CONFIDENTIAL AS/DEC 2019/CHM421

UNIVERSITI TEKNOLOGI MARA

FINAL EXAMINATION

COURSE ANALYTICAL CHEMISTRY

COURSE CODE CHM421

EXAMINATION DECEMBER 2019

TIME 2 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.

3. 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) the Question Paper

ii) a two - page Appendix
iii) an Answer Booklet - provided by the Faculty

5. Answer ALL questions in English.

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

This examination paper consists of 4 printed pages
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 CONFIDENTIAL 2 AS/DEC 2019/CHM421

QUESTION 1

a) Describe the term "quantitative analysis".

(2 marks)

b) The specific gravity of concentrated sulfuric acid is 1.354 and the density of water at 40 °C
is 0.9922 g/mL

i) Calculate the density of sulfuric acid in four significant figures.

(2 marks)

ii) The molarity of concentrated sulfuric acid solution is 18.4 M. Describe the preparation
of a 250 cm3 solution of 1.8 N from the concentrated sulfuric acid.
(4 marks)

c) Calculate the mass of solid calcium nitrate, (Ca(NOs)2) required to prepare 1.0 L of 20 ppm
nitrate (NO3") solution.
(4 marks)

d) Outline weighing by difference technique.

(3 marks)

e) Describe the preparation of aqua-regia cleaning solution.

(2 marks)

f) Differentiate between volumetric pipette and graduated pipette and identify the pipette as
either TC or TD.
(3 marks)

QUESTION 2

a) The result of an analysis of a compound is 78.04 g. Determine the relative error in parts
per million if the accepted value is 77.95 g.
(2 marks)

b) Compare between representative samples and replicate samples.

(2 marks)

c) List three ways to overcome interference in samples.

(3 marks)

d) Indicate the terms used in statistics to analyse the following terms:

i) Precision
(1 mark)

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 CONFIDENTIAL 3 AS/DEC 2019/CHM421

ii) Accuracy
(1 mark)

e) Potassium ion (K+) is added to fertilizers as itaids the synthesis of carbohydrates in plants
and affects sweetness of fruits. However, in high salinity environment, the K+ uptake is
reduced and may decrease the growth of plant. Maintenance of high cytoplasmic levels of
K+ is essential for survival of plants in saline habitats.

Four replicates of root of a plant were determined using an established method. The
concentrations of K+ (mmol/L) are 1062, 1310, 1356, 1270.

i) By using a Q-test at 90% confidence level (CL), decide if any ofthe data in rootsample
should be rejected or retained.
(3 marks)

ii) Calculate the 90% confidence interval for the mean value of K+ in root sample.

(4 marks)

Another four replicates taken from the shoot of the same plant was analysed and the
results are as follows: 650, 678, 690, 632 mmol/L. The true value for the shoot was
716 mmol/L.

iii) Apply a suitable statistical test to analyse whether the difference in the value of K+ in
the plants' shoot from the true value, is due to random or systematic error at 95% CL.

(5 marks)

QUESTION 3

a) i) Differentiate between direct titration and back titration in terms of concepts and
applications.
(4 marks)

ii) Give a reason why back titration is necessary to use in titration.

(1 mark)

iii) A 10 mL ethyl acetate (CH3COOC2H5) was diluted to 100 mL. A volume of 20.0 mL of
this diluted solution was refluxed with 45.00 mL of 0.0250 M KOH solution. The
reaction is as follows:

CH3COOC2H5 + OH" <-» CH3COO- + C2H5OH

After cooling, the excess OH- was back titrated with 3.50 mL of 0.050 M H2S04
solution. Calculate the weight of ethyl acetate in the initial sample.
(6 marks)

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 CONFIDENTIAL 4 AS/DEC 2019/CHM421

b) i) Give the full name of EDTA.

(1 mark)

ii) A zinc supplement tablet containing about 10 mg of zinc ion was added to water and
titrated with 0.01 M EDTA solution. The volume of EDTA solution used was 14.65 mL.
Calculate the actual zinc content of the tablet (in mg). Give your comment on the results
obtained.
(4 marks)

c) i) There are three methods used for determining end point in precipitation titration.
Differentiate between any two of the methods.
(4 marks)

ii) A 3.963 g sample of an alloy is dissolved in HN03 and is diluted to 250 mL. Titrating a
25.00 mL portion of the diluted sample with 0.1078 M KSCN require 27.19 mL to reach
the end point. Calculate the % w/w Ag in the alloy.
(4 marks)

QUESTION 4

a) Point out the steps of a gravimetric analysis.

(4 marks)

b) A copper ore was analysed by dissolving a 1.500 g sample in concentrated phosphoric

acid. The resulting solution was diluted with water and the copper(ll) was precipitated as
Cu3(P04)2.xH20. After filtration and washing, the residue was ignited at high temperature
to give 0.850 g of pure Cu3(P04)2(FW: 380.58 g/mol). Calculate the % of Cu in the sample.

