I.
Tujuan
1. Mengetahui dan memahami prinsip penetapan kadar dengan metode Spektrofotometri 2. Mengetahui dan memahami penerapan metode Spektrofotometri dalam bidang farmasi 3. Mampu menetapkan kadar sediaan obat dalam bentuk salep secara Spektrofotometri
II.
Dasar Teori
A. Pengertian Salep
Salep adalah sediaan setengah padat ditujukan untuk pemakaian topikal pada kulit atau selaput lendir. Dasar salep yang digunakan sebagai pembawa dibagi dalam empat kelompok yaitu dasar salep senyawa hidrokarbon, dasar salep serap, dasar salep yang dapat dicuci dengan air dan dasar salep larut dalam air. Salep obat menggunakan salah satu dari dasar salep tersebut (FI IV, hal. 18). B. Penggolongan Salep Berdasarkan Kerja Farmakologi (Art of Compounding, hal 339), ada 3 golongan:
1. Salep Epidermik Salep ini dimaksudkan hanya bekerja dipermukaan kulit untuk menghasilkan efek lokal. Diharapkan tidak diserap dan hanya berlaku sebagai pelindung, antiseptik, astringen melawan rangsangan (yaitu sebagai anti radang) dan parasitida. Dasar salep yang sering dipakai adalah vaselin. 2. Salep Endodermik Dimaksudkan untuk melepaskan obat ke kulit tetapi tidak menembus kulit, diserap sebagian saja. Salep ini dapat berlaku berlaku sebagai emolien, emolien, stimulan dan lokal iritan. Dasar salep terbaik yang digunakan adalah minyak tumbuhan dan minyak alami.
3. Salep Diadermik Salep ini dimaksudkan untuk melepaskan obat menembus kulit dan menimbulkan efek konstitusi (efek terapi yang diinginkan). Namun hal ini tidak lazim digunakan dan termasuk
Laporan Kimia Farmasi – Penentuan Senyawa Obat dalam Sediaan Salep
Page 1 Page 1
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pemakaian khusus obat-obat seperti senyawa raksa, iodida dan belladona. Dasar salep yang terbaik digunakan adalah lanolin, adeps lanae dan oleum cacao.
Berdasarkan Penetrasi (RPS 16, 1518-1519), salep dikelompokkan menjadi :
1. Mempunyai Mempunyai efek permukaan Mempunyai efek permukaan, memiliki aktivitas membentuk lapisan film yang bertujuan untuk mencegah hilangnya kelembaban (sebagai protektif), efek membersihkan
ataupun
sebagai
antibakteri.
Pembawa
(basis)
harus
dapat
memudahkan kontak dengan permukaan dan melepaskan zat aktif ke sasaran. 2. Mempunyai Mempunyai efek pada stratum korneum Contoh salep dengan efek ini adalah sediaan sunscreen yang mengandung asam pamino benzoat yang berpenetrasi ke stratum korneum. 3. Mempunyai Mempunyai efek epidermal Pada salep ini obat/zat aktif dapat penetrasi kelapisan kulit yang paling dalam.
Menurut konsistensinya salep dibagi menjadi :
1. Unguenta : adalah salep yang mempunyai konsistensi seperti mentega, tidak mencair pada suhu biasa tetapi mudah dioleskan tanpa memakai tenaga. 2. Cream : adalah salep yang banyak mengandung air, mudah diserap kulit. Suatu tipe yang dapat dicuci dengan air. 3. Pasta : adalah suatu salep yang mengandung lebih dari 50% zat padat (serbuk). Suatu salep tebal karena merupakan penutup atau pelindung bagian kulit yang diberi. 4. Cerata : adalah suatu salep berlemak yang mengandung persentase tinggi lilin (waxes), sehingga konsistensinya lebih keras. 5. Gelones Spumae : (Jelly) adalah suatu salep yang lebih halus. Umumnya cair dan mengandung sedikit atau tanpa lilin digunakan terutama pada membran mukosa sebagai pelicin atau basis. Biasanya terdiri dari campuran sederhana minyak dan lemak dengan titik lebur yang rendah.
