Daftar Pustaka
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2.
Haile, S. M., (2003), Fuel cell materials and components, Acta Materialia, 51, 5981– 6000
3.
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4.
Wagner, N., Application of Impedance Spectroscopy: Fuel Cell, In Impedance Spectroscopy Theory, Experiment, and Applications, E. Barsoukov and J. R. Macdonald, (2005), 2nd edition, Wiley-Interscience, New Jersey, 497-529
5.
Harvey, D., (2000), Modern Analytical Chemistry, McGraw-Hill, New York, 394; 745
6.
Kurita, K., (2001), Controlled Functionalization of The Polysaccharide Chitin, Prog. Polym. Sci., 26, 1921-1971
7.
Morrison, R. T. and Boyd, R. N., (1977), 3rd edition, Prentice-Hall of India, New Delhi, 1070-1106; 1112-1128
8.
Shahidi, F. and Synowiecki, J., (1991), Isolation and Characterization of Nutrients and Value-Added Products from Snow Crab (Chinoecetes opilio) and Shrimp (Pandalus borealis) Processing Discards, J. Agric. Food Chem., 39(8), 1527-1532
9.
Miao, J., Chen, G., Gao, C., Lin, C., Wang, D. and Sun, M., (2006), Preparation and characterization
of
N,O-carboxymethyl
chitosan
(NOCC)/polysulfone
(PS)
composite nanofiltration membranes, J. Memb. Sci., 280, 478-484 10.
Kurita, K., (2006), Chitin and Chitosan: Functional Biopolymers from Marine Crustaceans, Marine Biotechnology, 8, 203-226
11.
Mulder, M., (1996), Basic Principles of Membrane Technology, 2nd edition, Kluwer Academic Publishers, Dordrecht, 12-18; 22-49; 267-271
12.
Haile, S. M., (2003), Fuel cell materials and components, Acta Materialia, 51, 59816000
44
13.
Wan, Y., Creber, K. A. M., Peppley, B. and Bui, V. T., (2003), Ionic conductivity of chitosan membranes, Polymer, 44, 1057–1065
14.
Ledyastuti, M., (2007), Tesis, Institut Teknologi Bandung, Bandung, 31-34
15.
Suendo, V., Minagawa, M. and Tanioka, A., (2002), Membrane potential of a bipolar membrane: the effect of concentration perturbation of the intermediate phase around a certain value, Journal of Electroanalytical Chemistry, 520, 29-39
16.
Macdonald, J. R. and Johnson, W. B., Fundamentals of Impedance Spectroscopy, In Impedance Spectroscopy Theory, Experiment, and Applications, E. Barsoukov and J. R. Macdonald, (2005), 2nd edition, Wiley-Interscience, New Jersey, 1-12
17.
Austin, P. R., Chitin Solution, U. S. Patent, No. 4059457, 1977
18.
Li, Z., Zhuang, X. P., Liu, X. F., Guan, T. L. and Yao, K. D., (2002), Study on antibacterial O-carboxymethylated chitosan/cellulose blend film from LiCl/N,Ndimethylacetamide solution, Polymer, 43, 1541-1547
19.
Khan, T. A., Peh, K. K. and Ch'ng, H. S., (2002), Reporting Degree of Deacetylation Values of Chitosan: The Influence of Analytical Methods, J. Pharm. Pharmaceut. Sci., 5(3), 205-212
20.
Daniels, F., Alberty, R. A., Williams, J. W., Cornwell, C. D., Bender, P. and Harriman, J. E., (1970), Experimental Physical Chemistry, 7th edition, McGraw-Hill, New York, 157-166; 329-335
21.
Sun, S. F., (2004), Physical Chemistry of Macromolecules, 2nd edition, John Wiley & Sons, Inc., New Jersey, 170-175
22.
Zhang, X., Benavente, J. and Garcia-Valls, R., (2005), Lignin-based membranes for electrolyte transference, Journal of Power Sources, 145, 292-297
23.
Chen, L., Tian, Z. and Du, Y., (2004), Synthesis and pH sensitivity of carboxymethyl chitosan-based polyampholyte hydrogels for protein carrier matrices, Biomaterials, 25, 3725–3732
24.
Billmeyer, F. W., (1994), Textbook of Polymer Science, 3rd edition, John Wiley & Sons, Inc., Singapore
25.
