Analytical Chemistry Continuous Assessment 1

MCQs: choose the correct answer(s) (2pts)

1) In which chromatography stationary phase is more polar than mobile phase?

A. Ion exchange chromatography
B. Normal phase chromatography
C. Reversed chromatography
D. Size exclusion chromatography
2) In size exclusion chromatography, solute molecules are separated based on
A. Molecular geometry and size
B. Molecular composition
C. Molecular phase
D. Molecular formula
3) Ion exchange chromatography is based on?
A. Electroionic attraction
B. Electrical mobility of ionic species
C. Partition chromatography
D. Ion excitation
4) Column efficiency is measured in terms of number of theoretical plates, which is:
A. Inversely related to square root of height equivalent to theoretical plates
B. Directly related to square root of height equivalent to theoretical plates
C. Directly related to height equivalent to theoretical plates
D. Inversely related to height equivalent to theoretical plates

Q1): Define the following: a) Stationary Phase b) Gradient Elution (2pts)

Q2) List 4 applications of liquid chromatography.(2pts)
Q3) Differentiate between quantitative and qualitative chemistry?(2pts)
Q4) The partition coefficient for a solute in chromatography is K = Cs/Cm, where Cs is the
concentration in the stationary phase and Cm is the concentration in the mobile phase. The larger the
partition coefficient, the longer it takes a solute to be eluted. Explain why. (1pts)
Q5) Solute S has a partition coefficient of 4.0 between water (phase 1) and chloroform (phase 2)
Calculate the concentration of S in chloroform if [S(aq)] is 0.020 M.(1.5pts)
Q6) A chromatography column with a length of 10.3 cm and an inner diameter of 4.61 mm is packed
with a stationary phase that occupies 61.0% of the volume. If the volume flow rate is 1.13 mL/min,
(4pts)
a. find the linear flow rate in cm/min
b. How long does it take for solvent (which is the same as unretained solute) to pass through the
column?
c. Find the retention time for a solute with a retention factor of 10.0.
Q7) In a sample analysis, solvent passes through a column in 3.0 min but solute requires 9.0 min.
(3pts)
a) Calculate the retention factor, k.
b) What fraction of the time is the solute in the mobile phase in the column?
c) The volume of the stationary phase is 1/10 of the volume of the mobile phase of the column
(Vs = 0.10Vm). Find the partition coefficient, K, for this system.
Q8 a) List 2 destructives and 2 non-destructives gas chromatography detectors (2pts)
b) Briefly describe the principle of HPLC (4pts)
 Correction of Analytical Chemistry Continuous Assessment.1

MCQs: choose the correct answer(s) (2pts) 1B, 2A, 3B, 4D

Q-1:(2pts)

a) Stationary Phase: It is the phase through which the mobile phase passes. In most cases, it is a solid
phase or a layer of liquid that has been adsorbed onto the surface of the concrete.

b) Gradient Elution: A chromatographic separation in which the composition of the mobile phase
changes during the run. Typically found in liquid chromatography.

Q2) Answer: The various applications of liquid chromatography are: (2pts)

● Ink samples are tested using liquid chromatography.

● It's used in environmental testing and cleanliness checks.
● It's used in food testing and quality control.
● It is employed in the pharmaceutical and chemical industries.
● It is employed in forensic science as well as hospitals.

Q3) Qualitative analysis does not measure the amount of the substance but measures the quality of that
material whereas quantitative analysis in chemistry gives the absolute or relative quantity regarding
the concentration of one or more substances present in a sample or compound. (2pts)

Q4) Compounds with larger K values will take longer because they spend more time in the stationary
phase

Q5) Solute S has a partition coefficient of 4.0 between water (phase 1) and chloroform (phase 2)
Calculate the concentration of S in chloroform if [S(aq)] is 0.020 M.(1.5pts)

K =[Ss] / [Sm]

K = [S(CHCl3)]/[S(H2O)] [S(CHCl3)]

