Universiti

Malaysia
Q PAHANG

Engineering . Technology Creativity

FACULTY OF CHEMICAL & NATURAL RESOURCES ENGINEERING

FINAL EXAMINATION
COURSE

: ANALYTICAL CHEMISTRY

COURSE CODE

: BKF1243

LECTURER

: EMAN N. AL!
FARHAN BINTI MOHD SAID

DATE

: 17 JUNE 2O15

DURATION

: 3 HOURS

SESSION/SEMESTER

: SESSION 2014/2015 SEMESTER II

PROGRAMME CODE : BKB/BKC/BKG

INSTRUCTIONS TO CANDIDATE:
I.
2.
3.
4.

This question paper consists of FOUR (4) questions. Answer ALL questions.
All answers to a new question should start on new page.
All the calculations and assumptions must be clearly stated.
Candidates are not allowed to bring any material other than those allowed by
the invigilator into the examination room.

EXAMINATION REQUIREMENTS:
1.

APPENDICES

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

This examination paper consists of NINE (9) printed pages including front page.

CONFIDENTIAL

BKB/BKC/BKG/1415111BKF1243

QUESTION 1
Analytical chemistry results need to be evaluated before writing the reports. Therefore,
data evaluation consider as a normal practice while doing research work or analysis of
any product.
a) The following data (Table 1) shows the content of the glucose content in a sample
using ultraviolet-visible methods (UV-VIS) and high performance liquid
chromatography (HPLC). Determine whether there is a significant difference in
variance between the two methods.
Table 1: Data of glucose content on two different methods
No

Glucose content (mg/ml)

sample

UV-VIS

HPLC

13.8

13.0

13.6

15.2

14.6

14.0

13.5

13.3

15.0

13.5

(17 Marks)
b) In the titration of 10.00 0.14 ml of 0.10 0.05 M NaOH, 20.50 0.05 ml of HC1 is
required for neutralization. Determine the moiarity of HCl and identify the
uncertainty of the value.
(8 Marks)

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BKB/BKCIBKG/1415111BKF1243

QUESTION 2
Gravimetric methods are one of oldest techniques in analytical chemistry which is
considered the fundamental method.
a) Determine the mass of Cu (103) 2 can be formed from 0.500 g of CuSO4.51-120.
(4 Marks)
b) A 0.2 121 g sample of an organic compound was burned in a stream of oxygen, and
the CO2 produced was collected in a solution of barium hydroxide. Calculate the
percentage of carbon in the sample if 0.6006 g of BaCO 3 was formed.
(4 Marks)
c) Describe:
i)

Inclusion
(1.5 Marks)

ii)

Occlusion
(3 Marks)

d) Titration is a method of analysis using standard material as titrant to get the

concentration of the analyte. Describe the preparation of:
i)

500 mL of 0.0750 M AgNO 3 from the solid reagent.

(3 Marks)

ii)

2.00 L of 0.325 M HCL, starting with a 6.00 M solution of the reagent.

(2.5 Marks)

iii)

A 50.00 mL of 0.100 M NaOH is titrated with 0.100 M HCL. Calculate

the pH of the solution after addition of 0.00, 10.00, 50.00, and 60 mL of
acid, and draw a titration curve from the data.
(7 Marks)

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BKB/BKC/BKG/14151I1BKF1243

QUESTION 3
Measurements based on light and other forms of electromagnetic radiation are widely
used throughout analytical chemistry. The interactions of radiation and matter are the
subject of science called spectroscopy.
a) Beryllium (II) forms a complex with acetylacetone (166.2glmol). Calculate the molar
absorptivity of the complex, given that a 1.34 ppm solution has atransmittance of
55.7% when measured in a 1.00 cm cell at 295 nm.

