prof. dr. sudibyo martono, m.s., apt
DESCRIPTION
Kimia Analisis II. Prof. Dr. Sudibyo Martono, M.S., Apt. Kimia Analisis II Pendahuluan Radiasi Elektromagnetik [ REM ] Interaksi REM dengan senyawa (materi) Instrumentasi Struktur senyawa berwarna Analisis kualitatif. Kimia Analisis II. Mempelajari Tentang Spektrofotometri. - PowerPoint PPT PresentationTRANSCRIPT
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Prof. Dr. Sudibyo Martono, M.S., Apt.
Kimia Analisis II
2013, KA-II ke-1+2 1
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Kimia Analisis IIPendahuluanRadiasi Elektromagnetik [ REM ]Interaksi REM dengan senyawa (materi)InstrumentasiStruktur senyawa berwarnaAnalisis kualitatif
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Kimia Analisis IIKimia Analisis II
Mempelajari Tentang
Spektrofotometri
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PustakaPustaka
1. Harris, D.C., 1987, Quantitative Chemical Analysis, Second Edition, W.H. Freeman and Company, New York.
2. Pescok, R.L., Shields, L.D., Cairns, T., and McWilliam, I.G., 1976, Modern Methods of Chemical Analysis, Second Edition, John Wiley & Sons, New York.
3. Watson, D.G., 2003, Pharmaceutical Analysis, A Textbook for Pharmacy Students and Pharmaceuical Chemists, Churchill Living-stone.
4. Galichet, L.Y., (Managing editor), 2005 dan 2011, Clarke’s Analysis of Drugs and Poisons, in pharmaceuticals, body fluid and post-mortem material, Third Edition, The Pharmaceutical Press, London.
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Apa yang dinamakan
S p e k t r o f o t o m e t r i
?
SpektrofotometriSpektrofotometri
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Teknik analisis yang berhubungan dengan
penggunaan cahaya untuk
Mengukur konsentrasi bahan kimia
SpektrofofometriSpektrofofometri
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Prinsip dasar penyerapan dalam emisi radiasi oleh suatu molekul
Bagaimana proses tersebut diguna- kan dalam analisis kuantitatif ?
Akan dipelajari:Akan dipelajari:
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Didasarkan pada absorpsi (penyerapan) foton oleh analit (zat yang dianalisis)
Pada metode spektrofotometri, larutan sampel menyerap radiasi elektromagne-tik dari sumber yang cocok, dan jumlah yang diserap berhubungan dengan kon-sentrasi analit dalam larutan
SpektrofotometriSpektrofotometri
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Alat apa yang digunakan ?
Spektrofotometer
Instrumen (Alat)Instrumen (Alat)
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alat yang digunakan untuk mempelajari
absorpsi atau emisi radiasi elektromagnetik
sebagai fungsi panjang gelombang
SpektrofotometerSpektrofotometer
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Radiasi Elektromagnetik
[ REM ]
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Untuk tujuan ini, REM dapat dianggap sebagai suatu bentuk energi radian yang disebarkan sebagai gelombang garis melintang.
Gelombang tersebut bergetar tegak lurus arah perambatan dan ini memberikan gerakan gelombang ke arah pancaran
(lihat gambar berikut)
Radiasi Elektromagnetik(REM)
Radiasi Elektromagnetik(REM)
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Radiasi elektromagnetikRadiasi elektromagnetik
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PolarisasiPolarisasi
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Radiasi ElektromagnetikRadiasi ElektromagnetikRadiasi ElektromagnetikRadiasi Elektromagnetik
Energi radian bisa dipandang:1. Sebagai gelombang2. Sebagai partikel
partikel diskret = foton: - memiliki energi tertentu
- bergerak dalam ruang dengan kecepatan cahaya
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REM sebagai GelombangREM sebagai GelombangMoodel gelombang tersebut
Tidak dapatmenerangkan fenomena yang berhubungan
dengan :
Absorpsi + Emisi ( penyerapan ) ( pemancaran )
suatu
Energi radiasi
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REM sebagai partikelREM sebagai partikel
berkas suatu partikel yang terputus (diskontinyu)
paket gelombang suatu energi yang
disebut foton
[ energi sebuah foton frekuensi radiasi ]
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Radiasi ElektromagnetikRadiasi Elektromagnetik
o panjang gelombang (λ)
o frekuensi
o bilangan gelombang
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Unit dan SimbolUnit dan SimbolUnit dan SimbolUnit dan Simbol
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Energi Energi vs
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R E MR E M
Radiasi ekektromagnetik bervariasi dari
sinar gamma (energi sangat tinggi) hingga gelombang radio (energi sangat
rendah)
Spektrum elektromagnetik
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Radiasi ElektromagnetikRadiasi Elektromagnetik
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Terjadinya pelangiTerjadinya pelangi
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Daerah VisibelDaerah Visibel
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Colors of visible lightColors of visible lightColors of visible lightColors of visible lightλ maks.Absoprsi
[nm]
Warna yg diserap
Warna yg terlihat
380 – 420420 – 440440 – 470470 – 500500 – 520520 – 550550 – 580500 – 620620 – 680680 - 780
VioletViolet-blue
BlueBlue-green
GreenYellow-green
YellowOrange
RedPurple
Green-yellowYellowOrange
RedPurpleViolet
Violet-blueBlue
Blue-greenGreen
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Mengapa kita bisa melihat benda berwarna ?
