1. Course code : PCH1421M
Course title : Analytical chemistry
lab cum theory
Date : 19.07.2017
By,
J.Pradeepa,
1st PG Chemistry,
Lady Doak College.
2. What is an ICP-
AES….?• It is type of Atomic emission spectroscopy.
• It will dissociate a sample into its constituent atoms and
ions and exciting them to a higher energy level.
• It causes them to emit light at a characteristic wavelength.
• It measures the intensity of the light emitted by atoms or
ions of the element at particular wave length.
• Determines approximately all of the elements .
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3. Principle behind ICP-AES..!!! - Photo electric
effect
• Light from the Plasma source
• Absorption of energy by the electrons which
present in the sample.
• Jumping of electrons to higher energy levels.
• Emission of characteristic photons of energy,
that is wavelength.
• By isolating these photon wavelengths, types
and concentrations of the element present can
be determined.
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5. 1. Environmental analysis …
Water analysis including , natural, effluent, waste water,
and ocean.
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6. Water analysis requirements & outcome
the Liberty 200 Inductively Coupled
Plasma Atomic Emission Spectrometer
All standard solutions were prepared from
high purity ICP 10 000 ppm stock
standards
Standard 1 : Mn, Be, Cd, Pb, Zn.
Standard 2 : Cu, Fe, V, Co.
Standard 3 : Al, Cr, Ni.
Multi-element standards were prepared in
10% v/v HCl and contained 5 mg/L of each
element. The blank solution was 10% v/v
HCl solution.
Element Wavelength
(nm)
Detection
limit (ng/mL)
Al 167.081 1.5
Be 234.802 0.2
Cd 228.803 1.5
Co 238.893 5
Pb 220.353 14
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7. Soil analysis , sediment analysis, contaminated land ,
landfill sites, sludge analysis- solid and digested wastes
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9. Air – chimney exhaust filters, air filters of
contaminated sites, dusts
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10. 2. Petro chemical analysis…
Specifically oils & greases,
Petrochemicals applications at weak metal
analysis for industrial fleets, heavy industry by-
products.
Pains , additives, pigments, ink.
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16. It can detect most of the metals at a time.
Detection limits down to ppt for some elements.
Rapid simultaneous determination of selected
elements.(over 70 elements)
Suitable for routine analysis of multiple sample.
Capability to analyze a large amount of sample in a short
period of time. 15
17. Not effective for low levels of alkalies (less than 1ppm).
Suitable standards required on every run.
only elemental data is provided – no direct structural
information.
Doesn’t provide, in most cases, parts per billion or parts
per trillion data for all metals.
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18. Acceptable sample forms…
Solutions, preferably aqueous based with
minimal volume.
Minimal solution volume is 3-4 ml.
Solids can usually be dissolved using various
techniques.
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19. Suitable reagents…
For example, Concentrated nitric acid (for silver
containing metal/metal alloy)
Concentrated hydrochloric acid.
Aqua regia (for general metal/metal alloy)
Mix HNO3 and HCl in a ratio of 1:3.
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20. System operating parameter
Power 1.2 kW
Plasma gas flow 12.0 L/min
Auxiliary gas flow 0.75 L/min
Torch type Standard one piece quartz torch with 1.4 mm I.D. injector tube
Nebulizer type Glass concentric
Nebulizer pressure 160 kPa
Pump tube Grey-grey (inlet)
Blue-blue (outlet) Pump rate 15 rpm Sample uptake rate 1.4
mL/min Integration time 3 sec
Viewing height Optimised for SBR
Background correction Automatic
PMT voltage 650 V
Grating order Default
Filter position Default 19
21. Out come results :
for example calcium,
Figure : Scans of 1 ppm Al at 167.081 nm with the effect of 1000 ppm Ca.
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22. Detection limits for some of the metals
Element Wavelength ( nm ) Detection limit(ppb)
Cr 267.716 0.25
Cu 224.700 0.9
Fe 259.939 0.2
Mn 257.610 0.03
Ni 231.604 0.4
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23. References…
Boss, C.B. and freden, K.J. concepts, instrumentations and techniques
in inductively coupled plasma atomic emission spectroscopy, 1997.
Skoog, D. fundamentals of analytical chemistry, 2004.
Inductively coupled plasma in analytical atomic spectroscopy:
montaser,A.; goligthly D.W.,Eds.; VCH publishers: new york. 1988.
Fredeen, C.B. (n.d).
http://www.atoomspectrometrie.nl/Icpconceptsbook.pdf.
Inductively Coupled Plasma Atomic Emission Spectrometric Method
for trace element analysis of water and wastes, Method 200.7 CLP-M,
US Environmental Protection Agency, Cincinnati, Ohio 1985.
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