuit current, fill factor, power conversion efficiency, series resistance and charge transfer resistance Sub-Objective 2: 1 Week (2 days & 2 h each day) 1. Preparation of thin films of HTMs (Spiro-MeOTAD and PEDOT: PSS) on the Electrode 2. Cyclic-Voltammetry (CV) and Absorption Spectroscopy of the Hole Transport Materials 3. Evaluation of frontier molecular orbital energy levels from CV and absorption spectroscopy Sub-Objective 3: 1 Week (2 days & 2 h each day) 1. Introduction to Dye-Sensitized Solar Cells (DSSC), FETs, LEDs 2. Fabrication of an Organic Field Effect Transistor 3. Methods of electrical characterisation and analysis of the performance Sub-Objective 4: 1 Week (2 days & 2 h each day) 1. Introduction to Photocatalysis and Photoelectrocatalysis 2. The developed Perovskite will be evaluated for their Photocatalysis Performance 3. Efficiency of the Materials towards Photocatalysis will be calculated Sub-Objective 5: 1 Week (2 days & 2 h each day) 1. Basic theory behind ab initio calculations, many-electron Hamiltonian, Born Oppenheimer approximation, Hartree-Fock Assumption, Concepts of Basis Sets, DFT 2. Application of many-electron Hamiltonian for electronic structure calculations of molecules and band structure of solids 3. The role of singlet and triplet low-lying excited states in molecules and materials in OLEDs and solar cell applications Summary Quiz, Assignments, Lab. Report submission ---------------------------------------------------------------------------------------------------------------- Expt. No. 3 Polymer Drug Conjugates: Synthesis, Characterization, and Biological Applications Aim & Objective: Synthesis and Characterization of a Block Copolymer for Drug Encapsulation, Release and Biological Evaluations Sub-Objective 1: 2 Weeks (4 days & 2 h each day) Polymer synthesis and characterization 1. Introduction to living/Controlled Polymerization 2. Controlled synthesis of poly(methyl methacrylate) homopolymer 3. Controlled synthesis of block copolymer Sub-Objective 2: 1 Week (2 days & 2 h each day) Polymer Characterization 1. Characterization of Polymers by 1H NMR spectroscopy 2. Determination of Molecular Weights and Molecular Weight distributions by Size Exclusion Chromatography 3. Study micelle formation by fluorescence spectroscopy Sub-Objective 3: 1 Week (2 days & 2 h each day) Drug release study 1. Physical encapsulation of DOX drug in the polymer aggregate 2. Characterization of drug loading 3. Study drug release behavior Sub-Objective 4: 2 Weeks (4 days & 2 h each day) Measuring cytotoxicity and cellular uptake of the synthesized block copolymer 1. Carry out MTT based cytotoxicity assay 2. Study Cellular Uptake Assay 3. Analysis and Preparation of the Report Summary Quiz, Assignments, Lab. Report submission ---------------------------------------------------------------------------------------------------------------- Expt. No. 4 Controlling Properties of Pharmaceutical Solid Drugs: Synthesis, Crystallization, Polymorphs, Co-Crystals and Computation Aim & Objective: Controlling Properties of Paracetamol: Synthesis, Crystallization, Polymorphs, Co-Crystals and Computation Sub-Objective 1: 1 Week (2 days & 2 h each day) 1. Introduction to synthesis, crystallization, concepts of crystal engineering & synthons 2. Preparation of polymorphs, cocrystals 3. Characterization of the solid drugs by PXRD, IR, DSC, TGA, etc. 4. Preparation of reports and use of different crystallography Softwares/tools Sub-Objective 2: 1 Week (2 days & 2 h each day) 1. Introduction to the drug, paracetamol 2. Synthetic procedures and methods for preparing Paracetamol in gram scale quantity 3. Separation and purification of the drug 4. Characterization of the drug by TLC, NMR and other techniques Sub-Objective 3: 1 Week (2 days & 2 h each day) 1. Introduction to Computational tools to study Crystal Structures 2. Optimization of Crystal Structures and Lattice Energy Calculations 3. Methods to Calculate Lattice Energies 4. Analysis and Preparation of reports Sub-Objective 4: 2 Weeks (4 days & 2 h each day) Crystallization and Characterization 1. Crystallization of different Polymorphs, co-crystals of the drug 2. Characterization of different solids forms prepared 3. Analysis and preparation of the report Sub-Objective 6: 1 Week (2 days & 2 h each day) Computational Work 1. Computational work to optimize crystal structure, calculate Lattice Energies of Polymorphs using reported crystal structures from database 2. Analysis of results and preparation of reports Summary Quiz, Assignments, Lab. Report submission ---------------------------------------------------------------------------------------------------------------- Expt. No. 5. Asymmetric Catalysis using Organometallic Complexes for the Synthesis of Value Added Small Organic Molecules Aim & Objective: Enantioselective Alkenylations of Imines Catalyzed by Cu(I)-PyBOX Complexes'. Sub-Objective 1: 2 Weeks (4 days & 2 h each day) Synthesis of Pybox ligand from L-Phenylglycine (i) Coupling of amino alcohol with 2,6-pyridine dicarboxylic acid (iii) Condensation reaction to get (S,S)-Ph-PYBOX ligand (iv) Analysis of results and preparation of reports Sub-Objective 2: 1 Week (2 days & 2 h each day) Complexation with Cu(I) and Cu(II)-complexes (i) Cu(I)-(S,S)-Ph-PYBOX complexes (iii) EPR-studies of Cu(I)-(S,S)-Ph-PYBOX complexes (iv) Analysis of results and preparation of reports Sub-Objective 3: 2 Weeks (4 days & 2 h each day) Optimization of Catalytic Alkynylation Reactions (i) Asymmetric alkylation using terminal alkynes (from a step) (ii) HPLC run of Racemic sample and Enantioenriched sample and specific rotation (iii) Analysis of results and preparation of reports Sub-Objective 4: 1 Week (2 days & 2 h each day) Derivatization of alkynylation products (i) Catalytic hydrogenation of tripple bond of alkynyl amines (ii) Analysis of results and preparation of reports Summary Quiz, Assignments, Lab. Report submission ----------------------------------------------------------------------------------------------------------------