Mengapa kita bisa melihat benda berwarna ?
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E = h = hc/nE = h = hc/nKeterangan:
E = energi foton dalam Joulev = frekuensi radiasi elektromagnetikh = tetapan Planck = 6,624 x 10 - 34
Joule.detik c = kecepatan cahaya = 3 x 1010
cm/detikn = indeks bias medium = panjang gelombang
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Interaksi Radiasi Elektromagnetik
dengan Materi
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Apa Yang TerjadiApa Yang Terjadi
Apabila
Sinar / CahayaMengenai
Sampel / Benda???
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Sinar mengenai sampelSinar mengenai sampel
ditransmisikan diserap/diabsorpsi dipantulkan* dibiaskan* dihamburkan**) : tidak dikehendaki
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•Reflection
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•Refraction
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Refraction of RadiationWhen radiation passes at an angle through the
interface between two transparent media that have different densities, an abrupt change in direction, or refraction, of the beam is observed as a consequence of a difference in velocity of the radiation in the two media.
When the beam passes from a less dense to a more dense environment, as in Figure 6-10, the bending is toward the normal to the interface. Bending away from the normal occurs when the beam passes from a more dense to a less dense medium.
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Instrumen Spektrofotometer
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SpektrofotometerSpektrofotometer
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Conventional Spectrophotometer
Schematic of a conventional single-beam spectrophotometer
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Conventional Spectrophotometer
Optical system of a double-beam spectrophotometer
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Cells [ Cuvette ]
UV Spectrophotometer:
Quartz (crystalline silica)
Visible Spectrophotometer:
Glass
IR Spectrophotometer:
NaCl
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Transmission Characteristics of Cell Materials
Note that all materials exhibit at least approximately 10% loss in transmittance at all wavelengths
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Sinar ditransmisikanSinar ditransmisikan
Sejumlah sinar ditransmisikan (diteruskan) melewati sampel.
Transmitans ( T ) yang terukur merupakan fraksi sinar datang yang muncul
dari sisi lain
0P
PT
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Sinar DiserapSinar Diserap
Sejumlah sinar diserap oleh bahan Maka:
A = ε b cA = Absorban
ε = koefisien ekstingsi molarb = tebal larutan ( kuvet )
C = konsentrasi larutan
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To record a spectrum, sweep through the appropriate range of energies and look for absorption at particular values.
