CHEM 340

Tutorial 3 – ICP and AA - Solutions

1. With the aid of a simple illustration, briefly describe the absorption process which leads to
excitation and relaxation of an electron.

Answer:

E1
h
Eo

- Electron moves from ground state to an excited state So  S1

- Atom can be ionized A  An+

- Excited singlet state atom relapse back to the ground state S1  So by the loss
energy in form of fluorescence radiation

2. Using the diagram shown, discuss the components, construction and generation of
radiant wave lines from a hollow cathode tube.

The HCL contains a tungsten anode and hollow cathode made of the element to be
determined

Sealed in a glass tube with inert gas e.g. neon (at a certain pressure)

Ionisation of the inert gas atoms occurs by applying a potential difference between
anode and cathode

The ions that form bombard the cathode in a process called sputtering ejecting atoms in
the process

Some sputtered cathode atoms become excited and when they relax, emit radiation
characteristic of the metal
 The shape of the cathode concentrates the radiation into a beam which then passes
through a quartz window

3. Briefly explain the term sputtering.

Answer:

This is the process of the ejection of atoms from a sample as a result of bombardment by
energetic species. In and HCL, argon gas is ionized by an applied voltage on the cell,
causing the argon ions to accelerate to the cathode where they interact with the sample and
eject atoms

4. What is the function of the chopper in Atomic Absorption Spectroscopy?

Answer:

The function of the chopper in Atomic Absorption Spectroscopy is to break the steady light
into pulsating light. It is a rotating wheel placed between the flame and the source.

5. The picture gives the emission lines of hydrogen. Explain why there are several lines
and not just one, even though hydrogen has only one electron.

Although hydrogen has only one electron, it contains many energy levels. When the
hydrogen atom absorbs energy, the electron is excited to a higher energy level. However, its
electron can jumps from this higher energy level to a lower one, but not necessarily to the
ground state and in this way, it releases a photon. Because the electron can therefore jump
to several energy levels, those photons appear as lines with different wavelenghts.
6. Spark or arc atomic emission spectroscopy is used for the analysis of metallic elements in
solid samples. Discuss how this process is carried out.

An electric arc or spark is passed through the sample, heating it to a high temperature to
excite the atoms within it.
The excited analyte atoms emit light at characteristic wavelengths that can be dispersed with
a monochromator and detected.
For non-conductive materials, the sample is ground with graphite powder to make it
conductive.

7. Explain how the plasma in an ICP instrument is generated. Include the parts involved as
part of your discussion.

Initially argon gas and sample aerosol passes through a central quartz tube.
Ionization of the flowing argon is initiated by a spark from a tesla coil. Passing
current through the induction coil which is wrapped around the quartz tube sets up
an electro-magnetic field which is generated by a radio frequency (RF) generator.

The resulting cations and electrons then interact with the changing magnetic field
produced by the induction or load coil. This induces a circulating eddy current in the
argon gas stream and intense heat (thermal energy) is developed forming a flame
shaped plasma near the top of the torch with temperatures from 6000 to10000 K.

8. What is the main advantage of the simultaneous ICP-OES and what detector is usually
used in such an instrument?
Can measure simultaneously, the intensities of the emission lines of a large number
of elements (up to 60 elements). Usually diode array detector (DAD).

9. Atomisation is an important step in atomic absorption spectroscopy. Explain in a step wise

fashion, how atomisation occurs in AAS.

Aspiration of the sample into the energy source.

Nebulization – solution of the sample becomes fine droplets by spraying through a
thin nozzle.
Desolvation - droplets are heated to evaporate off the solvent leaving the analyte
and other matrix components.
Volatilization –solid analyte/matrix particles are converted into a gas
Dissociation –in the gas phase the molecules are broken-up into atoms
Ionization – during this step, the atoms become charged


10. Non-induction nebulizers in an AAS are of three types. Name two and briefly mention the
principle of operation of each.

 Enhanced Parallel Path: Liquid is delivered beside a gas orifice and drawn
into the gas stream by surface tension along a spout;
 Flow Blurring: liquid is injected by pressure into a gas stream;
 Vibrating Mesh: liquid is pushed through tiny holes by a vibrating ultrasonic
plate