PT.

Pandu Anugerah Analitika

 Spektroskopi atom
Perubahan analit dari bentuk ion
dalam larutan menjadi atom bebas
Atomic Absorption (AA)
• Atomic Emission (ICP)
• Atomic Fluorescence (AF)
• Mass Spectroscopy (MS)

PT. Pandu Anugerah Analitika

 Atomic Spectroscopy Systems

PT. Pandu Anugerah Analitika

 SPEKTROSKOP ATOM
• ABSORPTION ATOM
– NYALA
– GRAPHITE FURNACE
– COLD VAPOR FOR Hg
• EMISIATOMI
– NYALA
– INDUCTIVELY COUPLED PLASMA (ICP)

PT. Pandu Anugerah Analitika

 ATOMIC ABSORPTION
• HCL provides light of correct wavelength
• Electrons in sample atom absorb light
• Causes the electron to go to a higher energy
level
• Measure decrease in light intensity of lamp
• Relate decrease to concentration

PT. Pandu Anugerah Analitika

ATOMIC ABSORPTION

Absorb Light from a

Hollow Cathode Lamp

PT. Pandu Anugerah Analitika

 AA Schematic

Light Source Atom Source Absorption

Spectrum

PT. Pandu Anugerah Analitika

 FLAME ATOMIC ABSORPTION

Monochromator

HCL

Grating
Flame Mirror

Photomultiplier Tube

Cu Pb Zn Be As

Mn Cr Mg Ca Na

PT. Pandu Anugerah Analitika

GRAPHITE FURNACE ATOMIC
ABSORPTION
Monochromator

HCL
Grating
Graphite Furnace Mirror

Photomultiplier Tube

Cu Pb Zn Be As

Mn Cr Mg Ca Na

PT. Pandu Anugerah Analitika

 ATOMIC EMISSION
• Energy is put into system - ICP
• Electrons in atom are promoted to higher energy level -
temporary situation
• Electrons fall back to lower energy levels by giving up
energy
• Relate intensity at particular wavelength to
concentration
• Difference in energy level determines wavelength

PT. Pandu Anugerah Analitika

 ATOMIC EMISSION

• Excited Electrons Give

Up Energy As Light
• Emitted Light Characteristic of Element

PT. Pandu Anugerah Analitika

Emission vs. Absorption

PT. Pandu Anugerah Analitika

Energy Transitions and Wavelength
Atomic Energy States Atomic Spectrum

B
Wavelength
A

PT. Pandu Anugerah Analitika

 Temperature & Emission
5000o K

3000o K

2000o K

Room Temp

PT. Pandu Anugerah Analitika

 Various Source Temperatures

Air/Acetylene 2200o C
Nitrous Oxide 2800o C
Graphite Furnace 3000o C
Argon Plasma 10000o C

PT. Pandu Anugerah Analitika

 PROFILE ICP
ICP Benefits vs. AA

• Better linear range

• Freedom from Chemical Interferences
• No need to change lamps, gases, burner
height
• Easy to automate for un-attended operation

PT. Pandu Anugerah Analitika

 PROFILE ICP
ICP Benefits vs GFAAS

• Matrix modifiers are not required

• Special background corrections
techniques with magnetic fields not
required
• ICP much faster than GFAAS

PT. Pandu Anugerah Analitika

 ICP vs AAS
I# Parameter ICP AAS Flame AAS GF Notes
1 Detection ppb & <ppb ppm ppb
Limits
2 Application Good for Good for No good
all volatile for B, W,
elements, elements U,
best for refractories
refractories , P, S &
& non- halogens
metals
3 Elements 72 60 (VIS) 35 (Some
(UV&VIS) VIS)

PT. Pandu Anugerah Analitika

 ICP vs AAS
I# Parameter ICP AAS Flame AAS GF Notes
4 Sample 1-3 sec/el, 1- 4-5
throughput 100-150 2min/eleme min/eleme
samples/da nt nt
y 20-30 10
LL Seq ICP samples/day samples/da
y
5 Linear >1:1000000 1:1000 1:100
Dynamic
Range
6 Short-term 0.3-1% 2-3 % 3-5%
RSD
7 Long-term <2% > 10% > 10%
RSD

PT. Pandu Anugerah Analitika

 ICP vs AAS

I# Parameter ICP AAS Flame AAS GF Notes

8 Interfernce
s: Minimal Min. Min.
Spectral None Some Many
Chemical
9 Sample 0.03-5 ml 5-15 ml < 0.1
Volume
10 Total >20% < 5% > 20%
Dissolved
solids
11 Unattended Yes, short No Yes, but
-auto- & long- short time
operation overnight

PT. Pandu Anugerah Analitika

 ICP vs AAS

I# Parameter ICP AAS Flame AAS GF Notes

12 Cost
Initial Moderate Low Moderate
Long-term Low High High (+
GF)
13 Operating Low High High
cost HCL & HCL & GF
gases consumabl
es
14 Operator Factory Chemist Chemist
trained
technician

PT. Pandu Anugerah Analitika

PT. Pandu Anugerah Analitika
 Kelebihan metoda ICP
• Tidak memerlukan lampu katoda
• Kemampuan multiunsur (beberapa unsur
dapat diukur sekaligus)
• Batas deteksi rendah ( ~ µg/L )
• Daerah konsentrasi pengukuran yang luas
(~ 1 µg/L - 100 mg/L)

PT. Pandu Anugerah Analitika

 Kelemahan ICP
Konsumsi gas (argon) yang banyak
Kecuali ada fabrik pengolahan gas yang
dapat mengambil argon dari udara (argon di
udara ada ~ 1%

PT. Pandu Anugerah Analitika