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Lampiran 1 Diagram alir penelitian
Onggok tapioka
• Pencangkokan dan penautan
Polimer Prototipe I • Saponifikasi Polimer Prototipe II Analisis Kadar N Kjeldahl (Peubah “y”) Spektrum FTIR (Peubah “x”) Spektrum FTIR (Peubah “x”) Analisis Kadar N Kjeldahl (Peubah “y”) PLS PCA PLS PCA
Lampiran 2 Sintesis Onggok ter-grafting dan crosslinking akril amida (Graftized Crosslinked Onggok)
Onggok tapioka kasar • Dicuci dengan air • Dikeringudarakan
• Dihaluskan hingga lolos ayakan 100 mesh Onggok tapioka bersih & halus
• Dimasukkan ke dalam labu leher tiga • (+) 150 mL air, diaduk (overhead stirer) • ∆ 95°C, Embusan dengan gas N2, 30 menit
• ∆ 60°C − 65°C, (+) APS (dalam 12,5 mL air), 15 menit, diaduk
• (+) AA dan MBA (dalam 200 mL air), perlahan, 20 – 30 menit, suhu dijaga minimal 55°C, diaduk
• ∆ 70°C, 3 jam, diaduk
Graftized Crosslinked Onggok • Didinginkan
• (+) 200 ml MeOH, 0,5 jam, diaduk • (+) 200 ml EtOH, 5 menit, diaduk • Dipisahkan antara padatan dan cairan
Graftized Crosslinked Onggok
• (+) 150 – 200 ml aseton, direfluks selama 1 jam • Dipisahkan antara padatan dan cairan
MeOH + EtOH
Graftized Crosslinked Onggok Homopolimer PAA • Dikeringkan di oven pada suhu 60°C
Graftized Crosslinked Onggok
Fasa padat Fasa cair
Lampiran 3 Saponifikasi Graftized Crosslinked acrylamide Onggok (Nakason et al 2010)
Graftized Crosslinked Onggok (40g) • (+) 100 ml NaOH 1M • (+) 100 ml air destilata • Refluks (T=90oC)
• (+) HCl 1M sampai netral
• (+) MeOH sampai mengendap sempurna • Dipisahkan antara padatan dan cairan
• Dikeringkan pada suhu 60o
C (di oven) • Dihaluskan
Saponified Graftized Crosslinked Onggok (40g)
H–Saponified Graftized Crosslinked Onggok
Padatan Cairan
MeOH + NaCl(aq)
MUHAMAD FARID. Grafting degree Measurement of acrylamide onto polysaccharide using Infrared Spectrometry. Under direction of ZAINAL ALIM MAS’UD and H.M. ANWAR NUR.
Utilization of carbohydrate-based agricultural wastes has been carried out with the manufacture of derivatives by grafting and crosslinking with acrylamide. The success of the process is monitored by setting the levels of nitrogen in the product. This research work is trying to look for possible use of spectrometry Fourier Transform Infrared technique to determine level of nitrogen in the products. Preparation of powder with a reflectance technique gives satisfactory results for grafting product, also for saponified products very satisfactory. ANOVA test of the PLS for each processing the data on IR spectral of the grafted-crosslinked product and its saponified showed a smaller probability value of 0.05, it is indicate the model developed by the independent variable (wave number) is significant effect on nitrogen content at 95% confidence level. Results of Partial Least Square (PLS) model for each treatment to give the coefficient of determination (R2) ranged from 0.961-0.998, it is the model with the wave number of independent variables can predict nitrogen content as well. Results of PLS analysis also provide information that the processing of IR spectrum data does not affect the difference between the predictions and the values of the nitrogen content.
PENDAHULUAN
Latar Belakang
Indonesia sebagai negara agraris pada tahun 2008 menghasilkan singkong (Manihot esculenta) sebesar 21.593.100 MT dengan nilai US$ 1.524.288.000, dan merupakan negara peringkat 3 dunia penghasil singkong (FAOSTAT). Salah satu produk turunan singkong adalah tepung tapioka. Proses produksi tapioka dari singkong akan menghasilkan produk samping yang disebut onggok. Setiap 1 ton singkong akan menghasilkan 160 kg onggok (Dit PPHP DitJen BPHH Deptan, 2005; Bank Indonesia. 2005). Onggok mempunyai nilai jual rendah (Rp. 1800,- – 2300,-/kg). Salah satu kandungan utama dalam onggok adalah karbohidrat, dalam bentuk selulosa dan pati. Onggok selama ini digunakan sebagai pengisi saos, pembuatan obat nyamuk bakar, dan salah satu komponen pakan ternak. Sebagai pakan ternak pun, onggok tidak bisa langsung digunakan, melainkan harus difermentasi terlebih dahulu. Untuk meningkatkan nilai tambah dari onggok, maka harus dilakukan proses modifikasi kandungan utamanya sehingga diperoleh turunan yang mempunyai nilai jual tinggi.
Lanthong et al. (2006) dan Nakason et al. (2010) telah melakukan modifikasi tepung singkong (tepung tapioka) melalui reaksi pencangkokan dan penautanulang akrilamida membentuk super adsorben yang ramah lingkungan. Nur et al. (2011) melakukan riset yang analog dengan bahan baku onggok. Hasil penelitiannya menunjukkan bahwa keberhasilan proses pencangkokan dan penautan ulang bisa dipantau dengan menentukan kandungan nitrogen dalam produk reaksi. Kandungan nitrogen ditentukan menggunakan metode klasik yaitu Kjeldahl.
Teknik pengukuran spektrum inframerah dekat (Near infrared, NIR) telah banyak digunakan dalam analisis kuatitatif nondestruktif yang cepat. Dengan mengukur spekrum inframerah sejumlah tertentu bahan yang analog yang sudah diketahui kadar analatnya dengan metoda lain, kemudian dilakukan pengolahan data Partial Least Square (PLS) maka dapat dibuat model kalibrasi hubungan antara serapan pada bilangan gelombang tertentu serta kandungan analat yang dicari.
Tujuan Penelitian
Penelitian ini bertujuan mengkuantifikasi hubungan antara besaran serapan inframerah pada bilangan gelombang karakteristik gugus fungsi amida produk penautan ulang dan saponifikasi dengan kandungan nitrogen menggunakan teknik analisis statistik PLS.
Hipotesis
Serapan inframerah pada daerah bilangan gelombang karakteristik gugus fungsi amida (1450 – 1780 cm–1 dan 3030 – 3450 cm–1) dari hasil pencangkokan dan penautansilang akrilamida serta produk turunan hasil saponifikasinya mempunyai hubungan kuantitatif yang linear dengan kadar nitrogen Kjeldahl.