SYMPOSIUM
PROBLEMS OF LACTOSE CRYSTALLIZATION
CONCENTRATED
F. J. DOAN
Department of Dairy Seience~ The Pennsylvania State University~
University Park
Lactose crystallization always occurs during
the processing of sweetened condensed milk
products; usually occurs in the manufacture of
condensed and dried wheys, and may take place
in such products as ice cream, plain condensed,
dry, and frozen milks. The crystallization
more often happens, or becomes sensible, during
the holding periods following manufacture.
The fundamental reason for lactose crystal-
lization in all cases is either an insufficiency of
water to hold it in solution under the prevailing
conditions or sufficient water to furnish a labile
concentration when lactose is in the amorphous
or glass state.
The presence of lactose crystals in dairy
.products constitutes a defect when their size
is such as to create a mealy, sandy, or gritty
texture; when they tend to settle and form a
deposit; when their presence changes the physi-
cal character of the product or any of its in-
gredients, or when they interfere with use of
the product.
I n some dairy products, lactose crystalli-
zation can be prevented. I n others, this is im-
possible or inadvisable, so that attention is
necessarily focused on the limitation of crystal
size to insensible magnitudes.
Sweetened condensed milk. The necessity for
control of lactose crystallization in sweetened
condensed milk has been recognized from the
beginning, and this product served to focus the
attention of scientists on the idiosyncrasies of
milk sugar in the processing and storage o£
dairy products.
As sweetened condensed milk comes from
the evaporators, the lactose is at, or near, the
saturation point. Eventually, when cooled to
60 or 65 ° F., between two-fifths and two-
thirds of the lactose present will emerge as
crystalline a-lactose hydrate. This happens
because milk sugar is soluble to the extent of
only about 15 parts to 100 parts of the water
as found in this product (11). Actually, there
are 40 to 47 parts of lactose per 100 of water
in sweetened condensed milk of average com-
position, made up of an equilibrimn mixture
of about 40% a form and 60 per cent /~ form.
Crystallization of lactose, therefore, can not
be prevented, short of previous hydrolysis, and
Authorized as Paper No. 2189 in the Journal
series of the Pennsylvania Agricultural Experi-
ment Station.
325
IN
MILK PRODUCTS 1
desirable texture nmst be achieved by limiting
the size of the crystals. To obtain smooth
texture, it has been shown (23) that a narrow
range of crystal-size is necessary, averaging
from about 10 to 11 t~ along the longest edge.
At this size, there are between 200,000 and
300,000 crystals per nil. (23).
Theoretically, small crystals and a multitude
of them result when a rather highly supersatu-
rated solution is seeded under conditions of
vigorous agitation. Lactose readily forms super-
saturated solutions. I n common with other
sugars, it manifests a reluctance to crystallize,
especially in the absence of agitation, until the
excess sugar in solution is at a very high level
(7, 30). It has been noted, however, that too
great supersaturation actually reduces the
crystallization pressure and slows the mass
formation of crystal nuclei (31). Moreover,
in sweetened condensed milk the viscosity in-
creases rapidly with reduction of tempera-
ture, and interferes with diffusion to the crystal-
forming centers. Experiment has shown that
the greatest number o£ smallest crystals is ob-
tained when crystallization is forced by seed-
ing at temperatures between 80 and 95 ° F.,
depending on the composition of the sweetened
condensed milk and its viscosity (10,31).
Several texts contain data showing the final
solubility and the spontaneous crystallization
curves for lactose (1, 3~ 10~ 32). The area be-
tween these curves defines the metastable zone,
where forced crystallization should be practiced
for most desirable results. Forced crystalliza-
tion consists of adding 4 to 8 oz. of impact-
pulverized a-lactose hydrate dust, per 1,000
lb. o£ vigorously agitating product, in such a
way that maximum dispersion results, and of
continuing agitation for from 30 to 60 min.
without reduction of temperature.
Since the final cooling temperature of sweet-
ened condensed milk is 60 to 65 ° F., it should
be appreciated that more lactose will crystallize
on the nuclei already formed as the tempera-
ture is reduced following forced crystallization.
This occurs not only because of the decreasing
solubility of the a-lactose still in solution, but
because of the equilibrium relationship between
the a and B forms, which results in mutation
of the /~ form to a, as the a in solution is
decreased by crystallization. This mutation or
reversion is a relatively slow process. At 60 ° F.,
it is only about 90% complete after 8 hr. (8, 9),
326 JOURNAL OF D A I R Y
and for this reason a period of agitation is
desirable between final cooling and packaging
of the finished product. This agitation assists
in accelerating the ]~ to a reversion, and in
making uniform the crystal growth in a prod-
net as viscous as sweetened condensed milk.