Smitha, B., Sridhar, S. and Khan, A. A., (2005), Chitosan–sodium alginate polyion complexes as fuel cell membranes, European Polymer Journal, 41, 1859–1866
45
Lampiran
46
Lampiran A Penentuan Massa Molekul Rata-Rata Kitosan Secara Viskometri ( t0 = 3,67 s Pelarut CH3COOH 1% (v/v) C (g/100 mL)
trata-rata (s)
0,0050
3,8
0,0364
7,2727
0,0122
4,1
0,1182
9,6870
0,0217
4,6
0,2545
11,7302
0,0512
6,5
0,7727
15,0923
(100 mL/g)
16
ηsp/C (100 mL/g)
14
12
10
8
6 0,00
0,01
0,02
0,03
0,04
0,05
C (g/100 mL)
Dari kurva tersebut diperoleh persamaan garis y = 158,1x + 7,382 [η] = 7,382 , dengan K = 1,46×10-4 dan
[η] =
Jadi, 7,382 = 1,46×10-4 4,65
0,83
,
10 g/mol
47
Lampiran B Penentuan Derajat Deasetilasi Kitosan a. Spektrum serapan inframerah kitosan deasetilasi 1×4 jam
97.5 %T
6 5 9 .6 6 6 1 3 .3 6 5 9 6 .0 0
9 5 2 .8 4 1 1 5 5 .3 6 1 0 7 6 .2 8 1 0 2 6 .1 3
1 6 5 8 .7 8
75
1 3 7 9 .1 0
1 5 6 8 .1 3
82.5
1 3 2 1 .2 4
1 4 2 3 .4 7
7 5 0 .3 1
90
3 4 7 9 .5 8 3 4 4 1 .0 1
67.5
60
52.5 4500 4000 3500 Khitosan Sampel 1
3000
2500
2000
1750
1500
1250
1000
750
500 1/cm
A3450 = 0,4260 A1655 = 0,1717 % N-deasetilasi = 100
,
% = 100
, ,
,
% = 69,68 %
48
b. Spektrum serapan inframerah kitosan deasetilasi 2×4 jam
100 %T
65 9.66
344 2.9 4
80
1 082 .07 10 31.92
115 1.50
85
1 585 .49
1 658 .78
90
138 1.0 3
287 5.8 6
95
75
70 4500 4000 Khitosan
3500
3000
2500
2000
1750
1500
1250
1000
750
500 1/cm
A3450 = 0,3999 A1655 = 0,0891 % N-deasetilasi = 100
,
% = 100
, ,
,
% = 83,23 %
49
Lampiran C Spektrum Serapan Inframerah Kitin, Karboksimetil kitin dan Karboksimetil kitosan a.
Spektrum serapan inframerah kitin
100 %T 95
3448.72
70
65
586.36 559.36 528.50
750.31 696.30
894.97 975.98 950.91
1157.29 1116.78
3269.34
75
1072.42 1014.56
3111.18
80
1658.78 1629.85
2962.66 2929.87 2887.44
1568.13
85
1313.52
1377.17
90
60 4500 4000 sampel 4
3000
2500
2000
1750
1500
1250
1000
750
500 1/cm
Spektrum serapan inframerah karboksimetil kitin metode heterogen
100 %T
468.70 594.08 578.64 561.29 528.50
1072.42 1024.20
50
750.31 698.23
894.97 1157.29 1116.78
1379.10
1658.78 1627.92
3109.25
60
1554.63
2960.73 2929.87 2887.44
70
950.91
1313.52
1415.75
1726.29
80
1259.52 1203.58
90
40 3446.79
b.
3500
30 4500 4000 sampel 2
3500
3000
2500
2000
1750
1500
1250
1000
750
500 1/cm
50
Spektrum serapan inframerah karboksimetil kitosan
100 %T 95
85
1624.06
1527.62
80
1153.43 1089.78 1064.71 1014.56
1413.82 1381.03
2065.76
90
2924.09
75
70
65
3446.79
c.
60
55 4500 4000 sampel 3
3500
3000
2500
2000
1750
1500
1250
1000
750
500 1/cm
51
Lam mpiran D Kurva K Anaalisis Term mogravim metri (TGA A) dan Differrential Scaanning Caalorimetry (DSC) a. Kitossan •
TGA
5 52
•
DSC
553
b. Karb boksimetil Kitosan •
TGA
54
•
DSC
55
Lampiran E Analisis Potensial Membran a. Kitosan C1 (mol L-1)
C2 (mol L-1)
∆φ (mV)
0,001
0,001
0
0,001
0,01
20,1
0,001
0,1
9,4
0,001
1
-6,5
Data Eksperimen Hasil Fitting
25
20
Δφ (mV)
15
10
5
Data: DataChi_B Model: TMS Cation Exchange Chi^2 = 0.11999 Temp 298 ±0 C0 0.001 ±0 QX 0.00405 ±0.00009 W -0.26669 ±0.00492
0
-5
-10 1E-3
0,01
0,1
1
-1
C2 (mol L )
Curve fitting terhadap persamaan Teorell-Meyer-Sievers memberikan nilai Q+X+ sebesar 0,00405 mol L-1 dan W sebesar -0,26669.
