SCHCA032 TEST 1 05082022 Memo1

1.
Below is a single beam UV-vis spectrometer depicted with the different components, why is the
photomultiplier tube a preferred detector for UV-Vis Spectroscopy and how does it carry out its
function (5)
 PMT is a commonly used detector in UV-Vis spectroscopy

 It consists of a photoemissive cathode, several dynodes and an anode.
 A photon of radiation entering the tube strikes the cathode, causing the emission of
several electrons.
 The electrons strike the dynode, causing the emission of several electrons for each
incident electron.
6 7
 Each original photon has produced 10 - 10 electrons.
The resulting current is amplified and measured.
2. The following volumes of 10.0 ppb F- standard solution were added to four 10.00-mL aliquots of
a water sample: 0.00, 1.00, 2.00, and 3.00 mL. Precisely 5.00 mL of a solution containing an
excess of the strongly absorbing A-acid Alizarin Garnet R complex was added to each of the four
solutions, and they were each diluted to 50.0 mL. The intensity of the four solutions were as
follows:
Volume Standard Meter reading
Solution, mL
0 68.2
1 55.3
2 41.3
3 28.8
(i) Calculate the concentration in ppb of F- in the sample and standard deviation of the measured
concentration. (8)
i.
SCHA032 TEST 1 2022

Provide the equation for the least-squares line

y=-13.22x + 68.23
Calculate the concentration of F- in the analyte solution.
Cpd=(-bCs/mVs)=(68.23 x 10)/(-13.22 x 5)
= 10.32 ppm
Find the standard deviation of the measured concentration.
Sc= 0.11 ppm
(ii) Identify factors that cause the Beer’s law relationship to depart from linearity. (4)
3. Why is a double beam spectrophotometer preferred over single beam? (2)

Double beam instrument permits compensation for source power fluctuations greatly improving
S/N and extension to dilute solution samples and measurements with gases
OR
Double beam spectrophotometers operate faster and provide more reproducible
results because they perform an automatic correction for the loss of light intensity as the
beam passes through the sample and reference solution
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4. A solution containing 1.00 mg iron (as the thiocyanate complex) in 100 mL was observed to
transmit 70.0% of the incident light compared to an appropriate blank.
a) What is the absorbance of the solution at this wavelength? (2)
b) What fraction of light would be transmitted by a solution of iron four times more
concentrated than the original solution? (3)
 T = 0.700
 A = -log T
= - log (0.7) = 0.155
 According to Beer’s law, absorbance is linearly related to concentration. If the original

solution has an absorbance of 0.155, a four times more concentrated solution will have
an absorbance:
 A = 4 x 0.155= 0.620
 The transmittance will be:
T = 10-0.620 = 0.240
5. Write short notes about why water should be avoided in IR spectroscopy. (4)
 Water is considered as an active compound in IR spectroscopy due to its non-linear structure,
with 3 degrees of vibrational modes.
 It produces a peak due to its OH group at around 3500 cm-1.
 As a result, equipment should be kept in an oven to remove water moisture.
 The absorption spectra of water in IR will result in erratic results and will interfere with the
chemical of interest.
6. The OH bond has a length of 96pm and an observed dipole moment of 2.36. Calculate the
percent ionic character of this bond and elaborate what is meant by a dipole moment with
examples. (5)
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SCHA032 TEST 1 2022
 µ=Qr
 (1.6x10-19) (96x 10-12)
 µ= (1.536x10-29)(1D/3.34x10-30 C.M)
 µ = 4.6 D
% Ionic = u exp/u ionic
(2.36/4.6)x100
= 51% OH
7. Discuss 3 factors which affect the quantum yield or quantum efficiency of fluorescence or
phosphorescence? (6)
Temperature: increase fluorescence intensity with decreasing T (reduce number of deactivating
collisions).
Solvent: increase fluorescence with increased viscosity (decreased likelihood of external
conversion – radiationless deactivation)
Heavy atoms such as I, Br, Th increases ISC as a consequence φ decreases
f
-pH: Increased resonance structures (protonation or deprotonation)  stable excited state and
greater quantum yield
8. Explain the basic principle of ICP-MS in analytical chemistry and give a block diagram illustrating
its components? (6)
ICPMS is a type of mass spectrometry which is capable of detecting metals and several non-
metals at concentrations as low as one part in 1012 (part per trillion).
This is achieved by ionizing the sample with inductively coupled plasma and then using a mass
spectrometer to separate and quantify those ions.
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SCHA032 TEST 1 2022
9. Give a short explanation of the working principle of a quadrupole analyzer. (5)
 A Quadrupole is a mass analyzer that uses an electric field to separate ions.
 The Quadrupole consists of 4 parallel rods/ poles, √ where adjacent rods have opposite voltage
polarity applied to them.
 The electric force on the ions causes the ions to oscillate/orbit in the area between the 4 rods,
where the radius of the orbit is held constant.
 The ion moves in a very complex motion that is directly proportional to the mass of the ion,
voltage on the quadrupole, and the radio frequency.
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SCHA032 TEST 1 2022
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SCHA032 TEST 1 2022
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3Appendix
Xi yi xi2 yi2 xiyi
0 68.2 0 4651.24 0
1 55.3 1 3058.09 55.3
2 41.3 4 1705.69 82.6
3 28.8 9 829.44 86.4
, , ,
c= 3 x108 cm/s
N=6.023 x 1023 atom/mol
Q= 1.6x10-19
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SCHA032 TEST 1 2022
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1.

 PMT is a commonly used detector in UV-Vis spectroscopy

Provide the equation for the least-squares line

3. Why is a double beam spectrophotometer preferred over single beam? (2)

 According to Beer’s law, absorbance is linearly related to concentration. If the original

 Water is considered as an active compound in IR spectroscopy due to its non-linear structure,

with 3 degrees of vibrational modes.

 It produces a peak due to its OH group at around 3500 cm-1.

 As a result, equipment should be kept in an oven to remove water moisture.

its components? (6)

metals at concentrations as low as one part in 1012 (part per trillion).

spectrometer to separate and quantify those ions.

9. Give a short explanation of the working principle of a quadrupole analyzer. (5)

 A Quadrupole is a mass analyzer that uses an electric field to separate ions.

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