While many commercially used types of cool-
ing and crystallization equipment for sweetened
condensed milk make use of the forced crystal-
lization concept at the optinmm temperature,
a nolabh, eXCel)ti(m is the hmg and successfully
used submerged e(,il, or internal-tube, method,
wlwre milk from the evaporators is pumped
(.ontinmmsly through the cooling tubes to bring
it to its final temperature, with or without
l)rvvious seeding. ]t appears that in such equip-
ment seed crystals axe encountered in the cooler
when the temperature drops far enough to in-
sure a satisfactory degree of lactose supersatu-
ration. The crystallizing impulse is dissemi-
nated through tim mass of milk as it is forced
in a rolling motion through the tubes. Inasmuch
as there is no lengthy forced crystallization
period in this type of cooling, the desirability
of a hmgthy period of agitation before filling
would seem to be emphasized.
Some manufacturers, who practice standard-
ization of overconcentrated milk by adding
sterile water before filling, feel that a secondary
advantage of this practice is the reduction in
size of the lactose crystals by partial solution
in this water. No studies substantiating this
have been reported.
The sedimentation of lactose crystals, in a
given batch of sweetened condensed milk during
holding, is a function of crystal size, viscosity,
and time. I f crystallization techniques are
satisfactory, sedimentation can best be avoided
by adjusting the viscosity, by means of pre-
heating conditions and milk-solids-not-fat level,
keeping in mind the thickening tendency on
aging and the probable time and temperature of
storage. Variations in ambient temperature
during storage (heat-shock) are known to cause
growth in crystal size by solution of small
crystals, and subsequent increase in size of the
larger ones, as the temperature changes vary
the solubility of lactose.
Other highly concentrated products in which
lactose will crystallize during or following
manufacture, are generally treated like sweet-
ened condensed milk, utilizing a seeding pro-
ccdure and forced crystallization to assure small
crystals which will not grow to objectionable
size.
Some concentrated whey products are proc-
essed in this fashion, and sweetened condensed
whey and preserved concentrated ice cream
mix always are so treated. The latter product,
however, may include some sodium caseinate
as part of the serum solids, to reduce the level
of lactose present (32).
Plain condensed milk. Crystallization and
sedimentation of lactose in plain condensed
milks are not common, but occasionally do
SCIENCE
occur with high-solids products. Some crude
observations have indicated that 44o-1 whole
milk will usually crystallize under unagitated,
40 ° P. holding in 72 hr. ; similar skimmilk, not
until after 240 hr. The former product contains
about 40 parts of lactose to 100 water, and the
latter about 31 parts. At 34o-1 concentration,
where the highest lactose :water ratio is about
24 to 100, usually neither whole nor skimmilk
will show evidence of crystallization up to 480
hr. These results agree in general with those
which have been made on supersaturated water
solutions ()if lactose (7). It probably can be
said that lactose will not crystallize in plain
condensed milk during customary, unagitated
holding periods in refrigerated storage, so long
as the lactose : water ratio is not (/ver 30 parts
per :lO0--unless inadvertent seeding or some
other crystallizing impulse is furnished.
Some milk-drying plants, using continuous
methods, have experienced trouble with lactose
crystallization in the accumulation tanks feed-
ing the driers. These tanks are often uninsu-
lated and unagitated, and considerable cooling
may occur in quiescent areas, increasing the de-
gree of supersaturation of the lactose to a point
where spontaneous crystallization may take
place. Once this has happened, crystallization
builds up rapidly, because of the seed nmterial,
and a sludge may develop. It has been necessary
in some cases to suspend operations for clean-
ing, or to divert the milk to an auxiliary tank
until relnedial action can be taken. Knowledge
of this problem is meager, but some available
information indicates that when the tempera-
ture of the milk is uniformly maintained by
agitation at 120 ° F. or higher, no crystallization
occurs. This appears logical, inasmuch as
little or no supersaturation would exist at this
temperature. It also would seem possible to
avoid the problem by limiting the solids con-
tent of the skimmilk from the evaporators to
45%, for at this level the lactose :water ratio
would be 45 to 100, corresponding to a spon-
taneous crystallization temperature of 70 ° F.
or less.
Ice cream. The crystallization of lactose in
ice cream, causing sandy texture, is a recurring
problem to manufacturers. Evidence indicates
that in freshly hardened ice cream the equi- ~
libriunl mixture of the a and B forms of lactose
is in the glass state, and is stable as long as the
temperature remains at the hardening-room
level (7, 22, 27). I n the freezing of ice cream,
the lactose solution apparently passes through
the labile zone so rapidly and at so low a tem-
perature that no opportunity exists for the
molecules to diffuse and orient into crystal
structures. Undoubtedly, the high viscosity
of the unfrozen liquid is a crucial factor in this
connection (22).