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Menurut Efek Terapinya, salep dibagi atas :
1. Salep Epidermic (Salep Penutup) : Digunakan pada permukaan kulit yang berfungsi hanya untuk melindungi kulit dan menghasilkan efek lokal, karena bahan obat tidak diabsorbsi. Kadang-kadang ditambahkan antiseptik, astringen untuk meredakan rangsangan. rangsangan. Dasar salep yang terbaik adalah senyawa hidrokarbon (vaselin). 2. Salep Endodermic : Salep dimana bahan obatnya menembus ke dalam tetapi tidak melalui kulit dan terabsorbsi sebagian. Untuk melunakkan kulit atau selaput lendir diberi lokal iritan. Dasar salep yang baik adalah minyak lemak. 3. Salep Diadermic (Salep Serap) : Salep dimana bahan obatnya menembus ke dalam melalui kulit dan mencapai efek yang diinginkan karena diabsorbsi seluruhnya, misalnya pada salep yang mengandung senyawa Mercuri, Iodida, Belladonnae. Dasar salep yang baik adalah adeps lanae dan oleum cacao.
Menurut Dasar Salepnya, salep dibagi atas :
1. Salep hydrophobic yaitu salep-salep dengan bahan dasar berlemak, misalnya: campuran dari lemak-lemak, minyak lemak, malam yang tak tercuci dengan air. 2. Salep hydrophillic yaitu salep yang kuat menarik air, biasanya dasar salep tipe o/w atau seperti dasar hydrophobic tetapi konsistensinya lebih lembek, kemungkinan juga tipe w/o antara lain campuran sterol dan petrolatum.
Berdasar fisik-konsistensi (viskositas = kekentalan)
1. Cairan kental/encer : linimentum – pasta 2. Setengah padat : cream – cream – unguentum unguentum – pasta 3. Lebih bersifat padat : sapo medicatus, emplastrum
Dasar Salep
Menurut FI. IV, dasar salep yang digunakan sebagai pembawa dibagi dalam 4 kelompok, yaitu dasar salep senyawa hidrokarbon, dasar salep serap, dasar salep yang dapat dicuci dengan air, dasar salep larut dalam air. Setiap salep obat menggunakan salah satu dasar salep tersebut.
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kedalamnya. Salep ini dimaksudkan untuk memperpanjang kontak bahan obat dengan kulit dan bertindak sebagai pembalut penutup. Dasar salep hidrokarbon digunakan terutama sebagai emolien, sukar dicuci, tidak mengering dan tidak tampak berubah dalam waktu lama. 2. Dasar Salep Serap Dasar salep serap ini dibagi dalam 2 kelompok. Kelompok pertama terdiri atas dasar salep yang dapat bercampur dengan air membentuk emulsi air dalam minyak (parafin hidrofilik dan lanolin anhidrat), dan kelompok kedua terdiri atas emulsi air dalam minyak yang dapat bercampur dengan sejumlah larutan air tambahan (lanolin). Dasar salep ini juga berfungsi sebagai emolien. 3. Dasar Salep yang dapat dicuci dengan air. Dasar salep ini adalah emulsi minyak dalam air, antara lain salep hidrofilik (krim). Dasar salep ini dinyatakan juga sebagai dapat dicuci dengan air, karena mudah dicuci dari kulit atau dilap basah sehingga lebih dapat diterima untuk dasar kosmetika. Beberapa bahan obat dapat menjadi lebih efektif menggunakan dasar salep ini dari pada dasar salep hidrokarbon. Keuntungan lain dari dasar salep ini adalah dapat diencerkan dengan air dan mudah menyerap cairan yang terjadi pada kelainan dermatologik. 4. Dasar Salep Larut Dalam Air Kelompok ini disebut juga dasar salep tak berlemak dan terdiri dari konstituen larut air. Dasar salep jenis ini memberikan banyak keuntungannya keuntungannya seperti dasar salep yang dapat dicuci dengan air dan tidak mengandung bahan tak larut dalam air, seperti paraffin, lanolin anhidrat atau malam. Dasar salep ini i ni lebih tepat disebut gel. Pemilihan dasar salep tergantung pada beberapa faktor yaitu khasiat yang diinginkan, sifat bahan obat yang dicampurkan, ketersediaan hayati, stabilitas dan ketahanan sediaan jadi. Dalam beberapa hal perlu menggunakan dasar salep yang kurang ideal untuk mendapatkan stabilitas yang diinginkan. Misalnya obat-obat yang cepat terhidrolisis, lebih stabil dalam dasar salep hidrokarbon daripada dasar salep yang mengandung air, meskipun obat tersebut bekerja lebih efektif dalam dasar salep yang mangandung air.
