Sensory and Objective Measurement of Sandiness in Duke de Leche,
a Typical Argentine Dairy Product
GUILLERMO HOUGH, EDGARW MARTINEZ, and ADRIANA CONTARlNl
lnstituto Superior Experimental de Tecnologia Alirnentaria
ABSTRACT
Lactose crystallization in Dulce de
Leche can produce a sandiness defect.
The objective measurement and sensory
evaluation of this defect were the thrusts
of this study. The technique for the mi-
croscopic measurement of the number
and size of crystals is described in detail.
Sensory panel members found that iac-
tose crystals added to Dulce de Leche
produced a sandiness defect equivalent to
added sand crystals. The latter are far
easier to define by size so they were used
for magnitude estimation, where the ex-
ponent of Steven’s law was approxi-
mately 1. Based on this, seven-point a
sensory scale for sandiness was devel-
oped using Dulce de Leche mixed with
sand of crystal sizes varying between 0
and 1500 pm. A double enay table is
presented whereby the sensory sandiness
threshold can be read as a function of size
and number of crystals. With crystal size
below 6 pm sandiness is not detected,
even if all lactose in Dulce de Leche is
crystallized. Above this size, the detec-
tion threshold depends on number of
crystals.
(Key words: Dulce de Leche, sandiness,
sensory evaluation)
INTRODUCTION
Dulce de Leche, a typical Argentine dairy
product similar to sweetened condensed milk,
was described by Mor0 and Hough (12) in a
previous paper. A standard initial formulation
is 10 parts of milk and 2 parts of sucrose. This
Received December 1 , 1988.
Accepted July 24, 1989.
1990 J Dairy Sci 73:604-611
H. lrigoyen 931
6500 Nueve de Julio
Buenos Aires, Argentina
is concentrated to 70% total solids by boiling at
atmospheric pressure. From milk with 12% to-
tal solids and 4.5% lactose, lactose concentra-
tion in Dulce de Leche is 9.85 d l 0 0 g. Consid-
ering the water phase, the lactose concentration
is 33 @lo0 g water. Solubility of lactose at 15
and 30°C is 16.9 and 24.8 g/100 g water,
respectively (20). So even without interfer-
ences, lactose in Duke de Leche is initially in a
supersaturated solution. This is compounded by
the simultaneous presence of sucrose (146 g/
100 g water), which substantially reduces lac-
tose solubility (14). Under these conditions,
lactose crystallization is inevitable in Dulce de
Leche, which leads to the prevalent defect of
sandiness.
Technological methods have been developed
to eliminate this defect in Dulce de Leche (2,
16, 17, 18, 19) and in sweetened condensed
milk (1, 4, 7, 9), which is of similar composi-
tion.
To evaluate experimental results these au-
thors used arbitrary category scales for the sen-
sory measurement of sandiness, and in some
cases measured crystal size microscopically (5,
7, 9, 17).
Hunziker (7) is the only investigator to re-
late quantitatively the number and size of crys-
tals with a sensory scale for degree of sandi-
ness. Santos et al. (17) noted a contradiction in
that “no sandiness” was the score for crystals
smaller than 10 pm yet Hunziker recommended
seeding with 400-mesh lactose, which has a
37-pm aperture. According to Hunziker (7),
absence of sandiness is obtained when there are
more than 4 x lo8 crystals/cm3. With this
number, he calculated a corresponding 10-p
crystal size; in the calculation he used a lactose
solubility value, which does not coincide with
the solubility of lactose in the presence of
sucrose reported by Nickerson (14). Other
points of Hunziker’s sandiness scale are based
on an arbitrary reduction in number of crystals.
604
 MEASUREMENT OF SANDINESS IN DULCE DE LECHE
Clearly, for research and quality control of
sandiness in Dulce de Leche, the following
aspects need developing: 1) a sensory percep-
tion scale of sandiness in relation to objectively
measured size and number of crystals, and 2)
sensory threshold of sandiness as a function of
size and number of lactose crystals. The objec-
tive of this study was to cover both these
aspects.
