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Filtration of Pectin Extract from Grapefruit Peel and

Viscosity of Pectin Solutions

Nurhan Arslan & Hasan To&u1

Faculty of Engineering, Department of Chemical Engineering, Fu-at University,

23279 Elazlg, Turkey

(Received 4 September 1994; revised version received 3 January 1995;

accepted 31 January 1995)

ABSTRACT

The yield of pectin extracted (85C, pH=2*5, 90 min) by acidi.ed water

in a ratio of 25 parts per part of dry peel from dried grapefruit peel was

21.1% (DM basis).

The pectin extract was vacuum filtered at different temperatures and

under various pressure differences, and the average speciJ ic cake

resistances were determined. The specific cake resistance was highly

dependent on the filtration pressure. The cake compressibility

coeficients at lSC, 25C and 35C were calculated as O-387, 0.379

and 0.379, respectively. The jiltration rate observed at 15C was higher

than that at 25C due to flocculation at low temperature.

The efjects of temperature and concentration on the viscosity of

pectin solutions were examined at six different temperatures between

10C and 60C and four concentration levels between O-3 g/100 ml and

1.4gllOO ml. The activation energy for viscous flow was in the range

2.10-3.77 kcal mol-. Finally, the combined effect of temperature and

concentration on the viscosity was expressed as

r/=852x lop5 exp(-1~6162Cf1~807exp(0~5493C)I RT)

NOTATION

::

C

E,

&

Filter area (m)

Constant of eqn (10) ((g/100 ml)-)

Concentration (g/100 ml)

Activation energy of flow (kcal mol- )

Dimensional constant= 1 kg Pa- s- m-

191

192 N A&an, H. To&d

K

KCI

K,,K,

m

-AP

R

R,

s

t

T

V

VI

Constant of eqn (10) (Pa s)

Constant of eqn (7) (Pa s)

Constants of eqn (1) (Pa s m- and Pa s m-)

Ratio of wet cake to dry cake

Total pressure drop (Pa)

Gas constant (kcal mol- K-l)

Resistance of the filter medium (m-l)

Mass fraction of solid in slurry

Time (s)

Temperature (K or C)

Filtrate volume (m)

Fictitious filtrate volume (m)

Specific cake resistance (m kg-)

Specific cake resistance at unit pressure difference (m kg- Pa-)

Viscosity (Pa s)

Cake compressibility coefficient

Filtrate density (kg m-)

INTRODUCTION

Pectins are common components in the cell wall of fruits and have

important nutritional and technological properties, mainly because of their

ability to form gels. Characteristic structural features for this group of

heteropolysaccharides are 1,4 linked main chain a-D-galactopyranosyluronic

acid residues interspersed with a-L-rhamnopyranosyl residues. Some of the

rhamnose residues are branched with side chains comprising different

amounts of neutral sugar residues, primarily arabinose and galactose

(Westerlund et al., 1991). The carboxyl groups can be partially methylated,

and the C-2 and C-3 hydroxyl groups of the sugar ring can be acetylated

(Valverde et al., 1982).

The major use for pectins is as a gelling agent in jams and preserves.

Pectin is obtained mainly from the waste materials from the production of

apple, orange, grapefruit and lemon juices (Kratchanova et al., 1991). The

pectin content of citrus peel is usually high, 2530% of the dried peel mass

(Huong & Luyen, 1989).

Filtration is one of the major unit operations employed in the food

industry. The gelatinous precipitate of pectin precipitated with ethanol from

an acid extract can be filtered by vacuum filtration at constant pressure

differences. Although there are various methods of filtration (i.e. high

pressure systems, vacuum filtration, ultrafiltration), operational variables

which control filtration rates are the same in general, and the same filtration

theories apply to each of these processes. The effect of the operational

variables on filtration rates can be described easily by mathematical

equations. Pressure is one of the important operating variables (Baymduh et

al., 1989).

The viscosity of pectin is affected by molecular size, degree of

methylation, pH, presence of counter-ions and sucrose (Phatak et al., 1988).

Filtration of pectin extract from grapeffuit peel 193

Viscosity behaviour of pectin solutions changes with concentration and

temperature.

