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ATOMIC
ABSORPTION
SPECTROMETRY
SPECTROMETRY
Defined as
measurement of
intensity of light at
selected wavelength
Widely used method of
Quantitative and
Qualitative analysis
Types of spectrometry
Visible
Spectrophotometer
Ultraviolet-visible
spectrophotometer
Infrared
spectrophotometer
Flourescence
Spectrophotometer
Atomicc absorption
spectrophotometer
Atomic emission
spectrophotometer
AAS
Introduced by Alan
Walsh in 1955
Used for mining, medical
treatment and agriculture
Introduction
Commonly used to detect metals and metalloids in sample like
Aluminium Copper Lithium Magnesium Zinc etc
Used to measure concentration by detecting absorption of
electromagnetic radiation by atom rather than by molecules
Elements detectable by atomic absorption in the periodic table
PRINCIPLE
Technique in which a metallic atom in the sample absorbs light of a specific wavelength
Element is merely atomized and placed in a ground state
This ground state absorbs radiation at a bandwidth corresponding to it’s own line spectrum
A hollow cathode lamp with the cathode made of material to be analysed is used to produce a wavelength of
light specific for atom
When light from the cathode lamp enters the flame, some of it is absorbed by ground state atoms in the flame,
resulting in net decrease in intensity of beam from lamp
This process is called atomic absorption
Concentration measurements are determined after calibrating the instrument with standards of known
concentration
Components
Light Source Chopper Atomizer Monochromator Detector
Light Source
•A hollow cathode lamp cathode made
of material to be analyzed is used to produce a
wavelength of light specific for the atom
• It usually contains argon or neon gas at a pressure
of a few millimeters of mercury.
CHOPPER
A rotating wheel interposed between hollow cathode lamp and flame
It breaks steady light into pulsating light which is used to measure intensity of
light absorbed by elements without interference by radiaytion from flame itself
Pulsting light gives pulsating current in photocell
There is also steady current caused by light which is emitted by flame. But only
pulsating current is amplified and recorded
Atomizer
• Atomization is separation of particles into individual
molecules and breaking molecules into atoms.
• This is done by exposing the analyte to high temperatures in
a flame or graphite furnace
• Flame - air acetylene is used to generate flame
• Graphite tube - The graphite coated tubes are heated by high
current supply
Nebulizer
• Sucks up liquid at controlled rate & creates fine aerosol that
is mixed with the fuel & oxidant for introduction in to the flame
Monochromator
This is a very important part in an AA spectrometer.
A monochromator is used to select the specific wavelength of light
which is absorbed by the sample, and to exclude other wavelengths.
The selection of the specific light allows the determination of the
selected element in the presence of others.
Detector
Light selected by the monochromator - detector
(photomultiplier tube)
Which converts light signal into an electrical signal
proportional to the light intensity.
The processing of electrical signal is fulfilled by a signal
amplifier .
Calibration curve
•Calibration - known solutes
•Calibration curve of concentration vs absorbance is plotted.
•The absorbance of the element in this solution is measured .
•The unknown concentration of the element is then calculated from
the calibration curve
TYPES OF AAS
Flame AAS
F L A ME
T E M PERATURE
F O R VA R IOUS
G A S M IXT U RE
Flame AAS
• short analysis time
• good precision
• Easy to use
• cheap
Advantages
• Sensitivity
• Dynamic Range
• requires flammable gas
• Unattended operation not possible because of flammable gas
• must not contain excessive amount of dissolved solids
Limitation
GRAPHITE
FURNACE AAS
Graphite Furnace AAS
Advantages
• Small sample sizes
• Very little or no sample preparation
• High sensitivity due to
• Entire sample is atomized at one time
• Free atoms remain in optical path longer
• Reduced sample volume
• Ultra trace analysis possible
Limitation
• very slow
• fewer eleme nts can be analysed
• poorer precision
• more chemical interferences
• method development requires skill
• standard additions calibrations required more frequently
• expensive consumables
Spectral
Absorbance by molecular
species
Scattering by non volatile
salt particles ,oxides ..etc
Absorbance by closely
absorbing atoms
Non
spectral
Specific
Solute volatilization interference eg :
Po4 forms complexes with ca
Dissociation interference
Eg: Oxides & hydroxides etc
Ionization interference
Non specific
Viscosity
Surface tension
Density of analyte
INTERFERENCES
Microwave Digestion Sysytem
• MDS is technique for converting solid
samples into solutions suitable for analysis
by AAS
• Solid sample is chemically digested using
liquid reagent by microwave heating in a
closed container
• Closed container generates temp upto 260
degree Celsius which accelerates
digestion process
LEADCARE® II BLOOD LEAD
ANALYZER
About the LeadCare II
Blood Lead Analyzer
It is a portable device for testing
the amount of lead in capillary
whole blood.