When ice cream is warmed to, and held at,
dipping temperatures or dispensing-cabinet
temperatures, some ice melts, and there must be
produced an infinite variety of lactose concen-
 SYMPOSIUM
trations, over a period of time, as molecules
diffuse slowly into these water droplets from
the amorphous glass. Some of the concentra-
tions doubtless will be in the labile zone f.or
the temperature, and permit spontaneous
crystallization; others will be in the metastable
zone, where crystallization can occur if a stimu-
lus in the form of lactose crystal nuclei, or fine
particles of extraneous matter, exists. Because
of the low temperature, crystallization pressure
will be low and no mass crystallization would
be expected. Nevertheless, the nuclei formed
will act as a seed impulse for further crystal-
lization, as opportunity offers, and will them-
selves tend to grow slowly with time. Eventu-
ally, the ice cream will become sandy.
Since all ice cream, as conventionally made,
contains more lactose than is soluble in the
available water at the temperature, the wonder
is that all ice cream does not become sandy
after a few days in the dispensing cabinets.
The fact that limitation of the serum solids
content of the mix prevents, or at least greatly
delays, lactose crystallization can not be en-
tirely explained on the basis of our present
knowledge. However, it is true that with low
lactose mixes the sucrose : laotose ratio is
generally greater, and at comparable tempera-
tures the lactose-water concentration would be
lower in such nfixes.
An equation has been proposed (22) for cal-
culating a safe maximum serum solids content
for ice cream mixes. This establishes an aver-
age limit of 14.5% for the serum solids content
of the serum, but may be varied about 1%,
down or up, depending on whether conditions
will be conducive or nonconducive toward the
development of sandiness in the ice cream. Ex-
perience has shown that this method of con-
trolling the defect is generally, but not abso-
lutely, satisfactory.
F r u i t and nut ice creams are more prone to
become sandy than most plain flavors. The
usual explanation is that the added flavor sub-
stances either furnish fine particles capable
of acting as crystallization nuclei, or that they
absorb water from the serum.
Some manufacturers have used high levels of
serum solids and avoided the problem of sandi-
ness by employing skimmilk products from
which substantial proportions of. the lactose
have been removed. O~hers have utilized, for
this purpose, proteins (usually sodium casein-
ate) separated from milk products.
A method of obtaining high sermn solids ice
cream without texture problems was patented in
1932, but has not been used much commercially
(6). I n this procedure, a substantial portion
of the total serum solids is added in the form
of dry skimmilk to the partially frozen ice
cream. I t was claimed that inasnmch as the
lactose of the dry product can not go into
solution, because of the already supersaturated
condition of the ice cream, it therefore can not
crystallize later. This reasoning seems falla-
327
cious, in view of the fact that lactose in the
added dry milk is in the same glass state as
that i n the hardened ice cream. I f the latter is
capable of crystallizing with a rise in tempera-
ture, there seems no good reason why the former
should not do so under dispensing-cabinet con-
ditions. Nevertheless, this method does seem
to accomplish the purpose in view.
More recently, enzymatic hydrolysis of the
lactose of skimmilk has attracted some atten-
tion as a means of lowering the lactose level of
ice cream mixes (19), but the time element and
inconvenience would seem to militate against
its large-scale adoption.
A different approach to the problem of sandi-
ness which is of interest was patented in 1953
(4). This method is reminiscent of the psy-
chology: "If you can't beat 'era--join 'era."
I t takes the viewpoint that since lactose crystal-
lization is virtually impossible to prevent abso-
lutely, it is better to force crystallization to
occur and to control the size of crystals, as is
done with sweetened condensed milk. The
method has been studied in considerable detail
at California (13,14, J5). When ice cream
mix, immediately before freezing or in the
partially frozen state, is properly seeded with
fine lactose dust (3 to 7 t~ in particle size),
mass formation of crystal nuclei occurs. The
crystals are so small and so numerous that they
never reach sensible size, even though consider-
able quantities of ]~-laetose slowly revert to the
a-form and build up on them during the hold-
ing period. Ice cream containing 18% serum
solids has been produced by this procedure and
held for 10 too. at 12 ° F. without evidence of
sandy texture. I t has also been demonstrated
that dried products, such as dry skimmilk and
dry whey, added at the freezer, induce mass
crystallization in a manner similar to that of
the seed lactose (15). I t appears, therefore,
that the earlier patent covering' the addition of
dry skinmfilk at the freezer actually avoids
sandiness, not because the lactose of the dried
product fails to go into solution, but because
it induces mass crystallization in the form of
impalpable crystals. This method of over-
coming the problem of sandy ice cream de-
serves more study, and its possible effect on
body, texture, and melt-down characteristics
should be investigated.
