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Gamal A. Hamid
AtomicAbsorption
2
Thanks
To everyone who has helped us with support,
new books, hard/soft ware And over the internet
Special thanks for Thermo
http://www.thermofisher.com
AtomicAbsorption
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Contents
 Introduction
 Theory
 AAS Setup
 Validity
 Accessories
 Techniques and facilities
 Software
 Application
o Air
o Water & Soil
o Foods
o Clinical
o Petrochemicals
o Pharmaceutical
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Metals
 Metals account for about two thirds of
all the elements and about 24% of the
mass of the planet.
 Metals have useful properties including
strength, ductility, high melting points,
thermal and electrical conductivity, and
toughness.
 From the periodic table, it can be seen
that a large number of the elements
are classified as being a metal.
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Abundance of Metals in Earth’s crust
 Aluminum (7.5%)
 Iron (4.71%)
 Calcium (3.39%)
 Sodium (2.63%)
 Potassium (2.4%)
 Magnesium (1.93%)
 Titanium (0.58%)
 Manganese (0.09%)
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Abundance of Metals in the Human Body
 Calcium (1.4%)
 Magnesium (0.50%)
 Potassium (0.34%)
 Sodium (0.14%)
 Iron (0.004%)
 Zinc (0.003%)
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Toxic and nutrition elements
 Toxic metals
Pb, Cd, As, Hg, Al, Cr, Cu
 Nutrition elements
Ca, Mg, Na, K, P
 Micro-nutrients
Zn , Se, Mo, etc…
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Heavy metals
 Heavy metals are natural components of
the Earth's crust. They cannot be degraded
or destroyed.
 To a small extent they enter our bodies via
food, drinking water and air.
 As trace elements, some heavy metals (e.g.
copper, selenium, zinc) are essential to
maintain the metabolism of the human
body.
 However, at higher concentrations they
can be toxic.
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Absorption
 The process whereby the intensity of a
beam of electromagnetic radiation is
attenuated in passing through a material
medium by conversion of the energy of the
radiation to an equivalent amount of
energy appearing within the medium;
 The radiant energy is converted into heat
or some other form of molecular energy.
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The beer – Lambert Law
 The absorption that takes place in an atomic
absorption system follows beer law.
 A beam of light with intensity I0 is aimed at the
tested solution placed in a cuvette.
 The intensities of the entering beam I0 and the
emerging beam I1 are measured, and the absorbance
A - is calculated from the ratio of the two
A = - log (I1/I0)
 Different molecules absorb radiation of different
wavelengths. An absorption spectrum will show a
number of absorption bands corresponding to
structural groups within the molecule
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Atomic Absorption
Atomic absorption spectrometry
(AAS) is an analytical technique used
to measure a wide range of elements
concentration in samples.
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Atomic Absorption
Atomic absorption Mean
“The free atoms (Atomic)of the sprayed
element solution Absorbed
(Absorption)the radiation of the Hollow
cathode lamp of the analyzed element”
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Analyzed Elements
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Calibration
Optical absorption spectrometry is a
comparative technique in which the
signals by solutions of known
concentrations used to generate a
calibration curve is compared to the
signals of unknown samples to generate
results.
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AA Steps
 The sample is weighed and then dissolved.
 The resulting solution is sprayed into the
flame and atomized.
 Light of a suitable wavelength for a particular
element is shone through the flame.
 Some of this light is absorbed by the atoms of
the sample.
 The amount of light absorbed is proportional
to the concentration of the element .
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AA main parts
1. Lamp
2. Atomizer
3. Monochromator
4. Photomultiplier tube
5. Optical system
6. Automatic gas control
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1. Lamps
 Hollow Cathode Lamps (HCLs) are high
intensity, stable light sources that emit the
element specific spectral lines required for
Atomic Absorption spectrometry.
 Provide a constant intense beam of
analytical light.
 There are Coded or uncoded lamps.
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Deuterium Lamp
 The deuterium lamp emits radiation extending from 112
nm to 900 nm, although its continuous spectrum is only
from 180 nm to 300 nm.
 The Deuterium lamp emits a blue-white light.
 However, these lamps are used to produce Ultra-Violet
(UV) emissions which we can't see.
 The outer lamp envelope is made form quartz rather than
glass. because glass does not transmit short wave UV light.
 What makes Deuterium lamps so special, as a UV source,
is its continuous spectrum in the range from 180nm - 300
nm.
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Background
 Background interference is caused by either, non-specific absorption arising from light
scattering caused by solid particles or liquid droplets in the atomizing cell or, by light
absorption caused by molecules or radicals originating in the sample matrix.
 It is usually measured by separate experiment and subtracted from the absorption of the
sample solution.
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Background Correction
 The cathode lamp and the deuterium lamp are
sequentially pulsed with a chopper or electronically
with delay of about 2ms.
 When hollow cathode lamp is on and deuterium
lamp off total absorbance (AA + BG) is measured.
 When the HCL is off and the deuterium lamp on the
continuum energy recorded is (BG).
 The atomic signal is automatically calculated by
subtracting background from total absorbance.
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Zeeman Background
 Zeeman Background Correction is used
mainly in graphite furnace atomic
absorption systems. When an atom is
placed in a magnetic field and its
absorption of observed in polarized
light, the normal single line is split into
three components – б-, π and б
+displaced symmetrically about the
normal position
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Zeeman Background Correction
 Free atoms show Zeeman splitting in a magnetic field but molecules, liquid droplets
or solid particles show no Zeeman splitting and so advantage can be taken of
polarized light.
 The π component is linearly polarized parallel to the magnetic field while the б
components are circularly polarized perpendicular to the magnetic field.
 A polarizer is positioned in the optical system to remove the π components of the
transmitted radiation.
 This affords background measurement at the exact analyte wavelength when
magnetic field is applied. Since the background is measured at the analyte
wavelength and not averaged as in D2 system structural molecular background and
spectral interferences are easily corrected.
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2. Atomizers
 Metal in the sample must undergo
desolation and vaporization in a
high-temperature source such as a
flame or graphite furnace to be free
atoms.
 Destroy any analyte ions and
breakdown complexes
Create atoms (the elemental form)
of the element of interest
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Types of Atomizers
Atomizers main function is to generate a
free atoms.
1. Flame
2. Graphite
3. Hydride System
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3. Monochromator
 A monochromator is an optical device that
transmits a mechanically selectable narrow band
of wavelengths of light or other radiation chosen
from a wider range of wavelengths available at the
input.
 Echelle monochromator provides automatic
wavelength and band pass set-up.
 The high energy Quad Line background correction
system corrects for up to 2A of background with
less than 2 % error, and is fitted as standard to all
instruments.
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The Grating
 Grating An optical device within the
spectrometer used to separate the emitted light
into its component wavelengths.