The objectives of this research were to study the filtration of a gelatinous

precipitate of pectin from grapefruit peel at different temperatures and

under various pressure differences and the variation in viscosity of pectin

solution with temperature and concentration.

EXPERIMENTAL

Extraction of pectin from grapefruit peel

Fresh Turkish grapefruit from the Mersin region (citrus paradisi McFad.)

was purchased from a local retail market and peeled. Sun dried grapefruit

peel was ground to 50 mesh in a hammer mill to facilitate washing and

extraction. Before grapefruit peel was utilized for pectin production, the

peel oil was removed by petroleum ether and dried. The peel was heated to

97C in a water bath for about 10 min to inactivate pectin enzymes, washed

extensively with water to remove sugars and flavenoids, filtered through a

suction filter, dried at 50C and sieved. A 50 mesh fraction was used in

experiments; 10 g of dried grapefruit peel were mixed with 250 ml of

0.003 N hydrochloric acid (pH=2*5), preheated to 85C in a water bath. The

mixture was mechanically stirred for 90 min, while maintaining the

temperature at 85C. The liquid phase was then separated from the fruit

mass by filtering. The liquid phase, a turbid pectin extract, was allowed to

cool and settle for several hours. When it reached a temperature of about

37C the pH was raised to about 7.5 by adding 0.1 M sodium phosphate

buffer and 50 mg of protease enzyme (Sigma Chemical Co., P 5147) was

added. The extract was incubated overnight at 37C. The acid extract was

separated by filtering and the pectin was precipitated with an equal volume

of ethanol. The gelatinous precipitate was filtered and the pectin coagulate

was washed once with a hydrochloric acid/ethanol mixture (70% ethanol),

then with 70% ethanol until the reaction was neutral and finally with 96%

ethanol to speed up drying at 50C. The yield of raw pectin was determined

gravimetrically.

Filtration of gelatinous precipitate of pectin

The gelatinous precipitate of pectin was filtered by suction at different

temperatures and under various constant pressure differences. The filtration

equipment consisted of a 1.8 litre jacketed stainless steel filter, vacuum

section and filtrate tank. A schematic diagram of the laboratory set-up is

shown in Fig. 1. The filtration area was 52.8 cm2 and the fabric filter

medium employed in the experiments was a tightly woven (10 weft/cm and

30 warp/cm) synthetic cloth manufactured locally and used in the beet sugar

production industry. A perforated plate, 32.1% of its area consisting of

4 mm diameter holes, was covered with the fabric filter medium and placed

on the base of the stainless steel filter. Experiments were conducted at least

in duplicate, at different temperatures (15C 25C and 35C), under various

pressure differences (0.24 x lo5 Pa, O-43 x lo5 Pa and 0.79 x lo5 Pa). Water

194 h! A&an, H. To&d

14

Fig. 1.

3,

Schematic diagram of laboratory set-up (1, circulating water bath; 2, mixer;

thermometer; 4, feed tank; 5, valve; 6, jacketed stainless steel filter; 7, funnel; 8,

vacuum section; 9, vacuum pump; 10, vacuum manometer; 11, pressure control valve

(by-pass); 12, filtrate tank; 13, graduated glass level indicator; 14, filtrate outlet

valve).

from a constant temperature bath at the filtration temperature was

circulated through the jacket of the stainless steel filter to maintain the

constant temperature during filtration. Pectin extract was heated to the

filtration temperature and filtered under vacuum. During constant-pressure

filtration, the variation in filtrate volume with time was recorded after the

first 100 ml of filtrate was discarded.

Viscosity determination of pectin solution

Samples of 0.3, 0.6, 1.1 and 1.4 g of dried pectin were dissolved in 100 ml of

0.9% NaCl solution. The viscosities of pectin solutions at different

concentrations were determined at 10C intervals from 10C to 60C by

means of an Ubbelohde viscosimeter No. 13 (capillary no: Ic, ID: 0.84 mm).

Densities of solutions were measured using a pycnometer. All of the

experiments were replicated.

RESULTS AND DISCUSSION

Yield of pectin

The yield of pectin extracted using the extraction process described above

was 21.1% (DM basis). The yield, degree of esterification and gel strength

Filtration of pectin extract from grapefruit peel

195

of the pectin obtained depend on the type of raw material used (variety,

processing conditions) and the extraction method (Kratchanova et al., 1991).