K·[S(H2O)] = (4.0)(0.020M) = 0.080 M

Therefore [S(CHCL3)] = 0.08M

Q6) Solution:

a) u = (1.13 mL/min)*(1 cm3 /mL)*(1/Aeffective)

where Aeffective is the effective cross-sectional area = π*f*d2 /4
and f = fraction of column made up by mobile phase = (1 – 61.0/100)
Aeffective = π*0.390*(0.461 cm)2 /4 = 0.0651 cm2
u = (1.13 mL/min)*(1 cm3 /mL)/0.0651 cm2 = 17.4 cm/min

b) Time = distance/linear flow rate or

time = volume/flow rate
Time = 10.3 cm/17.4 cm/min = 0.593 min or
time = (10.3 cm)(Aeffective)/1.13 mL/min = 0.593 min
c) k = (tr – tm)/tm = 10.0 = (tr – 0.593)/0.593 tr = 5.93 + 0.59 = 6.53 min
Q7) In a sample analysis, solvent passes through a column in 3.0 min but solute requires 9.0 min.
(3pts)
d) Calculate the retention factor, k.
k=(tr-tm)/tm
k = (9-3)/3 = 2.0
e) What fraction of the time is the solute in the mobile phase in the column?
fraction of time = 3/9 = 0.33
f) The volume of the stationary phase is 1/10 of the volume of the mobile phase of the column
(Vs = 0.10Vm). Find the partition coefficient, K, for this system.
KD = k(Vm/Vs) = 2.0*(10) = 20.

Q8 a) Flame Ionization Detector (distructive); Thermal Conductivity Detector (non-distructive);

Nitrogen-Phosphorus Detector (distructive); Flame Photometric Detector (distructive); Micro-Electron
Capture Detector (non-distructive); Sulfur Chemiluminescence Detector(destructive)

b) The separation principle of HPLC is based on the distribution of the analyte (sample) between a
mobile phase (eluent) and a stationary phase (packing material of the column). Depending on the
chemical structure of the analyte, the molecules are retarded while passing the stationary phase. The
specific intermolecular interactions between the molecules of a sample and the packing material define
their time “on-column”. Hence, different constituents of a sample are eluted at different times.
Thereby, the separation of the sample ingredients is achieved. A detection unit (e.g. UV detector)
recognises the analytes after leaving the column. The signals are converted and recorded by a data
management system (computer software). In general, a HPLC system contains the following modules:
a solvent reservoir, a pump, an injection valve, a column, a detector unit and a data processing unit.
 Analytical Chemistry Continuous Assessment 2

1) Which of the following multicomponent analysis technique involves estimation of components that
show change in spectra in different pH medium?
A. Simultaneous equation
B. Derivative spectroscopy
C. Q Absorbance ratio
D. Difference spectroscopy
2) In mass spectrometry, fragmentation of ions is achieved through?
A. Ionization
B. Splitting
C. Solubilization
D. Coupling
3) In which chromatography stationary phase is more polar than mobile phase?
A. Ion exchange chromatography
B. Normal phase chromatography
C. Reversed chromatography
D. Size exclusion chromatography
4) In a chromatographic separation, which of the following is most appropriate for the qualitative
analysis of a substance?
A. Taking factor
B. Capacity factor
C. Retention time
D. Resolution

Q1) Define: stationary phase, gradient elution.(2pts)

Q2) Differentiate between quantitative and qualitative analysis? (2pts)

Q3) A chromatogram with ideal Gaussian bands has tr = 9.0 min and w1/2 = 2.0 min.(2pts)
a) How many theoretical plates are present?
b) Find the plate height if the column is 10 cm long.
Q4a) Solute S has a partition coefficient of 4.0 between water (phase 1) and chloroform (phase 2)
Calculate the concentration of S in chloroform if [S(aq)] is 0.020 M.(2pts)

b) An open tubular column has a diameter of 207 μm and the thickness of the stationary phase on
the inner wall is 0.50 μm. Unretained solute passes through in 63 s and a particular solute emerges in
433 s. Find the partition coefficient for this solute and find the fraction of time spent in the stationary
phase(5pts)

Q5) list the interferences that are usually encountered in flame photometry (2pts)

Q6) Chromatograms of compounds A and B were obtained at the same flow rate with two columns of
equal length. The value of tm is 1.3m in both cases.( 3pts)
(a) Which column gives a greater relative retention?
(b) Which compound has a higher retention factor?
(c) Which compound has a greater partition coefficient?
(d) What is the numerical value of the retention factor of peak A?
(e) What is the numerical value of the retention factor of peak B?
(f) what is the numerical value of reletive retention
 Correction of Analytical Chemistry Continuous Assessment 2

MCQs (2pts) 1D, 2A, 3B, 4C

Q1) a) Stationary Phase: It is the phase through which the mobile phase passes. In most cases, it is a
solid phase or a layer of liquid that has been adsorbed onto the surface of the concrete.

b) Gradient Elution: A chromatographic separation in which the composition of the mobile phase
changes during the run.Typically found in liquid chromatography

Q2) Qualitative analysis does not measure the amount of the substance but measures the quality of that
material whereas quantitative analysis in chemistry gives the absolute or relative quantity regarding
the concentration of one or more substances present in a sample or compound.

