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LEEOER
Dept. of Food Science, Rutgers University-The State University of New Jersey, New Brunswick, NJ 08903
SUMMARY-Experimental results show that the level of milk solids-not-fat normally used in ice teurization temperature and stirred into the
creams, alone, had sufficient emulsifying capacity to emulsify the fat present in a standard ice aqueous portion of the mix just before homog-
cream mix. The added chemical emulsifier. regardless of its HLB, contributed little to the stability enizing. The samples were homogenized at the
of the mix. This was true even where butteroil was used as a source of fat. Fat deemulsifiwtion pasteurization temperature in a Manton-Gaulin
during freezing increased with the HLB of the emulsifier while the dryness showed no meaningful
two-stage homogenizer using a pressure of 2000
psi on the first stage valve and 500 psi on the
trend. The meaning of the terms dryness, stiffness, melt resistance. and stand-up quality has been
second. During the homogenizing process the
clarified. mix in the hopper was stirred constantly in or-
der to avoid “oiling-off” of the fat. The samples
INTRODUCTION In this paper emulsifier action in ice were then cooled in cold running water and
cream was iniestigated utilizing the HLB stored at 40’F for 24 hr before freezing.
EARLIER THEORIES of emulsifier ac- Freezing the mix
concept. Physical effects of emulsifiers in
tion in ice cream were based on the
ice cream such as fat deemulsification, The mix was frozen in a model 5P Electra
knowledge of simple oil-in-water emul- Freeze soft-serve ice cream freezer. This partic-
dryness, and stiffness were studied in
sion systems. Thus the emulsifiers were ular model has an automatic temperature con-
relation to the emulsifiers and their HLB.
thought to control the surface phenom- trol and is capable of maintaining a constant
ena that favor a stable fat dispersion and temperature of 19 + 1°F.
decrease the tendency for fat particles to EXPERIMENTAL The procedure consisted of freezing a trial
coalesce (Snyder, 1949). Another theory mix until a temperature of 22°F was reached
Required HLB of au emulsion system and it was then drawn off. After an initial rins-
for the action of emulsifiers was one in
The optimum emulsifier HLB necessary to ing of the freezer barrel with the test mix, a
which the emulsifiers were thought to be make a stable emulsion, under a given set of half gallon of the test mix was introduced into
adsorbed at the air-serum interface mak- conditions, is called the required HLB of that the freezer. After each freezing trial the freezer
ing possible a fine, stable air cell, associ- particular emulsion and can be determined ex- barrel was washed out in order to eliminate car-
ated with a “dry” appearing product perimentally for many emulsion systems. The ry-over from sample to sample. The time re-
(Keeney and Josephson, 1958). These method used was based on the one described by quired for a test mix (at 40°F) to reach 22°F
theories were assumptions not based on Atlas Chemical Industries, Inc. (undated). In was about 3 min. The constant temperature of
experimental work with ice cream sys- this procedure an arbitrary tnnstant concentra- 19°F was reached between 6-9 min. The ice
tems. To transpose these simple theories tion (0.1% in this experiment) of emulsifiers cream was packaged in round pint paper car-
to a complex emulsion system such as ice with increasing HLB’s was added to each of a tons.
series of emulsions consisting of 12 parts but-
cream is erroneous since ice cream con- Determining the dryness of ice cream
teroil and 62 parts water. This is the ratio of oil
sists of other major constituents such as to water in a standard ice cream mix. The emul- “Dryness” is the absence of a wet, soft or
milk solids-not-fat (MSNF), sucrose and sions were heated to pasteurization temperature slack appearance. A dry product is dull in ap-
stabilizer gums. It is a well known fact (160”F), homogenized and held at 40°F for 24 pearance and less glossy, whereas a wet and
that MSNF have emulsifying properties hr before determining their stability with the slack-appearing product is highly glossy. This
emulsion stability test. The emulsifier HLB was the criterion of this test. The gloss was
and thus may contribute to the total
which produces the maximum emulsion stabil- measured by means of a Gardner Gloss Meter
emulsification requirements of ice cream. (model GG-9040 P-5 60’). Samples were col-
Counter to the theories mentioned ity is called the “required HLB” of that particu-
lar emulsion system. The HLB’s used in this lected from the freezer at the desired time in-
above, later evidence points to the fact procedure ranged from 2 to 18. tervals into shallow cups, the top surface lev-
that emulsifiers may actually deemulsify In order to determine the minimum concen- eled off with a knife held so that its flat surface
the fat emulsion, and this deemulsifica- tration of emulsifier (of the required HLB) nec- was perpendicular to the plane of the cup, and
tion is suggested as being responsible for essary to yield maximum stability, a series of the gloss reading taken immediately. The whole
dryness in ice cream (Kloser and Keeney, test emulsions were made as above with increas- operation was completed in a few seconds,and
1959). The once popular belief that ing concentrations of the emulsifier having the the same speed was maintained with all sam-
required HLB. After heating, homogenizing and ples. This was very important since the gloss
emulsifiers are necessary to prevent
holding at 40’F for 24 hr, the emulsions were value changes rapidly with time.