MATERIALS AND METHODS
Size and Number of Crystals
There is no published standard for measur-
ing the size and number of lactose crystals in
d a y products. Crystalline lactose in milk prod-
ucts can be detected simply by means of a
polarizing microscope (15). In this study an
Olympus BHI Model BH-2 (Tokyo, Jpn) mi-
croscope was used equipped with a polarizing
filter, PM-6/ENM-7 Olympus photography and
ocular with calibrated scale to allow sectorizing
an observed field and measurement of crystal
axis.
Lactose crystal numbers and size were mea-
sured as follows: a microscope slide and cover
were weighed. Approximately ,003 g of Dulce
de Leche was then weighed onto the slide. The
center of the cover slip was placed over the
Duke de Leche, and a slight pressure was
exerted. Care was taken not to crush crystals; if
this was observed through the microscope, the
slide was prepared again. The resulting sample
on the slide was circular in appearance. Crys-
tals were counted in each of 10 randomly cho-
sen microscopic fields and then averaged to
calculate:
N = nf rt R2/(FW)
where N = number of crystals per gram of
Dulce de Leche, nf = average number of crys-
tals observed in F, R = radius of sample (mm),
F = area of microscopic field (mm), and W =
weight of Dulce de Leche sample. The same
prepared slide was used for measuring crystal
size. The length of the longest axis of a-lactose
crystal is the most relevant to sensory analysis;
therefore, this is the measure in which sizes are
expressed. Within a Dulce de Leche sample,
lactose crystal sizes are not uniform; therefore,
averaging was required. A microscopic field
605
was randomly placed over the slide. Magnifica-
tion was selected until approximately 20 crys-
tals appeared in the field. If there were too
many crystals at maximum magnification, a
reticulated portion of the slide (ln, 1/4, etc.)
containing approximately 20 crystals was used.
Average size of individual measurements was
taken.
In some samples size stratification was clear.
In these cases, the number of crystals are re-
ported separately for each size.
Sensory Scale
Where crystal-free Duke de Leche (CFDL)
was necessary, it was provided from a fresh
batch by Mastellone Hnos, Buenos Aires, Ar-
gentinc who used P-galactosidase to reduce
lactose content and prevent sandiness. To en-
sure no crystals were present, samples were
first observed under the microscope with polar-
ized light.
Sand used for mixing with CFDL to simu-
late lactose crystals was obtained from local
construction stores. The sand was washed,
dried, and finally placed overnight in an oven at
130°C for sterilization. To obtain different
granulomeay, the sand was sieved through
standard-sized screens.
A 12-member panel was used for sensory
evaluations. Training included selection by per-
formance on taste tests and sequential analysis
(8), followed by 10 d of intensive training in
sensory practices (8).
Evaluations consisted of four 1-h sessions
where the panel evaluated different samples
using as a scale a IO-cm line marked on one
end “no sandiness” and “extreme sandiness” on
the other. This scale was used during training
and development of a consensus evaluation
procedure. Also at this stage, samples of
CFDL, mixed with washed and sterilized sand
of different granulometry, were presented to the
panel to compare sensory perception of this
sandiness with that of samples with lactose
crystals.
The next step was to establish sensory ver-
sus objective evaluation of sandiness. The fixed
modules magnitude estimation method was
chosen (1 1). For this, lactose crystals of defi-
nite size are needed, but these are difficult to
obtain. To allow lactose naturally present in
Dulce de Leche to crystallize to different sizes
Journal of Dairy Science Vol. 73, No. 3, 1990
606 HOUGH ET A L
TABLE 1. Sieves. resulting crystal size, and concentration of sand used for magnitude estimation of sensory versus
objective crystal size.
Sieve CrYd
aperture size
( m
... ...
125 115
250 307
700 622
840 895
1250 1207
I500 1490
'Standard number as presented to panelists.
was impractical because of lack of size unifor-
mity. Because of these difficulties, sand sieved
through different-sized screens was used as a
replacement. Concentration of sand in CFDL
was determined by approximating the number
of sand crystals to the number of lactose crys-
tals of similar size present in commercial Dulce
de Leche. The sieves, sand crystal sizes, and
concentrations used for magnitude estimation
are in Table 1 . Sizes cover the range found in
Dulce de Leche. Prior to the test, the panel
received an orientation session (13). Magnitude
estimation was done in duplicate on different
days.