Q3) A chromatogram with ideal Gaussian bands has tr = 9.0 min and w1/2 = 2.0 min.(2pts)
a) How many theoretical plates are present? N = 5.55(9.0 min/2.0 min)2 = 112
b) Find the plate height if the column is 10 cm long. H = 100 mm/112 = 0.89 mm
Q4a) Solute S has a partition coefficient of 4.0 between water (phase 1) and chloroform (phase 2)
Calculate the concentration of S in chloroform if [S(aq)] is 0.020 M.(2pts)

K =[Ss] / [Sm]

K = [S(CHCl3)]/[S(H2O)] [S(CHCl3)]

K·[S(H2O)] = (4.0)(0.020M) = 0.080 M

Therefore [S(CHCL3)] = 0.08M

b) An open tubular column has a diameter of 207 μm and the thickness of the stationary phase on the
inner wall is 0.50 μm. Unretained solute passes through in 63 s and a particular solute emerges in 433
s. Find the partition coefficient for this solute and find the fraction of time spent in the stationary
phase(5pts)

Ans: fraction of time spent in stationary phase = time spent in stationary phase/total time spent fraction
of time spent in stationary phase = (433 – 63 s)/433 s = 0.854 = 85.4%

k = (433 – 63 s)/63 s = 5.873

K = Cs/Cm = k(Vm/Vs)

Vm = Vcylinder = π(d2 /4)L = π[(0.207 mm)2 /4)L = 0.0337 mm2 L

Vs = Vtube = Vouter cylinder – Vinner cylinder = π[(0.207 mm)2 /4]L – π{[(0.207 mm – 2(0.0005 mm)]2
/4}L

Note: for a thin tube, Vtube = πtdL, where t = film thickness. This same equation also can be
calculated from the first equation (Vs = Vtube = Vouter cylinder – Vinner cylinder )

since Vtube = π[(0.207 mm)2 /4]L – π[(0.207 mm)2 /4]L + π(0.207 mm)(0.0005 mm)L – π(0.0005
mm)2 L. The first two terms cancel out and since 0.207 mm >> 0.0005 mm, the last term is
inconsequential.
Vs = Vtube = π(0.207 mm)(0.0005 mm)L = 0.000325 mm2L

K = k(Vm/Vs) = 5.873(0.0337 mm2 L/0.000324 mm2 L) = 609

Q5) list the interferences that are usually encountered in flame photometry (2pts)

 Spectral interference
 Ionised interferences
 Chemical interferences
Q6) We have chromatograms of chemicals A and B that were acquired at the same flow rate and with
two columns of equal length in this work. In both circumstances, the value of tm is the same.
(a) - neither, because in both columns, the retention time and the mobile phase elution time are the
same.
(b) - Compound B, due to the fact that it is eluted later.
(c) - Compound B is eluted later, indicating that it has a longer half-life, hence stronger preference for
the stationary phase
(d)- From the chromatogram, we can see that compound has a retention time of tr=8 mins
k=tr-tm/tm =5.2
(e) - From the chromatogram, we can see that compound B has a retention time of B tr= 10min
k=tr-tm/tm =6.7
(f) alpha=kB/KA = 1.3
 Analytical chemistry Exams(1)

MCQs choose the correct answer

1) Which of the following multicomponent analysis technique involves estimation of components that
show change in spectra in different pH medium
A. Simultaneous equation
B. Derivative spectroscopy
C. Q Absorbance ratio
D. Difference spectroscopy
2) The base peak in mass spectrum is?
A. The lowest mass peak
B. The peak corresponding to the parent ion
C. The highest mass peak
D. The peak set to 100% relative intensity
3) In a chromatographic separation, which of the following is most appropriate for the qualitative
analysis of a substance?
A. Taking factor
B. Capacity factor
C. Retention time
D. Resolution

4) Column efficiency is measured in terms of number of theoretical plates, which is:

A. Inversely related to square root of height equivalent to theoretical plates
B. Inversely related to height equivalent to theoretical plates
B. Directly related to square root of height equivalent to theoretical plates
D. Directly related to height equivalent to theoretical plates

Q1) Define the following: a) Stationary Phase b) Gradient Elution (1pts)

Q2) What is the difference between quantitative and qualitative chemistry? (2pts)

Q3) List 4 limitations of Graphite furnace atomic absorption? (2pts)

Q4) From the spectrum and the IR peak location index:(4pts)

