International Journal of Food Properties

ISSN: 1094-2912 (Print) 1532-2386 (Online) Journal homepage: https://www.tandfonline.com/loi/ljfp20

Optimization Study of Sulfur Dioxide Application in

Processing of Sultana Raisins

Dimitris Lydakis , Ioanis Fysarakis , Michael Papadimitriou & George

Kolioradakis

To cite this article: Dimitris Lydakis , Ioanis Fysarakis , Michael Papadimitriou & George
Kolioradakis (2003) Optimization Study of Sulfur Dioxide Application in Processing of Sultana
Raisins, International Journal of Food Properties, 6:3, 393-403, DOI: 10.1081/JFP-120020117

To link to this article: https://doi.org/10.1081/JFP-120020117

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 INTERNATIONAL JOURNAL OF FOOD PROPERTIES
Vol. 6, No. 3, pp. 393–403, 2003

Optimization Study of Sulfur Dioxide Application

in Processing of Sultana Raisins

Dimitris Lydakis,* Ioanis Fysarakis, Michael Papadimitriou, and

George Kolioradakis

Technological Education Institute of Crete, Heraklion, Crete, Greece

ABSTRACT

The current use of sulfur dioxide (SO2) fumigation to bleach Sultana raisins has a
number of limitations including poor absorption into the product and air pollution
problems. A study was conducted to improve the sulfitation process by use of SO2
solutions as an alternative. A factorial design was used to evaluate the effect of
concentration, temperature and raisin=solution ratio on the absorption of SO2 by
raisins. It was found that the most important variables were concentration and
temperature of the used solutions. The amount of SO2 absorbed by the raisins was
time dependent, but the absorption rate declined after the first 15 min of contact. The
use of SO2 solutions was found to be more efficient than fumigation with raisins
retaining from 9–21% of applied SO2 in solution compared to 3–5% of SO2 applied as
a gas. Higher final SO2 tissue concentrations could be achieved in the liquid application
method compared to the gas method. There were no negative consequences of the
proposed solution-based system with respect to post-treatment drying time and the
storability of the raisins.

Key Words: Bleaching; Raisin; Raisin processing; Sulfur dioxide; Sultana.

*Correspondence: Dimitris Lydakis, Technological Education Institute of Crete, Heraklion, Crete,

Greece 71110; Fax: 0032810 318204; E-mail: dlydakis@steg.teiher.gr.

393

DOI: 10.1081=JFP-120020117 1094-2912 (Print); 1532-2386 (Online)

Copyright # 2003 by Marcel Dekker, Inc. www.dekker.com
394 Lydakis et al.