 The grating has a dual feature: it diffracts the
light and focuses it on the slits.
 The grating is the main optic part of the
spectrometer;
 It separates the light into all the wavelength
that composes it.
 It Has 1800 grooves/mm.
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4. Photo multiplier tube PMT
 The PMT change the incidence
photons into electrical signal
 As the detector the PMT determines
the intensity of photons of the
analytical line exiting the
monochromator
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5. Optical System
Furnace
Toroid
Mirror
Flame Toroid Mirror
Plane Mirror
Rear Beam
Selector
Furnace
Plane
Mirror
Flame
HCL Carousel
D2 Lamp
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Auto-aligning Optics
 Perfect setup every time
 Auto-alignment and memory
 Lamp carousel for 6 lamps
 Dedicated power supply for each
position
 Data coding of both element and
lamp current
 High optical modulation frequency
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6. Automatic Gas Control
 Full safety monitoring facilities and safe
shutdown.
 Completely enclosed “kitchen” area.
 Automatic binary flow gas control system for
superb reliability and reproducibility.
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AA Analytical methods
A- Flame Atomic Absorption.
B- Furnace Atomic Absorption.
C- Vapor Atomic Absorption.
Flame
Furnace
Vapor
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A- Flame Atomic Absorption
 Atomization through flame
Air- Acetylene (9 psi) .
Air- Acetylene -Nitrous oxide
 Nitrous oxide (N2O) needs to be used with air (78%
N2 + 21% O2)
 The level of measuring is about mg/l (ppm)
 Support gases
Air 2.07 bar (30psi)
Nitrous oxide 2.75 bar (40psi)
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Flame System
 Universal Finned Titanium 50mm burner suitable for air/acetylene and nitrous
oxide/acetylene flame types.
 An inert fluoroplastic spray chamber incorporating an externally adjustable inert
impact bead and flow spoiler.
 An inert over-pressure membrane should be housed in the rear of the spray
chamber for maximum operator safety.
 Automatic gas system using binary flow control and programmable array state
logic for reliability
 Full safety interlocks, including pressure sensors on both lines, power failure
protection, burner interlock and flame sensor
 Fuel and oxidant flow rates software controllable
 Automatic flame ignition and optimization
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Flame Safety
 If carbon deposits appear, the flame
must be extinguished immediately
and the deposits removed.
 Aspiration of solutions of perchloric
acid and metal per chlorates into a
nitrous oxide supported flame can
increase the risk of explosion or
flashback
 Certain elements, notably Ag, Au
and Cu, can form unstable
acetylides, increasing the risk of
explosion or flashback.
 The use of organic solvents in flame
AAS is an inherently hazardous
procedure.
 The door must be closed when
lighting a flame, and during normal
operation.
 All flames produce large quantities
of heat and toxic combustion
products. These must be removed
by a suitable fume extraction
system.
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Burners
Two types of burner are available for
spectrometer:
 5 cm slot Universal Titanium Burner
suitable for general purpose use with all
flame types
 10 cm slot Titanium Burner
suitable for air/acetylene flames only.
Sensitivity for elements measured with this
flame will be improved compared to the
Universal Burner.
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B- Furnace atomic Absorption
 Electrothermal atomization (ETA) is a
technique for improving the sensitivity and
limit-of-detection (1000 times) for atomic
absorption measurements.
 A small amount of sample or standard
solution is placed inside a hollow graphite
tube.
 This is resistively-heated in a temperature
program to remove liquid, burn off organics,
atomize the residuals to form a plume of free
metal vapour, detect the metals and finally
clean the tube.
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Furnace main parts
The furnace main Technique parts
1. Electrical Thermal heating "power supply”.
2. Furnace head.
3. Auto sampler.
4. Shield and cleaning gas.
5. Cooling system.
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Furnace System
 Choice of Deuterium or Zeeman background correction furnaces
 Mount directly in dedicated compartment
 Binary flow controlled internal gas system
 Choice of alternate or inert gases
 Furnace cycle to allow up to 20 phases to be programmed
 Cuvette firings counter
 Furnace auto-sampler to be included with furnace head and power supply
 Slow injection and uptake options
 Wash and waste vessels to be part of the auto-sampler system and not occupy
extra space on the floor or bench of the laboratory
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Furnace Program
The main four Furnace programs
1. Drying phase, where the sample is
warmed to remove the solvent.
2. Ashing phase, where as much of the
sample matrix as possible is removed.
3. Atomization or measurement phase.
4. Cleaning phase, where the cuvette is
heated to a high temperature to
remove any previous sample.
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1. Furnace power supply
 200/220/240V at 50/60 Hz, 30A Single phase.
 Power consumption 7.2kVA. GF95Z - additional 1.5kVA
Description
 All cuvettes mount directly in an all-graphite containment
with end loaded contacts.
 Cuvettes are self aligning, and can be rapidly exchanged
with a single lever movement.
 The binary flow controlled internal gas system, with gas
stop, offers a choice of the inert gas or an alternate gas,
and the fixed external inert gas flow protects the cuvette
and purges the optical temperature sensor.
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2. Furnace Head
 Dynamic, optical cuvette temperature control, pre-heated
cuvette injection and coolant water temperature
compensation optimize analyses
 All graphite containment reduces contamination risk
 Very wide range of alternative cuvettes: Extended Lifetime
Cuvettes (ELC) provide uninterrupted overnight analysis and
lower cost of ownership
 Ash/Atomize self-optimization with SOLAAR software
 Maximum furnace sensitivity and the widest furnace dynamic
working range Correction up to 2A of background, with <2%
residual error for even the fastest transient signals
 The optional Zeeman Background Correction is performed at
the exact analyte wavelength
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The Zeeman Background
 The Zeeman background is the
splitting of spectral lines into several
polarized components as a result of
the effect of an applied magnetic field.
 On the application of the magnetic
field a central line appears at the same
wavelength as the original line (the π
line) having half the intensity of the
original line.
 On either side of the π line appears
two other lines (the σ± lines) having
one quarter of the intensity of the
original line.
 The π line is linearly polarized with the
electric vector parallel to the magnetic
field and the σ± lines are circularly
polarized at right angles to the
direction of the magnetic field.
 the π line is absorbed by both sample
and back ground whereas the σ±
components are only absorbed by the
background.
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Zeeman Background
 The magnet fitted to the GF95Z
Zeeman Furnace Head produces a
variable magnetic field up to 0.85
Tesla at mains frequency during the
atomization and auto zero phases.
 This can affect other electronic
systems in the vicinity.
