UNIVERSITY OF LIMPOPO

FACULTY OF SCIENCE AND AGRICULTURE

SCHOOL OF PHYSICAL SCIENCES

DEPARTMENT OF CHEMISTRY

DEGREE AND DIPLOMA SUPPLEMENTARY/AEGROTAT EXAMINATION NOV/DEC: 2021

MODULE: SCHA032 PAPER: P

(ANALYTICAL CHEMISTRY 3

TIME: 3 HOURS MARKS: 100

INTERNAL EXAMINER: PROF. KD MODIBANE

DR. NC HINTSHO-MBITA

EXTERNAL EXAMINER: DR FA MELATO

(TUT)

THIS PAPER CONSISTS OF …21…PAGES INCLUDING COVER PAGE

INSTRUCTIONS:

1) (i) ANSWER ALL QUESTIONS

(ii) Click "Submit" to hand-in your work, and NOT the "Enter" button.
(iii) Answer every question as it comes, DO NOT attempt to browse through the questions first.
This examination will save and submit automatically when the time expires.
2) The question paper is a multiple choice questions of 50 questions which accounts for 2 marks each.
3) The questions are randomized and you are not allowed to backtrack
4) The examination will start from 8:30 am till 11:30 pm
5) You have only 2 attempts to completing the examination
6) Data/network issues cannot be used as a means to get an aegrotat, ensure you are in a secured
and network friendly area
 SCHA032 NOV/DEC SUPPLEMENTARY/AEGROTAT EXAMINATION 2021

QUESTION 1

1. Which statement below is not true about UV-vis (ultraviolet visible spectroscopy).
A. The principle technique is based on the spectrum of sample containing an atom or a molecule.
B. The wavelength ranges between 200 – 400 nm.
C. The technique monitors the progress of the compound by utilizing colour change
D. It is a method used to measure how a chemical substance absorb light.
E. All molecules absorb or emit light within the ultraviolet range.

2. Which of the following statements best describes the role of dynodes in Photomultiplier tubes.

A. An electrode in a vacuum tube that serves as an electron multiplier through primary emission.
B. An electrode in a vacumm tube that serves as an electron multiplier through secondary
emission.
C. An electrode in a vacuum that serves as an electron multiplier through secondary emission.
D. An electrode in a vacuum tube that serves as an proton multiplier through secondary emission.
E. An electrode in a vacuum tube that serves as a multiplier through primary emission.

3. It is a known fact that in the electromagnetic spectrum, the strength of the radiation energy will
interact with the molecules in different ways. Which of the following wavelength ranges is associated
with producing vibrations in chemical bonds?
A. 0.8 – 500 µm
B. 400 – 100 nm
C. 380 – 750 nm
D. 700 – 1000 nm
E. 2000 – 500 nm

4. A fluorescent spectroscopy experiment was conducted where students were required to calculate
the Kf for trypthophan in water. The quantum yield was found to be 0.2 and the lifetime was 2.6 ns.
How fast was the excited state decayed away?

A. 7.63x10-6s-1

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B. 7.7x10-4s-1
C. 7.7x10-7s-1
D. 7.4x10-6s-1
E. 7.7x10-5s-1

5. In monochromaters, diffraction grating is mostly preferred over the prism. Which of the following
does not correlate with the above statement?

A. Monochromaters have a single pass and allows a narrow band of wavelengths to be selected.
B. Monochromaters produce a linear dispersion.
C. Monochromaters produce a high resolution.
D. Monochromaters are covered with aluminium so strong, they can be used for a lifetime.
E. Monochromaters are not affected by moisture.

6. Which of the following statements best describe the dual nature of light?
A. In some instances, light behaves as a wave, in other instances it has interferences
B. In some instances, light behaves as a wave, in other instances light behaves as a particle.
C. In some instances, light behaves as a wave which consists of constructive interferences and
destructive interferences.
D. In some instances, light behaves as a particle, and energy is emitted.
E. In some instances, light behaves as a wave and photons are emitted.

