Prelab Lecture Notes • Summer 2009
Lab 1-Unknowns
Main topics include:
• Goals and Objectives
• IR function
• Calculating IHD
• Calculating MF from Elemental Analysis
• Measuring boiling points
• Measuring melting points
Main topics include:
• Goals and Objectives
• IR function
• Calculating IHD
• Calculating MF from Elemental Analysis
• Measuring boiling points
• Measuring melting points
IR Primer
Main topics include:
• Functional groups
• Bonding
• Valence electrons
• Electronegativity
• Dipole moment
• Infrared Spectroscopy principles
• Sample IR spectra
Main topics include:
• Functional groups
• Bonding
• Valence electrons
• Electronegativity
• Dipole moment
• Infrared Spectroscopy principles
• Sample IR spectra
The
following lecture notes are presented by each
teaching assistant before the laboratory period.
These notes may be a source of additional
information, but are not intended to replace the
required readings in the textbook or course manual.
Click the images on the left for pdf versions of
these notes.
Lab 2-Chromatography
Main topics include:
• Goals and Objectives
• Definitions and Principles
• Partition Coefficient (Kc)
• Types of Chromatography
• Mobile Phases & Properties
• Stationary Phases & Properties
• Polarity & Elutropic Series
• Column and Thin-Layer Chrom.
• Stereoisomers
Main topics include:
• Goals and Objectives
• Definitions and Principles
• Partition Coefficient (Kc)
• Types of Chromatography
• Mobile Phases & Properties
• Stationary Phases & Properties
• Polarity & Elutropic Series
• Column and Thin-Layer Chrom.
• Stereoisomers
Lab 3-Simple Distillation and GLC
Analysis
Main topics include:
• Simple dist. applications and goals
• Boiling Point & Equilib. Vapor Press.
• Distillation apparatus
• Dalton's Law, Raoult's Law
• Distillate volume v. temp graph
• GLC principles
• Analysis of GLC graph, % composition
• GLC Equipment, Packed Column
Main topics include:
• Simple dist. applications and goals
• Boiling Point & Equilib. Vapor Press.
• Distillation apparatus
• Dalton's Law, Raoult's Law
• Distillate volume v. temp graph
• GLC principles
• Analysis of GLC graph, % composition
• GLC Equipment, Packed Column
Lab 4-Fractional Distillation and GLC
Analysis
Main topics include:
• Frxnl dist. applications and goals
• Frxnl distillation apparatus
• Temp. gradient and fractionation
• Temp-Comp Diagram
• Theoretical Plates/HETP
• Comparison V vs. T graphs
Main topics include:
• Frxnl dist. applications and goals
• Frxnl distillation apparatus
• Temp. gradient and fractionation
• Temp-Comp Diagram
• Theoretical Plates/HETP
• Comparison V vs. T graphs
Lab 5-Steam Distillation of Carvone from Caraway
Seeds/IR
Main topics include:
• Applications/goals
• Advantages & requirements
• Apparatus and setup
• Principles: Raoult's law; Dalton's law
• Principles: graphical.
• Extraction procedure notes
• Analysis: IR, TLC, smell
• Comparison to carvone IRs
Main topics include:
• Applications/goals
• Advantages & requirements
• Apparatus and setup
• Principles: Raoult's law; Dalton's law
• Principles: graphical.
• Extraction procedure notes
• Analysis: IR, TLC, smell
• Comparison to carvone IRs
Lab 6-Separation of Benzoic Acid & Acetanilide
by Base Extraction
Main topics include:
• Applications/goals, mps
• Base extraction process/scheme
• Ionizable functional groups
• Solubility: water vs. organic
• Determining Keq (acid-base rxn)
• Number of extractions & efficiency
• Requirements for extraction solvent
• Requirements for recrystallization
Main topics include:
• Applications/goals, mps
• Base extraction process/scheme
• Ionizable functional groups
• Solubility: water vs. organic
• Determining Keq (acid-base rxn)
• Number of extractions & efficiency
• Requirements for extraction solvent
• Requirements for recrystallization
Lab 8-Hydration of a Terminal
Alkyne.
Main topics include:
• Safety concerns
• Procedure Notes/Modifications
• Steam distillation apparatus
• Regioselectivity of hydration
• Roles of Hg2+ in hydration mech.
• Semicarbazone derivatization
• Semicarbazide mechanism
• Recrystallization
Main topics include:
• Safety concerns
• Procedure Notes/Modifications
• Steam distillation apparatus
• Regioselectivity of hydration
• Roles of Hg2+ in hydration mech.
• Semicarbazone derivatization
• Semicarbazide mechanism
• Recrystallization
Lab 7-Preparation of Alkyl Chlorides by
Nucleophilic Subst.
Main topics include:
• Goals; Data Collection Table
• Procedure Notes/Modifications
• Bicarbonate Warning
• SN1 vs. SN2
• AgNO3 test for alkyl chlorides
• NaI test for alkyl chlorides
• E1 competes with SN1
Main topics include:
• Goals; Data Collection Table
• Procedure Notes/Modifications
• Bicarbonate Warning
• SN1 vs. SN2
• AgNO3 test for alkyl chlorides
• NaI test for alkyl chlorides
• E1 competes with SN1
Lab 9-CASPiE: Diazo Coupling
Main topics include:
• Overview
• EDA safety
• Tasks to complete
• Reaction table
Main topics include:
• Overview
• EDA safety
• Tasks to complete
• Reaction table
Lab 10-CASPiE: Hydrogenation
Main topics include:
• Safety
• 1H-NMR analysis of last week's product
• Ni-catalyzed hydrogenation: ethyl 3-octynoate or 3-hexyn-1-ol
• Reaction table calculations
• Cis and Trans alkene J-values
• Calculating J-values
• Results from previous semesters
Main topics include:
• Safety
• 1H-NMR analysis of last week's product
• Ni-catalyzed hydrogenation: ethyl 3-octynoate or 3-hexyn-1-ol
• Reaction table calculations
• Cis and Trans alkene J-values
• Calculating J-values
• Results from previous semesters