Exercise 1: (Chapter 1: Introduction; Chapter 2: Signal & Noise; Chapter 3:AAS)

1. What are the domains in instrumentation and how are they converted?

Non-electrical domains=

Physical,(light intensity, colour),Chemical (pH),Scale Position (Length),Number (objects)

Electrical domains=

Current,Voltage,Charge.Frequency

Converts information stored in the physical or chemical characteristics of the analyte into useful
information

From Energystimulus to Analytes (in matrix) .then Analytical response and change to data after
information encode.

For an example, Spectrophotometry.The Instrument is spectrophotometer .the Stimulus is

monochromatic light energy.it Analytical response is photocell.the Data is electrical current and the
Data processor is a current meter .lastly its Readout is meter scale.

2. Define transducer, detector, and sensor

Detector

=Device that indicates a change in one variable in its environment (eg., pressure, temp, particles)

=Can be mechanical, electrical, or chemical

Sensor

= Device that converts chemical to electrical data

Transducer

=Devices that convert nonelectrical domains to electrical data

3. Differentiate between the analysis of quantitative concentration and
qualitative speciation
Qualitative, A type of chemical analysis by which the analyte or analytes in a sample are identified.
for example,the method are chromatography, electrophoresis and identification by measuring
physical property (e.g. spectroscopy, electrode potential)

Quantitative, A type of chemical analysis by which the amount of each analyte or analytes in a
sample is determined.for example,the methode are measuring property and determining
relationship to concentration (e.g. spectrophotometry, mass spectrometry).

4. Describe the criteria used in selecting analytical methods

Use Qualitative if identification by color, indicators, boiling or melting points, odors.

Use quatitative if identification by mass or volume (e.g. gravimetric, volumetric)

5. What signal to noise ratio is need for a reliable signal? If the signal mean is
100, what is the maximum standard deviation for a signal?
3:1

100/3 =33.33 minimum sd

6. What are the sources of noise?

Chemical Noise

–Uncontrollable variables that affect the chemistry of the system under investigation

–Variations in temperature, pressure, humidity, vibrations

Instrumental Noise (associated with components of instruments)

–Thermal or Johnson noise

–Shot noise

–Flicker noise

–Environmental noise

7. Compare boxcar averaging with ensemble averaging

Ensemble Averaging

•Successive sets of data stored in memory as array

•Summed up point by point (co-addition)

•Data are averaged

ensemble averaging can increase the S/N ratio

Smoothing irregularities

•Assume that irregularities are the result of noise

•Assume that the analog analytical signal varies only slowly with time and the average small number
of adjacent points is better measure of the signal than individual points

•Drawbacks: detail is lost ; cannot be used for signal changes rapidly with time

8. Explain the four stages of flame atomization in atomic absorption

spectroscopy (AAS).
Light Source, Atomizer(burner), Monochromator, Detector

Light source=Hollow Cathode Lamp involving process of Ionization, Sputtering, Excitation and
Emission.

Atomizer(burner)= Convert sample into atomic vapour. consists of: Nebulizer,Mixing (spray)
chamber,Burner

The liquid sample is sucked through a capillary tube by a high-pressure stream of gas flowing around
the tip of the tube. The sample is converted into a fine mist (small droplets of solution) through the
nebulizer.The sample is aspirated into a spray chamber. The impact of the sample with the glass
impact bead produces an aerosol mist. The aerosol mist mixes with combustion gases in the spray
chamber then Burner.At burner, combustion of fuel and oxidant occurs.The heat at the burner
vaporizes the aerosol particles turn into gaseous molecules, ions and free atoms.The analyte atoms
then absorb the radiation from the light source.(absorbance or conc)

Flame atomization=

1.Desolvation (drying) – the solvent is evaporated and the dry sample nano-particles remain;

2.Vaporization (transfer to the gaseous phase) – the solid particles are converted into gaseous
molecules;

3.Atomization – the molecules are dissociated into free atoms;

4.Ionization – depending on the ionization potential of the analyte atoms and the energy available in
a particular flame, atoms might be in part converted to gaseous ions.

9. A river water sample was prepared in aqua region and analyzed using AAS.
The river water contains iron, sodium, zinc, magnesium, calcium, phosphate
and other minerals. A series of standard iron solutions was prepared to
establish a standard calibration curve.

(i) Identify the possible interference encountered in this AAS analysis. Give your reason of why such
interference exists.
Ionisation Interferences.it is because it Occur when the flame temperature has enough energy to
cause the removal of an electron from the atoms to ions.thus,this will result in less ground state
atoms for radiation absorption and thus lowering absorbance.

(ii) Suggest four prevention measures to mitigate such interference.

Add excess of an easily ionisable element to the blank, standards and sample to suppress ionisation
of analyte.

Use a cooler flame, but chemical interferences may result.