(6 Marks)
b) Express the following absorbance in terms of percent transmittance:
i) 0.494
(2 Marks)
ii) 0.229
(1 Mark)
c) Convert the following transmittance data to absorbance:
i) 0.013
(2 Marks)
ii) 55.5%

(1 Mark)
d) A typical simple infrared spectrometer covers a wavelength range from 3 to 15 .im.
express the range in wavenumbers.
(4 Marks)
e) Explain wave property that is measured by Fourier Transform JR and the units for
this property?
(2 Marks)
f) Draw a simple spectrum using FTIR showing the following with naming x-y axis.
4

CONFIDENTIAL

i)

BKB/BKCIBKG/141511jB1cy1243

Transmittance and,
(2 Marks)
Absorbance
(2 Marks)

g) List the names of three equipments in applying spectroscopy technology.

(3 Marks)

QUESTION 4

a) An HPLC separation of two components pharmaceutical product yielded the

following results (Table 2).

Table 2: Retention time and peak width of caffeine and aspirin on HPLC
Compound

Retention time

Peak width at base

Peak width at V2

(mm)

(mm)

height (mm)

Solvent

30

Aspirin

75

6.5

3.0

Caffeine

86

8.1

3.25

Determine the following items:

i) The capacity factor, k, for each compound.
(4 Marks)
ii) The plat number of each compound using base widths.
(5 Marks)

iii) The resolution of the two compounds, R.

(3 Marks)
5

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BKB/BKCIBKG/1415111BKJ1243

iv) Given the column used in this analysis is 25 cm long, determine the height of the
theoretical plate?
(4 Marks)

b) The separation of two compounds on a packed and capillary column gave the
following data in Table 3:

Table 3: Data of two compounds on a packed and capillary column

Component

Packed column

Capillary column

Dead time (s)

15

30

Retention time of Component A (s)

160

75

Retention time of Component B (s)

170

86

Number of theoretical plates

6400

1967

Identify which column is giving the better resolution and, justify your answer.
(9 Marks)

END OF QUESTION PAPER

CONFIDENTIAL

BKB/BKC/BKG/1415111BKF1243

APPENDICES
hc
E = h V = - = hcv

xi
N

A = logT = log- = log-- = abC = sbC

po

R =

2Z

WA

PT

(x

2[(tR)B(tR)A]

+ WB

i=1

WA+WB

Ni

tRtM

k'

F2
exp
a (

t R)B

tM

( t R)A tM

u Xx -J

exp

N = 16(t/w)2

pX = - Jog [X]
H

_1JSA

+SB
2

R)
=
SR

;
r(L

)2

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BKB/BKC/BKG/1415111BKF1243

Table 1: F-table for one-tailed test at 95% confidence level

i:TabIe for One-Tailed Test at cc= 0.05
(95% Confidence Level)
i

2
4
5
6
8
9
10
ii
12
13
14
15
16
17
18
19
20
00

5
6
10
9
.---- 7 .-- 8 -161 4
1993
215.7
2244
2302
234.0 236.
238.9
2405
241,9
18.51
19.00
19.16
1925
1930
1933 1935
19.37
-19.38
19.40
10.13
91552
9.277
9.117
9013
8
8,845
8.812
8.786
7.709
6.944
5.591
6388
6.256
6.163 6.094
6.041
5.999
5964
5,786
6.608
5.409
5 192
5050
4.950 4.876
4818
4,735
4.772
5.987
5.143
4.757
4.534
4387
4284 4.207
4.147
4.099
4.060
5.591
4.737
4.347
4.120
3.972
3.666 3.787
1726
3677
3.637
5,318
4.459
4.066
3.838
3.587
3.581 3.500
3438
3.347
3.358
5.117
4256
3.863
3.63-3
3482
3374 3,293
3.230
3.179
1137
4.965
4.103
3.708
3,478
3.326
3.217 3.135
3.072
3.020
2.978
4.844
3.982
3.587
3.357
3204
3.095 3.012
1948
2896
2.854
4.747
3885
1490
3.259
3.196
2.996 2.913
2.849
1796
2.753 -
4.667
3.806
3.411
3.179
3.025
2,915 2.832
2767
2.714
2671
4.600
3.739
3.344
3.112
1958
2.848 2.764
2.546
2,602
2.699
4.534
3 682
3.287
3056
2.901
2.790 2707
2.641
2588
2.544
4.494
3.634
3.239
3.007
2.852
2.741
2.657
2.591
2.538
2.494
4.451
3.592
3.197
2.965
2.810
2.699 3614
2.450
2.494
2.548
4.414
3.555
3.160
2.928
2.773
2661 2.577
2.456
2,412
2.510
4.381
-3.552
3.127
2.740
2.895
2.628 2.544
2477
2.423
2.378
4.351
3.493
3.098
2.866
2.711
2.447
2.348
2.599 2.514
2.393
3.842
2.996
2.605
2.372
2.214
2.099 2.010
L831
1.938
1.880

