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Advanced Materials Division, Korea Research Institute of Chemical Technology, Yusung, Deajeon 305-600, Korea

(Received February 25, 2005;accepted June 12, 2005)

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Abstract:In this work, the calcium alginate microcapsules containing lemon oil were prepared by emulsification-internal gelation, and their potential use as aromatherapy was examined by the controlled release system. The lemon oil encapsulated in the alginate was successfully observed by Fourier transform (FT-IR) spectroscopy and differential scanning calorimeter (DSC) measurements. Analysis of the diameters and shapes of microcapsules was conducted by scanning electron microscopy (SEM). The mean diameters ranging from 4 to 7 µm and encapsulation yield ranging from 50 to 85% were obtained. The controlled release of the lemon oil at 37 × was demonstrated by the infrared moisture determination (IMDB). It was found that the amount of released lemon oil decreased with increasing concentrations of alginate and CaCl2 due to the higher the cross-linking density of the capsules prepared. The oil release from the capsule was measured as a function of physical force. We confirmed that the external factor could control the collapse of capsule wall and the release rate.

Keywords: calcium alginate, microcapsule, emulsification-internal gelation, infrared moisture determination.

†To whom correspondence should be addressed. E-mail: psjin@krict.re.kr

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Figure 1. FTIR spectra of sodium alginate powder, blank alginate beads, alginate microcapsules, and lemon oil.

lemon oil alginate microcapsules

blank alginate beads sodium alginate powder

Transmission(%)

7333# 6833# 6333# 5833# 5333# 4833# 4333# 833# Wavenumber(cm^-1)

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Figure 2. DSC thermograms of blank alginate beads, alginate microcapsules, and lemon oil.

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Heat flow(w/g)

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Figure 3. SEM photographs of microcapsules surface morphology by different kinds of temperature; (a) 25 ×, (b) 35 ×, and (c) 50 ×.

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(b)

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Figure 4. SEM photographs of microcapsules prepared by different kinds of temperature; (a) 25 ×, (b) 35 ×, and (c) 50 ×.

Table 1. Encapsulation Yield and Mean Diameter of Alginate Microcapsules

Concentration (%, w/w)

Encapsulation yield (%, w/w)

Mean diameter (µm)

Alginate 0.5 49.5 4.69

1 60.0 6.03

2 75.8 6.48

CaCl2

1

3 85.2 6.54

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1 75.8 6.48

2 81.7 5.84

Alginate 2

3 82.4 4.32

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1 wt%

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3 wt%

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45 9 3

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Particle size(µm)

Figure 6. The effect of CaCl2 concentration on the size distributions of microcapsules.

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37 ×; (a) with various concentrations of alginate at constant CaCl² con- centration of 1 wt% and (b) with various concentrations of CaCl2 at constant alginate concentration of 2 wt%.

0 0 0 0 0

0.5 wt.%

1 wt.%

2 wt.%

3 wt.%

73 63 53 43 3

ψ(%)

# 3# 58# 83# :8# 433#

Time(min) (a)

0 0 0 0

0.5 wt.%

1 wt.%

2 wt.%

3 wt.%

63

53

43

3

ψ(%)

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Time(min) (b)

Table 2. Tensile Strength and Elongation of Alginate Films Concentration

(%, w/w)

Tensile strength (MPa)

Elongation (%)

Alginate 0.5 5.81 60.2

1 26.0 62.8 2 28.9 65.7 CaCl2

1

3 40.1 78.1

CaCl2 0.5 18.2 48.6

1 28.9 65.7 2 38.3 60.7 Alginate

2

3 54.0 40.3 Figure 8. Change of lemon oil release from alginate microcapsules with various crashing force; alginate concentration, 2 wt% and CaCl2 con- centration, 1 wt%.

0 5 0 5 0

5.6 G^{10-2 J/cm2} 4.4 G^{10-2 J/cm2} 3.3 G^{10-2 J/cm2} 433#

:8#

83#

58#

3#

ψ(%)

3# 58# 83# :8# 433#

Time(min)

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