64
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Luminescence
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More Complex Electronic Processes• Fluorescence: absorption
of radiation to an excited state, followed by emission of radiation to a lower state of the same multiplicity
• Phosphorescence: absorption of radiation to an excited state, followed by emission of radiation to a lower state of different multiplicity
• Singlet state: spins are paired, no net angular momentum (and no net magnetic field)
• Triplet state: spins are unpaired, net angular momentum (and net magnetic field)
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Sinar DipantulkanSinar Dipantulkan
Sejumlah sinar yang dipantulkan
pada setiap permukaan
Akhirnya meninggalkan sampel dalam arah sumber sinar
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Sinar DihamburkanSinar Dihamburkan
Bila sampel berupa cairan, sinar dapat
dihamburkan
oleh: partikel debu dalam cairan
atau oleh molekul zat terlarut
yang sangat besar
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712013, KA-II ke-1+2
AbsorpsiAbsorpsi
Sinar yang mengenai molekul suatu senyawa akan diabsorpsi (diserap)
Bila yang diserap sinar :- Ultra violet (UV) atau Visibel (Vis)
: digunakan untuk transisi elektron
- Inframerah (IR): digunakan untuk vibrasi gugus
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722013, KA-II ke-1+2
Penyerapan RadiasiPenyerapan Radiasi
Apabila suatu atom atau molekul menyerap cahaya dengan energi (E) tertentu, E = h
maka dapat terjadi peristiwa :M + h M*
* : molekul tereksitasi
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732013, KA-II ke-1+2
Struktur AtomStruktur Atom
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742013, KA-II ke-1+2
HeliumHelium
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752013, KA-II ke-1+2
Penyerapan radiasi oleh Atom
Penyerapan radiasi oleh Atom
Diagram tingkat energi subkulit pd atom polielektron
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762013, KA-II ke-1+2
Konfigurasi ElektronKonfigurasi Elektron
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772013, KA-II ke-1+2
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782013, KA-II ke-1+2
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792013, KA-II ke-1+2
Penyerapan radiasi oleh MolekulPenyerapan radiasi oleh Molekul
Tingkat energi: elektronik, vibrasi, & rotasi molekuler
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802013, KA-II ke-1+2
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812013, KA-II ke-1+2
Ultraviolet Spectrum [ Fenobarbital ]
Ultraviolet Spectrum [ Fenobarbital ]
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822013, KA-II ke-1+2
Ultraviolet Spectrum [ Fenobarbital ]
Ultraviolet Spectrum [ Fenobarbital ]
C
H3C-H2CC
C
NH
N
C O
O
O
_
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832013, KA-II ke-1+2
Spektrum AbsorpsiSpektrum Absorpsi
Adalah plot energi yang diserap(intensitas berkas yang diemisikan)
sebagai fungsi (panj. gelbg.) atau (frekuensi)
Spesies tereksitasi dapat mengemisikan foton bila kembali
ke ground state
Emisi radiasi
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842013, KA-II ke-1+2
Ikatan KimiaIkatan KimiaDalam keadaan azas (dasar) suatu molekul
memiliki:
1. Elektron ikatan (bonding electron) seperti:- ikatan sigma (ikatan tunggal)- ikatan pi (ikatan rangkap)
2. Elektron non-ikatan (non-bonding electron)
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852013, KA-II ke-1+2
Asam salisilatAsam salisilat
C
O
OH
H
O
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Absorption occurs when light of a specific wavelength causes the electronic transition
Molecular Orbital Theory
2013, KA-II ke-1+2
86
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2013, KA-II ke-1+2 87
The UV Absorption process
• * and * transitions: high-energy, accessible in vacuum UV (max <150 nm). Not usually observed in molecular UV-Vis.
•n * and * transitions: non-bonding electrons (lone pairs), wavelength (max) in the 150-250 nm region.
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2013, KA-II ke-1+2 88
The UV Absorption process•n * and * transitions: most common transitions observed in organic molecular UV-Vis, observed in compounds with lone pairs and multiple bonds with max = 200-600 nm.
•Any of these require that incoming photons match in energy the gap corrresponding to a transition from ground to excited state.
•Energies correspond to a 1-photon of 300 nm light are ca. 95 kcal/mol
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892013, KA-II ke-1+2
Electronic molecular orbital energies
Electronic molecular orbital energies
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902013, KA-II ke-1+2
Transisi n π*Transisi n π*
Jenis transisi ini memiliki nilai ε kecil
Forbidden transition
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HOMO = highest occupied molecular orbital (σ, π, n)
LUMO = lowest unoccupied molecular orbital (π* , σ*)
Most transitions we will be concerned with are from HOMO to LUMO
The orbital types of HOMO/LUMO partially determine the energy required to make the transition
Molecular Orbital Theory
2013, KA-II ke-1+2
91
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2013, KA-II ke-1+2 92
UV Excitation of 1,3-butadiene
1,3-butadiene
Transisi *
*
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932013, KA-II ke-1+2
Benzen kromoforBenzen kromofor
A1%1 cm
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942013, KA-II ke-1+2
Electronic TransitionElectronic Transition
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2013, KA-II ke-1+2 95
Absorption Dien, Polyene
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2013, KA-II ke-1+2 96
Absorption Dien, Trien
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2013, KA-II ke-1+2 97
O
Aldehid dan Keton
O
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Struktur Senyawa Berwarna
2013, KA-II ke-1+2 98
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2013, KA-II ke-1+2
Absorption of visible light
Where has the energy that was within the photons gone to ?
