,

UNlVERSlTl
TEKNOLOGI
PETRONAS

COURSE CD83093 - ANALYTICAL CHEMISTRY

DATE 4 AUGUST 2019 (SUNDAY)
TIME 2.30 PM - 5.30 PM (3 HOURS)

INSTRUCTIONS TO CANDIDATES

1. Answer ALL questions in the Answer Booklet.

2. Begin EACH answer on a new page in the Answer Booklet.
3. Indicate clearly answers that are cancelled, if any.

4. Where applicable, show clearly steps taken in arriving at the solutions and
indicate ALL assumptions, if any.
5. DO NOT open this Question Booklet until instructed.

Note
i. There are ELEVEN (11) pages in this Question Booklet including the
cover page and appendices.
11. DOUBLE-SIDED Question Booklet.
Universiti Teknologi PETRONAS
 •
COB 3093

1. a. Richard and Willard determined the atomic mass of lithium and

collected the followingdata as shown in TABLE Q1.

TABLE Q1
Experiment
1
I
I
I
I
Molar mass (g/mol)
6.9391
l
I
2 6.9407
I
3 6.9409
4 6.9399
5 6.9341

i. Calculate the coefficient of variation for the data.

[6 marks]

ii. Discuss TWO (2) reasons that may cause the variation in
the experimental data.
[4 marks]

iii. If the true value for the atomic mass of lithium is 6.941 g/mol,
calculate the absolute error and the relative error of the
mean value.
[5 marks]

2
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COB 3093

b. Lithium is in the alkali-metal group and commonly used in batteries,

ceramics, air-conditioning, grease, electric cars, and in
pharmaceutical products. Lithium can be found in continental brine
water, geothermal waters, and oil-gas field brines.

i. Suggest the suitable instrument used to determine the

concentration of lithium ion in water sample and briefly
explain its basic principle(s).
[5 marks]

ii. Calculate the grams of hydrogen (MW = 1.00 g/mol) formed

by the complete reaction of 80.57 g of lithium (6.941 g/mol)
with water.
[5 marks)

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COB 3093

2. a. Cryolite, Na:AIF6 (MW = 210 g/mol), is an ore used in the

production of aluminium.

i. Construct an experimental outline to produce pure cryolite

from the reaction between aluminium oxide, sodium
hydroxide and hydrofluoric acid, and show the chemical
balance of the reaction.
[7 marks]

ii. Discuss ONE (1) possible impurity during the precipitation

process and suggest a method to avoid the impurity.
[3 marks]

iii. If 13.9 grams of aluminium oxide (MW = 101.96 g/mol),

50.4 grams of sodium hydroxide (MW = 40.0 g/mol) and
50.4 grams of hydrofluoric acid (MW = 20.0 g/mol) react
completely, calculate the mass of cryolite (in grams) that will
be produced.
[5 marks]

iv. Estimate the total mass of the excess reactant(s) remain

after the reaction is complete.
[6 marks]

b. A 0.2121 g sample of an organic compound was burned in a stream

of oxygen, and the C02 (MW= 44 g/mol) produced was collected in
a solution of barium hydroxide (MW = 171.34 ). Calculate the
percentage of carbon (MW = 12 g/mol) in the sample if 0.6006 g of
BaC03 (MW = 197.34 g/mol) was formed.

[4 marks]

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 CDB 3093

3. a. The Beer-Lambert's law is the linear relationship between

absorbance (A) and concentration (c) of absorbing species.

i. Develop a mathematical correlation between the absorbance

of a molecule to the concentration (c) and the path length (b)
of a sample.
[5 marks]

ii. A 1.25 g tablet containing drug D (MW = 270 g/mol) has a

molar absorptivity of 703 cm- 1 .moi- 1 .L at 262 nm was
dissolved in 1.50 L water. If the solution exhibits an
absorbance of 0.687 in a 10.0 mm cell, calculate the weight
percentage of the drug in the tablet.
[5 marks]

b. Without using energy level diagram, discuss the similarity and

differences of the radiation absorptivity of an atomic substance and
a molecular substance.
[6 marks]

c. Two organic compounds (CxHyOz) with a molecular weight of

72.11 g/mol produced two different Fourier-transform infrared
spectroscopy (FTIR) spectra, spectrum A and spectrum Bas shown
in FIGURE Q3a and FIGURE Q3b respectively. Analyze each
spectrum by considering ALL possible functional groups. Identify
and state the IUPAC name of both compounds.
[9 marks]

