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EFFECT OF SURFACE AREA AND PHYSICAL-CHEMICAL

PROPERTIES OF GRAPHIT AND GRAPHENE-BASED


MATERIALS ON THEIR ADSORPTION CAPASITY
TOWARDS METRONIDAZOLE AND TRIMETHOPRIM
ANTIBIOTICS IN AQUEOUS SOLUTION

PUTRI AYU NURMAKHMUDA (200604110070)


DIYAH AYU DWI LESTARI (200604110080)
TUJUAN PENELITIAN
Penetilitian ini bertujuan untuk :
1. Mengkaji adsorpsi senyawa farmasi pada bahan nano berdasarkan graphene
oxide (GO)
2. Mengetahui proses reduksi graphene oxide (GO)
3. Reduksi GO secara termal dalam ammonia (N-rGO) dengan luas permukaan
yang tinggi grafit (HSAG)
4. Mengetahui pengaruh pH terhadap kapasitas adsorpsi nanocarbon
5. Mengetahui hubungan kapasitas adsorpsi nanomaterial untuk karakteristik
kimia dan tekstur
6. Mengetahui keunggulan Adsorpsi mekanisme senyawa farmasi pada bahan
nano karbon
“Adsorpsi pada material berbasis graphene oxide (GO)
diterapkan untuk menghilangkan kontaminan yang berbeda
dari air, seperti pewarna, logam berat, organoklorin dan obat-
obatan”

NOVELTY
METODE
Karakterisasi
Materail Berbahan
01 BAHAN 03 Dasar Grafit dan
Grafena

Metode pembuatan Kuantifikasi


02 material berbasis 04 Metronidazole (MNZ)
dan Trimethopri (TMP)
grafena dan grafit
dalam Larutan Air
Metodologi
05 Pengadaan Data
Adsorpsi MNZ
atau TMP
METODE

BAHAN
1. Trimetoprim (TMP) 5. Grafit HSAG300
2. Metronidazole (MNZ) 6. Grafit HSAG400
3. Graphene Oxide (GO) 7. Grafit HSAG500
4. Grafit HSAG100 8. Grafit serpihan alami komersial
METODE
Metode pembuatan material berbasis
grafena dan grafit :
1. GO dikurangi secara termal dengan memasukkan tempat sampel yang mengandung sekitar 350 mg ke
dalam reactor vertical dan dibersihkan menggunakan N2 menggunakan suhu kamar dengan laju aliran 100
cm3 (STP)/menit selama 1 jam.
2. Setelah I jam, laju aliran dikurangi menjadi 87 cm 3 (STP)/menit dan diberikan gas N2 dan NH3 selama 5
jam.
3. Pada keadaan ini, sampel diperlakukan thermal dengan tiga suhu ramp.
4. Ramp pertama, GO dipanaskan dari suhu kamar hingga 100 OC dengan jangka 5OC/menit. Setelah
mencapai 100OC, suhu dipertahankan konstan selama 1 jam.
5. Ramp kedua, GO dipanaskan hingga suhu 300OC dengan jangka 5OC/menit.
6. Ramp terakhir, GO dipanaskan hingga 500OC dengan jangka 10OC/menit. Setelah mencapai 500OC, suhu
dipertahankan konstan selama 5 menit.
7. Sampel didinginkan hingga 400OC dan aliran H2 dan NH3 dihentikan.
8. Sampel didinginkan semalaman dibawah aliran N2.
9. Keesokan harinya, aliran N2 dihentikan dan sampel sudah menjadi N-rGo. (Tanpa adanya aliran NH 3,
nanomaterial hanya menjadi rGO).
METODE
Karakterisasi Materail Berbahan
Dasar Grafit dan Grafena :

1. Sifat tekstur ditentukan dengan fisisorsi N2 (N2 pada T = -196OC) yang memanfaatkan
percepatan luas permukaan, sistem porosimetri dan mikromeritik model ASAP 2020.
2. Untuk mengevaluasi luas permukaan (SBET), isotherm adsorpsi-desorpsi N2 diintepretasikan
menggunakan persamaan Brunauer-Emmett-Teller (BET).
3. Distribusi ukuran pori ditentukan melalui metode Barrett-Joyner-Halenda (BJH) ke cabang
desorpsi.
4. Kristalinitas sampel dianalisis menggunakan X-Ray Diffraction (XRD)
5. Gambar morfologi dari bahan GO, rGO dan N-rGO diambil melalui Mikroskop Elektron
Transmisi (TEM).
6. Penentuan konsentrasi gugus fungsi basa dan asam pada nanomaterial dapat ditentukan
mengguanakan prosedur titrasi volumetrik.
7. Kandungan gugus oksigen dievaluasi melalui Termogravimetri Analyzer (TGA), Instrumen TA.
METODE
Kuantifikasi Metronidazole (MNZ) dan
Trimethopri (TMP) dalam Larutan Air