99
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1002013, KA-II ke-1+2
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1012013, KA-II ke-1+2
PaprikaPaprika
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1022013, KA-II ke-1+2
Lycopene TomatoLycopene Tomato
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1032013, KA-II ke-1+2
Zeaxanthin CornZeaxanthin Corn
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1042013, KA-II ke-1+2
-Carotene Wortel-Carotene Wortel
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2013, KA-II ke-1+2 105
Asorbansi radiasi UV/VISoleh
Kompleks Logam mungkin berasal dari transisi :
- Eksitasi ion logam- Eksitasi ligan
- Charge transfer transition
Senyawa Anorganik
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2013, KA-II ke-1+2 106
- Dalam kompleks memiliki nilai
ε antara : 1 - 100 M-1.cm-1
- Tidak bermanfaat dalam analisis
kuantitatif
Eksitasi Ion Logam
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2013, KA-II ke-1+2 107
- Kebanyakkan ligan adalah senyawa organik
- Transisi yang mungkin adalah
* n *
Eksitasi Ligan
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2013, KA-II ke-1+2 108
Kompleks logam berwarna dikarenakan :
Charge transfer transition
Perpindahan elektron (e-) dari: ion logam ke ligan
atau sebaliknya
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1092013, KA-II ke-1+2
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2013, KA-II ke-1+2 110
Hal tersebut dapat berupa promosi
elektron dari :
• Tingkat pada ligan
• Orbital ikatan ke orbital tak terisi pada ion logam
• Orbital ikatan ke orbital tak terisi pada ion logam
Charge transfer transition
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1112013, KA-II ke-1+2
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Analisis Kualitatif SecaraSpektrofotometri
2013, KA-II ke-1+2 112
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1132013, KA-II ke-1+2
KA II = Spektrofotometri
KA II = Spektrofotometri
ANALISIS
Kualitatif dan Kuantitatif
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1142013, KA-II ke-1+2
Dasar AnalisisDasar Analisis
1. Kualitatif- Pola spektrum- Lamda ( ) maksimum dalam
pelarut tertentu
2. Kuantitatif- Hukum Lambert-Beer
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1152013, KA-II ke-1+2
-Kromofor- Auksokrom
TerminologiTerminologi
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1162013, KA-II ke-1+2
Adalah :bagian molekul yang bertanggung
jawab pada penyerapan cahaya
Suatu kelompok atom yang memberikan peningkatan absorpsi
di daerah UV-dekat
Setiap benda yang menyerap cahaya tampak
( visibel ) akan nampak berwarna
KromoforKromofor
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1172013, KA-II ke-1+2
Kebanyakan kromofor memiliki
ikatan tak jenuh
KromoforKromofor
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1182013, KA-II ke-1+2
gugus fungsi seperti-OH, -NH2, -OCH3
dan halogen ( F, Cl, Br, I )
yang memiliki elektron valensi tak berikatan
dan tidak menyerap
radiasi pada 200 nm
AuksokromAuksokrom
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1192013, KA-II ke-1+2
Tetapi auksokrommenunjukkan absorpsi
yang intens di daerah UV-jauh
( transisi n * )
AuksokromAuksokrom
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1202013, KA-II ke-1+2
suatu molekul dan ion :
hanya dihubungkan dengan transisi antara tingkat energi
elektronik tipe tertentu atau
gugus suatu atom dalam molekul dan tidak menandakan molekul tersebut secara keseluruhan
Spektra UV dan VisSpektra UV dan Vis
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1212013, KA-II ke-1+2
suatu molekul dan ion :
hanya dihubungkan dengan transisi antara tingkat energi
elektronik tipe tertentu atau
gugus suatu atom dalam molekul dan tidak menandakan molekul tersebut secara keseluruhan
Spektra UV dan VisSpektra UV dan Vis
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1222013, KA-II ke-1+2
(energi 100 kcal/mol)
Menyebabkan perubahan
elektronik, vibrasi & rotasi
