GC-AASGasChromatography-AtomicAbsorptionspectrometry Advancedspectralanalysis MPHARMACYMPCT

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GC-AAS (Gas Chromatography-Atomic Absorption spectrometry)
Presentation · August 2021

DOI: 10.13140/RG.2.2.29566.92485
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Subham Kumar Vishwakarma

Ujjain Institute Of Pharmaceutical Sciences
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ADVANCED SPECTRAL ANALYSIS (MPC201T) UNIT-IV_CHROMATOGRAPHY (GC-AAS)
Gas Chromatography GC is technique which is suited to the analysis of small, relatively volatile
molecules. It can be used both to identify and quantify substances. In general, for measurements a
sample or solution of the pure material and these are often obtained from specialist suppliers.
AAS quantitatively measures the concentrations of elements present in a liquid sample. It utilises
the principle that elements in the gas phase absorb light at very specific wavelengths which gives the
technique excellent specificity and detection limits.
The sample may be an aqueous or organic solution; indeed, it may even be solid provided it can be
dissolved successfully. The liquid is drawn in to a flame where it is ionised in the gas phase.
Light of a specific wavelength appropriate to the element being analysed is shone through the flame,
the absorption is proportional to the concentration of the element. Quantification is achieved by
preparing standards of the element.
INSTRUMENTATION: -
1. GC unit
2. Light source
3. Atomizer
4. Monochromators
5. Detector
6. Amplifier
7. Read out device
1. GC unit: -
GAS CHROMATOGRAPHY
✓ Carrier gas
✓ Flow regulators & Flow Meters
✓ Injection devices
✓ Columns
✓ GC-MS interface
✓ Ionization (Ion source)
✓ Mass analyzer
✓ Detectors
CARRIER GAS: -
Requirements of a carrier gas: -
Prepared by: - Subham Kumar Vishwakarma (shubhamkumarvishwakarma7@gmail.com), Guided by: - Dr. S Raja, Gitam
University Visakhapatnam (AP) 1|Page
• Inertness
• Suitable for the detector
• High purity
• Easily available
• Cheap
• Should not cause the risk of fire
• Should give best column performance
1. Hydrogen
better thermal conductivity
disadvantage: it reacts with unsaturated compounds & inflammable
2. Helium
excellent thermal conductivity
it is expensive
3. Nitrogen
reduced sensitivity
it is inexpensive
Flow regulators & Flow meters: -
Deliver the gas with uniform pressure/flow rate - Rota meter & Soap bubble flow meter
✓ Rota meter: - placed before column inlet
it has a glass tube with a float held on to a spring. the level of the float is determined by the
flow rate of carrier gas.
✓ Soap Bubble Meter: -Similar to Rota meter & instead of a float, soap bubble formed indicates
the flow rate.
Injection Devices: -
✓ The injection port consists of a septum through which a syringe needle is inserted to inject the
sample.
✓ The sample is injected into a stream of inert gas usually at an elevated temperature by a micro
syringe.
✓ The vapourised sample is carried into a column packed with the stationary phase.
✓ To ensure rapid & complete solute volatilization temp of injector → 30-50 degree Celsius
>column temp
The injection port Is a hollow, heated, glass-lined cylinder: -
✓ The injector is heated so that all components in the sample will be vaporized.
✓ If the temperature is too low, separation is poor and broad spectral peaks should result or no
peak develops at all.
✓ If the injection temperature is too high, the specimen may decompose or change its structure.
✓ The temperature of the sample port is usually about 50°C higher than the boiling point of the
least volatile component of the sample.
Injector Types
1. Split/ Splitless Injector
2. On-Column Injector
3. High Oven Temperature On-Column Injector
4. Large Volume On-Column Injector
5. Packed Column Injector
6. Purged Packed Injector
7. Programmable Temperature Vaporizing Injector
1. Split mode
✓ The split vent is open, part of the sample goes into the column.
✓ When analyzing high concentration or neat samples.
✓ Yields the sharpest peaks if the split gas is properly mixed.
✓ Standard for capillary columns.
Split-less mode
✓ The split vent is closed, most of the sample go into the column.
✓ When analyzing low concentration or diluted samples.
✓ Splitless times of ~ 1 minute are typical.
✓ Standard for capillary columns.
2. Large Volume on column injector: -

✓ LV-SL injection overcomes the limitation of the maximum sample volume to 1-2 µL of
classical splitless injection by exploiting the Concurrent Solvent Recondensation technique
(CSR).
✓ CSR technique allows injection of large volumes by combining a restricted evaporation rate
with an accelerated sample transfer granted by the pressure surge generated by solvent
evaporation and by the quick solvent recondensation in a precolumn.
LV-SL has the following advantages: -

