SSC 1293/SSCK1203

RANDOM QUESTIONS FROM PREVIOUS FINAL EXAMS

Topics 1-4
a.

Briefly define the following terms?

i.
Quantitative analysis
ii.
Blank (blank)
iii. Cone and quartering
iv. Accuracy
v.
Random error
vi. Supersaturated solution
vii. Co-precipitation
viii. Digestion

b.

You were given supplement tablets (each weighing 1.00 g) to be analyzed for iron content.
Exactly 0.200 g of a homogenized sample was mixed with concentrated HNO3 and heated for 2
hours in a beaker until the sample dissolves. The solution was then cooled, transferred to a 100
mL volumetric flask and diluted to the mark with distilled water for further analysis.
(i)
Briefly describe the steps you performed to produce the homogenous laboratory
sample prior to dissolution.
(ii) Name the dissolution procedure used.
(iii) If the result of the analysis was 150 ppm, calculate the percent weight (%w/w) of iron in
the sample and in each tablet.
(iv) If the sample matrix interfered in your analysis, suggest two ways to eliminate the
interference.

c.

What is meant by homogenous and representative in sampling process?

d.

A chemist came back from sampling a Pb-containing sample to find the AAS is out of order
and requires three days to be repaired. What should he do to the sample and why? (3 marks)

e.

Describe briefly the fusion and dry ashing technique. What is the difference between these
techniques?

f.

The determination of the concentration of selenium in a standard solution gave the following
values of 10.13, 9.99, 9.95, 10.03, 10.04, 10.03 ppm. Calculate the 95% confidence intervals
for the selenium concentration. If the given standard value is 10.00 ppm, does this indicate a
random error in the measurement?

g.

What is the minimum concentration of PO43- needed to start the precipitation of Ag3PO4 in 0.1
M AgNO3 solution? Ksp Ag3PO4 = 1.3 x 10-20

h.

Nitric acids converts an alloy of silver and copper to silver ions and copper(II) ions. Ag+ is
precipitated as AgCl by adding NaCl to the mixture and washed with nitric acid. Why is nitric
acid used for washing and will the total mass of AgCl affected.

i.

A 2.00 g sample containing iron(III) is dissolved in HCl 6 M and precipitated as Fe(HCO2)3 by

treatment with formic acid. The iron(III) formate so formed is collected and ignited, resulting in
the formation of 0.400 g Fe2O3. Calculate the percent iron in the sample. (Formula mass: Fe2O3
= 159.69, Fe = 55.485).

a.

What are the characteristics of a good analytical chemist?

b.

Define the following terms

a. Quantitative analysis
b. Matrix

c.

What is meant by homogenous and representative in sampling process?

In the determination of Pb content in soil, 5.0 g soil was placed in a 100 mL round bottom
flask. After addition of 20 mL of 6.0 M HNO3, the mixture was refluxed for two hours and
left to cool to room temperature. The mixture was then transferred to a 100 mL volumetric
flask and diluted with distilled water to the mark. For the above procedure, describe how
would you prepare the blank solution for the measurement?

e.

Overflow of pesticides, an organic compound, causes fish kill and pollute the river. You are
sent to investigate and confirm the pesticides and its concentration as the cause of fish kill.
Name the matrix in the study.

i.
ii.

State the sample preparation procedure you would carry out to determine the concentration of
pesticides in the water sample.

iii.

The fish sample was dried at 105oC for two hours, cone and quarter, and digested with heating
using aqua regia to solubilize the sample for the determination of pesticides. State the error(s),
and the correct procedure, IF ANY, of the above sample preparation step.

iv.

A 0.15 g of fish sample was prepared and diluted to 10 mL using the standard procedure, and
analyzed using gas liquid chromatography to give a concentration of 3.2 mg/L pesticides.
Calculate the concentration (ppm) of pesticides in the original fish sample.

f.

Although standard method to determine Hg was employed and statistical test was done on the
data, your lecturer refused to accept your result because of errors in the procedure. Give 3
possible errors that can cause the invalidity of your result?