Based on magnitude estimation, a sensory
scale was developed. With this, samples of
Dulce de Leche with different size and number
of lactose crystals were measured to control
scale validity. Also, for the same crystal size,
sand concentration was varied to see if it signif-
icantly affected sensory evaluation. These vari-
ations are summarized in Table 2.
Sandiness Threshold
As mentioned, for larger crystal sizes, sand
replaced lactose. For threshold sizes, solubiliza-
tion of lactose during sensory evaluation would
have probably influenced perception; therefore,
analytical grade lactose was used. It was
crushed in a mortar and then passed through a
series of sieves with apertures of 37, 44, 53,
and 62 p.Smaller apertures are not currently
available. The size of resultant crystals was
measured by dispersing them in CFDL in ap-
proximately 1?b concentration, obtaining the
following sizes: 45, 57, 69, 80, and 105 pm,
Journal of Dairy Science Vol. 73, NO. 3, 1990
Concentration
of sand in Sensory
Dulce Leche scale'
7 Wloog)
0 0
5 1
5 3
5 6
10 9
10 12
10 15
The reason crystal sizes are larger than the
corresponding aperture is because in measuring
size, the longest axis is considered. For the
smallest crystal size, Nestle's (Buenos Aires,
Argentina) microcrystalline lactose (used for
d i n g sweetened condensed milk) was em-
ployed as a standard. For this lactose, a 1.5%
mixture with CFDL provides a size and number
distribution as shown in Table 3.
The sensory analysis method used for
threshold determination is described by Lun-
dah1 et al. (10). The same testing panel de-
scribed earlier was used. To determine sensory
threshold four experiments were performed.
Experiment 1 . Sandiness threshold was de-
termined using six sizes of lactose crystals;
each one was mixed with CFDL in a 1.5%
concentration. Crystal sizes used were 45, 57,
69, 80, and 105 pn and microcrystalline lac-
tose (see Table 3). Mixtures of CFDL with
lactose were done within an hour of sensory
evaluation. Crystal-free Dulce de Leche was
used as the control sample (10). All samples,
TABLE 2. Sand concentration used to study influence of
this parameter on sensory perception of sandiness.
Concentrations
of sand
Sensory used in
scale Dulce
size de Leche
(g/lOo/g)
1 2.5, 5. 10
6 2.5. 5, 10
12 5 , 10, 20
 MEASUREMENT OF SANDINESS IN DULCE DE LECHE
TABLE 3. Size and number of lactose crystals in sample
prepared with 1.5% microcrystalline lactose in crystal-free
Duke de Leche.
crystal
size CNSdS
including control, were vigorously agitated
with a spoon in a serving cup before serving,
and panelists were instructed to do likewise
before taking the sample to mouth. This was
necessary to mix the lactose thoroughly and to
ensure uniformity in consistency of all samples.
The determination was done by duplicate.
Experiment 2. Sandiness threshold was de-
termined using 45-pm lactose crystals in six
different concentrations: . I , .25, .5, .75, 1, and
1.5%. Control and agitation were the same as
previous experiment.
Experiment 3. Experiment 3 was conducted
as Experiment 2 but lactose crystals were 105
P-
Experiment 4 . Presence of sensory sandiness
was determined in Dulce de Leche seeded with
microcrystalline lactose. To this purpose, Dulce
de Leche was made following a classical recipe
(12) and then seeded with Nestle's microcrys-
talline lactose according to the procedure given
by Hunziker (7) for sweetened condensed milk.
After 15 d of storage at room temperature, size
and number of crystals were measured micro-
scopically. Also, sensory evaluation was done
to see if the seeded sample was above or below
threshold. The sensory scale developed from
the magnitude estimation test was used. To
c o n f m the result, a paired comparison test
TABLE 4. Sensory sandiness scores, and crystal sizes and numbers of different Duke de Leche samdes.
crystal
Sample size cryds
(w) (no./@
A 190 4 x 104
B 650 1 x 103
C 78 7 x 104
'Confidence interval.
