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Bioresource Technology 99 (2008) 3528–3533

Decolorization of sugar syrups using commercial and sugar beet

pulp based activated carbons
H.L. Mudoga, H. Yucel, N.S. Kincal *

Department of Chemical Engineering, Middle East Technical University, Ankara 06531, Turkey

Received 3 November 2006; received in revised form 10 July 2007; accepted 28 July 2007
Available online 7 September 2007

Abstract

Sugar syrup decolorization was studied using two commercial and eight beet pulp based activated carbons. In an attempt to relate
decolorizing performances to other characteristics, surface areas, pore volumes, bulk densities and ash contents of the carbons in the
powdered form; pH and electrical conductivities of their suspensions and their color adsorption properties from iodine and molasses
solution were determined. The color removal capabilities of all carbons were measured at 1/100 (w/w) dosage, and isotherms were deter-
mined on better samples. The two commercial activated carbons showed different decolorization efficiencies; which could be related to
their physical and chemical properties. The decolorization efficiency of beet pulp carbon prepared at 750 °C and activated for 5 h using
CO2 was much better than the others and close to the better one of the commercial activated carbons used. It is evident that beet pulp is
an inexpensive potential precursor for activated carbons for use in sugar refining.
Ó 2007 Elsevier Ltd. All rights reserved.

Keywords: Sugar syrup; Decolorization; Activated carbon; Beet pulp

1. Introduction dioxide or hydrogen peroxide, however, although these

Activated carbon adsorbents having a large internal sur-
face area and relatively nonpolar surface are primarily
being used to remove organic compounds from both liquid
and gaseous streams (Smisek and Cerny, 1970). One signif-
icant application makes use of its decolorization properties
in several areas including beet and cane sugar refining. The
presence of colored compounds in the sugar syrups results
from reactions occurring during the production. The chem-
ical structure of some of these coloring materials is quite
complex and difficult to determine in many cases. The most
significant colored substances that develop during sugar
processing can be classified in three general groups: (a) mel-
anins (b) melanoidins and (c) caramels (Kearsley and
Dziedzic, 1995). Conventional methods to prevent forma-
tion of these compounds include treatment with sulfur
*
Corresponding author. Tel.: +90 312 2102617; fax: +90 312 2102600.
E-mail address: nskincal@metu.edu.tr (N.S. Kincal).
treatment steps retard the formation of some of these com-
pounds, they cannot eliminate them altogether. In order to
produce high quality white sugar or when very good clarity
is required in the syrup products such as those used in col-
orless soda drinks, a treatment of juice with activated car-
bon or ion exchange resins is usually required (van der Poel
et al., 1998).
Activated carbons can be produced from various carbon
containing species by physical and chemical activation
methods. Most common feed stocks for commercial produc-
tion may be given as coal, peat and wood (Smisek and
Cerny, 1970). Other commercial and potential feed stocks
include renewable agricultural by-products, namely nut
shells (hazelnut, walnut, pecan, etc.), fruit kernels/seeds/
stones (apricot, apple, etc.), hulls (soybean, rice, etc.), pulps
(paper, apple, beet) and olive stone (Balcı et al., 1994; Özer
et al., 1998; Baçaoui et al., 2001; Yun et al., 2001; Aygün
et al., 2003).
Ahmedna and co-workers (Ahmedna et al., 1997b,
2000) extensively studied the preparation, properties and

0960-8524/$ - see front matter Ó 2007 Elsevier Ltd. All rights reserved.
doi:10.1016/j.biortech.2007.07.058
 H.L. Mudoga et al. / Bioresource Technology 99 (2008) 3528–3533 3529