INTRODUCTION

Sulfur dioxide (SO2) and its derivatives have long been used in foods as general food
preservatives. They act as antioxidant, bleaching and reducing agents, and as such inhibit
non-enzymic browning, enzyme catalyzed reactions, and control microorganisms.[1] The
sulfiting process is generally performed by gas fumigation or by immersion in solutions of
SO2 generating compounds.
Sultana raisins are produced from sun-dried Sultanina grapes. The grapes are usually
dipped in 5–7% K2CO3 and 0.5% olive oil or 2.5% K2CO3 and 2% ethyl oleate before
drying.[2] In general, sun-dried Sultana raisins do not have a uniform color. In the same lot
of raisins, light yellow, brown, dark brown, and black-colored fruits can be found. The
color of the raisins during storage darkens due to browning reactions. This is known to be
caused by polyphenoloxidase (PPO) activity, and also by non-enzymic reactions.[3] Sulfur
dioxide is extensively used in Sultana raisins to improve their color and preserve their
quality. Sultana raisins treated with sulfur dioxide develop a lighter and more uniform
color. This is due to the bleaching of dark colored pigments, which are the products of the
aforementioned oxidative processes.
Sultana raisins are sulfited after sun drying, during industrial process. This is in
contrast to Golden Bleached and Sulfur Bleached raisins and many others dehydrated
fruits, which are treated with SO2 before drying. In Greece, Sultana raisins were formerly
fumigated for 1–2 hours placed on trays in purpose-constructed rooms, where sulfur
powder was burned to produce SO2.[4] The method in current usage was examined in a
preliminary study conducted in two Sultana processing factories located in Heraklion,
Crete, Greece. Sultana raisins are fumigated for 20–30 min in a rotating stainless steel tank
equipped internally with a worm screw. Sulfur dioxide used in this system is obtained by
expansion of compressed ‘‘liquid’’ SO2 contained in pressure tanks. Before fumigation,
raisins are thoroughly washed and are transferred to the fumigation tank wet. The presence
of a water film on the surface of the raisins is essential for successful treatment. The SO2
gradually dissolves in the water and is then absorbed by the raisins. Gaseous SO2
absorption through a dry raisin skin is minimal. Following fumigation, raisins are sprayed
with fresh water to wash out excess adsorbed SO2 and then dried in a convective air drier at
60–70
C to a water content of 14–15% (wet basis). The concentration of SO2 in treated
Sultana raisins after processing is lower than in other dehydrated fruits and normally
ranges between 500 and 1200 mg=kg. Higher concentrations are often desired, but are
hardly ever obtained in practice. This is due to the fact that the skin of the raisins is less
permeable than the skin of other SO2 treated fruits such as apricots, pears, peaches, etc. In
addition, a significantly higher part of the initially absorbed SO2 is desorbed during drying
due to the higher temperature levels used in the drying process of Sultanas compared to
sun drying process of other fruits.
The major disadvantage of the currently used fumigation system is the low ratio of
applied to absorbed SO2. Since the fumigation tank is both sides open to put in and out the
raisins, a significant part of the applied gas SO2 escapes into the environment, despite the
employment of various scrubbing systems. The system is also ineffective when high levels
of SO2 in the raisins are required e.g., to bleach dark colored raisins, or when large size
raisins are processed.
In this study, Sultana raisins were sulfited using SO2 solutions. In order to improve the
sulfiting process, the effects of the operating conditions, namely solution concentration,
Sulfur Dioxide and Sultana Raisins 395

temperature, raisin to solution ratio, and contact time on the SO2 level in raisins were
evaluated. The relation between fruit color and SO2 absorption was studied. Possible effects
of sulfiting method, (SO2 solutions vs. gas SO2 fumigation), on the drying rate was also
investigated. The final goal was to develop an alternative technique of SO2 application in the
Sultana processing industry, which is more effective with reduced environmental pollution.

MATERIALS AND METHODS

Plant Material

Sultana raisins were purchased from The Sultanina Growers Association of Greece,
Heraklion Crete, in September 2001. Selected raisins were dipped in 7% w=v
K2CO3 þ 0.5% olive oil and sun-dried. After drying, raisins were stored for 30 days in
plastic boxes at ambient temperature.

Sulfur Dioxide Treatment Conditions

Raisins were treated with SO2 solutions prepared by dissolving compressed SO2
(Laffort and Cie., Bordeux, France), in distilled water. Before treatment, raisins were
thoroughly washed with fresh tap water and then left to drain. Raisins were enclosed in
airtight plastic containers with the SO2 solutions. Containers were placed in a rotating
system at a speed of 20 rounds per min, to simulate the conditions in the rotating tanks
used in commercial practice. Control samples of raisins were fumigated with gaseous SO2
in airtight boxes. Following SO2 treatment raisins were thoroughly rinsed with water and
then dried at 65
C in a laboratory dry oven (Memmert, Schwabach, Germany) with forced
air for 60 min to a water content of 14–15% (wet basis).

Experimental Design

Effects of Concentration, Temperature, and Raisin to Solution Ratio on

Sulfur Dioxide Absorption

Raisins were treated for 20 min with SO2 solutions of different concentrations (2, 3, 4,
5, and 6% w=v). Temperature of the SO2 solution was adjusted before application at 20,
30, and 40
C in a temperature controlled water bath (Memmert, Schwabach, Germany).
Samples of 40 g (five replicates per treatment) were treated with 10, 20, and 40 cm3 of SO2
solution.