“churning” in ice creams made with A dry product being less glossy gives a lower
butter or butteroil as a source of fat, is no tested for their stability.
reading. Thus, a decreasein gloss value indicates
longer valid (Kloser and Keeney, 1959). Preparing the mix an increase in dryness. Usually a gloss reading
A new concept about emulsifiers was All the standard mixes were prepared in over 15 indicates a wet appearing product, and
developed by Griffin (1949) in which a l-gal batches using the following formula: a reading below 10 an extremely dry product,
specific emulsifier HLB (Hydrophile- with the readings between these values repre-
Fat 12 parts senting varying degrees of dryness.
Lipophile-Balance) is required to produce Milk solids-not-fat 11 parts
a particular type of emulsion. This theory Emulsion stability test
Sucrose 15 parts
has been shown to hold true with all Water 62 parts Principle. In emulsion stability studies, the
nonionic emulsifiers. increase in particle size with time is important
Simply stated, in the HLB system, The required quantities of hlSNF and sucrose since it results from flocculation and coales-
each emulsifier is assigned a numerical were weighed and thoroughly mixed. The mix- cence, that is, deemulsification. An increase in
ture was stirred into the weighed amount of particle size with time, other conditions being
value which is called its HLB. The num- water and stored at 40°F for 24 hr to attain the same, is thus an indication of instability.
ber indicates, essentially, the percentage complete solubility and hydration. The samples The time necessary for the particle size to
weight of the hydrophilic portion of the were pasteurized at 160°F for 30 min. The reach a maximum (thermodynamic equilib-
emulsifier molecule divided by 5. The emulsifiers were added when the temperature rium) in an “unstable” emulsion system may
whole HLB scale therefore ranges from reached 160’F. The fat (pure anhydrous milk- range from a fraction of a second to days or
O-20. fat) was melted, heated separately to the pas- months. On the other hand, a decrease in parti-
I 0’
= $40-
temperature.
The procedure consisted of transferring pint
207 samples which had been tempered in an ice
? s cream cabinet at S-7°F from their original con-
mg I tainers onto an aluminum wire-mesh screen
z‘lo (252 pores per sq in.) by peeling off the con-
$ s 60- ZQ
i$ tainer material. This method of transferring the
2 &? E-
0 4 I60 samples was preferable to the conventional
q
iii method of using a dipper which could intro-
3
80- $I duce several errors. The screen holding the sam-
r, a 860 l-y+;
5 G ple was placed on a beaker, and the amount of
: melted ice cream which had dripped through in
100 loo I h a period of 30 min was weighed and reported as
IO 12 14 16 18 0.0 0.1 0.2 0.3 04 05 1.0
grams of ice cream melted. The melting was
EMULSIFIER CONCENTRATION PERCENT IHLB 161 done at a temperature of approximately 70°F.
HL8
Fig. 1 -Effect of emulsifier HLB (0.1% concen- Fig. Z-Effect of emulsifier concentration on The greater the amount of melted ice cream,
tration) on the stabilitv of an oil-in-water emul- the stability of an oil-in-water emulsion possess- the faster the rate of meltdown. The samples
ing the same ratio as a standard ice cream mix.
used for the meltdown test were those collected
sion possessing the same ratio as a standard ice
after 12 min in the freezer.
cream mix.