decolorization applications of activated carbons produced Table 1

from agricultural by-products (sugar cane bagasse, rice
hulls, rice straw, pecan shells using different binders (beet
and sugar cane molasses, corn syrup and coal tar). They
found that the type of by-product, binder used and the acti-
vation method determine the physical and chemical proper-
ties and thus decolorization properties of granular
activated carbons.
It has been demonstrated previously that activated car-
bon can be produced from beet sugar pulp which is a by-
product of beet sugar processing (Özer et al., 1998 and
2002). Exploration of the sugar decolorization properties
of carbons made from sugar beet pulp was undertaken to
find another important outlet for this beet sugar plant
waste primarily being used as cattle food.
The aim of the present work was to compare the decol-
orization capabilities of beet pulp activated carbons pro-
duced locally in the laboratory scale with some
commercial sugar decolorizing activated carbons and to
look for possible correlations between the physical proper-
ties of activated carbons and their sugar syrup decoloriza-
tion capabilities; with the hope of shedding some light on
potential studies of preparing activated carbons for
decolorization.
2. Methods
2.1. Syrup
The syrup (thick juice) was obtained from the Ankara
Sugar Factory. A series of grab samples of the syrup were
collected at the point just before the sugar-boiling step in
the factory. The sampling was done every 6 h during a per-
iod of 48 h. The samples were stored in the refrigerator in a
plastic container. The properties of the syrup, determined
according to Anon (1994) are given in Table 1. The refrac-
tive index values of the syrup (determined using Abbe BS
60/70 Refractometer) were 1.4450 at its natural pH of
7.7; 1.3630 at pH 4 and 1.4048 at pH 9. The indicator
value, I.V., defined as the ratio of the refractive indices at
pH value of 9 to that at pH 7 (Kearsley and Dziedzic,
1995) can be estimated on the basis of these values to be
1.04, indicating the major colorants in the syrup to be mel-
Properties of the syrup
Color, ICUMSA units 3149
Brix, % 66.83
Polarity, % 61.73
Purity, % 92.37
Ash, % 4.01
Absorbance 2.4376
pH 7.7
anoidins (I.V. 1.0–1.2) or caramels (I.V. 1.0–1.5) Godshall
(1997).
2.2. Commercial activated carbons
Two reference commercial carbons, selected on basis of
the manufacturer’s recommendations, were obtained from
Waterlink Sutcliffe Carbons, England. The carbons used
were DCL320 (wood base, activated with phosphoric acid)
and DCL200 (coal base, steam activated).
2.3. Beet pulp activated carbons
Eight different beet pulp activated carbon samples pre-
pared by Özer et al. (1998) and Özer and Çam (2002) were
used. Two samples were prepared (Özer et al., 1998) by
direct carbonization and were activated at 750 °C under a
stream of carbon dioxide for 2 h or 5 h (750C2 and
750C5). Six samples were prepared (Özer and Çam, 2002)
by first impregnating with phosphoric acid overnight, fol-
lowed by activating under a stream of nitrogen at 300 °C
or 500 °C for 1.5–5 h (300P1.5, 300P3, 300P5, 500P1.5,
500P3, 500P5). In the coding of the samples, the first three
digits indicate the activation temperature; the following let-
ter is C for the directly carbonized – CO2 activated samples
and P for the phosphoric acid impregnated – N2 activated
samples; and the number following the letter indicates the
time of activation in hours.
2.4. Methods of characterization of the activated carbons
The commercial and beet pulp based activated carbons
are characterized with the methods below and the results
are given in Table 2.