Frozen mil]~. I n frozen milk, it is the loss of
stability on the part of the caseinate that de-
termines the length of the period of satisfactory
holding (5). I t is of interest, and possibly
highly significant, that a relationship between
casein flocculation and lactose crystallization
has been demonstrated in frozen concentrated
milk at the National Dairy Research Labora-
tories (29). This has been nicely confirmed and
extended by studies at the National Research
laboratories, Ottawa, Canada (17, 18, 25, 26).
I n 3 : 1 concentrated skimmilk, preheated
at temperatures below 170 ° F. and held in
frozen storage, the casein maintains its stability
328 J O U R N A L OF D A I R Y S C I E N C E
as long as the lactose remains as a supersatu-
rated solution, or glass. At temperatures of
- 20 ° F. and below, this condition seems more
- tose crystal nuclei formation prior to freezing
or tess permanent, and milk can be held for
very long periods. Between - - 1 0 ° and 0 ° F.,
lactose crystallizes rather reluctantly and only
after a considerable induction period. Above
0 ° F., however, it is only a nmtter of a few
days before lactose appears in crystal form,
and soon thereafter casein is found in the floc-
culated condition on defrosting.
Inei(hmtally, the similarity between lactose
crystallizati<)n in frozen milk and in ice cream
is (dose. as might hc expected. First, the te:n-
peratures at which crystallization occurs, or
does not occur, are very much alike in the two
products. Secondly, just as a reduction in the
serum solids content of ice cream mix acts to
postpone the dew'3opment of sandiness, so does
the lowering of the concentration ratio of' the
concentrated milk, prior to freezing, delay
crystallization in the frozen product. This is
in spite of the fa('.t that lac.tose concentration
in both frozen products is dependent not on
composition--but on temperature. For instance,
it has been shown that wimn fluid milk, and the
same milk concentrated to 30% solids, were each
frozen and held at J5 ° F. for 23 (b~ys, the
former exhibited no lactose crystallization and
no destabilization of the casein; whereas, in
the latter, 75% of the lactose had crystallized
and the casein was in an advanccd stage of
flocculation (28). Thirdly, the melt-down of
samty ice cream almost always exhibits a curdy
character, which is doubtless a result of casein
flocculation similar to that found in defrosted,
crystallized frozen milk.
There is also a kind of analogy between the
destabilization of casein in frozen concentrated
milk when lactose crystallizes, and the loss of
solubility and dispersibility of casein in dry
milk when lactose crystallization and lumpiness
occur, following absorption of moisture. Both
seem to become manifest as a result o£, or
at least subsequent to, lactose crystallization.
This analogy, however, seems not to hold in
the instantizing treatment of dried milk.
Why, or by what means, the change of lactose
from a molecularly dispersed state to a crystal
form influences the physical or physico-chemi-
cal properties of calcium caseinate, is not
known, but it nlay be pertinent to mention what
is known relative to the nature of the casein
floc as it appears in frozen milk.
The loss of dispersibility is noted on de-
frosting, especially on reconstitution. I n the
early stages, it is reversible with agitation
and/or heat, but with continued storage it
becomes irreversible. It is thought to result
from a salting-out effect caused by the high
concentration of solubles in the unfrozen water
of the frozen product. Casein of similar charac-
teristics can be obtained by aging skimmilk
saturated with sodium chloride at room tem-
perature (5). Instability of the casein can be
aggravated by heat denaturation of the whey
proteins and by anything which stimulates lac-
(18). Instability can be lessened by the pres-
ence of other sugars (17~ 33), by sequestration
or removal of calcium ions (33), and by enzy-
matic hydrolysis of a portion of the lactose
prior to freezing (28, 29).
It has been postulated that inasmuch as other
sugars in solution manifest a stabilizing influ-
ence on the caseinate (26, 33), lactose may act
similarly (29). When it crystallizes from solu-
tioin, it leaves the unfrozen water with lower
ostnotic pressur(~, so t~lat nlore water :~reezes
and intensiiies the salt concentration which in
turn, operates to floculate the casein (17).
Sugars, furthermore, contribute greatly to the
viscosity of the unfrozen liquid, tending to
block diffusion and slow any of the changes in
the system which affect casein stability. There
is also a possibility that sugars form com-
pounds with cahdum (7), an ion to which casein
is particularly sensitive.