Effects of Contact Time on Sulfur Dioxide Absorption

Raisins were treated for 10, 20, and 30 min with 4% w=v SO2 solutions at 20, 30, and
40
C. Samples of 40 g (five replicates per treatment) were used. After drying SO2 content
was measured.
396 Lydakis et al.

Effects of the Sulfiting Method on Raisin Color

Raisins were SO2 gas fumigated and treated with a 4% w=v SO2 solution at 20, 30,
and 40
C. After drying, color parameters were measured in 10 samples per treatment with
a SO2 content of 960–1010 mg=kg.

Effects of Fruit Color on Sulfur Dioxide Absorption

Raisins were classified in three lots with light brown, brown, and dark brown=black
color. Samples of 40 g prepared from each lot were treated with 4% SO2 solution for
20 min at 20, 30, and 40
C. Ten replicates per treatment were used. After drying SO2
content was measured.

Effects of Storage Time on Sulfur Dioxide Loss and Raisin Color

Raisins were treated with a 4% w=v SO2 solution and SO2 gas fumigated to a SO2
content of 780–840 mg=kg. Samples of 40 g (30 replicates per sulfiting method) were
stored at 20  2
C for up to six months, enclosed in thermo-sealed polyethylene bags.
Retained SO2 and color parameters were monitored at monthly intervals.

Effects of the Solution Sulfiting Method on Drying Rate

Raisins were treated for 20 min with 10, 20, and 40 cm3 of a 4% w=v SO2 solution.
Control samples were treated with 10 cm3 of water. Samples of 50 g (five replicates per
treatment) were used. Following treatment samples were dried at 65
C for 60 min. Weight
changes were monitored at 5 min intervals during drying.

Analysis

The SO2 analysis was carried out with the Optimized Monier-Williams method for
sulfites.[5] This method involves distillation of the SO2 formed from refluxing with
hydrochloric acid. The SO2 is quantified by titration with sodium hydroxide. The SO2
was measured in raisins after drying and results were expressed as SO2 mg=kg (wet basis).
The color of the raisins was measured using a Minolta Colourimeter model CR-300
(Minolta, Osaka, Japan). The raisins were placed in white cups of 5 cm diameter and 3 cm
depth. Every sample was pressed sufficiently, so that the surface appeared flat. Three
measurements were taken at different points of the sample. Cups were reloaded twice and
three measurements were taken (nine measurements per sample in total). Means of L*, a*,
and b* for each sample were automatically calculated. Subsequently, Chroma
(a*2 þ b*2)1=2 and Hue [atan(b*=a*)] were calculated.
The determination of the water content in raisins was conducted by drying 3 g of
ground raisins homogenized with diatomaceous earth to constant weight on a steam
bath.[6]
Sulfur Dioxide and Sultana Raisins 397

Statistics

Multiple Linear Regression Analysis was used to detect the effect of solution concen-
tration, temperature and raisin=solution ratio on SO2 content in raisins. Data were tested using
Statistica for Windows, StaSoft Inc, 1996.[7] Analysis of Variance (ANOVA) was performed
and Fisher’s LSD method was used to establish differences at P < 0.05.