RESULTS
Required HLB of a standard ice cream
IUiX
60
01 I
0 3 6 9 12 0 0.05 0.10
' -o.:550 0.20
TIME IN THE FREEZER (mint EMULSIFIER CONCENTRATION 0
Frg. 4-Relationship between fat deemulsifica- Frg. B-Effect of emulsifier concentration (con- Fig. 6-Effect of emulsifier HLB (constant con-
tion and dryness during freezing of a standard stant HLB 161 on fat deemolsification, dryness, centration, 0.05961 on fat deemulsification,
ice cream mix. and melting rate of ice cream at the end of 12 dryness and melting rate of ice cream at the end
min of freezing. of 12 min of freezing.
Table l-List of HLB values and their corre- Table J-Effect of increasing the HLB of the
sponding emulsifier composition Table Z-Effect of increasing the concentra- emulsifier at a constant concentration 10.05%01
tion of the emulsifier at a constant HLB (16) on drvness in a fat-free ice cream svstem
HLB Composition
on drvness in a fat-free ice cream
Time in the freezer (min)
2 8% Spana 80,92% Span 85 Time in the freezer (min)
4 88% Span 80,12% Span 85 Sample 3 6 9 12 15
3 6 9 12 15 Gloss values
6 83% Span 80,17% Tweenb 80
8 65% Span 80,35% Tween 80 Gloss values Control 24 9 1 I 8
10 46% Span 80,54% Tween 80 Control (0.00% HLB 2 22 9 8 9 7
12 28% Span 80,72% Tween 80 emulsifier) 24 6 6 6 9 HLB 6 17 8 10 10 6
14 9% Span 80,91% Tween 80 O.O25%conc 22 6 6 6 6 HLB 10 17 6 7 9 6
16 60% Tween 20c, 40% Tween 80d 0.05% cone 25 7 6 6 6 HLB 14 20 1 8 8 8
18 100% Tween 20e O.lO%conc 22 I 6 7 7 HLB 16 18 9 8 8 8
a
“Spans” are sorbitan esters of fatty acids.
b”Tweens” are polyoxyethylene sorbitan
esters of fatty acids.
c“20” series are laurate esters.
d”80” series are oleate esters.
eContains more oxyethylene groupings than
Tween 20.
promote dryness by actually deemulsify- fat globule membrane material had no The above relationship is very informa-
ing the fat emulsion. Fat deemulsification appreciable effect on the rate of deemul- tive since it explains the basis for varia-
has been considered necessary for proper sification or on dryness of the ice cream. tions in action between different types of
dryness in ice cream. In Figure 7 fat ice cream emulsifiers hitherto unex-
deemulsification and dryness data are plained. Thus “polys” (which are known
DISCUSSION to produce greater fat deemulsification in
plotted against each other in order to
show the range of fat deemulsification IT HAS BEEN shown that MSNF alone ice cream than the mono- and di-glycer-
values for each gloss value. Many factors provide the total emulsification require- ides) have an HLB over 10 (15 for Tween
apparently affect dryness. However, the ments of the ice cream mix, and the 80, which is commonly used) whereas the
data suggest that even though fat deemul- addition of a chemical emulsifier, regard- mono- and d&glycerides have an HLB
sification and dryness are associated, they less of its HLB or concentration, contrib- around 3. Egg yolk solids and buttermilk
may not be directly related; there may be uted little to the stability of the mix. solids were found to enhance fat deemul-
factors other than fat deemulsification This observation brings up an interest- sification in ice cream (Kloser and Kee-
which contribute to dryness. ing point, the fallacy of the earlier belief ney, 1959). This appears reasonable since
If fat deemulsification is not responsi- regarding the theory of emulsifier action lecithin, the active constituent of these
ble for dryness, it should be possible to in ice cream. It was believed that when a materials, is known to be highly hydro-
get dryness in the absence of fat deemul- normal ice cream mix containing fresh philic. The HLB-fat deemulsification rela-
sification or perhaps even a fat phase. cream was homogenized, the enormous tionship also explains the observation
Therefore, a study of dryness in a fat-free increase in surface area of the fat globules that polys are 20 times more powerful in
ice cream system was made. Tables 2 and which resulted could not be resurfaced by producing fat deemulsification than
3 contain results showing the effect of the limited amount of “natural emulsi- glyceryl mono-stearate (Klotzek, 1965).