7. Which of the following analyzers are mass filters that only allow ions of a certain mass-to-charge
ratio to pass.
A. Mass Analyzer
B. Sectors Analyzers
C. Quadrupole Mass Analyzers
D. Time of Flight Mass Analyzers
E. Digital Analyzers

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2+
8. At 580 nm, the wavelength of a maximum absorption in a 1.00 cm cell, the complex FeSCN has
3 -5
a molar absorptivity of 7.00 x 10 L/cm/mol. Determine the absorbance of a 7.25 x 10 M this
solution.
A. 0.5075
B. B.1.015
C. C.0.3105
D. D.0.5493
E. 0.3108

9. In the Electromagnetic spectrum, several regions with different energies cause various interactions.
In a specific region electronic transitions generally take place. Which region is referred to here and
what kind of coupling can take place.
A. UV-spin-spin coupling.
B. VIS –spin spin coupling.
C. IR- spin orbit coupling.
D. IR- spin spin coupling.
E. UV-VIS spin orbit coupling.

10. Pd(II) and Au(III) complexes can be determined simultaneously by reaction methiomerprazine. The
absorption maximum of Pd complex occurs at 480 nm, while that for the Au complex is at 635 nm.
Molar absorptivity data at theses wavelengths are as follows

Molar absorptivity, e

480 nm 635 nm

Pd complex 3 2
3. 55 x 10 5.64 x 10
Au complex 3 4
2.96 x 10 1.45 x 10
A 25.0 mL sample was treated with an excess of methiomeprazine and subsequently diluted to 50. 0
mL. Calculate the molar concentrations of Pd(II), and Au(III), in the sample if the diluted solution had
an absorbance of 0.533 at 480 nm and 0.590 at 635 nm when measured in a 1.00 cm cell.

A. Au(III) = 7.20 × 105 and Pd(II) = 2.40 × 10-4 M

B. Au(III) = 7.20 × 105 and Pd(II) = 1.20 × 10-4 M

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C. Au(III) = 3.60 × 10-5 and Pd(II) = 2.40 × 10-4 M

D. Au(III) = 3.60 × 105 and Pd(II) = 2.40 × 10-4 M
E. Au(III) = 7.20 × 10-5 and Pd(II) = 3.60 × 10-4 M

11. A solution containing 1.00 mg iron (as the thiocyanate complex) in 100 mL was observed to transmit
65.0% of the incident light compared to an appropriate blank. What fraction of light would be
transmitted by a solution of iron 2 times more concentrated than the original solution?
A. 0.10
B. 0.20
C. 0.31
D. 0.42
E. 0.53

12. Explain why molecular fluorescence often occurs at a longer wavelength than the exciting radiation
A. In fluorescence, an electron is excited to a higher energy state. A high-energy excitation can’t
produce a higher-energy output so fluorescent radiation needs a higher-energy shorter-
wavelength input
B. In fluorescence, an electron is excited to a higher energy state. A low-energy excitation can’t
produce a higher-energy output so fluorescent radiation needs a higher-energy shorter-
wavelength input
C. In fluorescence, stokes shift takes place and an electron gets excited to a higher energy state.
A high-energy excitation can’t produce a higher-energy output so fluorescent radiation needs a
higher-energy shorter-wavelength input
D. In fluorescence, an electron is excited to a higher energy state. A low-energy excitation might
produce a higher-energy output so fluorescent radiation needs a higher-energy shorter-
wavelength input
E. In fluorescence, stokes shift and band gap energy, an electron is excited to a higher energy
state. A high-energy excitation always produces a higher-energy output so fluorescent radiation
needs a higher-energy shorter-wavelength input

14. It is known that atoms in the IR region can vibrate in 6 different directions, which can be grouped
as 3 pairs of modes? Of the stretches below, which one causes a change in angle planes of 2
groups of atoms?
A. Bending
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B. Rocking
C. Twisting
D. Wagging
E. Scissoring

