ATOMIC EMISSION SPECTROMETRY

Proses Absorpsi Energi Oleh Atom Dilanjutkan Dengan Proses

Emisi Energi Oleh Atom Yang Tereksitasi.
Hubungan antara populasi keadaan dasar dan keadaan eksitasi
sebagai fungsi temperatur diberikan oleh persamaan boltzmann
kT
E
i
e
g
g
N
N
A

|
|
.
|

\
|
=
0 0
1
Dimana :
gi/go = angka banding bobot-bobot statistik untuk keadaan dasar dan keadaan eksitasi
E = Energi pada keadaan tereksitasi relative ke keadaan ground state (Eo=0)
k = konstanta Boltzmann (1.3807 x 10-23 J/K)
T = temperature (K)
N1 = banyaknya atom dalam keadaan eksitasi
N0 = banyaknya atom keadaan dasar
I. Introduction
Basic Schematic
Scanning instruments can detect multiple elements.
Many lines detected so sometimes it is a quantitatively
difficult method.
Source can be flame, but more commonly plasma because it is
much hotter.
Jenis-jenis teknik atomisasi
Jenis Atomisasi Temperatur Atomisasi (
o
C)
Flame (nyala) 1700-3150
Electrothermal vaporisation 1200-3000
Inductively coupled argon plasma (ICP) 4000-6000
Direct current argon plasma (DCP) 4000-6000
Microwave-induced argon plasma (MIP) 2000-3000
Glow-discharge plasma (GD) Nonthermal
Electric arc 4000-5000
Electric spark 40000 (?)
Fotometer nyala
Li
K
Na
Ca
Ba
Pemilihan digunakan filter
Detektor : foto sel

II. PLASMA SOURCES
Plasma - Campuran gas yang sebagian terion : Ar, Ne, He
There are three types of plasma sources:
A) Inductively coupled plasma (ICP) , plasma induktif gel radio
B) Direct current plasma (DCP), plasma arus searah
C) Microwave induced plasma (MIP) , plasma induksi gel mikro
ICP is the most common plasma source.
A. INDUCTIVELY COUPLED PLASMA (ICP)
Constructed of three concentric quartz
tubes.
Ke pipa Cu dilewatkan arus bolak
balik dgn kekuatan 0,5-1,5 KW.
Gas plasma berputar ke atas
Arus listrik lewat kumparan
menghasilkan medan magnit.
Pemancing plasma kumparan
tesla
Kumparan tesla menghasilkan listrik
tegangan tinggi
Medan magnit menghalangi muatan
elektron
Dorongan dari bawah dan hambatan
dari atas timbul panas
Di dalam panas timbul plasma
Gas naik mngelilingi tabung sekaligus
pendingin


A. INDUCTIVELY COUPLED PLASMA (ICP)
1. Sample Introduction
Sample nebulized in a stream of argon
with a flow rate of 0.3 1.5 L/min.
Sample aerosol enters the plasma at the
base through the central tube.
a. Liquid Samples
Nebulizer similar to FAAS
b. Solid Samples
Sample atomized by electrothermal
atomization and carried into the
plasma by a flow of argon gas.
A. INDUCTIVELY COUPLED PLASMA (ICP)
2. Plasma Appearance
Radiation from this region is a
continuum with the argon line
spectrum superimposed.
Temperature: 8000-10000K
a. Excitation Region
The bright, white, donut shaped
region at the top of the torch.
b. Observation Region
The flame shaped region above the
torch with temperatures ~1000-
8000K.
The spectrum consists of emission
lines from the analyte along with
many lines from ions in the torch.
A. INDUCTIVELY COUPLED PLASMA (ICP)
3. Analyte Atomization and Ionization
Advantage of ICP over flame:
a) Temperature is two to three times higher than in a flame or
furnace, which results in higher atomization and excitation
efficiencies.
b) There is little chemical interference.
c) Atomization in the inert (argon) atmosphere minimizes oxidation
of the analyte.
d) Linear calibration curves can cover up to five orders of
magnitude.
B. DIRECT CURRENT PLASMA (DCP)
Constructed of two graphite anodes in a Y
formation with a tungsten cathode.
The argon flows out around the anodes
and the plasma forms at the split in the Y.
The plasma is ignited by bringing the
cathode in contact with the anodes.
Sample is introduced into the plasma in a
stream of argon that flows from between
the two anodes.
The plasma excitation temperature is
10,000 K and the observation
temperature is 5000 K.
Advantages vs. ICP
Fewer emission lines.
Less argon required.
Less expensive and bulky.
Disadvantages vs. ICP
Poorer sensitivity
Higher maintenance.
Few commercially available.
ULTRASONIC NEBULIZER WITH DESOLVATION
Sampel yang masuk digetarkan oleh gel, menjadi kabut, di
dorong oleh gas masuk ke dalam nyala
III. PLASMA SOURCE INSTRUMENTS
Two basic instrument designs; sequential and multi-channel detection
Monochromator yang scan spektrum, berhenti pada masing-masing panjang
gelombang analitis untuk mencapai rasio signal-to-noise diinginkan
A. Sequential (Scanning) Instruments
Secara teoritis, tidak ada batas
jumlah analisa yang ditampilkan
pada sampel yang sama.
Pada kenyataannya, jumlah
analisa dibatasi oleh jumlah
sampel, tingkat konsumsi sampel,
dan waktu yang diperlukan untuk
masing-masing analisa.
III. PLASMA SOURCE INSTRUMENTS
B. Multi-channel Instruments
Multi-channel analyzer
allows for simultaneous
acquisition from each
PMT.
60 elements can be
analyzed in the same
amount of time that it
takes to analyze one
element on a scanning
instrument.
Sampai 60 photomultiplier tubes( PMT) ditempatkan secara langsung di
bidang fokus yang dibengkokkan suatu diffraction grating cekung.
1. Rowland Circle Instrument
Saves time, sample, and
money.
III. PLASMA SOURCE INSTRUMENTS
B. Multi-channel Instruments
Low resolution grating disperses the radiation onto a prism.
2. Echelle Polychromator Instrument
Radiasi satu dimensi dilewatkan melalui sebuah prisma lebih lanjut
diuraikan kembali ke arah yang berbeda sehingga terjadi spektrum dua
dimensi yang dipusatkan pada celah plate yang dicocokkan dengan PMTs
or diode arrays.
Menyediakan resolusi lebih baik dibanding monochromator tunggal dan
memungkin pendeteksian bersama beberapa unsur-unsur.
ULTRASONIC NEBULIZER WITH DESOLVATION
Sampel yang masuk digetarkan oleh gel, menjadi kabut, di
dorong oleh gas masuk ke dalam nyala
PICTURE OF AN INDUCTIVELY-COUPLED PLASMA ATOMIC
EMISSION SPECTROMETER