emulsifier concentration and HLB on the fier” (fat globule membrane material). The present work thus enables one to
dryness of a fat-free ice cream system. The added emulsifier was believed to explain why ice cream emulsifiers func-
From these data it may be seen that supply this deficit. It was also believed tion so differently even though they all
extreme dryness was obtained even in the that the need for an added emulsifier was belong to the same class of nonionic
total absence of fat which suggests that a even greater when butter or butteroil was emulsifiers.
fat phase and fat deemulsification are not used as a source of fat since these sources In a simple oil-in-water emulsion, the
required for dryness. It is also apparent are devoid of fat globule membrane mate- fact that the emulsifier molecule is ori-
that the emulsifier HLB or concentration rial. It was shown in this study that the ented at the oil-water interface is not
had little or no effect on dryness. contribution of the fat globule membrane sufficient to stabilize the emulsion parti-
material to the emulsification of the mix cle. Instead, the stability of the emulsion
Contribution of the fat globule membrane was practically negligible compared to the is dependent on the relative strengths
material to the emulsification of the mix contribution of the MSNF. The impor- (number) of the hydrophilic and lipo-
In order to study the contribution of tance of MSNF in ice cream emulsifica- philic groupings of the emulsifier used,
the fat globule membrane material to the tion is thus demonstrated. that is, the HLB of the emulsifier.
emulsification of the mix, two mixes The results in this study also confirm Thus, at a lower emulsifier HLB, since
were prepared, one with butteroil as a those of Keeney and Josephson (1962) in the hydrophilic groupings are weaker, the
source of fat and the other with 50% which emulsifiers were not found to bare fat globule is weakly associated with
cream as a source of fat and fat globule produce any difference in ice cream the aqueous phase and hence the emul-
membrane material. Microscopic exami- emulsion stability. sion is unstable. At a higher emulsifier
nation of the emulsions showed no differ- During freezing of the mix, with emul- HLB, since the hydrophilic groupings are
ence, and the emulsion droplet size in sifier concentration remaining constant, stronger, the bare fat globule is strongly
both cases was in the range of 1-3~. fat deemulsification increased with the associated with the aqueous phase and
In Figure 8 a comparison of fat de- HLB of the emulsifier. The coefficient of hence the emulsion is stable. However, if
emulsification and dryness during freez- correlation (r) between HLB of the emul- the HLB of the emulsifier used is ex-
ing of these mixes is shown. As may be sifier and fat deemulsification was found tremely high, the hydrophilic ends would
seen, the curves run in close proximity, to be + 0.87, indicating a high positive be so strong as to make a weak orienta-
indicating that the phospholipids in the correlation. tion of the lipophilic ends into the lipid
722 -JOURNAL OF FOOD SCIENCE-Volume 36 (1971)
phase. In such circumstances, there would phase and such dryness was not affected least amount of fat deemulsification
be instability. This was evident from the by the presence of an emulsifier. would mean selecting an emulsifier of
results which indicated that there was a Dryness apparently is only one of the approximately HLB 8. Interestingly
decrease in stability when an HLB of 16 desirable properties looked for in ice enough, some commercial blends of ice
was exceeded. cream. Other qualities such as melt resist- cream emulsifiers which claim to produce
The mechanism described above, how- ance, “stand up” quality, and stiffness are optimum results have an HLB ranging
ever, is unlikely in an ice cream mix in of equal importance. John and Sherman from 4.50-7.80.
view of the strong denatured protein film (1962) have shown a correlation between The knowledie gained by’the use of
enveloping the newly formed fat globules fat deemulsification and melt resistance, the HLB concept of emulsifier action in
(Walker, 1960). This protein film tends to which was confirmed in this study. ice cream thus enables one to select an
make the fat globules hydrophilic, and In the present work dryness was not emulsifier to meet individual production
the whole system behaves as a fat-free always related to good melt resistance; problems, and eliminates the laborious
system so far as the emulsifier action is conversely, good melt resistance was in- and rat her uncertain trial-and-error
concerned. Under these circumstances, variably accompanied by a low-gloss val- method of selecting the proper emulsifier
therefore, the emulsifier molecule, regard- ue. This observation is particularly inter- blend for the purpose.
less of its HLB, is situated remotely from esting since hitherto it has been generally
REFERENCES
the oil-water interface in the serum. This believed that a dry ice cream has a good
Anonymous. (Undated.) “Dryness in Ice
idea supports the findings of Keeney melt resistance quality. Apparently, this Cream.” Atlas Chemical Industries, Inc..