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Cuvettes
 Normal Cuvettes (Electro graphite)
 Volatile elements
 Coated Electro graphite (Pyrolytically coated)
 Carbide forming elements
 Medium volatile
 Refractory elements
 Extended Life-time Cuvettes (ELC’s)
 More stable
 Omega Platform ELC’s
 Volatile elements in ‘heavy’ matrices
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3. Autosampler
Features of the Furnace Autosampler
1. Automatic matrix modification - wet and dry
mixing options .
2. Automatic standard preparation - fixed and
variable volume may be used
3. Automatic re-concentration of samples, using
multiple injections .
4. Automatic, intelligent dilution of samples
5. Automatic standards addition preparation
6. Automatic re-scale and re-calibration
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4. Argon Gas
 This protects the hot cuvette from atmospheric
oxygen, and flushes sample vapours from the
cuvette interior.
 Argon is recommended; nitrogen can be used
with some loss of performance for some
elements.
 Connect the inert gas supply to the inlet port
labeled ARGON 2 at the rear of the Furnace
Power Supply unit.
 The inert gas supply must be regulated to
1.1±0.14 bar (15±2 psi).
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5. Cooling System
 A supply of reasonably clean (e.g. drinking) water, at a temperature of less than
30ºC and a pressure of 1.4 to 6.9 bar (20 - 100psi), capable of providing a
minimum flow rate of 0.7l/min is required.
 Do not allow the pressure to exceed 6.9 bar (100 psi).
 Connect the cooling water inlet and outlet hoses to the water inlet and outlet
connections on the Furnace Power Supply unit.
Recirculators
 The Furnace can be cooled by a temperature controlled Recirculators/chiller unit
instead of mains water.
 Set the recirculating water temperature to about 5ºC above ambient
temperature, providing that this is less than 30ºC.
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Chiller
 An air-cooled re-circulating water chiller
shall be provided to cool.
 suitable for operation with an ambient
temperature range +15 C to + 35 C
 Highly efficient cooling
 Accurate temperature control
 Environmental friendly (CFC - free)
 Quiet operation
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C- Vapor Atomic Absorption
 Parts per billion sensitivities for a
number of environmentally
important elements are not
attainable by conventional flame
atomic absorption spectrometry
and alternative techniques have to
be used.
 Hydride generation AAS is
applicable to mercury and the
arsenic group elements, and
provides cost effective analysis with
sub-ppb detection limits.
 The elements that can be
determined with the VP100 are
those that can form gaseous
hydrides, or in the case of mercury,
a mono-atomic vapour.
 These include As, Se, Bi, Te, Sb, Sn,
and Hg.
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Vapor AA
 Detection limits typically 1000x better than
those achieved by conventional flame analysis
 Hydrochloric acid + sodium borohydride
unstable hydride of 8 elements give free atoms
Hg - As - Se – Sb
Ge - Bi - Sn – Te
 For a volatile elements in the range of ug/l
(ppb)
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Vapor Reaction
 As3+ NaBH4 AsH3 (gas) + B2H6
 AsH3 (gas) As + 3/2 H2
 The arsenic ions are reduced by the strong
reducing agent sodium borohydride (NaBH4)
and the arsenic hydride is formed.
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4 Channel peristaltic pump
 Full automation
 All functions controlled through
software
 Simple Installation and Plumbing
 4 Colour coded channels
 Single RS232C connection to
spectrometer
 Compatible with all SOLAAR
supported auto-samplers
 Channel 1 – Reductant
 Channel 2 – Acid Reagent
 Channel 3 – Sample
 Channel 4 – Drain
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Peristaltic pump
 Stepper motor driven
 Precise and accurate
 Software controlled
 Pump speed is now a Method parameter
 Flexible operation
 Optimise reagent
consumption/sensitivity trade off
 Repeatable results
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Sophisticated new design
Gas Liquid Separator new design
 Mixing manifold
 Reaction zone
 Phase separation zone
 Semi-permeable membrane
 Pumped drain
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Lab Requirements
Ensure avoidance of:
 Direct sunlight.
 Proximity to heat sources.
 Draughts, particularly from such items
as air conditioning vents and fans.
 Excessive vibration.
 temperature is maintained between
+ 5 oC and + 40 oC with a maximum
temperature variation of less than 2oC
per hour.
 Relative humidity should be
maintained between 20% and 80%.
 These instruments are designed for
operation in clean air conditions.
 The laboratory must be free of all
contaminants that could have a
degrading effect on the instrument
components.
 Dust, acid and organic vapours must
be excluded from the work area..
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Fume Extraction
 All flames produce large quantities of heat and toxic
combustion products.
 These must be removed by a suitable fume extraction
system. Specifications of a suitable extraction system
are provided in the Pre-Installation Manual.
 The fume extraction hood must not be attached to the
chimney, and an air-gap of between 150 and 230mm
must be made.
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Slotted Tube Trap
 This accessory enhances the flame
sensitivity for certain elements by 2-5
times.
 It consists of a slotted tube held in the
flame .
 NEVER ATTEMPT TO LIGHT OR
EXTINGUISH A FLAME WITH The stat in
the operational position.
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ID 100 Auto-dilutor
 This is an accessory that will provide automatic sample
dilution and standard preparation for flame AAS
 ID 100 is not compatible with VP90 AND VP 100.
 The ID100 Auto dilutor System can automatically prepare
working calibration standards from a single master standard
as they are needed, so that no manual dilution steps are
required.
 It also simplifies the task of handling over-range samples by
intelligently diluting them into the calibration range, thus
extending the effective working range.
 Full automation is possible by combining the ID100 with any
of the Thermo Elemental range of AA Flame autosampler.
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Auto-sampler ASX520-ASXR8
 ASX520 Auto sampler
 A workhorse auto sampler for
unattended analysis
 with a maximum load of 360
samples for busier laboratories
 EXR8 Auto sampler
 A large sample load of up to 720
samples with automatic,
 unattended analysis for high
throughput laboratories
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EC 90 Electric heating
 It replaces the Flame Heated Measurement
Cell with an Electrically Heated Atomization
Cell, so that Vapor measurements can be made
without a flame.
 The accessory consists of two parts:
1. The EC90 Furnace Head.
2. The EC90 Power Supply
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Furnace Vision System GF TV
 CCD camera provides high definition images
 Uses spectrometer optical path for a clear, direct,
on-axis view of the cuvet
 Simplified method development
 Accurate adjustment of capillary possible
 Perfect sample injection depth
 Drying and ashing phases can be easily optimised
 High quality and reproducible results
 Images can be captured and stored
Correct depth
Capillary too low
Capillary too high
Correct depth
Capillary too low
Capillary too high
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ISQ – Intelligent Spectrometer Qualification
ISQ is an automatic, software driven process to demonstrate that your spectrometer
hardware is performing consistently to specification over the intended operating ranges.
