atomic absorption techniques & applications
TRANSCRIPT
AA Techniques & Applications
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Contents
Introduction
Theory
AAS Setup
Validity
Accessories
Techniques and facilities
Software
Application
Air
Water & Soil
Foods
Clinical
Petrochemicals
Pharmaceutical
Introduction
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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
3. Aluminum (7.5%)
4. Iron (4.71%)
5. Calcium (3.39%)
6. Sodium (2.63%)
7. Potassium (2.4%)
8. Magnesium (1.93%)
10. Titanium (0.58%)
13. 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
Low PPM levels in original material
Recent interest in radio-nuclides Pu, Am and Np.
Cs-137, Cs-134, Sr-90 and K-40
Nutrition elements
Ca, Mg, Na, K, P
%age to high PPM levels in original material
Micro-nutrients
Zn , Se, Mo, etc…
high PPM to PPB levels in original material
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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.
Theory
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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”
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Periodic table
70 elements can be analyze
using AA
About 80 of the 106 elements are metals
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Calibration
o 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.
AA Setup
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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
polarised 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
The main function is 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
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
FurnaceToroidMirror
Flame Toroid Mirror
Plane Mirror
Rear BeamSelector
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.
System Techniques
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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
(1) Air- Acetylene (9 psi) .
(2) Air- Acetylene -Nitrous oxide
Nitrous oxide (N2O) needs to be used instead of air
(78% N2 + 21% O2)
The level of measuring is about mg/l (ppm)
Support gases
1. Air 2.07 bar (30psi)
2. 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 Control
Burner type recognition
Gas pressure sensors
Auto-ignition of flame
Fully automatic gas control
Software change over of flame type
Auto flame shut down
Power failure protection
Spray chamber over pressure
protection
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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:
5cm slot Universal Titanium Burner
suitable for general purpose use with all
flame types
10cm 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
DryingAshingAtomizingCleanin
g
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1. Furnace power supply
Power
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
AA Facilities
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Secondary Wavelength
Using secondary wavelength
we can decrease the amount of light
inter the detector so increase the
concentration of the metal
measured
e.g. Zinc secondary wave length give
4000 X
Measure high conc. Of metals
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Atomic Emission Spectroscopy
Higher wavelength higher stability
of emission.
uses quantitative measurement of
the optical emission from excited
atoms to determine analyte
concentration
Environmental
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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
+5oC and +40oC 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.
Accessories
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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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Aliquot Micro-sampling
Simple accessory to allow you to use manual
Aliquot Micro sampling to measure your
samples when
1- The available volume of sample is limited
2- The sample is too viscous,
3- Contains too high concentration of
dissolved solids
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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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HG90 Mercury Concentration System
In the SOLAAR HG90 Mercury
Concentration System, the mercury vapor
from the HS90 is passed over a
gold/platinum gauze for a defined length
of time to collect it as an amalgam.
It is then released by heating the gauze
and a flow of argon transports it into the
measurement cell.
Collection for up to 120 seconds will give a
detection limit of about 20 ng/L (or ppt).
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Segmented Flow Injection
Flow Injection Operation
A peristaltic pump is used to generate
continuously flowing streams of reagents.
A 6 port valve and sampling loop are used
to inject discrete portions of the sample into
one of the reagent streams.
The reagent streams are mixed, and the
volatile hydrides are separated in a gas
liquid separator and transported to the
spectrometer for measurement.
The signal is measured as a peak.
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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.
Software
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Easy to learn SOLAAR Software
• Software design is essential to make the
instrument easy to learn, easy to use and the
full capabilities of the hardware.
• SOLAAR software was the first AA software
designed to run under Microsoft Windows.
• Evolutionary software development strategy
now on Version 10
• We incorporate Customer feedback Result –
Stable, refined full functionality.
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AA Software
Compatible with Windows 2000, XP Professional and VISTA Ultimate
Wizard based interface
Complete user help facility to provide a comprehensive AA Cookbook for all elements.
Context sensitive help
Automatic programming of up to 16 elements
Facility to record lamp usage
Capable of automatically switching lamps on and off in an intelligent manner to preserve
lamp life but also ensure lamps are warmed up sufficiently at time of use
Normal, standard addition and standard curve calibration methods supported
Flexible and comprehensive results database filters to select and display the required
data
Export of data to other applications possible
Integrated Quality Control protocols
Validation
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3M Validation
According to ISO/IEC 17025
“General requirements for the competence of testing and calibration laboratories”
Machine
Method
Man
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1. 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
o Log book
o Ca/Mg lamp
o Ni/Cr/Mn lamp
o Pyro coated cuvettes
o Ni, Cr, & Mn standard solutions
o ASTM type 1 water
o Optical filters
o Certificates
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Validation Unit
Tests performed
Wavelength Accuracy
Monochromator Resolution
Photometric Accuracy
Photometric Stability
D2 Background Correction
Polariser Orientation
Polariser 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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2. Validity of the method
Contaminant Methodolgy13
Antimony ICP-Mass Spectrometry Hydride-Atomic Absorption Atomic Absorption; PlatformAtomic Absorption; Furnace
Arsenic14 Inductively Coupled Plasma15ICP-Mass Spectrometry Atomic Absorption; Platform Atomic Absorption;
FurnaceHydride Atomic Absorption
Barium Inductively Coupled Plasma Atomic Absorption Furnace
According to EPA
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According to EPA
Contaminant Methodolgy13
Cadmium ICP-Mass Spectrometry Hydride-Atomic Absorption Atomic Absorption; PlatformAtomic Absorption; Furnace
Calcium Inductively Coupled Plasma15ICP-Mass Spectrometry Atomic Absorption; Platform Atomic Absorption;
Furnace
Chromium Inductively Coupled PlasmaAtomic Absorption Furnace
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3. Man Validation
Thermo Training Courses.
Thermo Technical support.
Meslo Training Courses.
Meslo Technical support.
Service after sell.
Service center.
Application Consultations.
Applications
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Applications
Environmental
Clinical
Pharmaceutical
Foods
Agriculture
Petrochemicals
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1. Environmental Applications
Waters – sea, fresh, waste
Plant materials
Soils, Sludges 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
analysed 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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4. Food and Drink Applications
No. Raw materials Intermediates Food Products
1 Cereals Flour Bread
2 Vegetables Sugars, Milk
3 Fruit syrups Butter
4 Meat Processed meat and fish candy
5 Dairy Processed dairy products Sweets
6 Fish Flavourings Juice
7 Water Additives Etc
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Toxic and nutrition elements
Toxic metals Pb, Cd, As, Hg, Al, Cr, Cu Low PPM levels in original material Recent interest in radio-nuclides Pu, Am and Np.
Cs-137, Cs-134, Sr-90 and K-40 Nutrition elements
Ca, Mg, Na, K, P %age to high PPM levels in original material
Micro-nutrients Zn , Se, Mo, etc… high PPM to PPB levels in original material
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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5. 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.
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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
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6. 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)
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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.
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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 certaintypes of bearings.
5 Tin Wear of certain types of bearings and coatings of connecting rods and iron pistons
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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 certaintypes of bearings.
9 Molybdenum Indicates wear in certain types ofbearing alloys and in oil coolers.