Syllabus

Expt. No. 1
Designing Small Molecules for Enzymatic Studies: Photophysical Studies and DFT Calculations

Aim & Objective:
Chemidosimetric Probes for Luminescence Response by Hydrolysis of the Phosphoester linkage by Alkaline Phosphatase (ALP) in Living Cells

Sub-Objective 1: 2 Weeks (4 days & 2 h each day)
Synthesis and Characterization of Chemidosimetric Probe
(i) Coupling of 3-(N,N-diethyl)amino phenol with active methylene compound
(ii) Synthesis of Chemidosimetric Probe having phosphate linkage
(iii) Analysis of results and preparation of reports

Sub-Objective 2: 1 Week (2 days & 2 h each day)
Photophysical Studies
(i) UV-VIS Spectroscopy of Chemidosimetric Probe
(ii) Fluorescence Spectroscopy of Chemidosimetric Probe with and without phosphate group
(iii) Analysis of results and preparation of reports

Sub-Objective 3: 1 Week (2 days & 2 h each day)
(i) Studies of Enzymatic Kinetics of Chemidosimetric Probe having phosphate linkage
(ii) Analysis of results and preparation of reports

Sub-Objective 4: 1 Week (2 days & 2 h each day)
(i) Life-Cell Imaging Studies using Chemidosimetric Probe having phosphate linkage
(ii) Analysis of results and preparation of reports

Sub-Objective 5: 1 Week (2 days & 2 h each day)
(i) Theoretical and Computational understanding of the behaviours of Chemidosimetric Probe
(ii) Analysis of results and preparation of reports

