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Moisture Sorption:
Practical Aspects of Isotherm
Measurement and Use

Theodore P. Labuza
Department of Food Science and Nutrition
University of Minnesota, St. Paul

Published by the
American Association of Cereal Chemists
St. Paul, Minnesota
Library of Congress Catalog Card Number: 83-73312
International Standard Book Number: 0-913250-34-1

©1984 by the American Association of Cereal Chemists

All rights reserved.

No part of this book may be reproduced in any form
by photocopy, microfilm, retrieval system, or any other means,
without written permission from the publisher.

Printed in the United States of America

The American Association of Cereal Chemists

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St. Paul, Minnesota 55121, USA

Deacidified using the Bookkeeper process.

Neutralizing agent: Magnesium Oxide
Treatment Date: UC] on
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 Preface and Acknowledgments

This book was written to serve as a training tool for people who wish to
use the concept of isotherms and water activity and gain some practical
skills. It is in response to a need both in the classroom and in the
laboratory, as became apparent from contacts made through consulting and in
workshops. Its examples, taken from the real world and student laboratory
exercises, should help the reader better understand the concept of water
activity and its uses. This monograph is intended to be a first step toward a
book on freezing and drying of foods. References in the text have been kept
to a minimum; however, an extensive bibliography has been added at the end.
Much of the background work was stimulated by my close association, as
both student and collaborator, with Dr. Marc Karel of the Massachusetts
Institute of Technology in Cambridge, Massachusetts. The information
contained in this handbook formed the basis for a course on water in foods
that I have been teaching for almost 20 years. Grants from the University of
Minnesota Agricultural Experiment Station (grant numbers 18-72 and 18-78) and
National Science Foundation contract 7910370 supported much of my research on
this subject. In addition, the Quaker Oats Company is acknowledged for its
support. Finally, I would like to acknowledge all those students who sat
through many hours of lecture, lab, and problem solving; their participation
helped to make this information understandable and usable.

cit
 TABLE OF CONTENTS

Page
vii List of Illustrations
Wiii List ‘of Tables

1 I. INTRODUCTION: DEFINITION OF WATER ACTIVITY

1 A. Moisture Exchange Experiments
Z B. Definition of Chemical Potential
3 C. Water Activity and the Moisture Sorption Isotherm: Definition for a
Food
4 D. Properties of Food that Control the Water Activity
4 1. Colligative effect
6 2. Capillary effect
7 3. Surface interaction

8 II. TYPICAL SORPTION ISOTHERMS

8 A. General Curve
8 B. Specific Curves--Lower a, Range
10 C. Hysteresis
13 D. Amorphous-Crystalline Transfer
16 E. Temperature Effect
21 F. Total Pressure Effect

Ze III. USE OF THE MOISTURE SORPTION ISOTHERM

22 -A. Monolayer Stability Value
22 1. Usefulness of the monolayer value
23 2. BET monolayer calculation
25 8B. Crispness/Hardness
27 C. Caking
a D. Microbiology
o27 E. Packaging Predictions
27 1. Theoretical considerations
30 2. Sample calculation: Moisture gain to critical a, for loss of
crispness of potato chips
38 F. Dry Ingredient Mixing
38 1. Introduction
59 2. Mathematical model for equilibrium
44 3. Mathematical models for the rate of gain or loss of moisture
49 _ 4, Determination of permeability and diffusion constants for moisture
gain/loss of ingredients
sgl G. Humectant Selection
51 1. Introduction
ay 2. Raoult's law method
53 3. Norrish equation
56 4. Grover equation
57 5. Ross equation
58 6. Example problem
62 H. Package Temperature Shift

64 IV. DETERMINATION OF MOISTURE SORPTION ISOTHERMS

64 A. Humidity Controlling Devices
64 1. Mechanical humidifiers
 64 2. Sulfuric acid/H70 mixtures
64 3. Glycerol/H720 mixtures
64 4. Salt solutions
65 5. Dry desiccator
67 B. Containers for Salt Solutions/Slurries
67 1. Desiccators
67 Peels
67 3. Fish tanks
67 C. Sample Preparation
67 1. Sample size/heterogeneit y
67 2. True adsorption isotherm--Sample initial preparation
68 3. Desorption isotherm--Wet tissue sample preparation
68 4. Working isotherm--Initial sample preparation
69 D. Isotherm Procedure
69 1. Water activity range/temperature choice
69 2. Initial sample preparation
70 3. Equilibration time
74 4. Calculation of final moisture content
2 E. Other Isotherm Method Problems
72 1. Isotherm at high temperature
hee. 2. Use of vacuum
US 3. Air mixing
73 4. Sample mixing
73. ¥F. Measuring a, Instead of Doing an Isotherm

73 V. DRAWING THE ISOTHERM

75 Literature Cited

77 Appendix A--Tables
84 Appendix B--AOAC Water Activity Methods

85 Reference Lists
85 Properties of Water
oT Moisture Content, a,, and Isotherm Measurement
95 Water Activity Predictions and Isotherm Properties
97 Sorption Hysteresis
100 Sorption Kinetics and Diffusion
102 Isotherms of Food and Food Ingredients
108 Dry Food Stability
118 Water Activity and Microbiology
140 Intermediate Moisture Foods
144 Dehydrated Food Packaging

147 Index

vi
 LIST OF ILLUSTRATIONS

Weight gain of dry cereal cracker.

Weight loss of beef muscle.
Question for a third moisture exchange experiment.
Typical moisture equilibrium vs water activity for foods.
Classification of standard moisture sorption isotherms.
Surface adsorption of water on crystalline material.
Adsorption-desorption hysteresis loop.
Sorption hysteresis effect from supersaturation of sugars.
Water vapor sorption hysteresis in dried apple slices.
=
DKDUNFWHDH
MH
CO Rate of loss of vitamin C as a function of temperature,
water activity, and sorption hysteresis.
rr
~— Moisture sorption isotherms of pure crystalline and
noncrystalline food systems.
— ip) Effect of exposure of amorphous sucrose on moisture
content and degee of crystallinity.
i Adsorption of water vapor by amorphous sucrose at various
relative humidities.
14 Adsorption of water vapor by amorphous glucose at various
relative humidities.
15 Water vapor sorption progress of amorphous and crystalline
solids.
16 Effect of temperature on moisture sorption of foods.
17 Plot of log a, vs temperature for predicting a.
18 Moisture adsorption and desorption isotherm for Sinton
wheat at 5°C.
19 Moisture adsorption and desorption isotherm for Sinton
wneat. at 157.C.
20 Moisture adsorption and desorption isotherm for Sinton
wneat-at.25 C.
pa Clausius-Clayperon plot of 1n a, vs temperature.
Ze Effect of a, on typical food deteriorative reactions.
23 Relationship of log (shelf life) to a,.
24 BET monolayer plot for sorption data.
25 Sensory crispness intensity as a function of water activity
for dry saltine crackers.
26 Working moisture isotherm superimposed on true isotherm.
27 Weight gain of bags packaged with desiccant.
28 Moisture sorption isotherm for potato chips.
Hh Unaccomplished moisture gain for potato chips stored in
polyethylene.
30 Unaccomplished moisture gain for potato chips stored in
mylar.
31 Moisture exchange in ingredients X and Y to an equilibrium
water activit.
a2 Example isotheruws for equation 34 solution.
a3 Representation of moisture distribution.
34 Moisture sorption isotherm of glycerol.
3) Humectant isotherms for example problem solution.
36 Shift in a, for food in a sealed pouch subjected to a
temperature shift.

vii
 LIST OF TABLES

Monolayer Values of Dehydrated Foods

Minimal a, Limits for Some Microorganisms of
Significance to Public Health
Water Activity of Some Foods and Susceptibility to
Spoilage by Microorganisms
Equilibrium Moisture Content of Dry Gum Powders at
Various Water Activities
Moisture Sorption Isotherm Data at 23°C--Food and Fiber
Sources
Equilibrium Moisture Content of Pharmaceutical Excipients
K Values for Norrish Equation
E; Values for Grover Equation
65-66 Tables of Values for the Equilibrium Relative Humidity
of Selected Saturated Salt Solutions

Vapor Pressure of Water below 100°C

Water Sorption Properties of Glucose
Water Sorption Properties of Fructose
Water Sorption Properties of Sucrose
Water Sorption Properties of Lactose
Water Sorption Properties of Corn Syrup Solids
Moisture Sorption Isotherms of High Fructose Corn Syrup
Water Sorption Properties of NaCl
Water Sorption Properties of Potassium Chloride
Glycerol Water Sorption Isotherm at 23°C
Water Sorption Properties of Propylene Glycol
Water Sorption Properties of 1,3-Butylene Glycol
Water Sorption Properties of Polyethylene Glycol 400

viii
Moisture Sorption:
Practical Aspects of Isotherm
Measurement and Use
 I. Introduction: Definition of Water Activity

‘A. Moisture Exchange Experiments

To define the physical-chemical relationship between water and food

components, it is best to begin with a simple experiment. In this experiment
we have an environmental chamber with an electronic control that will keep it
at exactly 25°C and 75% RH (relative humidity). Percent relative humidity is
defined as:

PH»0
x 100 Cr)
Po

where py.o is the partial vapor pressure of water in the air of the
chamber and p, is the vapor pressure that pure water would create at that
temperature when the space is totally saturated at 100% RH (Appendix Table Al
gives the value of p, for pure water as a function of temperature). Thus, at
100% RH, PH20 = Pos
In our first experiment, we will put a sample of a dry cereal product
(such as a cracker) initially at 3% moisture (wet basis [wb]) into the chamber
and follow its weight gain with time. As seen in Figure 1, the cracker will
gain moisture until it reaches some equilibrium value, for example 12% H)0-
Moisture will always go to this value if we repeat this experiment, so it is
termed an equilibrium moisture content.
It may take two to three weeks, however, for the cracker to reach the
equilibrium at a moisture content of 12% (wb). No weight change may be found
after that time, because the changes will be too small to measure. At this
point the cracker is removed and put into a small, sealed jar with little
headspace.

1s

wn

PERCENT
MOISTURE

~ vr wo © e
8

TIME (DAYS) 25°C 75”RH

Figure 1. Weight gain of dry cereal cracker exposed to 25°C and 75% RH.

1
 In our second experiment, meat (such as beef) initially at 60% moisture
(wb) is placed into this same environmental chamber. Unlike the cracker, the
meat loses moisture (Figure 2) until it reaches an equilibrium value of 20%.
It too is then removed and placed in a sealed jar.
The questions now for our third experiment (Figure 3) are: “What happens
when we mix at 25°C equal amounts of the beef and cracker that have been
equilibrated to 75% RH? Will they exchange moisture until they come to equal
4 H90? If not, why not?”
If this third experiment is done, what happens is nothing, no matter what
amount of meat or cracker we mix into a jar, as long as the headspace is
small. This is because they are at equilibrium with each other. More
correctly, the water in the cracker and the water in the meat both have the
same thermodynamic state as defined by chemical potential.

B. Definition of Chemical Potential

In describing the state of any system, an important factor besides

temperature, volume, concentration, etc., is the free energy (AG) of the
System. On a molar basis, this becomes the chemical potential M, which from
thermodynamics is:

fm fa. to Rle Ais a (2)

where mw is the chemical potential (calories per mole [cal/mole]) at some

standard state; R is the gas constant = 1.987 cal/mole °K; T is temperature in
°K = °C + 273.15; and a is the thermodynamic activity of the particular
substance.
Activity is either measured or defined from other equations, depending on
whether one is considering liquid, solid, or vapor systems. What is known

Z~WATER

9 N Tv w @ Qe

TIME (DAYS) 25° 75%RH

Figure 2. Weight loss of beef muscle exposed to 25°C and 75% RH.

2
 from thermodynamics is that if the chemical potential of a substance
(ingredient) is the same in two different states (or in two different complex
mixtures), that substance will be in equilibrium between the two states such
that if any exchange occurs, the loss from one state is made up by the gain
from the other state (or mixture). Thus, in our third experiment, since there
was no measurable exchange of moisture between the cracker and the meat, we
can say that they were at equal chemical potential for water, iee.,

(#450) cracker = (440) Meat . (3)

Since temperature was held constant, T is constant. In addition, My, and
R are constants; thus, the activity of water, a,, in the meat and in the
cracker is also constant. (For a more detailed discussion of activity and
chemical potential, see Franks [1982].) Looking again at our definition (2)
with respect to state, we can then also say that the activity of the water in
the headspace is also the same as it is in the meat and the cracker:

(a,) meat = (a,) cracker = Ca) airs (4)

As a side note, if the volume of air space in our third experiment were
large, the air might take up enough moisture from the two foods to change
their a,'s, but all three will eventually equilibrate to the same ae, OF
chemical potential. Note also that chemical potential difference is a measure
ofthe driving force for change between two states. It defines the direction
of change but says nothing about how fast the change will occur (i.e., rate of
change). The rate of change will be discussed in detail later.

C. Water Activity and the Moisture Sorption Isotherm: Definition for a Food

Since we found in the third experiment that the chemical potentials or

activities of the water in all three states (i.e., in the air, in the meat,
and in the cracker) were the same, we can use another thermodynamic equation
to further define the activity of water. In the gas state, under normal
conditions, the activity of one of the molecular species in the gas is equal
to its partial pressure divided by the total pressure the system would have at
that temperature if the space were completely saturated with that molecular
species. This means that, at 100% saturation, if any more of molecule X were
added to the system, other molecules of X would condense out as liquid or

Cracker

Figure 3. Question for a third moisture exchange experiment.

solid. In equation form, for water vapor, the activity of the water in the
vapor (a, or ay as used by food scientists) becomes:

PH20
ay = (5a
Po

This equation is very similar to equation 1 and thus tells us that if we know
the relative humidity of water in the air in a chamber, the activity of the
water in that air is:

- ARH (6)

In addition, since the water in the two foods in the third experiment was
also in equilibrium with the water in the air, the ay of the food is the
same as that of the air and can be measured by equation 6 if we know the % RH
when the water in a food has reached equilibrium in the air space surrounding
it. Sometimes this a, is designated as the % ERH (equilibrium relative
humidity) and thus:

a. = SERA e C7
Ww 100

It is extremely important to note that measurement of the a, of a food

by measuring the a, (or % RH) of the air headspace assumes that equilibrium
has been reached. Also important is the fact that foods with different
moisture contents will have different ay's depending on the state of water
in the food. This relationship between moisture content and a, is called
the moisture-sorption isotherm, isotherm because temperature must be constant
(see equation 2).

D. Properties of Food that Control the Water Activity

Certain properties of the food and the way that water interacts with the
components of a food result in different degrees of binding or tying up of the
water. The more tightly water is bound, the lower its chemical potential or
aye The degree of binding of water also has an effect on the quality of a
food, which will be discussed later. The three major physical effects that
lower water activity are listed below.

1. Colligative effect
When a solid solute dissolves in water, it interacts with the water in
three dimensions through dipole-dipole, ionic, and hydrogen bonds. These
interactions affect the properties of water based on the amount of the added
molecules relative to the amount of water molecules present. This interactio1
is called a colligative effect.
Some properties that are changed are boiling point, freezing point, and
vapor pressure. Vapor pressure is important because it affects the activity
in the headspace above the solution. Thus, if an added solute decreases the
activity of water in solution, the pyo in the air headspace above a
solution (and thus the a, of the air) also decreases to the same amount at
equilibrium. For solutions of low-molecular-weight electrolytes and

4
nonelectrolytes at low molal concentrations, this interaction can be evaluated
by Raoult's law,

NiD0
i) = i] 2 (8a)
NH50 + Ngolute

where:
Ny»0 moles of water in solution,
Nsolute moles of dissolved solute species in a solution of N50
moles of water, and
ay activity coefficient = 1 for ideal solute.

The Y value is a measure of the nonideality of a dissolved species. For

large molecules like gums, starches, and protein, y is very small and thus the
large molecules decrease a, much more than ideal solutes like sugars or salt
do. However, since their molecular weight (MW) is very large, the total a5
decrease is small. Electrolytes decrease the a, more than expected on a
molecular weight basis because they dissociate. For example, 1 mole of NaCl
is actually two moles of solutes, Nat and Cl-.
These electrolyte solutes also create dipole-dipole interactions with
water, which may increase or decrease Y depending on the forces. Fontan et al
(1979) have discussed the theoretical basis for the prediction of Y for
solutes used in foods; see their article for more in-depth coverage.
To illustrate the colligative effect, let us predict the lowering in a,
for 1 mole of NaCl (MW = 58.45) added to 1 liter (1,000 g) of water. This is
a l-molal solution of NaCl. The a, is:

1000
a, = 1 * —— ~——HW8 —___ = 0,965,
1000] , [58.45
18 58.45

Note the 2 in the denominator (which assumes complete dissociation),

denoting twice as many particles (called kinetic units), which assumes total
dissociation. Also note that y was assumed to be 1, for an ideal solution.
The actual measured value for l-molal NaCl is a, = 0.969. Thus, salt does
not lower the a, as much as predicted and,
0.969
= 1.004 ,
0.965

which is still close to 1. Raoult's law is usually fairly good to an a, of

0.95 for most low-molecular-weight species.
Freezing-point depression is another colligative property and can be
solved through Raoult's law to get the a,, where:

Mit es. 1 BOuN . (8b)

where N’s is the effective molesof solute per 1,000 g of water and AT'C is
the freezing-point depression. Thus, if freezing point is found, N’, can be
calculated and inserted as Neolute into equation 8a to predict a,. The
measured value of NS corrects for the nonideality; thus Y is assumed to be

)
l. mathematical
This manipulation is limited to dilute solutions and thus
high ay's. Some very sensitive instruments called cryoscopic osmometers
actually measure AT°C but read out in mOsm, which is milliosmoles or N’, x
103.
As an example, the following data have been found using a cryoscopic
osmometer for polydextrose, a potential new food ingredient for use in
reduced-calorie foods. Its average molecular weight is about 1,500. The true
lowering of a, is compared with the theoretical a,, and the activity
coefficient is calculated from these two values:

Measured Raoult's Law Actual Activity

Concentration Actual Ng N’s Predicted Measured Coefficient
(g/100 g H20)(moles/1000 g water) (mOsm/kg) ay ay a!
0.1 6.607 x 10™ SU) 0.999999 0.99995 0.99999
0.3 Deen Dicks: 0.99996 0.99990 0.99994
0c5 33333 x 1079 8.8 0.99994 0.99984 0.99990
1.0 6.667 x 1073 17..0 0.99988 0.99969 0.99981
1,5 1 x 1072 paeys) 0.99982 0.99954 0.99972
ae0 2 x 1072 iO Py) 0.99964 0.99909 0.99945
el 3.333 x 1072 85 0.99940 0.99847 0.99907
6.0 Ax 10-! 101.8 0.99928 0.99817 0.99889

As seen, even with 6 g of polydextrose per 100 g of water, the a, is

lowered only to 0.9982, whereas with almost 6 g of NaCl per 100 g of H90
(prior example), the a, reached 0.965. However, the polydextrose lowered
ay more than expected because the Y value was less than 1. Because of the
high molecular weight, however, the overall effect on ay is small.
One last question is whether solute colligative effects also operate at
low aye Recent work by Duckworth (1981) suggests that salts and sugars can
remain in solution to low ay's, so there should be colligative effects,
although they are not predictable from Raoult's law.

2. Capillary effect
A second effect that depresses water activity is the capillary effect.
The vapor pressure of water above a curved liquid meniscus is less than that
of pure water because of changes in the hydrogen-bonding between water
molecules as a result of the surface curvature. Since foods have a myriad of
capillaries, some lowering of the ay should result. The Kelvin equation
predicts this lowering by:

2 Ys cos@ Vz
i a ee (9)
where:
Ys = surface tension of liquid in a pore,
6 = wetting angle,
Vi, = molar volume of liquid in cm3/mole,
r = capillary radius,
R = gas constant (8.314 x 10/ ergs/°K mole), and
T= °K.

Most pores in foods are in the 10-300 um range. Assuming complete wetting

6
(cos@ = 1) and pure water (Ys = 72.3 dyne/cm) in the pores, the Kelvin
equation predicts an ay in the range of 0.989-0.9999. Thus, the ay is
lowered very litle by capillarity. However, 5-7% of the pore volume in foods
is for pores of 0.01-0.001 um, which lowers the ay above the vapor space to
values of 0.899-0.34. Thus, smaller capillaries have a greater effect on
lowering the ay, and those of small diameter will be the last to empty on
drying. Thus, capillary effects will occur over the whole isotherm. In terms
of water binding, this phenomenon is used successfully in the Bauman device to
measure water uptake of gums, fibers, and starches (Wallingford and Labuza,
1983; Rasper and Deman, 1979; Hermannson, 1972). Note that materials that
swell will take up more water because the pore space increases. Yet the ay
will be higher according to the Kelvin equation. This means that the water is
less tightly bound on the average as moisture content increases (a,>1.0).
The ideal ingredient would have a high moisture content at lower ay.