 Intelligent
 Identifies instrument in use
 Selects appropriate tests
 Software automatically controls tests
 Clear result display
 Spectrometer
 Tests the hardware of the spectrometer
 Helps to diagnose the source of any hardware problems at an early stage
 Qualification
 Verifies that the instrument is operating entirely within the designed specifications
 Confirms instrument is capable of producing sound analytical data.
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Validation of the Machine
Validation kit helps
1. Monitor the regulatory compliance status of
spectrometer.
2. Determine the conformity of an AA
spectrometer to internally established standards.
3. Provide confidence for managerial and regulatory
personnel that the system is under control
provide all the documentation, hardware and
standard solutions necessary for the
validation process.
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Validation Packages
Package contain
 Log book
 Ca/Mg lamp
 Ni/Cr/ Mn lamp
 Pyro coated cuvettes
 Ni, Cr, & Mn standard solutions
 ASTM type 1 water
 Optical filters
 Certificates
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Validation Unit
Tests performed
 Wavelength Accuracy
 Monochromator Resolution
 Photometric Accuracy
 Photometric Stability
 D2 Background Correction
 Polarizer Orientation
 Polarizer Repeatability
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Calibration
 Automatically peaks wavelength
 Automatically sets band pass
 Automatically adjusts lamp current
 Automatically recalls flame conditions
 Automatically balances D2 intensity
 Automatically sets baseline
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Applications
1. Environmental
2. Clinical
3. Pharmaceutical
4. Agriculture
5. Petrochemicals
6. Other’s
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1. Environmental Applications
 Waters – sea, fresh, waste
 Plant materials
 Soils, Sludge's and sediments
 Airborne particulates
 Biological samples
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Essential and Toxic elements
 Essential major elements
C N O P S Cl Na K Ca Mg
 Essential trace elements
F I Se V Cr Mn Fe Co Ni Cu ZnMo Si Sn As
 Toxic elements
Li Be Ba F Cl Br As Sb Bi Pb Sn Tl V Cr Mn Fe Co Ni Cu Zn Cd Hg
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2. Clinical Applications
 The majority of samples analysed are taken
from the main group of biological fluids, such
as whole blood, plasma, serum and urine.
 Hard and soft tissues, such as bone, finger
nails and hair
 Flame based analysis for the major and minor
essential elements, graphite furnace analysis
for the trace elements and vapour analysis for
the group of toxic
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Essential elements
 Essential major elements
Ca Mg Na K
 Essential minor elements
Zn Cu Fe
 Essential trace elements
Cr Mn Mo Co V Se Ni
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Toxic elements
 Toxic elements are often defined as those
that interfere with metabolic processes.
 The elements usually included in this group
are as follows:
 Lead, Mercury, Arsenic, Thallium, Cadmium,
Aluminum, Boron, Antimony.
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3. Pharmaceutical Applications
 Samples of diclofenac sodium for
Na, K, Ca and Al analysis
 Magnesium Stearate sample to be
analyzed for Cd, Ni and Pb.
 Samples of vitamin tablets Se
analysis
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Drug discovery and testing
 Most Pharmaceutical Companies these days
develop drugs which are targeted at specific
cells in the body.
 These drugs must be tested for correct
activity but more importantly for the absence
of any adverse side reactions.
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Toxic and nutrition elements
 Toxic metals
 Pb, Cd, As, Hg, Al, Cr, Cu
 Nutrition elements
 Ca, Mg, Na, K, P
 Micro-nutrients
 Zn , Se, Mo, etc…
 Process monitoring and control
 Fe, other transition elements in frying oil
 Ni in fat hydrogenation
 Levels vary with process, typically 1000 – 10PPM
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4. Agriculture Applications
 soil analysis provides a measure of a
soil‘s potential to supply the
necessary nutrients to plants.
 Plants may be sampled to monitor
nutrient uptake efficiency and also
to check for toxic metal
accumulation for health reasons.
AtomicAbsorption
85
Soil nutrient elements
 P, K, Ca, Mg Macro nutrients at %
level
 Cu, Fe, Mn, Zn Micro nutrients at
ppm level
 Al, B, Na, Mo, Se Other nutrient
elements
 As, Cd, Co, Cr, Ni, Pb Elements of
toxic interest
AtomicAbsorption
86
5. Petrochemical Applications
 Measure refinery contaminant elements
 Na, V, Fe, Ni by Flame-PPM
 Measure fuel elements
 Pb, Mn, usually low ppm-typically flame or furnace
 Measure lube oil elements
 Fresh - Ca, Ba, Mg, Zn, Mo, Na (flame)
 Used - Ag, Al, Cr, Fe, Mn, Ni, Pb, Sn, Ti, Zn (often furnace)
AtomicAbsorption
87
lubricating oils
 Every rotating mechanism in machinery of
all types depends on their use for smooth
operation.
 Like engines and gearboxes used in modern
transportation, such as aircraft, ships, cars
and lorries and heavy construction
equipment.
 Oils in use so that oil changes can be carried
out in time to prevent excessive wear
occurring in the components concerned.
AtomicAbsorption
88
Wear Metals
Wear metal Indicated condition
1 Silicon
Indicates dust intrusion, usually from improper air cleaner service.
Causes rapid engine wear and early failure.
2 Iron
Indicates wear originating from engine block, cylinder, gears, wrist
pins, rings (case iron), camshaft, oil pump, or crankshaft.
3 Copper
Usually indicates wear in bushings, injector shields, valve guides
,connecting rods, or piston pins.
4 Nickel
l Wear of plating on gears and certain
types of bearings.
5 Tin
Wear of certain types of bearings and coatings of connecting rods and
iron pistons
AtomicAbsorption
89
Wear Metals
Wear metal Indicated condition
6 Lead
In diesel engines indicates wear of bearings. In petrol engines fuel
blow by is indicated.
7 Chromium
Indicates ring wear or cooling system leakage if chromates are
used as inhibitors.
8 Aluminum
Indicates wear of pistons and certain
types of bearings.
9 Molybdenum
Indicates wear in certain types of
bearing alloys and in oil coolers.
Guide to Atomic Absorption Spectrometry

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Guide to Atomic Absorption Spectrometry

  • 2. AtomicAbsorption 2 Thanks To everyone who has helped us with support, new books, hard/soft ware And over the internet Special thanks for Thermo http://www.thermofisher.com
  • 3. AtomicAbsorption 3 Contents  Introduction  Theory  AAS Setup  Validity  Accessories  Techniques and facilities  Software  Application o Air o Water & Soil o Foods o Clinical o Petrochemicals o Pharmaceutical
  • 4.
  • 5. AtomicAbsorption 5 Metals  Metals account for about two thirds of all the elements and about 24% of the mass of the planet.  Metals have useful properties including strength, ductility, high melting points, thermal and electrical conductivity, and toughness.  From the periodic table, it can be seen that a large number of the elements are classified as being a metal.
