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-1 Universiti

I j Malaysia
PAHANG
Engineering . Technology Creativity

FACULTY OF CHEMICAL & NATURAL RESOURCES ENGINEERING


FINAL EXAMINATION
COURSE

: ANALYTICAL CHEMISTRY

COURSE CODE

: BKF1243

LECTURER

: EMAN N. ALl
FARHAN BT MOHD SAID

DATE

: 18 JUNE 2014

DURATION

: 3 HOURS

SESSION/SEMESTER

: SESSION 2013/2014 SEMESTER II

PROGRAMME CODE : BKB/BKC/BKG

INSTRUCTIONS TO CANDIDATE:
1.
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 - List of Formulas and Statistic Tables

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/1314111BK1F1243

QUESTION 1

a) Two different laboratories were participated in an inter-laboratory study involved


the determination of the Ca level in water samples. The following results are
replicated determination of the Ca for laboratories A and B in ppm.
Table 1: Ca levels of water sample of Sungai Gebeng for Laboratories A and B
Result

Ca level (ppm)

no.

i)

Laboratory A

Ca level (ppm)
Laboratory B

10.1

10.6

10.0

10.5

10.4

11.1

State the appropriate hypothesis of the above analysis


(2 Marks)

ii) Conduct a statistical test to determine whether the laboratories differ at the
95% confidence level?
(12 Marks)
iii) Do they differ at 99% confidence level (F 11 = 18)?
(2 Marks)

CONFIDENTIAL

BKB/BKCIBKG/1314111BKF1243

b) Ammoniacal nitrogen can be determined by a treatment of the sample with


chioroplatinic acid. The product is slightly soluble ammonium chioroplatinate:
H2PtC16 + 2NH4

(NHPtC16 + 2H

The precipitate was then decomposed on ignition, yielding metallic platinum and
gaseous products (02, NH3, HCI).
i)

Perform the complete reaction of the precipitation when the ignition process
complete.
(2 Marks)

ii) Determine the weight and percentage of ammonia in a sample, if 0.2115 g gave
rise to 0.4693 g of platinum.
(7 Marks)

QUESTION 2
a) A solution of Ba(OH) 2 was standardized against 0.1175 g of primary standard grade
benzoic acid, C61-15 COOH (122.12 g!mol). The end point was observed after
additional of 45 ml of base.
i) Determine the molarity of the base.
(7 Marks)
ii) If the standard deviation of weighing was 0.2 mg and for the volume was
0.03 ml, determine the standard deviation/absolute uncertainty of the molarity
of the base.
(5 Marks)

CONFIDENTIAL

BKB/BKC/BKG/131411JBKF1243

b) Titrimetric method based on silver nitrate is sometime called argentometric method.


As a new staff member in the Fleischmann's Company, you are asked to calculate
and sketch the titration curve of p1 for the titration of 50.0 ml of 0.0250M KI with
0.0500M AgNO3 . To sketch the curve, you should cover three reactions, which are
pre-equivalence, equivalence and post- equivalence.
Given: For AgI, Ksp = 8.3x10'7
(13 Marks)

QUESTION 3

Spectroscopic analytical method is one of analytical methods which are based on


measuring the amount of radiation produced or absorbed by molecular or atomic species
of interest. The absorbance and concentration relationship should follow Beer's Law.
a) The complex formed between Cu(I) and 1,10-phenanthroline has a molar
absorptivity of 7000 L cm -1 mo1 1 at 435 nm, the wavelength of maximum
absorption. Calculate:
i)

The absorbance of a 6.77 X 10 M solution of the complex when measured in


a 1.00 cm cell at 435 nm.
(4 Marks)

ii) The percent transmittance of the solution in (a).


(4 Marks)
iii) The concentration of a solution that in a 5.00 cm cell has the same absorbance
as the solution in (a).

(3 Marks)

CONFIDENTIAL

BKBIBKCIBKG/1314111BKF1243

iv) The path length through a 3.40 X 10 M solution of the complex that is needed
for an absorbance that is the same as the solution in (a).
(3 Marks)
b)

Identify factors that cause the Beer's law relationship to depart from linearity.
(5 Marks)

c)

A sophisticated ultraviolet/visible/near-JR instrument has a wavelength range of


185 to 3000 nm. What are its wave number and frequency ranges?
(4 Marks)

d)

Sketch the energy level diagram in case of absorption and emission.


