Guides
- Page ID
- 478294
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\(\newcommand{\avec}{\mathbf a}\) \(\newcommand{\bvec}{\mathbf b}\) \(\newcommand{\cvec}{\mathbf c}\) \(\newcommand{\dvec}{\mathbf d}\) \(\newcommand{\dtil}{\widetilde{\mathbf d}}\) \(\newcommand{\evec}{\mathbf e}\) \(\newcommand{\fvec}{\mathbf f}\) \(\newcommand{\nvec}{\mathbf n}\) \(\newcommand{\pvec}{\mathbf p}\) \(\newcommand{\qvec}{\mathbf q}\) \(\newcommand{\svec}{\mathbf s}\) \(\newcommand{\tvec}{\mathbf t}\) \(\newcommand{\uvec}{\mathbf u}\) \(\newcommand{\vvec}{\mathbf v}\) \(\newcommand{\wvec}{\mathbf w}\) \(\newcommand{\xvec}{\mathbf x}\) \(\newcommand{\yvec}{\mathbf y}\) \(\newcommand{\zvec}{\mathbf z}\) \(\newcommand{\rvec}{\mathbf r}\) \(\newcommand{\mvec}{\mathbf m}\) \(\newcommand{\zerovec}{\mathbf 0}\) \(\newcommand{\onevec}{\mathbf 1}\) \(\newcommand{\real}{\mathbb R}\) \(\newcommand{\twovec}[2]{\left[\begin{array}{r}#1 \\ #2 \end{array}\right]}\) \(\newcommand{\ctwovec}[2]{\left[\begin{array}{c}#1 \\ #2 \end{array}\right]}\) \(\newcommand{\threevec}[3]{\left[\begin{array}{r}#1 \\ #2 \\ #3 \end{array}\right]}\) \(\newcommand{\cthreevec}[3]{\left[\begin{array}{c}#1 \\ #2 \\ #3 \end{array}\right]}\) \(\newcommand{\fourvec}[4]{\left[\begin{array}{r}#1 \\ #2 \\ #3 \\ #4 \end{array}\right]}\) \(\newcommand{\cfourvec}[4]{\left[\begin{array}{c}#1 \\ #2 \\ #3 \\ #4 \end{array}\right]}\) \(\newcommand{\fivevec}[5]{\left[\begin{array}{r}#1 \\ #2 \\ #3 \\ #4 \\ #5 \\ \end{array}\right]}\) \(\newcommand{\cfivevec}[5]{\left[\begin{array}{c}#1 \\ #2 \\ #3 \\ #4 \\ #5 \\ \end{array}\right]}\) \(\newcommand{\mattwo}[4]{\left[\begin{array}{rr}#1 \amp #2 \\ #3 \amp #4 \\ \end{array}\right]}\) \(\newcommand{\laspan}[1]{\text{Span}\{#1\}}\) \(\newcommand{\bcal}{\cal B}\) \(\newcommand{\ccal}{\cal C}\) \(\newcommand{\scal}{\cal S}\) \(\newcommand{\wcal}{\cal W}\) \(\newcommand{\ecal}{\cal E}\) \(\newcommand{\coords}[2]{\left\{#1\right\}_{#2}}\) \(\newcommand{\gray}[1]{\color{gray}{#1}}\) \(\newcommand{\lgray}[1]{\color{lightgray}{#1}}\) \(\newcommand{\rank}{\operatorname{rank}}\) \(\newcommand{\row}{\text{Row}}\) \(\newcommand{\col}{\text{Col}}\) \(\renewcommand{\row}{\text{Row}}\) \(\newcommand{\nul}{\text{Nul}}\) \(\newcommand{\var}{\text{Var}}\) \(\newcommand{\corr}{\text{corr}}\) \(\newcommand{\len}[1]{\left|#1\right|}\) \(\newcommand{\bbar}{\overline{\bvec}}\) \(\newcommand{\bhat}{\widehat{\bvec}}\) \(\newcommand{\bperp}{\bvec^\perp}\) \(\newcommand{\xhat}{\widehat{\xvec}}\) \(\newcommand{\vhat}{\widehat{\vvec}}\) \(\newcommand{\uhat}{\widehat{\uvec}}\) \(\newcommand{\what}{\widehat{\wvec}}\) \(\newcommand{\Sighat}{\widehat{\Sigma}}\) \(\newcommand{\lt}{<}\) \(\newcommand{\gt}{>}\) \(\newcommand{\amp}{&}\) \(\definecolor{fillinmathshade}{gray}{0.9}\)- 1: The Schlenk Line
- This page explains the purpose and use of the Schlenk line in inorganic chemistry. The Schlenk line is an essential laboratory apparatus used for handling air-sensitive chemicals by providing an inert atmosphere (usually nitrogen or argon) and a vacuum system. The guide covers the basic setup, operation, and safety procedures required to use the Schlenk line effectively. It also highlights various techniques for removing solvents, conducting reactions, and purging air-sensitive materials.