(1962) that the emulsifier content was is not always true. Wilmington. Del.
Durham, K.. Jones, T.G., Shaw, D.J. and
higher in the serum portion, than in the Results of the present work suggest Walker. D.A. 1962. The ohvsical wooerties
fat portion, of melted ice cream. there is an error in relating gloss readings of ice cream. First Int. -C&gress of- Food
It has long been i known that the to melt resistance since the gloss meter Sci. and Technol. London, Eng. (Mimeo-
graphed).
emulsifiers belonging to the group called only indicates the surface gloss of the Griffin, W.C. 1949. Classification of surface-
polys (HLB 15) are better whipping samples and does not differentiate be- active agents. J. Sot. Cosmetic Chemists 1:
311.
agents than the emulsifiers of the mono- tween samples having varying degrees of John, M.G. and Sherman, P. 1962. The effect
d&glyceride type (HLB 3). Based on this fat deemulsification which is essential for zf stabiI+s an-d. emulsifying _ ^ agents
. _ -upon
tne BroDertles OI Ice cream. lam 1nt. IJalrv
fact, a probable mechanism for an in- stiffness and melt resistance. Conm&& Sec. VI, 1: 61.
crease in fat deemulsification with an The term “controlled fat deemulsifica- Keeney, P.G. 1962. Observation on the emulsi-
increase in emulsifier HLB is suggested. tion” is more in order than just fat fier content and fatty acid distribution in
the lipids associated with the air cell struc-
Due to increased whipping, a closer pack- deemulsification as being essential for ture in ice cream. J. Dairy Sci. 45: 658.
ing of the fat globules results in their structure, stiffness and melt resistance. Keeney, P.G. and Josephson. D.V. 1958. A
measure of fat stability in ice cream and its
eventual coalescence. The net effect being The results showed that melt resistance relationship to dryness. Ice Cream Trade
chains of coalesced fat globules surround- increased with fat deemulsification only J. 54(5): 32.
up to a point. Beyond this point there Keeney, P.G. and Josephson, D.V. 1962. Newer
ing the air cells in the ice cream. This concepts on the mode of action of emulsifi-
condition has been observed in this study were visible signs of “churned” fat as em. 16th Int. Dairy Congress Sec. VI, 1: 53.
and has also been reported by Durham et butter granules and wheying-off was ob- KIoser, J.J. and Keeney, P.G. 1959. A study of
some variables that affect fat stabilitv and
al. (1962). served. Thus, there is an optimum point dryness in ice cream. Ice Cream- Rev.
It has been generally believed that in the degree of fat deemulsification for 42(10): 36.
Klotzek. L.M. 1965. Factors affecting fat stabil-
emulsifiers were necessary to produce a good structure and melt resistance. ity in soft serve ice cream. M.S. thesis. Rut-
“dry” ice cream, and by so doing, they The role of the emulsifier therefore gers University, New Brunswick, N.J.
Snyder, W.E. 1949. Emulsifiers are useful. MiIk
invariably caused fat deemulsification. lies in producing a controlled deemulsifi- Plant Monthly 38(6): 30.
This led to the further belief that emulsi- cation which is influenced by the HLB of Walker, D.A. 1960. The aging of lipo-protein
fiers promote dryness by deemulsifying the emulsifier and its concentration. Any films at the oil-water interface. Third Int.
Congress of Surface Activity 4(41): 351.
the fat emulsion and that fat deemulsifi- desired level of fat deemulsification can Walter, D.A. 1963. Analysis of the factors influ-
cation is essential for dryness. be achieved by making use of the encing the structure of ice cream. J. Dairy
Sci. 46: 591.
In this study there was no evidence to HLB-concentration relationship. M S received 11/19/70; revised 3/13/71; ac-
support this theory since samples with no Since the HLB’s that cause the least cepted 3/14/71.
emulsifier produced extreme dryness. and greatest amount of deemulsification Paper of the Journal Series, New Jersey
Agricultural Experiment Station, Rutgers Uni-
Furthermore, extreme dryness could be are 2 and 16, respectively, a compromise versity-The State University of New Jersey,
obtained even in the absence of a fat to achieve good melt resistance with the New Brunswick, N.J.