INSTITUTE OF PUBLIC ANALYSTS OF NIGERIA

PE I – Paper 2: SPECTROSCOPIC AND MISCELLANEOUS METHODS OF

ANALYSIS
Instructions: Section A: Answer ALL questions in this section. Short answers are expected to
the questions in this section. Total marks allotted to the section are 40.
Section B: Answer question 1 and any two other questions. Total marks allotted to the section
are 60. Submit the question paper with your answer booklet.

Section A

1. Explain briefly the term ‘spectroscopy’.

2. Electromagnetic radiation can be described as a wave with certain properties. Mention any
two and define them.
3. Calculate the energy in Joules of one photon if a beam of IR has a wavelength of 5.00μm
(Planck’s constant is and speed of light is ).

4. Spectrum obtained from molecular species is usually broad. Explain why this is so.

5. Differentiate between emission and absorption spectroscopy.

6. Briefly explain the following:

i) Formal potential, E0'
ii) Non-radiative excitation process

7. How can an IR spectrometer be used to analyse a compound?.

8. Explain the following in IR spectroscopy:

i) “Finger print region”: 1430-910cm-1 (7-11 microns)
ii) Why bending frequency is not used very much in identification

9. Highlight how you can handle liquid and solid samples for analysis in IR spectroscopy

10. Give two examples of a reference electrode and two characteristics of an indicator electrode

11. The energy difference between the 3p and 3s orbitals for sodium is 2.107 eV. Calculate
the wavelength of radiation that would be absorbed in exciting the 3s electron to the 3s
orbitals. (l eV = 1.60 x 10-19 J).
 12. What are the major components of a typical spectrophotometer? Briefly explain the use
of any two of the components.

13. What do you understand by the term “atomization”? How critical is this to the sensitivity
of a measurement.

14. Why are atomic spectra made up of lines whereas molecular spectra are made up of
bands?

15. What is the one major cause of deviation from Beer’s law? How do modern instruments
compensate for this?

16. What are the major components of a typical spectrophotometer? Briefly explain the use
of any two of the components.

17. The cuvet can either be made of glass or quartz. Explain the major difference in their
usage.

18. List two basic differences between a single beam and a double beam spectrophotometer?

19. Draw a schematic diagram of the gas-liquid chromatographic system. Explain briefly
how any of its detectors work.

20. List out three differences between GLC and HPLC.

Section B

(Atomic masses: Ca=40, H=1,008, O=16, Cl = 35.5)

1. a) Draw a well labelled double beam fluorometer and highlight the measurement process
b) How may the instrument be standardised?
 c) Explain any two differences between continuous flow analysers and discrete analysers

2. a) Describe how you will prepare 2.00L of 0.01M potassium permanganate in the laboratory.
b) Show clearly how you will balance the redox equation:

c) Suppose a solution sodium thiosulphate was standardised by dissolving 0.0807g KIO3

(214.00 g/mole) in water, adding a large excess of KI, and acidifying with HCL. The
liberated iodine required 27.76 mL of the thiosulphate solution to decolorize the blue
starch/iodine complex. What is the molarity of the Na2S2O3?

d) What are the steps involved in an auto analyser.

3. Calcium in a sample is determined by atomic absorption spectrometry. A stock solution

of calcium is prepared by dissolving 1.834g CaCl2, 2H2O in water and diluting to 1 L.
This is diluted 1:10. Working standards are prepared by diluting the second solution,
respectively, 1:20, 1:10 and 1:5. Determine the concentrations of the standard solutions
thus prepared.
The sample is diluted 1:25. Strontium chloride is added to all solutions before dilution,
sufficient to give 1% (mass/vol) to avoid phosphate interference. A blank solution is also
prepared to give 1.5% SrCl2. Absorbance signals are acquired by a data system as the
solutions are aspirated into an air-acetylene flame, as follows: wastewater:

Solution (ppm) Absorbance Signal

Blank 1.5 units
Standard 1 10.6 units
Standard 2 20.1 units
Standard 3 38.5 units
Sample 29.6 units

(a) Construct a graph for the calibration curve taking the blank value into account
(b) Find the slope, intercept and standard deviation of the calibration curve.
(c) Determine the concentration of calcium in the sample in parts per million
(d) Determine the standard deviation of C above
4. (a) Describe how you would prepare of 100mL of 6.0 M HCl from a concentrated
solution that has a specific gravity of 1.18 and is 37% (w/w) HCl (36.5 g/mol).

(b) What mass of AgNO3 (169.9 g/mol) is needed to convert 2.33g of Na2CO3 (106.0
g/mol) to Ag2CO3? What mass of Ag2CO3 (275.7g/mol) will be produced?

(c) The following results were obtained in the replicate determination of the lead content
of a blood sample: 0.752, 0.756, 0.752, 0.751, and 0.760 ppm Pb. Calculate the mean
and standard deviation of this set of data.

(d) Several spectrophotometers have scales that read either in absorbance or in percentage
transmittance. What would be the absorbance reading at 20% T? At 80%T?
What would the transmittance reading be at 0.25 absorbance? At 1.00 absorbance?