50
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Daftar Pustaka
Acosta, J.L., Gonzales, L., Ojeda, M.C., Rio, C., (2003). Proton Conducting Materials Based on Thermoplastic Elastomer Silica Composites, J. Applied. Polymer Sci., 90, 2715-2720.
Atkins, P.W., (1999) Kimia Fisika, Irma Kartohadiprodjo (Penterjemah), jilid 2 edisi keempat, Penerbit Erlangga, Jakarta, 303.
Billmeyer, F. W. Jr., (1962). Textbook of Polymer Science, 1st edition. John Wiley & Sons Inc., New York, 12-14, 394-400
Billmeyer, F. W. Jr., (1971). Textbook of Polymer Science, 2nd edition. John Wiley & Sons Inc., New York, 3-6, 404-409
Chang, Raymond., (1998). Chemistry sixth edition. McGraw Hill., New York, 972.
Chen, Sheng-Li., Krishnan, L., Srinivasan, S., Benziger, J., Bocarsly, A.B., (2004). Ion Exchange Resin/polystyrene Sulfonate Composite Membranes for PEM Fuel Cell, J. Membrane Science., 243, 327-333.
Cowd, M., (1982), Kimia Polimer, Harry Firman (Penterjemah) (1991), Penerbit ITB, Bandung, 1, 55-58.
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Polymeric Electrolyte, J. Power Sources., 112, 395-400.
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Martins, C.R., Ruggeri, G., Paoli, M.A., (2003). Synthesis in Pilot Plant Scale and Physical Properties of Sulfonated Polystyrene, J. Braz. Chem. Soc., 14(5), 797-802.
Morais, S.A.L., Nascimento, E.A., Quetroz, C.R., (1999). Studies on Polyphenols and Lignin of Astronium urundeuwa Wood, J. Braz. Chem. Soc., 10, 447-452.
Qiang, F.R., Woo, J.J., Seo, S.J., Lee, J.S., Moon, S.H., (2008). Sulfonated Polystyrene/polyvinyl Chloride Composite Membranes for PEMFC Applications, J. Membrane Science.,309, 156-164.
51 Rahmawati, Fitriana., (2007), Skripsi, Institut Teknologi Bandung. Bandung, 5-16.
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Silverstein, R.M., (1998). Spectrometric Identification of Organic Compounds. John Willey & Sons Inc., New York. 71.
Smitha, B., Sridhar, S., Khan, A.A., (2003). Synthesis and Characterization of Proton Conducting Polymer Membranes for Fuel Cells, J. of Membrane Sci.,225, 63-76. Stevens, M., (2001), Kimia Polimer, Iis Sopyan (Penterjemah) (2001), Pradyna Pramita,
Jakarta. 1-9,35,209-210.
Won, Jongok., Choi, S.W., Kang, Y.S., Ha, H.Y., Oh, I.H., Kim, H.S., Kim, K.T., Jo, W.H., (2003). Structural Characterization and Surface Modification of Sulfonated Polystyrene-(ethylene-butylene)-styrene Triblock Proton Exchange Membrane, J. Membrane Science.,214, 245-257.
Zhang, Xiao., Benavente, J., Valls, R.G., (2005). Lignin-based Membranes for Electrolyte Transference, J. Power Source., 145, 292-297.
Zhang, Xiao Benavente, J., Valls, R.G., (2006). Porous Lignosulfonate Membranes for Direct Methanol Fuel Cells, J. Membrane Science., 276, 301-307.
52
7.
