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PRESENTED BY,
DEVIPRIYA P V
M MPARM
Department of Pharmaceutical Analysis
 Valid applications in every branch of chemical
analysis.
 An established procedure in analytical chemistry,
ceramics, mineralogy, biochemistry, water
supplies, metallurgy and soil analysis.
1. Qualitative analysis.
2. Quantitative analysis.
3. Simultaneous multi-component analysis.
4. Determination of metallic elements in biological
materials.
5. Determination of metallic elements in food industry.
6. Determination of Ca, Mg, Na and K in blood serum.
7. Determination of lead in petrol.
Qualitative analysis
 Different hollow cathode lamps are to be used for
each element.
 Only the element used in hollow cathode lamp can
be detected.
 Checking one element at a time.
 Rarely used.
Quantitative analysis
 Based on the determination of amount of radiation
absorbed by the sample.
 Amount of light absorbed = (πe2 / mc)Nf
 Quantitative measurements are based on calibration
curves.
 The absorbance values are plotted versus
concentrations.
 concentration of unknown solution is calculated using
equation:
A= mc
Absorbance = slope * concentration.
Sensitivity limits
ELEMENT Å SENSITIVITY (ppm)
Al 3092 1
Ca 4427 0.05
Cu 3247 0.1
Pb 2170 0.01
Ni 2320 0.1
K 7665 0.01
Na 5890 0.01
Zn 3601 50.0
Mg 2852 0.001
Hg 2537 1.0
Fe 2843 0.1
Ba 5535 0.2
Ag 3281 0.01
Calibration curve of Cu
 The parameters that influence a quantitative
determination and need to be controlled are:
: Flame system
: Wavelength
: Solution.
Simultaneous multi-component
analysis
 If multi-component emission source is available.
 Mitchell (1973) described a multielement atomic
absorption system using a multielement hollow
cathode source and a vidiocon detection system.
 Spectral region from 2320 to 3281 Å.
 Detect 8 elements (Zn, Cd, Ni, Co, Fe, Mn, Cu and Ag).
Determination of metallic
elements in biological materials
 Determination of trace metals.
 Organic matter is decomposed with 50% H2O2.
 Used in combination with conc HNO3 or H2SO4
 The acid depends on the nature of trace metal.
Determination of metallic
elements in food industry
 Copper , zinc and nickel.
 Extract trace elements by digestion with dilute
H2SO4 or with HNO3 or with 50% H2O2.
Determination of Ca, Mg ,Na and K
in blood serum
 Diagnosing many pathological conditions, diabetes
and primary aldosterionism.
 Dilute serum sample 10 , 20 or even 50 times in
presence of LaCl3.
 Aspirate in AA spectrophotometer and measure the
absorbance.
 Compare with aqueous standard solutions.
 Ca and Mg can be estimated in presence of LaCl3.
 Na and K can be determined by operating AA
spectrophotometer in emission mode in dilutions of
50 or 100:1.
Determination of lead in petrol
 Direct method.
 Indirect method.
Direct method :
 Used when nature of additive is known.
 Standard solution containing TEL/TML are prepared
in cyclohexanone.
 For TML the range of standard is 0.5 μg/ml.
 For TEL 0-50μg/ml.
 Aspiration at 283.3nm using air- acetylene mixture.
Indirect method:
 Nature of the lead additive is not known.
 Standard solution of lead containing 50, 25 , 10
and 5μg/ml are prepared in de-ionised water.
 Absorbance is measured at 283.3 nm .
 Treat petrol sample with bromine and extract with
dilute HNO3.
 Aspirated to AA spectrophotometer and record
absorbance.
 Pb= (s2-s1/s0-s2)(c)(1/10*s.g of original sample)
Also used for:
 Determination of Mg in tap water.
 Determination of Va in lubricating oil.
 Estimation of zinc in zinc insulin injection.
 Estimation of mercury in thiomersal solution.