(3 marks)

c) Describe volatilization method in gravimetric analysis. Propose one analysis of

volatilization method.
(2 marks)

QUESTION 5

a) Discuss the function of stationary and mobile phase in planar chromatography.

(2 marks)

b) The separation of a mixture of three compounds (X: less polar; Y: non-polar; Z: polar) was
purified using column chromatography. Elaborate on the elution order of the compound if
separation is done on a reverse phase column chromatography.
(4 marks)

END OF QUESTION PAPER

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Periodic Table of the Elements

IA 1>niA

1 2

H VII He
3
O 1.008 IIA UIA iva VA VTA 4.003
A
o
to. 3 4 Atomic Number 5 6 7 8 9 10
Li Be Symbol of Element B C N O F Ne
% 6.940 9.013 Relative Atomic Mass 10.82 12.01 14.01 16.00 19.00 20.18
11 12 13 14 15 16 17 18
Na Mg vniE Al Si P s CI Ar
22.99 24.32 IIIB IVB VB VIB VIIB *~ IB II B 26.98 28.09 30.98 32.07 35.46 39.94
19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36
>
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr TJ
39.10 40.08 44.96 47.90 50.95 52.01 54.94 55.85 58.94 58.71 63.54 65.38 69.72 72.60 74.91 78.96 79.92 83.80 TJ
m
37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 z
D
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
X
85.48 87.63 88.92 91.22 92.91 95.95 (99) 101.1 102.9 106.4 107.9 112.4 114.8 118.7 121.9 127.6 126.9 131.3
55 56 57 72 73 74 75 76 77 78 79 80 81 82 83 84 85 86
Cs Ba *La Hf Ta w Re Os lr Pt Au Hg TI Pb Bi Po At Rn
132.9 137.4 138.9 178.5 180.9 183.9 186.2 190.2 192.2 195.1 197.0 200.6 204.4 207.2 209.0 (210) (210) (222)
87 88 89 104 105 106 107 108 109 111 112 114
Fr Ra **Ac Rf Db sg Bh Hs Mt Uun Uuu Uub Uuq
(223) (226) (227) (261) (262) (263) (264) (265) (268) (269) (272) (277) (285)

58 59 60 61 62 63 64 65 66 67 68 69 70 71
Lanthanides Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
140.1 140.9 144.3 150.4 152.0 157.3 158.9 162.5 164.9 173.0 >
(147) 167.3 168.9 175.0 c/>
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90 91 92 93 94 95 96 97 98 99 100 101 102 103 m
o O
o ** Actinides Th Pa u Np Pu Am Cm Bk Cf Es Fm Md No Lw ro
(232) (231) 238.1 (237) (242) (243) (247) (249) (251) (254) (253) (256) (253) (257) o
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CONFIDENTIAL APPEIMDIX2 AS/DEC 2

TABLE 1 Values of t for Various Level of Probability

Degrees of Factor for Confidence Interval

Freedom 80% 90% 95% 99% 99.9%

1 3.08 6.31 12.7 63.7 637

2 1.89 2.92 4.30 9.92 31.6
3 1.64 2.35 3.18 5.84 12.9
4 1.53 2.13 2.78 4.60 8.61
5 1.48 2.02 2.57 4.03 6.87
6 1.44 1.94 2.45 3.71 5.96
7 1.42 1.90 2.36 3.50 5.41
8 1.40 1.86 2.31 3.36 5.04
9 1.38 1.83 2.26 3.25 4.78
10 1.37 1.81 2.23 3.17 4.59
OO
1.28 1.64 1.96 2.58 3.29

TABLE 2 Critical Values for F at 95% confidence level

Degrees of freedom (Numerator)

Degrees of freedom
(Denominator) 2 3 4 5 6 12

2 19.00 19.16 19.25 19.30 19.33 19.41

3 9.55 9.28 9.12 9.01 8.94 8.74
4 6.94 6.59 6.39 6.26 6.16 5.91
5 5.79 5.41 5.19 5.05 4.95 4.68
6 5.14 4.76 4.53 4.39 4.28 4.00
12 3.89 3.49 3.26 3.11 3.00 2.69

TABLE 3 Critical Values for the Rejection Quotient Q

Qcrit
Number of
Observations 90% Confidence 95% Confidence 99% Confidence

3 0.941 0.970 0.994

4 0.765 0.829 0.926
5 0.642 0.710 0.821
6 0.560 0.625 0.740
7 0.507 0.568 0.680
8 0.468 0.526 0.634
9 0.437 0.493 0.598
10 0.412 0.466 0.568

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