3. Surface interaction
Finally, water directly interacts with other chemical groups on molecules
through dipole-dipole forces, ionic bonds (H30t or OH~), van der Walls
forces (hydrophobic bond), and the hydrogen bond. These water molecules, so
bound, require extra energy to be transferred from the liquid into the vapor
state and thus are less free to the vapor, resulting in reduced a,, This
effect also occurs over the whole isotherm but is more pronounced at low ay.
Of criticai importance is the monolayer value. This is the moisture content
at which each polar and ionic group has a water molecule bound to it, to form
the start of a liquidlike phase. Generally, reactions below this moisture
content that depend on water as a reaction phase medium do not occur at
appreciable rates. The monolayer moisture content can be found from the
isotherm using the BET method, which is a mathematical model of the sorption
isotherm. A calculation will be given later.
All three of these major factors (Raoult's effect, Kelvin effect, and
direct bonding) occur over the whole moisture range for a food and result in
the characteristic moisture sorption isotherm. One really should not attempt
to distinguish the isotherm shape by these three mechanisms. For more
in-depth analysis, a surface chemistry book (such as Adamson, 1962) should be
reviewed.
II. Typical Sorption Isotherms

A. General Curve

Figure 4 shows the typical curve for equilibrium moisture content (m, in
grams of water per gram of solids) vs aw (or % ERH) that would apply to most
food systems and indicates the range where a particular food would fit. In
general, dehydrated foods have equilibrium ay's of less than 0.6; semimoist
foods, such as cereal grains, raisins, dates, syrups, and intermediate—
moisture pet foods usually have an aw between 0.62 and 0.92; and cheeses,
jams, jellies, meat, fish, etc., have a,'s greater than 0.92. Note in
Figure 4 that the ay does not begin to decrease much below 0.99 until the
moisture content is reduced to 1 g of H20 per gram of solid (50% wb). The
lowering of ay or moisture can be accomplished by drying, by adding
humectants that reduce the ay, through the effects of Raoult's law, or by
adding dry ingredients such as starch, gums, or fibers, which interact with
the water by the various mechanisms discussed earlier. Note that the isotherm
curve can be constructed either by an absorption process (starting from the
dry state) or by a desorption process (starting from the initial wet state).
Sometimes different curves are found. This phonomenon of different a,-vs-—
moisture values by the two methods is called moisture sorption hysteresis and
indicates some type of nonequilibrium.

B. Specific Curves--Lower a, Range

Of specific concern to most processing operations is the a, range below

0.95. The general moisture sorption isotherm for this range is represented in
Figure 5.
Most foods, such as cereals, follow the sigma-shaped curve represented as
a type II isotherm. The resultant curve is caused by the additive effects of

& Tissue Foods

cheese, sausage, candy

grains
syrups

Typical Isotherm
(lower region)

gH20
solids
100g

Water
—-
—>
Activity
dw
—>
esse
Yer
0> ik
| 2
Moisture Content(g H,O/g dry solids)
Figure 4. Typical moisture equilibrium vs water activity for foods. Insert
shows m vs ay isotherm.
Raoult's law, capillary effects, and surface-H90 interactions. Two bends
are noted, one around an ay of 0.2-0.4 and another at 0.6-0.7. These are
the result of the changes in magnitude of the separate physical-che
mical
effects.
The type I isotherm, an adsorption isotherm for pure crystalline sugar,
shows very little moisture gain until the ay goes above 0./7-0.8. This is
because the only effect of water is hydrogen-bonding to the -OH groups
that
stick out on the surface of the crystal (Figure 6). Since this is a surface

ze Tyee DL
w
Q
Ln)
-
}
wn
o
©
©
Ss
o

ie
saa

iw
2
S aye &
Ww
w
2
=
L
Tyee L
°
on |

=
8 i.) ~ .a w o 8
8 —

WATER ACTIVITY
Figure 5. Classification of standard moisture sorption isotherms. Type I,
crystalline substances; type II, dehydrated foods; type III, anticaking
agents.

ak
O::
7
H

©
1H
H

Figure 6. Surface adsorption of water on crystalline material such as

SUCTOSC.>
effect, grinding the sugar to smaller particles will increase the moisture
content at the low a,'s by the amount of surface increase. Thus,
for true crystalline materials, specificationof sieve size is important for
water content as a function of ay.
At low a,, the dielectric effect of water is not strong enough to break
the interactive forces between individual sugar molecules. However, as the
a, is increased, the overall net water-sugar interaction is enough to cause
sugar-sugar dissociation, and thus water begins to penetrate into the crystal,
dissolving sugar molecules and exposing new surface. At that point, the
moisture content rises dramatically because a solution is being created. The
ay at the beginning point of solution generally corresponds to the ay of a
saturated solution and is where the Raoult's law effect begins to occur.
The type III isotherm is typical of anticaking agents. This type of
ingredient also adsorbs water onto specific sites, but the binding energy is
very large, thus depressing the a, dramatically. That is why in Figure 5
the isotherm shows a sharp vertical rise at low aye When all the binding
sites are filled (as well as any narrow capillaries), any increase in moisture
content causes a large ay increase. This is because the material does not
dissolve, so the added water interacts only with the water already present,
through a weak hydrogen-bond, and a surface solution begins to occur.

C. Hysteresis

As mentioned previously, the moisture sorption curve can be generated from

an adsorption process (starting with a dry system in which ay = 0) or a
desorption process (starting with a wet system in which a, = 1.0). The
typical curves (shown in Figure 7 for a food product) result, with more water
being held at the same a, for the desorption curve than for the absorption
curve above and below some closure points. Hysteresis is, in fact, a
thermodynamic impossibility, since yy 0 (or a,) is a state function, and
thus the same composition and water content should always occur at a given

ADSORPTION
PESO LON, —-—>

LURE,
MOUS
TEN:
CON

Figure 7. Adsorption-desorption hysteresis loop, showing paths taken by: a dry

food during sorption (A), a sample prepared by adsorption to an intermediate
level (B), and a sample prepared by desorption (C).

10
aye The reasons for the differences in moisture content between the two
closure points are: 1) during drying (desorption) some solutes may
Supersaturate below their crystallization ay and thus would hold more water
as ay is lowered (Figure 8). Foods with high sugar content usually exhibit
this, as seen in Figure 9 for dry apple slices. The high moisture at zero
ay for desorption suggests that the moisture method did not supply enough
energy to get to m= 0 g H20/g solids, as it should, since theoretically the
isotherms should join near an ay Of 0.1-0.3; 2) capillaries can empty
differently upon desorption, i.e., narrow ends of surface pores will trap and
hold water internally below the a, where it should have been released--while

MOISTURE

SUPERSATURATION

INTO SOLUTION

WAVER ACTIVITY

Figure 8. Sorption hysteresis effect as caused by supersaturation of sugars.

35

30F @- ADSORPTION
A - DESORPTION
25

%0 0.1 O20 805) .047705: O6 ..07 -.O8.-..09

Ow
Figure 9. Water vapor sorption hysteresis in dried apple slices. (Isotherm
drawn from data of Wolf et al, 1972)

11
on adsorption, the narrow end prevents the larger body from filling; 3) the
surface tension,y,, and the wetting angle, 6, from the Kelvin equation
differ for adsorption and desorption, resulting in a higher moisture content
for desorption.
Hysteresis has some practical aspects. Obviously, if a moist, low-a,
product is desired, a large desorption hysteresis would be of benefit (iseus
there would be more water at the same ay). However, as seen in Figure 10 at
the same a,, the higher moisture system (desorption) also results in a
greater loss rate for chemical reaction, which can be undesirable.
Finally, there is the question of which isotherm direction would be
followed for a food product that is subjected to moisture change but does not
start out at zero moisture. It should be expected that if the initial ay is
at or below the monolayer (point A in Figure 7), then the adsorption isotherm
will be followed as it picks up moisture. However, if the initial moisture
content lies somewhere between the monolayer and the isotherm upper closure
point, upon desorption the curve that would be followed would depend on how
the product was first made. If the product was first dried to below the lower
closure point and then water was added to get to the initial value (point B),
any further gain or loss of moisture should be on the adsorption isotherm.
However, if the product was initially made by drying down to the wetted state
(point C), then on further drying the desorption curve would be followed, but
on rehumidification the product would begin to shift over to the adsorption

1,00

0.50

Oo iS

(e)oO oi
(day~')
k

OF
LOSS
C
RATE
VITAMIN

0.01

0.2 04 0.6 0.8 1.0

Figure 10. Rate of loss of vitamin C as a function of temperature, water

Fe sate and sorption hysteresis. (Drawn from data in Waletzko and Labuza,
1976

12
isotherm, represented by the dotted line in Figure 7. This latter phenomenon,
which includes a crossover between the desorption and adsorption curves, is,
in reality, the true “working isotherm" for most dried, baked, or extruded
food products, since they are usually dried to some level and then subjected
to either moistue gain or loss. d

D. Amorphous-Crystalline Transfer

As noted, low-molecular-weight carbohydrates (sugars such as lactose,

sucrose, fructose, etc.) present special problems in sorption studies. If one
dries a sugar solution below its saturation point, an amorphous solid glass
(noncrystalline) is usually formed. This solid material, if put through an
adsorption experiment, holds more water than does a crystalline solid of the
same material, as shown by the moisture sorption isotherms of the two systems
(Figure 11). This is because the amorphous noncrystalline material can
hydrogen-bond water internally, not just on the surface. However, another
factor comes into play. As the ay increases, the molecules of the sugar in
the amorphous solid become more mobile in the internal water phase.
Eventually the molecules collide, and formation of a crystal nucleus is
possible. After that, the whole matrix begins to recrystallize, expelling the
water into the environment around it. This increases the ay because the
solid is becoming more crystalline, as shown in Figure 12, in which X-ray
diffraction was used to measure the crystallinity increase of amorphous
sucrose held at 24°C/30% RH (Makower and Dye, 1956). As noted, it takes about
28 days for this to occur. For reference, Figures 13 and 14 represent
adsorption curves from the same study for sucrose and glucose at 24°C and
different % RH's maintained over the solid. The overall consequence is that
crystalline bridges form and water is expelled out of the solid. This means
that for any food ingredient that contains amorphous-form sugars (such as dry
whey, nonfat dry milk, dried fruit powders, tomato powder, or dried flavors),
the moisture sorption isotherm will be time-dependent, as indicated in Figure
ys

Crystalline Non-Crystalline
XXX O OS ee

COC S omer sae:

AMORPHOUS.

Moisture

dw dw
Figure 11. Moisture sorption isotherms of pure crystalline and noncrystalline
food systems.

|
 The amorphous material shows a Type II isotherm at week 1, but after one
month at the intermediate ay's, the recrystallization begins, bringing the
isotherm closer to the true crystal curve.

2 100
(a0)
Q

> ro
= 80 9
80 Sucrose
5
os

SOF ie
3m 40
B4
Q0 KX

WW

= Crystallinity —— 20

DAYS

Figure 12. Effect of exposure of amorphous sucrose at 30% RH and 24°C on

moisture content and degree of crystallinity. (Drawn from data of Makower and
Dye, 1956)

24.0 %R.H.
yo NS2 es R.H,

ene
ae
— OO)
O O

BASIS)
(DRY
WATER
PERCENT b4 ve 4.8% RH.
mee eal
Toxo) 150 200 O 400 600
SOOM SOCOM aOO
EXPOSURE TIME ( DAYS )

Figure 13. Adsorption of water vapor by amorphous sucrose at various relative

humidities. (Drawn from data of Makower and Dye, 1956)

14
 Obviously, then, one does not have true equilibrium when physical states
are changing over time. This complicates the interpretation of the true
sorption isotherm.

8.6 YR.H.
——
4.6% RH.

(DRY
BASIS)
WATER
PERCENT

200 400 600 800

EXPOSURE TIME (DAYS)

Figure 14. Adsorption of water vapor by amorphous glucose at various relative

humidities. (Drawn from data of Makower and Dye, 1956)

portal
crustaliwe
<= Gat)

Crmerth)
oe Amorphous

MOISTURE
CONTENT
SOLIDS
g/1@@g

WATER ACTIVITY

Figure 15. Water vapor sorption progress of amorphous and crystalline

solids.

15
E. Temperature Effect

In describing a moisture sorption isotherm, one must specify the

temperature and hold it constant. Because of the nature of water binding, at
constant a,, foods that follow a Type II isotherm (Figure 16) hold less
water at higher temperatures than at lower ones.
The effect of T follows the Clausius Clayperon equation:

ag Q 1
i, = ee fe mS al (10)

where:
a2 = water activity at temperature T2 aK
aj = water activity at temperature T, °K,
Qs = heat of sorption in cal/mole (function of moisture content), and
R = 1.987 cal/mole °K .

Qs, which is the excess binding energy for removal of the water, is the only
unknown and, unfortunately, there are no standard tables of Q, for different
foods. Therefore, to predict the ay of a food at any given temperature,
moisture sorption isotherms must be determined for at least two temperatures.
Then a plot of log a, vs 1/T °K will give a straight line at constant
moisture content, as seen in Figure 17, and the ay at any temperature for
that moisture can be found. The slope of the line (Q,/R) decreases to zero
as moisture content increases. This is indicative of reduced water
interactions (less binding energy).
In general, the effect of temperature on increasing the ay at constant
moisture content is greatest at lower to intermediate water activities. As
seen in Figure 16, ay increases as T increases for a constant moisture

CONTENT
MOISTURE
SOLIDS
g/1@8g

WATER ACTIVITY
Figure 16. Effect of temperature on moisture sorption of foods.

16
 content. As a practical example, the following data have been collected for
_the moisture vs % ERH values of Sinton wheat.

Relationship between moisture content and equilibrium relative humidity of

Sinton wheat:

Moisture Content Relative Humidity, % Ms!

Wet-Weight Basis Dry Basis Desorption Adsorption
(4) (g/100 g) DIG) aleCie 25° Cee -5°C slo Oe occ
2 9.89 26.7 20D = 32.5 31.0 34.0 36.0
10 1 ee i 3320) ~ 36.0 39.0 37.0 40.0 42.5
b2 13.64 47.0 50.0 54.5 D020 — (5329 760
14 16.28 61.5 64.0 68.0 64.0 66.7 ‘69.5
16 19.05 VW2eD oO THD © Lies 74.0 76.5 78.0
18 2195 Skso ~ S3s02 $4.5 82.38 = 83.5 S405
20 25.00 $3.0 -89.0- 89.5 88.5 89.07 8955
22 26021 92s0)- 59265. 92.5 9265) 926 eee
24 6 ers) 94.0 94.0 94.0 94.0 94.0 94.0

As an illustration of both hysteresis and the temperature effect, we can

plot the adsorption and desorption isotherms (dry-basis moisture versus a,)
for each temperature, as shown in Figures 18-20. For a given moisture
content, to determine the a, at any temperature we need to determine the
Qs, for that moisture. The following are the calculations for Q, at 10,
15, and 20 g H20/100 g solids.

In(
ACTIVITY)

/ ean?

Lae
Figure 17. Plot of log aw vs temperature for predicting awe

17
Sinton wheat--Calculation of heat of sorption:

Moisture content from isotherms

(g H0/100 g solids) 5°C 15°C Yds ©
10 0.30 0.34 05365
1Ws 0.58 OF6L 0.64
20 0.79 0.80 0.82
Lf Tok 3.595 x 1073 S347 3 0s" 3.354 x 1073

Pa = =Us De - il
a] R Ati, ET

Qs _ 263 log(az/aj)
R =e
T2 Ty

-R In(ap/a)) = 1.987 -1n(ag/aj) 42576 sLogCap/ay)

NS Se re Sey ES

ae arene beari
T2 T] T2 ry 1s) T]

Therefore:
at 20 g H20/100 g, Q, = 216 cal/mole,
at 15 g H720/100 g, Qg = 967 cal/mole, and
at 10 g H70/100 g, Q,g = 1,838 cal/mole.

CONTENT
MOISTURE
SOLIDS
g719@g

WATER ACTIVITY
Figure 18. Moisture adsorption and desorption isotherm for Sinton wheat at
SC.

18
 SOLIDS
g/7188g
CONTENT
MOISTURE
J 9
a o
-28

WATER ACTIVITY

Figure 19. Moisture adsorption and desorption isotherm for Sinton wheat at
15°C.

~wuw
re)
rr)

n8

MOISTURE
CONTENT
g/719@g
SOLIDS

WATER ACTIVITY

Figure 20. Moisture adsorption and desorption isotherm for Sinton wheat at
25-C.

Be
 As seen, Q, increases with decreasing moisture content, indicating a
stronger interaction energy. The plot of In a, vs 1/T, shown in Figure 21,
indicates the straight lines with a slope of Q,/R at constant moisture
content. We could use the lines to predict what would happen to the a, of a
product that was packaged at 25°C and 10 g H70/100 g solids and then was
transferred to 45°C, assuming no moisture gain or loss. The value could be
taken from the line, if extended, or could be calculated as follows:

At 10 g Hy0/100 g, Q, = 1,838 and a; = 0.365

For 45°C, 1/Tp = 3.143 x 1073; for 25°C, 1/T, = 3.354 x 1073 .

Thus,

a a -1838
ele in|| = [pag] 2-349 x 10° B03 S54e On|
ay 0.365 1.987

ay = 0.365e9°195 = (0,365) * (1.2155)

miei cs
Thus, the a, could increase to 0.44 if the food were brought to 45°C.
If this were the critical a, at which caking could start, the temperature
change would be a substantial problem.

WATER
ACTIVITY
i]
In

177K x1@°
Figure 21. Clausius-Clayperon plot of In ay VS reciprocal absolute
temperature for Sinton wheat.

20
F. Total Pressure Effect

Pressure also has an effect on the water activity of a food system, but
the effect is small. From thermodynamics, a change in total pressure of the
System will affect the vapor pressure. At equilibrium, any change in the
chemical potential of the liquid state will equal the change in chemical
potential of the vapor. Thus:

dyy, = V,dpr = du, = Vydpy ( 1 1)

where:
Vi, = molar volume of liquid,
V, = molar volume of vapor,
dpr = total pressure change, and
dp, = vapor pressure change,

then V. Vv
Saige Cac bingenl h (12)
dpy ies Ripe

Thus: Vv.
2 Sivas ee Lys (13)
Py eure

and:
ag Vi
ln a, a RT [Po oe Py] ’ (14)

where P); and Py are total pressures in mmHg for initial and final
pressure, respectively.
At 30°C, then:

tee
al [19.6 x07 | IP 2 e PIarse (15)

Thus, a sample equilibrated to 0.4 a, at sea level (760 mmHg) and brought to
Denver (570 mmHg) will have a decreased a, equal to:

ag =~ 0.9998 aj = 0.3999. (16)

As can be seen, the decrease is negligible and probably cannot be measured.

At higher pressures, such as occur in an extruder, the a, can be
significantly increased. If the moisture isotherm as a function of
temperature is known and equations 10 and 15 are used, one can predict the
increase in water activity in the extruder, assuming that the moisture content
does not change. For example, at 4,000 psi, which is used for extrusion of
some semimoist foods, a dough at 0.8 a, will increase by 1.22 times to an
a, of 0.976. What consequences this has on reaction rates and stability is
unknown and should be investigated.

Zi
III. Use of the Moisture Sorption Isotherm

The moisture sorption isotherm is an extremely valuable tool for the food
scientist because it can be used to predict potential changes in food
stability; it can be used for packaging selection and for ingredient
selection. In the section that follows, a few of the practical uses of the
isotherm are presented.

A. Monolayer Stability Value

1. Usefulness of the monolayer value

Studies of the rates of chemical reactions in foods have shown that for
most dry foods there is a moisture content below which the rates of quality
loss are negligible. This moisture content corresponds to the monolayer value
(m,), as determined from the BET isotherm equation, and is generally around
an a, of 0.2-0.4. Figure 22 represents typical findings, in which the rate
of quality loss begins to increase above a, = 0.3 for most chemical
reactions. At this a,, the amount of water adsorbed on surfaces and in
capillaries is enough to affect the overall dielectric properties such that
the water can now behave as a solvent. Thus, chemical species can dissolve,
become mobile, and react. The higher the a,, the faster the reaction rate
because of the greater solubility and increased mobility. However, at some
higher a, no more species dissolve and therefore an increase in ay
decreases the concentration of the reacting species. Since the rate of a
reaction is proportional to concentration on a molecular basis, the rate
should reach a maximum and then fall as shown. Between this maximum and the
monolayer, a semiplot of the ln rate (or rate constant, or shelf life) vs ay
generally results in a straight line, as shown in Figure 23. For most dry
foods, an increase in a, by 0.1 unit in this region decreases shelf life two
to three times.

Rate
Relative
———e
x
0.1.0.2 03 0.405 06 0708 09 10
Ow
Figure 22. Effect of a, on typical food deteriorative reactions. ce
represents lipid oxidation. II represents most other reactions, such as
nonenzymatic browning.