menghasilkan bentuk pita absorpsi yang melebar
Absorpsi energi di UVAbsorpsi energi di UV
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1232013, KA-II ke-1+2
-UV jauh, 100 – 190 nm
Instrumen yang ada umumnya dioperasikan di daerah UV-dekat,
karena : Silica (bahan kuvet, optik) & Oksigen
atmosfer Menghalangi pengukuran di daerah UV-
jauh
Daerah UV dan VisibelDaerah UV dan Visibel
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1242013, KA-II ke-1+2
PK. Amoksisilin, Spektro-UVPK. Amoksisilin, Spektro-UV
BM = 365,4
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1252013, KA-II ke-1+2
PK. Amoksisilin, Spektro-UVPK. Amoksisilin, Spektro-UV
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1262013, KA-II ke-1+2
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1272013, KA-II ke-1+2
(energi 5 kcal/mol)
Cukup untuk memacu molekul secara keseluruhan agar mengalami perubahan
vibrasi dan rotasi yang menggambarkan struktur
molekul secara menyeluruh
Absorpsi energi di IRAbsorpsi energi di IR
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1282013, KA-II ke-1+2
FenobarbitalFenobarbital
C
H3C-H2CC
C
NH
NH
C O
O
O
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1292013, KA-II ke-1+2
Spektrum FenobarbitalSpektrum Fenobarbital
C
H3C-H2CC
C
NH
N
C O
O
O
_
Ultraviolet Spectrum
C
H3C-H2CC
C
NH
N
C O
O
O
_
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1302013, KA-II ke-1+2
Fenobarbital dalam larutan bufer pH 9,2
Fenobarbital dalam larutan bufer pH 9,2
C
H3C-H2CC
C
NH
N
C O
O
O
_
Kromofor
Auksokrom
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1312013, KA-II ke-1+2
Spektrum propil barbitalSpektrum propil barbital
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1322013, KA-II ke-1+2
Spektrum propil barbitalSpektrum propil barbitalSpektrum propil barbitalSpektrum propil barbital
C
H3C-H2CC
C
NH
NH
C O
O
O
Fenobarbital
Propil barbital
C
C
NH
NH
C O
O
O
H2C=CH-CH2
H2C=CH-CH2
C
239254
241256
max [ nm ]
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2013, KA-II ke-1+2 133
DERIVAT SULFA
basa
S -N H -R
O
O
H 2N
asam
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1342013, KA-II ke-1+2
SulfadiazinSulfadiazin
N
N
H2N S
O
O
NH
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1352013, KA-II ke-1+2
Sulfadiazin
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1362013, KA-II ke-1+2
SulfamerazinSulfamerazin
H2N S
O
O
NH
N
N
CH3
![Page 137: Prof. Dr. Sudibyo Martono, M.S., Apt](https://reader033.vdokumen.com/reader033/viewer/2022061504/56814674550346895db397bc/html5/thumbnails/137.jpg)
1372013, KA-II ke-1+2
Sulfamerazin
![Page 138: Prof. Dr. Sudibyo Martono, M.S., Apt](https://reader033.vdokumen.com/reader033/viewer/2022061504/56814674550346895db397bc/html5/thumbnails/138.jpg)
1382013, KA-II ke-1+2
SulfamezatinSulfamezatin
N
N
H2N S
O
O
NH
CH3
CH3
![Page 139: Prof. Dr. Sudibyo Martono, M.S., Apt](https://reader033.vdokumen.com/reader033/viewer/2022061504/56814674550346895db397bc/html5/thumbnails/139.jpg)
1392013, KA-II ke-1+2
Sulfamezatin
![Page 140: Prof. Dr. Sudibyo Martono, M.S., Apt](https://reader033.vdokumen.com/reader033/viewer/2022061504/56814674550346895db397bc/html5/thumbnails/140.jpg)
2013, KA-II ke-1+2 140
N
N
H2N S
O
O
NH
H2N S
O
O
NH
N
N
CH3
N
N
H2N S
O
O
NH
CH3
CH3
Sulfadiazin
Sulfamerazin
Sulfamezatin
![Page 141: Prof. Dr. Sudibyo Martono, M.S., Apt](https://reader033.vdokumen.com/reader033/viewer/2022061504/56814674550346895db397bc/html5/thumbnails/141.jpg)
N
N
H2N S
O
O
NH
H2N S
O
O
NH
N
N
CH3
N
N
H2N S
O
O
NH
CH3
CH3
Sulfadiazin
Sulfamerazin
Sulfamezatin
max [ nm ]
242254
242255
243258
2013, KA-II ke-1+2 141
![Page 143: Prof. Dr. Sudibyo Martono, M.S., Apt](https://reader033.vdokumen.com/reader033/viewer/2022061504/56814674550346895db397bc/html5/thumbnails/143.jpg)
1432013, KA-II ke-1+2
![Page 144: Prof. Dr. Sudibyo Martono, M.S., Apt](https://reader033.vdokumen.com/reader033/viewer/2022061504/56814674550346895db397bc/html5/thumbnails/144.jpg)
1442013, KA-II ke-1+2