15. 10.0-mL aliquots of a platinum sample solution were transferred to two 50.0-mL volumetric flasks
labelled A and B. 30.0 mL of standard 14.5 μg/mL Pt solution was added to flask B, and each flask
was diluted to the mark with distilled water. The absorbance of the solutions in flasks A and B were
measured by an AAS instrument to be 0.206 and 0.409, respectively. Calculate the concentration
of Pt in the sample solution.
A. 4.40 μg/mL
B. 44.2 μg/mL
C. 2.00 μg/mL
D. 14.7 μg/mL
E. 1.00 μg/mL

16. Every Atomic Spectroscopy instrument has a detection limit for specific elements, of the mentioned
below, which instrument is the most sensitive?
A. FAAS
B. GFAAS
C. FAES
D. ICP-MS
E. ICP-AES

17. 10-mL aliquots of a natural water sample were pipetted into 50.00-mL volumetric flasks. Exactly
0.00, 5.00, 10.00, 15.00 and 20.00 mL of a standard solution containing 11.1 ppm of Fe3+ were
added to each, followed by an excess of thiocyanate ion to give the red complex Fe(SCN)2+. After
dilution to volume, absorbances for the five solutions, measured with a photometer equipped with
a green filter, were found to be 0.240, 0.437, 0.621, 0.809 and 1.009, respectively (.0982-cm cells).
Calculate the standard deviation of the y-intercept.
A. 0.12
B. 1.26 x 10-4
C. 3.07× 10-4

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D. 3.76 × 10-3
E. 2.16 x 10-6

18. 10-mL aliquots of a natural water sample were pipetted into 50.00-mL volumetric flasks. Exactly
0.00, 5.00, 10.00, 15.00 and 20.00 mL of a standard solution containing 11.1 ppm of Fe3+ were
added to each, followed by an excess of thiocyanate ion to give the red complex Fe(SCN)2+. After
dilution to volume, absorbances for the five solutions, measured with a photometer equipped with
a green filter, were found to be 0.240, 0.437, 0.621, 0.809 and 1.009, respectively (.0982-cm cells).
Calculate the standard deviation of the concentration of Fe3+ in mol/L.
A. 0.12
B. 1.26 x 10-4
C. 3.07× 10-4
D. 3.76 × 10-3
E. 2.16 x 10-6

19. 5.00-mL sample of blood was treated with trichloroacetic acid to precipitate proteins. After
centrifugation, the resulting solution was brought to a pH of 3 and was extracted with two 5-mL
portions of methyl isobutyl ketone containing the organic lead complexing agent APCD. The extract
was aspirated directly into an air-acetylene flame yielding an absorbance of 0.502 at 283.3 nm.
Five-milliliter aliquots of standard solutions containing 0.400 and 0.600 ppm of lead were treated in
the same way and yielded absorbances of 0.396 and 0.599. Find the concentration of lead (ppm)
in the sample assuming that Beer's law is followed.
A. 0.5044
B. 5.044 x 10-4
C. 2.424 x 10-6
D. 1.015
E. -0.01

20. Which of the following statements best describes Beers Limitations?

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A. Radiation reaching the sample is of a single wavelenght

B. There is a linear relationship between absorbance and concentration
C. Acid base titrations can be monitered
D. Radiation reaching the sample consists of other miniature wavelenghts
E. Radiation reaching the sample consists of several other miniature wavelenghts and the main
wavelength

21. Which of the following types of chromatography involves the process, where mobile phase moves
through the stationary phase by the influence of gravity or capillary action?
A. Column Chromatography
B. High Pressure Liquid Chromatography
C. Supercritical Fluid Chromatography
D. Gas Chromatography
E. Planar Chromatography

22. In Thin layer chromatography, the stationary phase is made of _________ and the mobile phase
is made of _________
A. Solid, liquid
B. Liquid, liquid
C. Liquid, gas
D. Solid, gas
E. Solid, supercritical fluid

23. A solute has a Kd between water and chloroform of 5.00. Suppose we extract a 50.00-mL sample
of a 0.050 M aqueous solution of the solute using 15.00 mL of chloroform. What volume of
chloroform do we need if we wish to extract 99.9% of the solute?
A. 0.999
B. 9.99
C. 999
D. 0.001
E. 0.0001

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24. Cinnamaldehyde is the component responsible for cinnamon flavour. It is also a potent antimicrobial
compound present in essential oils (see M. Friedman, N. Kozukue, and L. A. Harden, J. Agric. Food
Chem., 2000, 48, 5702, DOI: 10.1021/ jf000585g). The GC response of an artificial mixture
containing six essential oil components and methyl benzoate as an internal standard is shown in
the figure below.