22
 Figure 22 also showed one other factor, that is, quality loss below the
monolayer value. If a food is susceptible to oxidation of unsaturated fats,
such as occurs in cereal grains, the rate increases as ay decreases. Thus,
since most foods contain some unsaturated fat, manufacturing the food to the
BET monolayer value (mj) and keeping it there will maximize shelf life.
This BET value can be viewed as a critical moisture content or critical ay
value.

2. BET monolayer calculation

The general equation for the BET isotherm model is:
a = —-
1
+ dd ———
en)
(1-a)m Migc Mpc : ey

where:
m = moisture content (db) at water activity a and temperature T,
c = constant, and
Mo = monolayer value.

This equation can be rearranged to give:

a
GBA oe I+Sea (18)

where I = intercept and S = slope. Thus, a plot of a/(l-a)m vs a gives a

straight line. Then the monolayer value from this plot is:

ea . (19)

ACTIVITY
WATER

- N m r wn wnra@eane i) e @ @aaeeda”d
- ta) rw wROM
SHELF LIFE (WEEKS)

Figure 23. Relationship of log (shelf life) to a,,

Z3
 As an example of a BET monolayer calculation, the following data are for a
dry cracker. The value of a/(l-a)m for each a/m data pair appears in the
third column.

Dry cracker at 25°C:

a m (g H90/100 g solids) a/(l-a)m

0.11 3.58 0.0345
0.22 5.09 0.0554
0203 6.67 0.0738
0.44 7.34 0.1070
0.54 Sie 1 0.1348
0.64 Erett 0.1600

Using linear regression for the plot of a/(l-a)m vs a, we find:

for ay 0.11-0.44, r2 = 0.981, I = 0.0087, S = 0.2145, mo = 4.479;

for a, 0.11-0.54, r2 jo) \o oe)1S) HH e 0.0047, S = 0.2331, m, = 4.205;
for a, 0.11-0.64, r2 oil "oil020026; S*="072412 "my = 3-8 rue

Figure 24 shows the visual plot of the data. Using solely eyeball
techniques, we find:

I = 0.0125, S = 0.1980, and m = 4.75, ag = 02185.

The above calculations and the visual plot in Figure 24 demonstrate some
interesting conclusions. The BET mp value achieved by visual plotting,
using only a, values up to 0.44 (generally ay values above 0.45-0.5 are
precluded because the equation theoretically is not applicable above this

-28

aZ(l-a)dm

WATER ACTIVITY
Figure 24. BET monolayer plot for sorption data of a dry cracker.

24
range), gives an a) of 0.185. The use of regression analysis for values up
to the same range gives an m, of 4.479 and an ag of 0.170. These two
ay Values differ, but not by much. In fact, most a, measurement
techniques are only good to + 0.02 units, which is about this difference. A
moisture difference of 0.27 g per 100 g of solids is also a small difference
and within normal error. Thus, use of a visual plot is as acceptable as
standard linear regression by least squares. However, when a wider range of
ay's is used in the equations, the r2 (coefficient of determination)
increases, even though the equation is theoretically not applicable. It is
suggested that if four a, values below 0.45 are available, then only those
be used to calculate mj); otherwise the data point at ay = 0.54 should also
be included. For example, the data presented earlier (p. 17) for Sinton wheat
does not have enough points below an a, of 0.45, and thus higher ay points
are needed, as shown below. (Note that adsorption--not desorption--data
should be used.)

BET - adsorption data for Sinton wheat:

m (g H20/100 g solids) or a/(l-a)m

9.89 G3 0.0454 r2 = 0.997
Psi 0.37 0.0529
Sec 13.64 0.50 0.0733 Mp* = 6.79
t6.28 0.64 0.109

9.89 =" 0234 0.0521 r2 = 0.996

fist 0.40 0.060
sexe 13.64 0.535 0.0844 mo* = 6.171
16.28 0.667 0.1230

9.89 0.36 0.0569 r2 = 0.994

25°C Piet 0.425 0.0665
13.64 0.57 0.0972 Mo* = 5.54

*g H20/100 g solids.

Table 1 presents some calculated BET monolayer moisture values for various
foods.

B. Crispness/Hardness

The crispness of dry, cereal-based foods (e.g., crackers, RTE's, fried

snacks, and chips) is a strong function of a,, as was found by Katz and
Labuza (1981). Figure 25 shows the decrease in crispness intensity of saltine
crackers as a function of ay. At an ay of 0.4-0.45, the cracker loses
desirable crispness. In fact, for most cereal-based products, significant
loss of crispness occurs in this ay range. Thus, the moisture sorption
isotherm can be used to predict the critical moisture content or aw above
which the product should not go during distribution. The reasons for loss of
crispness have not been thoroughly explained but may be caused partially by
changes in the rate at which the starch molecules can slip past each other and

ZD
 TABLE 1
Monolayer Values of Dehydrated Foods

Food Mo (g H20/100 g solids)

Beans eel
Cocoa
Coffee
Cheese (dried)
Chicken
Egg
Egg albumin fon e wn
Fish
Gelatin e

Lima bean |©
NWDHM
Meat !
e
e606. e

Milk (dried whole) OV

—
Milk (instant) ee

Peas >

Potato | ~S e oe)

Potato starch
Raspberry
Rhubarb
Starch
Strawberry Ww
©
UMN
wFUD
FUN
FOMndWnwWwuUr
oe
Corer
FWO
DNNOWNOO™NeH
WR
SDNR

o- —_—_ VERY CRS 2

° _MODERATELY _CRISP.
INTENSITY

SLIGHTLY
CRISPNESS _CRISP_

0.2 06 08

Figure 25. Sensory crispness intensity as a function of

water activity for
dry saltine crackers. (Data plotted from Katz and Labuza, 1981)

26
 4)

partially by the decrease in the velocity and intensity of sound waves as

_moisture content increases. ano
Hardness, on the other hand, is a problem with semimoist foods such as
pet foods or fruit pieces. Not enough data exist to predict a lower critical
ayy for hardness because this critical a, depends on product composition.
Fat and glycols, for example, can lower the critical a, for the products
ence are in. For most semimoist foods, the critical a, Will be around
-5-0.6.

C. Caking
The amorphous-crystalline state transfer was explained earlier with
respect to a,. In general, for most foods high in amorphous-state sugars,
the rate of phase change during storage will become significant at room
temperature if the product gains moisture to above a critical a, of 0.4,
where sufficient water is available to mobilize the sugar molecules. If this
occurs in a sealed package (the amorphous sugar picks up the moisture by
transfer from other ingredients while equilibrium is being achieved) or
through the semipermeable film, bridges between the sugars will occur,
resulting in a plastic, caked mass. The released water is then picked up by
the other ingredients, causing an overall ay increase and an increase in
degradation rates. Thus, to predict the extent of this problem, knowledge of
the curve of a, vs moisture content for each ingredient is required. Very
little data exist on the rate of this transfer in engineered foods.

D. Microbiology

A critical a, also exists below which no microorganisms can grow. For

most foods, this is in the 0.6-0.7 a, range. Thus, with knowledge of the
moisture sorption isotherm, one can predict the maximum moisture that the food
can be allowed to gain during storage. Of course, higher ay' Ss can be
allowed if other factors such as pH, salt, antimicrobial agents, and
temperature are taken into consideration. Table 2 lists the minimum a, for
growth and toxin production by pathogens, and Table 3 lists the typical a,
range for microbes that can spoil foods (for more details, see Beuchat, 1981).

E. Packaging Predictions

1. Theoretical considerations
The above discussion presented some typical critical a,"s that can be
used to determine a maximum allowable moisture gain or loss from the initial
state. The moisture sorption isotherm can also be used to determine this
critical moisture content. Fairly simple equations have been derived to
estimate the gain or loss of moisture for a food held in a semipermeable
package. (For a review, see Labuza and Contreras Medellin, 1981.) Note that
these equations could also be used to predict change in weight from the legal
net weight. For moisture gain, then:

De - m ki A p (20)
Ink = In = =a 2-294
Me - m x awe. D

yal
 TABLE 2
Minimal ay Limits for Some Microorganisms
of Significance to Public Health

e
a a S Eee

Microorganism Minimal a, for

Growth Toxin Production
eee ee I ee ee eS eee

Aspergillus clavatus 0.85 0.99 (patulin)

A. flavus 0.78-0.80 0.83-0.87
A. ochraceus 0.77-0.83 0.83-0.87
road (ochratoxin)
A. ochraceus 0.70-0.81 0.80-0.88
a (penicillic acid)
A. parasiticus 0.82 0.87 (aflatoxin)
Bacillus cereus 0.93-0.95
Byssochlamys nivea 0.84
Clostridium botulinum 0.93(A)-0.95(A) 0.94-0.95(A)
0.93-0.94(B) 0.94(B)
0.95(E)-0.97(E) 0.97(E)
Clostridium perfringens 0.93-0.95
Penicillium cyclopium 0.82-0.87 0.97 (penicillic acid)
P. cyclopium 0.81-0.85 0.8/7-0.90
(ochratoxin)
P. expansum 0.83-0.85 0.99 (patulin)
P. islandicum 0.83
P. martensii O3/9=0.65 0.99
(penicillic acid)
P. patulum 0.81-0.85 0.85-0.95
(patulin)
P. viridicatum 0.83 0.83-0.86
(ochratoxin)
Salmonella spp. 0.92-0.95
Stachybotrys atra 0.94 0.94
(stachybotryn)
Staphylococcus aureus 0.86 0.87-0.90
(enterotoxin A)
0.97 (enterotoxin B)
Trichothecium roseum 0.90
Vibrio parahaemolyticus 0.94

*Derived from Beuchat (1981).

28
 TABLE 3

Water Activity of Some Foods and Susceptibility

to Spoilage by Microorganisms*
eee an 9 Cate oe PE ee eet
_ Microorganisms generally inhibited Examples of foods generally
Range of ay by lowest ay in this range within this range of ay

1.00 - 0.95 Pseudomonas, Escherichia, Proteus, Highly perishable foods (fresh

Shigella, Klebsiella, Bacillus, and canned fruits, vegetables,
Clostridium perfringens, some meat, fish) and milk; cooked
yeasts sausages and breads; foods
containing up to ca. 40% (w/w)
sucrose or 7% NaCl

0.95 - 0.91 Salmonella, Vibrio parahaemolyticus, Some cheeses (Cheddar, Swiss,

C. botulinum, Serratia, Lactobacillus, Muenster, Provolone), cured
Pediococcus, some molds, Rhodotorula, meat (ham), some fruit juice
Pichia concentrates; foods containing
55Z (w/w) sucrose or 12% NaCl

0.91 - 0.87 Many yeasts (Candida, Torulopsis, Fermented sausage (salami), sponge
Hansenula), Micrococcus cakes, dry cheeses, margarine;
foods containing 65% (w/w) sucrose
(saturated) or 15% NaCl

0.87 - 0.80 Most molds (mycotoxigenic penicillia), Most fruit juice concentrates,
Staphylococcus auréus, most Saccharo- sweetened condensed milk, choco-
myces (baillii) spp., Debaryomyces late syrup, maple and fruit syrups,
flour, rice, pulses containing
15-17% moisture; fruit cake;
country style ham, fondants,
high- sugar cakes

O5805—" 0275 Most halophilic bacteria, myco- Jam, marmalade, marzipan, glace
toxigenic aspergilli fruits, some marshmallows

Os Us) = Oss Xerophilic molds (Aspergillus cheva- Rolled oats containing ca. 10%
lieri,A. candidus, Wallemia sebi), moisture, grained nougats, fudge,
Saccharomyces bisporus marshmallows, jelly, molasses, raw
cane sugar, some dried fruits, nuts

0.65 - 0.60 Osmophilic yeasts (Saccharomyces Dried fruits containing 15-20%

rouxii), few molds (Aspergillus moisture; some toffees and
echinulatus, Monascus bisporus) caramels, honey

0.50} Noodles, spaghetti, etc. containing

} ca. 12% moisture; spices containing
} ca. 10% moisture
}
0.40} Whole egg powder containing
} No microbial proliferation ca. 5% moisture
}
0.30} Cookies, crackers, bread crusts,
} etc. containing 3-5% moisture
}
0.20} Whole milk powder containing 2-3%
moisture; dried vegetables con-
taining ca. 5% moisture; corn
flakes containing ca. 5% moisture;
dehydrated soups; some cookies,
crackers
Se

*Adapted from Beuchat (1981).

29
where:
[ = unaccomplished moisture ratio, sometimes called gamma,
M, = the moisture content on the isotherm that is in equilibrium with
the external temperature and humidity (g H20/g solids), based on
the straight line approximation,
mj = initial moisture content (db),
m = moisture content (db) found at timeO@,

= film permeability in g H70/day m2 mmnlg,

A = package area (m2),

Ws = weight of dry solids (g),
Po = vapor pressure of pure water at temperature T, in mmHg, and
b = isotherm slope in g H70/g solids per a, unit.

The moisture sorption isotherm is used for two values in this equation:
1) the equilibrium moisture content (mg) and 2) the slope of the line (b)
representing the isotherm. The solution is based on the moisture content
traversing the “working isotherm," which is represented by a straight line
equation and the dashed line in Figure 26.
Note that: PE ad par ae aa (21a)

Maes (Ded autac (21b)

where: b = slope in g H,0/g solid,
c = intercept,
m, iS = equilibrium value from the assumed straight
line determined at the external % RH (a, = % RH + 100).

Obviously, the isotherm must be for the temperature at which the moisture
gain is predicted. In the real world, we generally don't know the external
conditions. However, the equation can be used to predict the gain or loss
under extreme abuse conditions. The equation for loss is similar to equation
20 and is:

>
InI = In [Zaz |= bs so Pog (22)
a WS =D

where I‘ is the unaccomplished moisture content, m; is initial moisture, m,

is equilibrium moisture, k/x is the film permeance in g H)0/day m2 mmHg, A
is the area of the package, p, is the vapor pressure of pure water at the
temperature of the test (not Pout» the actual vapor pressure outside the
package, but py, the saturation vapor pressure), b is the moisture sorption
isotherm slope, and m is the moisture content at any time@. A plot of 1nI vs
O will give a straight line, and a plot of m vs © shows a curved line. This
curvature is because the driving force for moisture gain decreases as moisture
is picked up (internal vapor pressure increases).

2. Sample calculation: Moisture gain to critical a, for loss of crispness

of potato chips
The chips, which become organoleptically unacceptable at a, = 0.45, were
stored in mylar and polyethylene bags at an abuse condition of 35°C/100% RH
and showed the following moisture gains.

30
Moisture gain for chips in pouches held at 35°C, 100% RH:

Time _____ Package Weight in Grams*

(days) Polyethylene Mylar
A B A B
0 11.84 13.42 10.00 9.58
1.93 12.02 13.61 10.27 9.83
3.76 12.09 13.69 10.38 9.91
5.7/8 12.22 13.84 10.5 10.07
7.66 12.23 13.87 10.56 10.08
9.99 12.32 13.95 10.66 10.17

Bag alone, g 3.22 3e22 0.92 0.92

Total area
of both sides, m2 0.02908 0.02904 0.03017 0.0264

*Sealed with chips at mj = 1 g H20/100 g solids.

To solve the problem, we need to know the film permeabilities. These were
reported in the industrial literature as follows:

Dupont polyethylene 300-A: WVIR = 9.3 g/m2 day at 100°F/90% RH

(ASTM-E96)

Dupont mylar 50-H24: WVTR = 17 g/m2 day at Dupont condition

39.5°C/90% RH

MOISTURE
CONTENT
SOLIDS
g/718@g

WATER ACTIVITY

Figure 26. Working moisture isotherm for use in solutions of packaging

predictions, superimposed on true isotherm. Dotted lines represent the
initial (mj), critical (mg), and equilibrium (mg) moisture limits.

31
 Note that the permeabilities are in water vapor transmission rate (WVTR)
units and must be converted to k/x to solve the equation. For the
polyethylene, the WVIR test was reportedly done at 100°F/90% RH, which gives
an external water vapor pressure (Ppoyt) of 49.2 (po value at 10078) x<059
(%4 RH +100), or 44.28 mmHg. The WVTR test (ASTME-96) is done by sealing the
film over dry desiccant in a special test cup. Thus the water vapor pressure
inside (pin) is zero. The driving force for moisture transfer across the
film to the desiccant is constant, and the rate of gain of moisture is:

AW g H20 k
= = A [Pout - Pin! (23)
AO day

for Poyt constant and pj, = 0. Then:

AW k
x

where Poyt is the outside vapor pressure. WVIR is defined in g H20/day

m“ so:
AW
igo (WVTR) A , (255

which is the slope of weight gain vs time for the straight-line portion of the
test data. WVTR is the slope Aw/AO divided by the package area. Thus,

x Pout (A) Pout ;

Therefore, for the given conditions for polyethylene:

ee = 0.21 g H90/day m2 mmHg .

— —~N

|
x

Since actual values of k/x can vary because of film stretching, end seals,
etc., it is best to do actual measurements using bags suspended over a vapor
source. The bags are filled with desiccant, sealed, and then weighed
periodically for up to 7 days. The results of such a study at 35°C/100% RH
(Pout = 42-2 mmHg) are in the following data table.

32
Weight (g) of bags with desiccant in storage at 35°C/100% RH:

Polyethylene (P) Mylar (M)

Time (hr) A B A B
0 81.45 85.06 83.24 83.01
28.5 81.59 85.19 83.42 83.20
AJ ee 81.63 85.20 83.44 Sonez
70.75 81.65 85.26 83.56 83.38
97.00 8) 7d 85.40 83577 837
Wa 81.80 85.48 83.84 83.65
143.6 81.93 85.56 84.04 83.85
167.0 81.95 S5.52 84.14 83.96

Bag size (cm) inside seal:

PA —- [11.7 x 10.95] x 2 2.56 x 1072 m2

PBRo— [10.9 xv11.55] x-2- = 2452 -« 1072 m2
MA - [10.9 x 11.9] x2 = 2.59 x 1072 m2
MB - [10.95 x 12.25] x 2 2.68 x 1072 m2

If these data are plotted as weight vs time, a straight line is found for
each film, as seen in Figure 27. The slope of the line can be determined
visually or by regression.
The results are as follows:

WEIGHT
TOTAL

TIME (HOURS)

Weight gain of bags packaged with desiccant (packaging study of

Figure 27.
potato chips).

20
Measures of film permeance:

k/x Value Polyethylene Mylar

(g H20/day m2 mmHg) A B A B
Me asur ed 0.074 0.071 0.118 0.119
Aver age 0.073 0.1185
Literature 0.21 0.3544

The manufacturer's data are about three times higher than the actual
values. In some cases, the values may be closer. The difference is probably
because the film k/x itself can vary by a factor of two to three times
depending on how it is stretched and how the seals are made.
The sorption isotherm for the chips (Figure 28) is also needed to solve
the problem. We must draw a straight line on the isotherm that fits the data
best for the region that the product moisture will traverse. The initial
moisture (mj) is 1 g H20/100 g solids and the critical moisture (mc) for
loss of crispness is 4.6 g H20/100 g solids at an ay of 0.45. Thus, a
straight line is drawn through these points, which gives a slope (b):

b = 0.0882 g H20/g solids

The solution also requires me, which is the moisture the product would
reach if left in the external atmosphere. Since we will test under abuse
conditions of 35°C/100% RH, we need me at 100% RH, or ay = 1.0. The data
of Figure 28 only go to an a, of 0.5, but this is okay since the equation
solution is based not on actual values but on the assumed straight line; thus
we can use equation 2la to get mg at a, = 1.0, which is 9.5 g H20/100 g ®
solids.
Using equation 22, then, I can be calculated for each value of the data
for weight gain vs time for the packaged chips. Note that to get m, we must
take the total weight at any time, subtract the initial weight at time zero,

MOISTURE
g/7188
CONTENT
SOLIDS
g

WATER ACTIVITY

Figure 28. Moisture sorption isotherm for potato chips at 22°C.

34
divide by the weight of dry solids, and then add this to the initial moisture
content.
Thus:

(W at time ®) - (Winitial)
dry solids

and
% . |4 solids (28
dry solids = (Winitial ~ Wpackage) 100 :

and
io/ — mi

where mj is in g H20/g solids.

Thus, for example, for the polyethylene at 1.93 days:

% solids
Y — 100 j{1 iaraneOl
=~ Sr0.Ul = 99201 ,

- oe oe + 0.01 = 0.03109 g H0/g solids.

Therefore, at 1.93 days (note that since this is a ratio, moisture values
used in the equation can be either g/100 g solids or g/g solids):
=; 9.5 a 1 =

4 e bay Ail 1.33

Doing this for every data point gives the following data, which are
plotted in Figures 29 and 30.