  • 6. AtomicAbsorption 6 Abundance of Metals in Earth’s crust  Aluminum (7.5%)  Iron (4.71%)  Calcium (3.39%)  Sodium (2.63%)  Potassium (2.4%)  Magnesium (1.93%)  Titanium (0.58%)  Manganese (0.09%)
  • 7. AtomicAbsorption 7 Abundance of Metals in the Human Body  Calcium (1.4%)  Magnesium (0.50%)  Potassium (0.34%)  Sodium (0.14%)  Iron (0.004%)  Zinc (0.003%)
  • 8. AtomicAbsorption 8 Toxic and nutrition elements  Toxic metals Pb, Cd, As, Hg, Al, Cr, Cu  Nutrition elements Ca, Mg, Na, K, P  Micro-nutrients Zn , Se, Mo, etc…
  • 9. AtomicAbsorption 9 Heavy metals  Heavy metals are natural components of the Earth's crust. They cannot be degraded or destroyed.  To a small extent they enter our bodies via food, drinking water and air.  As trace elements, some heavy metals (e.g. copper, selenium, zinc) are essential to maintain the metabolism of the human body.  However, at higher concentrations they can be toxic.
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  • 11. AtomicAbsorption 11 Absorption  The process whereby the intensity of a beam of electromagnetic radiation is attenuated in passing through a material medium by conversion of the energy of the radiation to an equivalent amount of energy appearing within the medium;  The radiant energy is converted into heat or some other form of molecular energy.
  • 12. AtomicAbsorption 12 The beer – Lambert Law  The absorption that takes place in an atomic absorption system follows beer law.  A beam of light with intensity I0 is aimed at the tested solution placed in a cuvette.  The intensities of the entering beam I0 and the emerging beam I1 are measured, and the absorbance A - is calculated from the ratio of the two A = - log (I1/I0)  Different molecules absorb radiation of different wavelengths. An absorption spectrum will show a number of absorption bands corresponding to structural groups within the molecule
  • 13. AtomicAbsorption 13 Atomic Absorption Atomic absorption spectrometry (AAS) is an analytical technique used to measure a wide range of elements concentration in samples.
  • 14. AtomicAbsorption 14 Atomic Absorption Atomic absorption Mean “The free atoms (Atomic)of the sprayed element solution Absorbed (Absorption)the radiation of the Hollow cathode lamp of the analyzed element”
  • 16. AtomicAbsorption 16 Calibration Optical absorption spectrometry is a comparative technique in which the signals by solutions of known concentrations used to generate a calibration curve is compared to the signals of unknown samples to generate results.
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  • 18. AtomicAbsorption 18 AA Steps  The sample is weighed and then dissolved.  The resulting solution is sprayed into the flame and atomized.  Light of a suitable wavelength for a particular element is shone through the flame.  Some of this light is absorbed by the atoms of the sample.  The amount of light absorbed is proportional to the concentration of the element .
  • 19. AtomicAbsorption 19 AA main parts 1. Lamp 2. Atomizer 3. Monochromator 4. Photomultiplier tube 5. Optical system 6. Automatic gas control
  • 20. AtomicAbsorption 20 1. Lamps  Hollow Cathode Lamps (HCLs) are high intensity, stable light sources that emit the element specific spectral lines required for Atomic Absorption spectrometry.  Provide a constant intense beam of analytical light.  There are Coded or uncoded lamps.
  • 21. AtomicAbsorption 21 Deuterium Lamp  The deuterium lamp emits radiation extending from 112 nm to 900 nm, although its continuous spectrum is only from 180 nm to 300 nm.  The Deuterium lamp emits a blue-white light.  However, these lamps are used to produce Ultra-Violet (UV) emissions which we can't see.  The outer lamp envelope is made form quartz rather than glass. because glass does not transmit short wave UV light.  What makes Deuterium lamps so special, as a UV source, is its continuous spectrum in the range from 180nm - 300 nm.
  • 22. AtomicAbsorption 22 Background  Background interference is caused by either, non-specific absorption arising from light scattering caused by solid particles or liquid droplets in the atomizing cell or, by light absorption caused by molecules or radicals originating in the sample matrix.  It is usually measured by separate experiment and subtracted from the absorption of the sample solution.
  • 23. AtomicAbsorption 23 Background Correction  The cathode lamp and the deuterium lamp are sequentially pulsed with a chopper or electronically with delay of about 2ms.  When hollow cathode lamp is on and deuterium lamp off total absorbance (AA + BG) is measured.  When the HCL is off and the deuterium lamp on the continuum energy recorded is (BG).  The atomic signal is automatically calculated by subtracting background from total absorbance.
  • 24. AtomicAbsorption 24 Zeeman Background  Zeeman Background Correction is used mainly in graphite furnace atomic absorption systems. When an atom is placed in a magnetic field and its absorption of observed in polarized light, the normal single line is split into three components – б-, π and б +displaced symmetrically about the normal position
  • 25. AtomicAbsorption 25 Zeeman Background Correction  Free atoms show Zeeman splitting in a magnetic field but molecules, liquid droplets or solid particles show no Zeeman splitting and so advantage can be taken of polarized light.  The π component is linearly polarized parallel to the magnetic field while the б components are circularly polarized perpendicular to the magnetic field.  A polarizer is positioned in the optical system to remove the π components of the transmitted radiation.  This affords background measurement at the exact analyte wavelength when magnetic field is applied. Since the background is measured at the analyte wavelength and not averaged as in D2 system structural molecular background and spectral interferences are easily corrected.
  • 26. AtomicAbsorption 26 2. Atomizers  Metal in the sample must undergo desolation and vaporization in a high-temperature source such as a flame or graphite furnace to be free atoms.  Destroy any analyte ions and breakdown complexes Create atoms (the elemental form) of the element of interest
  • 27. AtomicAbsorption 27 Types of Atomizers Atomizers main function is to generate a free atoms. 1. Flame 2. Graphite 3. Hydride System
  • 28. AtomicAbsorption 28 3. Monochromator  A monochromator is an optical device that transmits a mechanically selectable narrow band of wavelengths of light or other radiation chosen from a wider range of wavelengths available at the input.  Echelle monochromator provides automatic wavelength and band pass set-up.  The high energy Quad Line background correction system corrects for up to 2A of background with less than 2 % error, and is fitted as standard to all instruments.
  • 29. AtomicAbsorption 29 The Grating  Grating An optical device within the spectrometer used to separate the emitted light into its component wavelengths.  The grating has a dual feature: it diffracts the light and focuses it on the slits.  The grating is the main optic part of the spectrometer;  It separates the light into all the wavelength that composes it.  It Has 1800 grooves/mm.