Chromatogram. (From M. Friedman, N. Kozukue, and L.A. Harden, J. Agric. Food Chem.,
2000, 48, 5702. Copyright 2000 American Chemical Society.)
The figure that follows is an idealized enlargement of the region near the cinnamaldehyde peak.
Determine the retention time for cinnamaldehyde.

Enlarged chromatogram.

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A. 19.2 minutes
B. 18.8 minutes
C. 18.6 minutes
D. 19.0 seconds
E. 19.0 minutes

25. Which type of species can be separated by HPLC but not by GC?
A. Mixture compounds
B. Volatile compounds
C. Simple compounds
D. Complex compounds
E. Non-volatile compounds

26. Given the following set of data for experiment of ethanol content determination using GC-FID:

Concentration, Ethanol n-propanol (8%)

%
Peak area Peak height Peak area Peak height

2.00 1722382 709069 5213719 4385597

3.00 3576879 1727233 7820820 6362669

6.00 6227217 2844402 6644106 5569003

9.00 8544284 3647759 6359744 5076839

35.00 31296672 10344985 6066515 3042734

Unknown 5059899.5 3252624 10506015 3954938

Using peak heights, determine the unknown percentage of ethanol if equal volumes of 8% n-
propanol internal standard were added to both standards solutions and the sample prior analysis.

A. 4.58
B. 10.0
C. 3.57
D. 6.00
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E. 9.00

27. If the distribution constant, Kd, for I2 between chloroform and water is 87. What fraction of I2 initially
present in 50 mL of water is expected to partition into the organic phase after a single extraction
with 50 mL of chloroform when initial concentration is 750 M?

A. 0.99
B. 9.9
C. 0.50
D. 1.00
E. 0.75

28. Given the following set of data for experiment of ethanol content determination using GC-FID:

Concentration, Ethanol n-propanol (8%)

%
Peak area Peak height Peak area Peak height

2.00 1722382 709069 5213719 4385597

3.00 3576879 1727233 7820820 6362669

6.00 6227217 2844402 6644106 5569003

9.00 8544284 3647759 6359744 5076839

35.00 31296672 10344985 6066515 3042734

Unknown 5059899.5 3252624 10506015 3954938

Using peak areas, determine the unknown percentage of ethanol if equal volumes of 8% n-propanol
internal standard were added to both standards solutions and the sample prior analysis.

A. 4.58
B. 10.0
C. 3.57
D. 6.00
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E. 9.00

29. Peak positions, heights, and widths for four components separated isocratically using a 10 cm
reverse phase column and a flow rate of 0.2 cm/s. Detection was via UV-vis absorption.

Assuming equal molar absorptivities, which of the analytes is of highest concentration in the
sample?
A. D
B. B
C. C
D. A
E. insufficient information provided

30. If the distribution constant, Kd, for I2 between chloroform and water is 87. What aqueous
concentration of I- should be used to remove roughly 99% of the I2 initially present in 50 mL of
chloroform using 5 extractions with 50 mL volumes of water when initial concentration is 750 M?

A. 0.075 M
B. 0.298 m
C. 0.174 M
D. 1.74 M
E. 0.274 M

31. Which of the following statements is accurate?

A. Capillary column GC generally has higher efficiencies than HPLC because of a lower plate
height in GC
B. HPLC has higher efficiencies than capillary column GC because the column length is longer
C. Gradient elution is an important approach in capillary GC to deal with the general elution problem

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D. Capillary column GC generally has higher efficiencies than HPLC because of a much greater
column length in GC
E. Mobile phase composition is an important experimental variable in both GC and LC

32. What does the retention factor, k', describe?

A. The distribution of an analyte between the stationary and the mobile phase
B. The migration rate of an analyte through a column
C. The velocity of the mobile phase
D. The distribution of an analyte on the stationary phase
E. The distribution of an analyte on the mobile phase

33. Peak positions, heights, and widths for four components separated isocratically using a 10 cm
reverse phase column and a flow rate of 0.2 cm/s. Detection was via UV-vis absorption.