Chip moisture data:

Polyethylene A Polyethylene B _
days mM Tr se ee m he ine
0 0.999 1.0 0 0.9995 I 0
1.93 re i |Ps 0.285 2.88 1.28 OW25
616 36929 1.53 0.422 3.67 1.45 0.376
52/8 Det) 2.099 0.742 5.16 1.96 0.672
7.66 Des 2216 Oes7 5-46 ANG 0.743
9.99 6.6025) 29D 1.084 6225 2.61 0.961

Mee: Mylar A 0: ety. Mylar. _—

days m rT int m he In
0 ISS ist 0 a> 0.999 1 Orgs:
1.93 4.003 1.546 0.436 Je GLO elie 22-0 .420
3.76 5.227 1.989 0.688 4.849 1.827 0.603
5578 [PRUGESS eesoho eedBrea Ga) lo 360522 Le ll6
7.66 Ve229- Bef 43 “12320 GeS3l 321865 1.158
9.99 S234 7.334 1.993 IeOok O«e250 1.6598
 In
GAMMA

TIME (DAYS)

Figure 29. Unaccomplished moisture gain (IT) for potato chips stored in
polyethylene at 100% RH and 35°C, showing time at which lines cross the value
I, at the critical moisture content for loss of crispness.

In
GAMMA

TIME (DAYS)

Figure 30. Unaccomplished moisture gain (IT) for potato chips stored in mylar
at 100% RH and 35°C, showing the time at which the lines cross the value of
[. at the critical moisture content for loss of crispness.

36
 Although somewhat scattered, the data fit the theoretical lines drawn in
Figures 29 and 30 fairly well. These were drawn simply by using the
calculated theoretical slope, where:

A
slope = 7 bt (30)

The slopes were as follows:

polyethylene A 0.073 x 0.02908 x 42.2 _

Ses 35 in0 0Ssoe) oe Ue LIS
0.073 x 0.02904 x 42.2
polyethylene B 10.099 x 0.0882 0.103

Pe O es rxe0.03017 x 42.2.
mylar A = 00882
8.99 + cae el eee
SOLOS xt 0. 02668x- 4202
mylar B = gree race corey RG T-70 0.1746

Note that the measured average k/x was used in each case rather than the
literature value.
This example shows that, in fact, no long-term moisture gain studies are
needed. All we need is the moisture sorption isotherm, the proposed package
type (k/x) and area-to-solids ratio (A/w,), and the external conditions.
Thus, the time to reach some critical moisture, m,, can be quickly
calculated or graphed. This is indicated graphically in Figures 29 and 30,
while the equation shows that the critical time at m, is:

i InI,
oO. = ———_—— ,, (31)
k A Po
i

At the conditions of the test, equation 31 and the graphs show that
polyethylene would give a shelf life of 4-5 days while mylar would give a
shelf life of only 3 days. Of course, in real life, the external temperature
and humidity are less, so shelf life is longer. The value of the equation is
to show how one can determine shelf life quickly.
More elaborate solutions for changing external conditions are available;
see the references in the bibliography. In fact, this method has been coupled
with reaction kinetic data for prediction of the extent of chemical
deterioration in situations where the rate of quality loss is also a function
of temperature and humidity.
The moisture prediction method could also be used in reverse to calculate
whether a particular film would be acceptable for a given real condition. For
example, suppose we wanted 90 days of shelf life for a 3-oz bag of chips at

37
 on moisture gain to the critical moisture for loss of
73°F/50% RH based
crispness. Then:

k = InI, (32)

< Po ep Oc
be We

where:
mj = 1 g H90/100 g solids,
mo = 4.6 g H20/100 g solids,
Me = 5.05 g H 90/100 g solids (value from linear isotherm),
grat US a % solids & 84.37 g, and
Ws = (3 oz x 28.4 g/oz) i aot

Note that p, can be calculated to within 2% error from:

In pp = 22588 + 21.03 . (33)

Using these data, the predicted k/x is 0.227 g H20/day m2 mmHg.

Since both films have k/x values less than this, they will be adequate, but a
cost-reduced film with a higher k/x might be appropriate.

F. Dry Ingredient Mixing

1. Introduction
Many combination food products involve the partitioning of two ingredients
that have different a,'s and thus different chemical potentials. During
storage, moisture is exchanged because of the chemical potential difference
between them until a final equilibrium water activity (deg ) is reached.
Unfortunately, dry bakery materials may gain too acne moisture from a
filling and thus lose their desirable crispness and/or begin to develop off-
flavors, whereas semimoist high-ay ingredients, such as fruit fillings, dry
out and become either gummy, sticky, or undesirably hard. Simple mathematical
models can be used to predict both the equilibrium final ay of a mixture of
two ingredients and the time needed to reach the final equilibrium ay when
they are mixed. In addition, methods could be developed whereby the important
physical parameters that are used to predict equilibrium and rate can be
easily obtained in the laboratory so as to speed product development time and
quickly determine whether a potential problem exists.

38
2. Mathematical model for equilibrium
When two ingredients of different a,'s are mixed together in a sealed
package, they will exchange moisture until an equilibrium chemical potential
and thus an ag, is reached, as shown in Figure 31. This ag, will depend
on the ratio os the materials and the slopes of their respective moisture
sorption isotherms.
Assuming that the total initial moisture in the system equals the total
moisture after equilibration and that the moisture isotherm of each ingredient
follows a straight line in the form:

m = bate (21a)

where:
a water activity,
b = _ slope, and
c = intercept,

it has been shown by Salwin and Slawson (1959) that the equilibrium water
activity can be predicted from the equation:

yaibiwi a
a -—————— 34
= Dy biwi

where :
gree t0itiat a, of each ingredient i,
by = absolute value of slope of moisture isotherm of each
ingredient i, and
wi = weight of dry solids of each ingredient i.

20

SOLIDS
g/1@@g
CONTENT
MOISTURE

WATER ACTIVITY

Figure 31. Moisture exchange in ingredients X and Y to some equilibrium water

activity (aeq)-
a)
 Thus, to predict deg» one needs the moisture isotherms of each component
at the possible temperature at which the product will be stored. Note that
this equation gives the final a, but says nothing about how long it will
take to reach it. The equation can also be used to design the system so that
the percent of each ingredient is such that no ingredient crosses the critical
water activity that makes it unacceptable. If this can't be done, then
ingredient modification is the next possible solution. To get the ratio of
each ingredient, some critical a, is chosen and is substitu ted for deg in
the above equation. Of course, what is needed is the isotherm for each
ingredient. Recently Iglesias and Chirife (1983) publishe d a compilat ion of
many food isotherms, which would be invaluable for this purpose. Also, Tables
4-6 give isotherm data for some gums and food fiber material s, as well as for
materials used in dry drug preparations.

Table 4 . Equilibrium moisture content of dry gum powders at various water

activities (T = 22°C)

Moisture Contents (g water/100 g solids)

LM agar- locust HM
_ aw pectin agar xanthan _bean_ karaya guar pectin carrageenan* gelatin*

0 1.6 0.9 3 1.1 1.6 0.3 0.8 0 0

0.11 5.9 10.2 6.8 6.7 D9 Jel 4.9 8 7

O22 07.8 14.8 9.7 9.9 723 8.7 6.5 14 13

0.33 9.2 ele | 11.0 11.8 Ay 1033 {ee 18 15

0.40 10.1 1952 9 12.6 1052 10.9 8.8 19 16

0.44 10.5 20.0 1276 12.8 Be | Pie 9.5 22 19

0.52 12.4 21.9 15.4 14.2 tZao 1230 L126 23 20

0.65 18.5 24.9 19.8 yep 1<3 L625) haar 26 22

0.75 ~29°4 28.3 26.3 20.9 18.4 2052 HW6s7 33 28

0.85 46.3 3229 36.7 26.9 30.4 Ziad) Macon 48 41

05947. 7654" > *40:0 S13 37.4 46.3 39.7 44.9 78 82

0.98 127.0 50.9 90.3 TAs | 97 <5 65.1 80.5 101 113

*From Wallingford and Labuza (1983).

40
 TABLE 5

Moisture Sorption Isotherm Data at 23°C--Food and Fiber Sources*

ee

Apple Citrus
Cellular Pulp Avicel Avicel Avicel Avicel Powdered
ay Fiber Fiber pH 101. pH 105 kC591 CL 611 #£Cellulose

0.11 1.89 3290 2.18 2.10 2.01 2.81 2.10

0.22 39D 5.08 2.81 3.80 3.45 4.29 o6l9

0.33 5.09 5.83 3.84 5.00 4.38 Die DT. Jel 2

0.44 8.04 8.07 5.00 5289 6.09 6.99 4.96

0.52 8.46 8.56 5.01 6.01 6.45 7.05 5.07

0.65 P7556 12.89 6.79 8.76 9.01 10.53 Todz

0.75 26.26 16.56 3.00 11.05 11.26 12025 8.89

0.85 oh SW 19.89 12.37 13.82 15.42 LS. 79 19.35

0.98 141.65 57.08 14.97 ay Leo 3 21.40 19.977

Solka Solka Solka Corn Oat Wheat Soy Rice

Floc Floc Floc Bran Bran Bran Bran Bran Wheat
ay SsW-40 BW-40 BW-300 Flour Flour Flour Flour Flour Flour

0.22 2.66 3.9F 3.55 5.7/7 syle) 5242 5.20 5.39 3.76

0.33 4.07 4.18 Deol 7.34 6.56 USS) 6.83 6.95 6.84

0.44 5.13 Sel 7.07 8.45 8.11 8.78 dene 8.26 8.60

0.52 5.89 6.5/7 7.30 9.2/7 8.59 9.66 8.7/6 8.7/7 9.81

0.65 7.42 8.49 10.44 12.53 11.12 oat 11.04 11.46 14.52

0.75 9.78 10.43 12.94 14.68 12.78 14.28 13.71 14.67 17.29

0.85 12623 13.19 Leos 1OehOrg 10216, 821.235 18.74 19.20 20.84

0.98 17./0 17.81 1315 6 es 0 2 40.505 ~L10.33', 56.00 104.92 31.92

ee E

*g of HzO per 100 g of solids.

41
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Jo “Te ZR6I usasds)Skep (wiey,OST

*
 Figure 32 shows the isotherms for a food product with a high-a, soft
center filling and a low-a, crispy crust. The initial ay's are shown
(a, and ap), along with the visual plotted slopes for a projected linear
isotherm to fit equation 34. Assuming a 50/50 mix of the two components, what
would the equilibrium a, be?
The following data table is set up for 100 g of the mixture:

Component Wi by
Weight a my Weight of Isotherm
Component (g) 1 (g H90/100 g) solids Slope
Crisp shell (s) 50 0.061 2.3 48.88 15.19
Senter, fill-(c) 50 0.536 19.2 41.95 38.1

as bsWs + acb cWe

(35)
bsgWs == bewWe

=e eCOs00l) ©) 15.19 * 48.88) + (0.536 ° 38.1 + 41.95)

0.385

. Thus, if the outer shell lost crispness at 0.45, at a predicted 0.39 ay

it would remain crispy but the filling might be too hard, and this product
would become unacceptable in storage. One could then manipulate the amount of
each ingredient in the equation to determine how much less filling would
result in an acceptable, final, higher ay-

38

Center Fill_»

MOISTURE
SOLIDS
g/1@@g
CONTENT

WATER ACTIVITY

Figure 32. Example isotherms for equation 34 solution.

43
3. Mathematical models for the rate of gain or loss of moisture

(a) General model

The general model assumes that there are three barriers to moisture
exchange. These include the diffusion resistance of water inside ingredient
X, the resistance of water transport in the air space, and ingredient Ys
internal diffusion resistance to moisture transfer. For simplicity, ome can
either consider these as permeabilities, 61, where Bj is in units of g
H)0/day m* mmHg (driving force), or as diffusivities, De¢¢, which are
used in unsteady state approximation solutions (in units of cm2/sec).
Several general assumptions are necessary to solve any situation.
(1) The vapor space volume is small compared to X and Y, and thus the air
is not a major sink for moisture.
(2) Ingredients X and Y are in intimate contact with each other at a
contact area, A, which is the total surface of the ingredient with the
smaller percent in the formula (e.g., for 20-30% raisins in 80-70%
cereal, the transfer area is controlled by the raisins).
(3) No moisture exchange of significance occurs across the package barrier
to or from the outside environment.
(4) Temperature is constant.
Given this, then, the rate of exchange of water from X to Y (assuming that X
is.at a high a.) is:

dw A (px — Py)
dO te id ak ae Oe
Bx BarR By

where:
dw
qo 7 «& Ho0/day,
A = contact area,
Px = vapor pressure of water in ingredient X at timeO@,
Py = Vapor pressure of water in ingredient Y at timeO@,
Bx = permeability of moisture in X (g H90/day m2 mmHg),
By = permeability of moisture in Y (g H»0/day m2 mmHg), and
BarR = permeability of moisture in air space.

Note that permeabilities are considered to be constant, i.e, not a function of

the moisture content.

(b) Simplistic model I--External p/p, constant

In the simplest form, which would constitute an accelerated shelf life
test, each ingredient is assumed to behave independently, and the external
environment (i.e., the air and other ingredients) is assumed to already be at
deg and to act as an infinite sink.
Thus,

407 0 ee ee (37)

44
 ao. = ByA (py- Pe) (38)
where:

Pe = vapor pressure of package environment at deg = Pal Dom.

Thus, a simple solution exists if one assumes that the moisture sorption
isotherm for each ingredient behaves as a straight line between initial vapor
pressure and pe, as was done for the packaging example (pp. 30-38) with the
same linear equation.
Since the isotherm equation can be represented as:

m = b p/ppte (39)

where:
b = slope of isotherm and
en =" intercept,

then, at any time:

Pp
Dx = ie my + Cx (40a)

Py =
Po
by My a7 ©
/y (40b)

P
Dea is (me), ne e*5 (41a)

Pee
Ent
= by
eake
Me y
eine y
(41b)

where Po = vapor pressure of pure water at temperature T. Also, since

SELES LE ES change of moisture content (42)

dO - Ws do on dry basis,

where Wo = weight of dry solids of ingredient, then for loss of moisture

from ingredient X, substituting in for px and Pe,

dm A Po (43)
-—+ = —— - (mg)

45
and

mM O¢
Z rae Sale op) fale = (44)
u my a Me), Sy by
i

py are lie eePee Ro ese (45)

pot 8 ee Ws, by

where mp is the moisture at time Of.

This is very similar to the packaging equation. Basically, this equation
states that equilibrium can never be reached because when mp = m,, the
left hand side of the equation goes to infinity. However, one can come close
if m, is known from a,, and m; is defined. Thus, one could set mg at
some level, e.g., 99.9% of mg or at some weighing error such as 0.001 g
H)0/g solids (an error of 0.1-1% depending on sample size). Then the
equilibrium timeO¢ for component X is:

2 Wer abe
Sein ln =| Rar et Sh (46)
x

A similar equation for gain of moisture by ingredient Y is:

= ain, W b
Sree pein eas | bee (47)
LS hee . ABy Po

Comparison of Be. and B¢ _ will indicate which ingredient will

become unacceptable first. Note, however, that in reality, the above
equations will severely underpredict true shelf life because, for gain or
loss, the driving force will decrease as p, decreases and p, increases.
These equations should thus be used only as a first approximation. Also note
that B, and By need to be determined,

(c) Model II--Source/sink act as point sources

For a more realistic model, it can be assumed that the major resistances
to moisture transport are at the surfaces of each ingredient and that, in
general, as each ingredient absorbs or desorbs, it instantaneously
equilibrates over its whole volume. Thus, again:

‘ Py)
dQoe i eee (48)

or
cb = |
D tae}he =
|
uo) VY
re)
| c= : (49)
46
where

fy -= [a8 = total permeability . (50)

Bx ParR By
To solve this equation, one must again put the vapor pressure in terms of
the moisture content of one ingredient. We saw that:

- AW, = AW y (51)
i.ee., Y gains and X loses an equal amount of water. We can solve this problem
by aEE ea
iteration, using the following computer-based solution.
Set zero time values for all variables, e.g., Pxg? Py»
neg YO"
(2) Choose some small time increment AO(e.g., 1/2 day).

(3) From equation 49, using initial values Px, and Py»
calculate the initial moisture loss of X, which is:

AW, = BrA (Px,- Py,) AO. (52)

(4) Calculate the new moisture content of X, where:

m x = os - Te “ C55)

(5) From the isotherm equation for X, determine the new p,, where:

Po
Pee iahee Teg eo)

(6) Similarly, for ingredient Y, calculate the new moisture content,

where:

Ee eS (55)

(7)

Po /
a elders miy+Cy-e (56)
y

(8) Total time =) AO =O ,

Total AW, =>, AW, : (57)

47
 (9) Repeat iteration starting at step (3) by substituting Px,
Px and py = P ye

(10) Continue going from (3) to (8) until equilibrium:

DAW, = (my - me) Wy, (58)

(d) Model II--Source and sink are not point sources

In many cases, such as in a cream-filled pastry, the dimensions of X and Y
are such that one cannot assume that each behaves as a point source. In this
case, a moisture gradient will exist inside each ingredient, which slows down
the moisture exchange even more. One can assume that all the resistance is
internal and exists as a diffusion coefficient. Crank (1956) has developed
simple solutions for a system in which the internal diffusion coefficient is
known and an error function solution for a two-ingredient system that must be
solved on a computer. A general idea of the equation assumptions is presented
below.
In this analysis, one assumes that when two semiinfinite solids, one at a
uniform moisture concentration m, and the other at another concentration
My, are placed in perfect contact, the following equations describe the
moisture distribution with time:

a
gatots bth ect] =| (59)

where: D, = diffusivity of water in ingredient X,

o characteristic thickness of X, and

yn L
aa = be | (60)
ey iy 2VDy

where: Dy = diffusivity of water in ingredient Y, and

Ly = characteristic thickness of Y.

After some short period of time, the concentration of water at the

interface is my, = my, = ee as shown in Figure 33, which is the

Air Space

X Se —e_n a My

Figure 33. Representation of moisture distribution.

48
 Steady state value of m at the interface. This value can be approximately
calculated for any time from the following relationship:

‘gio pleas DS: (61)

Thus, if mj is known, error function solutions (erf) for equations 59

and 60 can be used to predict the times for each to reach a given moisture
content. This analysis has been used for studying salt concentration changes
in cheese when two slabs of cheese with different salt content are brought in
contact.
For food products that do not conform to fixed geometric shapes, finite
element analysis on a computer can be used. For this, several computer
solutions are available as long as values for D, and Dy are known. These
are too complex to describe here.

4, Determination of permeability and diffusion constants for moisture

gain/loss of ingredients

(a) Mathematical model

Several models, all based on the same experimental data, can be used to
determine the overall diffusion coefficient (Dx) or permeability value
(8;) for foods. Of concern is that the value determined could be a function
of sample geometry, test temperature, and test humidity. The simplest model
is to expose the ingredient to a constant % RH (at some T) and to have a
static environment because in a real food package there are no convection
currents. The environment volume should be large compared to the sample so
that there will be only a minor change in environment % RH. The sample is
then weighed periodically until equilibrium is obtained. This is similar to
our initial experiments, but more data are collected.
If one can assume 1) that no moisture gradient exists inside the product,
2) that all the resistance can be viewed as a permeability, and 3) that the
isotherm can be drawn linearly, then for a point source solution:

edwi-= pA = (62)
w,dO Ps Ws Por Pegs

which, for moisture gain by ingredient X, gives

mn 2m, A p
ln [= |= int = 6, — —O , (63)
as ~ a W, - by

with all constants the same as before, and [J is the unaccomplished moisture
ratio, as used in the packaging example. This should give a straight line
when lnI’ vs time is plotted. Bs
both A and Wg, are known for an ingredient in the chamber, Yi can be
If
calculated as g H»0/day m2 mmHg from the slope of the line. Using this
model, one also should:

49
 (1) collect data at several % RH's to evaluate the effect of humidity on
B;. The choice of these can be based on the range the product will
go through when approaching deg: A plot of 1n 8; vs % RH should
normalize to a straight line.
(2) collect data at several temperatures to get the effect on Pi, “A ples
of ln By vs (1/T°K) should give a straight line.
For high-a, samples, it is suggested that 35 and 45°C be used at 0% RH
(desiccant) and 32% RH (MgCl). For dry samples, the same temperatures at
75 and 85% RH would be desirable to achieve the plots quickly.
After values of 8; are collected for both ingredients, a judgment about
their relative resistances can be made in order to solve for moisture
diffusion times in the previous equations. Data collected in the literature
for freeze-dried foods show a range of 10~4-107> g Hy 0/cm2 sec mmHg
for B;, which is about 102 times higher than that found for dense foods
such as pasta. This value, however, is much smaller than the diffusion rate
in air, which, in comparable terms for a contact space of about 1 mm, would be
about 1072-1073 g/cm sec mmHg. Thus, the assumption that the food is
the major resistance to moisture exchange is correct.
If there will be an appreciable moisture gradient within the product, then
the solutions involve an effective diffusivity, D;, which also can be a
function of temperature and external relative humidity. The same test
parameters as for a point source are used except that in this case, if
possible, the characteristic dimensions of the object are needed. For a
typical pop-tart or center-filled bakery product, the object can be
represented as two slabs with diffusion in one direction. For the single
ingredient, several solutions exist.