What is the difference between:

i.
Accuracy and precision
ii.
Determinate and random errors

The zinc content of a vitamin-mineral supplement was measured using a new analytical
method. Five measurements yielded: 15.2, 14.8, 15.5, 15.3 and 14.7 mg Zn per capsule.
Calculate:
i.
The standard deviation
ii
The confidence interval of the mean value at 95% confidence level
iii.
If the actual content of zinc is 15.0 mg per capsule, is there any evidence of
systematic error in the analysis?

a.

Discuss Mohr and Fajans method in precipitation titration method.?

b.

Differentiate beteween direct and indirect EDTA complexometric titration to determine Mg in

water.

c.

Based on the table given, choose and explain your choice of the most suitable indicator used
in the titration of the following acid-base reactions.
Indicator name
Transition pH range
Bromocresol green
3.8 5.4
Bromothymol blue
6.0 7.6
Phenolphthalein
8.0 9.6
i.
ii.
iii.

d.

HCl with NaOH (HCl dengan NaOH)

CH3COOH with NaOH (CH3COOH dengan NaOH)
HCl with NH3 (HCl dengan NH3)
Calculate the pH of titration mixture of 25 mL of NaOH 0.1000 M with 50 mL acetic acid
0.1000 M (Ka CH3COOH = 1.76 x 10-5)

a.
What is von Weimarn ratio and describe how to get a good precipitate by
manipulating this ratio.
b.

Explain the following terms :i. Coprecipitation

ii. Occlusion
iii. Mechanical entrapment

c.

In a gravimetric analysis, an ore (0.6250 g) containing lead was analysed and

precipitated as PbSO4 (0.4264 g). Calculate the percentage of lead in the sample.

a.

Differentiate between the equivalence point and end point. What are their
implications on titration accuracy?.

b.

Explain the basic principle of Mohr, Volhard and Fajan method in precipitation
titration.

c.
i.
ii.

Calculate the pH after the addition of

75 mL and
100 mL of 0.1000 M NaOH
in the titration with 100 mL of 0.1000 M acetic acid. (Ka CH3COOH = 1.76 x 10-5 )

(Topics 5-6)

1.

Complete the table below:

Types of
Stationary phase
chromatography

Mobile Phase

Mechanism of
separation

Gas Liquid
Chromatography
Gas Solid
Chromatography
2.

Why is GC complementary to HPLC?

3.

What is the function of the mobile phase in GC? Give three criteria for the mobile
phase.

4.
i.
ii.

Define the following terms:

Isothermal temperature:
Temperature programming:

5.

Write down the differences between a packed column and a capillary column in the
following table.

Packed column

Capillary column

6.

Write down Beer Lambert Law, indicating what each symbol means.

7.

Why is % transmittance not normally used in measuring absorption compared to

absorbance?

8.

Calculate the molar absorptivity, of a solution of KMnO4 given that the %

transmittance of a solution of 5.5 x 10-5 M KMnO4 is 37.5 % in a 1 cm cell.

9.

Define chromatography.

10.

Give the appropriate chromatographic technique for the following:

Separation based on sieving mechanism: _________________________________
Separation based on ionic interactions: ___________________________________
Separation based on specific interaction between analyte and stationary phase:
__________________________________________

11.

Answer the following questions based on the chromatogram below which was
obtained using high performance liquid chromatography
3.5 min

5.0 min

Detector
response

(a)
(b)
(c)
(d)

(e)

Time/min

What is a chromatogram?
What is the retention time of peak A and peak B?
Which compound is retained longer in then column? Explain your answer
Calculate the resolution between peak A and B given that the width at the base of
peak A is 0.25 min and width at base of peak B is 0.35 min. Comment on your
answer.
Suggest two ways of making the two peaks sharper (i.e how to increase efficiency)

12.

Complete the blanks in the box below

Chromatography
Gas Liquid Chromatography
(GLC)
Thin Layer Chromatography
(TLC)

Stationary Phase

Mobile Phase

a.
i.
ii.
iii.

Briefly define these terms used in chromatography:

tr retention time
N plate efficiency
R Resolution

b.

