27 Jul

TITRASI ARGENTOMETRI

MAKALAH ANALISIS FISIKOKIMIA

 TITRASI ARGENTOMETRI 

DI SUSUN OLEH :

AGUS AFRIANTO

 1141420010

  

LABORATURIUM KIMIA

JURUSAN TEKNIK KIMIA

FAKULTAS TEKNIK

INSTITUT TEKNOLOGI INDONESIA

SERPONG, TANGSEL, BANTEN

2016

 

 KATA PENGANTAR

 

Puji syukur kehadirat Tuhan Yang Maha Esa yang telah memberikan saya  berbagai macam nikmat, sehingga aktivitas hidup yang saya jalani akan selalu membawa keberkahan, baik kehidupan di alam dunia ini maupun kehidupan akhirat kelak, sehingga semua cita-cita serta harapan yang ingin saya capai menjadi lebih mudah dan penuh manfaat.

Terima kasih sebelum dan sesudahnya saya ucapkan kepada dosen serta teman-teman sekalian yang telah membantu, baik bantuan berupa moril maupun materil, sehingga makalah ini dapat terselesaikan dalam waktu yang telah ditentukan.

Saya menyadari di dalam penyusunan makalah ini masih jauh dari kesempurnaan serta banyak kekurangannya baik dari segi tata bahasa maupun dalam hal yangpengkonsolidasian kepada dosen serta teman-teman sekalian, untuk itu  besar harapan saya jika ada kritik maupun saran dari dosen maupun teman-teman sekalian yang membangun untuk lebih menyempurnakan makalah-makalah saya.

Harapan yang paling besar dari penyusunan makalah ini ialah mudah-mudahan apa yang saya susun memberikan manfaat baik untuk pribadi, teman-teman, serta orang lain yang ingin mengambil atau menyempurnakan lagi atau mengambil hikmah dari judul ini (argentometri) sebagai tambahan dalam referensi yang telah ada.

 

 

Serpong, 22 Juli 2016

        Penyusun

 

 

DAFTAR ISI

BAB I

PENDAHULUAN

1.1  Latar Belakang

Titrasi pengendapan merupakan titrasi yang melibatkan pembentukan endapan dari garam yang tidak mudah larut antara titran dan analit. Hal dasar yang diperlukan dari titrasi  jenis ini adalah pencapaian keseimbangan pembentukan yang cepat setiap kali titran ditambahkan pada analit, tidak adanya interferensi yang mengganggu titrasi, dan titik akhir titrasi yang mudah diamati.

Salah satu jenis titrasi pengendapan yang sudah lama dikenal adalah melibatkan reaksi pengendapan antara ion halida ( Cl-, I-, Br- ) dengan ion perak Ag+. Titrasi ini biasanya disebut sebagai argentometri, yaitu titrasi penentuan analit yang berupa ion halida dengan menggunakan larutan standar perak nitrat AgNO3.

Dasar titrasi argentometri adalah pembentukan endapan yang tidak mudah larut antara titrant dan analit. Sebagai contoh yang banyak dipakai adalah titrasi penentuan NaCl dimana ion Ag+ dari titran akan bereaksi dengan ion Cl-dari analit membentuk garam yang tidak mudah larut.

 

1.2  Rumusan Masalah

  1. Apa yang dimaksud dengan titrasi argentometri ?
  2. Apa saja metode yang ada dalam titrasi argentometri ?
  3. Apa saja kelebihan dan kekurangan titrasi argentometri ?
  4. Apa saja faktor-faktor yang Mempengaruhi Pengendapan ?
  5. Bagaimana pembentukan Endapan Berwarna ?
  6. Apa saja faktor-faktor yang mempengaruhi kelarutan ?
  7. Mengetahui Contoh penelitiandari Titrasi Argentometri.

 

1.3  Tujuan Penulisan

  1. Mampu memahami titrasi dalam argentometri
  2. Mampu memahami titrasi argentometri berdasarkan metode yang ada
  3. Mampu mengetahui kelebihan dan kekurangan titrasi argentometri
  4. Mampu mengetahui faktor-faktor yang Mempengaruhi Pengendapan
  5. Mampu mengetahui pembentukan Endapan Berwarna
  6. Mampu mengetahui faktor-faktor yang mempengaruhi kelarutan

 

 