(b) Method of successive approximations with an error function

Given the initial boundary condition of low moisture (i.e., mj ~ 0), we
can derive the following equation for moisture pickup:

n =CoO

nee
m, 1 a7) > -
ee [exe= Dy(2n + 1)* 2p 1“Q/L¢)
el alae (64)
n= 0

where L is the total thickness for one-sided diffusion.

Substituting into the equation, we find that for n=l, all terms in the
series drop out because they are much smaller than the term for n = 0.
Thus

mS
Me
= geal
r2
ex
P
LDi2-8
pee (65)
6

where Lo is the characteristic thickness (half-thickness for two-sided

adsorption or total thickness for one-sided adsorption).
Thus,

|- =% - °e. (66)

50
 A plot of In [1 - (m/mg)] vs time @should give a straight line with the
slope equal to

Dy7 2
slope = - 5 : (67)
L°

Thus Dj can be determined. Similarly, for moisture loss, an analysis by

unsteady-state diffusion through the error function gives:

mS 8 2D;
pe Wale slgice== wl ig z (68)
my ic: Me me Lo2

As above, a plot of InI (the unaccomplished moisture change) vs time®@

will give a straight line with a slope similar to the above equation,

a
coal
slope = - = ‘ (69)
Lo”
For two-sided drying where L is the total thickness, the slope is

4n2D
slope = - S ° (70)
L2

This form, which might compensate for edge effects, might be more convenient
to use.
In both these cases, Dj can be obtained. In fact, if me is known from
the isotherm, then the experiment need only be carried out to m= 0.5 mg
since from this:

D, = 22049 Lo” (71)

01/2
where 0) /2 is the time when m= 0.5 me for either adsorption or
desorption.
Note here that the diffusivity value generally falls in the range of
1074-10719 cm2/sec for moisture transport in a porous solid, whereas the
effective diffusion coefficient (De¢¢) for water in air is about 0.26-0.29
em2/sec at 25-40°C. Thus, as before, the assumption that the solids, not
the air, are limiting moisture diffusion is generally good. An example
calculation will be presented in a later section.

Ge Humectant Selection

1. Introduction
One method of creating intermediate-moisture food products is to add
solutes such as salts, sugars, or polyols to depress the water activity. The
extent to which a, is lowered can be calculated from Raoult's law, but as

J
noted earlier, this becomes inapplicable below an ay of 0.95 unless the
activity coefficient Y is known. Several other mathematical solutions are
available, some of which require knowledge of the moisture sorption isotherm
of the humectant. Since some of these ingredients are crystalline materials,
both the desorption and adsorption isotherms are needed. Appendix Tables
A2-A7 show data for sugars; Appendix Tables A8 and A9 contain data for NaCl
and KCl, respectively; and Appendix Tables Al10-Al3 show data for polyols.
Note that most of the humectants show hysteresis, as seen by the difference it
adsorption and desorption data. The VPM data were collected by directly
measuring the vapor pressure of a solution on a vapor pressure manometric
(VPM) device (Sloan, 1975). Interestingly, glycerol showed
no hysteresis
(Figure 34). When used for predicting the ay of intermediate-moisture
foods, the desorption data best apply down to an ay of about 0.7. When
crystalline material is added to a system below aw 0.6, the adsorption data
should be used.

2. Raoult's law method

As noted earlier, Raoult's law follows the form:

ay erie
= wan teeNy»0
Bees ° (2
Ny50 + Nsolute

Tables of Y can be found for many solutes in the International Critical

Tables or in the article by Fontan et al (1979) mentioned earlier. In
general, it can be assumed to be 1 for a rough calculation. Suppose we have
100 g of meat at 50% moisture and we want to know what the a, would be if we
added 20 g of propylene glycol (MW = 76).

340

al© - ADSORPTION
DESORPTION
4 - DESICCATOR
@-VPM

SOLIDS)
g
H20/100
(g
Mg BiS)
ro)
o@fe)
3°
fe)

Db (2)

N oO

Figure 34. Moisture sorption isotherm of glycerol at 22°C.

a2
 Thus:

50/18 |
ae aie
+ 00776 0.9135.
This assumes that the glycol does not interact with the food components
and that all the water is available to it. It also assumes that Y= l.
Actually, the isotherm data for the VPM method in Table All can be plotted and
the deviation from ideality determined directly. If this is done at a
moisture content of 50 g of water per 20 g of glycol (250 g H70/100 g
glycol), the actual ay is 0.89, showing that glycol reduces the a, more
than predicted by Raoult's law. Thus, use of the isotherm data would be
better.
A second example is the case in which we want to know how much of a
humectant such as glycol is needed to reach a given a, such as 0.85. Using
Raoult's law, then:
2.778
ee
578s

Nsolute = 0.491 moles glycol = 0.491 x 76 = 37.34 g propylene glycol.

From the isotherm at ay = 0.85, the moisture content is 180 g/100 g

glycol. Thus: 180 50
100 - x
x 27.28 g propylene glycol.

Again this shows that actual data predict a greater lowering of a, for
propylene glycol than would be expected.
Some general equations have been developed by Chirife et al (1980) for
isotherm data of sugars in the following forms, where myx is in moles per
kilogram of solution.

Fructose a, = 1.0126 - 0.02462 m + 0.000362 m (72)

Glucose ay = 1.0042 - 0.02011 m (73)
Sucrose a, = 1.0014 - 0.02117 m - 0.000635 my (74)
Maltose a, = 0.9986 - 0.01924 m, C75)

Other such polynomials could be derived from the data in the tables based on
moisture content rather than from moles, as above.

3. Norrish equation
Norrish (1966) developed an equation that accounted for the deviation,
using the Hildebrand and Scott assumptions, which state that:

ny = KiX42 (76)

where:
Vv" =) the activity coefficient,
Kj = a constant for each solute,
Ng
Saute mote fractionyor solute i: = —-————. , (77)

23
 mole fraction of water = » and (78)
X]

Ng total moles of all solutes.

Note that X; is moles of solute i divided by total moles of water, of

solute i, and of all other solutes. For a complex mixture, then:

iniea. se eLey Xj! [(-ea)1/ 2x2 + (-K3)1/2x3 + veeeed]?, (79)

whereas for one solute:

In ay = 1nX] + KX22. (80)

Table 7 lists reported K values for typical food solutes used to lower
aye Note that for solutes like NaCl when used in equation 79, the value of
(-Ky,)1/2x5 is calculated as (Ky) 1/2x5. Thus, it is subtracted
from the total in the brackets.

TABLE 7
K Values for Norrish Equation

Compounds |

PEG 600 =30 are

PEG 400 -26.6 + 0.8
lactose -10.2
lysine =? 1x053
lactulose -8.0 + 0.3
sucrose -6.47 + 0.06
ornithine 6.4 +0.4
eLtric acid -6.17 + 0.49
DE 42 =—553k05
Cattaric. acid —4,68-+ 0.5
maltose -4.54 + 0.02
proline -3.9 + 0.1
a-aminobutyric acid 2.57 + 0.37
alanine —2.52 + 0.37
glucose/fructose -2.25 + 0.02
malic acid -1.82 + 0.13
sorbitol -1.65 + 0.14
lactic acid -1.59 + 0.2
xylose -1.54 + 0.02
glycerol = LO + 0.01
propylene glycol =1 50
mannitol =) 91+ Ose
NaCl +17.48
KCl +10.81
urea +2..02
glycine +0.87 + 0.11

54
 Using the same examples as before, we can determine the effect of 20 g of
glycol on a, lowering and calculate how much glycol is needed to reach an
ay Of 0.85. In the first case, if we add 20 g of propylene glycol to the 50
g of water in the meat, we have:

50
N50 = T3 c= ZattS Py

Nglycol = = = 0.263 ;

oe 2.788 Sacoes ie
2.778 + 0.263

Xp = 1-0.91 = 0.09,
Kagy) =eo-).0.(from Table 8).

Then

In ay = In (0.91) - 1.0 (0.09)2 = -0.1024 , and

ae f=: 0,903 .
Note that this a, is higher than that found from the isotherm data
(0.89) but lower than that from Raoult's law (0.914).
In the second case example, where we want a final a, of 0.85, we have:

aw = 0°85, In aw = -0.1625,

Se a aoe
t= 2 = (lb = xy) +, and
Kgly — —-] e

Therefore:
- 0.1625 = In X} - 1 (1 - X})2.
This cannot be solved directly, but one could assume additions of
different levels of glycol (for example, 10, 20, 30, and 40 g) and calculate
ln ay for each case.
Then a plot of 1n a, vs amount added is made, and the correct amount is
read off the graph where In ay = -0.1625 (or ay = 0.85). In this case, we
have:

g glycol added calculated a,

10 0.953
20 0.903
30 0.862
40 0.8197

Thus, interpolating on the graph of ln a, vs glycol added, a value of 32.3 g

of glycol is found. Note that Raoult's law predicted 37.34 g and the actual
isotherm gives 27.28 g.

55
4, Grover equation
Grover (1947) used actual measured data from studies made with
confectionary solids to develop a polynomial expression of the form:

ay x 100 = 104-10E° + 0.45(E°)2 (81)

where

rae) oes my

Ej is a value from Table 8 for ingredient i, and mj is the ingredient

moisture content in grams of water per gram of ingredient. The Ej values
were based on setting the Ej value for sucrose to 1 and then comparing the
relative water binding.

Table 8
Ej Values for Grover Equation
Component Ei
sucrose 1.0
lactose YO
invert 1.3
42 DE 0.8
protein NAS,
starch 0.8
gums 0.8
acids 26D
glycols 4.0
salts 9.0
fat 0

To use the Grover equation, we need to know more about the composition of
the system. If the meat has the following composition, we will find:

Meat Component grams Loe E Ei/mj

water 50 * ca -
protein 15 35353 1.3 0.390
carbohydrate 1 50 0.8 0.016
fat 34 1.47 0 0
E° = 0.406

* A value for water is not included in the calculation.

Therefore, the initial a, of the meat is

ay = [104 - 4.06 + 0.45 (0.406)2] + 1.00 & 1.00

which is reasonable.
Chirife and Fontan (1982) recently published values of ay for fresh
foods based on measurement of freezing point depression. Fresh meat runs from
0.99 to 0.998, which is what should be expected. The average is about 0.992.

56
 The my for glycol is equal to 50/20 = 2.5. If we add 20 g of glycol,
which has an Ej of 4, there is an added E;j/mj of 4/2.5 = 1.6. Thus, the
new E° is 1.6 + 0.406 = 2.006, which gives a calculated a, Of 0.85. This is
considerably lower than the a, from the other calculation methods. To
determine the amount of glycol needed to achieve an ay Of 0.85, we have:

85 = 104 - 10 E° + 0.45-(E°)2 ,
Therefore,
(Eo)=)190.9 Fo 42.00 = 0 >
using

- B+~/B4 - 4AC
E° = — (82)

where A, B, and C are the coefficients of the equation. Solving, we find that
a = 2,10. Since the meat contributes a value of 0.406, the added glycol must
contribute an Ej/mj of 2.10 - 0.406 = 1.694. At an Ey = 4 for propylene
glycol, then:

e694 ake
mi

my = 2.361 = “g) Ho0/2 glycol”.

and
rae
x DA SEYEMG os

Therefore, X = 21.18 g of glycol is needed for the meat to reach an a, of

0.85.

5. Ross equation
| Perhaps the best prediction equation is the Ross equation, which assumes
that each solute behaves independently and dissolves in all of the water of
the system. The equation is:

Gye SP Gi © 3H) : aH ° 213 ecccece any (83)

where:
af the final water activity.
aj the initial water activity before adding solute i. For fresh
foods the Chirife and Fontan (1982) values can be used, and for
complex foods the Grover equation can be used.
ony the water activity the solute would have if it dissolved in
all the water. Use of the solute isotherms is recommended
for this term.

As with the prior examples, we can first calculate what the a, would be
if 20 g of propylene glycol were added to 100 g of meat at 50% moisture.

?
0.992 from Chirife and Fontan (1982),
water activity at a moisture of 250 g H20/100 g glycol from
values in Table All = 0.89.

|
Thus, af = 0.992 x 0.89 = 0.88 °

This is lower than the value from Raoult's law and the Norrish equation
but higher than the value from the Grover equation. Studies in the literature
show the Ross equation to be the best to use when comparing calculated values
to actual measured ay values.
For the problem of how much propylene glycol to use to achieve an ay of
0.85, we have

0.85 0.992 4H 9 and

any 0.857 e

Extrapolation from Table All gives an m of 180 g of H20 per 100 g of

propylene glycol. Thus, for 50 g of water in the meat, we need 27.8 g of
propylene glycol.

6. Example problem
Your company is presently making a semimoist dog food with a final a, of
0.84. It has the following formula:

meat by-products 50% (20% fat, 20% protein, 60% H20)

oat hulls 10% (90% cellulose/starch, 10% H90)
wheat feed flour Lo? (90% cellulose/starch, 10% H90)
salt 3%
sucrose 15%
propylene glycol 6.8%
K sorbate/minerals/
vitamins __ 0.24
TOTAL 100% (moisture content, 32.5% [wb])

Sucrose presently costs 30 cents/1lb and the new high-fructose corn solids
(HFCS), which are dry solids, are about 35 cents/lb. HFCS solids have the
following composition: glucose, 50%; fructose, 50%. Figure 35 gives the
isotherm data for the humectants.

(a) Calculate the theoretical a, of the above system by the Grover method
and compare it to the ay calculated by the Ross equation:

Amount (g) Fat Protein Water Starch

Meat 50 10 10 30
Oat hulls 10 eee cee 1 9
Wheat feed Me Ae eee Loo t3.5
Salt 3
Sucrose |
bss
PG 6.8
Vit amins 0.2
S Led

Total H90 = 32.5 g/100 g formula or 48.15 g/100 g solids

Actual a, =

58
 Grover equation solution:
| ay ° 100 = ERH = 104 - 10 E° + 0.45 (E°)2
Calculation of E°:
m (g H)0/g
Ingredient grams solids) Ej Ej/mj
Water S265 * % *
Starch 225 1.44 0.8 0.554
Protein 10 De2o Les 0.400
Fat 10 Be29 0 0
Sucrose 15 2.17 el) 0.462
Glycol 6.8 4.78 eS) 0.837
Salts** See 10.16 9.0 0.887
E° = 3.139
*As before, the E; value for water is zero.
**Note that “salts” includes the vitamins as a first approximation.

Therefore,
105 = "10 (32139) +0245 €32139)2 = 77.14
TITA4/100° = 62771

Ross equation solution:

af ~ 41° “Healt * “"Hsucrose ° “HpG

ayy ee (To approximate the Grover equation--exclude sucrose/
glycol/vitamins and salt, since these are added.)

fe ees 34199 — 0,462 — 0.837 -— 0.887 = 0.953

Therefore, using the Grover equation to get a; for an E° value of 0.953:

ay = 0.949 e

To find the a, of the salts:

/ l 1015 g H 0
Sze H50/3.2 solids m a
PUeaics © sppy: : 100 g salt

ay Se
= TTOLS7I8) 1015/18
+ (100/58.5) x 2 _ 0.943 from Raoult's, law,

assuming all salts have the molecular weight of NaCl. However, from the
isotherm data (Figure 35), the a, = 0.908.

To find the a, of sucrose:

a O32. ¢ 450/15 Ersucrose = m = TO0rgesueacee

Hsucrose

Dg
 216/18 T ’ 1
.
law
=

0.976 from Raoult’s

216-7/18) + (100/342.3)
=

aw

while from the isotherm data (Figure 35), the a, = 0.955.

To find the a, of propylene glycol:

Ap @ 32.5 g H)0/6.8 g glycol = m = 478 g H90/100 g PG

ag = eee oe = 0.953 from Raoult's law

(478/18) + (100/76)

while from the isotherm data (Figure 35), the a, = 0.943.

Therefore:
using isotherm data, ag = 0.949 ° 0.908 ° 0.955 ° 0.943 0.776.
using Raoult's law, ag = 0.949 * 0.971 ° 0.976 * 0.953 0.856.

From a practical standpoint, the isotherm data should be used. Comparison of

the Grover and Ross equations shows that they agree fairly closely and are
within the usual error of measurement (+ 0.02 ay units).

Grover Ross
Ona 0.776

2888

1688

1688

1488

1288

MOISTURE
CONTENT
SOLIDS
g/71@@g

WATER ACTIVITY

Figure 35. Humectant isotherms for example problem solution.

60
 (b) Calculate the amount of HFCS needed to replace sucrose: Using the
Grover equation value as the initial value, how much HFCS would you need to
add to replace the sucrose entirely and achieve the same a,?
Compare the
Grover solution with the solution using the Ross equation.

Grover equation--Amount of HFCS to replace sucrose:

final a, = 0.771 (Grover equation)

Calculate E°:

E° = 3.139 with sucrose

E° = 2.677 without sucrose
AE° = 0.462

0.462 = Ey/my

Ej; for glucose/fructose = 1.3

iees ;
a Ej
mi ~ 9.462 ~ 00462 ~ 2-981 g Hg0/g solide

g solids = = 11.6 g HFCS needed as compared to 15 g sucrose.

Ross equation: Amount of HFCS to replace sucrose:

final a, = 0.776 (Ross equation)

Therefore:

@p = ag ° anpcg = 0.776

where a; is the a, without sucrose using the Grover equation. Then:

aj = a, ° agait ° apg = 0-949 ° 0.908 * 0.943 = 0.813

where a, is the water activity of the system without all humectants, found
using the Grover equation.
Using Raoult's law to find the HFCS concentration for the final ay of
0.776 gives:

0.776 3225/18
> 220.955 te
4HFCS 0.813 3225/18 + 2(n)

05955) (1.6067 + 20) = 1.806 .

Thus, n = 0.426 moles of HFCS.

61
 The 2 is used in the denominator of the equation because each gram of
HFCS contains 50% each of glucose and fructose, or 1 mole dissociates into two
kinetic units of a molecular weight of 180.2. Thus, HFCS needed = 0.426 x
180.2 = 7.67 g, as compared to 15 g of sucrose.

No isotherm data exist at 0.955 for fructose, but Table Al2 has data for
glucose. Thus, using the data for glucose plotted in Figure 35, we can
estimate the HFCS concentration by the isotherm method where:

270 g #90 32.5 g H20

100 g solids X

X=212.0 ¢ HFCS «
This value is close to the Grover value and probably more accurate.

(c) To find the cost saving, calculate the original cost of sucrose per
100 1b of finished product:

15 lb sucrose
ToOeeMGo lida 30 cents/1lb = $4.50/100 1b finished product .

From the Grover equation solution, we found that we needed 11.6 g of

glycol to replace 15 g of sucrose; the Ross equation predicted 12 g using the
isotherm data. Thus, using 11.8 1b as an average value of HFCS to replace 15
lb of sucrose:

COO Ss Pe ab are x 35 cents/1b HFCS = $4.13/96.8 lb product

WS aks x
aiG-6 100
X = $4.27 per 100 1b finished product.

Thus, HFCS is cheaper to use by 23 cents per pound of finished product.

H. Package Temperature Shift

As noted earlier, the moisture sorption isotherm is dependent on
temperature. Of concern to the food technologist is the fact that, during
storage, a product in a sealed package may be exposed to long periods at a
temperature higher than the temperature at which it was packaged. Thus, if
the moisture content remains the same, the product will increase to a higher
a, (Figure 36).

62
 Thus, any reactions that can lead to quality loss will be increased in
rate by an increase in both a, and temperature. For example, if ay
increases by 0.1, which doubles the rate of quality loss, and if the 10°C
shift has a Qi9 effect of 4, then shelf life would be decreased by 2 x 4 or
a factor of eight times. Therefore it is imperative to do moisture sorption
isotherms for sensitive dry products at a minimum of two temperatures to
determine the magnitude of the shift. For intermediate-moisture foods, this
should not be a problem, as the different isotherms generally join above an
ay Of 0.7.

AMOUNT
ADSORBED

ACTIVITY

Figure 36. Shift in a, for a food in a sealed pouch subjected to a

temperature shift.

63
IV. Determination of Moisture Sorption Isotherms

A. Humidity Controlling Devices

In general, the simplest approach to creating a moisture sorption isotherm

for a food is to put it into a controlled humidity chamber at constant
temperature and measure weight gain with time until equilibrium occurs.
Various means that can be used to create the constant % RH include:

1. Mechanical humidifiers
These generally are only good to +54 RH because of the wet bulb
controllers used. Excellent chambers do exist, albeit at high cost ($3,000
apiece).

