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STUDENT NUMBER: _______________________SURNAME, INITIALS: ___________________

INSTRUMENTAL ANALYSIS MOCK TEST 26 APRIL 2024

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1. Introduction to Spectroscopy (10 Marks)

1.1 Define or explain the following terms used in spectrometric methods:

1.1.1 transmittance
1.1.2 absorptivity
1.1.3 absorbance (6)

1.2 A solution containing 3.92 mg/100 mL of A (335 g/mol) has a transmittance of 64.1% in a
1.50 cm cell at 425 nm. Calculate the molar absorptivity of A at this wavelength. (4)

2. Atomic Absorption Spectroscopy (10 Marks)

2.1 Briefly discuss the principle of atomic absorption spectroscopy. (3)

2.2 The chromium in an aqueous sample was determined by pipetting 10.0 mL of the unknown
into each of five 50.0 mL volumetric flasks. Various volumes of a standard containing
12.2 ppm Cr were added to the flasks, following which the solutions were diluted to volume.
The absorbance readings of each standard were then determined by Flame Atomic
Absorption Spectrometry.

SAMPLE (mL) STANDARD (mL) ABSORBANCE

10.0 0.0 0.201
10.0 10.0 0.292
10.0 20.0 0.378
10.0 30.0 0.467
10.0 40.0 0.554

2.2.1 Determine an equation for the relationship between absorbance and volume of standard.
(2)

2.2.2 Determine the concentration of Cr in ppm in the sample. (3)

2.2.3 Find the standard deviation of the result in 2.2.2. (2)

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3. Atomic Emission Spectroscopy (10 Marks)

3.1 What are some of the advantages of plasma sources compared with flame sources for
emission spectrometry? (4)

3.2 Manganese was used as an internal standard for measuring iron by ICP-OES. A standard
mixture containing 2.00 𝜇𝑔 𝑀𝑛/𝑚𝐿 and 2.50 𝜇𝑔 Fe/𝑚𝐿 gave a quotient (Fe signal/Mn
signal) = 1.05/1.00. A mixture with a volume of 6 mL was prepared by mixing 5.00 mL of
unknown Fe solution with 1.00 mL containing 13.5 𝜇𝑔 Mn/𝑚𝐿. The absorbance of this
mixture at the Mn wavelength was 0.128, and the absorbance at the Fe wavelength was
0.185. Find the molarity of the unknown Fe solution. (6)

4. Atomic X-Ray Spectroscopy (10 Marks)

4.1 List the THREE types of sources used in X-Ray instruments designed for analytical work.
(3)

4.2 Briefly discuss the principle of X-Ray Fluorescence Spectroscopy. (2)

4.3 A solution of I2 in water has a density of 0.49 kg L-1. A 15 mm sample layer was found to
transmit 28 % of radiation from a Mo Kα (0.711 Å) source. Mass absorption coefficients for I,
H and O were found to be 39.2, 0.00 and 1.50 respectively. Calculate the percent I 2 in this
solution. (5)

5. UV-Visible Spectrometry (15 Marks)

5.1 A solution containing 7.35 ppm KMnO4 had a transmittance of 0.145 in a 1.00 cm cell at
520 nm. Calculate the molar absorptivity of KMnO4 at 520 nm.

5.2 Discuss the principle of UV/Visible spectroscopy.

5.3 Define or explain the term “chromophore”.

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5.4 A method was developed for the routine determination of iron in groundwater. A standard
solution was put through appropriate dilutions to give various concentrations of iron
solutions. The iron(II)-1,10,phenanthroline complex was then formed in 25.0 mL aliquots of
these solutions, following which each was diluted to 50.0 mL. The following absorbances
(1.00-cm cells) were recorded at 510 nm:

Fe(II) Concentration Absorbance @

(ppm) 510 nm
4.00 0.160
10.0 0.390
16.0 0.630
24.0 0.950
32.0 1.260
40.0 l.580

5.4.1 Plot a calibration curve from these data.

5.4.2 Use the method of least squares to find an equation relating absorbance and the
concentration of iron(II).

5.4.3 Calculate the concentration (as ppm Fe) of iron in 25.0 mL aliquot of groundwater that
yielded an absorbance of 0.143 in a 1.00 cm cell.

6. IR Spectrometry (15 Marks)

6.1 Give the wavenumber range of the most used infra-red (IR) spectral region.

6.2 Give one reason why molecules such as O2, N2, or Cl2 do not produce an IR spectrum.

6.3 List five advantages of a Fourier Transform infrared (FTIR) spectrometer compared with a
dispersive instrument.

6.4 The presence of ethylene in samples of ethane is determined by using the absorption band
of ethylene at 1443 cm-1. A series of standards measured by using a FTIR spectrometer
fitted with an ATR accessory gave the following data:

% Ethylene 0.50 1.00 2.00 3.00

Absorbance 0.120 0.240 0.480 0.719

Calculate the percentage of ethylene in an unknown sample that gave an absorbance of

0.412 when the same instrument was used.

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6.5 The molecular formula of a certain compound is C3H3Cl. Use correlation charts to deduce
the structure that is consistent with the infrared spectrum given below. There may be more
than one possible answer.

7. NMR Spectrometry (15 Marks)

7.1 Briefly discuss the principle of NMR spectrometry.

7.2 The compound that gives the following NMR spectrum has the formula C3H6Br2. Draw its
structure.

7.3 Distinguish between wide-line and high-resolution NMR spectra.

7.4 Define the chemical shift parameter.

7.5 Explain the difference in the way a CW and an FT-NMR experiment is performed.

INST 471 Dr AN Gounden