BAB II

PEMBAHASAN

2.1 Pengertian

Argentometri berasal dari bahasa latin Argentum, yang berarti perak. Argentometri adalah titrasi pengendapan sample yang dianalisis dengan menggunakan ion perak. Biasanya, ion-ion yang ditentukan dalam titrasi ini adalah ion halida (Cl-, Br-, I-), atau untuk lebih jelas yang di maksud pada titrasi argentometri yaitu suatu analisa volumetri yang didasarkan pada reaksi  pengendapan dengan AgNO3 sebagai larutan standar. Penentuan khlor, brom dapat dilakukan dengan mentitrasi halogenida tersebut dengan AgNO3 dengan menggunakan indikator kalium khromat, ion khromat akan bereaksi dengan ion perak bila seluruh Cl telah diendapkan secara kuantitatif oleh ion Ag sehingga titik akhir  titrasi ditandainya dengan terbentuknya endapan merah dari Ag2CrO4. Titrasi pengendapan adalah golongan titrasi dimana hasil tirasinya merupakan endapan atau garam yang sukar larut.Prinsip dasarnya adalah reaksi pengendapan yang cepat mencapai kesetimbangan dan untuk mendapatkan hasil pada titik akhir titrasi maka perlu di tambahkan indikator. Titrasi yang melibatkan reaksi pengendapan hampir tak sebanyak titrasi yang melibatkan reaksi asam basa dalam analisis titrimetri. Presipitimetri adalah cara titrasi dimana terjadi endapan.

Contoh : AgNO3+ NaCl → AgCl + NaNO3

 

Ada 3 macam  metode argentometri:

2.1.1 Metode Mohr (pembentukan endapan berwarna)

Titrasi ini ditandai dengan terbentuknya andapan berwarna  dan titrasi berlangsung dengan AgNO3. Kegunaan metoda ini untuk menentukan konsentrasi klorida yang tidak bisa digunakan untuk menentukan konsentrasi iodida dan tiosianat. Metode Mohr dapat digunakan untuk menetapkan kadar klorida dan bromida dalam suasana netral dengan larutan standar AgNO3 dan penambahan K2CrO4 sebagai indikator. Titrasi dengan cara ini harus dilakukan dalam suasana netral atau dengan sedikit alkalis (basa), pH 6,5 – 9,0. Dalam suasana asam, perak kromat larut karena terbentuk dikromat dan dalam suasana basa akan terbentuk endapan perak hidroksida. Reaksi yang terjadi adalah :

 

Asam : 2CrO42- + 2H ↔ CrO7 2- + H2O

Basa  : 2 Ag+ + 2 OH ↔ 2 AgOH

2AgOH ↔ Ag2O + H2O

Kelemahan Titrasi Mohr :

Kemungkinan terjadi kelebihan titran yang menyebabkan indikator mengendap sebelum titik ekivalen tercapai yang mengakibatkan titik akhir titrasi jadi tidak tajam. Sebagai solusi dilakukan pengadukan secara cepat.

Prinsip penetapannya larutan klorida atau bromida dalam suasana netral atau agak alkalis dititrasi dengan larutan perak nitrat menggunakan indikator kromat. Apabila ion klorida atau bromida telah habis diendapkan oleh ion perak, maka ion kromat akan bereaksi dengan ion perak membentuk endapan perak kromat yang berwarna coklat merah sebagai titik akhir titrasi. Larutan standarnya yaitu larutan perak nitrat menggunakan indikator larutan kalium kromat.

Reaksinya:

NaCl + AgNO₃ –> AgCl (endapan) + NaNO₃

2AgNO₃ + K₂CrO₄ (endapan) + 2KNO₃

Titik akhir titrasi terjadi perubahan warna pada endapan menjadi merah coklat (AgCrO₄). Titrasi harus dilakukan pada suasana netral atau sedikit alkalis karena:

  1. Dalam suasana asam endapan AgCrO₄akan larut karena terbentuk perak dikromat (Ag₂Cr₂O₇)
  2. Dalam suasana basa perak nitrat akan bereaksi dengan ion hidroksida membentuk endapan perak hidroksida

AgNO₃ + NaOH –> AgOH (endapan) + NaNO₃

Gangguan pada titrasi ini antara lain disebabkan oleh:

  1. Ion yang akan mengendap lebih dulu dari AgCl, misalnya: F, Br, CNSˉ
  2. Ion yang membentuk kompleks dengan Ag⁺, misalnya: CNˉ, NH₃diatas Ph 7
  3. Ion yang membentuk kompleks dengan Clˉ, misalnya: Hg²⁺
  4. Kation yang mengendapkan kromat, misalnya: Ba²⁺

Hal yang harus dihindari: cahaya matahari langsung atau sinar neon karena larutan perak nitrat peka terhadap cahaya (reduksi fotokimia).

 

2.1.2 Model Volhard (Penentu zat warna yang mudah larut).

Metode Volhard pertama kali diperkenalkan oleh Jacobus Volhard, ahli kimia dari Jerman pada tahun 1874. Dengan metode ini, larutan standar AgNO3 berlebih ditambahkan ke dalam larutan yang mengandung ion halogen (misalnya Cl-). Kelebihan ion Ag+ dalam suasana asam dititrasi dengan standar garam tiosianat (KSCN atau NH4SCN) menggunakan indikator larutan Fe3+. Sampai titik ekivalen, terjadi reaksi antara titran dan Ag+ membentuk endapan putih. Kelebihan titran menyebabkan reaksi dengan indikator membentuk senyawa kompleks tiosianato ferrat (III) yang berwarna merah.

