BAB V. KESIMPULAN DAN SARAN
A. Kesimpulan
Berdasarkan hasil pembahasan di atas dapat diambil kesimpulan sebagai berikut :
1. Ni/Al-hidrotalsit dapat diaplikasikan sebagai katalis dalam reaksi isomerisasi eugenol menggunakan pemanasan gelombang mikro.
2. Kenaikan daya gelombang mikro meningkatkan pembentukkan trans-isoeugenol tetapi tidak pada pembentukkan cis-trans-isoeugenol.
3. Kenaikan waktu reaksi isomerisasi meningkatkan pembentukkan trans-isoeugenol tetapi tidak pada pembentukkan cis-trans-isoeugenol.
B. Saran
Berdasarkan penelitian yang telah dilakukan penulis memberikan saran, perlu dilakukan penelitian lanjutan tentang pemurnian isoeugenol hasil reaksi isomerisasi eugenol dengan katalis Ni/Al-hidrotalsit menggunakan pemanasan gelombang mikro.
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LAMPIRAN 1. Desain Penelitian
Sintesis Katalis Ni/Al-Hidrotalsit
Karakterisai Katalis ( XRD)
Aplikasi Katalis dalam Reaksi Isomerisasi Eugenol
Variasi Daya (300, 400, 500 watt)
Variasi Waktu Kontak ( 30, 40, 50, 60 menit)
Penentuan Daya Optimum Penentuan Waktu Kontak
Optimum
Analisa GC Senyawa Reaktan
LAMPIRAN 2. Skema Pembuatan Katalis Ni/Al-hidrotalsit
200 mmol NiCl2.6H2O 50 mmol AlCl3.6H2O
400 mL Na2CO3
400 mmol 200 mL akuades
diaduk dengan magnet stirer
Dilarutkan
tetes per tetes dengan kecepatan 5 mL/menit Dijaga pH 10 NaOH 1 M Suspensi Larutan T 60-63 °C , 1 jam didiamkan diaduk dengan magnet stirer T 60-63 °C , 18 jam Endapan terpisah disaring Endapan akuades
Sampai bebas ion Cl
-Endapan bebas ion Cl- Tidak terbentuk AgCl AgNO3 1 M
dioven pada T 80 oC ,16 jam
Endapan kering
dikalsinasi pada T 263 °C,1 jam
Katalis Ni/Al-hidrotalsit dihaluskan
LAMPIRAN 3. Perhitungan Pembuatan Larutan
1. NiCl2.6H2O 200 mmol:
Mr NiCl2.6H2O = 58,710 + (2 X 35,453) + (6 X 18,015) = 237,706 g/mol Massa NiCl2.6H2O = mol NiCl2.6H2O X Mr NiCl2.6H2O
= 0,2 mol X 237,706 g/mol = 47,541 g
2. AlCl3.6H2O 50 mmol :
Mr AlCl3.6H2O = 26,982 + (3 X 35,453) + (6 X 18,015) = 241,431 g/mol Massa AlCl3.6H2O = mol AlCl3.6H2O X Mr AlCl3.6H2O
= 0,05 mol X 241,431 g/mol = 12,072 g 3. Na2CO3 400 mmol : Mr Na2CO3 = (2 X 22,990) + 12,011 + (3 X 15,999) = 105,988 g/mol Massa Na2CO3 = mol Na2CO3 + Mr Na2CO3 = 0,4 mol X 105,988 g/mol = 42,395 g 4. NaOH 1 M sebanyak 400 mL : Mr NaOH = 22,990 + 15,999 + 1,008 = 39,997 Massa NaOH = V NaOH X M NaOH X Mr NaOH
= 0,4 L X 1 mol/L X 39,997 g/mol = 15,999 g
5. AgNO3 0,1 M :
Mr AgNO3 = 107,870 + 14,007 + (3 X 15,999) = 169,874 g/mol Massa AgNO3 = V AgNO3 X M AgNO3 X Mr AgNO3
= 0,01 L X 0,1 mol/L X 169,874 g/mol = 0,170 g
LAMPIRAN 4. Data X-Ray Diffraction (XRD) Ni/Al-hidrotalsit Hasil Sintesis
Peak Search Report (17 Peaks, Max P/N = 7.3) [Ni-Al Hidrotalsite-sebelum.raw] Ni-Al Hidrotalsite
PEAK: 47-pts/Parabolic Filter, Threshold=3.0, Cutoff=0.1%, BG=3/1.0, Peak-Top=Summit
2-Theta d(Å) BG Height I% Area I% FWHM 4,989 17,6986 68 8 2,6 16 0,1 0,1 10,011 8,8281 75 107 34,3 1980 9,8 0,296 11,48 7,7017 140 312 100 20128 100 1,097 15,012 5,8967 29 6 1,9 12 0,1 0,1 19,96 4,4447 34 3 1 6 0 0,1 22,78 3,9005 101 111 35,6 5096 25,3 0,78 24,98 3,5617 38 5 1,6 10 0 0,1 29,98 2,9781 27 3 1 6 0 0,1 34,191 2,6203 42 101 32,4 2474 12,3 0,416 34,86 2,5716 115 84 26,9 4334 21,5 0,877 35,001 2,5615 127 63 20,2 3130 15,6 0,795 39,038 2,3054 84 29 9,3 1369 6,8 0,755 39,98 2,2532 91 3 1 6 0 0,1 44,98 2,0137 61 2 0,6 4 0 0,1 46,306 1,9591 68 19 6,1 612 3 0,515 50,009 1,8223 46 7 2,2 14 0,1 0,1 55 1,6682 26 7 2,2 14 0,1 0,1
LAMPIRAN 5. Data JCPDS Ni/Al-hidrotalsit (Takovite) PDF#15-0087: QM=Indexed(I); d=Debye-Scherrer(114.6mm); I=Film/Visual Takovite
Ni6 Al2 ( O H )16 ( C O3 , O H ) !4 H2 O Blue-green Radiation=CuKa Lambda=1.5418 Filter=
Calibration= 2T=11.727-149.602 I/Ic(RIR)= Ref: Bish, D., Brindley.