How the LeadCare II System Works
The LeadCare II System uses an electrochemical
technique called Anodic Stripping Voltammetry (ASV)
to determine the amount of lead in a blood sample
Blood is mixed with LeadCare Treatment
Reagent and the red blood cells (RBC)
are lysed, which releases the lead that is
bound to the RBC wall.
A negative potential is applied to the sensor
to accumulate lead atoms on the test
electrode. The potential is rapidly reversed
releasing the lead ions.
The current produced is directly proportional
to the amount of lead in the sample. The area
underneath the curve is used to calculate a
quantitative blood lead result.
1
3
2 Reduction step Oxidation (stripping) step
The testing procedure consists of the following steps:
1. Verify you have the required materials.
2. Perform quality control testing on both levels of quality control and
verify the results are within the acceptable ranges.
3. Collect capillary blood sample. Check the capillary tube for correct
filling.
4. Add blood to the treatment reagent tube.
5. Insert a sensor and match the sensor lot number with the display.
6. Using a dropper, obtain sample from the treatment reagent tube,
touch the dropper tip to the X on the sensor and squeeze the walls to
dispense the sample.
7. Read and record the test result.
8. Remove used sensor.
STEP 1:
COLLECT BLOOD
STEP 2:
PREPARE
SAMPLE
STEP 3:
ANALYZE THE
SAMPLE
Interpreting Patient
Test Results
The result is in micrograms (μg) of lead per
deciliter (dL) of whole blood
No calculation is needed.
The reportable range of the LeadCare II system is
3.3 to 65 μg/dL.
“Low” in the display window indicates a blood
lead test result less than 3.3 μg/dL.
“High” in the display window indicates a blood
lead test result greater than
65 μg/dL
“High” results on LeadCare II should be
followed up immediately as an emergency
laboratory test.
AAS.pptx

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AAS.pptx

  • 2. SPECTROMETRY Defined as measurement of intensity of light at selected wavelength Widely used method of Quantitative and Qualitative analysis
  • 4. AAS Introduced by Alan Walsh in 1955 Used for mining, medical treatment and agriculture
  • 5. Introduction Commonly used to detect metals and metalloids in sample like Aluminium Copper Lithium Magnesium Zinc etc Used to measure concentration by detecting absorption of electromagnetic radiation by atom rather than by molecules
  • 6. Elements detectable by atomic absorption in the periodic table
  • 7. PRINCIPLE Technique in which a metallic atom in the sample absorbs light of a specific wavelength Element is merely atomized and placed in a ground state This ground state absorbs radiation at a bandwidth corresponding to it’s own line spectrum A hollow cathode lamp with the cathode made of material to be analysed is used to produce a wavelength of light specific for atom When light from the cathode lamp enters the flame, some of it is absorbed by ground state atoms in the flame, resulting in net decrease in intensity of beam from lamp This process is called atomic absorption Concentration measurements are determined after calibrating the instrument with standards of known concentration
  • 8.
  • 9. Components Light Source Chopper Atomizer Monochromator Detector
  • 10. Light Source •A hollow cathode lamp cathode made of material to be analyzed is used to produce a wavelength of light specific for the atom • It usually contains argon or neon gas at a pressure of a few millimeters of mercury.