Metoda ini ditandai dengan terbentuknya kompleks berwarna dan didasarkan pada pengendapan perak tiosianat dalam AgNOdengan menggunakan besi (III). Berikut reasksi yang terjadi pada metoda Volhard :

Ag+  + SCN    →    AgSCN

Fe3+ + SCN     →    Fe(SCN)2+

Titrasi volhard dilakukan dalam suasana asam. Jika dalam suasana netral, indikator akan terhidrolisa.

Fe3+ + OH     →      Fe(OH)3

Fe3+ + H2O     →      Fe(OH)3 + H+

Metode ini digunakan dalam penentuan ion Cl, Br, dan I dengan penambahan larutan standar AgNO3. Indikator yang dipakai adalah Fe3+ dengan titran NH4CNS, untuk menentralkan kadar garam perak dengan titrasi kembali setelah ditambah larutan standar berlebih. Kelebihan AgNO3 dititrasi dengan larutan standar KCNS, sedangkan indikator yang digunakan adalah ion Fe3+ dimana kelebihan larutan KCNS akan diikat oleh ion Fe3+membentuk warna merah darah dari FeSCN.

Kegunaan nya untuk penetapan kadar perak atau garamnya, penetapan kadar halida (Cl, Br, I). Prinsip penetapan kadar perak ditetapkan dengan cara titrasi langsung. Larutan standarnya larutan tiosianat (KCSN atau NH₄CNS). Indikator menggunakan besi (III) amonium sulfat. Titik akhir titrasinya terbentuk kompleks besi (III) tiosianat Fe(CNS)²⁺yang larut, berwarna merah.

Reaksinya:

Ag⁺ + NH₄CNS–> AgCNS (endapan putih) + NH₄⁺

Jika Ag⁺ sudah habis, maka kelebihan 1 tetes NH₄CNS + Fe³⁺ –> Fe(CNS)²⁺ + NH₄⁺

2.1.3 Metode Fajans (Indikator Absorbsi)

Titrasi argentometri dengan cara fajans adalah sama seperti pada cara Mohr, hanya terdapat perbedaan pada jenis indikator yang digunakan. Indikator yang digunakan dalam cara ini adalah indikator absorbsi seperti cosine atau fluonescein menurut macam anion yang diendapkan oleh Ag+. Titrannya adalah AgNO3  hingga suspensi violet menjadi merah. pH tergantung pada macam anion dan indikator yang dipakai.

Indikator absorbsi adalah zat yang dapat diserap oleh permukaan endapan dan menyebabkan timbulnya warna. Pengendapan ini dapat diatur agar terjadi pada titik ekuivalen antara lain dengan memilih macam indikator yang dipakai dan pH. Sebelum titik ekuivalen tercapai, ion Cl berada dalam lapisan primer dan setelah tercapai ekuivalen maka kelebihan sedikit AgNO3 menyebabkan ion Cl akan digantikan oleh Ag+ sehingga ion Clakan berada pada lapisan sekunder.

Pembentukan Endapan Berwarna Seperti sistem asam, basa dapat digunakan sebagai suatu indikator untuk titrasi asam-basa. Pembentukan suatu endapan lain dapat digunakan untuk menyatakan lengkapnya suatu titrasi pengendapan. Dalam hal ini terjadi pula pada titrasi Mohr, dari klorida dengan ion perak dalam mana digunakan ion kromat sebagai indikator. Pemunculan yang permanen dan dini dari endapan perak kromat yang kemerahan itu diambil sebagai titik akhir (TE). Titrasi Mohr terbatas untuk larutan dengan perak dengan pH antara 6,0 . 10,0. Dalam larutan asam konsentrasi ion kromat akan sangat dikurangi karena H2CrO4 hanya terionisasi sedikit sekali. Lagi pula dengan hidrogen kromat berada dalam kesetimbangan dengan dikromat terjadi reaksi :

2H+ + 2CrO4    ↔      2H2CrO4     ↔     Cr2O72- + 2H2O

Proses argentometri termasuk dalam titrasi yang menghasilkan endapan dan pembentukan ion kompleks. Proses argentometri menggunakan AgNO3 sebagai larutan standar. Proses ini biasanya digunakan untuk menentukan garam-garam dari halogen dan sianida. Karena kedua jenis garam ini dapat membentuk endapan atau senyawa kompleks dengan ion Ag+ sesuai dengan persamaan reaksi sebagai berikut :

NaCl + Ag+ → AgCl ↓ + Na+

KCN + Ag+ → AgCl ↓ + K+

KCN + AgCN ↓ → K [Ag(CN)2 ]

Karena AgNO3 mempunyai kemurnian yang tinggi maka garam tersebut dapat digunakan sebagai larutan standar primer. Dalam titrasi argentometri terhadap ion CNtercapai untuk garam kompleks K [Ag(CN)2 ] karena proper tersebut dikemukakan pertama kali oleh Lieberg, cara ini tidak dapat dilakukan dalam suasana amoniatial karena garam kompleks dalam larutan akan larut menjadi ion komplek diamilum.