15

co

20

2459
248.0
2543
19.43
19.46
19.50
S..660 8.526
8.703
5628
5.858
5.803
4.619
4.558 4365
3.874 3.669
3.938
3,445 3230
3.511
1218
3.150 2.928
2.935 2307
3.006
2374 2338
2.845
2 646 2,404
2.719
2.544
1296
2.617
2.459 2.206
2.533
2.131
2.388
2.463
2.066
2403
2.328
2.352
2.276 2.010
1.960
2.230
2.308
1.917
2.191
2.269
2134
2.155
1.878
2.124
1.843
2.203
1.666
1570
1000

'e degrees of freedom in numerator v2 = degrees of freedom in denominator

Table 2: F-table for two-tailed test at 95% confidence level

F-Table for Two-Tailed Test at a = 0.05
(95% Confidence Level)
V31V11
1
2

3
4
5
6
7

8
9
10
11
12

13
14
15

10

15

20

984.9
993.1 1018
963.3
968.6
921.8
937.1
948.2
956.7
864.2
899.6
647.8
799.5
39,43
39.39
39.40
39-45
39498
39.36
39.37'
39.30
39.33
39.17
39.25
38.51
39,00
14.25
14.17
13.902
14.62
14.54
14.47
14,42
14.73
15.10
14.88
15.44
16.04
17.44
9.074
8.980
8.905
8.844
8.657
8.560
8.257
9.197
9,605
9.364
9.979
10.65
12.22
6.619
6.015
6.681
6.428
6.329
6.757
6.978 6.853
7.146
7.388
7.764
8,434
10.01
5.600
5.523
5.461
5,269
4.849
5.168
5.820 5.695
5.988
6.227
6.599
7.260
.8.813
4.823
4.761
4.568
4.467
4,142
4.899
5.119 4.995
5.285
5.890
5.523
6.542
8.073
4.529
4.433
4.357
4,295
4.101
1670
4.652
3.999
4.817
5.053
5.416
6.059
7.571
4.102
4.026
3.964
3.769
1667
3.333
4.484
4.320 4.197
4.718
5.078
5.715
7.209
3.855
3,779
3.717
4.072 3,950
3.522
3.419
3.080
4.236
4.468
4,826
5.456
6.937
3.588
3.526
2283
3,759
3.664
3330
3.226
4.044
3.881
4275
4.630
5.256
6.724
3.436
3.374
3.512
3.177
3.073
2.725
3.728 3.607
3.891
4.121
4.474
5.096
6.544
2.948
3.604 3.483
3.388
3.31-2
3.250
3.053
2.596
3.767
3.996
4.347
4.965
6,414
3.380
3.285
1209
3.147
2.949
2.844
2.487
3.501
3.663
3.892
4.242
4.857
6.298
2.756
3.199
3.123
3.060
2.862
2.395
3,415 3.293
3.576
3.804
4.153
4.765
6.200
Ov, =degrees of freedom

In

numerator v3 degrees of freedom in denominator

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BKB/BKC/BKG/1415111BKF1243

Table 3: Table of critical value of Q test

(Rtji.ci ii

Q
Ntmber of
Obsrvation

90% Confidence

>

Q.

5% ConiIdence

99% Confidence

0.970
0.829
0.710
0.625
0L56

04994
0.926
0.821
0.740
0.68()
0.634
0,598
0.568

3
4
5
6
7

0.941
0.765
(o.oi
0.560
0.507
O46

0.526

9
JO

0.437
0.412

0.493
0.466

Table 4: Periodic Table

The Periodic Table of the Elements