Lampiran
Lampiran A Perhitungan Derajat Polimerisasi (DPn)
Derajat Polimerisasi Polistiren
# mol benzoil peroksida = 0.1316 gram / 242 gram.mol-1 = 5.4328 x 10-4 mol
# massa stiren = 30 mL x 0.91 gram.mL-1 = 27.30 gram
mol stiren = 27.30 gram / 104 gram.mol-1 = 0.2625 mol
# mol stiren : mol benzoil peroksida 0.2625 mol : 5.4328 x 10-4 mol 483 : 1
Massa Molekul Polistiren
Massa Molekul Polistiren = DPn x Mr unit ulang polistiren
= 483 x 104
53
Lampiran B Perhitungan % Rendemen
# % Rendemen Polistien (PS) :
# Massa polistiren = mol BPO x DPn x Mr polistiren (teoritis) = 5.4328 x 10-4 x 483 x 104 gram.mol-1
= 27.29 gram
# % rendemen = (massa hasil sintesis / massa teoritis) x 100% = (26.3542 gram / 27.29 gram) x 100 % = 96.57 %
% Rendemen Polistien Tersulfonasi (PSS) :
# Mol PS = mol PSS = 2 gram / 104 gram.mol-1 = 0.01923 mol
# Massa dari gugus pada PS tergantikan oleh –SO3H (teoritis) :
= mol PSS x Mr PSS x % derajat sulfonasi = 0.01923 mol x 184 gram.mol-1x (8.48%/100%) = 0.3 gram
# Massa PS yang tidak mengalami sulfonasi :
= (100%-8.48%) x 0.01923 mol x 104 gram.mol-1 100%
= 1.8303 gram # Massa PSS yang seharusnya diperoleh :
= massa PS (yang tersulfonasi + tidak tersulfonasi) = 0.3 + 1.8303
= 2.13 gram
# % rendemen = (massa hasil sintesis / massa teoritis) x 100% = (2.0177 gram / 2.13 gram) x 100 %
54
Lampiran C Perhitungan Derajat Sulfonasi
Massa H2C2O4 yang digunakan adalah 0.0495 gram. Setelah itu H2C2O4 tersebut dilarutkan dengan aqua dm hingga volume 50 mL.
H2C2O4 .2H2O + 2 NaOH → Na2C2O4 + 4 H2O
# M H2C2O4 (dalam 50 mL) = (0.0495 gram / 126 gram 1
mol-1) 50 x 10-3 L
= 7.857 x 10-3 mol.L-1
Sebanyak 10 mL larutan H2C2O4 dititrasi dengan NaOH. Volume rata-rata NaOH yang dibutuhkan adalah 1.7 mL, sehingga konsentrasi NaOH dapat ditentukan dengan cara :
MNaOH . VNaOH = 2 MH2C2O4 .. VH2C2O4 M NaOH = (2 x 7.857 x 10-3 x 10) / 1.7
= 0.0924 M
Setelah volume NaOH yang diperlukan untuk melakukan titrasi pada sampel polistiren tersulfonasi diperoleh, maka derajat sulfonasi dapat ditentukan dengan perhitungan sbb: # mol NaOH = [NaOH] x volome titran rata-rata
= 0.0924 M x 0.75 x 10-3 L = 6.93 x 10-5 mol