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Beberapa contoh – contoh – contoh contoh dasar salep :
1. Dasar salep hidrokarbon Vaselin putih ( = white petrolatum = whitwe soft paraffin), vaselin kuning (=yellow petrolatum = yellow soft paraffin), campuran vaselin dengan cera, paraffin cair, paraffin padat, minyak nabati. 2. Dasar salep serap (dasar salep absorbsi) Adeps lanae, unguentum simpleks (cera flava : oleum sesami = 30 : 70), hydrophilic petrolatum ( vaselin alba : cera alba : stearyl alkohol : kolesterol = 86 : 8 : 3 : 3 ) 3. Dasar salep dapat dicuci dengan air. Dasar salep emulsi tipe m/a m/ a (seperti ( seperti vanishing cream), emulsifying ointment B.P., emulsifying wax, hydrophilic ointment. 4. Dasar salep larut air Poly Ethylen Glycol (PEG), campuran PEG, tragacanth, gummi arabicum
C. Kualitas dasar salep yang baik adalah:
1. Stabil, selama dipakai harus bebas dari inkompatibilitas, tidak terpengaruh oleh suhu dan kelembaban kamar. 2. Lunak, semua zat yang ada dalam salep harus dalam keadaan halus, dan seluruh produk harus lunak dan homogen. 3. Mudah dipakai 4. Dasar salep yang cocok 5. Dapat terdistribusi merata
D. Persyaratan salep menurut FI ed III
1. Pemerian 2. Tidak boleh berbau tengik 3. Kadar Kecuali dinyatakan lain dan untuk salep yang mengandung obat keras atau narkotik, kadar bahan obat adalah 10 %. 4. Dasar salep 5. Homogenitas
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6. Penandaan Pada etiket harus tertera “obat luar” l uar” (Syamsuni, 2005).
E. Aturan umum pembuatan salep
Bagian – bagian yang dapat larut dalam sejumlah campuran lemak yamg diperuntukkan bilamana perlu dilarutkan dengan pemanasan di dalamnya. Zat-zat yang mudah larut dalam air kecuali ditentukan lain ,bila banyak nya air yang dipergunakan untuk pelarutan dapat dipungut oleh jumlah campuran lemak yang telah ditentukan, mula-mula dilarutkan dalam air; banyaknya air yang dipergunakan mula-mula dikurangi dari jumlah yang telah ditentukan dari campuran lemak. Zat-zat yang dalam lemak dan dalam air atau kurang cukup dapat larut harus sebelumnya dijadikan serbuk, dan diayak melalui dasar ayakan B40. Pada pembuatan unguenta ini zat yang padat sebelumnya dicampur rata dengan lemak, yang beratnya sama atau setengahnya,bilamana perlu sebelumnya dilelehkan dan kemudian sejumlah sisa lemaknya telah atau tidak dilelehkan ditambahkan sebagian demi sebagian. Apabila unguenta dibuat dengan perlelehan, maka campurannya harus diaduk sampai dingin.