- 2: Cycling onto the Schlenk Line
- This page outlines the procedure for transferring air-sensitive materials into an inert atmosphere. The process involves evacuating the flask to remove air, followed by flushing with inert gas to create a controlled environment. This cycle is repeated several times to ensure the absence of oxygen and moisture, which is crucial for safe handling of sensitive reactions.
- 3: Performing Sensitive Reactions without a Schlenk Line
- This page discusses techniques for handling air-sensitive materials in less controlled environments. Key methods include using a glovebox, performing reactions in sealed vessels, or employing inert gas techniques. The importance of thorough preparation, including drying reagents and glassware, is emphasized. The guide also outlines safety precautions and monitoring for moisture and oxygen to protect sensitive compounds.
- 4: Transferring Liquids
- The guide on transferring liquids describes methods for safely moving air-sensitive liquids in a Schlenk line setup. It emphasizes using a syringe or cannula to avoid exposure to air and moisture. The process involves connecting the transfer apparatus to the source and receiving vessel, ensuring inert gas flow to maintain an oxygen-free environment. The guide also highlights the importance of pre-drying glassware and careful handling to prevent contamination.
- 5: Inert Atmosphere Filtrations
- This guide discusses the process of filtering air-sensitive solutions in an inert atmosphere. It emphasizes the importance of using a vacuum filtration setup and maintaining an inert gas flow to prevent contamination. The guide provides tips for choosing appropriate filter media and ensuring that all equipment is dry and free of moisture before use. Proper sealing and handling techniques are also highlighted to preserve the integrity of sensitive materials during the filtration process.
- 6: NMR Preparation
- The "NMR Preparation" section focuses on the procedures for preparing samples for Nuclear Magnetic Resonance (NMR) spectroscopy while maintaining an inert atmosphere. It covers techniques for handling air-sensitive materials, ensuring solvent removal, and the importance of using dry, clean NMR tubes. Proper sealing and transferring methods are highlighted to preserve sample integrity, which is essential for obtaining reliable NMR results.
- 7: Distillations
- This section provides an overview of distillation techniques for purifying solvents and separating compounds under reduced pressure to prevent decomposition. It describes two main methods: static vacuum distillation, where the system is evacuated and held at a constant pressure, and dynamic vacuum distillation, which involves continuous vaporization and condensation.
- 8: Freeze-Pump-Thaw
- The "Freeze-Pump-Thaw" method described on LibreTexts is a procedure used to remove dissolved gases from a solution in chemistry. It involves freezing the solution, reducing pressure via vacuum pumping, and allowing the substance to thaw, thereby releasing trapped gases. This cycle is repeated multiple times to ensure efficient gas removal. The technique is especially useful in sensitive experiments where gas contamination could affect results.
- 9: Drying Solvents
- This page explains methods for drying organic solvents, critical for Schlenk line chemistry. Traditional solvent stills use refluxing with desiccants, but pose safety risks. Modern labs use solvent purification systems, where solvents pass through columns to remove contaminants like water and oxygen. Activated molecular sieves can also be used for drying, and solvent dryness can be tested with the Karl Fischer method or ketyl radical tests.
- 10: Removing Solvent
- This page discusses removing solvents using a Schlenk line describes steps to safely evaporate solvents under vacuum without exposure to air. It emphasizes the need for careful handling to prevent bumping during evaporation, use of an external trap for large or reactive solvent volumes, and techniques to ensure all solvents are completely removed. The process involves controlling vacuum application, stirring the solution, and using liquid nitrogen traps to collect volatiles. The page also highli
- 11: Addition of Solids
- This page explains two primary methods for adding solids to a Schlenk flask: (1) for air- and moisture-stable solids, using a powder funnel under inert gas flow; (2) for more sensitive solids, using a solid addition tube under an inert gas environment. The latter method involves transferring the solid from a glovebox, attaching the tube to the Schlenk flask, and gently agitating to facilitate the addition of crystalline solids or salts.
- 12: Refluxing Under an Inert Atmosphere
- This page explains how to safely heat a reaction mixture while maintaining a protective gas layer, like nitrogen or argon, to prevent reactions with air or moisture. It covers setting up a reflux apparatus, using a Schlenk line, and managing flow rates of inert gas. Proper use of a condenser, the importance of monitoring pressure, and methods for sealing the system to avoid contamination are emphasized for maintaining a stable, inert environment during extended heating.
- 13: Gloveboxes
- Gloveboxes are sealed environments that facilitate handling sensitive or hazardous materials under an inert atmosphere, mainly used for air and moisture-sensitive solids. They allow for sample preparation and test-scale reactions, maintaining low levels of oxygen and moisture by using purified inert gases like nitrogen or argon. Items are cycled into the glovebox through antechambers, requiring vacuum/inert gas cycles for proper introduction.