Table 2
Some properties of the activated carbons
Activated carbon pH of susp. Electrical cond. of susp, lS Ash, mg g1 Pore size, nm Pore volume, cm3 g1 Density, g cm3
DCL 320 4.5 285 36 3.6 1.30 0.28
DCL 200 6.7 17.1 168 2.6 0.54 0.35
750C5 6 24.8 183 2.2 0.65 0.28
750C2 10.2 972,000 348 3.8 0.25 0.25
500P5 2.8 3200 210 3.3 0.55 0.67
500P3 2.8 2600 183 2.7 0.27 0.60
500P1.5 2.8 2410 193 2.6 0.22 0.58
300P5 2.8 1820 197 3.5 0.28 0.62
300P3 2.8 2320 192 3.4 0.28 0.71
300P1.5 2.8 1870 202 4.3 0.20 0.61
3530 H.L. Mudoga et al. / Bioresource Technology 99 (2008) 3528–3533
2.4.1. Surface area, pore volume and pore size
The BET surface area of the samples were determined
by nitrogen adsorption at 77 K using Micrometrics ASAP
2000 automatic surface area analyzer after the samples
were dried under vacuum at 100 °C for 3 h to remove
moisture. The surface area was determined using the N2
adsorption data at 77 K in the relative pressure range of
0.05–0.25, and taking the cross-sectional area of the nitro-
gen molecule to be 0.162 nm2. The total pore volume was
based on the N2 amount adsorbed at relative pressure
greater than 0.98, and taking the liquid molar volume of
N2 to be 34.65 cm3/g at 77 K.
The average pore diameter, D, was calculated from the
equation based on uniform cylindrical pores as given below
 For the syrup decolorization experiments, syrup samples
ð4Þ ðPore volumeÞ
D¼
BET area
2.4.2. Bulk density
Powdered activated carbon samples were placed in grad-
uated cylinders, tapped several times until constant volume
(10 mL) was obtained, and measuring the weight, the bulk
density was calculated as the ratio of weight to volume.
2.4.3. Moisture and ash contents
Moisture content was determined by the measurement of
dry weight after bringing the sample (about 1 g) to constant
weight in an air circulation oven at 115 °C; and ash content
was determined based on the weight of the residue obtained
after 1.5 h in a furnace at 950 °C under air circulation.
2.4.4. pH
Suspensions of the samples (1% w/w) in distilled water
were heated to 90 °C, subjected to continuous stirring for
20 min, cooled to room temperature and the pH of the
solution was determined using a Leeds Northrup 7415
pH-meter (Ahmedna et al., 1997b).
2.4.5. Electrical conductivity
Suspensions of the samples (1% w/w) in distilled water
were subjected to continuous stirring for 20 min, and the
electrical conductivity of the solution was measured
(Ahmedna et al., 1997b) at 25.6 °C using a Jenway 4020
conductivity-meter.
2.4.6. Iodine test, molasses test and syrup decolorization
experiments
These experiments were all similar in the sense that an
iodine solution, diluted molasses or sugar syrup was con-
tacted with the active carbon; the color of this sample was
compared to that of a blank prepared and treated the same
way without the activated carbon (Pendyal et al., 1999;
Ahmedna et al., 1997a, 1997b). For the iodine test,
100 mL of stock solution (2.7 g I2 and 4.1 g KI in 1 L of
solution) was added to 0.5 g activated carbon in 10 mL of
5% HCl solution, 5 min contact time was allowed, the sam-
ple was filtered through Whatman No. 110 filter paper and
the percentage color removal was based on the volumes of
0.1 M sodium thiosulphate required (using starch as the
indicator) for the sample and the blank filtrates. For the
molasses test, the test solution was prepared by dissolving
10 g of sugar beet molasses and 15 g of Na2HPO4 in
500 mL of water and sufficient H3PO4 to make pH 6.5,
diluting to 1 L and filtering through a thin layer of filter
aid (diatomaceous earth). Fifty milliliter of this solution
was added to 0.5 g of activated carbon; the mixture was well
stirred, and was placed on a heating plate along with the
blank and brought to boil. The percentage color removal
was based on the absorbance readings taken 420 nm using
a Hitachi U-3200 Spectrophotometer after the sample and
the blank were filtered through Whatman No. 4 filter paper.
were adjusted to pH 7.0 using 0.1 M HCl and Thymol Blue
indicator, two 100 g of samples were brought to 80 °C in a
water bath with shaking at 160 rpm, 0.2–1.0 g of activated
carbon was added to one of the samples, and 20 min was
allowed, which had been verified to be sufficient for the
attainment of equilibrium. Then, the samples were clarified
in two steps. The first filtration was through Whatman No.
110 filter paper, followed by addition of 1% diatomaceous
earth and heating to 70 °C for reducing the viscosity. The
second filtration was through Nalgene Filtering assembly
with a 0.45 lm membrane for removal of very fine carbon
particles generated by attrition. The absorbance was deter-
mined at 420 nm on the clarified sample. The color was
expressed in ICUMSA units (IU) defined according to
equation (Anon, 1994);
IU ¼ 1000 A=ðb cÞ;
where
A = absorbance at 420 nm of the test sample
b = length (cm) of the adsorbing path
c = concentration (g sugar/mL) of the test sample
The IU is therefore a measure of the weight ratio of a
hypothetical coloring substance to the sugar present.
All activated carbon samples were studied for their
sugar syrup decolorization properties at 1.0 g per 100 g
syrup, and the effect of level of carbon dosage was studied
for samples showing better decolorization capability. The
color removal at different carbon dosages were expressed
as adsorption isotherms. The amount of adsorbate held
per g of activated carbon was expressed as the difference
between initial and residual levels of color in IU divided
by the carbon dosage in g/100 g syrup. Similar approaches
were used by Agudo et al. (2002) and Çelebi and Kincal
(2007) in their isotherm expressions.
3. Results and discussion
The syrup decolorization performances of the activated
carbons are given in Fig. 1 along with their iodine and
 H.L. Mudoga et al. / Bioresource Technology 99 (2008) 3528–3533 3531

100

Syrup, Iodine or Molasses Decolorization, %

90 Syrup

80 Iodine

70
Molasses
60

50

40

30

20

10

0
5

2
20

00

.5
5

3
0C

1.
0P

0P

0P

0P

P1
L3

L2

0P
50

50

30

30
75

75

0
C

50

30
D

Fig. 1. Performances of commercial and prepared activated carbons in the decolorization of sugar syrup, molasses and iodine solutions.