(2 Mark)

QUESTION 4
Chromatography analytical method is the most general and common separation
technique, where separation, identification and determination of compound can be done.
a) The following data were obtained by gas-liquid chromatography on a 40 cm packed
column.
Compound

tR (mm)

W(min)

Air

1.9

Methylcyclohexane

10.0

0.76

Methylcyclohexane

10.9

0.82

Toluene

13.4

1.06

Calculate:
i) An average number of plates from the data.
(5 Marks)

CONFIDENTIAL

BKB/BKC/BKG/1314111BKF1243

ii) An average plate height for the column.


(3 Marks)
iii) The resolution for Methylcyclohexane and Methylcyclohexane.
(3 Marks)
iv) The resolution for Methylcyclohexane and Toluene.
(2 Marks)
v) If the resolution 1.5 is desired in separating Methylcyclohexane and
Methylcyclohexane. How many plates are required to get the required
resolution?
(3 Marks)
vi) How long must the column be if the same packing is employed?
(3 Marks)
vii) What is the retention time for Toluene on the column in part (vi).
(3 Marks)
b) Sketch the three main parts in gas chromatography.
(3 Marks)

END OF QUESTION PAPER

CONFIDENTIAL

BKBIBKC/BKG/1314IIJBKFI 243

APPENDICES
Appendix A
Table 2: F-table for one-tailed test at 95% confidence level
FTabIe forOne-Tajied lest at c 005
(95% Confidence Level)
.1
1

161 4

18.51

-3

10.13

2
199.5
19.00

3
215.7
19.16

4. ,
224.6
19.25

5 -
230.2 1930

2.34.0
1933

236.8
19.35

10

15

20

238.9

240.5

2439

2459

248.0

1937

19.38

19.40

19.43

19.45

2543
19.50

9.552

9.277

9.117

9013

7.709

6.941

8941

8.587

8.945

8.812

8.786

8-703

6591

6383

6.256

6.608

5.786

6.153

6.041

5.999

5364

5-409

S 192

5050

4.950

60-4
4.876

5.987

5143

4.613

4.772

4.733

5.858
4.619

4.757

4.534

37

4394

5391

4.207

4337

4.147

4, 0-59

4.060

3933

4.347

4.120

1972

3.866

3.787

1637

4.459

4,066

3.838

3.687

3.581

3.500

3.3SS

3.347

3.511
1210

3.445

5,318

3.677

3.726
3438

3.150

2.928

9
10

5.117
4.965

4.256
4.103

1863
3.708

3.633
3.479

3482
3326

3,374
3.217

1293
3.135

3.230
3.072

3.179
3.020

3,137
2.978

3.005
2,845

2.938
2.774

11

4.844

3.982

3.587

3.337

3.095

3012

2.948

2.896

2854

2.719

2 646

12

4.747

3.885

3.490

3.259

3.204
3106

2.707
2S38
2.404

2.996

2.913

2.849

2.753

2.617

2.544

2.296

13

4.667

3.806

3.411

3.179

3.025

2,915

2.832

2,767

2.796
2.714

2671

4.600

3.739

3.344

3.112

2.958

2.848

2.699

2.646

2.602

15

4.534

3.682

3.287

2.901

2.790

2.641

2.583

2.544

2.403

2.328

2.131
2.066

16

4.494

3.634

3.239

3.056
3.007

2.764
2.707

2.459
2,388

2.206

14

2.533
2.463

2.852

2.741

2.657

2.276

2.010

3.592

3.197

2.965

2810

2.699

3614

2.538
2.494

2.352

4451

2.591
2.548

2.494

17

2.450

2.308

2.230

1.960

18

4.414

3.555

3.150

2.928

4.381

3.552

3.127

2.895

2661
2.628

2.577
2,544

2.510
2477

2,456
2.423

2412

19

2.773
2.740

2.378

2.269
2.234

2.191
2.155

1.878

20

4.351

3,493

3.098

2865

2.711

2.599

2.514

2.447

2.393

2.348

2.203

2.124

1.843

3.842

2.996

2.605

2.372

2.214

2.099

2.010

1.938

1,880

1.831

1,656

1.570

1.000

9.660
5303
4.558
3.874

8526
5.628
4365
3.669
3.230

1,917

= degrees of freedom in numerator v = degrees of freedom in denominator

Table 3: F-table for two-tailed test at 95% confidence level


F-Table for Two-Tailed Test at a = 0.05
(95% Confidence Level)
v2lv ia
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15

