UNIVERSITI TUNKU ABDUL RAHMAN

Faculty : Lee Kong Chian Faculty of Engineering & Science

Programme : BEng (Hons) Chemical Engineering
Course : UEMK2023 INSTRUMENTAL ANALYSIS
Session : : May 2017 Due Date : : 19 July 2017 (Fri Week 8)
Lecturer : : Dr Tioh Ngee Heng Expected Duration to : : 3 weeks
Complete Assignment

Assignment No. 1
Section A (60 marks)

Answer ALL questions. All questions carry equal marks.

1) Define Beers law. Identify the factors that cause the Beers law relationship to depart from
linearity. Correlate these factors with the assumptions made in deriving the Beers law.

2) Critically evaluate the graphite furnace and vapour generation as modes for the generation
of atomic vapour in atomic absorption spectrophotometric analysis and their operational
process on the consequential impacts on the interferences in atomic absorption
measurements.

3) Temperature programming and gradient elution are used in gas chromatography and high
performance liquid chromatography respectively. Evaluate the relative merits of
temperature programming over isothermal in GC as well as gradient elution over isocratic
separations in HPLC.

4) Critically evaluate the role of hollow cathode lamp in atomic absorption spectrophotometric
analysis, citing the process for the production of atomic line and its interaction with the
atomic species as the key factors.

5) Relate the use of temperature programme as applied to graphite furnace atomic absorption
technique and explain all the processes involved.

6) Explain the following observations.

a) For the same concentration of nickel, the absorbance at 352.4 nm was found to be
about 30% greater for a solution that contained 50% ethanol than for an aqueous
solution.
b) The emission spectrum of a hollow-cathode lamp for molybdenum has a sharp line at
313.3 nm as long as the lamp current is less than 50 mA. At higher currents, however,
the emission line develops a cuplike crater at its maximum.
 Section B (40 marks)

7) The chromatogram shows the separation of 4 sugars using normal phase HPLC (more polar
stationary phrase less polar mobile phase) with a 4.6 x 250 mm column. (20 marks)

Compound Retention Time (min.) Baseline Peak Width (min.)

Unretained Peak 1.583 -
Fucose 5.879 0.49488
N-Acetylglucosamine 6.881 0.60192
Galactose 8.295 0.43632
Glucose 9.121 0.56112

i) Calculate the retention factor (k) of fucose.

ii) Calculate the number of plates and plate height (in mm/plate) using the
glucose peak. )

iii) Calculate the resolution (Rs) and the separation factor () between galactose
and glucose.

iv) Methylglucopyranoside can be made from glucose in the reaction shown

below ( form only shown assume no other forms of the sugars exist).
Predict whether you would expect methylglucopyranoside to be eluted
before or after glucose. Explain your prediction in terms of polarity
considerations.
 8) The IR below is for C4H8O2. Identify and label four (4) peaks in the spectrum that are
consistent with the molecular formula given. Does the molecule contain a carboxylic
acid? (10 marks)

9) You are given the following IR spectrum and the molecular formulae of Compound
A, Compound B and Compound C. Which of the compound match the IR spectrum,
giving your reasoning and evidence for the match. (10 marks)

Dr Tioh NH & Dr Tee SF

May 15, 2017