RESULTS AND DISCUSSION

The SO2 contents measured in Sultana raisins treated with SO2 solutions are shown in
Fig. 1 and the Regression Analysis results in Table 1. The results indicate that the absorption
of SO2 increased as the concentration and the temperature increased. On the contrary,
increasing the raisin=solution ratio decreased the absorption of SO2. At each temperature
level, SO2 measured in raisins increased in an approximately linear fashion as the
concentration of the SO2 solutions increased. Increasing the temperature of the SO2 solution
from 20 to 30, and 40
C increased SO2 content on, an average between 46–47% and 75–86%,
respectively. Similar effects of temperature and solution concentration on the absorption of
SO2 were found in apricots[8] and flint corn.[9] Sulfur dioxide diffusivity also increased in
green bananas when they were treated with sodium metabisulfite solutions at increasing
temperatures and concentrations.[10] Results obtained from treatments performed under the
same operating conditions of temperature and solution concentration, lead to the conclusion
that doubling the raisin=solution ratio decreased the SO2 content by 23–25%.
Sulfur dioxide levels in Sultana raisins treated under the experimental conditions used
in this study range from 500–3000 mg=kg. Different combinations of the treatment
conditions resulted in similar levels of SO2 content. It is suggested therefore that the
proposed sulfiting system is quite flexible and efficient to establish the highest levels of
SO2 content allowed (2000 mg=kg).[11] In the study contacted in Sultana processing Greek
factories it was found that, in the fumigation system in use, 15–30 kg of gas SO2=1000 kg
of raisins are used to establish a SO2 concentration in raisins of 500–1200 mg=kg. Raisins
are normally fumigated for 20–30 min. When higher levels of SO2 are required, fumigation
time increases and the SO2 used often exceeds the 50 kg=1000 kg raisins treated. It means
that in practice, the raisins retain only 3–5% of the applied SO2. In this experimental study,
raisins treated at 20
C with 10 cm3 SO2 solution=40 g retained 9.1–10% of the applied SO2
(Table 2). When the SO2 solutions were pre-warmed at 30 or 40
C, 11.4–16.1% and
13.2–20.9% of the applied SO2, respectively, were retained. The percentage of retained
SO2 decreased when 40 g of raisins were treated with 20 or 40 cm3 of SO2 solution.
However, if such a treatment should be applied, e.g., to achieve a SO2 level of
1500–2000 mg=kg at ambient temperature, a significant part of the applied solution
could be drained and re-used.
Sulfur dioxide absorbed by raisins treated with equal quantities of 4% w=v SO2
solutions at 20, 30, and 40
C was found to be time dependent (Fig. 2). The absorption rate,
however, was significantly higher during the first 15 min of contact and subsequently
declined. An analogous absorption curve was obtained by Epanomeritakis,[4] after dipping
Sultana raisins in water for 5–30 min. Maize steeped in water or SO2 solutions also showed
a very rapid initial absorption, followed by a subsequent absorption that was directly
proportional to the square root of the time.[12]
398 Lydakis et al.

Figure 1. Sulfur dioxide content measured in Sultana raisins treated for 20 min with SO2 solutions
of different concentrations (2–6%) at 20 (r), 30 (j), and 40
C (m), with a raisin=solution ratio of
1 : 1 (up), 2 : 1 (middle), and 4 : 1 (down); n ¼ 5. Vertical bars show SEM; n ¼ 15.

Color is a major quality attribute of any food and consumers tend to prefer a light and
uniform color in Sultana raisins. During this study the relation between color and SO2
content was investigated. Absorption of SO2 by the raisins caused color changes.
Compared to the raw product, SO2 treated raisins acquired higher L* and b*, but slightly
Sulfur Dioxide and Sultana Raisins 399

Table 1. Regression analysis results.

t-Value p-Level
CON 36.04 <0.0001
RAT 26.75 <0.0001
TEMP 37.62 <0.0001

Note: SO2 ¼ 199.28 þ 236.27 (CON)  198.98

(RAT) þ 47.76 (TEMP).
Dependent variable ¼ SO2 (mg=kg), independent
variables ¼ solution concentration CON (% w=v),
temperature TEMP (
C), and raisin=solution ratio
RAT (g=mL). R2 ¼ 0.94, F ¼ 1143.3, df ¼ (3,
221), p < 0.0001.

lower a* values. Color changes induced by SO2, were found to be dependent on the
concentrations of SO2. In apricots, treatment with SO2 gas and metabisulfite solutions
caused differences in the color of the dried apricots as the former gave slightly higher
Hunter L and lower þa and þb values.[13] In raisins with similar concentrations of SO2,
either gas fumigated or treated with SO2 solutions at 20
C, the color parameters changed
similarly and no significant differences were found (Table 3). On the contrary, raisins
treated with pre-warmed SO2 solutions at 30 or 40
C obtained a lighter and more uniform
color compared to raisins with similar SO2 content treated at 20
C. It is known that during
the sulfiting of the raisins, a simultaneous process of SO2 absorption and chemical reaction
with different substances in raisins occurs. It can be assumed that the color differences in
raisins with similar SO2 content treated at different temperature levels are related to the
higher bleaching activity of SO2 at higher temperature levels.
Similar levels of SO2 were measured in light brown and brown colored raisins, while
in dark brown and black raisins treated under the same conditions significantly higher
levels of SO2 were found (Table 4). It is known that fruit skin integrity, among other
factors, affects raisin color during drying and storage. Pangavhane et al.[14] found that
raisins with better skin integrity had much lighter color. By contrast, mechanically abraded

Table 2. Percentage retention of the applied SO2 measured in raisins treated for 20 min with
different concentrations of SO2 solutions (2–6%) at 20, 30, and 40
C.

