AS/DEC 2019/CHM571
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UNIVERSITI TEKNOLOGI MARA
FINAL EXAMINATION
COURSE BASIC INSTRUMENTAL ANALYSIS
COURSE CODE CHM571
EXAMINATION DECEMBER 2019
TIME 2 HOURS
INSTRUCTIONS TO CANDIDA ttES
1. This question paper consists of six(6) 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 one - page Appendix
iii) an Answer Booklet - provided by the Faculty
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/CHM571
QUESTION 1
a) Briefly define the terms absorbance and transmittance.
(2 marks)
b) Calculate the wavenumber of 3.7 pm wavelength.
(4 marks)
c) State the Beer Lambert's Law and explain one of its deviations.
(4 marks)
d) Distinguish between line source and line spectra.
(4 marks)
QUESTION 2
a) Briefly explain what is a chromophore and the effect of an auxochrome when it is
attached to a chromophore.
(3 marks)
b) Asolution containing 3.94 x 10"5 MKMn04 had a transmittance of 0.195 in a 1.00 cm cell
at 525 nm. Calculate the molarabsorptivity of KMn04 at 525 nm.
(4 marks)
c) Identify which ofthe following molecules absorb or not absorb ultraviolet/visible radiation
Discuss the type of electronic transition that occurs within that molecule.
i) pentane
ii) benzene
(5 marks)
QUESTION 3
a) Explain the rules that must be met to ensure infrared absorption to occur.
(4 marks)
b) Using the absorption bonds in infrared spectra, differentiate between 1-hexene
(CH3(CH2)3CH=CH2) and 1-hexanol (CH3(CH2)3CHCH2OH).
(4 marks)
c) Explain the most common sample preparation method for insoluble solid in infrared
analysis.
(3 marks)
d) List two (2) advantages of Fourier Transform Infrared (FTIR) instrument over dispersive
instrument.
(2 marks)
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QUESTION 4
a) Elaborate the atomization process involve in the conversion of a sample solution to
atomic vapors.
(4 marks)
b) State two (2) types of chemical interferences often encountered in atomic spectroscopy.
Explain how these interferences can be minimized.
(6 marks)
c) One of the advantages of plasma sources in emission spectroscopy is little chemical
interferences (due to ionization problem). Justify how this interference can be minimized
in a plasma source.
K (2 marks)
d) Five milliliters of an unknown solution were pipetted into different 50.0 mL volumetric
flasks. Various volumes of standard containing 50 ppm of calcium (Ca) were added to
the flasks, followed by dilution with deionized water. Given the linear equation obtained
from the calibration graph of absorbance (A) vs volume (mL) for the Ca standard below:
y = 0.5 x + 0.35
Calculate the concentration of Ca in the sample.
(3 marks)
QUESTION 5
a) Define the following terms:
i) Retention time
ii) Resolution
' (2 marks)
b) The following gas chromatography (GC) data was obtained for a mixture separated using
a 50.0 mlong capillary column at a column temperature of 195°C.
Compound Retention time, tR (min) Peak width, W (min)
2.35 0.09
2.46 0.08
Q
Calculate the resolution for compound P and Q and comment if the resolution obtained
will qive a baseline separation.
a (3 marks)
c) Define temperature programming in GC analysis and explain when it is necessary to
employ this program.
(3 marks)
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CONFIDENTIAL 4 AS/DEC 2019/CHM571
d) For each of the following, name the suitable gas chromatography detector which:
i) requires the use of hydrogen gas
ii) is well-suited for pesticide residue analysis
iii) uses a radioactive source
iv) is universally applicable but not very sensitive
(4 marks)
QUESTION 6
a) Differentiate between isocratic and gradient elution in High Performance Liquid
Chromatography (HPLC).
(4 marks)
b) State two (2) criterias for choosing a solvent as a mobile phase in HPLC.
(2 marks)
c) Most HPLC analysis installs a guard column to the analytical column. Explain what is
guard column and the purpose of this installation.
(4 marks)
d) Naphthalene and anthracene are eluted from a reverse phase Cia column with a mobile
phase consisting of 60 % acetonitrile and 40 % water. Predict the order of elution of the
compounds and what will happen to the retention time if the mobile phase is changed to
80 % acetonitrile and 20 % water. Justify your answer.
(4 marks)
END OF QUESTION PAPER
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APPENDIX 1 AS/DEC 2019/CHM571
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SOME CHARACTERISTICS OF IR ABSORPTION BANDS
Wavenumber, cm-1 Intensity Structure
730-770; 690-710 m Mono (aromatic)
1090-1400 C - O (in ethers, alcohols and esters)
1315-1475 m - s C - H (in alkanes)
C = C bond in aromatic ring (usually shows
1450-1600 several peaks)
1620-1680 m C = C
2100-2200 m C = C
1690-1750 C = O (in carbonyl compounds and esters)
1740-1725 C = O (in aldehydes)
1700-1730 C = O (in carboxylic acids)
1320-1210 m C - O (in carboxylic acids)
2760 - 2700
w C - H (of aldehyde group, a pair of bands)
2860 - 2800
2400 - 3400 s, vb O - H in COOH
3000-3100 m C - H (C is part of aromatic ring)
3300 C - H (sp)
3020 - 3080 m C - H (sp2)
2800 - 3000 m - s C - H (sp3)
3200 - 3600 s, b O - H (in H-bonded ROH and ArOH)
Intensities:
s = strong m = medium w = weak b = broad vb = very broad
h = 6.63x10"34J.s
c = 3.00 x 108ms'1
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