Zat-zat yang dapat dilarutkan dalam dasar salep
Umumnya kelarutan obat dalam minyak lemak lebih besar daripada dalam vaselin. Champora, Mentholum, Phenolum, Thymolum dan Guayacolum lebih mudah dilarutkan dengan cara digerus dalam mortir dengan minyak lemak. Bila dasar salep mengandung vaselin, maka zat-zat tersebut digerus halus dan tambahkan sebagian (+ sama banyak) Vaselin sampai homogen, baru ditambahkan sisa vaselin dan bagian dasar salep yang lain. Champora dapat dihaluskan dengan tambahan Spiritus fortior atau eter secukupnya sampai larut setelah itu ditambahkan dasar salep sedikit demi sedikit, diaduk sampai spiritus fortiornya menguap. Bila zat-zat tersebut bersama-sama dalam salep, lebih mudah dicampur dan digerus dulu biar meleleh baru ditambahkan dasar salep sedikit demi sedikit. Zat-zat yang mudah larut dalam air
Bila masa salep mengandung air dan obatnya dapat larut dalam air yang tersedia
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salep yang dapat menyerap air antara lain ialah Adeps lanae, Unguentum Simplex, hydrophilic ointment. Dan dasar salep yang sudah mengandung air antara lain Lanoline (25% air), Unguentum Leniens (25%), Unguentum Cetylicum hydrosum (40%).
Zat-zat yang kurang larut atau tidak larut dalam dasar salep
Zat-zat ini diserbukkan dulu dengan derajat halus serbuk pengayak no.100. setelah itu serbuk dicampur baik-baik dengan sama berat masa salep, atau dengan salah satu bahan dasar salep. Bila perlu bahan dasar salep tersebut dilelehkan terlebih dahulu, setelah itu sisa bahan-bahan yang lainditambahkan sedikit demi sedikit sambil digerus dan diaduk hingga homogen. Untuk pencegahan pengkristalan pada waktu pendinginan, seperti Cera flava, Cera alba, Cetylalcoholum dan Paraffinum solidum tidak tersisa dari dasar salep yang cair atau lunak.
F. Sifat-sifat salep
Sifat-sifat dari salep yang digunakan untuk mengobati penyakit-penyakit kulit, harus : 1. Bersifat antiseptika (mencegah infeksi) 2. Bersifat protektiva (bahan yang mampu melindungi kulit yang luka atau yang sakit) 3. Bersifat emolien (bahan yang mampu m ampu menghaluskan dan melemaskan kulit) 4. Bahan-bahan yang dapat mengurangi rasa gatal 5. Bahan-bahan yang cepat menguap sehingga terjadi pendinginan setempat Misalnya : kamfer,menthol 6. Bahan-bahan yang dapat menahan rasa sakit setempat. Misalnya : phenol, anaesthesin
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ditambahkan pada campuran yang sedang mengental setelah didinginkan dan diaduk. Cara pembuatan salep ditinjau dari zat khasiat utamanya :
1. Zat padat a. Zat padat dan larut dalam dasar salep Camphorae Dilarutkan dalam dasar salep yang sudah dicairkan didalam pot salep tertutup (jika tidak dilampaui daya larutnya). Jika dalam resepnya terdapat minyak lemak (Ol. sesami), camphorae dilarutkan lebih dahulu dalam minyak min yak tersebut Jika dalam resep terdapat salol, menthol, atau zat lain yang dapat mencair jika dicampur (karena penurunan titik eutektik), camphorae dicampurkan supaya mencair, baru ditambahkan dasar salepnya Jika camphorae itu berupa zat tunggal, camphorae ditetesi lebih dahulu dengan eter atau alkohol 95%, kemudian digerus dengan dasar salepnya
Pellidol Larut 3% dalam dasar salep, pellidol dilarutkan bersama-sama dengan dasar salepnya yang dicairkan (jika dasar salep disaring tetapi jangan lupa harus ditambahkan pada penimbangannya sebanyak 20% ). Jika pellidol yang ditambahkan melebihi daya larutnya, maka digerus dengan dasar salep yang mudah dicairkan.
