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4.5:

Sublimation

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Analytical Chemistry
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JoVE 核 Analytical Chemistry
Sublimation

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Sublimation is the direct phase transformation from the solid to the gaseous phase, bypassing the liquid state.

For example, solid carbon dioxide, or dry ice, sublimes to gaseous carbon dioxide at room temperature and pressure.

This transition occurs at the solid–gas phase boundary and is not observed above the triple point.

In simple sublimation, the substance is heated in a beaker covered with an upturned watch glass as a secondary surface.

The pure substance is deposited on the watch glass, while impurities are left behind.

Lyophilization, or, freeze-drying is the low-temperature dehydration of heat-sensitive materials with applications in chemistry, biology, and food preservation.

Here, the sample is frozen, and placed in a vacuum. When the temperature is raised, the ice sublimes to water vapor, yielding a cryo-desiccated product.

4.5:

Sublimation

Sublimation is the direct transformation of a solid to a gaseous state. For instance, at standard pressure and room temperature, solid carbon dioxide sublimes to gaseous carbon dioxide. The phase diagram depicts the conditions required for sublimation. This process occurs at the solid-gas phase boundary and is not observed above the triple point of the substance. The reverse of sublimation is called deposition, where a gaseous substance condenses directly into a solid. Sublimation and deposition can both be used to separate an analyte from interferents.

In simple sublimation, a solid sample is heated in a beaker covered with an inverted watch glass acting as the secondary surface. The analyte sublimes into a gas, and then cools to a solid again when it meets the watch glass. For successful purification, the sublimation temperature must be high enough to ensure high vapor pressure, but low enough to avoid either melting or decomposing the substance. Iodine is an example of a substance amenable to purification by simple sublimation.

If the sample is sensitive to heat, low-temperature sublimation techniques such as freeze-drying (also known as lyophilization) can be used. These techniques are often applied to dehydrate the desired material. Here, the sample is frozen using an ultra-low-temperature mixture (dry ice/acetone), and placed in a vessel attached to a vacuum pump. The ice in the sample sublimes to water, leaving behind the desired, cryo-desiccated product. Lyophilization is used extensively in purifying enzymes for use in biochemistry, molecular biology, and food preservation.