MKI80004 - Instrumentasi Kimia
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MKI80004 - Instrumentasi Kimia
Minggu Ke
Isi Pertemuan Keterangan
1 Uraian Perkuliahan: Isi Kuliah; Cara; dan EvaluasiPendahuluan/Introducton to Spectrometry
Lecturing & Discussion
2 Optical Spectroscopy and Instrumentation; UV-Vis [Absorption, Reflectance aspect] Spectrometry; Luminescence Spectroscopy
Lecturing & Discussion
3 Infra Red [Absorption Spectrometry, Reflectance aspect ] Spectrometry
Lecturing & Discussion
4 Introduction to Atomic SpectrometryAtomic Emission SpectroscopyAtomic Absorption Spectroscopy
Lecturing & Discussion
5 Atomic Spectrometry with X Ray:XRFXPS
Lecturing & Discussion
6
7 Class Discussion and Evaluation
8 Overview Other Instrumental Methods: Hyphenated Techniques Lecturing & Discussion
9 Topic of Choice I [1& 2] Active Learning
10 Topic of Choice II [1& 2] Active Learning
11 Topic of Choice III [1& 2] Active Learning
12 Topic of Choice IV [1& 2] Active Learning
13 Evaluation Short Talk
14 Final Evaluation
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Cuvet
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Violet: 400 - 420 nm Indigo: 420 - 440 nm Blue: 440 - 490 nm Green: 490 - 570 nm Yellow: 570 - 585 nm Orange: 585 - 620 nm Red: 620 - 780 nm
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Chromophore Example Excitation λmax, nm ε Solvent
C=C Ethene π __> π* 171 15,000 hexane
C≡C 1-Hexyne π __> π* 180 10,000 hexane
C=O Ethanaln __> π*π __> π*
290180
1510,000
hexanehexane
N=O Nitromethanen __> π*π __> π*
275200
175,000
ethanolethanol
C-X X=Br X=I
Methyl bromide
Methyl Iodide
n __> σ*n __> σ*
205255
200360
hexanehexane
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Terminology for Asorption Shifts
Nature of ShiftDescriptive
Term
To Longer Wavelength
Bathochromic
To Shorter Wavelength
Hypsochromic
To Greater Absorbance
Hyperchromic
To Lower Absorbance
Hypochromic
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Empirical Rules for Absorption Wavelengths of Conjugated Systems
Woodward-Fieser Rules for Calculating the λmax of Conjugated Dienes and Polyenes
Core Chromophore Substituent and Influence
Transoid Diene
215 nm
R- (Alkyl Group) .... +5 nmRO- (Alkoxy Group) .. +6 X- (Cl- or Br-) ......... +10 RCO2- (Acyl Group) .... 0
RS- (Sulfide Group) .. +30R2N- (Amino Group) .. +60
Further π -ConjugationC=C (Double Bond) ... +30C6H5 (Phenyl Group) ... +60
Cyclohexadiene*
260 nm
(i) Each exocyclic double bond adds 5 nm. In the example on the right, there are two exo-double bond components: one to ring A and the other to ring B. (ii) Solvent effects are minor.* When a homoannular (same ring) cyclohexadiene chromophore is present, a base value of 260 nm should be choosen. This includes the ring substituents. Rings of other size have a lesser influence.
λmax (calculated) = Base (215 or 260) + Substituent Contributions
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Some examples that illustrate these rules follow.
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Woodward-Fieser Rules for Calculating the π __> π* λmax of Conjugated Carbonyl Compounds
Core Chromophore Substituent and Influence
R = Alkyl 215 nm
R = H 210 nmR = OR' 195 nm
α- Substituent R- (Alkyl Group) +10 nm Cl- (Chloro Group) +15 Br- (Chloro Group) +25 HO- (Hydroxyl Group) +35 RO- (Alkoxyl Group) +35 RCO2- (Acyl Group) +6 β- Substituent R- (Alkyl Group) +12 nm Cl- (Chloro Group) +12 Br- (Chloro Group) +30 HO- (Hydroxyl Group) +30 RO- (Alkoxyl Group) +30 RCO2- (Acyl Group) +6 RS- (Sulfide Group) +85 R2N- (Amino Group) +95 γ & δ- Substituents R- (Alkyl Group) +18 nm (both γ & δ) HO- (Hydroxyl Group) +50 nm (γ) RO- (Alkoxyl Group) +30 nm (γ)
Further π -Conjugation C=C (Double Bond) ... +30 C6H5 (Phenyl Group) ... +60
Cyclopentenone202 nm
(i) Each exocyclic double bond adds 5 nm. In the example on the right, there are two exo-double bond components: one to ring A and the other to ring B. (ii) Homoannular cyclohexadiene component adds +35 nm (ring atoms must be counted separately as substituents)(iii) Solvent Correction: water = –8; methanol/ethanol = 0; ether = +7; hexane/cyclohexane = +11
λmax (calculated) = Base + Substituent Contributions and Corrections
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Figure 1: Schematic diagram of UV-vis diffuse reflectance measurement system.
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Figure 2: UV-vis diffuse reflectance spectrum for bulk Bi2O3.
The Kubelka-Munk function, F(R), allows the optical absorbance of a sample to be approximated from its reflectance:
F(R) = (1-R)2
2R
For a semiconductor sample this allows the construction of a Tauc Plot - (F(R).hv)n vs hv. For a direct band gap semiconductor the plot n = 1/2 will show a linear Tauc Region just above the optical
absorption edge. Extrapolation of this line to the photon energy axis yields the semiconductor band gap- a key indicator of its light harvesting efficiency under solar illumination. Indirect band gap materials show a Tauc Region on the n = 2 plot.
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Figure 3: Tauc Plot (n = 1/2) for bulk Bi2O3 after Finlayson et al. Phys. Stat. Sol.
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• Katalis
• Hasil Pengukuran Reflectant
• Acessories
• IR
• XRF dan XPS