04 - Spektroskopi UV-Vis - 3

ANALISIS INSTRUMEN
I
SPEKTROSKOPI UV-VIS
Spektroskopi UVVis
APLIKASI SPEKTROSKOPI UV-VIS
Analisis
Instrumen I
Analisis Kualitatif
Memprediksi jenis/golongan senyawa
Analisis Kuantitatif
Menentukan kandungan senyawa dalam sampel
~ Arie BS
Analisis
Spektroskopi UVInstrumen I
Vis
UV-VIS untuk Analisis Kualitatif
Woodward-Fieser Rules for Dienes
Homoannular
(cisoid)
=253 nm
Parent
Heteroannular
(transoid)
=214 nm
=217 (acyclic)
Increments for:
Double bond extending conjugation
30
30
Alkyl substituent or ring residue
Exocyclic double bond
-OC(O)CH3
-OR
-Cl, -Br
-NR2
60
60
-SR
30
30
Polar groupings:
~ Arie BS
Analisis
Vis
CONTOH
Transoid:
217 nm
Alkyl groups or ring residues:
3x5=
15 nm
Calculated:
232 nm
Observed:
234 nm
Cisoid:
253 nm
2x5=
10 nm
Calculated:
263 nm
Observed:
256 nm
~ Arie BS
Analisis
Vis
CONTOH
Transoid:
214 nm
3x5=
Exocyclic double bond:
15 nm
5 nm
Calculated:
234 nm
Observed:
235 nm
Cisoid:
253 nm

4x5=
20 nm
5 nm
Calculated:
278 nm
Observed:
275 nm
~ Arie BS
Analisis
Vis
Woodward's Rules for Conjugated Carbonyl Compounds
Base values:
X=R
Six-membered ring or acyclic parent enone
=215 nm
Five-membered ring parent enone
=202 nm
Acyclic dienone
=245 nm
X=H
=208 nm
X = OH, OR
=193 nm
~ Arie BS
Analisis
Vis
Increments for:
Double bond extending conjugation
30
Exocyclic double bond
Endocyclic double bond in a 5- or 7-membered ring for

X = OH, OR
Homocyclic diene component
39
Alkyl substituent or ring residue
~ Arie BS
10
12
or higher
18
Analisis
Vis
Polar groupings:
-OH
-OC(O)CH3
-OCH3
-Cl
-Br
-NR2
35
30
50
35
30
17
31
15
12
30
25
95
Solvent correction*:
variable
~ Arie BS
max (calc'd)
total
Analisis
Vis
Solvent
max shift (nm)
Water
+8
chloroform
-1
ether
-7
cyclohexane
- 11
dioxane
-5
hexane
- 11
~ Arie BS
Analisis
Vis
CONTOH
Acyclic enone:
215 nm
-Alkyl groups or ring residues:

10 nm
2 x 12 =
24 nm
Calculated:
249 nm
Observed:
249 nm
Five-membered ring parent

enone:
202 nm

2 x 12 =
24 nm
5 nm
Calculated:
231 nm
Observed:
226 nm
~ Arie BS
Analisis
Vis
CONTOH
Six-membered ring or alicyclic

parent enone:
202 nm
Extended conjugation:
30 nm
Homocyclic diene component:
39 nm
2 x 12 =
18 nm
Calculated:
302 nm
Observed:
300 nm
Five-membered ring parent enone:
202 nm
-Br:
25 nm

2 x 12 =
24 nm
5 nm
Calculated:
256 nm
Observed:
251 nm
~ Arie BS
Analisis
Vis
CONTOH
Carboxylic acid:
193 nm
10 nm
12 nm
Calculated:
215 nm
Observed:
217 nm
Ester:
193 nm
10 nm
12 nm
Endocyclic double bond in 7-membered ring:
5 nm
Calculated:
220 nm
Observed:
222 nm
~ Arie BS
Analisis
Vis
CONTOH
Aldehyde:
208 nm

10 nm
2 x 12 =
24 nm
Calculated:
242 nm
Observed:
242 nm
Aldehyde:
208 nm
Extended conjugation:
30 nm
Homodiene component:
39 nm
10 nm
18 nm
Calculated:
304 nm
Observed:
302 nm
~ Arie BS
Analisis
Vis
UV-VIS untuk Analisis Kuantitatif
Biasanya dilakukan pada larutan berair

Spektroskopi UV-Vis untuk analisis kuantitatif bercirikan:
1. Dapat diaplikasikan untuk berbagai senyawa, baik organik
maupun anorganik.
2. Mempunyai sensititivitas yang baik: 10-4 hingga 10-5 M
3. Selektif
4. Mempunyai akurasi yang baik
5. Mudah dalam pengumpulan data
~ Arie BS
Analisis
Vis
PROSEDUR:
1. Pemilihan panjang gelombang maksimum ( maks)

Dilakukan dengan scanning dari 200 800 nm.
Pengukuran dilakukan pada maks karena:
a. Memiliki sensitivitas terbesar (A/c terbesar)
b. Pada puncak, kurva absorpsi flat (rata) sehingga Hukum LambertBeer menjadi lebih valid.
Variabel yang mempengaruhi spektra absorpsi:
a)Solven
b)pH
c) Temperature
d)Matriks sample matrix (mis: konsentrasi elektrolit dan
spesies yang dapat berinterferensi)
~ Arie BS
Analisis
Vis
PROSEDUR:
1. Pembuatan kurva
kalibrasi
Dapat digunakan kurva kalibrasi eksternal, standar
internal, maupun addisi standar
siapkan seri larutan baku (minimal 5 buah)
ukur setiap larutan baku pada maks
lakukan pengukuran terhadap blanko
buat hubungan antara absorbansi vs konsentrasi
siapkan sampel (jika perlu lakukan pengenceran)
sehingga absorbansi sampel masuk dalam rentang
kurva kalibrasi
~ Arie BS

04 - Spektroskopi UV-Vis - 3

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04 - Spektroskopi UV-Vis - 3

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ANALISIS INSTRUMEN

Alkyl substituent or ring residue

Exocyclic double bond

Alkyl groups or ring residues:

Alkyl groups or ring residues:

Alkyl groups or ring residues:

Exocyclic double bond:

Alkyl groups or ring residues:

Five-membered ring parent enone

Exocyclic double bond

Endocyclic double bond in a 5- or 7-membered ring for

Homocyclic diene component

Alkyl substituent or ring residue

max shift (nm)

-Alkyl groups or ring residues:

Five-membered ring parent

-Alkyl groups or ring residues:

Six-membered ring or alicyclic

Homocyclic diene component:

-Alkyl groups or ring residues:

Five-membered ring parent enone:

-Alkyl groups or ring residues:

-Alkyl groups or ring residues:

-Alkyl groups or ring residues:

-Alkyl groups or ring residues:

-Alkyl groups or ring residues:

Endocyclic double bond in 7-membered ring:

-Alkyl groups or ring residues:

-Alkyl groups or ring residues:

-Alkyl groups or ring residues:

Biasanya dilakukan pada larutan berair

1. Pemilihan panjang gelombang maksimum ( maks)

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