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46

Lampiran

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) (100 mL/g) 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 0,00 0,01 0,02 0,03 0,04 0,05 6 8 10 12 14 16 ηsp /C (1 00 m L /g) C (g/100 mL)

Dari kurva tersebut diperoleh persamaan garis y = 158,1x + 7,382 [η] = 7,382

[η] = , dengan K = 1,46×10-4 dan 0,83 Jadi, 7,382 = 1,46×10-4 ,

48

Lampiran B Penentuan Derajat Deasetilasi Kitosan

a. Spektrum serapan inframerah kitosan deasetilasi 1×4 jam

A3450 = 0,4260 A1655 = 0,1717 % N-deasetilasi = 100 _, % = 100 ,_{, ,} % = 69,68 % 500 750 1000 1250 1500 1750 2000 2500 3000 3500 4000 4500 1/cm 52.5 60 67.5 75 82.5 90 97.5 %T 347 9. 58 3 441 .0 1 1658 .7 8 1 568 .1 3 142 3. 47 13 79. 1 0 1321 .2 4 1 155 .3 6 107 6. 28 1 026 .1 3 952 .8 4 7 50. 3 1 6 59. 6 6 6 13. 3 6 59 6. 00 Khitosan Sampel 1

b. Spektrum serapan inframerah kitosan deasetilasi 2×4 jam A3450 = 0,3999 A1655 = 0,0891 % N-deasetilasi = 100 _, % = 100 ,_{, ,} % = 83,23 % 500 750 1000 1250 1500 1750 2000 2500 3000 3500 4000 4500 1/cm 70 75 80 85 90 95 100 %T 344 2 .9 4 287 5 .8 6 1 658 .7 8 1 585 .4 9 138 1. 0 3 115 1. 50 10 8 2 .0 7 10 31. 9 2 65 9. 66 Khitosan

50

Lampiran C Spektrum Serapan Inframerah Kitin, Karboksimetil

kitin dan Karboksimetil kitosan

a. Spektrum serapan inframerah kitin

b. Spektrum serapan inframerah karboksimetil kitin metode heterogen

500 750 1000 1250 1500 1750 2000 2500 3000 3500 4000 4500 1/cm 60 65 70 75 80 85 90 95 100 %T 3 448 .7 2 326 9. 34 311 1. 18 296 2. 66 292 9. 87 28 87. 4 4 1658 .7 8 162 9. 85 15 68. 1 3 137 7. 17 1313 .5 2 1 157. 29 1116 .7 8 1 072. 42 10 14. 5 6 9 75. 9 8 950. 91 89 4. 97 75 0. 31 6 96. 3 0 586 .3 6 559 .3 6 528 .5 0 sampel 4 500 750 1000 1250 1500 1750 2000 2500 3000 3500 4000 4500 1/cm 30 40 50 60 70 80 90 100 %T 34 46 .7 9 31 09 .2 5 29 60 .7 3 29 29 .8 7 28 87 .4 4 17 26 .2 9 16 58 .7 8 16 27 .9 2 15 54 .6 3 14 15 .7 5 13 79 .1 0 13 13 .5 2 12 59 .5 2 12 03 .5 8 11 57 .2 9 11 16 .7 8 10 72 .4 2 10 24 .2 0 95 0. 91 89 4. 9 7 75 0. 3 1 69 8. 2 3 59 4. 08 57 8. 64 56 1. 29 52 8. 50 46 8. 7 0 sampel 2

c. Spektrum serapan inframerah karboksimetil kitosan 500 750 1000 1250 1500 1750 2000 2500 3000 3500 4000 4500 1/cm 55 60 65 70 75 80 85 90 95 100 %T 3446 .7 9 292 4. 09 2065 .7 6 1624 .0 6 1527 .6 2 1413 .8 2 13 81. 03 11 53. 43 10 89. 78 1 064. 71 101 4. 56 sampel 3

Lam

a. Kitos •

mpiran D K

Differ

san TGA

Kurva Ana

rential Sca

alisis Term

anning Ca

mogravim

alorimetry

metri (TGA

(DSC)

5

A) dan

52

b. Karb • boksimetil K TGA itosan 554

56

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 1E-3 0,01 0,1 1 -10 -5 0 5 10 15 20 25 Data Eksperimen Hasil Fitting 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

Δφ

(mV) C₂ (mol L-1)

Curve fitting terhadap persamaan Teorell-Meyer-Sievers memberikan nilai Q+X+ sebesar

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 1E-3 0,01 0,1 1 -5 0 5 10 15 20 25 30 35 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

Karboksimetil Kitosan (Hasil Fitting) Karboksimetil Kitosan (Data Eksperimen)

Δφ

(m

V

)

C₂ (mol L-1)

Curve fitting terhadap persamaan Teorell-Meyer-Sievers memberikan nilai Q+X+ sebesar

58

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

0 lnCf C − terhadap t sesuai dengan persamaan 0 ln f f C Ap t C V

− = . Dari kurva diperoleh persamaan garis:

6

y = 3,58206 10× − 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.

0 1000 2000 3000 4000 5000 6000 0,000 0,005 0,010 0,015 0,020 0,025 -l n( Cf /C 0 ) 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

0 lnCf C − terhadap t sesuai dengan persamaan 0 ln f f C Ap t C V

60 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 1000 2000 3000 4000 5000 -0,01 0,00 0,01 0,02 0,03 0,04 0,05 0,06 0,07 0,08 -ln(C f /C 0 ) t (s)

Lampiran G Kurva Konduktivitas

a. Kitosan • Kurva Bode 0 500000 1000000 1500000 2000000 0 60 120 180 Regresi Linier 1 Regresi Linier 2 Z' ( Ω ) f (Hz)

Frekuensi ambang dan tahanan saat frekuensi ambang diperoleh dari perpotongan antara persamaan regresi linier 1 dengan persamaan regresi linier 2.

• Kurva Nyquist 0 20 40 60 80 100 120 140 160 -20 0 20 40 60 80 100 120 140 160 -Z'' ( Ω )

62 b. Karboksimetil Kitosan • Kurva Bode 0 500000 1000000 1500000 2000000 0 100 200 300 400 500 Z' ( Ω ) f (Hz) • Kurva Nyquist 0 100 200 300 400 500 0 100 200 300 400 500 -Z'' ( Ω ) Z' (Ω)