Anhydrogalacturonic acid content, degree of esterification, ash content and

optical rotation of pectin from the grapefruit peel studied were 74-O%,

68*2%, 56% and +216, respectively.

Filtration of pectin extract

The filtration rate equation for constant-pressure filtration is written

(Bennett & Myers, 1988) as

dVdt=( -AP)l(K,V+K,)

(I)

Equation (1) can be integrated analytically, since - AP, K1 and K2 are

constant. The result is

where

and

t/V=K, V/2( - AP) +&/( - AP)

K1 =spqal( 1 -ms)A 2g,

(2)

(3)

&=Rmy~IAgc

(4)

in which dV/dt is the rate of change of the filtrate volume with respect to

time (the filtration rate), V is the filtrate volume, t is the time, -AP is the

pressure difference across the filter, s is the mass fraction of solid in the

slurry, p is the filtrate density, y is the filtrate viscosity, x is the specific cake

resistance, m is the ratio of wet cake to dry cake, A is the filtration area, R,

is the filter medium resistance, and g, is the dimensional constant; R, may

be expressed in terms of the resistance of a hypothetical layer of cake which

corresponds to the collection of a hypothetical volume of filtrate l/m:

R,=spaV,,,l(l -ms)A

(5)

It should be noted that the intercept of eqn (2) is difficult to determine

accurately because of the large potential experimental error in observing the

time of the start of filtration and the time-volume relationship during the

first moments when the filtration rate is high. The value of R, calculated

from the intercept may vary appreciably from test to test, and will always be

different from the value measured with clean medium in a permeability test

(Perry & Green, 1984).

The experimental t/V for various pressure differences were plotted versus

V to obtain the values of the constants K, and K2 in eqn (2) (Figs 2-4).

The increased filtration rate (V/t) at 15C compared with the filtration

rate at 25C was due to flocculation at low temperature. The filtration rate

at 35C was higher than the filtration rate at 25C.

The constants from eqns (l)-(5) were calculated from the experimental

data and are shown in Table 1.

The densities and the viscosities of filtrates at 15C, 25C and 35C were

1.267 x lo3 kg mp3, 1.251 x lo3 kg mp3, 1.242 x lo3 kg rnh3 and 4.18 mPa s,

2.85 mPa s, 2.60 mPa s, respectively. All the experiments were done in

196 h! Arslan, H. To@ul

8-

0 100 200 300 4

v w

0

Fig. 2. Plot of t/V versus I/ for pectin extracts filtered at 0.24 x lo5 Pa pressure

difference at different temperatures: temperature (C): (0) 15; (m) 25; (*) 35.

or

0

I I I

100

V2gl,

300 4 0

Fig. 3. Plot of t/V versus V for pectin extracts filtered at 0.43 x 10 Pa pressure

difference at different temperatures: temperature (C): (0) 15; (w) 25; (+) 35.

duplicate. The maximum variation in the experiments was about _+6% in

the filtrate volumes.

Under experimental conditions, the variation in fictitious filtrate volume

resulted from the properties of the filter cake and the turbulence caused by

rapid rate of flow (Foust et al., 1960).

Filtration of pectin extract from grapefruit peel 197

0 100 200 3cn3

v w

Fig. 4. Plot of t/V versus V for pectin extracts filtered at 0.79 x lo5 Pa pressure

difference at different temperatures: temperature (C): (0) 15; (m) 25; (+) 35.

TABLE 1

Calculated Values of K, and K2, c1 and V,,, Obtained from an Analysis of the

Experimental Filtration Data

- AP (Pa) Experimental data

Temperatures (C)

0.24 x 10 K, x 10W5 (Pa s rn- )

K2 x lo- (Pa s rn-)

!z x lo- (m kg-)

V, (ml)

S x 10

m

r2

0.43 x 10

0.79 x lo5

K1 x lo- (Pa s mph)

Kz x lo- (Pa s m-)

cx x lo- (m kg-)

V, (ml)

S x lo2

m

r2

K1 x 1O-5 (Pa s rn~-)

K, x I O- (Pa s rn-)

n x lo- (m kg-)