10

15

20

993.1 1018
9. 68.6
984.9
948.2
956.7
9613
937.1
899.6
921.8
864.2
647.8
799.5
39.498
3943
3945
39.39
39.36
39.37
39.40
39.33
39.30
39.25
39.17
38.51
39,00
14.17
1.3.902
14.25
14.54
14.47
14.42
14.62
14.73
14.88
15.10
15.44
16.04
17.44
8.560
8.257
8.844
8.657
8380
8.905
9.074
9.197
9,605
9.364
9.979
10.65
12.22
6.015
6.619
6:428
6329
6.681
6.757
6.853
6.978
7.146
7.388
7.764
8,434
10.01
4.849
5.461
5.269
5.168
5.523
5.695
5.600
5.820
5.988
6.227
6.599
7.260
8.813
0.142
4.467
4.761
4.568
4.823
4.899
5.119
4.995
5.285
5.523
5.890
6.542
8.073
4.101
3.999
3.670
4,433
4.357
4.295
4.652 4.529
4.817
5.053
5.416
6.059
7.571
3.667
3,769
3333
4.102
4.026
3.964
4.320 4.197
4.484
4.718
56078
5.715
7.209
1080
3.522
3.717
1419
1855
3.779
3.950
4.072
4.236
4.468
4.826
5.456
6:937
2.883
3.526
3.330
3.226
3,664
3.588
3.759
4.044
3.881
4.275
4630
5156
6.724
2.725
3.436
3.374
3.073
3.177
3.607
3.512
3.728
3.891
4.121
4474
5.096
6.544
2.948
2.596
3.250
3.312
3.053
3.388
1483
3.604
3.767
3.996
4.347
4.965
6.414
2.844
2.487
3.285
1209
3,147
2149
3380
3.501
3663
3.892
4.242
4.857
6.298
2.39.5
2.862
2.756
3,123
1060
3.293
3.199
3.415
3.576
3.804
4.153
4.765
6,200

= degrees of freedom in numerator; v 2 = degrees of freedom in denominator

VA

CONFIDENTIAL

BKB/BKCIBKG/1314111BKF1243

The Periodic Table of the Elements

IA

LuBe

19

13

L 2431
20

21

23

22

24

VIJIB

14

Si

i1

17

Cl

is
Ar
38.95

III

HR

20.98

30.08

34.97

32.07

25.45

20

77

28

29

343

31

32

33

34

35

345

Co

Ni

Cu

Zn

Ga

Ge

As

Se

Br

Kr

72.61

14.92

18.90

78.90

8300

Ca

Sc

Ti

Cr

Mn

Fe

39.10

40.00

44.56

47.61

60.94

52,05

54.44

05.55

55.93

68.69

'82.00

50.39

68.72

41

47

43

44

06

.16

17

49

49

Ag

Cd

Sn
1001

Sb
121.43

Te

30

39

40

Sr

Zr

Nb Mo

(4

58.91

9122

92.91

95.54

(50)

109,1

102,9

'(00.4

107.0

112.4

57

72

73

74

75

75

77

75

79

85

51

92

84

85

55

83

55

Ba
137.3

La
130.4

Hf
178.5

Ta
150.9

Re

Au
197.0

Hg

TI

Bi

2006
.

204.4

Po
(200)

At
(210)

153.5

Pt
195.1

Pb

Cs

59

104

106

(06

Ac

Rf

1Db

55

59

1325

87.62

FrlIRa

RPd

Tc

Ir

160.2

Os
850.2

192.2

107

150

108

Sg

Bh

Hs

Mt

(.0

-51

04

227.2

005.0

877,8

026.5

112
UunUuu Uub
110

Iii

...

--

Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
5409 54

91

('0

(231)

04
Pu'

Pa

Th

20

04

(145)

(244)

9
]

67

mBkf

(043)

(Li

(24 fl

(251)

(252)
s21.0

(257)

258

54

in
114.3

E8547

20.98

05

15

26

VB VIB VflB

IIIB 1V13

Al

1i

99,00

10.81

ri

I Mg

Na
2295

MT

0F

4.003

VA VIA VIIA

WA

lilA

hA
-

(259) [i!

138.3
88

Rn
222)

BKBIBKC/BKG/1314111BKF1243

CONFIDENTIAL

Appendix B

Po
2AZ

R =
WA + WB

hcE=hv==hcv

PT

2[(tR)B(tR)A]
WA+WB
Z

- tR
kA

= -X -

tM
tM
XThLI0

(tR)3-tM
(tR)A tM
(tR)l - ( R)
- (R,
(R)

(t

N=16(t/w)2

-;-

xp_

(R) 1 -

(R)2j

IN

N= L/H

s=1J

j1
Ni

SR -SA+SB

- z
ii= X

/('4)

Fexp

+1

R1,ftA) B)

SA

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