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Course code : PCH1421M
Course title : Analytical chemistry
lab cum theory
Date : 19.07.2017
By,
J.Pradeepa,
1st PG Chemistry,
Lady Doak College.
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 .
1
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.
2
3
1. Environmental analysis …
 Water analysis including , natural, effluent, waste water,
and ocean.
4
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
5
 Soil analysis , sediment analysis, contaminated land ,
landfill sites, sludge analysis- solid and digested wastes
6
Soil analysis requirements &
outcome
METHODS REAGENTS
3050B HNO3/H2O2/HCl
3050B HNO3/H2O2/HCl
3051A HNO3/HCl
200.2 HNO3/HCl
ILMO4.0 HNO3/H2O2/HCl
Analyte CRDL (µg/L)
aluminum 200
antimony 60
arsenic 10
barium 200
beryllium 5
cadmium 5
calcium 5000
7
 Air – chimney exhaust filters, air filters of
contaminated sites, dusts
8
2. Petro chemical analysis…
 Specifically oils & greases,
 Petrochemicals applications at weak metal
analysis for industrial fleets, heavy industry by-
products.
 Pains , additives, pigments, ink.
9
3. Metallurgical analysis….
 Steels and alloys.
 Precious metals.
 Bulk materials- bronze, brasses.
 Traces- contaminants.
10
4. Geological analysis…
 Rock samples, cements, ceramics, glasses…etc.,
11
5. Food stuff analysis…
 Animal feed, crop analysis, toxins in food.
Crop analysis
12
 Trace analysis in micronutrients, metallic compounds in
wine, arsenic in food , and trace element in bound protein.
13
6. Coals and paper products…
14
 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
 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.
16
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.
17
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.
18
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
Out come results :
for example calcium,
Figure : Scans of 1 ppm Al at 167.081 nm with the effect of 1000 ppm Ca.
20
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
21
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.
22
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Applications of ICPAES

  • 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 . 1
  • 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. 2
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  • 5. 1. Environmental analysis …  Water analysis including , natural, effluent, waste water, and ocean. 4
  • 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 5
  • 7.  Soil analysis , sediment analysis, contaminated land , landfill sites, sludge analysis- solid and digested wastes 6
  • 8. Soil analysis requirements & outcome METHODS REAGENTS 3050B HNO3/H2O2/HCl 3050B HNO3/H2O2/HCl 3051A HNO3/HCl 200.2 HNO3/HCl ILMO4.0 HNO3/H2O2/HCl Analyte CRDL (µg/L) aluminum 200 antimony 60 arsenic 10 barium 200 beryllium 5 cadmium 5 calcium 5000 7
  • 9.  Air – chimney exhaust filters, air filters of contaminated sites, dusts 8
  • 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. 9
  • 11. 3. Metallurgical analysis….  Steels and alloys.  Precious metals.  Bulk materials- bronze, brasses.  Traces- contaminants. 10
  • 12. 4. Geological analysis…  Rock samples, cements, ceramics, glasses…etc., 11
  • 13. 5. Food stuff analysis…  Animal feed, crop analysis, toxins in food. Crop analysis 12
  • 14.  Trace analysis in micronutrients, metallic compounds in wine, arsenic in food , and trace element in bound protein. 13
  • 15. 6. Coals and paper products… 14
  • 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. 16
  • 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. 17
  • 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. 18
  • 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. 20
  • 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 21
  • 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. 22