Presentation of ICP Instrumentation at IICT Hyderabad

1. CRCL Group A Officer’s Training at IICT
Welcome
Distinguished Faculty Members of IICT
& Officers of Revenue Laboratories.

2. CRCL Group A Officer’s Training at IICT
Topic: ICP-OES Spectroscopy
Group-III
Team Members:
1. T.R Suresh
2. A.J Aleyamma
3. Ajay Kumar Singh
4. H S Bhandarkar
5. K Thambidurai

3. CRCL Group A Officer’s Training at IICT
Topic to be Covered
1. Introduction
2. Basic Principle of Inductively Coupled Plasma Optical Emission Spectroscopy
3. Instrumentation
4. General Applications
5. Application in CRCL Samples

4. CRCL Group A Officer’s Training at IICT
1. Introduction:
 Interaction of an atom in the gas phase with
electromagnetic radiation (EMR).
 Samples are solids, liquids and gases.
 ICP OES is a Inductively Coupled Plasma – Optical Emission
Spectroscopy and it is also called ICP AES.

5. Comparison: AAS & ICP-OES
• AAS: Absorption Spectroscopy, Single element,
ppm/ppb range, – Cheap, simple
– Small dynamic range
– GFAAS about 100 times more sensitive than FAAS,
but also more challenging
• ICP-OES: Emission Spectroscopy, Multi-element,
ppb range
– Limited spectral interferences, good stability, low
matrix effects

6. CRCL Group A Officer’s Training at IICT
2. Basic Principle:
M + e* → M*
M* → M + Energy
The energy emitted is directly proportional to
the concentration of analyte present the
solution.

7. Inductively coupled plasma optical emission
spectrometry (ICP-OES) - is a type of emission
spectroscopy that uses the inductively coupled plasma to
produce excited atoms and ions that emit
electromagnetic radiation at wavelengths characteristic of
a particular element.
Sample solution
containing elements
Formation of
liquid droplets
atomization
excitation
Emission of
Radiation at a
Specific Wave
Length
Measure the
intensity of
emitted
radiation

8. 3 Instrumentation
Schematic Diagram of ICP-OES

9. 1. Sample Introduction
2. Plasma
3. Detector
3 Instrumentation

10. Sample Introduction: liquid samples



Often the largest source of noise
Sample is carried into flame or plasma as
aerosol, vapour or fine powder
Liquid samples introduced using nebuliser

11. PUMPS:
Peristaltic pumps are almost exclusively
the pumps of choice for ICP-AES.
• The pumps utilize a series of rollers that
push the sample solution through the tubing
using a process known as peristalsis.
• With a pumped solution, the flow rate of
the solution into the nebulizer is fixed and is
not as dependent on solution parameters such
as viscosity and surface tension.

12. SPRAY CHAMBER:


Aspray chamber is placed between the
nebulizer & the torch.
The primary function of the spray chamber
is to remove large droplets from the aerosol.


The secondary purpose is to smooth out pulses
that occur during nebulization due to pumping of the solution.
It is designed to allow droplets with diameters
of about 10 micrometre or smaller to pass to the plasma.

14. What is a Plasma?
•Plasma source provides atomization
•Plasma: ―a gas-like phase of matter that
consists of charged particles‖
•ICP-AES plasma source is from the carrier
Gas typically argon is used
Emission Source: Plasma

15. Plasma Gas (15~16 L/min)
ICP torch schematic
Auxiliary Gas (1L/min)
Carrier Gas (1.2L/min) +
Sample Blend Gas (0.6L/min)
Plasma Generation
In ICP, the plasma is generated from radio frequency
magnetic fields induced by a copper coil which is wound
around the top of a quartz torch.

17. ICP temperatures
The Temperature of ICP flame is about 6000 K and up to
10000 K at its hottest point.

18. Excitation/ionization of atoms in Plasma
Achieved by three mechanisms:
1. Collisional transfer of excitation energy
e* + M → M* + e
M* → M+ + e
2. Through meta stable states of argon atoms/ions
(Penning ionization)
Ar* + M → Ar + M*
M* → M+ + e
3. Charge transfer between argon ions and the analyte
atoms
Ar + + M → Ar + M+

19. Radial or axial configuration
Axial
Sometimes called a “Horizontal
Plasma” ■ Useful analysis in
many different sample matrices
■ Excellent Detection Limits ■
Has certain limitations ■ Matrix
Interferences ■ Na and K can
have problems ■ The solution
complicates sample
preparation
Radial:
Original ICP View ■ Sometimes called “Vertical” or “Side-On”
Plasma ■ Accommodates all ICP matrices ■ Detection Limits
similar to Flame AA ■ Better for Refractory Si, Ti, B, W, Mo ■
Can analyze S, P and Halogens

20. PMT is to convert optical rotation(photons) into an electrical signal(electrons).The
vaccum tube devices are very sensitive&cover a large wavelength range.
It consists of a vaccum photocell with an anode, photocathode and a number
of dynodes which have an increasingly positive potential with respect to the photocathode.

21. ICP-OES wavelengths

22. Comparison: Detection limits and
working ranges
http://pubs.acs.org/hotartcl/tcaw/99/oct/element.html

23. 4
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ClinicalAnalysis: metals in biological fluids (blood, urine).
Environmental Analysis: trace metals and other elements in waters, soils,
plants, composts and sludges.
Pharmaceuticals: traces of catalysts used; traces of poison metals (Cd, Pb
etc).
Industry: trace metal analysis in raw materials; noble metals determination.
Forensic science: gunshot powder residue analysis, toxicological examination
( e.g., thallium (Tl) determination.
4.General Applications of ICP -OES

24. 1. Estimation of elements Metals and Alloys.
2. Estimation of Heavy metals in Vegetable, Mineral Oil
and Waste Oils.
3. Analysis of trace elements in Ores & Minerals
Applications in CRCL Laboratories
5.Applications of ICP –OES in CRCL

25. 1. From 1000 ppm Multiple STD Stock solution prepare
1 ppb, 5 ppb and 10 ppb etc.
2. Digest the suitable quantity of sample using
Microwave Digestion and made up to 100ml SMF.
3. Analyse both STD and sample in ICP-OES in a
following manner.
Preparation of Standards and Sample Solution
Applications of ICP –OES in CRCL
Analysis of Tin, Zinc and Manganese in Metal samples

26. 32
Microwave digestion
Supplied with dedicated vessels (e.g. PTFE)
Closed vessel digestion minimises sample contamination
Faster, more reproducible, and safer than conventional methods
Rotor

28. Calculation:
Calculation (ppb)
Concentration of unknown sample = Sample conc (ppb) - Blank conc (ppb) × Volume (mL)
Sample weight in gram
1000000000*.
100*100*
%
1000000000*.
100*100*
%
1000000000*.
100*100*
%
SplWt
ppb
Mn
SplWt
ppb
Zinc
SplWt
ppb
Tin




29. CRCL Group A Officer’s Training at IICT
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