By wyoulbehenve acid/H 70 mixtures

Tables of vapor pressure above solutions of various H 2504
concentrations exist. These solutions can be put into the bottom of a
desiccator and the food exposed to the vapor. Innumerable isotherm points can
be obtained. Of concern is the corrosive nature of the acid, especially at
low ay (high concentration), since accidents can result in the acid coming
in contact with the food or the experimenter. In addition, if moisture is
gained or lost from the solution as equilibrium is achieved, the solution must
be titrated to obtain the correct final concentration and therefore a,,

3. Glycerol/H70 mixtures
The noncorrosive nature of glycerol relieves some of the problems
associated with H9S04; however, it also must be analyzed at equilibrium
(by gas-liquid chromatography). In addition, the glycerol can also volatilize
and adsorb into the food, causing error if weight gain is used as the moisture
measurement.

4. Salt solutions
Saturated solutions of various organic acids and bases as well as
inorganic salts produce a constant vapor pressure in the water above them at
constant temperature. Several cautions are necessary.

(a) The salt and water must be pure. Only distilled water and ACS grade
salts should be used, and they should be mixed in clean containers. Care
should be taken, as some saturated solutions are very caustic (e.g., potassium
dichromate, potassium chloride) or highly toxic (e.g., lithium chloride,
sodium nitrite). The actual solution should be a slurry with excess crystals
present. Alkaline solutions (e.g., K2C03) absorb larger amounts of C02
with time, which will decrease the a, significantly.

(b) The slurry should be made at or above the temperature at which the
isotherm is to be done. Saturated salt slurries transferred to a higher
temperature may end up at a significantly higher a, because the solubility
of many salts increases significantly with temperature and the excess salt may
not be enough. Low-a, salts usually require an inordinate amount of solids.

(c) When the slurry is introduced into the container, it should cover the
entire bottom of the container. No crystals should protrude above the top
liquid layer, which should be no more than 1.5-2 mm thick. During an

64
 experiment, gain or loss of moisture may change the a, of the top layer, so
the solution should be checked occasionally and stirred to achieve
equilibrium.

(d) Table 8 lists some common salts useful for isotherms and shows the
temperature effect for each (Greenspan, 1977). For other temperatures, a plot
of ay on a semilog scale vs T~! (°K)7! can be used for extrapolation
and/or interpolation. Unlike food systems, most salts exhibit a decrease in
a, With increased temperature because they have a negative heat of solution
with increased solubility as T increases. Other salts for control of ay are
available from selected references. The Greenspan data in Table 9 represent a
statistical analysis of published information up to 1977 and are not
necessarily correct but are accepted by the FDA for regulatory purposes.

(e) Some salts are potentially toxic if they contaminate the food being
humidified. Thus KBr72, LiCl2, NaNO2, and K2Cr204 should not be
used in humidifying samples that are to be given sensory testing. In
addition, foods held above K-acetate will take on a vinegarlike flavor and
foods held over sodium nitrite absorb nitrous oxide, which catalyzes lipid
oxidation.

5. Dry desiccator
_ For essentially zero water activity, some type of material that has a type
I isotherm is needed. Commonly, calcium sulfate (Drierite) is used. This
product, which is doped with cobalt chloride, is useful because it turns from
blue to pink when it reaches its upper saturation limit. It can be
regenerated by drying in air at 150°C for 24 hours. It produces an a, of
around 0.001. Another choice is phosphorus pentoxide, but this becomes
explosive if it absorbs too much water or organic volatiles.

TABLE 9
Tables of Values for the Equilibrium Relative Humidity (% ERH)
of Selected Saturated Salt Solutions*

0 Ammonium Ammonium Potassium Stronium Potassium Potassium

Chloride Sulfate Chloride Nitrate Nitrate Sulfate

) 82.27 + 0.90 88.61 + 0.53 966339259 O77 - isi)

5 82.42 + 0.68 87.67 + 0.45 92.38 + 0.56 96.27 + 2.1 98.48 + 0.91
10 80.55 + 0.96 82.06 + 0.51 86.77 + 0.39 90.55 + 0.38 95.96 + 1.4 98.18 + 0.76
15 79.89 + 0.59 81.70 + 0.38 85.92 + 0.33 88.72 + 0.28 95.41 + 0.96 97.89 + 0.63
20 279.23 F O44 81.34 + 9.31 85.11 + 0.29 86.89 + 0.29 94.62 + 0.66 97.59 + 0.53
25m 78.57-+ 0-40 80.99 + 0.28 84.34 + 0.26 85.06 + 0.38 93.58 + 0.55 97.30 + 0.45
30 77.90 + 0.57 80.63 + 0.30 83.62 + 0.25 92.31 + 0.60 97.00 + 0.40
35 80.27 + 0.37 82.95 + 0.25 90.79 + 0.83 96.71 + 0.38
40 79.91 + 0.49 82.32 + 0.25 89.03 + 1.2 96.41 + 0.38
45 79.56 + 0.65 81.74 + 0.28 87.03 + 1.8 96.12 + 0.40
50 79.20 + 0.87 81.20 + 0.31 VT = Oo 95.82 + 0.45
55 ~*~ 80.70 + 0.35 an as
60 80.25 + 0.41
65 79.85 + 0.48
70 79.49 + 0.57
75 Qi se Ole
80 78.90 + 0.77
85 78.68 + 0.89
90 78.50 + 1.0
95
100
(continued on next page)

65
 Table 9 (continued)
i ee
EEE eee ee ee ee ee ee

ab Sodium
0c Magnesium Cobalt Potassium Strontium Sodium
Nitrate Chloride Iodide Chloride Nitrate Chloride

O- 60.35 + 0.55 ID 0.34

5 58.86 + 0.43 73.30 + 0.34 Wi ils) Gr Oe l 78.57 + 0.52 Tisye 0.27
10 57.36 + 0.33 iZntiee 0.31 75.66 + 0.09 77.53 + 0.45 75. O22
15 55.87 + 0.27 70.98 + 0.28 74.13 + 0.06 76.46 + 0.39 Oe 0.18
20 54.38 + 0.23 69.90 + 0.26 MPoard ae ADAG, 75.36 + 0.35 13% 0.14
25 52.89 + 0.22 64.92 + 3.5 68.86 + 0.24 70.85 + 0.04 714.25 + 0.32 13s O12
30 51.40 + 0.24 61.83 + 2.8 67.89 + 0.23 69.12 + 0.03 73.14 #:0.31 13d Oa ut
35 49.91 + 0.29 58.63 + 2.2 66.96 + 0.23 72065 FROL2 74, 0.12
40 48.42 + 0.37 55.48 + 1.8 66.09 + 0.23 Ti 00 ENOL SG: 74. fon)co OnrS
45 46.93 + 0.47 5256 01 <5 65.26 + 0.24 69.99 + 0.37 74. 0.16
50 45.44 + 0.60 50.01 + 1.4 64.49 + 0.26 69.04 + 0.42 74. 0.19
55 4 48.02 + 1.4 63.78 + 0.28 68.15 + 0.49 74. 0.24
60 46.74 + 1.5 63.11 + 0.31 67.25 # O57 74. 0.30
65 46.33 + 1.9 62.50 + 0.34 66.64 + 0.67 74. 0.37
70 46.97 + 2.3 61.93 + 0.38 66.04 + 0,79 1D 0.45
7: 48.80 + 2.9 61.43 + 0.43 65.56 + 0.91 15 0.55
80 52.01 + 3.7 60.97 + 0.48 65.22 °F 121 76.
85 60.56 + 0.54 O08 se 14141414
+/+
+IFIFIFIF
LHI 0.65
90 60.21 + 0.61 65 OOM an4
95
100

i
oc Potassium Sodium Lithium Potassium Magnesium Potassium
Hydroxide Hydroxide Chloride Acetate Chloride Carbonate

0 11.23 + 0.54 33.66 + 0.33 43.13

Se MONEYaeae 11.26 + 0.47 33.60 + 0.28 43513
10 12.34 + 1.4 11.29 + 0.41 23). 300 OD 33.47 + 0.24 43.14
15 10.68 + 1.1 9.57 + 2.8 11.30 + 0.35 23.40 + 0.32 33.30 + 0.21 43.15
20 9.32 + 0.90 8.91 + 2.4 11.31 + 0.31 2300 0.25 33.07 + 0.18 43.16
25 8.23 + 0.72 8.24 + 2.1 11.30 + 0.27 Zoi eee Ole 32, 2) SataOG 43.16
30 7.38 + 0.56 PE 58eP Ve] 11.28 + 0.24 POL Se (a 5)S) 32.44 + 0.14 43.17 1414141414
J++
35 6.73 + 0.44 6.92 + 1.5 11.25 + 0.22 32.05 + 0.13
40 6.26 + 0.35 6.26 + 1.2 11 2100.21 31.60 + 0.13
45 5.94 + 0.29 5.60 + 1.0 1%. L65F4021 SIF 10 nOn3
BO 35572220.27 4.94 + 0.85 11.10 + 0.22 30.54 + 0.14
Dp. 25e + 0.28 4.27 + 0.73 11.03 49023 29.93 + 0.16
60 5.49 + 0.32 3.61 + 0.65 10.95 #20226 29.26 + 0.18
65 5.41 + 0.39 2.95 + 0.60 10.86 + 0.29 28.54 + 0.21
10), “S282-4-0:50 2.29 + 0.60 10.75 + 0.33 27.770 # 0.25
75 1.63 + 0.64 10.64 + 0.38 26.94 + 0.29
80 10.51 + 0.44 26.05 + 0.34
85 10.38 + 0.51 25.11 + 0.39
90 10.23 + 0.59 24.12 + 0.46
95 10.07 + 0.67 23.07 + 0.52
100 9.90 + 0.77 21.97 + 0.60

*Adapted from Greenspan (1977).

66
B. Containers for Salt Solutions/Slurries

Depending on the amount of testing and With tehes several types of

containers can be used.

l. Desiccators
These are the standard containers for doing sorption isotherms. The large
plastic Ace desiccator with a vacuum valve on the top is most suitable and can
easily contain triplicate samples of three different foods. Glass desiccators
are more fragile, and their tops are difficult to remove if a vacuum is
eee The plastic is generally inert to the saturated slushes up to
OieGe

2. Jars
To save money, glass jars such as Mason jars can be used if an inert
plastic support for the sample can be made (e.g., inverted plastic strawberry
baskets). Care should be taken to ensure a good seal, with any cardboard in
the cover being removed and replaced with foil. At high ay, the metal tops
may tend to rust and could contaminate the food samples.

3. Fish tanks
Fish tanks make excellent humidity-control chambers, especially for
storage studies in rooms with controlled temperature. Because of their size
(5, 10, or 20 gal), a large amount of sample can be humidified, but since the
air volume is large, equilibrium time is slowed down. A tightly sealed cover
is needed, and a lucite internal platform for the samples must be used. One
should ensure that at least a l-in. deep slurry of the salt covers the bottom
to serve as the vapor source. At each sampling time, it is advisable to stir
the slurry to ensure that the top layer has not dried out or become
unsaturated. The same is true for the desiccators. The tanks permit one to
have multiple storage-test humidities in a single controlled-temperature
walk-in cabinet.

C. Sample Preparation

1. Sample size/heterogeneity
With most dry ingredients, which are very homogeneous, a sample size of
1-3 g is adequate. Problems exist with heterogeneous engineered foods such as
a cream-filled pastry, a filled pet food, or a granola bar. At point of
manufacture, the heterogeneous product may not have an equilibrated a,, In
fact, one may want to prevent equilibration (e.g., raisins and crisp cereal).
Thus, common sense must be used in deciding what sample to use. If the
product has already equilibrated, then taking a slice or using the whole
system is justifiable because grinding might induce interactions that would
not normally have occurred. If possible, each ingredient should be done
separately.

2. True adsorption isotherm--Sample initial preparation

For a true adsorption isotherm, the samples must be dried down to as close
to zero moisture level as possible without inducing any adverse reactions that
could change the system. The recommended system is drying at 30°C in a vacuum
oven in which the pump is connected through a dry ice/alcohol or liquid

67
nitrogen trap (LN>) to achieve about 27-28 in. of vacuum. Drying should be
for at least 30-40 hours. A freeze-drier operating at 100 wmHg and 80-90°F is
also adequate, but 48 hours may be required. The product could be left over
desiccant for 4-8 weeks to dry, but this increases the time needed for the
experiment.
If one is not sure that the product is truly dry at the end of this
period, some other type of moisture measurement, such as the Karl Fischer
technique, should be used. One other concern is that some products, such as
intermediate-moisture pet foods, may lose extra weight during drying due to
volatile loss or loss of glycol. A lower temperature during drying helps
prevent this.

3. Desorption isotherm--Wet tissue sample preparation

For a true desorption isotherm of tissue foods, the sample can be used as
is. The initial moisture can be measured by some reliable laboratory drying
technique (not a Cenco-type infrared oven), or the final weight loss in the
dry desiccator can be used. As above, concerns about moisture measurement
should take into account:
(a) sample heterogeneity--a large enough sample should be used.
(b) drying time/temperature--higher temperatures speed drying but allow
reactions to take place in the sample that could result in weight
losses other than those from water.
(c)direct volatile/glycol loss--this leads to errors.
(d)vacuum vs air--in general, a vacuum oven will speed drying and reduce
many of the above problems except for volatile/glycol loss. If such
loss occurs, the Karl Fisher method must be used.
In an industrial analytical laboratory, the standard moisture method and
procedure may not be the best to use in preparing the isotherm needed for
product development. However, at some point, one may have to run a comparison
test to get a correlation curve that compares moisture found in the analytical
lab to moisture used in research. One must also remember to convert moisture
contents to a dry basis, where:

H50 (% H50)
3 Neto ela ae 2 (84)
g solids 100 - (% H50)

(4 H20) = wet basis % moisture content .

To convert back to wet basis from dry basis, use:

(% H90) = 100 ° fF= |: (85)

4. Working isotherm--Initial sample preparation

For the working isotherm, the same procedure as for the desorption
isotherm is used. Either the initial sample moisture content is measured
using a proper technique (vacuum oven, freeze-drier, or Karl Fisher), or
the
final weight in the dry desiccator is taken as the dry weight to calculate

68
moisture content. The initial moisture of samples for the working isotherm or
desorption isotherm using the desiccator value is:

Wi - WwW
(%4H)0) = 100 - a (86)
oa.

where:
We = final weight of a sample after equilibrium in a dry desiccator,
and
Ww, = initial weight of the same sample.

Other devices for measuring moisture (near-infrared nuclear magnetic

resonance, dielectric, etc.) are good for commodities only if the instrument
has already been calibrated for the particular ingredient.

D. Isotherm Procedure

1. Water activity range/temperature choice

(a) Dry systems

For most dry systems, a,'s from 0.001 to 0.92 are useful to get an
isotherm that can be used over the practical food stability range. However,
if the ingredient is to be used as a humectant, higher ay' Ss would be needed.
One problem is that at a's above 0.85, rapid microbial growth may occur in
the sample and ruin it. To prevent this, a small vial of toluene (~5 cc) may
be placed in the desiccator, but such samples should not be used for
organoleptic evaluation. Other antimicrobial agents might be incorporated
into the food but might change the a),
Isotherms should be done at constant temperature, not room temperature,
because the room temperature can rise or fall dramatically over weekends. The
optimal choice would be any two temperatures from among these: 20, 25, 30, 35
and 40°C. Using two isotherms, one can construct the isotherm at the other
temperature values, which suggests that 20 and 40°C are optimal. This
procedure will also help to identify the magnitude of any possible
a,,/temperature shifts. Separate sets of desiccators allow the two
temperature isotherms to be done simultaneously.

(b) Semimoist foods

A narrower range of the isotherm can be used, generally with a low of
0.4-0.5 if the product has a critical ay in this range due to hardness, and
a higher critical a, of 0.9-0.92 due to microbial degradation. Again, two
isotherms should be done, but in the high-ay range there may be little
temperature shift effect, so one isotherm may be enough.

2. Initial sample preparation

As noted earlier, isotherms may be started with absolutely dry, with wet,
or with intermediate moisture contents. The key problem is sample
heterogeneity, which can be solved by taking a larger sample. However, this
does slow down the equilibration time. Grinding or slicing may help. Another
problem is that if equilibration is slow, microbes may grow on a wet sample
and ruin ite Toluene in the headspace can prevent this. For most dry
ingredients, a 1-5 g sample is adequate for doing the isotherm at each a,,

69
 Triplicate samples should be used if enough space is possible, and
weighing should be to 0.0001 mg. Either glass or aluminum weighing dishes
that have previously been dried in a desiccator over calcium sulfate should be
used. Covers are not necessary if the weighing is done quickly. The bulk
food sample should be covered (e.g., kept in a jar) to prevent it from losing
or gaining moisture before weighing. It is advisable to do the weighing in a
closed balance away from air currents and fluctuating temperatures. The
balance can be kept dry by storing open beakers of Drierite in the corners.

3. Equilibration time
In a vacuum or air chamber when the water vapor space concentration is
adequate, the gain or loss of moisture from the sample will depend basically
on internal resistance to moisture change and heat transfer in or out of the
sample. If the amount of sample begins to approach the total air volume, thet
the vapor pressure of water in the space cannot be maintained adequately by
evaporation from the salt slurry surface. Generally a large ratio (>10:1) of
slurry surface to sample surface prevents this, and a 20:1 ratio of air volume
to sample volume is adequate. Air holds little water; thus, increasing the
sample volume without adequate slurry surface can delay the equilibration
time. For example, at 80% RH/25°C and 760 mmHg total pressure, 1 L of space
will hold about 18.4 mg of H)0. Thus, a rapid uptake by a dry 5-g sample of
20 mg of water (i.e., to 0.4 g/100 g solids) would deplete the space moisture
entirely. Devices such as magnetic stirrers in the slurry or fans in the
space will help to maintain an adequate supply of moisture into the space but
do not speed up equilibration very much.
In general, the rate of uptake of moisture, if external diffusion of wate1
in the air space is not limiting, can be predicted from:

pete ieee, eeaDeree (87

Mo. - m Lo”

where:
Me = final equilibrium moisture,
m; = initial moisture,
m = moisture at time 9,
Deff = effective diffusion coefficient (cm/sec), and
Lo* = thickness squared (assuming drying from only one side).

As noted on pp. 45-46, this form of the equation, because of its logarithmic
nature, suggests that an infinite time is needed for the sample to reach
moisture equilibrium. However, since the error in moisture measurement is
usually + 0.24 or 2 mg per gram, the moisture reaches pseudoequilibrium in
reasonable time. The EEC recently studied 34 laboratories doing sorption
isotherms on microcrystalline cellulose; the standard deviation for any sampl.
was found to be = + 0.25 g H90/100 g solids, and the variance of all the
data was +0.17 g H)0 g/100 g solids (Spiess and Wolf, 1983). The equation
also says that the equilibrium time is proportional to thickness squared;
doubling the thickness increases the time needed by a factor of 4. Thus
sample thickness should be uniform for the triplicate samples, or errors will
result if they are assumed to reach equilibrium simultaneously. Literature
values of Dug¢ range from about 10-° cm2/sec for most freeze-dried
tissue foods to 10 *» cm*/sec for dense foods such as raisins and pasta
(as measured in drying experiments or by sorption in air). Diffusion

70
coefficients increase by a factor of around 10 when a vacuum desiccator is
used, suggesting that the presence of air in the pores of the food reduces the
rate dramatically.
As an example of calculation of equilibrium time, if an absolutely dry
l-g
sample (0.5 cm thick) was equilibrated at 32 and 82% RH (with mg's of 0.05
and 0.20 g/g solids, respectively) and if the Deff was around ors!
em2/sec, then (using an m of 0.048 g H20/100 g solids at 0.32 ay as
pseudoequilibrium, i.e., 2 mg less gain of water per gram of sample, which is
about the generally observed error in moisture measurement) ,

at 32% RH,

|0.05 - 0.0 |
Sequilibration In oe eee - (0.5)2
Soa NOt!

8.15 x 1095 sec = 9.44 days,

and at 82% RH (using an m of 0.198 g H90/100 g solids at 0.82 ay),

I0.20 - 0.0 |
Ssequilibration _ in | LO-20 — 0.198
(0.5)2
we © 1077

1.17 x 106 sec = 13.5 days.

These calculations show that, for dry samples, equilibration takes longer
for higher humidities and that the time generally will fall between 10 and 21
days for thin samples with a moderate diffusion coefficient if an error of
2 mg/g of dry solids is used. Thick samples (such as whole granola bars) or
dense samples (such as fruit pastes, raisins, and syrups) will take much
longer. Unfortunately, tables of De¢¢ do not exist for most foods. In
addition, this equation is based on no moisture limitation in the space
volume. If the evaporation rate of water from the slurry falls, then the
equilibration time will increase proportionally. At each weighing, it would
be wise to stir the slurry and to check it to ensure saturation.
Based on this, the following recommended weighing times should be used:

(a) Air desiccator

Weigh at 7-day intervals until each sample does not change by more than
2 mg/g dry weight. Generally this should take about 3 weeks, but
equilibration times at % RH values distant from the initial a, value of the
sample will be longer. Samples undergoing recrystallization will exhibit an
increase and then a decrease in weight in this period. For all samples, at
least three weighings beyond initial value are needed to ensure that
equilibrium has been reached. Grinding the sample to decrease the thickness
will speed up equilibration but might change the sorption characteristics due
to possible melting during the process.