  • 30. AtomicAbsorption 30 4. Photo multiplier tube PMT  The PMT change the incidence photons into electrical signal  As the detector the PMT determines the intensity of photons of the analytical line exiting the monochromator
  • 31. AtomicAbsorption 31 5. Optical System Furnace Toroid Mirror Flame Toroid Mirror Plane Mirror Rear Beam Selector Furnace Plane Mirror Flame HCL Carousel D2 Lamp
  • 32. AtomicAbsorption 32 Auto-aligning Optics  Perfect setup every time  Auto-alignment and memory  Lamp carousel for 6 lamps  Dedicated power supply for each position  Data coding of both element and lamp current  High optical modulation frequency
  • 33. AtomicAbsorption 33 6. Automatic Gas Control  Full safety monitoring facilities and safe shutdown.  Completely enclosed “kitchen” area.  Automatic binary flow gas control system for superb reliability and reproducibility.
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  • 35. AtomicAbsorption 35 AA Analytical methods A- Flame Atomic Absorption. B- Furnace Atomic Absorption. C- Vapor Atomic Absorption. Flame Furnace Vapor
  • 36. AtomicAbsorption 36 A- Flame Atomic Absorption  Atomization through flame Air- Acetylene (9 psi) . Air- Acetylene -Nitrous oxide  Nitrous oxide (N2O) needs to be used with air (78% N2 + 21% O2)  The level of measuring is about mg/l (ppm)  Support gases Air 2.07 bar (30psi) Nitrous oxide 2.75 bar (40psi)
  • 37. AtomicAbsorption 37 Flame System  Universal Finned Titanium 50mm burner suitable for air/acetylene and nitrous oxide/acetylene flame types.  An inert fluoroplastic spray chamber incorporating an externally adjustable inert impact bead and flow spoiler.  An inert over-pressure membrane should be housed in the rear of the spray chamber for maximum operator safety.  Automatic gas system using binary flow control and programmable array state logic for reliability  Full safety interlocks, including pressure sensors on both lines, power failure protection, burner interlock and flame sensor  Fuel and oxidant flow rates software controllable  Automatic flame ignition and optimization
  • 38. AtomicAbsorption 38 Flame Safety  If carbon deposits appear, the flame must be extinguished immediately and the deposits removed.  Aspiration of solutions of perchloric acid and metal per chlorates into a nitrous oxide supported flame can increase the risk of explosion or flashback  Certain elements, notably Ag, Au and Cu, can form unstable acetylides, increasing the risk of explosion or flashback.  The use of organic solvents in flame AAS is an inherently hazardous procedure.  The door must be closed when lighting a flame, and during normal operation.  All flames produce large quantities of heat and toxic combustion products. These must be removed by a suitable fume extraction system.
  • 39. AtomicAbsorption 39 Burners Two types of burner are available for spectrometer:  5 cm slot Universal Titanium Burner suitable for general purpose use with all flame types  10 cm slot Titanium Burner suitable for air/acetylene flames only. Sensitivity for elements measured with this flame will be improved compared to the Universal Burner.
  • 40. AtomicAbsorption 40 B- Furnace atomic Absorption  Electrothermal atomization (ETA) is a technique for improving the sensitivity and limit-of-detection (1000 times) for atomic absorption measurements.  A small amount of sample or standard solution is placed inside a hollow graphite tube.  This is resistively-heated in a temperature program to remove liquid, burn off organics, atomize the residuals to form a plume of free metal vapour, detect the metals and finally clean the tube.
  • 41. AtomicAbsorption 41 Furnace main parts The furnace main Technique parts 1. Electrical Thermal heating "power supply”. 2. Furnace head. 3. Auto sampler. 4. Shield and cleaning gas. 5. Cooling system.
  • 42. AtomicAbsorption 42 Furnace System  Choice of Deuterium or Zeeman background correction furnaces  Mount directly in dedicated compartment  Binary flow controlled internal gas system  Choice of alternate or inert gases  Furnace cycle to allow up to 20 phases to be programmed  Cuvette firings counter  Furnace auto-sampler to be included with furnace head and power supply  Slow injection and uptake options  Wash and waste vessels to be part of the auto-sampler system and not occupy extra space on the floor or bench of the laboratory
  • 43. AtomicAbsorption 43 Furnace Program The main four Furnace programs 1. Drying phase, where the sample is warmed to remove the solvent. 2. Ashing phase, where as much of the sample matrix as possible is removed. 3. Atomization or measurement phase. 4. Cleaning phase, where the cuvette is heated to a high temperature to remove any previous sample.
  • 44. AtomicAbsorption 44 1. Furnace power supply  200/220/240V at 50/60 Hz, 30A Single phase.  Power consumption 7.2kVA. GF95Z - additional 1.5kVA Description  All cuvettes mount directly in an all-graphite containment with end loaded contacts.  Cuvettes are self aligning, and can be rapidly exchanged with a single lever movement.  The binary flow controlled internal gas system, with gas stop, offers a choice of the inert gas or an alternate gas, and the fixed external inert gas flow protects the cuvette and purges the optical temperature sensor.
  • 45. AtomicAbsorption 45 2. Furnace Head  Dynamic, optical cuvette temperature control, pre-heated cuvette injection and coolant water temperature compensation optimize analyses  All graphite containment reduces contamination risk  Very wide range of alternative cuvettes: Extended Lifetime Cuvettes (ELC) provide uninterrupted overnight analysis and lower cost of ownership  Ash/Atomize self-optimization with SOLAAR software  Maximum furnace sensitivity and the widest furnace dynamic working range Correction up to 2A of background, with <2% residual error for even the fastest transient signals  The optional Zeeman Background Correction is performed at the exact analyte wavelength
  • 46. AtomicAbsorption 46 The Zeeman Background  The Zeeman background is the splitting of spectral lines into several polarized components as a result of the effect of an applied magnetic field.  On the application of the magnetic field a central line appears at the same wavelength as the original line (the π line) having half the intensity of the original line.  On either side of the π line appears two other lines (the σ± lines) having one quarter of the intensity of the original line.  The π line is linearly polarized with the electric vector parallel to the magnetic field and the σ± lines are circularly polarized at right angles to the direction of the magnetic field.  the π line is absorbed by both sample and back ground whereas the σ± components are only absorbed by the background.
  • 47. AtomicAbsorption 47 Zeeman Background  The magnet fitted to the GF95Z Zeeman Furnace Head produces a variable magnetic field up to 0.85 Tesla at mains frequency during the atomization and auto zero phases.  This can affect other electronic systems in the vicinity.
