UNIVERSITY OF EAST ANGLIA

School of Chemistry
Main Series UG Examination 2015-16

INSTRUMENTAL ANALYTICAL CHEMISTRY

CHE-5501Y

Time allowed: 2 hours

Answer THREE questions.

You are advised to spend an equal amount of time on each question.

All questions carry an equal number of marks.

Answer EACH question in a SEPARATE answer book.

The breakdown of marks within each question is indicated by the percentage figures
in brackets on the right.

The following is provided:

Graph paper

Do not take this question paper out of the examinations room.

Notes are not permitted in this examination.

Do not turn over until you are told to do so by the Invigilator.

(CHE-5501Y) Module co-ordinator: Dr Andrew Mayes (CHE)

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1. Answer ALL parts (a) to (c).

(a) Define the analytical terms: technique, method and procedure. Explain what is
meant by the limit of detection within the context of random noise arising from the
instrument being used. [24%]

(b) Explain, within the framework of an analytical programme, how you, as the
Chief Analyst for a company would demonstrate that the company, across all its
manufacturing sites, is meeting its stated requirement for a caffeinated beverage to
contain 0.1 mg mL-1 of caffeine. [40%]

(c) As part of a study into the trace metals found in the natural waters in Lithuania
the iron content was determined by atomic absorption spectroscopy at 248.3 nm.

For the analysis, a standard solution of iron was prepared with a concentration of
0.204 mg L-1. A series of standard addition samples was then prepared by adding
1.00 mL of the natural water into a 10 mL class A volumetric flask and adding a
known volume of standard solution as shown in the table below. The solution was
then made up to the mark in the volumetric flask using distilled water. Samples were
then taken from the diluted solutions and the absorbance at 248.3 nm in the atomic
absorption spectrum measured.

Sample Volume of Volume of Absorbance at

water / mL standard / mL 248.3 nm
1 1.00 0.00 0.042
2 1.00 1.00 0.113
3 1.00 2.00 0.156
4 1.00 3.00 0.225

Use a graphical method to determine the concentration (mg L-1) of the iron in the
original natural water. [36%]

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2. Answer ALL parts (a) to (d).

(a) Describe, with the aid of an appropriately labelled diagram, the key
components of a combination pH electrode and outline how the device detects the
pH of a solution. [40%]

(b) The potential difference detected by an ion-selective electrode is given by the

expression below.
2.303RT
E ISE = Cell const + β log10 [ A]
jF

Explain the meaning of each term in this expression and give the units of any physical
constants. [20%]

(c) A pH electrode gives a reading of 0.532 V when placed in a solution with a pH

of 3.00. When placed in a solution with a pH of 5.9, the same electrode gives a reading
of 0.363 V. Calculate the electromotive efficiency of this electrode assuming to
be 0.02562 [25%]

(d) The apparent pH recorded by the electrode from (c) was monitored as a
function of [OH-]. The data recorded using NaOH or NH4OH as the source of OH-
ions are shown in the figure. Account for these observations. [15%]

log[OH¯]

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3. Answer ALL parts (a) to (c).

(a) A tungsten lamp is an example of an incandescent filament lamp.

How, and why, do the intensity and wavelength of the output from such a lamp vary
with the temperature of the filament? What is the purpose of adding iodine to the
lamp envelope? [40%]

(b) Optical filters are used in spectrometers to block the transmission of selected
wavelengths. Explain the difference between interference (Fabry-Perot) and
absorption filters and describe how these two categories of filter differ in their
appearance to the eye? [40%]

(c) Why is a photomultiplier tube not used as a detector at infrared wavelengths.

[20%]

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4. Answer ALL parts (a) to (d).

(a) Explain the following terms relating to chromatography:

(i) stationary phase

(ii) mobile phase
(iii) separation
(iv) resolution [20%]

(b) What key properties must an analyte have in order to be quantitated using
gas chromatography? [10%]

(c) Many different types of detectors can be used to detect analytes in gas
chromatography (GC), but the flame ionisation detector is still one of the most
common. With the help of a labelled diagram, explain how a flame ionisation
detector works. [45%]

(d) For many years the standard internal diameter of most HPLC columns has
been 4.6 mm. During the last few years there has been a trend towards using smaller
diameter columns.

(i) Calculate how much less solvent is required to carry out a separation
using a 2.1 mm internal diameter column compared with a 4.6 mm internal
diameter column of the same length, assuming that the linear mobile phase
velocity is kept the same in both columns and that no other separation
parameters change as a result of the column change. [10%]

(ii) What are the key benefits of reducing solvent consumption during HPLC
analysis. [5%]

(iii) Explain why the heights of the peaks in the detector response increase,
when switching from a 4.6mm internal diameter column to a 2.1 mm one. [10%]

END OF PAPER

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