Summary
Quiz, Assignments, Lab. Report submission
----------------------------------------------------------------------------------------------------------------

Expt. No. 2
Perovskite Solar Cell/Dye-Sensitive Solar Cell for Energy Application: Detailed Studies with Theoretical Aspects

Aim & Objective:
Application of Hybrid Perovskites and Organic Dyes in Photovoltaics, Optoelectronics, and Photoelectrocatalysis

Sub-Objective 1: 1 Week (2 days & 2 h each day)
1. Fabrication of n-i-p type photovoltaic devices with bulk CH3NH3PbI3-xClx (synthesis of the perovskite, TiO2 coated FTO substrate, Spin Coating, Thermal deposition)
2. Current-Voltage measurements, Electrochemical Impedance Spectroscopy
3. Data plotting - Open-circuit voltage, short-circuit current, fill factor, power conversion efficiency, series resistance and charge transfer resistance

Sub-Objective 2: 1 Week (2 days & 2 h each day)
1. Preparation of thin films of HTMs (Spiro-MeOTAD and PEDOT: PSS) on the Electrode
2. Cyclic-Voltammetry (CV) and Absorption Spectroscopy of the Hole Transport Materials
3. Evaluation of frontier molecular orbital energy levels from CV and absorption spectroscopy

Sub-Objective 3: 1 Week (2 days & 2 h each day)
1. Introduction to Dye-Sensitized Solar Cells (DSSC), FETs, LEDs
2. Fabrication of an Organic Field Effect Transistor
3. Methods of electrical characterisation and analysis of the performance

Sub-Objective 4: 1 Week (2 days & 2 h each day)
1. Introduction to Photocatalysis and Photoelectrocatalysis
2. The developed Perovskite will be evaluated for their Photocatalysis Performance
3. Efficiency of the Materials towards Photocatalysis will be calculated

Sub-Objective 5: 1 Week (2 days & 2 h each day)
1. Basic theory behind ab initio calculations, many-electron Hamiltonian, Born Oppenheimer approximation, Hartree-Fock Assumption, Concepts of Basis Sets, DFT
2. Application of many-electron Hamiltonian for electronic structure calculations of molecules and band structure of solids
3. The role of singlet and triplet low-lying excited states in molecules and materials in OLEDs and solar cell applications

Summary
Quiz, Assignments, Lab. Report submission
----------------------------------------------------------------------------------------------------------------

Expt. No. 3
Polymer Drug Conjugates: Synthesis, Characterization, and Biological Applications

Aim & Objective:
Synthesis and Characterization of a Block Copolymer for Drug Encapsulation, Release and Biological Evaluations

Sub-Objective 1: 2 Weeks (4 days & 2 h each day)
Polymer synthesis and characterization
1. Introduction to living/Controlled Polymerization
2. Controlled synthesis of poly(methyl methacrylate) homopolymer
3. Controlled synthesis of block copolymer

Sub-Objective 2: 1 Week (2 days & 2 h each day)
Polymer Characterization
1. Characterization of Polymers by 1H NMR spectroscopy
2. Determination of Molecular Weights and Molecular Weight distributions by Size Exclusion Chromatography
3. Study micelle formation by fluorescence spectroscopy

Sub-Objective 3: 1 Week (2 days & 2 h each day)
Drug release study
1. Physical encapsulation of DOX drug in the polymer aggregate
2. Characterization of drug loading
3. Study drug release behavior

Sub-Objective 4: 2 Weeks (4 days & 2 h each day)
Measuring cytotoxicity and cellular uptake of the synthesized block copolymer
1. Carry out MTT based cytotoxicity assay
2. Study Cellular Uptake Assay
3. Analysis and Preparation of the Report

Summary
Quiz, Assignments, Lab. Report submission
----------------------------------------------------------------------------------------------------------------

Expt. No. 4
Controlling Properties of Pharmaceutical Solid Drugs: Synthesis, Crystallization, Polymorphs, Co-Crystals and Computation

