Professional Documents
Culture Documents
CHEMISTRY
PRACTICALS
2010 - 2011
Table of Contents
Page
Title
Module Skills tested
#
3
Standardisation of sodium hydroxide
2
5
Calibration of a pipette
2
ORR, A&I
6
Redox Titration / H2O2 vs KMnO4
2
M&M
8
Back Titration
2
10
Gravimetric analysis of hydrated salt
2
11
Flame tests
2
12
Reactions of ethanol
1
ORR,A&I
13
Paper Chromatography
2
14 Theoretical: Functional groups in organic compounds
1
15
Water polluting inorganic ions
3
16
Distillation of a sample of rum
3
17
Salted peanuts Fuller
2
P&D
18
Identity of sample X
3
M&M, A&I
19
Comparing simple and fractional distillation
2
20
Margarine vs Butter
1
P&D
page 3 of 20
Trial
page 4 of 20
2
Initial
Volume used/cm3
average titre/cm3
Treatment of results:
1. Write a balanced equation for the reaction between sodium carbonate and hydrochloric acid.
page 5 of 20
CALIBRATION OF A PIPETTE
26
28
30
32
34
36
page 6 of 20
REDOX TITRATION
Introduction
Your task is to use 0.020 moldm-3 potassium manganate (VII) solution to find the actual concentration of a
solution of hydrogen peroxide, H2O2, which is believed to have partially decomposed.
Procedure
a)
Prepare 250 cm3 of a solution of hydrogen peroxide by adding 7.5 cm3 of the stock solution
supplied to the volumetric flask and diluting to the required volume.
b)
c)
d)
Titrate the mixture against the potassium manganate (VII) until a permanent pale pink colour
appears in the conical flask.
e)
Record the titre volume and repeat until concordant values are obtained.
f)
Do not write a full lab report, write your results in the table below and answer the questions that
follow.
Results
Burette
Reading/cm3
(to 2 decimal
places)
Final
Trial
Initial
Volume
used/cm3
average
titre/cm3
page 7 of 20
Questions
1. Write the relevant half equations for
i) the reduction of MnO4- ions to Mn2+ in acidic solution
ii) the oxidation of H2O2 to O2 in acidic solution
2. Using the two half equations from question 1, write the full balanced ionic equation.
3. If the stock solution of hydrogen peroxide had a molar concentration of 1.67 mol dm-3, determine the
molar concentration of the hydrogen peroxide solution prepared by you.
4. Determine the molar concentration of the hydrogen peroxide solution prepared by you using your
titration results.
5. Determine the error in your results.
6. Suggest a reason for the partial decomposition of the hydrogen peroxide.
page 8 of 20
To determine the percentages of calcium carbonate and calcium chloride in a mixture of the two.
THEORY:
Sometimes a direct titration would involve a reaction which is too slow and thus an incomplete reaction would
occur, therefore a back titration is more suitable. In a back titration, a known excess of the reagent is used to
ensure complete reaction and then a second reagent is titrated against the mixture which reacts with the
remaining reagent which allows via calculation, the amount of the reagent that was used in the initial reaction.
PROCEDURE:
1. Weigh 1.5 g of the solid mixture of calcium carbonate and calcium chloride and place in a conical flask.
2. Measure 25 cm3 of the 1 mol dm-3 HCl solution and place in the conical flask.
3. Rinse and fill the burette with 0.2 mol dm-3 NaOH solution.
4. Once all effervescence in the conical flask has ceased, add 2 drops of phenolphthalein indicator to the flask
and swirl the flask.
5. Titrate the sodium hydroxide against the reaction mixture until the first permanent pale pink colour is seen.
6. Repeat steps 1-5 until consistent results are obtained. (In the interest of time and materials, please try to
be as accurate as possible to minimise the number of trials)
7. Do not write a full lab report. Record your readings in the table below and answer the questions that follow.
RESULTS
Burette
Reading/cm3
(to 2 decimal
places)
Final
Trial
Initial
Volume
used/cm3
Average volume (please tick the values used to determine your average)
page 9 of 20
TREATMENT OF RESULTS
1.
2.
Using the average volume of NaOH used, calculate the # of mol of NaOH used in the titration.
3.
Write the balanced equation for the reaction between HCl and NaOH and thus determine the # of
mol of HCl remaining after the initial reaction in the conical flask was complete.
4.
Write a balanced chemical equation for the reaction between calcium carbonate and HCl.
5.
Using your answers from question 1 and question 3, determine the # of mol of HCl that reacted with
the calcium carbonate.
6.
Determine
a) the # of mol of CaCO3
b) the mass of CaCO3 present in the mixture
7.