V, (ml)

s x lo2

m

r2

15 2.5 35

1.004

0.279

258

27.8

2.0

1.10

0.994 1

1.153

0.3 12

3.28

27.1

1.X

1.51

0.9987

1.541

0.263

4.03

17.1

Go

0.9986

1.254 0.62)

0.209 WOO6

2.67 2.65

16.7 1.0

2.9 2.0

7.25 1.13

0.9979 0.9954

1.326 0.705

0.297 0.089

3.34 3.32

22.4 12.6

2.5 1.7

7.79 4.28

0.9985 0.9975

1.697 1.157

0.264 0.125

4.13 4.10

15.6 10.8

2.0 1.7

18.89 17.78

0.9988 0.9989

198 h! Arslan, H. To&d

It can be seen from Table 1 that specific cake resistance is a strong

function of applied pressure difference, indicating the highly compressible

character of the filter cake. The data could be correlated as

cl=/?( -AP)

(6)

in which p is the specific cake resistance at unit pressure difference (m kg-

Pa-) and v is the cake compressibility coefficient.

The logarithm of specific cake resistances at a given temperature was

plotted versus the logarithm of pressure difference (Fig. 5). The values of

the constants in eqn (6) for each temperature are given in Table 2.

Viscosity of pectin solution

The viscosity of pectin solutions at different concentrations and

temperatures are given in Table 3.

It can be seen that, as would be expected, the higher the temperature the

lower the viscosity, and the viscosity increases with concentration.

Diluted organic solutions (true solutions) are generally Newtonian in

character (Kirk & Othmer, 1970). It has been reported (Chou & Kokini,

1987) that hot break tomato paste pectin solutions at concentrations of 2%

26. 2 1 I I I

10. 0 10. 4 10. 8 11. 2

I n( - AP)

Fig. 5. Plot of In a versus In (- AP) for different temperatures: temperature (C):

(0) 35; (w) 25; (*) 15.

TABLE 2

Values of the Constants /3 and v at Different Temperatures

Temperature (C) j (mkg- Pa _ ) V r2

1.5 5-20 x lo9 0.387 0.9970

25 5.82 x lo9 0.379 0.9988

35 5.77 x lo9 o-379 O-9987

Filtration of pectin extract from grapefruit peel 199

TABLE 3

Relationship between Viscosity and Concentration of Pectin Solutions at Different

Temperatures

Cone. (g/100 ml)

10C 20C

1 (mpa s)

30C 40C 50C 60C

0.3 2.03 1.84 1.66 150 1.29 1.17

0.6 3.03 2.74 2.43 2.07 1.77 1.60

1.1 654 4.99 3.77 3.38 2.80 2.69

1.4 7.75 5.57 4.70 3.81 3.22 2.80

TABLE 4

Values of Arrhenius-type Constants E, and K0 for Pectin Solutions at Different

Concentrations

Cont.

CgllOO ml)

E,

{kcal mol-)

K0

Pa s)

r2

0.3 2.10 4.98 x lo- 5 0.9902

0.6 2.52 3.57 x lop5 0.9880

1.1 3.46 1.34 x lop5 0.9624

1.4 3.77 0.91 x lop5 0.9888

or lower and citrus pectin solutions at concentrations of 3% or lower were

Newtonian. Therefore, it has been assumed that the pectin solutions studied

were Newtonian.

The effect of temperature on the viscosity

The viscosity of liquids usually decreases with an increase in temperature.

The influence of temperature on viscosity can be described by an Arrhenius-

type equation (Ibarz et al., 1992):

q=K, exp(E,/RT)

(7)

where q is the viscosity, K0 is a constant, E, is the activation energy of flow,

R is the gas constant, and T is the absolute temperature in K.

The logarithm of the experimental viscosity at a given concentration was

plotted versus l/T to obtain the values of the constants E, and K0 in eqn (7).

These are given in Table 4.