# mol PSS = mol NaOH = 6.93 x 10-5 mol Massa PSS = mol PSS x Mr PSS
= 6.93 x 10-5 mol x 184 gram.mol-1 = 0.01275 gram
Massa PSS sampel yang ditimbang adalah 0.1504 gram, sedangkan massa PSS yang diperoleh dengan menggunakan perhitungan adalah 0.01275. Sehingga derajat sulfonasi dapat dihitung dengan cara :
# Derajat sulfonasi = (massa PSS / massa sampel) x 100% = (0.01275 / 0.1504) x 100%
55
Lampiran D Spektrum FTIR Polistiren 500 750 1000 1250 1500 1750 2000 2500 3000 3500 4000 4500 1/cm 30 40 50 60 70 80 90 100 %T 3 0 8 0 .3 2 3 0 5 9 .1 0 3 0 2 6 .3 1 2 9 2 2 .1 6 2 8 4 8 .8 6 1 6 0 0 .9 2 1 4 9 0 .9 7 1 4 4 8 .5 4 1 3 7 1 .3 9 1 0 6 8 .5 6 1 0 2 6 .1 3 9 0 6 .5 4 7 5 4 .1 7 6 9 8 .2 3 5 3 8 .1 4 4 5 1 .3 4 Polistiren Polistiren Tersulfonasi (PSS) 500 750 1000 1250 1500 1750 2000 2500 3000 3500 4000 4500 1/cm 20 30 40 50 60 70 80 90 100 %T 3 4 1 2 .0 8 2 9 2 4 .0 9 1 6 3 1 .7 8 1 4 4 8 .5 4 1 3 2 1 .2 4 1 2 8 4 .5 9 1 2 2 6 .7 3 1 1 7 8 .5 1 1 0 6 8 .5 6 1 0 0 8 .7 7 8 8 5 .3 3 8 5 0 .6 1 7 5 2 .2 4 6 9 6 .3 0 6 1 3 .3 6 5 7 8 .6 4 5 4 0 .0 7 4 5 7 .1 3 4 0 1 .1 9 PSS 20 menit
56 Lignin 500 750 1000 1250 1500 1750 2000 2250 2500 2750 3000 3250 3500 3750 4000 4250 4500 1/cm 30 40 50 60 70 80 90 100 %T 3 3 9 0 .8 6 3 0 0 3 .1 7 2 9 3 1 .8 0 2 8 5 0 .7 9 2 3 6 2 .8 0 2 3 3 5 .8 0 1 7 0 7 .0 0 1 6 5 4 .9 2 1 6 0 0 .9 2 1 5 1 0 .2 6 14 6 0 .1 1 1 4 2 3 .4 7 1 3 3 0 .8 8 1 2 1 5 .1 5 1 1 2 0 .6 4 1 0 3 1 .9 2 8 3 7 .1 1 6 1 7 .2 2 4 5 5 .2 0 Lignin Lignin tersulfonasi 500 750 1000 1250 1500 1750 2000 2250 2500 2750 3000 3250 3500 3750 4000 4250 4500 1/cm 20 30 40 50 60 70 80 90 100 %T 3 4 1 9 .7 9 2 9 3 7 .5 9 2 8 4 8 .8 6 1 6 0 4 .7 7 1 5 1 2 .1 9 1 4 5 8 .1 8 1 4 2 5 .4 0 1 2 0 9 .3 7 1 0 3 9 .6 3 8 1 3 .9 6 7 2 1 .3 8 6 6 1 .5 8 6 5 0 .0 1 5 2 8 .5 0 4 5 5 .2 0 Lignin tersulfonasi
5 7 P S S 15 % : L ign in 1% 5 0 0 7 5 0 1 0 0 0 1 2 5 0 1 5 0 0 1 7 5 0 2 0 0 0 2 5 0 0 3 0 0 0 3 5 0 0 4 0 0 0 4 5 0 0 1 /c m 2 0 30 40 50 60 07 80 90 %T 100 3446.79 2978.09 2924.09 2850.79 2781.35 2463.10 1948.10 1874.81 1805.37 1656.85 1600.92 1583.56 1492.90 1442.75 1381.03 1253.73 1114.86 1022.27 964.41 943.19 906.54 842.89 756.10 