  • 48. AtomicAbsorption 48 Cuvettes  Normal Cuvettes (Electro graphite)  Volatile elements  Coated Electro graphite (Pyrolytically coated)  Carbide forming elements  Medium volatile  Refractory elements  Extended Life-time Cuvettes (ELC’s)  More stable  Omega Platform ELC’s  Volatile elements in ‘heavy’ matrices
  • 49. AtomicAbsorption 49 3. Autosampler Features of the Furnace Autosampler 1. Automatic matrix modification - wet and dry mixing options . 2. Automatic standard preparation - fixed and variable volume may be used 3. Automatic re-concentration of samples, using multiple injections . 4. Automatic, intelligent dilution of samples 5. Automatic standards addition preparation 6. Automatic re-scale and re-calibration
  • 50. AtomicAbsorption 50 4. Argon Gas  This protects the hot cuvette from atmospheric oxygen, and flushes sample vapours from the cuvette interior.  Argon is recommended; nitrogen can be used with some loss of performance for some elements.  Connect the inert gas supply to the inlet port labeled ARGON 2 at the rear of the Furnace Power Supply unit.  The inert gas supply must be regulated to 1.1±0.14 bar (15±2 psi).
  • 51. AtomicAbsorption 51 5. Cooling System  A supply of reasonably clean (e.g. drinking) water, at a temperature of less than 30ºC and a pressure of 1.4 to 6.9 bar (20 - 100psi), capable of providing a minimum flow rate of 0.7l/min is required.  Do not allow the pressure to exceed 6.9 bar (100 psi).  Connect the cooling water inlet and outlet hoses to the water inlet and outlet connections on the Furnace Power Supply unit. Recirculators  The Furnace can be cooled by a temperature controlled Recirculators/chiller unit instead of mains water.  Set the recirculating water temperature to about 5ºC above ambient temperature, providing that this is less than 30ºC.
  • 52. AtomicAbsorption 52 Chiller  An air-cooled re-circulating water chiller shall be provided to cool.  suitable for operation with an ambient temperature range +15 C to + 35 C  Highly efficient cooling  Accurate temperature control  Environmental friendly (CFC - free)  Quiet operation
  • 53. AtomicAbsorption 53 C- Vapor Atomic Absorption  Parts per billion sensitivities for a number of environmentally important elements are not attainable by conventional flame atomic absorption spectrometry and alternative techniques have to be used.  Hydride generation AAS is applicable to mercury and the arsenic group elements, and provides cost effective analysis with sub-ppb detection limits.  The elements that can be determined with the VP100 are those that can form gaseous hydrides, or in the case of mercury, a mono-atomic vapour.  These include As, Se, Bi, Te, Sb, Sn, and Hg.
  • 54. AtomicAbsorption 54 Vapor AA  Detection limits typically 1000x better than those achieved by conventional flame analysis  Hydrochloric acid + sodium borohydride unstable hydride of 8 elements give free atoms Hg - As - Se – Sb Ge - Bi - Sn – Te  For a volatile elements in the range of ug/l (ppb)
  • 55. AtomicAbsorption 55 Vapor Reaction  As3+ NaBH4 AsH3 (gas) + B2H6  AsH3 (gas) As + 3/2 H2  The arsenic ions are reduced by the strong reducing agent sodium borohydride (NaBH4) and the arsenic hydride is formed.
  • 56. AtomicAbsorption 56 4 Channel peristaltic pump  Full automation  All functions controlled through software  Simple Installation and Plumbing  4 Colour coded channels  Single RS232C connection to spectrometer  Compatible with all SOLAAR supported auto-samplers  Channel 1 – Reductant  Channel 2 – Acid Reagent  Channel 3 – Sample  Channel 4 – Drain
  • 57. AtomicAbsorption 57 Peristaltic pump  Stepper motor driven  Precise and accurate  Software controlled  Pump speed is now a Method parameter  Flexible operation  Optimise reagent consumption/sensitivity trade off  Repeatable results
  • 58. AtomicAbsorption 58 Sophisticated new design Gas Liquid Separator new design  Mixing manifold  Reaction zone  Phase separation zone  Semi-permeable membrane  Pumped drain
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  • 60. AtomicAbsorption 60 Lab Requirements Ensure avoidance of:  Direct sunlight.  Proximity to heat sources.  Draughts, particularly from such items as air conditioning vents and fans.  Excessive vibration.  temperature is maintained between + 5 oC and + 40 oC with a maximum temperature variation of less than 2oC per hour.  Relative humidity should be maintained between 20% and 80%.  These instruments are designed for operation in clean air conditions.  The laboratory must be free of all contaminants that could have a degrading effect on the instrument components.  Dust, acid and organic vapours must be excluded from the work area..
  • 61. AtomicAbsorption 61 Fume Extraction  All flames produce large quantities of heat and toxic combustion products.  These must be removed by a suitable fume extraction system. Specifications of a suitable extraction system are provided in the Pre-Installation Manual.  The fume extraction hood must not be attached to the chimney, and an air-gap of between 150 and 230mm must be made.
  • 62.
  • 63. AtomicAbsorption 63 Slotted Tube Trap  This accessory enhances the flame sensitivity for certain elements by 2-5 times.  It consists of a slotted tube held in the flame .  NEVER ATTEMPT TO LIGHT OR EXTINGUISH A FLAME WITH The stat in the operational position.
  • 64. AtomicAbsorption 64 ID 100 Auto-dilutor  This is an accessory that will provide automatic sample dilution and standard preparation for flame AAS  ID 100 is not compatible with VP90 AND VP 100.  The ID100 Auto dilutor System can automatically prepare working calibration standards from a single master standard as they are needed, so that no manual dilution steps are required.  It also simplifies the task of handling over-range samples by intelligently diluting them into the calibration range, thus extending the effective working range.  Full automation is possible by combining the ID100 with any of the Thermo Elemental range of AA Flame autosampler.
  • 65. AtomicAbsorption 65 Auto-sampler ASX520-ASXR8  ASX520 Auto sampler  A workhorse auto sampler for unattended analysis  with a maximum load of 360 samples for busier laboratories  EXR8 Auto sampler  A large sample load of up to 720 samples with automatic,  unattended analysis for high throughput laboratories
  • 66. AtomicAbsorption 66 EC 90 Electric heating  It replaces the Flame Heated Measurement Cell with an Electrically Heated Atomization Cell, so that Vapor measurements can be made without a flame.  The accessory consists of two parts: 1. The EC90 Furnace Head. 2. The EC90 Power Supply
  • 67. AtomicAbsorption 67 Furnace Vision System GF TV  CCD camera provides high definition images  Uses spectrometer optical path for a clear, direct, on-axis view of the cuvet  Simplified method development  Accurate adjustment of capillary possible  Perfect sample injection depth  Drying and ashing phases can be easily optimised  High quality and reproducible results  Images can be captured and stored Correct depth Capillary too low Capillary too high Correct depth Capillary too low Capillary too high
  • 68. AtomicAbsorption 68 ISQ – Intelligent Spectrometer Qualification ISQ is an automatic, software driven process to demonstrate that your spectrometer hardware is performing consistently to specification over the intended operating ranges.  Intelligent  Identifies instrument in use  Selects appropriate tests  Software automatically controls tests  Clear result display  Spectrometer  Tests the hardware of the spectrometer  Helps to diagnose the source of any hardware problems at an early stage  Qualification  Verifies that the instrument is operating entirely within the designed specifications  Confirms instrument is capable of producing sound analytical data.