(b) Vacuum desiccator system

Weigh twice weekly until the weight varies by no more than 2 mg/g of dry
solids. For dense samples, the vacuum system may have little advantage

ia
 external resistance will be small and the vacuum will have little
because
effect on the internal pores if they are very small.

4. Calculation of final moisture content :

e content;
Each sample should be treated individually to calculate moistur
weights should not be initially pooled or averaged . Thus, any outliers
resulting from nonequilibrium can be rejected. The calculation used depends
on the way the initial sample was treated.
(a) For an absolutely dry initial sample (i.e., mj = 0):

ee Se aie ls Bk (88)
2 g solids Wi

(b) for an initial sample at some moisture content (% H90) wet basis:

(% H90)
Gwe aw) ee eit : «|
(89)
Ez =a oy
Wi
100

E. Other Isotherm Method Problems

Several problems such as sample size, sample heterogeneity, equilibration

time, etc., have been discussed above. In addition, other problems can occur.

1. Isotherm at high temperature

Condensate will form on the inside surface of a desiccator containing
samples held at high temperature when it is brought out to room temperature
for weighing. This is because water condenses as the dew point is reached
during surface cooling. This water could drop onto the sample and cause
weighing errors. Thus, the desiccator should not be moved from the storage
temperature. It is also unwise to put good electronic weighing balances into
a high-temperature room. Rather, one should take a large empty desiccator
into the high-temperature room, quickly transfer the samples into it, and then
take the desiccator out for external weighing. The hot samples may need to
cool down for 10-20 minutes at room temperature; if they are hot when put on a
balance, the convection currents during cooling make the weight change
continuously and a measurement becomes a guess.

2. Use of vacuum
Pulling a vacuum on a desiccator to speed up equilibration time presents
several problems that may not be worth the effort.
(a) During the pulling of the vacuum, the saturated solution will begin
to boil in a few minutes. This will cause spattering of the samples
and introduce error. Putting a small layer of glass wool, about 1/2
in. thick, over the desiccator plate will prevent spattering. In
fact, this technique should be used for air Systems as well.
(b) If the vacuum is released too fast, the air streaming in could
blow
any dry powdery samples out of the weighing dishes. Slow release is
needed,

lig
 (c) During vacuum release of a hot desiccator brought into room
temperature, the colder air will cause dew point condensation, thus
contaminating the sample with water droplets.

3. Air mixing
Each time a desiccator is opened to weigh the samples, the volume of
space is disturbed and the possibility of changing the relative humidity
arises. Thus, it is important to leave the top off for as little time as
possible and to stir up the slurry before putting the samples back in. If
this is done, the previously described equilibration times will be adequate.

4. Sample mixing
Different types of samples may be put in the desiccator, but it is not
advisable to have a high-moisture sample for desorption and a dry one for
adsorption in the same chamber. This will slow equilibrium considerably.

F. Measuring ay Imstead of Doing an Isotherm

One other method is possible to create an isotherm. A set of dry samples

can be wetted with water (or a series of wet ones dried down) and allowed to
equilibrate, and then the ay, and moisture content can be measured by some
meanse This is acceptable as long as the a, device is properly calibrated
and is sensitive enough for the whole range. The AOAC standards for ay
measurement devices are given in Appendix B. A major question is how long the
sample should equilibrate before the ay is measured. Three to five days
should be adequate. This method can also be used to determine the extent of
hysteresis by doing both drying and wetting, and the a, at different
temperatures (constant moisture) can be used to get a set of isotherms as a
function of temperature.

V. Drawing the Isotherm

After data has been collected, a plot of moisture (dry basis) on the Y
axis vs ay on the X axis is made. Each sample should be a separate point on
the plot. Rather than plotting and then connecting the dots, one can draw a
smooth curve through the data. However, when the isotherm is used to
calculate the BET monolayer to get the slope for mixing or packaging studies,
the actual data points should be used and a regression analysis made. The
1983 international congress on water in foods agreed that the best equation
for describing the full shape of a type II food/moisture sorption isotherm is
called the GAB isotherm (Guggenheim-Anderson-de Boer model). It was found to
accurately fit many hundreds of food isotherms (van den Berg, 1983). The
equation has the form:

(ho ate Peete (90)

My (1 = Kay) (1 = Kay + CjKa,)

where all terms are as described before for the BET equation and C) and K
are constants. Unfortunately, one needs a minicomputer with a chip of 16 or

yh)
32 bits or larger to do the nonlinear regression needed to determine the
constants in the equation. The Federal Nutrition Research Laboratory in
Karlsruhe, Germany, has compiled a list of isotherms with these constants.
Note that since there are three constants and two variables, at least five
isotherm points are needed to solve the equation. Iglesias and Chirife (1983)
have used other isotherm equations, such as the Hailwood and Horrobin
equation, rather than the GAB model. These are linear, three-parameter
equations and thus are easier to solve for on a small computer. The Hailwood
and Horrobin equation is:

aw
eee Ch 4.Cyaan
Cuan ae (91

where C,, Cy), and C3 are constants. This does not give the monolayer
value and is therefore not as useful.
Finally, a few laboratories have resurrected the old Smith isotherm
equation, which is:

LoaGh.= as) = 0) aptaco. (92

Again, C,; and Cj are constants. This is easily solved for by plotting
In(1 - ay) vs the moisture content. As with the Hailwood and Horrobin
equation, one cannot determine the monolayer value; however, this is the
easiest one to use to extrapolate or interpolate other a,/moisture values.
As with any mathematical model, care should be taken in giving it any physical
meaning, and one should understand the limitations of the data.

74
 LITERATURE CITED

Adamson, A.W. 1962. Physical Chemistry

of Surfaces. Academic Press, New
York. ai ae
ASTM. 1979. Method E-96. Water vapor transmission rate (WVTR) method. Book of
ASTM Standards. American Society for Testing and Materials, Philadelphia.
Beuchat, L. 1981. Microbial stability as affected by water activity. Cereal
Foods World 26:345-349.
Callahan, J.C., G.W. Cleary, M. Elefant, G. Kaplan, T. Kensler, and R.A. Nash.
1982. Equilibrium moisture content of pharmaceutical excipients. Drug
Dev. Ind. Pharmacol. 8(3):355-362.
Chen, J., M. Piva, and T.P. Labuza. 1984. Evaluation of water binding capacity
of food fiber sources. J. Food Sci. In press.
Chirife, J., and C. Fontan. 1982. Water activity of fresh foods. J. Food
Sci. 47:661-663.
Chirife, J., C.F. Fontan, and E.A. Benmergui. 1980. The prediction of water
activity in aqueous solutions in connection with intermediate moisture
foods. a, prediction in aqueous non-electrolyte solutions. J. Food
Technol. 15:59-/0.
Crank, J. 1956. The Mathematics of Diffusion. Oxford University Press, London.
Duckworth, R.B. 1981. Pages 295-318 in: Water Activity: Influences on Food

Fontan, C.F., J. Chirife, and E.A. Benmergui. 1979. The prediction of water
activity in aqueous solutions in connection with intermediate moisture
foods. II. On the choice of the best a, lowering single strong
electrolyte. J. Food Technol. 14:639-646.
Franks, F. 1982. Water activity as a measure of biological viability and
quality control. Cereal Foods World 27:403-407.
Greenspan, L. 1977. Humidity fixed points of binary saturated aqueous
solutions. J. Res. Natl. Bur. Stand. Sect. A. 81:89-102.
Grover, D.N. 1947. The keeping properties of confectionary as influenced by
its water vapor pressure. J. Soc. Chem. Ind. 86:201-203.
Hermannson, A.M. 1972. Functional properties of proteins for food swelling.
Lebensm. Wiss. Technol. 5(1):24-29.
Iglesias, H.A., and J. Chirife. 1983. Sorption Isotherms of Foods; 1983.
Academic Press, New York.
Katz, M., and T.P. Labuza. 1981. The effect of water activity on the sensory
crispness and mechanical deformation of snack food products. J. Food Sci.
46:403-409.
Labuza, T.P., and R. Contreras Medellin. 1981. Prediction of moisture
protection requirements for foods. Cereal Foods World 26:345.
Makower, B., and W.B. Dye. 1956. Equilibrium moisture content and
crystallization of amorphous sucrose and glucose. J. Agric. Food Chem.
4:72-84.
Norrish, R.S- 1966. An equation for the activity coefficients and equilibrium
humidities of water in confectionary syrups. J. Food Technol. 1:25-31l.
Rasper, V.F., and J.M. DeMan. 1979. Measurement of hydration capacity of wheat
flour/starch mixtures. Cereal Chem. 57:2/-31.
Salwin, H., and V. Slawson, 1959. Moisture transfer in combinations of
dehydrated foods. Food Technol. 8:58-6l.
Sloan, AE. 1975. Ph.D. thesis. University of Minnesota, St. Paul.

19
Spiess, W., and W. Wolf. 1983. Standardization of isothem measurements.
Abstracts of Int. Symp. on Properties of Water, 3rd. Beaune, France.
van den Berg, C. 1983. Development of BET like models for sorption of water
on foods. Proc. Int. Symp. on Porperties of Water, 3rd. Beaune, France.
Waletzko, P., and T. P. Labuza. 1976. Accelerated shelf life testing of an
intermediate moisture food system. J. Food Sci. 40:137-139.
Wallingford, L., and T.P. Labuza. 1983. Evaluation of the water binding
properties of food hydrocolloids by physical/chemical methods and in a
low fat meat system. J. Food Sci. 48:1-4.
Wolf, M., J. E. Walker, and J.G. Kapsalis. 1972. Water vapor sorption
hysteresis in dehydrated foods. J. Agric. Food Chem. 20:1073-1076.

76
 APPENDIXES
Appendix A

TABLE 1
VAPOR PRESSURE OF WATER BELOW 100°C
(Pressure of aqueous vapor over water in mm Hg for temperatures
from —15.8 to 100°C).

0.0 0.4 0.6 0.8 Temp. °C 0.0 0.2 0.4 0.6 0.8
1.436 1.390 1.368 1.345 42 61.50 62.14 62.80 63.46 64.12
1.560 1.511 1.485 1.460 43 64.80 65.48 66.16 66.86 67.56
1.691 1.637 1.611 1.585 44 68.26 68.97 69.69 70.41 71.14
1.834 1.776 1.748 1.720
1.987 1.924 1.893
45 71.88 72.62 73.36 74.12 74.88
1.863
46 75.65 76.43 77.21 78.00 78.80
2.149 2.084 2.050 2.018 47 79.60 80.41 81.23 82.05 82.87
2.326 2.254 2.219 2.184 48 83.71 84.56 85.42 86.28 87.14
2.514 2.437 2.399 2.362 49 88.02 88.90 89.79 90.69 91.59
2.715 2.633 2.593 2.553 50 92.51 93.5 94.4 95.3 96.3
2.931 2.843 2.800 2.757 51 97.20 98.2 99.1 100.1 101.1
3.163 3.069 3.022 2.976 52 102.09 103.1 104.1 \ 105.3 106.2
3.410 3.309 3.259 3.211 53 107.20 108.2 109.3 110.4 111.4
3.673 3.567 3.514 3.461 54 112.51 113.6 114.7 115.8 116.9
3.956 3.841 3.785 3.730 55 118.04 119.1 120.3 121.5 122.6
4.258 4.135 4.075 4.016 56 123.80 125.0 126.2 127.4 128.6
4.579 4.448 4.385 4.320 57 129.82 131.0 132.3 133.5 134.7
4.579 4.715 4.785 4.855 58 136.08 \ 137.3 138.5 139.9 141.2
4.926 5.070 5.144 5.219 59 142.60 143.9 145.2 146.6 148.0
5.294 5.447 5.525 5.605 60 149.38 150.7 152.1 153.5 155.0
5.685 5.848 5.931 6.015 61 156.43 157.8 159.3 160.8 162.3
6.101 6.274 6.363 6.453 62 163.77 165.2 166.8 168.3 169.8
6.543 6.728 6,822 -6.917 63 171.38 172.9 174.5 176.1 177.7
7.013 7.209 7.309 7.411 64 179.31 180.9 182.5 184.2 185.8
7.513 Te 7.828 7.936 65 187.54 189.2 190.9 192.6 194.3
8.045 8.267 8.380 8.494 66 196.09 197.8 199.5 201.3 203.1
8.609 8.845 8.965 9.086 67 204.96 206.8 208.6 210.5 212.3
9.209 9.458 9.585 9.714 68 214.17 216.0 218.0 219.9 221.8
9.844 10.109 10.244 10.380 69 223.73 225.7 227.7 229.7 231.7
10.518 10.799 10.941 11.085 70 233.7 235.7 237.7 239.7 241.8
11.231 11.528 11.680 11.833 71 243.9 246.0 248.2 250.3 252.4
11.987 12.302 12.462 12.624 72 254.6 256.8 259.0 261.2 263.4
12.788 13.121 13.290 13.461 73 265.7 268.0 270.2 272.6 274.8
13.634 13.987 14.166 14.347 Ta C2772 279.4 281.8 284.2 286.6
14.530 14.903 15.092 15.284 75 289.1 291.5 294.0 296.4 298.8
15.477 15.871 16.071 16.272 76 301.4 303.8 306.4 308.9 311.4
16.477 16.894 17.105 17.319 Ch 314.1 316.6 319.2 322.0 324.6
17.535 17.974 18.197 18.422 78 327.3 330.0 332.8 335.6 338.2
18.650 19.113 19.349 19.587 79 341.0 343.8 346.6 349.4 352.2
19.827 20.316 20.565 20.815 80 355.1 358.0 361.0 353.8 366.8
21.068 21.583 21,845 22.110 81 369.7 372.6 375.6 378.8 381.8
22.377 22.922 23.198 23.476 82 384.9 388.0 391.2 394.4 397.4
23.756 24.326 24.617 24.912 83 400.6 403.8 407.0 410.2 413.6
25.209 25.812 26.117 26.426 84 416.8 420.2 423.6 426.8 430.2
26.739 27.374 27.696 28.021 85 433.6 437.0 440.4 444.0 447.5
28.349 29.015 29.354 29.697 86 450.9 454.4 458.0 461.6 465.2
30.043 30.745 31.102 31.461 87 468.7 472.4 476.0 479.8 483.4
31.824 32.561 32.934 33.312 88 487.1 491.0 494.7 498.5 502.2
33.694 34.471 34.864 35.261 89 506.1 510.0 513.9 517.8 521.8
35,663 36.477 36.891 37.308 90 525.76 529.77 533.80 537.86 541.95
37.729 38.584 39.018 39.457 91 546.05 550.18 554.35 558.53 562.75
39.898 40.796 41.251 41.710 92 566.99 571.26 575.55 579.87 584.22
42.175 43.117 43.595 44.078 93 588.60 593.00 597.43 601.89 606.38
44.563 45.549 46.050 46.556 94 610.90 615.44 620.01 624.61 629.24
47.067 48.102 48.627 49.157 95 633.90 638.59 643.30 648.05 652.82
49.692 50.774 51.323 51.879 96 657.62 662.45 667.31 672.20 677.12
52.442 53.580 54.156 54.737 97 682.07 687.04 692.05 697.10 702.17
55.324 56.51 57.11 57.72 98 707.27 712.40 717.56 722.75 727.98
58.34 59.58 60.22 60.86 99 733.24 738.53 743.85 749.20 754.58
100 760.00 756.45 770.93 776.44 782.00
101 787.57 793.18 798.82 804.50 810.21
 TABLE A2
Water Sorption Properties of Glucose
Adsorption Desorption Desorption
(Desiccator) (Desiccator) (VPM)
aw ae ayy M,* ay m,*
Oo LL -08 0.11 2.98 (crystallized out
below a, = 0.73)
0.33 07 0.33 3.66

0.44 ah 0.44 3.56 0.73 52.00

0.52 =20 0.52 10.23 0.78 61.00

0.68 9.33 0.68 11.86 0.83 82.00

0.75 10.06 0275 12.00 0.91 113.00

0.85 10.600 0.85 12525 0.92 150.00

0.88 9.99 0.88 1Wiape? fe 0.96 400.00

0.91 90.85 0.91 Dipeas 0.97 900.00

0.97 185.37 0.97 384.05

TABLE A3
Water Sorption Properties of Fructose 2
Adsorption Desorption Desorption
(Desiccator) __ @esiccator) (VPM)
ayy mM¢* aw M¢* aw mo*
0.11 -02 0.11 3.o7 (crystallized out
below a. 5 0.73)
0.33 45 0.33 8.98

0.44 99 0.44 oe iz 0.73 39.00

O52 -60 O52 14.25 0.82 67.00

0.68 31.91 0.68 26,72 0.89 150.00

0.75 43.40 0.75 45.25 0.91 163.00

0.85 69.19 0.85 68.96 0.93 233.00

0.88 79.47 0.88 82.00 0.95 400.00

0.351 uO oe be 0.91 T4 Sh. 0.97 900.00

0.97 368.04 0.97 mold

*mc = moisture content = g water/100 g solids @ 23°C.

78
 TABLE A4
Water Sorption Properties of Sucrose
Adsorption Desorption Desorption
(Desiccator) (Desiccator) (VPM)
ay mi,.* ay mo* ay m,*

0.11 -02 0.11 2.18 (crystallized out

below a, =.0.63)
0.33 -02 0.33 2o2k

0.44 -03 0.44 1.68 0.63 25.00

0.52 -03 10352 2533 0.86 49.00

0.68 cen 0.68 3.89 0.92 82.00

0.75 224 0.75 10.10 0.93 100.00

0.85 5.38 0.85 48.76 0.94 150.00

0.88 49.62 0.88 56.48 0.96 233.00

0.91 EY Ps , OF91: 74.08 0.97 567.00

0.97 2iic28 0.97 253.64

TABLE A5
Water Sorption Properties of Lactose ae
Adsorption Desorption Desorption
(Desiccator) (Desiccator) rout SVPMe =
ay Mc* ayy Me™ ay Mc*
OL -08 Ost1 2507 (crystallized out
/ below ae 0.93)
0.33 - 06 0.33 2.68

0.44 29 0.44 2.68 0.93 120.00

OF52 nap 0.52 2.94 0.94 190.00

0.68 mat Ss 0.68 3.00 0.95 233.00

0.75 Pe BS) O.73 3.09 0.97 400.00

0.85 ok 0.85 3.09

0.88 19 0.88 3.08

0.91 <3 0.91 3.16

0.97 ded 0.97 246.64

¥mo = moisture content = g water/100 g solids @ 23°C.

79
 TABLE A6
Water Sorption Properties of Corn Syrup Solids
Adsorption Desorption Desorption
(Desiccator) (Desiccator) (VPM)
ay M* ay Me* ay Me*
Ogi ee O2EL 5.29 (crystallized out
below a, = 0.61)
0233 2.45 0233 6.26

0.44 6.57 0.44 8.88 0.61 18.00

0.52 10.00 0.52 10.78 G272 25.00

0.68 18.53 0.68 19.71 0.83 43.00

0.75 23°77 0.75 233015 0.86 53.00

0.85 B72 42 0.85 33226 0.92 100.00

0.88 44.24 0.88 43.77 0.96 150.00

0.91 94.07 0.91 mold 0.97 233.00

0.97 196.95 0.97 243.08

*m. = moisture content = g water/100 g solids @ 23°C. >

TABLE A7
Moisture* Sorption Isotherms of High Fructose Corn Syrup (11 weeks)
Clinton Isomerose Clinton Isomerose Clinton lsomerose

0 0.08772 0.08714 0.08656 0.08588

0.11 0.07957 0.09041 0.07536 0.07410

0.22 0.11258 0.08644 0.07942 0.07382

Ons) 0.08302 0.08484 0.08370 0.07493

0.40 0.0959 0.10366 0.09994 0.09716

0.44 0.12622 0.11136 0.13030 0.12974
On52 0.12145 0.12208 0.16485 0.12901
0.65 0.18859 0.18136 0.25010 0.25160
OR75 0.34014 0.37329 0.39191 0.39598

0.85 0.60901 0.60358 0.61767 0.61984

0.98 (1.88637) ** @e24155) (2.29310) (2.17738)

2.21667 PLS SVT 2.39139 2.39736

ee ll

*Moisture = g H90/g solids.