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b. Zat padat larut dalam air Protargol Taburkan diatas air, diamkan ditempat gelap selama ¼ jam sampai larut Jika dalam resep resep terdapat gliserin, gliserin, tambahkan
gliserin tersebut, baru baru
ditambahkan airnya dan tidak perlu ditunggu ¼ jam lagi karena dengan adanya gliserin, protargol atau mudah larut. Colargol Dikerjakan seperti protargol Argentum nitrat (AgNO3) Walaupun larut dalam air, zat ini tidak boleh dilarutkan dalam air karena akan meninggalkan bekas noda hitam pada kulit yang disebabkan oleh terbentuknya Ag2O, kecuali pada resep obat wasir. Fenol/fenol Sebenarnya fenol mudah larut dalam air, tetapi dalam salep tidak dilarutkan karena akan menimbulkan rangsangan atau mengiritasi kulit dan juga tidak boleh diganti dengan Phenol liquifactum (campuran fenol dan air 77-81,5% FI ed.III). Bahan obat yang larut dalam air tetapi tidak boleh dilarutkan dalam air, yaitu :
1. Argentum nitrat : stibii et kalii tartras 2. Fenol : oleum iocoris aselli 3. Hydrargyri bichloridum : zink sulfat 4. Chrysarobin : antibiotik (misalnya penicilin)
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3. Air Ditambahkan terakhir karena berfungsi sebagai pendingin; disamping itu, untuk mencegah permukaan permukaan mortir menjadi licin. l icin. 4. Gliserin Harus ditambahkan ke dalam dasar salep yang dingin, karena tidak bisa bercampur dengan bahan dasar salep yang sedang mencair dan harus ditambahkan sedikit demi sedikit karena tidak mudah diserap oleh dasar salep.
5. Marmer album Dimasukkan terakhir karena dibutuhkan dalam bentuk kasar, yang akan memberikan pengaruh percobaan pada kulit.
c.
Zat padat tidak larut dalam air.
Umumnya dibuat serbuk halus dahulu, misalnya : 1. Belerang (tidak boleh diayak) 2. Ac. Boricum (diambil bentuk yang pulveratum) 3. Oxydum zincicum (diayak dengan ayakan No. 100/B40). 4. Mamer album (diayak dengan ayakan a yakan No.25/B10) 5. Veratrin (digerus dengan minyak, karena jika digerus tersendiri akan menimbulkan bersin).
2. Zat cair
Sebagai pelarut bahan obat a. Air Terjadi reaksi
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b. Cairan kental Umumnya dimasukan sedikit demi sedikit. Contohnya : gliserin, pix lithantratis, pix liquida, balsem peruvianum, ichtyol, kreosot. c. Bahan berupa ekstrak/extractum Extractum sicccum /kering Umumnya larut dalam air, maka dilarutkan dalam air, dan berat air dapat dikurangkan dari dasar salepnya Extractum spissum/kental spissum/kental Diencerkan dahulu dengan air atau etanol Extractum liquidum Dikerjakan seperti pada cairan dengan spiritus.
d. Bahan-bahan lain
1. Hydrargyrum Gerus dengan adeps lanae dalam lumpang dingin, sampai halus (<20µg) atau gunakan resep standar, misalnya : Unguentum Hydrargyri (Ph.Belanda V) yang mengandung 30% dan Unguentum Hydrargyri Fortio (C.M.N) mengandung 50% 2. Naphtolum Dapat larut dalam sapo kalicus, larutkan dalam sapo tersebut. Jika tidak ada sapo, dikerjakan seperti Camphorae. Mempunyai Mempunyai D.M/T.M untuk obat luar. 3. Bentonit Serbuk halus yang dengan air akan membentuk massa seperti salep.
H. Pengawetan salep
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I. Fungsi salep
1. Sebagai bahan pembawa substansi obat untuk pengobatan kulit. 2. Sebagai bahan pelumas pada kulit. 3. Sebagai pelindung untuk kulit yaitu mencegah kontak permukaan kulit dengan larutan berair dan rangsang kulit.
