Spektrofotometri emisi

Page 1
Basic principle of emission
spectrophotometry

emisi

Intensitas emisi 
konsentrasi contoh
Page 2
Atomization Emission Sources

– Flame – still used for metal atoms

– Electric Spark and Arc
– Direct Current Plasmas
– Microwave Induced Plasma
– Inductively Coupled Plasma – the
most important technique

Page 3
 Flame spectrophotometry
• Untuk analisis kation yg mudah tereksitasi
ke tingkat lebih tinggi pd temperatur nyala
yg rendah
• Li, Na, K, Rb, Cs, Ca, Ba, Cu
• Nonlogam tdk menghasilkan atom netral
yg terisolasi dlm nyala  tdk cocok utk
dianalisis dg metode flame

Page 4
Kelebihan
 sederhana, murah, cepat, sensitif
 dpt diaplikasikan untuk sampel klinis,
biologis dan lingkungan
 atom fasa gas dalam nyala memiliki
garis emisi yg sempit dan karakteristik

relatif bebas dari gangguan unsur lain

Page 5
1. nebulisasi Preparasi
sampel
2. desolvasi/

volatilisasi
3. atomisasi

4. eksitasi/emisi

5. separasi/ deteksi

detektor

Page 6
Instrumentasi

Page 7
Flame structure

Page 8
Reaksi yang terjadi

Page 9
Kelemahan
Temperatur rendah :
metode sangat sensitif thd stabilitas
flame dan kondisi aspirasi

Hal yg perlu diperhatikan

Faktor yg mempengaruhi intensitas emisi :
 laju alir dan kemurnian bahan bakar &
oksidan
 laju aspirasi
 viskositas larutan
 konkomitan dlm sampel
Page 10
ICP – Atomic Emission
Spectrophotometry

ICP-AES

Page 11
 menggunakan PLASMA sbg
ICP-AES sumber atomisasi & eksitasi

campuran gas yg terion (highly

PLASMA ionized gas) dan elektron
muatan netto = netral

Page 12
 before we go further….
answer this question !
1. What is plasma ?
2. Is plasma the same as flame ? If it is not, what is the
difference ?
3. How is ICP produced ?
4. Draw a schematic diagram of ICP-AES instrumentation !
5. Can solid sample be determined directly by ICP-AES
without converting it to liquid/solution phase ?

Page 13
Page 14
Page 15
ICP torch

Page 16
Page 17
The operating conditions of an ICP-OES instrument are
determined by a number of variable parameters.

The most common parameters that are varied,

depending on the design of the instrument, are
integration time, PMT voltage, argon flow
rates, and RF power.

Other variable parameters may include

pump speed and viewing height.

Wavelength is certainly an important

variable parameter on many
instruments.

Page 18
For liquid samples

Page 19
 Many forces can be used to break up a liquid into an aerosol;
however, only two have been used successfully with an ICP,
pneumatic forces and ultrasonic mechanical forces.

Meinhard® nebulizers
concentric nebulizer
micro-concentric nebulizer
cross-flow nebulizer

Babington nebulizer

Page 20
Page 21
Page 22
Ultrasonic nebulizer with desolvation

Page 23
For solid samples

Laser ablation – ICP/MIP AES

separated tandem source

Source 1
Source 2
The LA, releases Source 2
interface
materials, produces Excitation
free atoms and form Excitation
the analyte species

Page 24
Laser ablation – ICP- AES

1. laser
2. laser ablation
chamber
3. PTFE transportation
tube
4. optical bench
5. ICP torch
6. ICP match box
7. échelle
polychromator

Page 25
Laser ablation – MIP- AES
1. laser
2. laser ablation
chamber
3. PTFE transportation
tube
4. plasma gas in
5. Optical bench
6. PTFE vapor
transport valve
7. quartz plasma torch
8. rectangular
microwave cavity
9. tunning screw
10. lens
11. échelle
polychromator

Page 26
Schematic of overall optical system used for MIP source

Page 27
 1. silica window
2. chamber
3. Ar gas inlet port
4. gas outlet tube

Photograph of laser ablation chamber

Page 28
Direct Current Plasma (DCP)

• Plasma forms by
bringing graphite
and W electrodes in
contact with one
another
• Temp @ core
10,000K
in viewing region
5000K

Page 29
ICP DCP Comparison

Page
• 30
DC
Aux
 Comparison of Plasma to Flame
Emission Sources
• Plasma sources offer significantly better
quantitative data than do other flame emission
sources
- High stability
- Low noise
- Low background
- Freedom from interferences

Page 31
Page 32
 Quantitative analysis
The intensity of the emitted
radiation (P) is proportional to
the number of excited
atoms N*
N0 = number of atoms in the
ground state

The intensity of the emitted light

will be directly proportional to
the concentration of the element
introduced into the flame

Page 33
Pengolahan data

Page 34
Teknik adisi standar

Page 35
 Teknik standar internal
Li (ppm) Na (ppm) Intensitas
Na/Li
0 10 0 0
1 10 2 15,8
2 10 4 31,4
3 10 6 45,4
4 10 8 58,1
5 10 10 70,2
contoh 10 unknown 43,2

Page 36
Page 37