Atomic Absorption Spectroscopy Applications

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Atomic Absorption Spectroscopy Applications

  • 1. PRESENTED BY, DEVIPRIYA P V M MPARM Department of Pharmaceutical Analysis
  • 2.  Valid applications in every branch of chemical analysis.  An established procedure in analytical chemistry, ceramics, mineralogy, biochemistry, water supplies, metallurgy and soil analysis.
  • 3. 1. Qualitative analysis. 2. Quantitative analysis. 3. Simultaneous multi-component analysis. 4. Determination of metallic elements in biological materials. 5. Determination of metallic elements in food industry. 6. Determination of Ca, Mg, Na and K in blood serum. 7. Determination of lead in petrol.
  • 4. Qualitative analysis  Different hollow cathode lamps are to be used for each element.  Only the element used in hollow cathode lamp can be detected.  Checking one element at a time.  Rarely used.
  • 5. Quantitative analysis  Based on the determination of amount of radiation absorbed by the sample.  Amount of light absorbed = (πe2 / mc)Nf  Quantitative measurements are based on calibration curves.  The absorbance values are plotted versus concentrations.  concentration of unknown solution is calculated using equation: A= mc Absorbance = slope * concentration.
  • 6. Sensitivity limits ELEMENT Å SENSITIVITY (ppm) Al 3092 1 Ca 4427 0.05 Cu 3247 0.1 Pb 2170 0.01 Ni 2320 0.1 K 7665 0.01 Na 5890 0.01 Zn 3601 50.0 Mg 2852 0.001 Hg 2537 1.0 Fe 2843 0.1 Ba 5535 0.2 Ag 3281 0.01
  • 8.  The parameters that influence a quantitative determination and need to be controlled are: : Flame system : Wavelength : Solution.
  • 9. Simultaneous multi-component analysis  If multi-component emission source is available.  Mitchell (1973) described a multielement atomic absorption system using a multielement hollow cathode source and a vidiocon detection system.  Spectral region from 2320 to 3281 Å.  Detect 8 elements (Zn, Cd, Ni, Co, Fe, Mn, Cu and Ag).
  • 10. Determination of metallic elements in biological materials  Determination of trace metals.  Organic matter is decomposed with 50% H2O2.  Used in combination with conc HNO3 or H2SO4  The acid depends on the nature of trace metal.
  • 11.
  • 12. Determination of metallic elements in food industry  Copper , zinc and nickel.  Extract trace elements by digestion with dilute H2SO4 or with HNO3 or with 50% H2O2.
  • 13. Determination of Ca, Mg ,Na and K in blood serum  Diagnosing many pathological conditions, diabetes and primary aldosterionism.  Dilute serum sample 10 , 20 or even 50 times in presence of LaCl3.  Aspirate in AA spectrophotometer and measure the absorbance.  Compare with aqueous standard solutions.  Ca and Mg can be estimated in presence of LaCl3.  Na and K can be determined by operating AA spectrophotometer in emission mode in dilutions of 50 or 100:1.
  • 14. Determination of lead in petrol  Direct method.  Indirect method. Direct method :  Used when nature of additive is known.  Standard solution containing TEL/TML are prepared in cyclohexanone.  For TML the range of standard is 0.5 μg/ml.  For TEL 0-50μg/ml.  Aspiration at 283.3nm using air- acetylene mixture.
  • 15. Indirect method:  Nature of the lead additive is not known.  Standard solution of lead containing 50, 25 , 10 and 5μg/ml are prepared in de-ionised water.  Absorbance is measured at 283.3 nm .  Treat petrol sample with bromine and extract with dilute HNO3.  Aspirated to AA spectrophotometer and record absorbance.  Pb= (s2-s1/s0-s2)(c)(1/10*s.g of original sample)
  • 16. Also used for:  Determination of Mg in tap water.  Determination of Va in lubricating oil.  Estimation of zinc in zinc insulin injection.  Estimation of mercury in thiomersal solution.