Assuming a plate height of 0.014 cm, at what distance along the column was component B
separated from component A with a resolution of 1.5?

A. 10.0 cm
B. 6.1 cm
C. 8.2 cm
D. 4.3cm
E. insufficient information provided.

34. Peak positions, heights, and widths for four components separated isocratically using a 10 cm
reverse phase column and a flow rate of 0.2 cm/s. Detection was via UV-vis absorption.

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How much time did component C spend in the mobile phase?

A. 94 s
B. 147 s
C. 53 s
D. 7 s
E. insufficient information is provided.

35. A good reason to increase flow rate in chromatography is

A. to minimize band broadening due to mobile phase mass transport.

B. to minimize band broadening due to mass transport in the stationary phase.

C. to minimize eddy diffusion.

D. to minimize column bleed.

E. to minimize band broadening due to longitudinal diffusion.

36. A solute has a Kd between water and chloroform of 5.00. Suppose we extract a 50.00-mL sample
of a 0.050 M aqueous solution of the solute using 15.00 mL of chloroform. Determine the extraction
efficiency for two identical extractions.
A. 100%
B. 99.9%
C. 93.6%
D. 84.0%
E. 50%

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37. A solute has a Kd between water and chloroform of 5.00. Suppose we extract a 50.00-mL sample
of a 0.050 M aqueous solution of the solute using 15.00 mL of chloroform. Determine the extraction
efficiency for three identical extractions and for three identical extractions
A. 100%
B. 99.9%
C. 93.6%
D. 84.0%
E. 50%

38. What is the main difference between HPLC and UPLC?

A. HPLC is reverse-phase whereas UPLC is normal-phase
B. UPLC employs smaller stationary-phase particle size
C. HPLC and UPLC employ different mobile phases
D. HPLC and UPLC employ different detection methods
E. HPLC operates at higher mobile phase pressures

39. Which of the following statements is accurate?

A. Capillary column GC generally has higher efficiencies tha HPLC because of a lower plate height
in GC
B. HPLC has higher efficiencies than capillary column GC because the column length is longer
C. Gradient elution is an important approach in capillary GC to deal with the general elution problem
D. Capillary column GC generally has higher efficiencies than HPLC because of a much greater
column length in GC
E. Mobile phase composition is an important experimental variable in both GC and LC

40. Which of the following properties is not used as a basis for physical separation of analyte
species in analytical chemistry?

A. mass
B. polarity
C. molar absorptivity
D. physical state
E. size
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41. If 612C of charge is passed through a solution of CuSO4 during an electrolysis experiment, what is
the number of moles of copper metal deposited at the cathode?
A. 0.00790 moles
B. 0.000790 moles
C. 0.00158 moles
D. 0.00316 moles
E. 0.001580 moles

42. Which of the following factors are considered as electrode variable?

A. Material used
B. Surface area and geometry surface condition
C. Material used, surface area and geometry surface condition
D. Surface area
E. Material used and geometry surface condition

43. Below is a series of interfacial steps (not in order) that takes place when redox reaction for the given
general reaction, thus 𝑂 + 𝑛𝑒 − ↔ 𝑅
I. Charge transfer occur between the electrode and 𝑂 and 𝑅 is formed.
II. 𝑅 must be transported away from the electrode surface back into the bulk solution
III. 𝑂 must be successfully transported from the bulk solution to the electrode surface
IV. 𝑅 must be desorbed from the electrode surface
V. 𝑂 must adsorb transiently onto electrode surface
Which of those step/s is/are nonfaradaic process/es
A. II
B. IV and V
C. I
D. II and III
E. I and IV

44. Species gaining electrons will be reduced and act as

A. reducing agent
B. oxidizing agent

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C. neutralizing agent
D. reagent
E. redox agent