1) Characterize the major peaks.
2) Identify possible functional groups and list them.
3) Identify the structure from the list of possibilities.
4) Write the structure and the name of the molecule.
Q5) Guanosine has a maximum absorbance of 275nm, ϵ275 = 8400M-1 cm-1 and the path length is 1cm.
Using a spectrophotometer, you find that; A275 = 0.70. What is the concentration of guanosine?(2pts)

Q6) There is a substance in a solution (4 g/liter). The length of cuvette is 2 cm and only 50% of the
certain light beam is transmitted. What is the absorption coefficient? (2pts)

Q7) An open tubular column has a diameter of 200 μm and the thickness of the stationary phase on the
inner wall is 0.50 μm. Unretained solute passes through in 53 s and a particular solute emerges in 433
s. Find the partition coefficient for this solute and find the fraction of time spent in the stationary
phase (5pts)
 Analytical chemistry Exams 1 correction

MCQs choose the correct answer.1)D, 2)D, 3) C, 4) B.

Q1) Answer:

a) Stationary Phase: It is the phase through which the mobile phase passes. In most cases, it is a solid
phase or a layer of liquid that has been adsorbed onto the surface of the concrete.

b) Gradient Elution: A chromatographic separation in which the composition of the mobile phase
changes during the run.Typically found in liquid chromatography.

Q2) What is the difference between quantitative and qualitative chemistry? (2pts)

Qualitative analysis does not measure the amount of the substance but measures the quality of that
material whereas quantitative analysis in chemistry gives the absolute or relative quantity regarding
the concentration of one or more substances present in a sample or compound.

Q3) List 4 limitations of Graphite furnace atomic absorption? (2pts)

 Slower analysis time

 Chemical interferences
 Element limitations
 1-6 elements per determination
 No screening ability
 Limited dynamic range

Q4) From the spectrum and the IR peak location index:(4pts)

Answer
-1 -1
1. 3000 cm 1715 cm propanoic acid
strong broad strong narrow
-OH group C=O group
alcohol ketone or aldehyde

Q5) 2pts)
Solution:
To solve this problem, you must use Beer's Law.
A = ϵlc
0.70 = (8400 M-1 cm-1 )(1 cm)( c)
Next, divide both side by (8400 M-1 cm-1 )(1 cm) (1 cm)]
C= 8.33x10-5 mol/L
Q6) (2pts)
Solution Using Beer-Lambert Law, we can compute the absorption coefficient. Thus,

A= -log[ (0.5)/(1)] = 8 ϵ
This implies that A = 8ϵ , Therefore, ϵ=0.0376
Q7) Ans: fraction of time spent in stationary phase = time spent in stationary phase/total time spent
fraction of time spent in stationary phase = (433 – 53 s)/433 s = 0.854 = 87.75%
 k = (433 – 53 s)/53 s = 7.169

K = Cs/Cm = k(Vm/Vs)

Vm = Vcylinder = π(d2 /4)L = π[(0.20 mm)2 /4)L = 0.0337 mm2 L

Vs = Vtube = Vouter cylinder – Vinner cylinder = π[(0.2 mm)2 /4]L – π{[(0.2 mm – 2(0.0005 mm)]2
/4}L

Note: for a thin tube, V tube = πtdL, where t = film thickness. This same equation also can be calculated
from the first equation (Vs = Vtube = Vouter cylinder – Vinner cylinder )

Vs = Vtube = π(0.2 mm)(0.0005 mm)L = 0.000314 mm2L

K = k(Vm/Vs) = 7.169 (0.0337 mm2 L/0.000314 mm2 L) = 769

 Analytical Chemistry Exams(2)

Q1): Define the following: a) Stationary Phase b) Gradient Elution (2pts)

Q2) What is the difference between quantitative and qualitative chemistry? (2pts)

Q3a) Guanosine has a maximum absorbance of 275nm, ϵ275 = 8400M-1 cm-1 and the path length is 1cm.
Using a spectrophotometer, you find that; A275 = 0.70. What is the concentration of guanosine?(2pts)

Q3b) An open tubular column has a diameter of 207 μm and the thickness of the stationary phase on
the inner wall is 0.50 μm. Unretained solute passes through in 63 s and a particular solute emerges in
433 s. Find the partition coefficient for this solute and find the fraction of time spent in the stationary
phase(4pts)

Q4) list the interferences that are usually encountered in flame photometry (1,5pts)

Q5) list the basic components of atomic absorption instrument (2.5)

Q6) From the spectrum and the IR peak location index (3pts)
1) Characterize the major peaks.
2) Identify possible functional groups and list them.
3) Identify the structure from the list of possibilities.
4) Write the structure and the name of the molecule next to the spectrum.