Syarat pH untuk titrasi fajans dengan indikator eosin yaitu : tidak terlalu rendah, karena kebanyakan indikator adsorbsi bersifat asam lemah yang tidak dapat dipakai dalam larutan yang terlalu asam. Tapi tidak semua indikator seperti itu. Ada beberapa indikator adsorbsi ”kationik” yaitu bersifat basa lemah sehinggga baik untuk dititrasi dalam suasana asam.

Contoh – contoh indikator Adsorbsi :

o   Ortholoro              : Syarat larutan netral pH 0,02 M

o   Eosin                     : Syarat pH 2 – 8 dari pink ke merah

o   Avorestein             : Syarat pH 7 – 8

o   Lembayung metil  : Syarat larutan harus asam

 

2.2 Metode Titrasi Argentometri

Pada umumnya titrasi argentometri dapat dibedakan atas tiga metode berdasarkan indicator yang dipakai dalam titrasi tersebut, yaitu:

2.2.1 Indikator kalium kromatografi K2CrO4

Titrasi argentometri dengan menggunakan indicator ini biasa disebut sebagai argentoetri dengan metode Mohr. Ini merupakan titrasi langsung titrant dengan menggunakan larutan standar AgNO3. Titik akhir titrasi diamati dengan terbentuknya endapan Ag2CrO4 yang brwarna kecoklatan.

  1. Indikator Fe3+

Titrasi argentometri dengan indicator ini disebut sebagai titrasi argentometri dengan metode volhard. Titrasi ini merupakan titrasi tidak langsung dimana larutan standar AgNO3 ditambahkan secara berlebih dan kelebihan ini dititrasi dengan larutan standart SCN-.

  1. Indikator adsorbsi

Titrasi argentometri dengan indicator adsorbsi disebut sebagai titrasi argentometri dengan menggunakan metode Fajans. Indikator yang dipakai adalah indicator adsorbsi. Dimana indicator ini akan berubah warnanya jika teradsorbsi pada permukaan endapan.

Selain menggunakan teknik diatas maka titrasi argentometri juga dapat dilakukan dengan menggunakan indicator yang berupa indicator electrode. Plot antara Esel dengan jumlah titran akan dapat diperoleh kurva titrasi dengan grafik ini maka kita nantinya dapat menentukan titik akhir titrasi

  1. Indikator Adsorbsi Pada Titrasi Argentometri

Pada titrasi argentometri dengan metode Fajans, Jika AgNO3 ditambahkan pada larutan NaCl yang mengandung flourescein maka titik akhir titrasi akan diamati dengan perubahan warna dari kuning cerah ke merah muda. Warna endapan yang terlihat akan tampak berwarna sedangkan larutannya tampak tidak berwarna hal ini disebabkan adanya indikator adsorbsi yang teradsorb pada permukaan endapan AgCl. Warna dari endapan akan termodifikasi saat indikator teradsorbsi pada permukaan endapan. Reaksi adsorbsi ini dapat dilihat dengan contoh indikator yang bermuatan negatif seperti flouroscein.

Misalnya flouroscein dilambangkan sebagai Fl-. Pada saat larutan berada pada kelebihan ion Cl- yaitu saat titrasi belum mencapai titik ekuivalen maka indikator FL- tidak teradsorbsi pada permukaan endapan, hal ini disebabkan permukaan endapan masih dikelilingi oleh ion Cl- sehingga antara endapan dan FL- saling tolak-menolak

(AgCl)Cl-  + FL- -> tidak ada adsorbsi

akan tetapi begitu terjadi titik ekuivalen maka dengan penambahan sejumlah kecil ion Ag+ untuk mendapatkan titik akhir titrasi maka sekarang dalam larutan terdapat kelebihan jumlah ion Ag+ sehingga pada permukaan endapan sekarang terdapat ion Ag+ dengan demikian FL- akan teradsorbsi melalui gaya elektrostatis pada permukaan endapan sehingga terjadilah perubahan warna indikator.

(AgCl)Ag+  + FL- -> (AgCl)(AgFL) ada reaksi dan indikator teradsorbsi

Semua indikator adsorbsi bersifat ionik sehingga dapat teradsorbsi pada permukaan endapan. Indikator adsorbsi yang dipakai untuk titrasi sulfat dengan ion barium dalam pelarut aseton biasa dipergunakan thorin atau alizarin.

Indikator adsorbsi memiliki keunggulan memiliki eror dalam penentuan titik akhir titrasi yang kecil, dan perubahan warna pada saat teradsorbsi umumnya dapat terlihat dengan jelas. Indikator adsorbsi baik dipergunakan untuk titrasi penendapan dimana endapan yang dihasilkan memiliki luas permukaan yang besar dengan demikian indikator dapat teradsorbsi dengan baik.