45. An electrochemical cell consists of two copper electrodes dipping into aqueous CuSO4 solution; the
electrodes are connected to a battery. Which statement about the electrolysis process in this cell is
incorrect?
A. Cu2+ ions are produced at the anode.
B. Copper is deposited on the cathode.
C. Reduction occurs at the anode.
D. Copper in transferred from anode to cathode.
E. Electrons transferred from anode to cathode

46. The exchange current density for the evolution of hydrogen platinum is 8.00 A/m2. What is the
current density at 298 K for an overpotential of 2 mV?
A. -75.8 A/m2
B. -8.74 A/m2
C. 2.07 A/m2
D. 15.9 A/m2
E. 8.74 A/m2

47. Below is a series of interfacial steps (not in order) that takes place when redox reaction for the given
general reaction, thus 𝑂 + 𝑛𝑒 − ↔ 𝑅
I. Charge transfer occur between the electrode and 𝑂 and 𝑅 is formed.
II. 𝑅 must be transported away from the electrode surface back into the bulk solution
III. 𝑂 must be successfully transported from the bulk solution to the electrode surface
IV. 𝑅 must be desorbed from the electrode surface
V. 𝑂 must adsorb transiently onto electrode surface
The correct sequence for those steps is
A. I, II, III, IV and V
B. I, III, V, IV and II
C. III, V, I, IV and II
D. III, V, IV, I and II

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E. III, I, V, IV and II

48. Below is a series of interfacial steps (not in order) that takes place when redox reaction for the given
general reaction, thus 𝑂 + 𝑛𝑒 − ↔ 𝑅
I. Charge transfer occur between the electrode and 𝑂 and 𝑅 is formed.
II. 𝑅 must be transported away from the electrode surface back into the bulk solution
III. 𝑂 must be successfully transported from the bulk solution to the electrode surface
IV. 𝑅 must be desorbed from the electrode surface
V. 𝑂 must adsorb transiently onto electrode surface

Which of those step/s is/are faradaic process/es

A. II
B. IV and V
C. I
D. I and III
E. I and IV
49. The concentration of As(III) in water can be determined by differential pulse polarography in 1 M
HCl. The initial potential is set to –0.1 V versus the SCE and is scanned toward more negative
potentials at a rate of 5 mV/s. Reduction of As(III) to As(0) occurs at a potential of approximately –
0.44 V versus the SCE. The peak currents for a set of standard solutions, which are corrected for
the residual current, are shown in the following table.

[As (III)] (M) ip (µA)

1.00 0.298
3.00 0.947
6.00 1.83
9.00 2.72

The concentration of As(III) in a sample of water if its peak current is 1.37 μA is

A. 0.449 M
B. 4490 M
C. 4.490 M
D. 4.49 M
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E. 4.49 x 10-6 M

50. A 25.0‑mL sample of Ni2+ gave a wave height of 2.36 µA (corrected for residual current) in a
polarographic analysis. When 1.00 mL of solution containing 28.7 mM Ni2+ was added, the wave
height increased to 3.79 µA. Find the concentration of Ni2+ in the unknown.
A. 0.900 mM
B. 1.71 mM
C. 0.450 mM
D. 17.2 mM
E. 9.00 mM

[50 X 2 = 100]

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Appendix

Xi yi xi2 yi2 xiyi

0 0.209 0 0.043681 0
5 0.329 25 0.108241 1.645
10 0.455 100 0.207025 4.55
15 0.581 225 0.337561 8.715
20 0.707 400 0.499849 14.14
25 0.833 625 0.693889 20.825
Sum 75 3.114 1375 1.890246 49.875

, , ,
c= 3 x108 cm/s
N=6.023 x 1023 atom/mol

A=ebc
[A]i = (Vaq/(VorgK + Vaq))i[A]0
N=eV/2D
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 = L / tR
u = L / tM
k=(tR-tm)/tm
Rs= 2(tRB-tRA)/(WB+WA)
N=16(tR/W)2
N= L/H
 = k B / kA
i = i0nF/RT
zF
ln i  ln i0  
RT
ip = 2.69 x 105 n3/2A D½ ½ C0
F = 96500 C mol-1
R = 8.314 J mol-1 K-1

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