Q7) ) Chromatograms of compounds A and B were obtained at the same flow rate with two columns
of equal length. The value of tm is 1.3m in both cases.( 3pts)

(a) Which column gives a greater relative retention?

(b) Which compound has a higher retention factor?
(c) Which compound has a greater partition coefficient?
(d) What is the numerical value of the retention factor of peak A?
(e) What is the numerical value of the retention factor of peak B?
(f) what is the numerical value of reletive retention
 Correction of Analytical Chemistry Exams(2)

Q1): Define the following: a) Stationary Phase b) Gradient Elution (2pts)

Answer:

a) Stationary Phase: It is the phase through which the mobile phase passes. In most cases, it is a solid
phase or a layer of liquid that has been adsorbed onto the surface of the concrete.

b) Gradient Elution: A chromatographic separation in which the composition of the mobile phase
changes during the run. Typically found in liquid chromatography.

Q2) Differentiate between quantitative and qualitative chemistry? (2pts)

Qualitative analysis does not measure the amount of the substance but measures the quality of
that material whereas quantitative analysis in chemistry gives the absolute or relative quantity
regarding the concentration of one or more substances present in a sample or compound.

Q3a) Guanosine has a maximum absorbance of 275nm, ϵ275 = 8400M-1 cm-1 and the path length is 1cm.
Using a spectrophotometer, you find that; A275 = 0.70. What is the concentration of guanosine?(2pts)

Solution:
To solve this problem, you must use Beer's Law.
A = ϵlc
0.70 = (8400 M-1 cm-1 )(1 cm)( c)
Next, divide both side by (8400 M-1 cm-1 )(1 cm) (1 cm)]
C== 8.33x10-5 mol/L

Q3b) An open tubular column has a diameter of 207 μm and the thickness of the stationary phase on
the inner wall is 0.50 μm. Unretained solute passes through in 63 s and a particular solute emerges in
433 s. Find the partition coefficient for this solute and find the fraction of time spent in the stationary
phase(4pts)

Ans: fraction of time spent in stationary phase = time spent in stationary phase/total time spent fraction
of time spent in stationary phase = (433 – 63 s)/433 s = 0.854 = 85.4%

k = (433 – 63 s)/63 s = 5.873

K = Cs/Cm = k(Vm/Vs)

Vm = Vcylinder = π(d2 /4)L = π[(0.207 mm)2 /4)L = 0.0337 mm2 L

Vs = Vtube = Vouter cylinder – Vinner cylinder = π[(0.207 mm)2 /4]L – π{[(0.207 mm – 2(0.0005 mm)]2
/4}L

Note: for a thin tube, Vtube = πtdL, where t = film thickness. This same equation also can be
calculated from the first equation (Vs = Vtube = Vouter cylinder – Vinner cylinder )

Vs = Vtube = π(0.207 mm)(0.0005 mm)L = 0.000325 mm2L

K = k(Vm/Vs) = 5.873(0.0337 mm2 L/0.000324 mm2 L) = 609 (note how L cancels out so the column
length is not needed).

Q4) list the interferences that are usually encountered in flame photometry (1.5pts)
  Spectral interference
 Ionised interferences
 Chemical interferences
Q5) list the basic components of atomic absorption instrument (2.5)
There are five basic components of an atomic absorption instrument:
1) The light source that emits the spectrum of the element of interest;
2) An "absorption cell" in which atoms of the sample are produced (flame, graphite furnace,
MHS cell, FIAS cell, FIMS cell);
3) A monochromator for light dispersion;
4) A detector, which measures the light intensity and amplifies the signal;
5) A display that shows the reading after it has been processed by the instrument electronics?
Q6) From the spectrum and the IR peak location index :(4pts)
Answer
-1 -1
1. 3000 cm 1715 cm propanoic acid
strong broad strong narrow
-OH group C=O group
alcohol ketone or aldehyde

Q7) solution

We have chromatograms of chemicals A and B that were acquired at the same flow rate and with two
columns of equal length in this work. In both circumstances, the value of tm is the same.

(a) - neither, because in both columns, the retention time and the mobile phase elution time are the
same.

(b) - Compound B, due to the fact that it is eluted later.

(c)? - Compound B is eluted later, indicating that it has a longer half-life, hence stronger preference
for the stationary phase

(d)- From the chromatogram, we can see that compound has a retention time of tr=8 mins

k=tr-tm/tm =5.2

(e) - From the chromatogram, we can see that compound B has a retention time of B tr= 10min

k=tr-tm/tm =6.7

(f) alpha=kB/KA = 1.3