An Accessible Mercury-Free Vacuum Schlenk Line for Air-Free Techniques

Linn, Donald E.

doi:10.1021/ed200734t

Cited by 5 publications

(4 citation statements)

References 12 publications

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“…Manual inert-and controlled-atmosphere chemistry has, on the other hand, developed largely in the past 50 years due to the increasing availability of technologies such as positive-pressure gloveboxes, Schlenk lines and solvent purification systems [16][17][18][19] . In tandem, the ability to investigate and exploit species that react readily under atmospheric conditions has expanded rapidly.…”

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confidence: 99%

Autonomous Execution of Highly Reactive Chemical Transformations in the Schlenkputer

Cronin,

Bell,

Boser

et al. 2023

Preprint

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We demonstrate how it is possible to design a modular programmable inert-atmosphere Schlenkputer (Schlenk-line-computer) for the synthesis and manipulation of the most highly reactive compounds including those which are air- and moisture sensitive or pyrophoric. To do this we have designed and built a programmable Schlenk Line using the Chemputer architecture for the inertization of glassware which can achieve a vacuum line pressure of 1.5 10^-3 mbar and integrated a range of automated Schlenk glassware for the handling, storage, and isolation of reactive compounds at sub ppm levels of O2 and H2O. Utilising this hardware in conjunction with our platform has allowed the automation of a range of common organometallic reaction types for the synthesis of four highly reactive compounds from across the periodic table: [Cp2TiIII(MeCN)2]+ , CeIII{N(SiMe3)2}3, B(C6F5)3 and {DippNacNacMgI}2 which are variously sensitive to temperature, pressure, water and oxygen. Automated purification by crystallisation, filtration and sublimation are each demonstrated along with analysis using inline NMR or reaction sampling for UV/Vis. Finally, we demonstrate automated ultra-low temperature reactivity, down to −90 °C as well as safe handling and quenching of alkali metal reagents, using dynamic feedback from an in-situ temperature probe.

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confidence: 99%

Autonomous Execution of Highly Reactive Chemical Transformations in the Schlenkputer

Cronin,

Bell,

Boser

et al. 2023

Preprint

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“…Since the introduction of the Bissey valve, a few alternative designs have surfaced to allow for the use of oil as an alternative while still maintaining the integrity of the air-free system, with the Lafler design being one of the best examples . Additionally, Linn reported, in this Journal , a mercury-free bubbler alternative utilizing an oil-based Bissey valve followed by a pressure check valve; however, this was designed specifically for an Ace-Burlitch Air-Free system. , The mercury-free bubbler replacement described herein can be applied to any air-free manifold system without modifications. Furthermore, the described apparatus maintains much of the simplicity and easy visual cues that have lent to the common mercury bubbler’s practicality.…”

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confidence: 99%

“…11 Additionally, Linn reported, in this Journal, a mercury-free bubbler alternative utilizing an oil-based Bissey valve followed by a pressure check valve; however, this was designed specifically for an Ace-Burlitch Air-Free system. 12,13 The mercury-free bubbler replacement described herein can be applied to any air-free manifold system without modifications. Furthermore, the described apparatus maintains much of the simplicity and easy visual cues that have lent to the common mercury bubbler's practicality.…”

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confidence: 99%

A Simple, Inexpensive, Mercury-Free Bubbler Apparatus

Johnson

West

2021

J. Chem. Educ.

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Inert gas manifolds for the handling of air-sensitive materials are commonplace in the inorganic chemistry curriculum as well as in research laboratories specializing in inorganic and organometallic synthesis. Mercury bubblers are ubiquitously implemented for maintaining a positive internal pressure for air-free manifold systems, commonly known as Schlenk lines. This has rendered them difficult to replace with equivalent and accessible alternatives. This communication describes the setup and implementation of a simple, inexpensive alternative to the traditional mercury bubbler that is modular and flexible enough to fit most any laboratory space.

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“…However, most academic institutions are reticent to maintain these experiments in their curricula because mercury electrodes are used. The risk of toxicity that working with mercury entails has led to proposals for the removal of mercury-containing devices, ranging from thermometers to vacuum lines, from educational laboratories. − …”

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confidence: 99%

Substitution of Mercury Electrodes by Bismuth-Coated Screen-Printed Electrodes in the Determination of Quinine in Tonic Water

et al. 2013

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The bismuth-coated screen-printed electrode is shown to be a suitable and safe alternative to the classical mercury electrode in the voltammetric determination of quinine in tonic water. This experiment is appropriate for undergraduate analytical courses as it helps students understand the fundamentals of electroanalysis using preplated screen-printed electrodes and the importance of green electrochemistry. Student interest is piqued by using a familiar real-world sample, tonic water.

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An Accessible Mercury-Free Vacuum Schlenk Line for Air-Free Techniques

Cited by 5 publications

References 12 publications

Autonomous Execution of Highly Reactive Chemical Transformations in the Schlenkputer

Autonomous Execution of Highly Reactive Chemical Transformations in the Schlenkputer

A Simple, Inexpensive, Mercury-Free Bubbler Apparatus

Substitution of Mercury Electrodes by Bismuth-Coated Screen-Printed Electrodes in the Determination of Quinine in Tonic Water

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