Mechanically refrigerated gas streams for studies to -70°C

Rudman, Reuben

doi:10.1107/s0021889872009033

Cited by 2 publications

(3 citation statements)

References 6 publications

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“…These elements influence the formation of excess gas and hence the flow rate of the gas stream. For constructive details in the field of gas supply units, the reader should consult the original papers (ref [29][30][31][32][33][34][35][36][37][38][39] for the evaporation technique and ref 26b and [40][41][42][43][44][45][46][47] for the heat exchange technique).…”

Section: Gas Supply Unitmentioning

confidence: 99%

Low-temperature x-ray structure techniques for the characterization of thermolabile molecules

Veith¹,

Frank²

1988

Chem. Rev.

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Contents I. Introduction 81 A. General Aspects 81 B. Brief Comparison of the Methods for me 82 Characterization of Unstable Intermediates 11. Methods and Devices 82 A. General Remarks 82 B. Main Elements of Gas Stream X-ray 83 Diffraction Cooling Devices 1. Basic Principles 83 2. Gas Supply UnR 83 3. Delivery Nozzle 84 4. Transfer Line 84 5. Refill System 84 8. Automatic Temperature Control 85 85 Crystals 1. Crystal Growth in a Capillary 85 2. Crystal Growth in One Place and 86 Transfer to the Diffraction Device under Protective Conditions Elsewhere 111. Use of Three-Dimensional Structures of 87 Unstable Inorganic Molecules and Solids in the Evaluation of Their Reactivity C. Growih and Handling of Thermolabile Single A. Correlation of Instability and Molecular 87 B. Reaction Intermediates 89 C. Unstable Phases in Solid-state Chemistry 90 IV. Conclusion and Outlook 90 V. Acknowledgments 90 VI. References 90 Structure I. Introductlon A. General Aspects The chemist is currently confronted with compounds that are unstable for either kinetic or thermodynamic reasons. I f these compounds are produced during t h e course of a reaction sequence, t h e y are designated as reaction intermediates. As well as chemical procedures, a variety of physicochemical methods has been used (see n e x t chapter) to elucidate t h e composition and three-dimensional structure of t h e intermediate. T h e most complete and exact results are obtained by diffraction methods, followed by three-dimensional structure determinations. With X-ray diffraction on single crystals, the sample has to be cooled because of its instability, and the crystal growth and transfer must b e performed under low-temperature conditions. In this review the special techniques for the synthesis and handling of single crystals of unstable compounds are described. As far as we know, there is only one

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Section: Gas Supply Unitmentioning

confidence: 99%

Low-temperature x-ray structure techniques for the characterization of thermolabile molecules

Veith¹,

Frank²

1988

Chem. Rev.

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“…A schematic diagram of the system, which is an improved version of a previously described system (Rudman, 1972), is shown in Fig. 1.…”

Section: Low-temperature Systemmentioning

confidence: 99%

“…It has recently been shown that a heat exchanger immersed in a bath cooled by a mechanical refrigerator can be used for cooling a gas stream (Rudman, 1972;Marsh & Petsko, 1973). Temperatures as low as -70°C were reported.…”

Section: Introductionmentioning

confidence: 99%

A mechanically refrigerated gas stream (to -120°C) and some useful accessories

Lippman¹,

Rudman²

1976

J Appl Cryst

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A system for cooling a stream of dry air to −120°C is described. Mechanically refrigerated cooling units are used to maintain the cold baths in which heat exchangers are immersed. Adapters for converting a precession camera to a flat‐plate oscillation‐rotation camera and for mounting crossed polaroids on the precession camera are described. These devices are particularly useful for examining and aligning crystals grown in situ at low temperatures. They can also be used for aligning crystals on the precession camera even when monochromated radiation is used.

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Mechanically refrigerated gas streams for studies to -70°C

Cited by 2 publications

References 6 publications

Low-temperature x-ray structure techniques for the characterization of thermolabile molecules

Low-temperature x-ray structure techniques for the characterization of thermolabile molecules

A mechanically refrigerated gas stream (to -120°C) and some useful accessories

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