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In-Depth Information
[138] . Several authors have discussed, in detail, major hazards with hydrothermal
autoclaves [37,139] .
Overheating of the furnace resulting from the malfunction of the control system
is a common reason for vessel failure. Hence, furnaces should be properly shielded.
Burns from hot vessels represent another major hazard with cold-seal laboratories.
If it is necessary to handle a hot vessel, it should be done by grasping the relatively
cool closure assembly wearing special insulated gloves.
Note that any vessel to be heated must never be filled completely with an
aqueous solution. Fluids expand on heating and are capable of generating extreme
pressures when further heated beyond the PT limits of the autoclave. It is criti-
cally important to calculate the thermal expansion of the aqueous phase and to
allow at least 20% of the total volume of the vessel for uncertainty or temperature
overturn. An apprenticeship in an operating hydrothermal laboratory is strongly
recommended to learn, to anticipate, and to cope with the dangers of such experi-
ments. For those planning to set up a hydrothermal laboratory, it is advisable to
visit other existing laboratories to review safety procedures as well as designs.
Therefore, autoclave maintenance and safety make hydrothermal experiments
quite expensive.
References
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ials processing, J. Ceram. Soc. Japan 117 (2009) 236 244.
[2] A. Rabenau, The role of hydrothermal synthesis in preparative chemistry, Angew.
Chem. (English Ed.) 24 (1985) 1026 1040.
[3] R.A. Laudise, J.W. Nielsen, in: F. Seitz, D. Turnbull (Eds.), Hydrothermal Crystal
Growth, Solid State Physics, vol. XII, Academic Press, New York, NY, 1961.
[4] D. Clauss, Engineer's Guide to High-Temperature Materials, McGraw-Hill, New York,
NY, 1969, pp. 1 612.
[5] C.J. Smithells, Metals Reference Handbook, 1, Plenum Press, New York, NY, 1967.
p. 378.
[6] R. Speed, A. Filice, Quartz glass pressure vessels for hydrothermal studies, Am. Min.
49 (1964) 1114 1119.
[7] V.I. Popolitov, Hydrothermal growth of crystals under visual examination, in: K. Byrappa
(Ed.), Hydrothermal Growth of Crystals, Pergamon Press, Oxford, 1991, pp. 255 297.
[8] B.N. Litvin, D.A. Tules, Apparatus for hydrothermal synthesis and growth of mono-
crystals, in: A.N. Lobachev (Ed.), Crystallization Processes Under Hydrothermal
Conditions, Studies in Soviet Science, Consultant Bureau, New York, NY, 1973,
p. 139.
[9] H. De Senarmont, Recherches sur les Propri´t´s optiques bir´fringentes des corps iso-
morphes, Ann. Chim. Phys. 32 (1851) 129
132.
[10] M. Daurree, Sur le Metamorphisme et Recherches Experimentales Sur Quelques-uns,
Ann. Mines 12 (1857) 289 326.
[11] E.T. Allen, J.L. Crenshaw, J. Johnston, Am. J. Sci. Fourth Ser. 33 (1912) 167.
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