1. Penentuan kuantitatif MNZ dilakukan dengan spektroskopi UV-Vis.


2. Absorbansi larutan MNZ diukur menggunakan Spektrofotometer sinar ganda
dengan panjang gelombang 320 nm.
3. Penentuan kuantifikasi TMP dilakukan menggunakan kromatografi cair yang
yang dilengkapi detector UV-Vis (panjang gelombang 286 nm).
4. TMP bisa ditentukan menggunakan spektroskopi UV-Vis tetapi metode HPLC
terntentu karena memiliki batas deteksi yang lebih rendah dan rentang
konsentrasi yang lebih luas.
METODE
Metodologi Pengadaan Data Adsorpsi MNZ
atau TMP :
1. Larutan antibiotik difiksasi dalam labu volumetrik 50 ml dengan konsentrasi variasi
antara 50-450mg/L dan 50-1000 mg/L untuk TMP dan MNZ.
2. pH larutan awal ditetapkan pada nilai tertentu dengan mencampurkan larutan HCl dan
NaOH 0,1 M dan laritan antibiotic sampel (5mL) untuk mengkonfirmasi konsentrasi
awalnya.
3. Eksperimen adsorpsi dilakukan dengan menambahkan sejumlah nano material dan 45 mL
larutan TMP atau MNZ ke dalam adsober batch eksperimental (botol plastik 50 mL) dan
diatur dalam penangas air yang dikontrol secara termostastik.
4. Adsober dilrtakkan diatas shaker untuk mencampur larutan penyerap selama 20 menit
tiga kali per hari.
5. pH larutan dipertahankan konstan dengan menambah volume kecil 0,1 M larutan HCl dan
NaOH selama adsorpsi.
METODE
Metodologi Pengadaan Data Adsorpsi MNZ
atau TMP :

5. Volume keseluruhan dari solusi ditambah untuk menyesuaikan pH lebih kecil dari 1,0%
dari volume asli. Dengan demikian, volume asli larutan pennyerap tidak berubah.
6. Pada awal percobaan diamati bahwa keseimbangan adsorpsi didekati dalam 7 hari.
Setelah setimbang, partikel nanomaterial dipisahkan dari larutan melalui sentrifugasi
larutan antibiotic pada 2500 rpm selama 5 menit dan kesetimbangan konsentrasi MNZ
atau TMP dievaluasi.
7. Jumlah antibiotic yang teradsorpsi dapat dihitung dengan persamaan :
q=
dimana,
CA0 = konsentrasi MNZ dan TMP pada awal proses (mg/L)
CAe = konsentrasi kesetimbangan MNZ atau TMP (mg/L)
M = jumlah nanocarbon (g)
q = jumlah TMP atau MNZ yang diserap (mg/g)
V = volume larutan didalam penyerap (L)
HASIL DAN
KESIMPULAN
• Sudut karakteristik 2θ = 14,9O dari GO pindah
ke 11,6O di GOrehydpH10 menyebabkan
perluasan ruang interlayer dari 0,594 nm
menjadi 0,762 nm.
• Perluasan interlayer antara GO dengan
MNZ teradsorpsi sedikit lebih tinggi dari
pada GOrehydpH10.
• MNZ tidak menyerap dalam ruang
interlayer
Grafik XRD dari GO
HASIL DAN
KESIMPULAN
• Pola ini dievaluasi untuk analisis interkalasi TMP dalam
struktur GO.
• Pola XRD dari GO, GOrehydpH10 dan GO dengan TMP
teradsorpsi pada pH = 10 (GO+TMP10)
• GO mengkonfirmasi hilangnya kristalinitas pada GOrehydpH10
dan GO+TMP10.
• Pergeseran bidang dianggap berasal dari air diselingi
pH = 10 dan adanya TMP.
• Ruang interlayer GOrehydpH10 dan GO+TMP10 adalah 0,762 nm
dan 0,884 nm sehingga adsorpsi TMP menyebabkan perluasan ruang
interlayer, tetapi peningkatan tidak cukup untuk membenarkan
interkalasi TMP di ruang interlayer GO.
• Karna peningkatan TMP, peneglupasan GO dikesampingkan.
• Sedikit puncak muncul pada sudut 2θ = 26 °, membuktikan bahwa Pola XRD dari GO, GOrehydpH10 dan
beberapa struktur grafit baik. GO dengan TMP teradsorpsi pada pH =
10 (GO+TMP10)
HASIL DAN
KESIMPULAN
• Dua puncak muncul pada sudut 2θ dari 31,9 ° dan 45,6
dalam pola XRD rGO+tmp10 DAN N-rGO+TMP10 dan
tidak ada informasi yang dapat menunjukkan
kemunculan kedua puncak tersebut.
• Adsorpsi TMP pada rGO dan N-rGO menyebabkan
peningkatan kristalinitas, yaitu susunan bidang, karena
puncak pada 2ÿ sedikit di atas 26 °, sesuai dengan
pantulan grafit (002), lebih tinggi dari pada di rGO dan
N-rGO.
• Ruang interlayer tidak berbeda secara signifikan selama
adsorpsi TMP.
• Hasil ini menguatkan bahwa bahan grafit menghadirkan Pola XRD dari rGO, N-rGO,
mekanisme adsorpsi seperti karbon aktif rGO+TMP10 dan N-rGO+TMP10
HASIL DAN
KESIMPULAN
Adsorpsi antibiotik pada bahan berbasis grafit dan oksida grafena tereduksi
sebagian besar disebabkan oleh interaksi dispersif -T karena interaksi ini
tergantung pada besarnya luas permukaan ketika konsentrasi kelompok
permukaan oksigen rendah. Analisis XRD menunjukkan bahwa adsorpsi MNZ
atau TMP dari larutan air pada GO, rGO dan N-rGO tidak terjadi di ruang
interlayer. TMP; oleh karena itu, pengelupasan GO dapat dikesampingkan.
Selain itu, sedikit puncak muncul pada sudut 2θ = 26 °, membuktikan bahwa
beberapa struktur grafit baik.
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