2.3 Kelebihan dan kekurangan titrasi argentometri

Titrasi pengendapan adalah anilisis titrimetri berdasarkan proses terbentuknya endapan antara reagen dengan analit dan reagen dengan indikator dengan warna yang berbeda. Hal dasar yang diperlukan dari titrasi pengendapan adalah pencapaian keseimbangan pembentukan yang cepat setiap kali titran ditambahkan pada analit, tidak adanya interferensi yang menggangu titrasi, tetapi ditambah dengan titik akhir titrasi yang mudah diamati.

Adapun dalam titrasi pengendapan terdapat kelebihan dan kekurangan yang signifikan, diantaranya :

–         Jumlah metode titrasi pengendapan tidak sebanyak titrasi asam-basa ataupun titrasi reduksi-             oksidasi (redoks).

–          Kesulitan dalam mencari indikator yang sesuai dalam titrasi pengendapan.

Komposisi endapan pada titrasi pengendapan seringkali tidak diketahui pasti, terutama jika terdapat efek kopresipitasi.

2.4  Faktor-faktor yang Mempengaruhi Pengendapan

Keberhasilan proses pengendapan sangat dipengaruhi oleh berbagai macam faktor diantaranya

2.4.1 Temperatur

Kelarutan semakin meningkat dengan naiknya suhu, jadi dengan meningkatnya suhu maka pembentukan endapan akan berkurang disebabkan banyak endapan yang berada pada larutannya.

2.4.2     Pemilihan pelarut

Garam anorganik mudah larut dalam air dibandingkan dengan pelarut organik seperti alkohol atau asam asetat.  Perbedaan kelarutan suatu zat dalam pelarut organik dapat dipergunakan untuk memisahkan campuran antara dua zat. Setiap pelarut memiliki kapasitas yang berbeda dalam melarutkan suatau zat,  begitu juga dengan zat yang berbeda memiliki kelarutan yang berbeda pada pelarut tertentu.

2.4.3 Efek ion-sekutu

Kelarutan endapan akan berkurang jika dilarutkan dalam larutan yang mengandung ion sejenis dibandingkan dalam air saja. Sebagai contoh kelarutan Fe(OH)3 akan menjadi kecil jika kita larutkan dalam larutan NH4OH dibanding dengan kita melarutkannya dalam air,

Fe(OH)3           Fe3+ + 3OH

NH4OH            NH4+ + OH

Hal ini disebabkan dalam larutan NH4OH sudah terdapat ion sejenis yaitu OH.Sehingga akan mengurangi konsentrasi Fe(OH)3 yang akan terlarut.  Efek ini biasanya dipakai untuk mencuci endapan dalam metode gravimetric

2.4.4 Evek aktifitas

Kelarutan AgCl dan BaSO4  dalam larutan KNO3

Terlihat bahwa dalam 0.010 M KNO3, kelartan dari AgCl meningkat dari nilai dalam air sekitar 12 %, dan di dalam BaSO4 sekitar 70 % .

Molaritas merupakan aktivitas yang terjadi dalam larutan yang sangat encer, jika konsentrasi larutan makin pekat maka koefisien aktivitas (f) menurun cepat, akibat gaya tarik lebih besar dari yang terjadi antara ion yang berbeda muatan. Efektivitas ion-ion (pada kondisi setimbang) juga menurun dan penambahan endapan harus dilakukan agar aktivitas kembali kesemula.

2.4.5 Evek pH

Kelarutan endapan garam yang mengandung anion dari asam lemah dipengaruhi oleh pH, hal ini disebabkan karena penggabungan proton dengan anion endapannya. Misalnya endapan AgI akan semakin larut dengan adanya kenaikan pH disebabkan H+ akan bergabung dengan I membentuk HI.

AgI                   Ag+  + I

H3O+               H+ + H2O

2.4.6     Evek hidrolisis

Jika garam dari asam lemah dilarutkan dalam air maka akan dihasilkan perubahan konsentrasi H+. Dimana hal ini akan menyebabkan kation garam tersebut mengalami hidrolisis dan hal ini akan meningkatkan kelarutan garam tersebut

2.4.6     Hidrolisis Metal

Ketika Sebuah Hidroksida Metal terurai dalam air,disituasi ini anok dengan pembahasan efek hidrolisis, dimana pH dapat berubah secara nyata.

2.4.7 Efek pembentukan kompleks

Pengaruh ini dapat kita jadikan sebagai dasar untuk memahami titrasi argentometri dan gravimetri.

2.5      Pembentukan Endapan Berwarna

Seperti sistem asam, basa dapat digunakan sebagai suatu indicator untuk titrasi asam-basa. Pembentukan suatu endapan lain dapat digunakan untuk menyatakan lengkapnya suatu titrasi pengendapan. Dalam hal ini terjadi pula pada titrasi Mohr, dari klorida dengan ion perak dalam mana digunakan ion kromat sebagai indikator. Pemunculan yang permanen dan dini dari endapan perak kromat yang kemerahan itu diambil sebagai titik akhir (TE).