• It is simpler because it allows injections of up to 50 µL in a conventional split/split-less injector
without any special tuning of operating parameters;
• It is robust versus sample by-products or contaminants and extremely suitable for food
matrices.
COLUMNS: -
✓ Column is one of the important parts of GC which decides the separation efficiency. Columns
are made up of glass and stainless steel.
✓ Is where the chromatographic separation of the sample occurs.
✓ Several types of columns are available for different chromatographic applications.
✓ The heart of the system.
✓ It is coated with a stationary phase which greatly influences the separation of the compounds.
✓
Classification of columns: -
Depending on its use:
✓ Analytical column
✓ Preparative column
Depending on its nature Column Types: -
✓ Packed column: - Are available in packed manner commercially and hence are called as
Packed column. Different columns ranging from non-polar to polar are available.
✓ Open tubular/ Capillary Column: - They are made up of long capillary tubing of 30-90
meters in length and have diameter of 0.025 to 0.075 cm. These are made up of stainless steel
and are in the form of a coil. The inner wall of the capillary is coated with stationary phase
liquid in the form of a thin film.
2. Light Source: -
Hollow Cathode Lamps: -
HCL is the most common radiation source in AAS. It contains a tungsten anode and a hollow
cylindrical cathode made of the element to be determined. These are sealed in a glass tube filled with
an inert gas (neon, argon). Each element has its own unique lamp which must be used for that analysis.
ELECTRODELESS DISCHARGE LAMP: -
A small amount of the metal or salt of the element for which the source is to be used is sealed inside
a quartz bulb. This bulb is placed inside a small, self-contained RF generator or “driver”. When power
is applied to the driver, an RF field is created. The coupled energy will vaporize and excite the atom
inside the bulb causing them to emit their characteristic spectrum. They are typically much more
intense and, in some cases, more sensitive than comparable HCL. Hence better precision and lower
detection limits where an analysis is intensity limited. EDL are available for a wide variety of
elements, including Sb, As, Bi, Cd, Cs, Ge, Pb, Hg, P, K, Rb, Se, Te, Th, Sn and Zn.
3. ATOMIZER: -
Atomization is separation of particles into individual molecules and breaking molecules into atoms.
This is done by exposing the analyte to high temperatures in a flame or graphite furnace Atomiser
converts the liquid into small droplets which are easily vaporised.
Types of Atomisers: -
I. Flame atomizer: -
a.) Total consumption burner- Total consumption burner. In this whole sample is atomized into
the flame, hence named as total consumption burner. In this burner, the sample solution, the
fuel, and oxidizing gases are passed through separate passages to meet at the opening of the
base of flame. Then the flame breaks the sample in liquid form into the droplets which are
evaporated and burns. Leaving the residue which is reduced to atoms.
➢ Fuel used – H2 /acetylene,
➢ Oxidant – O2
b.) premixed burner- It is most widely used because of uniformity in flame intensity. In this the
sample solution, fuel and oxidant are mixed before they reach the tip. The fine droplets get carried
out along with the fuel gas at outlet, the large drops of sample get collected in chamber and are drained
out.
Advantages
➢ Non-turbulent
➢ Noiseless
➢ Stable
Disadvantages
➢ Only 5% sample reaches to the flame
➢ Rest 95% is wasted.
Flame temperature for various gas mixtures
II. Non-flame atomizer (Electrothermal atomizer)
Nebulization- Conversion of the liquid sample to a fine spray

Desolvation- Solid atoms are mixed with the gaseous fuel.
Volatilization- Solid atoms are converted to a vapor in the flame.
There are three types of particles that exist in the flame:
1) Atoms
2) Ions
3) Molecules
Nebulization: - Before the liquid sample enters the burner, it is converted into droplets this method
a formation of small droplets its called nebulization. Common method of nebulization is by use of
gas moving at high velocity, called pneumatic nebulization.
4. Monochromators: -
Important part in an AA spectrophotometer. It is used to separate out all of the thousands of
lines. Without a good monochromator, detection limits are severely compromised. A
monochromator is used to select the specific wavelength of light which is absorbed by the
sample, and to exclude other wavelengths. The selection of the specific light allows the
determination of the selected element in the presence of others.
They are of two types:
Prism monochromator: - Quartz material is used for making prism, as quartz is transparent over
entire region.
Grating monochromator: - it consists of a series of parallel straight lines cut into a plane surface.
5. Detector: - The light selected by the monochromator is directed onto a detector that is typically
a photomultiplier tube, whose function is to convert the light signal into an electrical signal
proportional to the light intensity. The processing of electrical signal is fulfilled by a signal
amplifier. The signal could be displayed for readout, or further fed into a data station for printout
by the requested format.
Photomultiplier Tubes
Components
• Made of a glass vacuum tube
• Photocathode
• Several dynodes
• One anode
APPLICATION: -
➢ Quantitative metal concentrations in solution
➢ Analysis of lead in paint
➢ Monitoring of trace metals in industrial effluent streams
➢ Trace elements in product/raw materials along with ICP-MS
➢ Analysis of additives and purity in steels and other metal alloys
Analysis of low-level contaminants
University Visakhapatnam (AP)
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See discussions, stats, and author profiles for this publication at: https://www.researchgate.

GC-AAS (Gas Chromatography-Atomic Absorption spectrometry)

Presentation · August 2021

Subham Kumar Vishwakarma

SYNTHESIS AND CHARECTERIZATION OF 5- AMINOTETRAZOLE View project

The user has requested enhancement of the downloaded file.

2. Large Volume on column injector: -

LV-SL has the following advantages: -

II. Non-flame atomizer (Electrothermal atomizer)

Nebulization- Conversion of the liquid sample to a fine spray

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