The activation energies of flow increased with concentration while K0

decreased. Their relationship with concentration were fitted to the following

equations including the concentration

E,=1+307 exp(Oe5493C)

(8)

Z&,=8.52 x 1O-5 exp( - 1.6162C)

(9)

200 N A&an, H. To&d

TABLE 5

Effect of Concentration on Viscosity at Different Temperatures. Values of the

Constants K and Al for Pectin Solutions at Different Temperatures

T (C)

K (Pa s)

AI ((g/100 ml) -)

r2

10 1.42 x 1O-3 1.273 0.9801

20 1.41 x 1o-3 1.042 0.9696

30 1.32 x 1O-3 0.934 0.9894

Zk? 1.04 1.20 x x lo- lo- 0.843 0.869 0.9789 0.9847

60 0.95 x lop3 0.834 0.9538

where the concentration, the activation energy of flow and constant & were

expressed in g/100 ml, kcal mol- and Pa s, respectively. The correlation

coefficients of eqns (8) and (9) were O-991 and 0.990, respectively. The

constants of eqns (8) and (9) are applicable only in the range of

temperatures and concentrations studied.

The effect of concentration on the viscosity

The viscosity of most fluids increases with concentration. Change of viscosity

with concentration can be described by an exponential type equation (Rao et

al., 1984):

q=Kexp(AIC)

(10)

where K and A1 are constants, and C is the concentration.

To evaluate these constants, the experimental viscosity-concentration

data were fitted to the linearized form of eqn (10) by the least-squares

method. The estimates of the parameters of the exponential equation at

different temperatures are summarized in Table 5. From the results, it can

be observed that constants K and A1 decrease with temperature.

The combined effect of temperature and concentration on the viscosity

It is useful to get a simple equation describing the combined effect of

temperature and concentration on the viscosity of pectin solutions. This was

obtained by combining eqns (7), (8) and (9):

~=8*52 x lo- exp( - 1*6162C+ l-807 exp(05493C)IRT)

(11)

where C is the concentration in g/100 ml, T is the temperature in K, v is the

viscosity of pectin solution in Pa s, and R is the gas constant in kcal mol-

K-l.

REFERENCES

Baymdrrh, L., Gzilgen, M. & Ungan, S. (1989). Modeling of apple juice filtrations.

J. Food Sci., 54 (4) 1003-6.

Bennett, C. 0. & Myers, J. E. (1988). Momentum, Heat, and Mass Transfer, 3rd edn.

McGraw-Hill Fong and Sons Printers Pte Ltd, Singapore.

Filtration of pectin extract from grapefruit peel 201

Chou, T. D. & Kokini, J. L. (1987). Rheological properties and conformation of

tomato paste pectins, citrus and apple pectins. J. Food Sci., 52 (6), 1658-64.

Foust, A. S., Wenzel, L. A., Clump, C. W., Maus, L. & Andersen, L. B. (1960).

Principles of Unit Operations. John Wiley, New York, London.

Huong, D. M. & Luyen, D. V. (1989). Optimization of pectin extraction from dried

peel of citrus grandis. Polym. Bull., 22, 599-602.

Ibarz, A., Pagan, J. & Miguelsanz, R. (1992). Rheology of clarified fruit juices. II:

blackcurrant juices. J . Food Engng, 15, 63-73.

Kirk, D. E. & Othmer, D. F. (1970). Encyclopedia of Chemical Technology, Vol. 21,

3rd edn. John Wiley, New York.

Kratchanova, M., Benemou, C. & Kratchanov, C. (1991). On the pectic substances

of mango fruits. Carbohydr: Polym., l&271-82.

Perry, R. H. & Green, D. (1984). Penys Chemical Engineers Handbook, 3rd edn.

McGraw-Hill Kosaido Printing Co., Ltd, Japan.

Phatak, L., Chang, C. K. & Brown, G. (1988). Isolation and characterization of

pectin in sugar-beet pulp. J . Food Sci., 53 (3), 830-3.

Rao, M. A., Cooley, M. J. & Vitali, A. A. (1984). Flow properties of concentrated

juices at low temperatures. Food Technol., 38 (3), 113-19.

Valverde, C. V., Blanco, I. & Hidalgo, E. R. (1982). Substances in fresh, dried,

desiccated, and oleaginous Spanish fruits. J . Agric. Food Chem., 30, 832-5.

Westerlund, E., Aman, P., Andersson, R. & Andersson, R. E. (1991). Chemical

characterization of water-soluble pectin in papaya fruit. CarbohydK Polym., 15,

67-78.

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