607
against CFDL was performed; panelists an-
swered which of the two samples presented
sandiness. The seeded sample and CFDL dif-
fered in color and flavor; therefore, to avoid
bias, two deliberately confusing pairs were
added at each session. These were: CFDL with
1.5% added lactose of 105-pm crystal size
(slightly above threshold), tested against the
seeded sample or against CFDL. Each panelist
tested 10 pairs in total, divided in two different
sessions. Subtracting the confusing pairs gave
six answers per panelist.
Statistical Analysis
Magnitude estimation results were analyzed
as described by Mori et al. (11) and threshold
results as proposed by Lundahl et al. (10). In all
cases, significance was determined at Pc.05.
RESULTS AND DISCUSSION
Size and Number of Crystals
The microscopic method to measure size and
number of crystals was replicated 11 times on
the same Dulce de Leche. Average and stan-
dard deviation for number of crystals were,
respectively, 2.2 x lo9 and 9.9 x lo8 crystals/g.
As to size, the mean was 4.1 pn and the
standard deviation was .28 pm. If quadruplicate
measurements are performed, the confidence
interval (b.05)for number of crystals is 2.05
x 109 crystais/g; for size it is .5 pm. Both are
considered adequate for practical purposes.
Sandiness Scale
The first responses from the sensory panel
provided a consensus sensory technique for
evaluating sandiness: one-half teaspoonful of
Sensory scores
Mean 95% Cll
1.7 .5
1.0 .8
.55 .39
Journal of Dairy Science Vol. 73. No. 3, 1990
608 HOUGH ET AL.

Figure 1 . Duke de Leche with a) laclose crys(als and b) sand crystals as seen through microscope ( 1 0 0 ~ )with
polarized light. Both samples were classified as equivalent sandiness by panel. Each scale division corresponds to 14.7 pm.

Journal of Dairy Science Vol. 73. No. 3, 1990

 MEASUREMENT OF SANDINESS IN DULCE DE LECHE 609
TABLE 5. Size and number of lactose crystals present in l sizes found in Dulce de Leche, i.e., 0 to
t
a
Dulce de Leche &ed with microcrystalline lactose during 1500 pm. Intermediate standards prepared with
cooling.
CFDL and sand are shown in Table 1. For
Crystal size crystals evaluation, a 15-cm line anchored with stan-
(W) (no./g) dards at equivalent lengths is used for presenta-
6 8 x lo8 tion to panelists. Three samples of Dulce de
15 9 x 106 Leche with different sizes of lactose crystals
20 5 x 104 were measured objectively and also using the
sensory scale. Results are in Table 4. Close
correspondence is observed, confirming validity
of scale. Analysis of variance of results from
h l c e de Leche was placed on tongue, pressed sand concentration variations (see Table 2) did
against the palate, and size of crystals as per- not show significant (F5.05) differences in sen-
ceived between the tongue and palate was eval- sory evaluation by the panel.
uated. From these results a reproducible sensory
The sensory panel concluded that use of sandiness scale was developed, which is equiv-
sand in replacement of lactose crystals to stim- alent to microscopic measurement of crystal
ulate sandiness produced an equivalent re- size.
sponse. Similarities in crystal appearance are
shown in Figure 1. A t test on sensory evalua-
tion means of these samples (using the 10 cm Sandiness Threshold
unstructured scale) showed equivalent sandi- Experiment I . Sandiness threshold was
ness. found to be between the sample of CFDL
Results from magnitude estimation were mixed with 1.5% microcrystalline lactose and
correlated according to Steven's law (13): the sample of CFDL mixed with 1.5% lactose
crystals 45 pm in size. Therefore, sandiness
s = C" will not be perceived at or below the crystal
where S = perceived sandiness, C = crystal sizes and numbers shown in Table 3.