J. Pengemasan dan penyimpanan salep
Salep biasanya dikemas baik dalam botol atau dalam tube, botol dapat dibuat dari gelas tidak bewarna, warna hijau, amber atau biru atau buram dan porselen putih. Botol plastik juga dapat digunakan. Wadah dari gelas buram dan berwarna berguna untuk salep yang mengandung obat yang peka terhadap cahaya. Tube dibuat dari kaleng atau plastik, beberapa diantaranya diberi tambahan kemasan dengan alat bantu khusus bila salep akan digunakan untuk dipakai melalui rektum, mata, vagina, telinga, atau hidung. Tube umumnya diisi dengan bertekanan alat pengisi dari bagian ujung belakang yang terbuka (ujung yang berlawanan dari ujung tutup) dari tube yang kemudian ditutup dengan disegel. Tube salep untuk pemakaian topikal lebih sering dari ukuran 5 sampai 30 gr. Botol salep dapat diisi dalam skala kecil oleh seorang ahli farmasi dengan mengemas sejumlah salep yang sudah ditimbang kedalam botol dengan memakai spatula yang
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K. Asam Benzoat
Asam benzoat, C 7H6O2 (atau C6H5COOH), adalah padatan kristal berwarna putih dan merupakan asam karboksilat aromatik yang aromatik yang paling sederhana. Nama asam ini berasal dari gum benzoin (getah kemenyan), kemenyan), yang dahulu merupakan satu-satunya sumber asam
benzoat. Asam lemah ini beserta garam turunannya digunakan sebagai pengawet pengawet makanan. Asam benzoat adalah prekursor yang penting dalam sintesis banyak bahan-bahan kimia lainnya. Sejarah Asam benzoat pertama kali ditemukan pada abad ke-16. Distilasi kering getah kemenyan pertama kali dideskripsikan oleh
Nostradamus (1556), dan
selanjutnya oleh Alexius Pedemontanus Pedemontanus (1560) dan Blaise de Vigenère (1596). Justus von Liebig dan Friedrich Wöhler berhasil menentukan struktur asam benzoat pada tahun 1832. Mereka juga meneliti bagaimana asam hipurat berhubungan dengan asam benzoat.Pada tahun 1875, Salkowski menemukan bahwa asam benzoat memiliki aktivitas anti jamur.
Produksi Pembuatan secara industri
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Dengan hidrolisis
Sama seperti nitril ataupun amida lainnya, benzonitril dan benzoamida dapat dihidrolisis menjadi asam benzoat ataupun basa konjugatnya dalam keadaan asam maupun basa.
Dari benzaldehida
Disproporsionasi benzaldehida yang diinduksi oleh basa dalam
reaksi
Cannizzaro akan menghasilkan sejumlah asam benzoat dan benzil alkohol dalam jumlah yang sama banyak. Benzil alkohol kemudian dapat dipisahkan dari asam benzoat dengan distilasi.
Dari bromobenzena
Bromobenzena dapat diubah menjadi asam benzoat dengan "karbonasi" zat anatara fenilmagensium bromida: C6H5MgBr + CO2 → C6H5CO2MgBr C6H5CO2MgBr + HCl → C 6H5CO2H + MgBrCl
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L. Asam Salisilat (C7H6O2)
Asam salisilat merupakan turunan dari senyawa aldehid. Senyawa ini juga biasa disebut o-hidroksibensaldehid, o-formilfenol atau 2-formilfenol. Senyawa ini stabil, mudah terbakar dan tidak cocok dengan basa kuat, pereduksi kuat, asam kuat, dan pengoksidasi pengoksidasi kuat. Sifat-sifat fisik dari asam salisilat No.
Penampakan
Tidak berwarna menjadi kuning pada larutan dengan bau kenari pahit
1
Titik lebur
1-2 C
2
Titik didih
197 C
3
Kerapatan
4,2
4
Tekanan uap
1 mmHg pada 33 C
5
Daya ledak
1,146 g/cm
6
Titik nyala
76 C
0
0
Dari hasil penelitian ditetapkan apabila dimakan oleh tikus dengan dosis 520 mg/kg merupakan dosis yang mengakiibatkan kematian 50 % (LD50), dan apabila terkena
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III.