Titrasi Mohr terbatas untuk larutan dengan perak dengan pH antara 6,0 – 10,0. Dalam larutan asam konsentrasi ion kromat akan sangat dikurangi karena HCrO4- hanya terionisasi sedikit sekali. Lagi pula dengan hidrogen kromat berada dalam kesetimbangan dengan dikromat terjadi reaksi :

2H+ + 2CrO4

– ↔ 2HCrO4 ↔ Cr2O7

2- + 2H2O

Mengecilnya konsentrasi ion kromat akan menyebabkan perlunya menambah ion perak dengan sangat berlebih untuk mengendapkan ion kromat dan karenanya menimbulkan galat yang besar. Pada umumnya garam dikromat cukup dapat larut. Proses argentometri termasuk dalam titrasi yang menghasilkan endapan dan pembentukan ion kompleks. Proses argentometri menggunakan AgNO3 sebagai larutan standar. Proses ini biasanya digunakan untuk menentukan garam-garam dari halogen dan sianida. Karena kedua jenis garam ini dapat membentuk endapan atau senyawa kompleks dengan ion Ag+ sesuai dengan persamaan reaksi sebagai berikut :

NaCL + Ag+ → AgCl ↓ + Na+

KCN + Ag+ → AgCl ↓ + K+

KCN + AgCN ↓ → K [Ag(CN)2 ]

Karena AgNO3 mempunyai kemurnian yang tinggi maka garam tersebut dapat digunakan sebagai larutan standar primer. Dalam titrasi argentometri terhadap ion CN- tercapai untuk garam kompleks K [Ag(CN)2 ] karena propes tersebut dikemukakan pertama kali oleh Lieberg, cara ini tidak dapat dilakukan dalam suasana amoniatial karena garam kompleks dalam larutan akan larut menjadi ion komplek diamilum.

2.6      Faktor – Faktor Yang Mempengaruhi Kelarutan

Pengendapan merupakan metode yang paling baik pada anlisis gravimetri. Kita akan memperhatikan faktor-faktor yang mempengaruhi kelarutan. Parameter-parameter yang penting adalah temperatur, sifat pelarut, adanya ion-ion pengotor, pH, hidrolisis, pengaruh kompleks, dan lain-lain .

Kelarutan bertambah dengan naiknya temperatur. Kadangkala endapan yang baik terbentuk pada larutan panas, tetapi jangan dilakukan penyaringan terhadap larutan panas karena pengendapan dipengaruhi oleh faktor temperatur. Garam-garam anorganik lebih larut dalam air. Berkurangnya kelarutan di dalam pelarut organik dapat digunakan sebagai dasar pemisahan dua zat. Kelarutan endapan dalam air berkurang jika lanitan tersebut mengandung satu dari ion-ion penyusun endapan, sebab pembatasan Ks.p(konstanta hasil kali kelarutan). Baik kation atau anion yang ditambahkan, mengurangi konsentrasi ion penyusun endapan sehingga endapan garam bertambah. Pada analisis kuantitatif, ion sejenis ini digunakan untuk mencuci larutan selama penyaringan.

Beberapa endapan bertambah kelarutannya bila dalam lanitan terdapat garam-garam yang berbeda dengan endapan. Hal ini disebut sebagai efek garam netral atau efek aktivitas. Semakin kecil koefesien aktivitas dari dua buah ion, semakin besar hasil kali konsentrasi molar ion-ion yang dihasilkan. Kelarutan garam dari asam lemah tergantung pada pH larutan. Jika garam dari asam lemah dilarutkan dalam air, akan menghasilkan perubahan (H). Kation dari spesies garam mengalami hidrolisis sehingga menambah kelarutannya .

Kelarutan garam yang sedikit larut merupakan fungsi konsentrasi zat lain yang membentuk kompleks dengan kation garam tersebut. Beberapa endapan membentuk kompleks yang larut dengan ion pengendap itu sendiri. Mula-mula kelarutan berkurang (disebabkan ion sejenis) sampai melalui minuman. Kemudian bertambah akibat adanya reaksi kompleksasi. Reaksi yang menghasilkan endapan dapat dimanfaatkan untuk analisis secara titrasi jika reaksinya berlangsung cepat, dan kuantitatif serta titik akhir dapat dideteksi. Beberapa reaksi pengendapan berlangsung lambat dan mengalamikeadaan lewat jenuh. Tidak seperti gravimetri, titrasi pengendapan tidak dapat menunggu sampai pengendapan berlangsung sempurna. Hal yang penting juga adalah hasil kali kelarutan (KSP) harus cukup kecil sehingga pengendapan bersifat kuantitatif dalam batas kesalahan eksperimen. Reaksi samping tidak boleh terjadi, demikian juga kopresipitasi. Keterbatasan utama pemakaian cara ini disebabkan sedikit sekali indikator yang sesuai. Semua jenis reaksi diklasifikasi berdasarkan tipe indikator yang digunakan untuk melihat titik akhir.