Am. Mineral., v62 p458 (1977)
Rhombohedral - Powder Diffraction, R-3m (166) Z=0.375 mp= CELL: 3.025 x 3.025 x 22.595 <90.0 x 90.0 x 120.0> P.S=hR7 (?)
Density(c)=2.790 Density(m)=2.700 Mwt=810.35 Vol=179.06 F(30)=11.2(0.064,42/1) Ref: Ibid.
Strong Lines: 7.54/X 2.55/8 3.77/7 2.27/7 1.92/6 1.51/5 1.48/5 1.40/3 1.26/3 1.71/3 NOTE: Specimen from Takovo, Serbia, Yugoslavia.
2-Theta d(Å) I(f) ( h k l) Theta 1/(2d) 2pi/d n^2 11.727 7.5400 100.0 ( 0 0 3) 5.864 0.0663 0.8333 23.579 3.7700 70.0 ( 0 0 6) 11.790 0.1326 1.6666 34.385 2.6060 5.0 ( 1 0 1) 17.192 0.1919 2.4110 35.121 2.5530 80.0 ( 0 1 2) 17.561 0.1958 2.4611 37.817 2.3770 15.0 ( 1 0 4) 18.908 0.2103 2.6433 39.709 2.2680 70.0 ( 0 1 5) 19.854 0.2205 2.7704 44.438 2.0370 10.0 ( 1 0 7) 22.219 0.2455 3.0845 47.279 1.9210 60.0 ( 0 1 8) 23.639 0.2603 3.2708 48.157 1.8880 1.0 ( 0 0 12) 24.078 0.2648 3.3280 53.512 1.7110 25.0 ( 1 0 10) 26.756 0.2922 3.6722 56.896 1.6170 20.0 ( 0 1 11) 28.448 0.3092 3.8857 61.209 1.5130 50.0 ( 1 1 0) 30.604 0.3305 4.1528 62.585 1.4830 50.0 ( 1 1 3) 31.292 0.3372 4.2368 64.276 1.4480 20.0 ( 1 0 13) 32.138 0.3453 4.3392 66.546 1.4040 30.0 ( 1 1 6) 33.273 0.3561 4.4752 68.196 1.3740 15.0 ( 0 1 14) 34.098 0.3639 4.5729 72.608 1.3010 25.0 ( 2 0 2) 36.304 0.3843 4.8295 73.460 1.2880 3.0 ( 1 1 9) 36.730 0.3882 4.8783 75.442 1.2590 30.0 ( 2 0 5) 37.721 0.3971 4.9906 76.588 1.2430 20.0 ( 1 0 16) 38.294 0.4023 5.0549 78.765 1.2140 5.0 ( 0 2 7) 39.383 0.4119 5.1756 80.676 1.1900 15.0 ( 2 0 8) 40.338 0.4202 5.2800 85.665 1.1330 5.0 ( 0 2 10) 42.833 0.4413 5.5456 88.387 1.1050 10.0 ( 2 0 11) 44.194 0.4525 5.6861 90.673 1.0830 2.0 ( 1 0 19) 45.336 0.4617 5.8016 92.763 1.0640 1.0 ( 1 1 15) 46.381 0.4699 5.9053 94.972 1.0450 5.0 ( 0 2 13) 47.486 0.4785 6.0126 98.472 1.0170 2.0 ( 2 0 14) 49.236 0.4916 6.1782 102.701 0.9863 10.0 ( 1 2 2) 51.350 0.5069 6.3705 105.685 0.9665 15.0 ( 1 2 5) 52.843 0.5173 6.5010 109.026 0.9460 2.0 ( 2 1 7) 54.513 0.5285 6.6418 111.208 0.9335 10.0 ( 1 2 8) 55.604 0.5356 6.7308 116.446 0.9061 5.0 ( 2 1 10) 58.223 0.5518 6.9343 119.610 0.8912 5.0 ( 1 2 11) 59.805 0.5610 7.0503 123.777 0.8733 3.0 ( 3 0 0) 61.889 0.5725 7.1948 125.356 0.8670 5.0 ( 3 0 3) 62.678 0.5767 7.2470 127.271 0.8597 3.0 ( 2 1 13) 63.635 0.5816 7.3086 129.801 0.8506 2.0 ( 3 0 6) 64.900 0.5878 7.3868 131.448 0.8450 1.0 ( 1 2 14) 65.724 0.5917 7.4357 138.247 0.8244 2.0 ( 3 0 9) 69.124 0.6065 7.6215 144.315 0.8092 2.0 ( 0 2 22) 72.158 0.6179 7.7647 149.602 0.7982 2.0 74.801 0.6264 7.8717