56
b. Karboksimetil Kitosan C1 (mol L-1)
C2 (mol L-1)
∆φ (mV)
0,001
0,001
0
0,001
0,1
19,2
0,001
1
2,2
0,001
2
-3,5
35
Karboksimetil Kitosan (Hasil Fitting) Karboksimetil Kitosan (Data Eksperimen)
30 25
Δφ (mV)
20 15 Data: DataCMChi_B Model: TMS Cation Exchange Chi^2 = 0.0305 Temp 298 ±0 C0 0.001 ±0 QX 0.00658 ±0.0001 W -0.30328 ±0.0032
10 5 0 -5 1E-3
0,01
0,1
1
-1
C2 (mol L )
Curve fitting terhadap persamaan Teorell-Meyer-Sievers memberikan nilai Q+X+ sebesar 0,00658 mol L-1 dan W sebesar -0,30328.
57
Lampiran F Analisis Permeabilitas Metanol a. Kitosan Waktu (s)
Luas Puncak Metanol (a.u.)
0
0
600
0,00403
1200
0,00668
1800
0,00997
2400
0,01207
3000
0,01485
3600
0,01606
4200
0,0206
4800
0,02206
5400
0,01933
6000
0,02077
Koefisien permeabilitas diperoleh dengan mengalurkan kurva − ln
dengan persamaan − ln
Cf C0
=
Cf C0
terhadap t sesuai
Ap t . Dari kurva diperoleh persamaan garis: Vf
y = 3,58206 × 10−6 x + 0, 00256 Dengan diameter membran 4,3 cm dan Vf = 100 cm3 diperoleh p = 2,467 × 10-5 cm s-1. Permeabilitas terhadap metanol diperoleh melalui persamaan P = pl , dengan l = 0,21 mm. Jadi, P = 5,1807 × 10-7 cm2 s-1.
58
0,025
0,020
-ln(Cf/C0)
0,015
0,010
0,005
0,000
0
1000
2000
3000
4000
5000
6000
t (s)
b. Karboksimetil Kitosan Waktu (s)
Luas Puncak Metanol (a.u.)
0
0
0,01029
600
0,02434
1200
0,03657
1800
0,0426
2400
0,04364
3000
0,05685
3600
0,0772
4200
0,06043
4800
Koefisien permeabilitas diperoleh dengan mengalurkan kurva − ln
dengan persamaan − ln
Cf C0
=
Cf C0
terhadap t sesuai
Ap t . Dari kurva diperoleh persamaan garis: Vf
y = 1,42927 ×10−5 x + 0, 00479 59
Dengan diameter membran 4,3 cm dan Vf = 100 cm3 diperoleh p = 9,842 × 10-5 cm s-1. Permeabilitas terhadap metanol diperoleh melalui persamaan P = pl , dengan l = 0,24 mm. Jadi, P = 2,3621 × 10-6 cm2 s-1.
0,08 0,07 0,06
-ln(Cf/C0)
0,05 0,04 0,03 0,02 0,01 0,00 -0,01 0
1000
2000
3000
4000
5000
t (s)
60
Lampiran G Kurva Konduktivitas a. Kitosan •
Kurva Bode
180
Z' (Ω)
120
Regresi Linier 1 Regresi Linier 2
60
0
0
500000
1000000
1500000
2000000
f (Hz)
Frekuensi ambang dan tahanan saat frekuensi ambang diperoleh dari perpotongan antara persamaan regresi linier 1 dengan persamaan regresi linier 2. •
Kurva Nyquist
160 140 120
-Z'' (Ω)
100 80 60 40 20 0 -20 0
20
40
60
80
100
120
140
160
Z' (Ω)
61
b. Karboksimetil Kitosan •
Kurva Bode
500
400
200
100
0 0
500000
1000000
1500000
2000000
f (Hz)
•
Kurva Nyquist
500
400
300
-Z'' (Ω)
Z' (Ω)
300
200
100
0
0
100
200
300
400
500
Z' (Ω)
62