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!r\IFRARED SPECTRUr'v1
1.0 I

0 8
!-
~
r-
~'-----------~-·-- ·------._r·
~.,"'·~
! $,
,, j

\f
w
u f I \l \j

~
z 0.6~
<(
l
~
l
l

:::2:
I
l/1
z<( 0.4~ I
I \JI
a: I l il
f-
0.2 ~
l ~
0.0
r
3000 2000 1000
Wavenumber (cm-ll

FIGURE Q3a

INFRARED SPECTRUM

3000 2000 1000

Wavenumber (cm-1)

FIGURE Q3b

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 COB 3093

4. a. As an engineer, you are responsible to investigate the contaminant

in the gas composition (mainly hydrocarbons) before entering the
plant.

i. Suggest a chromatography instrument to separate the gas

composition and briefly explain the basic principle(s) of the
instrument used during the analysis. Explain your answer
using the schematic diagram of the instrument.
[6 marks]

ii. If the chromatogram results show that some of the

compounds are not completely separated, propose TWO (2)
ways to improve the separation.
[4 marks]

b. Table Q4 shows the gas chromatography data for three different

compounds. Estimate the number of theoretical plates (N) for each
compound and the average number of theoretical plates for the
column.

TABLE Q4
Compound Retention time Width at the base
tr (min) w (min)
A 8.04 0.15
B 8.26 0.15
c 8.43 0.16

[5 marks]

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c. High performance liquid chromatography (HPLC) is a technique in

analytical chemistry used to separate, identify, and quantify
component present in a mixture.

i. Provide TWO (2) examples of detectors used in HPLC.

[2 marks]

ii. The separation efficiency in HPLC increases as the size of

the particles in stationary phase decreases. Discuss this
statement.
[3 marks]

iii. The chromatograms a, b and c shown in FIGURE Q4 are

obtained from HPLC analysis of a mixture using the same
mobile phase, flow rate and different temperatures (T = 25,
35 and 45 °C). Label the chromatograms a, b and c in terms
of column temperature (T) and resolution of each
chromatogram. Justify the observed differences in the
resolution.
[5 marks]

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FIGURE Q4

-END OF PAPER-

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APPENDIX A

FTIR Group Frequencies for Organic Functional Groups

Type of Compound Frequency Intensity

Range, cm- 1
Alkanes 2850-2970 Strong
1340-1470
Alkenes 3010-3095 Medium
675-995 Strong
Alkynes 3300 Strong
Aromatic rings 3010-3100 Medium
690-900 strong
Monomeric alcohols, phenols 3590-3650 Variable
Hydrogen-bonded alcohols, phenols 3200-3600 Variable,
Monomeric carboxylic acids 3500-3650 sometimes broad
Hydrogen-bonded carboxylic acids 2500-2700 Medium
broad

Amines, amides 3300-3500 medium

Alkenes 1610-1680 Variable

Aromatic rings 1500-1600 Variable

Alkynes 2100-2260 Variable
Arnines, amides 1180-1360 Strong

Nitriles 2210-2280 Strong

Alcohols, ethers,carboxylic acids, esters 1050-1300 Strong

Aldehydes, ketones, carboxylic acids, esters 1690-1760 Strong

Nitro compounds 1500-1570 Strong

1300-1370

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APPENDIX B
List of Formula

Area of Gaussian peak

= 1.064 X h X W112
= 1.064 X h X 2.35 a

Adjusted retention time. ( = L- tr,

Capacity factor, k'=(t-t 11,)/Ln = t)t,r,

Plate height, H = LIN

Resolution =~\Uwav
= \4N (a~~) (1:~?av)
Response factor:

Rl=F(~)

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