International
Tables for
Crystallography
Volume F
Crystallography of biological macromolecules
Edited by M. G. Rossmann and E. Arnold

International Tables for Crystallography (2006). Vol. F, ch. 10.1, p. 199   | 1 | 2 |

Section 10.1.3. Principles of cooling equipment

H. Hopea*

aDepartment of Chemistry, University of California, Davis, One Shields Ave, Davis, CA 95616-5295, USA
Correspondence e-mail: hhope@ucdavis.edu

10.1.3. Principles of cooling equipment

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There are many ways to construct a low-temperature apparatus based on the cold-stream principle that functions well, but they are all made according to a small number of basic principles.

All gas-stream crystal-cooling devices must have three essential components: (a) a cold gas supply, (b) a system of cold gas delivery to the crystal, and (c) a system for frost prevention at the crystal site.

10.1.3.1. Cold gas supply

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Two methods are commonly used: generation of gas by boiling liquid N2 with an electrical heater, and cooling of a gas stream in a liquid-N2 heat exchanger.

Because precise voltage and current control are easily realized, the boiler method has the advantage of providing very accurate control of the flow rate with minimal effort. Precise control of the flow rate is typically not attained when the rate is controlled with standard gas-flow regulators, because they control volume, not mass.

In addition to control of the flow rate, precise control of the temperature requires exceptional insulation for the cold stream. The longer the stream path, the higher the requirements for insulation. As a rule, temperature rise during transfer should not exceed 15 K at a flow rate of 0.2 mol N2 min−1; preferably, it should be significantly lower. Higher cooling loss leads to excessive coolant consumption and to instability caused by changes in ambient temperature. High flow rates also tend to cause undesirable cooling of diffractometer parts. No commercially offered device should be accepted if it does not meet the criterion given above.

Appropriate insulation can be readily attained either with silvered-glass Dewar tubing or with stainless-steel vacuum tubing. Glass has the advantage of being available from local glassblowing shops; it generally provides excellent insulation. The main disadvantages are fragility and a rigid form that makes accurate positioning of the cold stream difficult. Stainless steel can provide superb insulation, given an experienced manufacturer; unsatisfactory insulation is quite common. A major advantage is the availability of flexible transfer lines that greatly simplify the positioning of the cold stream relative to the diffractometer.

10.1.3.2. Frost prevention

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Three areas must be kept frost-free: the crystal, the crystal mount and the delivery end of the transfer tube. The first successful solution to this problem was the dual-stream design of Post et al. (1951[link]). It provides for a cold stream surrounded by a concentric warm stream. If the warm stream is sufficiently dry, this will prevent frost around the outlet. The crystal will remain frost-free only if mixing of the two flows occurs downstream from the crystal. For a stream aligned with the axis of the goniometer head, an additional shield is needed to keep the goniometer head frost-free.

References

Post, B., Schwartz, R. S. & Fankuchen, I. (1951). An improved device for X-ray diffraction studies at low temperatures. Rev. Sci. Instrum. 22, 218–220.








































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