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Summary to Date

Solutions are thermodynamically stable within a


range of temperatures and compositions.
Solutions more concentrated than their limit will
tend to crystallize until the residual solution is
back at the saturation limit.
Crystal formation requires the formation of a
nucleus which can be a slow process due to the
trade off between surface energy costs (G>0) and
volume energy gains giving a free energy barrier
for the formation of small crystals.

Almost always heterogeneous nucleation is


faster than homogeneous nucleation.
More solid will then deposit on the nuclei
(crystal growth) until the supersaturation is
relieved.

Inventors: Alan J. Forage & William J. Byrne


Assignee: Arthur Guinness Son & Co., Ltd.
The gas pod in the can is blow molded with nitrogen (N).
A laser zaps a hole in the pod. (they experimented with holes
between 0.2mm and 2.5mm finding that 0.61 mm as ideal)
Pod is inserted in the bottom of can.
Can is filled with CO2/N supersaturated stout. N is present at 1.5%
v/v min up to 3.5% v/v. (FYI, vol/vol is the number of volumes of gas
which are dissolved in a unit volume of beverage at 760mm of Hg &
15.6 oC) CO2 is present at between 0.8 and 1.5% v/v.
During filling, foam rises to top of can. This clears the air.
A charge of liquid N is added to the stout.
Can is sealed.
As liquid N boils off in can during pasteurisation (60 oC for 15-20
min), top of can pressurizes and forces the stout into the pod, thus
compressing the ambient pressure N in the pod.
Equilibrium is reached at about 25 psi.

Mechanism of Growth
Crystal

Melt

There is a surface
tension between phases

Solid molecules strongly


attract other ice molecules

Small Crystals

Solid molecules in small


crystals are less strongly
attached than those in large
crystals

s 2. .M
RT ln
s
.r
r = crystal radius
s = crystal solubility

increase in solubility

The Kelvin Equation


100.00%
10.00%
1.00%
0.10%
0.01%
0.001 0.01

0.1

Particle size

Ostwald Ripening
<<disappear>>
diffusion

diffusion

diffusion

diffusion

Stages in Crystal Growth


Nucleation (homogeneous or
heterogeneous)
Growth (no change in crystal number)
Perfection

What if it doesnt crystallize?


(at a molecular level, how do things
crystallize?)

Fondant Manufacture
Cook to 114-120C
Cool quickly and gently to 45C
Vigorously mix until all clarity is lost and a
creamed malleable mass is formed
Ripen and mature for 24 h

Th
t r a er m
ns od
iti y n
on a

mi
c

pr
es

su
re

fo
r

ph
a

la
u
c
le
o
M

it
l
i
b
o
rm

se

Glass
transition
temperature

Melting point

Temperature

15

Log

GLASS

12

RUBBER

SOLUTION

20-100oC

0
Tg

Tm

Solution

Temp, oC

60

S.S.
soln.

30
0

TE

Ice+Soln.

Tg

Ice+S.S. Soln.

Glass

Ice+S.S. glass

Conc. Solute, %

100

Ice Crystals in Ice Cream

50 m

Crystal detectability

Sensory smoothness

Sensory Effects of Ice Crystals

25

50
Ice Crystal Size (m)

Thermodynamics of
Crystallization
Temperature

Solution

Glass

Concentration

Freezing Point Curve


Water frozen

100%

50%

0%
0

-10

-20
Temp /C

-30

-40

Simplified Flow Chart


-18C

-5C
Freezer

Hardening

-15C
Distribution

The Ice-Cream Freezer


Mix is cooled to
about -10oC
Vigorous mixing
Air is incorporated

Effect of Dasher

1. Ice crystals
grow from cold
wall

2. Dasher cuts
off dendrite

3. Dendrite grows
in barrel center

Domestic vs Commercial
Freezers
Why do commercial freezers make
smoother ice cream than domestic
freezers?
Boiling ammonia 30C
Saturated brine 10C

Hardening
At the freezer exit the product is packed
and cooled to -18C in a tunnel freezer
How does the
number and size
of crystals change
in the hardening
room?

Water frozen

100%

50%

0%

-10

-20
Temp /C

-30

-40

Distribution

Plant freezers
Refrigerated distribution
Store freezers
Domestic freezers

transfer
transfer
transfer

How does the number and size of crystals


change during distribution?

Ice Coarsening
Ice cream may coarsen during storage,
particularly if:
stored too warm
temperature fluctuation during storage

Coarsened product is associated with a cold,


icy, and gritty mouthfeel
Caused by many, large crystals (>55 m)

Effect of Unfrozen Matrix

Diffusion

Tg?
Stabilizers?

Simplified Flow Chart


-18C

-5C
Freezer

Hardening
~35 m
50% Frozen

Nucleation
Growth

Growth

-15C
Distribution

~45 m
80% Frozen
Melting
Growth
Ripening

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