Aim & Objective:
Controlling Properties of Paracetamol: Synthesis, Crystallization, Polymorphs, Co-Crystals and Computation

Sub-Objective 1: 1 Week (2 days & 2 h each day)
1. Introduction to synthesis, crystallization, concepts of crystal engineering & synthons
2. Preparation of polymorphs, cocrystals
3. Characterization of the solid drugs by PXRD, IR, DSC, TGA, etc.
4. Preparation of reports and use of different crystallography Softwares/tools

Sub-Objective 2: 1 Week (2 days & 2 h each day)
1. Introduction to the drug, paracetamol
2. Synthetic procedures and methods for preparing Paracetamol in gram scale quantity
3. Separation and purification of the drug
4. Characterization of the drug by TLC, NMR and other techniques

Sub-Objective 3: 1 Week (2 days & 2 h each day)
1. Introduction to Computational tools to study Crystal Structures
2. Optimization of Crystal Structures and Lattice Energy Calculations
3. Methods to Calculate Lattice Energies
4. Analysis and Preparation of reports

Sub-Objective 4: 2 Weeks (4 days & 2 h each day)
Crystallization and Characterization
1. Crystallization of different Polymorphs, co-crystals of the drug
2. Characterization of different solids forms prepared
3. Analysis and preparation of the report

Sub-Objective 6: 1 Week (2 days & 2 h each day)
Computational Work
1. Computational work to optimize crystal structure, calculate Lattice Energies of Polymorphs using reported crystal structures from database
2. Analysis of results and preparation of reports

Summary
Quiz, Assignments, Lab. Report submission
----------------------------------------------------------------------------------------------------------------

Expt. No. 5.
Asymmetric Catalysis using Organometallic Complexes for the Synthesis of Value Added Small Organic Molecules

Aim & Objective:
Enantioselective Alkenylations of Imines Catalyzed by Cu(I)-PyBOX Complexes'.

Sub-Objective 1: 2 Weeks (4 days & 2 h each day)
Synthesis of Pybox ligand from L-Phenylglycine
(i) Coupling of amino alcohol with 2,6-pyridine dicarboxylic acid
(iii) Condensation reaction to get (S,S)-Ph-PYBOX ligand
(iv) Analysis of results and preparation of reports

Sub-Objective 2: 1 Week (2 days & 2 h each day)
Complexation with Cu(I) and Cu(II)-complexes
(i) Cu(I)-(S,S)-Ph-PYBOX complexes
(iii) EPR-studies of Cu(I)-(S,S)-Ph-PYBOX complexes
(iv) Analysis of results and preparation of reports

Sub-Objective 3: 2 Weeks (4 days & 2 h each day)
Optimization of Catalytic Alkynylation Reactions
(i) Asymmetric alkylation using terminal alkynes (from a step)
(ii) HPLC run of Racemic sample and Enantioenriched sample and specific rotation
(iii) Analysis of results and preparation of reports

Sub-Objective 4: 1 Week (2 days & 2 h each day)
Derivatization of alkynylation products
(i) Catalytic hydrogenation of tripple bond of alkynyl amines
(ii) Analysis of results and preparation of reports

Summary
Quiz, Assignments, Lab. Report submission
----------------------------------------------------------------------------------------------------------------

References

Course Credit Options

Sl. No.	Programme	Semester No	Course Choice
1	IP	2	Not Allowed
2	IP	4	Elective
3	IP	6	Not Allowed
4	MP	2	Core
5	MP	4	Not Allowed
6	MR	2	Not Allowed
7	MR	4	Not Allowed
8	MS	10	Not Allowed
9	MS	4	Not Allowed
10	MS	6	Not Allowed
11	MS	8	Not Allowed
12	RS	1	Not Allowed
13	RS	2	Not Allowed

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Details of CH4220 (Spring 2023)

Course Credit Options