2.7      Contoh Penelitian

Pada percobaan ini akan dilakukan analisis senyawa turunan xanthin yakni theobromin yang selanjutnya akan ditentukan kadarnya dengan menggunakan metode argentometri. Argentometri merupakan suatu metode penentuan kadar dimana theobromin akan membentuk endapan dengan larutan perak nitrat dalam suasana basa karena mempunyai atom hidrogen yang dapat dilepaskan.

Analisis senyawa theobromin ini dianggap penting khususnya bagi mahasiswa farmasi karena sebagaimana diketahui senyawa turunan xanthin diketahui memiliki beberapa aktivitas farmakologis diantaranya sebagai bronkodilator yaitu senyawa yang dapat melebarkan bronkus yang biasa digunakan sebagai obat asma. Meskipun ada efek samping seperti penekanan jantung dan sistem saraf pusat tetapi itulah pentingnnya dilakukan analisis untuk melihat bagaimana kualitas mutu dari sediaan yang dibuat.

Derivat xantin terdiri dari kofein, theofilin dan teobromin ialah alkaloid yang terdapat dalam tumbuhan. Sejak dahulu ekstrak tumbuh-tumbuhan ini digunakan sebagai minuman. Kofein terdapat dalam kopi yang didapat dari biji Coffea arabica. Teh dari daun Theasinensis mengandung kofein dan teofilin. Cocoa yang didapat dari biji Theobroma cacaomengandung kofein dan teobromin. Penelitian membuktikan bahwa kofein berefek stimulasi. Inilah daya tarik minuman yang mengandung kofein. Kemudian ternyata belum ada senyawa sintetik yang mempunyai keunggulan terapi seperti senyawa alam. Ketiganya merupakan derivat xantin yang mengandung gugus metil. Xantin sendiri ialah dioksipurin yang mempunyai struktur mirip dengan asam urat. Kofein ialah 1,3,7-trimetilxantin; teofilin ialah 1,3-dimetilxantin dan teobromin ialah 3,7-dimetilxantin (1).

Teofilin, kofein dan teobromin mempunyai efek farmakologi yang sama yang bermanfaat secara klinis. Obat-obat ini menyebabkan relaksasi otot polos, terutama otot polos bronkus, merangsang SSP, otot jantung, dan meningkatkan dieresis, teobromin tidak bermanfaat secara klinis karena efek farmakologinya rendah (2).

Xantin merangsang SSP, menimbulkan dieresis, merangsang otot jantung, dan merelaksasi otot polos terutama bronkus (2).

Xantin merupakan alkaloid yang bersifat basa lemah, biasanya diberikan dalam bentuk garam rangkap. Untuk pemberian oral dapat diberikan dalam bentuk basa bebas atau bentuk garam, sedangkan untuk pemberian parenteral perlu sediaan dalam bentuk garam (2).

Kofein, disebut juga tein, merupakan Kristal putih yang larut dalam air dengan perbandingan 1:46. Teofilin berbentuk Kristal putih, pahit dan sedikit larut dalam air (3).

Senyawa xantin merupakan basa lemah dengan pKb antara 13 sampai 14. Teofilin dan teobromin merupakan asam lemah dengan pKa 8,6 dan 9,9. Kofein tidak bersifat asam karena tidak mempunyai atom hidrogen yang dapat dilepaskan sehingga kofein merupakan basa yang sangat lemah dan garamnya mudah terurai oleh air, karenanya kofein dapat disari dari larutan asam atau basa (lebih mudah dari larutan basa) dengan kloroform. Tetapi kofein mudah terurai oleh basa kuat, sehingga larutan dalam basa harus segera disari (3).

Analisis kimia farmasi kuantitatif dapat didefinisikan sebagai aplikasi prosedur kimia analisis kuantitatif terhadap bahan-bahan yang dipakai dalam bidang farmasi terutama dalam menentukan kadar dan mutu dari obat-obatan dan senyawa-senyawa kimia yang tercantum dalam Farmakope-Farmakope serta buku-buku resmi lainnya seperti formularium-formularium (4).

Teobromin dan teofilin dengan perak nitrat membentuk endapan dalam suasana basa. Sementara itu, kofein tidak bereaksi dengan perak karena tidak mempunyai atom hidrogen yang dapat dilepas (5).

 Titrasi pengendapan didasarkan atas terjadinya penendapan kuantitatif, yang dilakukan dengan penambahan larutan pengukur yang diketahui kadarnya pada larutan senyawa yang hendak ditentukan, titik akhir titrasi tercapai bila semua bagian titran sudah membentuk endapan (6).