**Eight-week sample (adsorption-desiccator method).

80
 TABLE A8
Water Sorption Properties of NaCl
Adsorption Desorption Desorption
(Desiccator) (Desiccator) (VPM)
aw aS ayy Mo* ayy m,*
Oe -13 O1L 16.97 (crystallized out
below a, = 0.75)
0.33 ke 0.33 15.92

0.44 oiZ 0.44 Tos12 0/3.) 270.00

0.52 wi2 0.52 bic19 0.85 567.00

0.68 <3 0.68 15.93 0.93 1328.00

OntS 6.44 On /5 330.85 0.96 1900.00

0.85 391.46 0.85 437.58 0.97 2400.00

0.88 473.15 0.88 545.68

0.91 600.31 Om oa: 752.99

0.97 1037.31 0297! = ane2h70a15

TABLE A9
Water Sorption Properties of Potassium Chloride ‘ee
Adsorption Desorption Desorption
(Desiccator) (Desiccator) (VPM)
ay m,* ay Me* ayy Nc*
Ct 08 O72) (crystallized
out below
0.33 08 0.33 2,03 = 0.86)

0.44 Lt 0.44 2.61 0./86-- 6370.00

G25? meaat 0.52 2.66 0.89 588.00

0.68 RA 0.68 2.84 0.93 900.00

0.75 Bt 4 0.75 eet 0.96 1900.00

0.85 oh 0.85 6.43

0.88 Peba 0.88 315.14

0.91 Pik 0.91 448.84

0.97 1128.59 0-97 2228.59

*mo = moisture. content = g water/100 g solids @ 23°C.

81
 TABLE A10
Glycerol Water Sorption Isotherm at 23°C*

Moisture Content
ay (g water/100 g solids)

0.95 625
0.90 pat8,
0.85 145
0.80 108
0.75 82
0.70 64
0.60 41
0.50 27
0.40 18
0.30 12
0.20 10
0.10 »,

*(Note: no hysteresis by any method.)

TABLE All
Water Sorption Properties of Propylene Glycol beh toe
Adsorption Desorption Desorption
(Desiccator) (Desiccator) (VPM)
ay Mo* aw Mc* ay m,*
0.11 0.558 Coie evap. 0 0

0.33 7.99 0.33 evap. 0-30 11.00

0.44 14.98 0.44 evap. 0.50 25.00

0.52 27.46 0252 evap. 0.67 54.00

0.68 a2720 0.68 evap. 0.78 100.00

0.75 64.47 0275 evap. 0.86 186.00

0.85 147537 0.85 147.50 0.93 400.00

0.88 162,01 0.88 184.20 O29 566.00

0.91 204.59 bese 254.40 0.97 900.00

0.97 408.15 0.97 738.90 0.99 1329.00

a
a a ee

*m. = moisture content = g water/100 g solids @ 23°C.

82
 TABLE Al2
Water Sorption Properties of 1 ,3-Butylene Glycol
Adsorption Desorption Desorption
(Desiccator) (Desiccator) (VPM) "
ow m,* aw Me* ayy M,*
0.11 1.30 Gort evap. 0 0

0.33 3210 0.33 evap. 0.35 11.00

0.44 6.13 0.44 evap. 0.57 25.00

0.52 9.41 0.52 evap. 0.74 54.00

0.68 16,12 0.68 40.30 0.83 100.00

0.75 23.46 OF75 48.90 0.89 186.00

0.85 89.12 0.85 98.40 0-93 400.00

0.88 125.94 0.88 124.70 0.94 471.00

0.91 170. 34 0591 180.00 0.97 900.00

0.97 410.15 Co is 107210

TABLE Al13
_____ Water Sorption Properties of Polyethylene Glycol 400 _
Adsorption Desorption Desorption
(Desiccator) (Desiccator) x (VPM)
aw M¢* aw Mc* aw Me*
O. 11 fWe 0.11 Zeou 0 0

0.33 6.77 0.33 6.84 0.42 11.00

0.44 10.30 0.44 18 WR 02 0.59 25.00

i pe 4 LOs39 0-52 £6,090 275 54.00

0.68 33.05 0.68 33302 0.88 100.00

0.75 47.04 0.75 44.01 0793S 186.00

0.85 75.08 0.85 7162S 0.96 400.00

0.88 81.02 0.88 80.72 0.965 567.00

0.91 117.45 0.91 £15.99 0.97 900.00

0.97 282.93 0.97 456.87

*mo = moisture content = g water/100 g solids @ 23°C.

83
32. Vegetable Products, Processed
(f) Water bath.—Capable of maintaining temp. const
Water Activity (7)}—Official First Action
0.1° at 25+1°: capacity sufficient to hold measuring chan
32.004 Principle selected app.
Water activity, a,, is ratio of vapor pressure of H,O in product (g) Hydrophilic solid.—Microcryst. cellulose, Type |
to vapor pressure of pure H,O at same temp. It is numerically (FMC Corp., 2000 Market St, Philadelphia, PA 19103, or ¢
equal to 1/100 of feiative humidity (RH) generated by product (h) Reference salts.—ACS reagent grade, fine cryst
in closed system. RH can be calcd from direct measurement of Table 32.01.
partial vapor pressure or dew point or measured indirectly by
sensors whose physical or elec. characteristics are altered by
RH to which they are exposed. Instruments are checked or Table 32:01 Water Activity of Reference Salt Slushes
calibrated on basis of RH generated by std salt slushes. Sait a Sait
MgCl, 0.328 KBr 0.
32.005 Instruments and Systems K,CO, 0.432 (NH,),SO, 0.

(Select 1 of following instruments or systems to perform test. Mg(NO3;)2 0.529 KCI 0.

Each hes different application limitations because of interfer- NaBr 0.576 Sr(NO3)2 0.
ences from other volatile components of products being meas- CoCl, 0.649 BaCi, 0.
ured. Check with instrument manufacturer for more specific SrCh 0.709 KNO, 0.
limitations.) NaNO, 0.743 K,SO, 0.
NaCl 0.753
(a) Change in electrical conductivity of immobilized salt
so/n.—instrument available from American Instrument Co.;
Beckman Instruments, Inc., 89 Commerce Rd, Cedar Grove, NJ
07009; Nova Sina AG, Andreastrasse 7-11, CH 8050, Zurich,
Switzerland; or Rotronic AG, CH 8047, Zurich, Switzerland. 32.007 Preparation of Reference Saft Si
jsnmobilized salt sensors are affected by polyols such as glycerol Place selected ref. salt in test container to depth of ca
and glycol and by volatile amines. for more sol. salts (lower 8.), to depth of ca 1.5 cm for les
(b) Change in electrical capacitance of polymer thin films.— salts (higher @.), and to intermediate depth for interme
Instrument available from WeatherMeasure, 3213 Orange Grove, salts. Add H,O in ca 2 mL increments, stirring well with s¢
N Highlands, CA 95660 or General Eastern Corp., 36 Maple St, after each addn, until salt can absorb no more HO as evid
Watertown, MA 02172. Note: Polymer thin film sensors are by free liq. Keep free liq. to min. needed to establish satn «
affected by HOAc. with H,O. Slushes are ready for use upon completion of m
(c) Dew point by chilled mirror technic.—instrument available and are usable indefinitely (except for some high a,
from EG&G, Inc., Environmental Equipment Div., 151 Bear Hill susceptible to bacterial attack), if contained in manner to pr
Rd, Waltham, MA 02154 or General Eastern Corp. Dew point substantial evapn losses. Some siushes, e.g., NaBr, may s¢
measurements can be affected by condensables with lower gradually by crystal coalescence, with no effect on a,.
critical temp. than H,O.
(d) Longitudinal change in dimensions of water-sorbing fi- 32.008 Calibt
ber.—instrument available from Abbeon Cal, Inc., 123 Gray Ave,
Santa Barbara, CA 93101 or G Lufft Metallbarometerfabrik, D- Select 25 salts to cover a,, ranges of interest or range of s
7, Postfach 692, Neue Weinsteige 22, Stuttgart, West Germany. being used. Measure humidity generated by each salt sit
(e} Partis/ water vapor pressure by manometric system.— terms of instrument readout, as in 32.009. Plot readout a
Partial H,O vapor pressure measurements can be made useless 8, values given in Table 32:01 for selected salts, using «
by living products that respire, such as grains or nuts; by active section paper scaled for recding to 0.001 a, unit. Draw be
fermentation; or by products that expand excessively when smooth line thru plotted points. Use this calibration li
subjected to high vac. transiate sensor instrument readout of samples toa, or to:
(f) Relative weight of moisture sorbed by anhydrous hydro- vapor pressure or dew point instruments for proper functic
philic solid, e.g., microcrystalline cellulose.—See J. Agr. Food
Chern. 22, 326(1974). 32.009 Determin

32.006 Apparatus and Reagents Place calibration slush or sample in forced-draft cabine
or H,0O bath, (f), until temp. is stabilized at 25+1°. Transfe
{As needed for instrument or system selected) slush or sample to test container, (e), seal container with se
(a) Dew point instrument.—Equipped to measure temp. to device attached, and place in temp. control device. Use \
+0.1°. See 32.005(c). sample or slush >1/20 total vol. sample container plu
(b) Forced-draft cabinet.—Const temp., set to maintain 25=1°: associated void vol. of sensing system, but not so much
capacity =0.06 m® (2 cu ft); with access port to accomodate interfere with operation of system. Record instrument res
instrument sensor leads. Use in conjunction with (ec). at 15, 30, 60, and 120 min after test container is placed in
(c) insulated box with cover.—Large enough to hold test control device, or record response on strip chart. Two cx
container, (e), and small enough to fit in forced-draft cabinet, utive readings, at indicated intervals, which vary by <0
(b); with access port to accomodate instrument sensor leads. unit are evidence of adequately close approach to equilit
Protect test container from short-term temp. fluctuations. Continue readings at 60-min intervals, if necessary. Conve
(d) Manometric system.—Sensitive to pressure differential of reading to 4, by calcn from physical measurements or t
+0.01 mm Hg (1.33 Pa). See 32.005(e). to calibration line. Make all measurements within ran
(e) Test containers.—120 or 240 mL (4 or 8 oz) wide-mouth calibration points; do not extrapolate calibration line. Mi
or Mason glass jars with Al- or Teflon-lined screw caps and measurements in same direction of change, and, if requi
gaskets. Check integrity of cap seals and sensor leads by any Properties of sensor, expose sensor to controlled RH
means available, e.g., ability of system to hold vac., using Tesla ambient before starting each measurement.
coil.

AOAC. 1980. Official Methods of Analysis, 13th ed. Assoctatilonvor Officials

Analytical Chemists, Washington, DC. pp. 537-538. Used by permission.

84
 REFERENCE LISTS

The following references are segregated by category; however, some are in

more than one category.

PROPERTIES OF WATER

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412301-303

85
Chang, C.C., and B.G. Kyle. 1979. Sorption and desorption kinetics of carbor
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Goto, S., and T. Isemura. 1964. Studies of the hydration and the structure
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 MOISTURE CONTENT, a, AND ISOTHERM MEASUREMENT

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146
 INDEX

Activity Critical a, values, 23, 26, 27,

thermodynamic, 2 69
Gr water, 1.73 Critical moisture content, 23, 25,
Activity coerfecient, 5,°6, 52,°53 27
Air currents, effect on isotherm, Cryoscopic osmometers, 6
70 Crystalline materials, 10, 52
Air space, effect of its volume on isotherm curve, 9, 13, 15
as, 35°73 from noncrystalline substances,
Amorphous material, 13, 14, 15 N36)
Amorphous-crystalline transfer, Curves, isotherm
bo=Eoy 27 general, 8
Anticaking agents, 10 type see
isotherm curve, 9 type II, 9, 14
AOAC standards, 84 type III, 9
Approximations, successive, 50-51
ay, defined, 4. See also Water Dehydrated foods, 8
activity isotherm curve, 9
monolayer values, examples, 26
Barriers, to moisture exchange, Desiccant, 325 53
. 44 Desiccator, 6/7, 68, 69
BET method, 7 alert
isotherm equation, 22, 23, 24 vacuum, 71-72
monolayer calculation, 23, 24, Deterioration, of foods, 22, 43,
73 63
Binding energy, excess, 16 Dielectric measuring devices, 69
Binding of water, 7 Diffusion
effect on chemical potential, 4 constants, 49-51
effect on quality, 4 limited by solids, 50, 51
Bonding one-sided, 50
hydrogen, 6, 13 two-sided, 5l
hydrophobic, 7 Diffusion coefficient
Bonds, 7 effective 51] ,-/70,, 71
dipole-dipole, 4 internal, 48
hydrogen, 4, 7, 9, 10 overall, 49
fouie, 4, / Diffusivity, 48
1,3-Butylene glycol, 83 barrier to moisture exchange, 44
effective, 50
Caking, of sugars, 27 Dry foods, 63, 69
Calcium sulfate, 65, 70
Capillary effect, 6-7, 9 EEC study, 70
Chemical potential, 4, 21, 32 Effective diffusivity, 50, 70
defined, 2-3 Ej values, 56
Clausius Clayperon equation, 16, Electrolytes, 4, 5
20 Energy, free, 2
Cobalt chloride, 65 Engineered foods, 27, 67
Colligative effect, 4-6 Equilibration, 3
at low aw» 6 time, 67; 69, :/0-/2;./3
Computer-based solutions, 47, 49 Equilibrium moisture content, l,
Containers, for salt solutions, B06 ot 40242
67 Equilibrium relative humidity, 4,
Corn syrup solids, 80 L745 6D
Crispness, of dry foods, 25-26 Equilibrium water activity, 38, 39
and infinity, 46, 70
mathematical model, 39

147
Error Headspace
of measurement, 60, 70, 71 activity in. oy 4
sources, (04.65, 69, -72 amount ‘of, 1, 2
Error function solution, 48, 49 Heterogeneity, of isotherm sample,
Examples 67,0085" 09
dog food, 58-62 High-fructose corn
potato chips, packaging solids, 58, 61-62
film for given shelf life, syrup, 80
BA=38 Humectant, 8, 52, 69
time to loss of crispness, selection, 51-63
SUeor Humidifiers, mechanical, 64
propylene glycol, added to meat, Humidity, devices to control, 64
52-59 Hydrogen bonds, 4, 7
Experiments, moisture exchange, Hydrophobic bonds, 7
I=2 Hysteresis, 9-I35 Li, 525403
Extruder, ay in, 21 by adsorption process, 9
defined, 8
Federal Nutrition Research by desorption process, 10
Laboratory, Germany, 74 and initial a,, 12
Film permeability. See practical aspects, 12
Permeability
Fish tanks, to contain slurries, Intermediate moisture foods, 5l,
67 203i," OS
Food Isotherms
properties controlling a,, 4-7 adsorption, 8, 52, 6/7, 68
quality, 4. See also Quality constants, 74
loss curve, general, 8
Free energy, 2 defined, for food, 3-4
Freeze-dried foods, 50, 70 desorption, 8, 52, 68
Freezing point, 4 determination of, 64-73
depression, 5, 56 different, for analysis and
Pructose, 13, 53;,54,,58,.7/8 product development, 68
drawing, 73-74
Gas for fibers, 41
activity of molecular species for gums, 40
in 33 at high temperature, 72
a, in, 4 for humectants, 78-83
Glucose.w14), 53. 54, 305:02,,40 problems, 72-73
Glycerol, 52, 54, 82 procedure, 69-72
with water, to control humidity, shapes, typical, 8-21
64 at high a,, 43
Glycol. See Polyethylene glycol at low ay, 8-10, 43
Grover equation, 56, 57, 58, 59, uses, 22-63
60 working, 13
E; values, 56 Iteration, 47
prediction by, 58-59, 61,62
Guggenheim-Anderson-de Boer Jars, to contain slurries, 67
isotherm model, 73
K values, 54
Hailwood and Horrobin isotherm Karl Fischer technique, 68
equation, 74 Kelvin equation, 12
Hardness, 69 defined, 6
Otuarysroods , 25.27, effect, 7
predictionibysay
Kinetic mmdts ss

148
 Lactose, 13, 54, 79 Mylar bags, 30, 36, 37
Lithium chloride, 64, 65 calculation of permeability,
Bu38 3)
Maltose,
53, 54
Microbiology, 27 Near-infrared nuclear magnetic
Microorganisms resonance devices, 69
growth of, on sample, 69 Noncrystalline substances,
spoilage by, 29 isotherm curve, 13
toxins from, 28 Norrish equation, 58
Mixtures, of dry ingredients, defined, 53
36-51 K values for, 54
equilibrium ay, 39-43
permeability and diffusion Package temperature shift, 62
constants, 49-51 Packaging example, 30-38
rate of moisture gain/loss, Partial vapor pressure, 1
44-49 Percent relative humidity,
Models, mathematical defined, 1
for determination of Permeability, 30, 49
permeability and diffusion, barriers to moisture exchange,
49—51 44
for equilibrium in mixtures, calculation of , 31-35
39-43 constants, 49, 5l
for rate of moisture gain/loss measures of, 34
in mixtures, 44-49 value, 49-50
assumptions, 44 Phosphorus pentoxide, 65
external environment constant, Polydextrose, 6
44-46 Polyethylene bags, 30, 36, 37
general, 44 calculation of permeability,
source/sink not point sources, Sg 1S)
48-49 Polyethylene glycol 400, 54, 83
source/sink point sources, Peres in foods, °6, 71, 72
46-48 Potassium chloride, 54, 64, 81
Moisture content Potassium dichromate, 64, 65
prierears 23, 25>, 313234, 37 Potato chips. See Examples
dry-wet basis conversions, 68 Prediction
equilibrium, 1, 30, 31, 40, 42 of change in ay, 5, 53-58
final, calculation of, 72 for packaging, 27, 30-38
ined, 82 e302 549 685° 69 Preparation of sample, for
Moisture exchange isotherm, 6/7
experiments, l inte tale OS. 09-70
rate of uptake, 70 wet sample, 68
Moisture gain/loss Pressure
equations, 27, 30 partial, 3
mathematical models, 44-51 botal, v3-7-21
maximum allowable, 27 vapor, ly 4, 245, 30
permeability and diffusion Propylene glycol, 52, 54, 58, 60,
constants, 49-51 68, 82. See also Examples
sample calculations, 30-38 Pseudoequilibrium, 70
Moisture gradient, 48, 49
Moisture sorption hysteresis. See Quality Loss, 22,-57,,63
Hysteresis. below the monolayer value, 23
Moisture sorption isotherms. See
Isotherms RACdTtAS Law 1,00; lO ols oo.
Monolayer value, 7, 12, 22, 74 De DOG OUT Ol
examples, for dehydrated foods, defined, 5
26

149
 effects 2/29 Time
prediction Dbyww6.052-53 to ay equilibrium, 46, 70-72
Recrystal lization, 13,14, 71 critical, for crispness loss, 37
Regression analysis, 25, 73 weighing, 71-72
Ross equation, 57-58 Toluene, 69
prediction by, 59-60, 61-62 Total pressure effect, 21
Transfer, of moisture, across
Sample preparation, for isotherms, fi ims az
67
heterogeneity, 67, 68, 69 Unaccomplished moisture
ipttial. 67-65., /2 change, 51
size, 67, 69 content, 30
Samples gain, 36
aEY {250.71 ratio, 30, 49
high aw, 50 Uses of isotherms, 22-63
thick, </1
Poen 7b Vacuum, on desiccator, 72-73
Salt solutions, to control _ van der Walls forces, 7
humidity, 64, 65 Vapor pressure, 1, 30, 77
Semimoist food systems, 8, 27, 69 colligative effect on, 4
Shelf life, 23, 37, 46 external, 32
Oredryetoods, 22,, 63 internal, 32
Slurries, use in determining partial, l
isotherms, 64-67 Vapor pressure manometric method,
starring. ‘70% 73 bya, sy)
Smith isotherm equation, 74
Sodium chloride, 54, 81 Water activity
Sodium nitrate, 64, 65 controlled by food properties,
Solids 4-7
amorphous, 13 critical values, 23, 26, 27, 69
crystalline, 13 defined, 1, 3,4
Solute equilibrium, 38
to depress ay, 51, 54 in headspace, 3
ideal, 5 low range
Solutions colligative effect in, 6
from crystals, 10 isotherm curves in, 8-10
Saturated, 10, 64, 65-66 surface interaction in, 7
SUC DOSC Rr AS10504, 098.5 measuring instead of doing
DonkO2s 19 isotherm, 73
replacement of, example, 61-62 range, choice for isotherm, 69
Sulfuric acid/water mixtures, to standards, AOAC, 84
control humidity, 64 Water sorption properties, of
Surface adsorption, 9 ingredients, 78-83
Water vapor transmission rate
Temperature, 68, 69, 70, 73 unites; 32
choice of, for isotherm, 69 Wheat, 17,5: 18, 299 20g2>
constant, 4, 16 Working isotherm, 13, 30
effect, 16-20 for packaging prediction
isotherm dependent on, 4, 62 examples, 31
Smite, 62, 63,-69 preparation of sample, 68-69
Thermodynamic activity, 2
Thickness, of sample, 48, 50, 70,
71
uniformity needed, 70
$945
150
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