696.30 663.51 617.22 538.14 P S S 1 5 lig n in 1 P S S 15 % : L ign in 5% 5 0 0 7 50 1 0 0 0 1 2 5 0 1 5 00 1 7 50 2 0 0 0 2 5 0 0 3 0 0 0 35 0 0 40 0 0 4 5 0 0 1/ c m 4 5 5 2 .5 60 6 7 .5 75 8 2 .5 90 9 7 .5 % T 3425.58 2958.80 2926.01 2779.42 1946.18 1876.74 1716.65 1658.78 1602.85 1458.18 1381.03 1118.71 1024.20 840.96 752.24 698.23 619.15 538.14 P S S 1 5 lig n in 5
58 PSS 15% : Lignin 7% 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 4 4 6 .7 9 2 9 2 6 .0 1 1 9 4 6 .1 8 1 8 7 6 .7 4 1 6 5 8 .7 8 1 6 3 9 .4 9 1 6 0 2 .8 5 1 4 9 0 .9 7 1 4 4 8 .5 4 1 3 8 4 .8 9 1 2 5 1 .8 0 1 1 7 8 .5 1 1 1 0 9 .0 7 1 0 2 6 .1 3 9 8 3 .7 0 7 5 4 .1 7 6 9 8 .2 3 6 6 5 .4 4 6 1 9 .1 5 5 3 8 .1 4 PSS 15 lignin 7 PSS 15% : Lignin 10% 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 3 4 4 8 .7 2 2 9 2 6 .0 1 1 9 4 6 .1 8 1 6 6 0 .7 1 1 4 9 2 .9 0 1 4 4 2 .7 5 1 3 8 8 .7 5 1 1 0 3 .2 8 10 2 4 .2 0 7 5 0 .3 1 6 9 6 .3 0 5 4 0 .0 7 PSS 15 lignin 10
59
Lampiran E Perhitungan Berat Molekul Polimer.
Data Perhitungan Berat Molekul Polistiren
c (g/mL) t1 t2 t3 t4 t5 t rata-rata ηr ηsp ηred 0 3,06 3,07 3,08 3,06 3,08 3,07 - - - 0,001 3,2 3,2 3,2 3,23 3,23 3,212 1,046254 0,046254 46,25407 0,002 3,26 3,24 3,26 3,26 3,26 3,256 1,060586 0,060586 30,29316 0,003 3,37 3,37 3,38 3,39 3,38 3,378 1,100326 0,100326 33,44191 0,004 3,48 3,48 3,47 3,47 3,49 3,478 1,132899 0,132899 33,22476 0,005 3,52 3,57 3,57 3,57 3,56 3,558 1,358015 0,358015 71,60305 [η] = K. Mva 44,78 = (1,05 x 10-2) x Mv0,73 Mv = 93.855,53 gram/mol
60
Data Perhitungan Berat Molekul Polistiren Tersulfonasi
c (g/mL) t1 t2 t3 t4 t5 t rata-rata Ηr ηsp ηred 0 3,02 3,02 3,01 3,03 2,98 3,012 - - - 0,001 3,09 3,1 3,07 3,09 3,1 3,09 1,025896 0,025896 25,89641 0,002 3,2 3,19 3,18 3,15 3,17 3,178 1,055113 0,055113 27,55644 0,003 3,27 3,27 3,24 3,28 3,28 3,268 1,084993 0,084993 28,33112 0,004 3,36 3,39 3,38 3,35 3,37 3,37 1,118858 0,118858 29,71448 0,005 3,48 3,53 3,48 3,48 3,49 3,492 1,159363 0,159363 31,87251 [η] = K. Mva 24,44 = (1,05 x 10-2) x Mv 0,73 Mv = 40.945,68 gram/mol.
61
Lampiran F Termogram DTA/TGA Membran Poliblend.
PSS 15% : Lignin 1%.
62
PSS 15% : Lignin 7%.