Calculate the length of column required to resolve two gas chromatography peaks
with retention times of 85 and 100 s, respectively, using a column that has an H value
of 1.5cm/plate. Assume the two peaks have the same band width.

c.

Describe the principle of Size Exclusion Chromatography and what is the exclusion
limit?

d.

Sketch and label the shematic diagram of a High Performance liquid Chromatography
(HPLC)

e.

Predict the order of elution in a separation of a mixture containing 3 subtances which

is A, B and C using normal phase chromatography and reverse phase
chromatography. Given increasing polarity order of the subtances is A > B > C.

a.
i.
ii.
iii.

Define the following terminologies

Resolution (Rs)
Retention time (tr)
Capacity factor (k)

b.
i.
ii.
iii.

State the stationary and moving phase in each type of chromatography below:
thin layer chromatography
liquid chromatography
gas chromatography

c.

Study the GC chromatogram (below) of a mixture of compounds A and B run on a

non-polar column

i.
ii.
iii.
iv.

What are the retention times of compound A and B?

Which compound is present in a larger amount? Explain your answer.
Which compound has the lower boiling point?
What would happen to the retention times of compounds A and B if the column
temperature were raised?
Compound B is suspected to be octane. What can you do to provide supporting
evidence for this hypothesis?

v.

d.

Discuss how resolution can be improved for the two peaks as shown in the
chromatogram below.

e.

Calculate the length of column required to resolve two gas chromatography peaks with
retention times of 85 and 100 s, respectively, using a column that has an H value of
1.5cm/plate. Assume the two peaks have the same band width.

f.

Three compounds, A, B and C, exhibits retention factors on a column having only 500
plates of kA = 1.4, kB = 1.85 and kC = 2.65. Can they be separated with a minimum
resolution of 1.05?

g.

What are he compounds that can be separated by gas chromatography and how does
temperature programming improve separations?
.

h.

Describe the principle of Size Exclusion Chromatography and what is the exclusion
limit?
Answer stationary phase as molecular sieve and has an open network, which
excludes solutes above a certain size. Solutes with formula weight above the limit are
not retained by the column and can be separated from the smaller solutes. Exclusion
limit formula weight that is excluded by the molecular sieve.

a.

Briefly define the following terms

(i)
Chromopores (kromofor)
(ii)
Wavelenght (panjang gelombang)
(iii) Wave number (nombor gelombang)
(iv)
Nebulization (penebulaan)

b.

What kind of transitions are responsible for absorption of ultraviolet radiation

c.

Explain why electrothermal atomizers are more sensitive in atomic absorption

spectrophotometry?

d.
e.

Sketch the schematic diagram of Flame Atomic Absorption Spectrophotometry.

Sketch the schematic diagram of Flame Emission Spectrophotometry.

f.

A drug tolbutamine (FW = 270) has a molar absorptivity of 703 at 262 nm. One tablet
is dissolved in water and diluted to 2L. If the solution exhibits a UV absorption of
0.687 at 262 nm in a 1 cm cell, how many grams of tolbutamine are contained in the
tablet?

a.
b.
c.

State Beer Lamberts Law. What is the significance of this law?

What is the significance of the molar absorptivity, ?
Why is it generally preferable to use absorbance as a measure of absorption rather
than % Transmittance?

d.

A compound of formula weight 280 absorbed 65.0 % of the radiation at a certain

wavelenght in a 2 cm cell at a concentration of 15.0 g mL-1. Calculate its molar
absorptivity.

e.

Draw a schematic diagram of an atomic absorption spectrophotometer (AAS) and

give the function of the components.

f.

Study the energy level diagram given below showing the various kinds of electronic
excitation that may occur in an organic molecule.

Identify the two transitions corresponding to the two lowest energy level differences.

g.

Define:
i
Chromophores absorbing group in molecule.
ii
Wavelength distance one complete cycle.
iii
Wave number number waves in a unit distance.
iv
Nebulization process of sample broken into fine spray due to partial vacuum
at the end of a capillary.

h.

Explain why electrothermal atomizers are more sensitive in atomic absorption

chromatography?