Raisin : solution ratio

4:1 2:1 1:1

SO2
concentration 20
C 30
C 40
C 20
C 30
C 40
C 20
C 30
C 40
C
2% 10.0 15.9 20.4 6.7 10.0 14.1 4.3 6.7 8.2
3% 9.9 15.7 19.1 6.4 9.7 12.7 3.8 5.7 7.1
4% 9.6 14.9 17.5 6.0 8.7 10.9 3.6 5.1 6.2
5% 9.7 12.3 15.7 5.5 8.1 9.6 3.3 4.7 5.5
6% 9.1 11.8 14.3 5.1 7.2 8.4 3.2 4.2 4.9
400 Lydakis et al.

Figure 2. Sulfur dioxide content measured in Sultana raisins treated with 4% w=v SO2 at 20 (r),
30 (j), and 40
C (m) for 10, 20, and 30 min; n ¼ 5. Vertical bars show SEM; n ¼ 15.

berries were found to produce a darker final product.[15] Dark brown and black colored
Sultana raisins are normally produced from berries, which have been insect infested,
diseased with fungi, or those in which the skin was mechanically interrupted.[2] It is
conceivable that skin disruption, make the absorption of O2 easier and this accelerates the
formation of black pigments through enzymic and chemical oxidation reactions. Skin
cracks were detected by light microscopy in most of the black colored raisins examined in
this study. Corn kernels with apparent surface cracks or other breaks in the pericarp also
showed increased sorption of SO2.[16] Despite the higher SO2 levels, color parameters in
black colored raisins did not changed proportionally. Nevertheless, acceptable levels of
bleaching were achieved in black colored raisins after treatments with pre-warmed
solutions, due to the high SO2 concentration in combination with the higher bleaching
activity of SO2 at these temperature levels.
During storage, SO2 concentration in dehydrated fruits declines.[17,18] In our study, the
percentages of the initial SO2 concentration retained by the raisins treated either with SO2
solutions or gas fumigated, were monitored for six months after treatment (Table 5).
Retained SO2 decreased in a similar fashion in all samples, regardless of the sulfiting

Table 3. Lightness (L*), chroma (C*), and hue of Sultana raisins treated either with
SO2 solution at 20, 30, and 40
C or SO2 gas fumigated. These color parameters were
measured with a Minolta colorimeter CR-300. Similar letters indicate non-statistically
significant differences.

Treatment SO2 content (mg=kg) L* C* Hue (grade)

Control 0 31.16a 17.39d 49.2h
20
C (gas) 987.8 35.16b 18.45e 58.76i
20
C (sol.) 964.5 34.76b 18.62e 58.60i
30
C (sol.) 1010.3 37.77c 19.63f 63.90j
40
C (sol.) 998.4 38.22c 21.45g 67.01k
Sulfur Dioxide and Sultana Raisins 401

Table 4. Sulfur dioxide concentrations (mg=kg wet basis)

measured in light brown, brown, and dark brown=black
Sultana raisins treated with 4% w=v SO2 solutions at 20,
30, and 40
C. Similar letters indicate non-statistically
significant differences.

