voltage recommended by the mantle manufacturer. Higher voltages will cause a mantle to overheat, melting the fiberglass insulation and exposing the bare heating element.

Some heating mantles are constructed by encasing the fiberglass mantle in an outer metal case that provides physical protection against damage to the fiberglass. If such metal-enclosed mantles are used, good practice is to ground the outer metal case either by using a grounded three-conductor cord from the variable autotransformer or by securely affixing one end of a heavy braided conductor to the mantle case and the other end to a known electrical ground. This practice protects the laboratory personnel against an electric shock if the heating element inside the mantle short-circuits against the metal case. Placing the heating mantle on a laboratory jack and holding the flask or container being heated by clamps attached to a separate ring stand or grid work is the recommended procedure. This allows for rapid removal of heat in the case of overheating or exothermicity.

7.C.5.4 Oil, Salt, or Sand Baths

When using oil, salt, or sand baths, take care not to spill water and other volatile substances into the baths. Such an accident can splatter hot material over a wide area and cause serious injuries.

Electrically heated oil baths are often used to heat small or irregularly shaped vessels or to maintain a constant temperature with a stable heat source. For temperatures below 200 °C, a saturated paraffin oil is often used; for temperatures up to 300 °C, a silicone oil should be used. Care must be taken with hot oil baths not to generate smoke or have the oil burst into flames from overheating. Always monitor an oil bath by using a thermometer or other thermal sensing device to ensure that its temperature does not exceed the flash point of the oil being used. For the same reason, fit oil baths left unattended with thermal-sensing devices that turn off the electric power if the bath overheats. Heat these baths by an enclosed heating element, such as a knife heater, a tubular immersion heater such as a calrod, or its equivalent. The input connection for this heating element is a male plug that fits a female receptacle from a variable autotransformer (e.g., Variac) output line. Alternatively, a temperature controller can be used to control the temperature of the bath precisely. Temperature controllers are available that provide a variety of heating and cooling options. Thermocouples used by controlling devices must be clamped securely in place to maintain contact with the medium or object being heated at all times.

Oil baths must be well mixed to ensure that there are no hot spots around the elements that take the surrounding oil to unacceptable temperatures. This problem can be minimized by placing the thermoregulator fairly close to the heater. Contain heated oil in either a metal pan or a heavy-walled porcelain dish; a Pyrex dish or beaker can break and spill hot oil if struck accidentally with a hard object. Mount the oil bath carefully on a stable horizontal support such as a laboratory jack that can be raised or lowered easily without danger of the bath tipping over. Always clamp equipment high enough above a hot plate or oil bath that if the reaction begins to overheat, the heater can be lowered immediately and replaced with a cooling bath without having to readjust the clamps holding the equipment setup. Never support a bath on an iron ring because of the greater likelihood of accidentally tipping the bath over. Provide secondary containment in the event of a spill of hot oil. Wear proper protective gloves when handling a hot bath.

Molten salt baths, like hot oil baths, offer the advantages of good heat transfer, commonly have a higher operating range (e.g., 200 to 425 °C), and may have a high thermal stability (e.g., 540 °C). The reaction container used in a molten salt bath must be able to withstand a very rapid heat rise to a temperature above the melting point of the salt. Care must be taken to keep salt baths dry, because they are hygroscopic, a property that can cause hazardous popping and splattering if the absorbed water vaporizes during heating.

7.C.5.5 Hot Air Baths and Tube Furnaces

Hot air baths can be useful heating devices. Nitrogen is preferred for reactions in which flammable materials are used. Electrically heated air baths are frequently used to heat small or irregularly shaped vessels. Because of their inherently low heat capacity, such baths normally must be heated considerably above the desired temperature (≥100 °C) of the vessel being heated. Purchase or construct these baths so that the heating element is completely enclosed and the connection to the air bath from the variable autotransformer is both mechanically and electrically secure. These baths can be constructed from metal, ceramic, or, less desirably, glass vessels. If a glass vessel is used, wrap it thoroughly with heat-resistant tape so that if the vessel breaks accidentally, the glass will be contained and the bare heating element will not be exposed. Fluidized sand baths are usually preferred over air baths.

Tube furnaces are often used for high-temperature reactions under reduced pressure. The proper choice of glassware or metal tubes and joints is required, and the procedures should conform to safe practice with electrical equipment and evacuated apparatus.



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