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The isopiestic method is one of the most common techniques for establishing water absorption
isotherms or the relationship of water activity in a sample to gravimetric water content. The theory
behind it relatively simple. A sample is placed in a vacuum chamber along with an open container of
reference saly solution and is allowed to equilibrate. Over time the chamber air will come to the
relative humidity of the reference salt. As the system reaches equilibrium the sample will either lose
or take up water from the air to reach the same water activity of the reference salt solution. The
gravimetric water content of the sample is determined by drying in an vacuum oven or by Karl Fischer
titration. Combining the sample water activity with its gravimetric water content will provide one
point on its sorption isotherm. By repeating with several reference salt solutions (typically at least 8
points are necessary) across a range of water activities, the resulting set of points can be fit with any
one of the number of sorption isotherm equations.
Assuming the makeup of the sample does not change future values of water activity can be
interpolated from a measure of water content. Typical equilibration times are from 10 to 21 days
where equilibrations for samples with lower water activity. Will fall in the upper end of the range.
Often many chambers are set up at once to allow for simultaneous equilibration, but this method
considerable amount of space
The isopiestic method is attractive because it is free from contamination concerns and most
importantly inexpensive. In addition, it is a straight forward method that is not difficult to set up. Its
main disadvantages are space and time requirements.
There is another drawback to the isopiestic method that may not be apparent. Because of the long
equilibration times, samples can change during equilibration. These changes may take the form of
mould growth on the sample, or transitions from a good to rubbery or crystalline texture.
Water profoundly influences product attributes such as quality and safety. To completely
understandwater relations in a product requires an understanding of the amount of water (moisture
content) that can be held at a given energy state (water activity). Moisture sorption isotherms describe
the relationship between water activity and moisture content at a constant temperature. The nature
of this relationship depends on the interaction between water and other ingredients. The amount of
water vapor that can be absorbed by a product depends on its chemical composition, physical-
chemical state, and physical structure. Consequently, the isotherm shape is unique to each product
type due to differences in capillary, surface, and colligative effects (Figure 1). Products that lie in the
low water activity portion of the isotherm are often referred to as dry, those in the range of 0.60 aw
to 0.90 aw are intermediate moisture products, and those having water activities higher than 0.90 are
high water activity products.
For ease of interpretation, isotherms are often identified by Brunauer classifications (Brunauer, 1945).
Most food and pharmaceutical products fall under type I, II, or III. Type I isotherms are typical of very
hygroscopic materials, Type II (sigmoidal) isotherms are typical for intermediate moisture products,
and type III (J-shaped) isotherms are typical for crystalline and coated materials. These general
classifications proved useful when conducting isotherms on every product was not feasible due to
time and labor constraints. However, with automation and improved speed, isotherms can easily be
conducted on any product and the uniqueness of each isotherm often proves more valuable than
placing them in a common classification.
Sorption isotherms of food materials are generally in sigmoid shape (type II). The effects of
Raoult’s law, capillary effects, and surface–water interactions are important in sorption curves
and they are additive.
Type I isotherm is observed in pure crystalline sugar. It shows very little moisture gain up to
a water activity of 0.7 to 0.8 since the only effect of water is hydrogen bonding to the –OH
groups present on the surface of the crystal
Thus, surface effect is important, which means grinding the sugar to smaller particles will
increase the moisture content at low water activity values. As the water activity is increased,
water begins to penetrate into the crystal, causing dissociation of sugar–sugar interactions
and a solution is obtained. At this stage, the effect of Raoult’s law is important.
The type III isotherm is observed in the case of anticaking agents. In these types of materials,
binding energy is so large that water activity is depressed while water is absorbed. When all
the binding sites are filled, the increase in moisture content causes water activity to increase
drastically.