63 Lampiran G Data Hasil Analisis Kekuatan Mekanik.
Tebal rata2Lebar rata2Luas (mm2) F (kgf) Δl (mm) F/A (Δl/l
0
)x 100%
ε
ε rata2 F/A rata2 (Δl/l
0
)x 100% rata2 ε rata2
PSS : LG 1%
1
0,230 0,220 0,240 3,700 3,700 3,700 0,2300 3,7000 0,8510
0,5
0,57 0,5875
0,1425
4,1231 5,1202 0,6456
0,1283
5,0303
2
0,280 0,280 0,280 3,480 3,480 3,480 0,2800 3,4800 0,9744
0,7
0,45 0,7184
0,1125
6,3857
3
0,310 0,310 0,310 3,580 3,580 3,580 0,3100 3,5800 1,1098
0,7
0,52 0,6307
0,1300
4,8519
PSS : LG 5%
1
0,270 0,270 0,270 3,520 3,520 3,520 0,2700 3,5200 0,9504
1,2
0,82 1,2626
0,2050
6,1592 6,1421 1,1401
0,1867
6,1075
2
0,300 0,310 0,300 3,420 3,420 3,420 0,3033 3,4200 1,0374
1,0
0,75 0,9639
0,1875
5,1411
3
0,235 0,240 0,235 3,540 3,540 3,540 0,2367 3,5400 0,8378
1,0
0,67 1,1936
0,1675
7,1260
PSS : LG 7%
1
0,130 0,130 0,130 3,270 3,270 3,280 0,1300 3,2733 0,4255
0,5
0,40 1,1750
0,1000
11,7500 9,8049 1,0604
0,1100
9,6401
2
0,140 0,140 0,140 3,140 3,140 3,140 0,1400 3,1400 0,4396
0,5
0,55 1,1374
0,1375
8,2720
3
0,160 0,150 0,160 3,670 3,670 3,680 0,1567 3,6733 0,5755
0,5
0,37 0,8688
0,0925
9,3927
PSS : LG 10% 1
0,180 0,180 0,180 4,110 4,120 4,120 0,1800 4,1167 0,7410
0,5
0,32 0,6748
0,0800
8,4345 6,1364 0,5325
0,0883
6,0280
2
0,160 0,160 0,160 4,060 4,040 4,040 0,1600 4,0467 0,6475
0,2
0,37 0,3089
0,0925
3,3394
3
0,200 0,200 0,200 4,080 4,060 4,080 0,2000 4,0733 0,8147
0,5
0,37 0,6137
0,0925
6,6351
Uji Tarik
64
65 Lampiran H Data Hasil Analisis Konduktivitas.
Komposisi
Poliblend
%
Luas (cm2)
1
2
1
2
1
2
1
2
1
2
1
2
1
2
PSS : Lignin 15 : 1 %
0,64
80
100
60
90
3200
12500
10000 16666,67 11111,11
312,5
0,028
0,02533 12187,5 9687,5 16354,17 10798,61 1,44E-06
15 : 5 %
0,64
80
110
65
90
3200
12500 9090,909 15384,62 11111,11
312,5
0,025
0,032 12187,5 8778,409 15072,12 10798,61 1,56E-06
15 : 7 %
0,64
160
150
120
100
3200
6250 6666,667 8333,333
10000
312,5
0,031
0,017 5937,5 6354,167 8020,833 9687,5 3,38E-06
15 : 10 %
0,64
200
140
190
120
3200
5000 7142,857 5263,158 8333,333
312,5
0,016
0,03867 4687,5 6830,357 4950,658 8020,833 2,85E-06
Kondk.
Rata2
Pengukuran Hantaran
1/R
elektroda
(μS)
R
elektroda
(ohm)
Tebal (cm)
Rmem (ohm) 1kHz Rmem(ohm) 50Hz
1/R(µS) pada 1kHz 1/R(µS) pada 50Hz
R sel(ohm) pada 1kHz
Rsel (ohm)pada 50
66
Lampiran I Data Analisis IEC
Kompolsisi Poliblend % Mo vol NaOH vol NaOH rata2 Hasil (mEq/gram) PSS : Lignin 15 : 1 % 0,0354 5,17 5,17 5,17 1,9769 15 : 3 % 0,0281 5,10 5,15 5,13 3,1132 15 : 5 % 0,0374 5,25 5,25 5,25 1,0396 15 : 7 % 0,0189 5,25 5,25 5,25 2,0571 15 : 10 % 0,0256 5,25 5,25 5,25 1,5187