This newly discovered relationship between
lactose nucleatim~ and casein instability in con-
centrated milks deserves further study.
Dried milk.~. Lactose does not normally cryst-
allize in the drying of milk by the usual spray
and drum methods, lilt is found as an equilib-
rium mixture oil a and fl forms in the amor-
phous glass state (27, 5'2)~ in fresh powder, and
will so remain if the product, which is very
hygroscopic, is protected frnm moisture.
Lmnping and caking of dried milk after
manufacture is generally conceded to be caused
by the gradual absorption of moisture, which
dilutes the lactose glass to the point where a
supers~Jturated solution in the labile zone is
obtained. Crystallization of a-lactose hydrate
usually results, and the masses of growing
crystals form a structure causing lumpiness
and, eventually, solidification (27). fl-lactose
also may take part in this crystallization, when
c.nditions are favorable (20). The decrease in
solubility which usually accompanies lumping
may be due to the loss of casein stability, as
noted in frozen concentrated milk, when lactose
crystallizes (29). Air-tight packages are es-
sential in preventing crystallization and in
maintaining the quality o£ dry milk.
The process of producing instantly soluble
dry milk by humidifying the freshly dried
product~ clustering the particles and redrying,
permits partial crystallization of lactose before
the moisture level is again reduced below the
point where crystals can form. Such instant
milk contains about three parts a-lactose to
two parts fl-~ instead of the usual two a- and
three ,8- (2). Lactose crystallization is ap-
parently not necessary /or the improved dis-
persibility, inasmuch as instant milk made by
other techniques, where the equilibrium ratio
of a- and B-lactose is not disturbed, shows
good dispersion characteristics, at least when
freshly made (2).
 svMPosIu~ 329

Dried whey. The d r y i n g of w h e y is compli- Same. U. S. P a t e n t 1,878,127. Septem-

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(16) O~:'~INo, H. E., AND QULLIGAN, J. J. Ice
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COMMERCIAL PRODUCTION OF LACTOSE

M. E . H ~ L
Research Division, Armour and Company~ Chicago

There have been so many excellent papers

LACTOSE PRODUCTION IN U, S.
published within the last 15 yr. on the methods
of manufacture of lactose that a review of this
literature would be repetitious, ttowever, it 5O
might be desirable to refer to some of the more
important reviews. Webb and Ramsdell (7),
Webb and Whittier (8), Whittier (10), and
Whittier and Webb (11), have published ex-
cellent reviews of the subject. Those by Hun-
ziker (5), Kastens and Baldauski (6), and g
Weisberg (9) should also be included.
These papers have been very helpful to the 30
dairy industry. Those from the Bureau of Dairy
Industry (7, 10), published during World W a r z
II, undoubtedly were responsible for elimi- -<2 20
nating a considerable amount of confusion, as
well as saving much time and product, when
the production of penicillin caused an increase
of more than 200% in the production of lactose
i
IO
within a 3-yr. period.
Figure 1 gives the annual production of
crude lactose in the United States from 1943
to 1955. This figure shows the effect of peni- O' t I , , , i I i i i , I ,
1945 t950 1955
cillin upon lactose production. P r i o r to 1944,
YEARS
lactose had been produced at a level similar
FIG-. 1. Production of crude lactose from 1943
to that of 1943, at approximately 7.3 million
lb. When it was found that lactose increased to 1955.
the growth rate of Penicillium notatum~ result-
ing in large increases in the yield of penicillin, of it is recovered, then less than 7% of the
then the lactose production curve followed that available supply is used for this purpose.
of penicillin. The peak production figure of Since it is desirable to have many outlets for
50,156,000 lb. in 1951 has been reported to be products which have not been fully utilized,
due to the combined effect of the Korean war it is of interest to explore some of the reasons
and the use of penicillin as a growth stimulant why so little whey is used f o r lactose produc-
in animal feeds. The curve for the last 3 yr. tion. The probable reasons are:
is still ascending at a rate comparable to that
of the 1943-1948 period. I t is also evident 1. Need for more uses for lactose.
that the production of 35,356,000 lb. f o r 1955 2. Need for better methods of obtaining lac~
is about a fivefold increase during a 12-yr. tose.
period. 3. Need for more uses for the lactose mother
I t is estimated that about 10 billion lb. of liquor in the making of edible or pharma-
whey are obtained yearly in the United States ceutical products.
from cheese and casein manufacture. Assuming
that there is 5% lactose in whey and that 60% The last two needs will be discussed in the