size, and n = exponent of Steven's law. Experiment 2. Sensory threshold was be-
In Equation [l], n is the parameter of inter- tween the sample of CFDL mixed with . l %
est, because it indicates whether variations in lactose crystals 45 pm in size and the sample of
crystal size are amplified or diminished through CFDL mixed with .25% lactose crystals of the
sensory evaluation. In this case, n was 1.08, same size. The number of 45-pm crystals in
with its 95% confidence limits (6) including 1. concentrations of .1 and .25% were measured
Thus, sensory versus objective evaluation of microscopically. Results were 1.2 x 16 and 3.1
sandiness can be considered linear. Current lit- x I@ crystals/g, respectively. Thus, for crystals
erature (3, 13) offers no comparative values for of 45 pm or smaller, threshold will be between
n; the closest comparison would be visual ob- these numbers of crystals.
servation of length (3) with n = 1. Experiment 3. As in experiment 2, only the
Considering n = 1, a sensory scale of sandi- lowest concentration was below threshold.
ness was developed covering the range of crys- Numbers of 105-pm crystals in concentrations

TABLE 6. Sensory threshold perception of sandiness according to number and size of crystals.
Size
crystals 105 p 45 p 15 P 6Pn
WJg)
Between 0 and 4 x IO3 NQ No No No
Between 4 x Id and 1 6 Yes No No No
Between 16 and IO7 Unreal Yes No No
Between lo7 and IO9 unreal UIUeal ? No

Journal of Dairy Science Vol. 73, No. 3, 1990

610 HOUGH ET AL.
TABLE 7. Maximum number of lactose crystals present in
Dulce de Leche, according to size.
crystal Maximum
size crystals
(w) (no&)
6 1.3 x 109
15 9.2 x 10’
45 3.1 x 106
105 2.4 x 16
of .1 and .25% were 3800 and 8500 crystal&
respectively. Thus, for 105 pm or smaller,
threshold will be between these number of
crystals.
Experiment 4. Using the sensory sandiness
scale described, the mean score for Duke de
Leche seeded with microcrystalline lactose was
.22 (scale from 0 to 15) with a standard devia-
tion of .54. This is not significantly (b.05)
different from 0, i.e., no sandiness present.
Confirming this result, the paired difference
tests showed no significant (b.05)difference
between seeded Dulce de Leche and CFDL.
Results of size and number of crystals mea-
sured microscopically for seeded Dulce de
Leche are in Table 5 . Thus, below values
shown in Table 5 , sandiness will not be per-
ceived.
Results indicate that according to the size of
the lactose crystals present, the sandiness
threshold will depend on the number of crys-
tals; i.e., there is no single threshold. A sum-
mary of these results is presented in Table 6.
This table is useful for quality control of the
sandiness defect: the size and number of crys-
tals of a sample can be measured microscopi-
cally, and values from the table will indicate
whether sandiness will be perceived or not. In
Table 6, for certain sizes, it is indicated when
the number of crystals would probably not oc-
cur Le., when more lactose crystallized is indi-
cated than is normally present in Dulce de
Leche. The maximum number of crystals for a
given size were calculated as follows:
As mentioned in the introduction, lactose
concentration in Dulce de Leche is 9.85 dl00 g
of Dulce de Leche. Lactose density is 1.54 g/
cm3 (20), therefore, supposing it is completely
crystallized, it occupies .0639 cm3/g of Dulce
de Leche. To calculate the volume of a single
tomahawk-shaped a-lactose crystal, Hunziker
Journal of Dairy Science Vol. 73, No. 3. 1990
(7) indicated that the longest axis of this crystal
is 1.33 times the diameter of an equal volume
sphere. With the volume of a single crystal, and
the volume occupied by lactose in totally crys-
tallized Dulce de Leche, the maximum number
of crystals per gram were calculated. Results
are shown in Table 7.
Hunziker’s threshold for sandiness in swee-
tened condensed milk is more than 4 x lo8
crystals/cm3 (7). This is within the order of
values from Tables 6 and 7, considering Dulce
de Leche’s density approximately 1.3 s/cm3
(12).
ACKNOWLEDGMENTS
Authors acknowledge financial support of
the Argentine Scientific and Technological Sec-
retariat (SECYT) and Buenos Aires Province
Research Committee (CIC).
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Journal of Dairy Science Vol. 73, No. 3, 1990