Raisin color 20
C 30
C 40
C

Light brown 886.9a 1267.0c 1769.8e
Brown 905.0a 1284.7c 1784.5e
Dark brown=black 994.1b 1512.6d 2002.2f

method used. After three and six months in storage, approximately 68% and 51%,
respectively, of the initial SO2 was retained. Despite the higher rates of SO2 loss during
the first three months of storage practically no browning was observed. This is probably
due to the presence of adequate quantities of non-bound SO2 to prevent oxidative
processes in that period. Once this period was over, the presence of browning (mainly
manifested as a reduction of C* and hue values), could be related to the decrease in SO2
content.
Figure 3 presents the weight changes of raisins treated for 20 min with plain water and
SO2 solutions. The initial weight of control samples treated with 10 cm3 of plain water
increased by 6.9%. In samples treated with 10, 20, and 40 cm3 of 4% SO2 solution the
initial weight increased by 8.3, 9.2, and 10%, respectively (Fig. 3). These results indicate
that the presence of SO2 increased the absorption rate of the raisins. Similarly, the
absorption rate of SO2 solutions was found to be higher than in plain water during the

Table 5. Changes in SO2 content and color parameters lightness (L*), chroma (C*), and hue of
Sultana raisins treated either with SO2 solution or SO2 gas fumigated and stored for six months at
room temperature (20  2
C). Similar letters indicate non-statistically significant differences.

Storage period (months)

Treatment 0 1 2 3 4 5 6
Retained SO2%
SO2 sol. 100a 79.27b 71.79c 68.56d 64.81f 63.39g 61.64h
SO2 gas 100a 81.18b 69.70c 68.10d 66.11e 63.52g 60.64h
L*
SO2 sol. 34.07a 33.73a 33.42a 32.68b 31.56c 30.07d 28.94e
SO2 gas 33.85a 33.75a 33.03ab 32.87b 30.28cd 29.7d 29.25de
C*
SO2 sol. 17.58a 17.21a 16.74b 16.33bc 15.10d 12.90e 11.80f
SO2 gas 17.30a 17.74a 17.00ab 16.17c 14.80d 12.83e 11.83f
Hue (grade)
SO2 sol. 58.45a 58.88a 59.98ab 60.24b 58.62a 52.69c 49.46d
SO2 gas 58.28a 57.59a 57.70a 59.44a 57.76a 51.93c 48.09d
402 Lydakis et al.

Figure 3. Weight changes in raisins (40 g) treated either with 10 mL of plain water or with 10, 20,
and 40 mL of 4% w=v SO2 solution and dried at 65
C for 60 min; n ¼ 5. Vertical bars show SEM;
n ¼ 20.

steeping process of three maize hybrids.[12] Sulfur dioxide was also found to increase the
permeability of the skin and the drying rate in grapes[18] and apricots.[12] In apricots,
acceleration of drying was analogous to the SO2 concentration. Nevertheless, apricots
sulfited by dipping in sodium metabisulfite (Na2S2O5) solution at a lower concentration of
SO2 compared to gas SO2 treated, resulted in the same drying rate. In our study, control
and SO2 treated raisins dried at 65
C regained their initial weight in approximately
13–15 min. In this drying period, raisins responded similarly to apricots, resulting in higher
drying rates as the applied quantity of SO2 solution, and, consequently, absorbed SO2
increased. At the completion of the 60 min drying time, however, all the samples weighted
5.3–5.7% less, and no significant differences were found between control and SO2 treated
raisins. It can be concluded that the contact with SO2 solutions, although increases
significantly the initial weight compared to control samples, it does not affect the drying
time of the raisins.

CONCLUSIONS

From the results of this study it is concluded that when raisins are treated with SO2
solutions, the SO2 absorbed and subsequently retained by the raisins, is determined by the
concentration, the temperature, the contact time and the quantity of the used solution.
Compared to the currently used gas fumigation method, the proposed system is more
flexible since the targeted level of SO2 can be achieved by modifying the aforementioned
four parameters. The system is also more efficient, since the same quantity of SO2 yields
significantly higher levels of SO2 and the highest levels of SO2 content allowed could be
achieved. The use of pre-warmed solutions can overcome the difficulty of bleaching dark
colored raisins. Moreover, the use of SO2 solutions would help to reduce air pollution
since only a small part of the pre-dissolved gas escapes from the solution compared to the
use of the gas as a fumigant.
Sulfur Dioxide and Sultana Raisins 403

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Received June 28, 2002

Accepted December 23, 2002