  • 69.
  • 70. AtomicAbsorption 70 Validation of the Machine Validation kit helps 1. Monitor the regulatory compliance status of spectrometer. 2. Determine the conformity of an AA spectrometer to internally established standards. 3. Provide confidence for managerial and regulatory personnel that the system is under control provide all the documentation, hardware and standard solutions necessary for the validation process.
  • 71. AtomicAbsorption 71 Validation Packages Package contain  Log book  Ca/Mg lamp  Ni/Cr/ Mn lamp  Pyro coated cuvettes  Ni, Cr, & Mn standard solutions  ASTM type 1 water  Optical filters  Certificates
  • 72. AtomicAbsorption 72 Validation Unit Tests performed  Wavelength Accuracy  Monochromator Resolution  Photometric Accuracy  Photometric Stability  D2 Background Correction  Polarizer Orientation  Polarizer Repeatability
  • 73. AtomicAbsorption 73 Calibration  Automatically peaks wavelength  Automatically sets band pass  Automatically adjusts lamp current  Automatically recalls flame conditions  Automatically balances D2 intensity  Automatically sets baseline
  • 74.
  • 75. AtomicAbsorption 75 Applications 1. Environmental 2. Clinical 3. Pharmaceutical 4. Agriculture 5. Petrochemicals 6. Other’s
  • 76. AtomicAbsorption 76 1. Environmental Applications  Waters – sea, fresh, waste  Plant materials  Soils, Sludge's and sediments  Airborne particulates  Biological samples
  • 77. AtomicAbsorption 77 Essential and Toxic elements  Essential major elements C N O P S Cl Na K Ca Mg  Essential trace elements F I Se V Cr Mn Fe Co Ni Cu ZnMo Si Sn As  Toxic elements Li Be Ba F Cl Br As Sb Bi Pb Sn Tl V Cr Mn Fe Co Ni Cu Zn Cd Hg
  • 78. AtomicAbsorption 78 2. Clinical Applications  The majority of samples analysed are taken from the main group of biological fluids, such as whole blood, plasma, serum and urine.  Hard and soft tissues, such as bone, finger nails and hair  Flame based analysis for the major and minor essential elements, graphite furnace analysis for the trace elements and vapour analysis for the group of toxic
  • 79. AtomicAbsorption 79 Essential elements  Essential major elements Ca Mg Na K  Essential minor elements Zn Cu Fe  Essential trace elements Cr Mn Mo Co V Se Ni
  • 80. AtomicAbsorption 80 Toxic elements  Toxic elements are often defined as those that interfere with metabolic processes.  The elements usually included in this group are as follows:  Lead, Mercury, Arsenic, Thallium, Cadmium, Aluminum, Boron, Antimony.
  • 81. AtomicAbsorption 81 3. Pharmaceutical Applications  Samples of diclofenac sodium for Na, K, Ca and Al analysis  Magnesium Stearate sample to be analyzed for Cd, Ni and Pb.  Samples of vitamin tablets Se analysis
  • 82. AtomicAbsorption 82 Drug discovery and testing  Most Pharmaceutical Companies these days develop drugs which are targeted at specific cells in the body.  These drugs must be tested for correct activity but more importantly for the absence of any adverse side reactions.
  • 83. AtomicAbsorption 83 Toxic and nutrition elements  Toxic metals  Pb, Cd, As, Hg, Al, Cr, Cu  Nutrition elements  Ca, Mg, Na, K, P  Micro-nutrients  Zn , Se, Mo, etc…  Process monitoring and control  Fe, other transition elements in frying oil  Ni in fat hydrogenation  Levels vary with process, typically 1000 – 10PPM
  • 84. AtomicAbsorption 84 4. Agriculture Applications  soil analysis provides a measure of a soil‘s potential to supply the necessary nutrients to plants.  Plants may be sampled to monitor nutrient uptake efficiency and also to check for toxic metal accumulation for health reasons.
  • 85. AtomicAbsorption 85 Soil nutrient elements  P, K, Ca, Mg Macro nutrients at % level  Cu, Fe, Mn, Zn Micro nutrients at ppm level  Al, B, Na, Mo, Se Other nutrient elements  As, Cd, Co, Cr, Ni, Pb Elements of toxic interest
  • 86. AtomicAbsorption 86 5. Petrochemical Applications  Measure refinery contaminant elements  Na, V, Fe, Ni by Flame-PPM  Measure fuel elements  Pb, Mn, usually low ppm-typically flame or furnace  Measure lube oil elements  Fresh - Ca, Ba, Mg, Zn, Mo, Na (flame)  Used - Ag, Al, Cr, Fe, Mn, Ni, Pb, Sn, Ti, Zn (often furnace)
  • 87. AtomicAbsorption 87 lubricating oils  Every rotating mechanism in machinery of all types depends on their use for smooth operation.  Like engines and gearboxes used in modern transportation, such as aircraft, ships, cars and lorries and heavy construction equipment.  Oils in use so that oil changes can be carried out in time to prevent excessive wear occurring in the components concerned.
  • 88. AtomicAbsorption 88 Wear Metals Wear metal Indicated condition 1 Silicon Indicates dust intrusion, usually from improper air cleaner service. Causes rapid engine wear and early failure. 2 Iron Indicates wear originating from engine block, cylinder, gears, wrist pins, rings (case iron), camshaft, oil pump, or crankshaft. 3 Copper Usually indicates wear in bushings, injector shields, valve guides ,connecting rods, or piston pins. 4 Nickel l Wear of plating on gears and certain types of bearings. 5 Tin Wear of certain types of bearings and coatings of connecting rods and iron pistons
  • 89. AtomicAbsorption 89 Wear Metals Wear metal Indicated condition 6 Lead In diesel engines indicates wear of bearings. In petrol engines fuel blow by is indicated. 7 Chromium Indicates ring wear or cooling system leakage if chromates are used as inhibitors. 8 Aluminum Indicates wear of pistons and certain types of bearings. 9 Molybdenum Indicates wear in certain types of bearing alloys and in oil coolers.