Alat Bahan Alat
Jumlah
Bahan
Buret 50 ml
1 buah
Padatan NaOH 0,1 N
Spatula
1 buah
Padatan Oksalat p.a
Labu takar 100 ml
1 buah
Sampel salep
Corong gelas
1 buah
Fe(NO3)3 1%
Batang pengaduk
2 buah
Indikator pp
Pipet tetes
1 buah
Aquadest
Erlenmeyer 250 ml
2 buah
Larutan Standar Asam Salisilat ?? ppm
Gelas kimia 100 ml
1 buah
Air bebas CO2
Gelas kimia 250 ml
2 buah
Gelas ukur 50 ml
1 buah
Gelas kimia 500 ml
1 buah
Gelas kimia 1 L
1 buah
Hote plate
1 buah
Labu takar 250 ml
1 buah
Pipet volume 25 ml
1 buah
Pipet volume 25 ml
1 buah
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IV.
Cara Kerja
1. Pembakuan NaOH 0,1 N
Menimbang gram oksalat
Menambahkan 3 tetes indicator fenolftalein
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2. Preparasi Sampel
Menimbang 1,0000 gram salep dalam gelas kimia 250 ml
Menambahkan 100 ml aquadest panas 75 oC dan 2 tetes indikator fenolftalein
Menambahkan NaOH 0,1 N sampai timbul warna merah jambu
Memanaskan Memanaskan larutan tersebut sampai suhu sekitar 85 oC
Menambahkan lagi NaOH 0,1 N sampai timbul
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3. Pengukuran
1
2
3
4
•
Mengambil sekitar 16 ml filtrate dari langkah b
•
Memasukannya kedalam labu takar 50 ml
•
Menambahkan 5 ml ferri nitrat 1%
•
Menambahkan aquadest sampai tanda batas
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4. Pembuatan kurva standar
1
2
3
•
Membuat larutan yang mengandung mengandung asam salisilat 5 gram dalam 250 ml
•
Kemudian menyaring larutan tersebut
•
Membuat variasi konsentrasi konsentrasi larutan 20 , 40 , 60 , 80 , 100 ppm
•
4
5
•
Memipet ferri nitrat nitrat kedalam masing-masing labu takar 2,5 ml , 5 ml , 7,5 ml , 10,0 ml , 12,5 ml Menambahkan aquadest hingga tanda batas
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b. Standarisasi larutan standar sekunder NaOH ± 1,000 N
-
Larutan standar primer
: H2C2O4 2H2O
-
Konsentrasi H2C2O4 2H2O
: 0,1000N
-
Volume H2C2O4 2H2O yang dipipet
: 10,00 ml
-
Volume NaOH yang dibutuhkan
: 1. 10,45 ml 2. 10,40 ml Rata-rata = 10,43 ml
-
Reaksi
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Volume Sampel ( ml )
Volume NaOH sebelum
Volume NaOH setelah
pemanasan ( ml )
pemanasan ( ml )
11,30
0,2
25
Volume Sampel ( ml )
Volume NaOH (dua) ( ml )
25
0,1
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510
22,2
0,654
520
21,4
0,670
530
21,2
0,674
540
21,4
0,670
550
22,1
0,655
560
23
0,639
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d. Pengukuran larutan standar dan sampel Konsentrasi Standar
%T
Absorbansi
20
60,0
0,222
40
36,7
0,435
60
22,8
0,642
(ppm)
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PERHITUNGAN
Perhitungan Konsentrasi NaOH
Voksalat x Noksalat = VNaOH x N NaOH 10 ml x 0,1 N = 10,43 10,43 ml x N NaOH N NaOH
= 0,0959 N
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= 27,1111 ppm x 5 = 135,56 ppm 135,56 ppm
= 135,56 mg/L = 0,1356 gram/1 L = 0,01356 gram/100 ml = 0,0136 %
Jadi, kadar asam salisilat dalam sampel adalah 0,0136 %
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VI.
PEMBAHASAN
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Larutan sampel yang sudah dalam keadaan dingin selanjutnya diencerkan ke
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Sampel salep “Pagoda” memiliki kandungan asam salisilat dan asam benzoat, jadi
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DAFTAR PUSTAKA
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