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CONFIDENTIAL

EH/OCT 2012/CHE335/393

UNIVERSITI TEKNOLOGI MARA


FINAL EXAMINATION

COURSE

BASIC INSTRUMENTAL ANALYSIS

COURSE CODE

CHE335/393

EXAMINATION

OCTOBER 2012

TIME

3 HOURS

INSTRUCTIONS TO CANDIDATES
1.

This question paper consists of five (5) questions.

2.

Answer ALL questions in the Answer Booklet. Start each answer on a new page.
Do not bring any material into the examination room unless permission is given by the
invigilator.

4.

Please check to make sure that this examination pack consists of:
i)
ii)
iii)

the Question Paper


a one-page Appendix
a Answer Booklet - provided by the Faculty

DO NOT TURN THIS PAGE UNTIL YOU ARE TOLD TO DO SO


This examination paper consists of 6 printed pages
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EH/OCT 2012/CHE335/393

QUESTION 1

a) Sketch the energy level diagram which consists of rotational, vibrational and electronic
energy levels.
(5 marks)
b) A transducer can produce an electrical signal that is easily amplified and has a low
electrical noise level. List three (3) examples of transducers used in spectroscopic
instruments.
(3 marks)
c) A solution containing 5 ppm of KMn0 4 has a transmittance (T) of 0.360 measured in a
1.5 cm cell at 500 nm. Calculate the molar absorptivity (s) of KMn0 4 in L.mol"1.cm"1.
Given:
Molecular weight KMn0 4 = 158 g.mol"1
(4 marks)
d) The molar absorptivities, (s) at two wavelengths (A) of Co(N0 3 ) 2 and Cr(N03)3 in the
unknown sample are summarized in the following table.
Table 1 Molar absorptivities of Co(N0 3 ) 2 and Cr(N0 3 ) 3

Molar absorptivity
(M*1crrT)
/ Component
510
575

Co(N03)2

Cr(N03)3

36200
5520

1240
16500

The detected absorbance at wavelength {X) of 510 nm and 575 nm are 0.671 and
0.330 respectively. The cell's path length (b) is 1.0 cm. Calculate the concentration (c) of
Co(N0 3 ) 2 and Cr(N03)3.
(7 marks)
QUESTION 2

a) Figure 1 shows two analyte bands in two different High Performance Liquid
Chromatography (HPLC) columns, Column X and Column Y, which have the same
length, 150 mm.

A B

Figure 1 Two analyte bands in Column X (left) and Column Y (right)


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i)

EH/OCT 2012/CHE335/393

Regardless of the concentration of the analytes, sketch the peaks of the


chromatogram of both columns that correspond to the separation results.
(6 marks)

ii) Suggest a method to improve resolution in column X.


(2 marks)
b) Identify four (4) characteristics of an ideal detector of Gas Chromatography (GC).
(4 marks)
c) Explain a difference between Flame Ionization Detector (FID) and Thermal Conductivity
Detector (TCD) and give an advantage for each of them.
(6 marks)
d) State two (2) characteristics of immobilized liquid stationary-phase in GC.
(2 marks)

QUESTION 3

a) Explain the two (2) functions of guard column and one (1) function of degasser in High
Performance Liquid Chromatography (HPLC).
(6 marks)
b) Explain a difference between gradient elution and isocratic elution. From these two types
of elution, state which could give a better separation and explain why.
(6 marks)
c) The following data apply for liquid chromatography on a 25 cm packed column. A
chromatogram of a mixture of species A and B provided the following data.
Species
A
B

Retention Time (tR), min


17.30
19.92

Width of Peak Base (W), min


1.10
1.22

Determine the following.


i)

The column resolution (Rs).

(2 marks)

ii) The average number of plates (Nav) in the column.

(4 marks)

iii) The plate height (H).

(2 marks)

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EH/OCT 2012/CHE335/393

QUESTION 4

a) Figure 2 presents the FTIR spectrum for an alkene.


i)

If the spectrum belongs to 1-octene, draw the chemical structure.


(2 marks)

ii) Referring to Figure 2, list two (2) possible bonds which correspond to the highlighted
regions and verify the spectrum is for 1-octene.
(4 marks)
iii) State the intensity of the transmittance of both peaks either it is strong, medium or
weak.
(4 marks)
b) Double beam in time is the most common type of spectrophotometer instrument which is
commercially available. Figure 3 below shows a schematic diagram of this instrument.
Label all the components in this figure.
too.
50- ^ 1

o***

( > <

^ ft

f - - T

j P i

ruH HB

B
C
Figure 3: Schematic diagram of Double Beam In Time.
(9 marks)

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EH/OCT 2012/CHE335/393

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EH/OCT 2012/CHE335/393

QUESTION 5
a) Define atomization.
(3 marks)
b) Determine the longer wavelength using these two data sets; light with a frequency of
7.84 x 1013 s"1 and light with energy of 5.13 x 10"13 J. Given c = 3.00 x 108 ms"1 and
fc = 6.63x10-34J-s.
(6 marks)
c) List the three (3) steps of heating process in electrothermal atomizers.
(3 marks)
d) The two most common methods of sample atomization encountered in Atomic
Absorption Spectrometry (AAS) are flame atomization and electrothermal atomization.
Flame atomizer is an example of a discrete atomizer and it is the critical step because a
lot of complex ions produce in the flame.
i) Sketch and label the diagram of flame region for AAS.
(4 marks)
ii) Explain the atomization process occurred for every region.
(6 marks)

END OF QUESTION PAPER

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Functional Group
Alcohol
O-H
O-H
C-0
Alkane
C-H
-C-H
Alkene
=C-H
=C-H
C=C
Alkyl Halide
C-F
C-CI
C-Br
C-l
Alkyne
C-H
-c.sr.
Amine
N-H
C-N
N-H
Aromatic
C-H
C=C
Carbonyl
C=0
Ether
C-0
Nitrile
CN
Nitro
N-0

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APPENDIX 1

EH/OCT 2012/CHE335/393

Type of Vibration

Characteristic
Absorptions (cm' 1 )

(stretch, H-bonded)
(stretch, free)
(stretch)

3200-3600
3500-3700
1050-1150

Stretch
Bending

2850-3000
1350-1480

stretch
bending
stretch

3010-3100
675-1000
1620-1680

stretch
stretch
stretch
stretch

1000-1400
600-800
500-600
500

stretch
stretch

3300
2100-2260

stretch
stretch
bending

3300-3500
1080-1360
1600

stretch
stretch

3000-3100
1400-1600

stretch

1670-1820

stretch

1000-1300(1070-1150)

stretch

2210-2260

stretch

1515-1560 & 1345-1385

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