Pada percobaan ini dilakukan analisis kuantitatif salah satu senyawa turunan xanthin yakni theobromin dengan menggunakan metode argentometri. Awalnya sampel theobromin yang ingin dipakai harusnya dari suatu sediaan farmasi misalnya tablet yang mengandung senyawa theobromin, namun karena ketidak patuhan praktikan sehingga digunakan theobromin murni saja dan perhitungan kadarnya pun sederhana.

Telah diketahui bahwa analisa ini cukup penting diketahui mengingat senyawa turunan xanthin memiliki efek farmakologi yang bermanfaat secara klinis dimana dapat menyebabkan relaksasi otot polos, khususnya otot polos bronkus, merangsang sistem saraf pusat, otot jantung dan meningkatkan dieresis, meskipun dari ketiga turunan xanthin lainnya seperti theofilin dan kofein, theobrominlah yang memiliki efek farmakologi yang rendah dibandingkan keduanya.

Theobromin dianalisis dengan metode argentometri yang merupakan salah satu metode titrasi pengendapan dimana titrasi ini merupakan titrasi yang melibatkan pembentukan endapan dari garam yang tidak mudah larut antara titran dan analit serta hal dasar yang diperlukan dari titrasi jenis ini adalah pencapaian keseimbangan pembentukan yang cepat setiap kali titran ditambahkan pada analit, tidak adanya interferensi yang mengganggu titrasi dan titik akhir titrasi yang mudah diamati.

Prinsip percobaan ini yaitu theobromin membentuk endapan dengan larutan perak nitrat dalam suasana basa dengan melepaskan gugus H.

Hal pertama  yang dilakukan dalam percobaan ini adalah menimbang sampel theobromin murni sebanyak 100 mg, kemudian dilarutkan dalam aquadest sebanyak 50 ml dan ditambahkan fenol merah 0,1% sebanyak 1 ml dan H2SO4 0,8161 N sebanyak 4 ml. Fenol merah digunakan sebagai indikator dan menunjukkan perubahan warna menjadi merah, kemudian ditambahkan H2SO4 sebagai pereaksi. Selanjutnya, larutan tersebut dididihkan selama 15 menit, supaya theobromin benar-benar melarut sempurna dan didinginkan kembali hingga suhu 400C. Setelah itu, ditambahkan NaOH 1 N hingga berwarna merah kebiruan tetapi dalam percobaan hingga 5 ml NaOH ditambahkan tidak ada perubahan yakni tetap berwarna merah. Kemudian, ditambahkan H2SO4 0,8161 N tetes demi tetes hingga 7 ml juga tidak ada perubahan, padahal diharapkan dari warna merah kebiruan menjadi kuning. Setelah itu, ditambahkan larutan AgNO3 0,1 N sebanyak 5 ml dan dititrasi dengan NaOH 0,1 N sampai merah kebiruan, tetapi tetap tidak berubah warna.

Jadi, dari data pengamatan didapatkan bahwa terjadi kesalahan, dimana seharusnya titik akhir titrasi dicapai dengan terjadinya perubahan warna dari kuning menjadi merah kebiruan. Hal ini bias disebabkan karena kesalahan-kesalahan didalam praktikum misalnya bahan yang digunakan sudah tidak bagus, konsentrasi bahan yang digunakan tidak cocok untuk memperoleh titik akhir, ketidaktelitian praktikan dan lain sebagainya.Volume titrasi yang didapatkan yaitu 17 ml dan setelah dihitung kadar theobromin yang diperoleh dari metode argentometri ini adalah sebanyak 216,24 gram.

 

 

BAB III

PENUTUP

 

3.1  Kesimpulan

Titrasi AgNO3 dan NaCl merupakan titrasi dengan Metode Mohr dan Titrasi sampel termasuk dalam Metode Fajans karena sampel mengandung ion I-.Argentometri adalah titrasi pengendapan dengan larutan standar AgNO3.Ada 3 metode argentometri yaitu metode Mohr, Volhard, Vajans. Pada titrasi argentometri, zat pemeriksaan yang telah dibubuhi indikator dicampur dengan larutan standar garam perak nitrat (AgNO3).Dengan mengukur volume larutan standar yang digunakan sehingga seluruh ion Ag+ dapat tepat diendapkan, kadar garam dalam larutan pemeriksaan dapat ditentukan.

 

DAFTAR PUSTAKA

 

Harjadi W, (1993), Ilmu Kimia Analitik Dasar, PT Gramedia, Jakarta.

Khopkar, (1990), Konsep Dasar Kimia Analitik, Universitas Indonesia,

Jakarta. Day RA. Jr dan Al Underwood.1992. Analisis Kimia Kuantitatif. Edisi Kelima. Jakarta : Erlangga

Harizul, Rivai. 1995. Asas Pemeriksaan Kimia. Jakarta : UI Press

  1. L. Underwood. 1989. Analisa Kuantitatif Edisi Keempat. Jakarta : Erlangga
    Day RA. Jr dan Al Underwood.1992. Analisis Kimia Kuantitatif: Edisi Kelima. Jakarta : Erlangga

 

 

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