molasses decolorization performances. The beet pulp car- sample 750C2, the BET surface area of which is a little less
bon 750C5 is almost as good as the commercially used than 400 m2 g1 exhibits almost no decolorization poten-
DCL320 and better than DCL200. Comparing the decolor- tial; while the samples 500P5 and 500P3, both of which
ization of syrup with those of the iodine solution and exhibiting around 45% decolorization have substantially
diluted molasses with all samples of activated carbons, different BET surface areas. It appears that the iodine
iodine solution decolorization performance seems to be a decolorization is the best indicator of the syrup decoloriza-
better indicator of syrup decolorization performance. tion performance, followed by molasses decolorization,
The BET surface areas of the activated carbons are and the BET surface area is a poorer indicator than these
given in Fig. 2. Comparison of the decolorization perfor- two properties.
mances of the carbons in Fig. 1 with their BET surface The pH values of 1% suspensions of the activated car-
areas in Fig. 2 shows that the three best decolorizing car- bons are given in Table 2. The suspensions of the three best
bons, which can remove more than 60% of the color, all decolorizing carbons, which can remove more than 60% of
have BET surface areas above 800 m2 g1. However, the the color (Fig. 1) have pH values in the range of 4.5 and

Fig. 2. BET surface areas of the commercial and prepared activated carbons.
3532
6.7; while the other suspensions are highly alkaline or
highly acidic. Moderate pH values seem to favor the decol-
orization performance.
The electrical conductivity values of 1% suspensions of
activated carbons were measured as an indicator of their
soluble ash contents, and are given in Table 2. The extre-
mely poor decolorization performance of 750C2 seems to
be best explained by the extremely high (3–4 orders of mag-
nitude higher) electrical conductivity of its suspension.
The comparatively lower BET surface areas, and the
acidic pH values and high electrical conductivities of the
suspensions of phosphoric acid activated prepared carbons,
which may be the reason of their poorer performance, may
be due to traces of the acid occluded in the pores in spite of
thorough washing right after preparation.
The ash content, average pore size, pore volume and
densities of the activated carbons are given in Table 2.
These properties do not seem to indicate any direction in
the syrup decolorization performance. For example, the
ash content does not seem to be a good indicator; although
the poorest performer has considerably high ash content
compared to the others, the beet pulp carbons activated
at 500 °C and 300 °C, having ash contents similar to that
of 750C5 are much poorer performers. Similarly, the best
performing carbons have higher pore volumes, but another
carbon with similar pore volume (500P5) has quite poorer
performance.
The ability of an activated carbon sample to adsorb
organic substances is essentially related to its textural and
surface properties. The hydrophobic and apolar nature of
the adsorbent is essential for a carbon to remove the
organic substances responsible for color. Indeed, the sam-
ples with best performance are those with nearly neutral
pH and low conductivity, both characteristics indicating
a more nonpolar surface. Although the number of samples
is too small to conclude it from this set of data alone, decol-
orizing ability is proportional to surface area, as should be
expected, for the materials with more apolar surfaces.
Beet pulp being abundantly available as a raw material,
the effect of sorbent loading (0.2–1.0 g carbon/100 g syrup)
was studied for the best performing one of the beet pulp
8000
(IUo-IUeq)/(g C/100 g syrup)
y = 3.365x
6000
R2 = 0.9979
4000
2000
0 Optimization of conditions for the preparation of activated carbons
0 500 1000 1500
Residual color, IU
Fig. 3. Sorption isotherms for the better decolorizing carbons.
H.L. Mudoga et al. / Bioresource Technology 99 (2008) 3528–3533
activated carbons, namely 750C5, and the commercial car-
bons DCL 320 and DCL 200. The results are shown in
Fig. 3 as adsorption isotherms.
The isotherms were found to be in the linear range as
indicated by the very high regression coefficients for
straight lines through the origin. The studied range of col-
oring substance loadings appears to be low enough for
Henry’s law to be valid. Studies at higher activated carbon
dosages would be necessary to obtain the whole isotherm.
4. Conclusion
The activated carbon obtained from sugar beet pulp by
direct carbonization for 5 h at 750 °C under a stream of
carbon dioxide has a decolorization performance that can
compete with commercially used activated carbons.
Among the studied physical characteristics of the acti-
vated carbons, iodine decolorization performance appear
to be the best indicator of sugar syrup decolorization per-
formance, followed by the molasses decolorization perfor-
mances, electrical conductivities of their suspensions and
their BET surface areas. Suspension pH values between
4.4 and 6.7 and electrical conductivities less than 300 lS
are indicated; while the syrup decolorization performance
does not seem to be related to the pore volume or size, den-
sity or ash contents.
Acknowledgements
The authors would like to thank Dr. Ahmet Özer of
Fırat University for kindly providing the beet pulp based
activated carbons.
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