  • 11. CHOPPER A rotating wheel interposed between hollow cathode lamp and flame It breaks steady light into pulsating light which is used to measure intensity of light absorbed by elements without interference by radiaytion from flame itself Pulsting light gives pulsating current in photocell There is also steady current caused by light which is emitted by flame. But only pulsating current is amplified and recorded
  • 12. Atomizer • Atomization is separation of particles into individual molecules and breaking molecules into atoms. • This is done by exposing the analyte to high temperatures in a flame or graphite furnace • Flame - air acetylene is used to generate flame • Graphite tube - The graphite coated tubes are heated by high current supply Nebulizer • Sucks up liquid at controlled rate & creates fine aerosol that is mixed with the fuel & oxidant for introduction in to the flame
  • 13. Monochromator This is a very important part in an AA spectrometer. A monochromator is used to select the specific wavelength of light which is absorbed by the sample, and to exclude other wavelengths. The selection of the specific light allows the determination of the selected element in the presence of others.
  • 14. Detector Light selected by the monochromator - detector (photomultiplier tube) Which converts light signal into an electrical signal proportional to the light intensity. The processing of electrical signal is fulfilled by a signal amplifier .
  • 15. Calibration curve •Calibration - known solutes •Calibration curve of concentration vs absorbance is plotted. •The absorbance of the element in this solution is measured . •The unknown concentration of the element is then calculated from the calibration curve
  • 18. F L A ME T E M PERATURE F O R VA R IOUS G A S M IXT U RE
  • 19.
  • 20. Flame AAS • short analysis time • good precision • Easy to use • cheap Advantages • Sensitivity • Dynamic Range • requires flammable gas • Unattended operation not possible because of flammable gas • must not contain excessive amount of dissolved solids Limitation
  • 22. Graphite Furnace AAS Advantages • Small sample sizes • Very little or no sample preparation • High sensitivity due to • Entire sample is atomized at one time • Free atoms remain in optical path longer • Reduced sample volume • Ultra trace analysis possible Limitation • very slow • fewer eleme nts can be analysed • poorer precision • more chemical interferences • method development requires skill • standard additions calibrations required more frequently • expensive consumables
  • 23. Spectral Absorbance by molecular species Scattering by non volatile salt particles ,oxides ..etc Absorbance by closely absorbing atoms Non spectral Specific Solute volatilization interference eg : Po4 forms complexes with ca Dissociation interference Eg: Oxides & hydroxides etc Ionization interference Non specific Viscosity Surface tension Density of analyte INTERFERENCES
  • 24. Microwave Digestion Sysytem • MDS is technique for converting solid samples into solutions suitable for analysis by AAS • Solid sample is chemically digested using liquid reagent by microwave heating in a closed container • Closed container generates temp upto 260 degree Celsius which accelerates digestion process
  • 25. LEADCARE® II BLOOD LEAD ANALYZER
  • 26. About the LeadCare II Blood Lead Analyzer It is a portable device for testing the amount of lead in capillary whole blood.
  • 27. How the LeadCare II System Works The LeadCare II System uses an electrochemical technique called Anodic Stripping Voltammetry (ASV) to determine the amount of lead in a blood sample
  • 28. Blood is mixed with LeadCare Treatment Reagent and the red blood cells (RBC) are lysed, which releases the lead that is bound to the RBC wall. A negative potential is applied to the sensor to accumulate lead atoms on the test electrode. The potential is rapidly reversed releasing the lead ions. The current produced is directly proportional to the amount of lead in the sample. The area underneath the curve is used to calculate a quantitative blood lead result. 1 3 2 Reduction step Oxidation (stripping) step
  • 29. The testing procedure consists of the following steps: 1. Verify you have the required materials. 2. Perform quality control testing on both levels of quality control and verify the results are within the acceptable ranges. 3. Collect capillary blood sample. Check the capillary tube for correct filling. 4. Add blood to the treatment reagent tube. 5. Insert a sensor and match the sensor lot number with the display. 6. Using a dropper, obtain sample from the treatment reagent tube, touch the dropper tip to the X on the sensor and squeeze the walls to dispense the sample. 7. Read and record the test result. 8. Remove used sensor.
  • 33. Interpreting Patient Test Results The result is in micrograms (μg) of lead per deciliter (dL) of whole blood No calculation is needed. The reportable range of the LeadCare II system is 3.3 to 65 μg/dL. “Low” in the display window indicates a blood lead test result less than 3.3 μg/dL. “High” in the display window indicates a blood lead test result greater than 65 μg/dL “High” results on LeadCare II should be followed up immediately as an emergency laboratory test.