LAMPIRAN 6. Perbandingan Harga d Sample dengan Standar Ni/Al-HT Sample standar d(Å) Height d(Å) Height selisih d 17,6986 8 8,8281 107 7,7017 312 7,54 100 0,1617 5,8967 6 4,4447 3 3,9005 111 3,77 70 0,1305 3,5617 5 2,9781 3 2,6203 101 2,606 5 0,0143 2,5716 84 2,5615 63 2,553 80 0,0085 2,3054 29 2,377 15 -0,0716 2,2532 3 2,268 70 -0,0148 2,0137 2 2,037 10 -0,0233 1,9591 19 1,921 60 0,0381 1,8223 7 1,888 1 -0,0657 1,6682 7 1,711 25 -0,0428
LAMPIRAN 7. Perhitungan Persentase Kandungan Ni/Al-hidrotalsit (Takovite)
1. Kemurnian Ni/Al-hidrotalsit (takovite) dalam Sampel Kemurnian takovite = I takovite dalam sampel X 100 %
I total sampel = 654 X 100 % 870
LAMPIRAN 9. Data Hasil IR dari SDBS
Welcome to Spectral Database for Organic
Compounds, SDBS.
This is a free site organized by National Institute of Advanced Industrial Science and Technology (AIST), Japan.
SDBS
Information
SDBS No.: 91 Compound Name: eugenol Molecular Formula: C10H12O2 Molecular Weight: 164.2CAS Registry No.:
97-53-0
LAMPIRAN 10. Kondisi Kromatografi Gas Hewlett Pacard 5890 Series II
Kromatografi gas yang digunakan adalah kromatografi gas Hewlett Pacard 5890 Series II, dengan kondisi analisa sebagai berikut :
Jenis Kolom : HP 5 Suhu Kolom
Suhu Awal : 120 °C Suhu Akhir : 280 °C Waktu Awal : 2 menit Kenaikan Suhu : 10°C / menit Jenis Detektor : FID
Suhu detektor : 300 °C Suhu Injektor : 280 °C Gas pembawa : Helium Total Flow : 80 Split (Kpa) : 60 Jumlah Injeksi : 0,06 μL
LAMPIRAN 13. Data Kromatografi Gas Hasil Reaksi pada Daya 500 watt, Waktu Reaksi 30 menit, dengan Katalis Ni/Al-hirotalsit
LAMPIRAN 14. Data Kromatografi Gas Hasil Reaksi pada Daya 500 watt, Waktu Reaksi 40 menit, dengan Katalis Ni/Al-hirotalsit
LAMPIRAN 15. Data Kromatografi Gas Hasil Reaksi pada Daya 500 watt, Waktu Reaksi 50 menit, dengan Katalis Ni/Al-hirotalsit
LAMPIRAN 16. Data Kromatografi Gas Hasil Reaksi pada Daya 500 watt, Waktu Reaksi 60 menit, dengan Katalis Ni/Al-hirotalsit
LAMPIRAN 17. Data Kromatografi Gas Hasil Reaksi pada Daya 400 watt, Waktu Reaksi 60 menit, dengan Katalis Ni/Al-hirotalsit
LAMPIRAN 18. Data Kromatografi Gas Hasil Reaksi pada Daya 300 watt, Waktu Reaksi 60 menit, dengan Katalis Ni/Al-hirotalsit
LAMPIRAN 19. Data Kromatografi Gas Hasil Reaksi pada Daya 500 watt, Waktu Reaksi 60 menit, Tanpa Katalis Ni/Al-hirotalsit
LAMPIRAN 20. Data Kromatografi Gas Hasil Reaksi pada Daya 400 watt, Waktu Reaksi 60 menit, dengan Katalis Ni/Al-hirotalsit, dengan Teknik Spiking