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

Lippman, R.; Rudman, Reuben

doi:10.1107/s002188987601100x

Cited by 3 publications

(3 citation statements)

References 5 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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“…Two reports (93,115) on cryostats suitable for use down to essentially liquid helium temperature have appeared along with two reports of gas flow systems for automatic singlecrystal diffractometry down to liquid nitrogen temperature (31, 40). Lippman and Rudman (91) have investigated the use of mechanically refrigerated units to cool gas streams to about -120 °C and a specially constructeddiffractometer for the study of liquids and glassy materials at very low temperatures has been described by Bizid et al (15). In the high-temperature field, a review by Viswamitra (155) on high-temperature single-crystal diffraction methods has appeared.…”

Section: Instrumentationmentioning

confidence: 99%

X-ray diffraction

Pfluger¹

1978

Anal. Chem.

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“…The immersion method does not allow a fine temperature control. The gas stream method (Lippman and Rudman 1976;Burbank 1973), though easily adaptable to any instrument, is not so convenient due to the cumbersome nature of cryogen handling (liquid N 2 or compressed gas), temperature instability during cryogen refilling and frosting problems, which persist even with proper insulations during the actual working of a cryo-system over prolonged periods of time as in neutron diffraction.…”

Section: Introductionmentioning

confidence: 99%

A low-temperature attachment for a four-circle neutron diffractometer

1986

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A single-stage closed-cycle helium gas cryogenerator, capable of cooling between 77 K and 300 K, has been installed on the 4-circle neutron diffractometer at CIRUS. The cryo-tip assembly has been incorporated directly on the ~o-circle of the fu/1-clrde crysta/ orienter in place of the goniometer head used in room temperature experiments. The salient features of this low-temperature attachment and its performance are discussed. Keywords. Low temperature diffraction; diffractometer cryo-assembly; helium gas cryo-tip; closed-cycle cryogenerator.

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

Cited by 3 publications

References 5 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

X-ray diffraction

A low-temperature attachment for a four-circle neutron diffractometer

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