Hence calculate the percentages of CaCO3 and CaCl2 present in the solid mixture.
page 10 of 20
page 11 of 20
MODULE 2
TITLE:
FLAME TESTS
INTRODUCTION:
Many cations of s and d-block elements may be identified by a flame test. The energy from the burning gas
causes promotion of electrons in the ions to higher energy levels. The excited ions then lose energy and
undergo electronic transition to a lower energy level, giving off the extra energy in the form of electromagnetic
radiation. The frequency of this radiation usually falls in the visible region of the spectrum, so a coloured flame
is observed.
PROCEDURE:
1. Clean a nichrome or platinum wire by dipping it in concentrated hydrochloric acid and placing it in a
non-luminous Bunsen flame.
2. Continue this cleaning process until no colour at all is produced when the wire is in the flame.
3. Moisten the wire with concentrated hydrochloric acid, dip it in the sample, and hold it in the flame
again.
4. Record the colour observed.
5. Carry out a flame test on each of the other samples supplied.
6. Record your results in the table below.
7. Do not write a full lab report.
Results
Metal
ion
Colour
Treatment of results:
1. Why are different colours observed?
2.
(a) Identify any ion or ions for which there was no colour imparted to the flame.
(b) Suggest an explanation for this.
3. Why is the cleaning of the nichrome wire necessary before performing a flame test?
page 12 of 20
MODULE 1
TITLE:
REACTIONS OF ETHANOL
To 5 drops of ethanol in a test tube, add 2 drops of potassium dichromate (VI) then 10 drops
of dilute sulphuric acid. Leave to stand in a beaker of hot water (water bath) for 10 minutes.
Carefully smell the product.
2.
Repeat test 1 using potassium manganate (VII) in place of potassium dichromate (VI)
3.
Pour 2 cm3 of ethanol and 1cm3 of glacial ethanoic acid into a test tube. Carefully add 2-3
drops of concentrated sulphuric acid. Warm gently for a few minutes in a water bath. DO
NOT BOIL. Pour the product carefully into a beaker containing sodium carbonate solution.
Stir and smell carefully.
4.
To 1cm3 of ethanol add concentrated sulphuric acid (carefully) and bubble the gas evolved
into an acidified solution of potassium manganate (VII).
5.
Write a full lab report. Use a tabular form to express the results of the practical.
TREATMENT OF RESULTS:
1. For each test: a) Name the type of chemical reaction b) Give the name and fully displayed formula of
the most likely organic product.
2. Describe a simple chemical test that may be used to distinguish between the organic products formed in
tests 1 and 2.
3. Write a chemical equation for the production of the gas in test 4, and for its reaction with potassium
manganate (VII)
4. Which of the tests is/are typical of all alcohols. Justify your choice.
page 13 of 20
PAPER CHROMATOGRAPHY
page 14 of 20
MODULE 1
TITLE:
INTRODUCTION:
Combined with other methods of analysis, qualitative tests for the presence of specific functional groups aid in
the identification of organic compounds. Use your knowledge of functional group reactions to complete the
table shown below.
COMPOUND TEST
A
OBSERVATION
Bromine in 1,1,1-trichloroethane
Decolourisation
PCl5
I2 in NaOH
STRUCTURAL FORMULA
OF FUNCTIONAL GROUP
B
Yellow ppt
C
Litmus test
Blue to red
Ense white fumes
PCl5
D
Litmus test
Blue to red
Br2(aq)
White ppt
QUESTION:
Compound B is a fragrant liquid which when heated with excess concentrated H2SO4 produces a gas, G, which
decolourises aqueous bromine. When G reacts with HBr, two isomeric compounds, E and F, with relative
molecular mass of 123 are obtained. Write the displayed formula for EACH of the following.
E
page 15 of 20
INTRODUCTION:
Nitrate (V), Phosphate (V), cyanide, and Lead (II) ions may be found in contaminated water. The typical
reactions of the NO3 - , PO4 3- , and Pb2+ ions will be carried out in this practical. CN- ions are highly poisonous
and will be considered theoretically.
PROCEDURE:
Carry out the following tests. Record all observations and inferences in Tabular form.
1. Nitrate (V) anions:
(a) Add Devardas alloy followed by sodium hydroxide. Warm mixture and test gas evolved.
(b) Mix with iron (II) sulphate crystals, Pour concentrated sulphuric acid slowly down the side of the tube,
so that two layers of liquid are formed.
(c) Add some copper turnings then add concentrated sulphuric acid. [ TEACHER DEMONSTRATION]
2.Phosphate (V) anions
(a) Add aqueous silver nitrate. Test solubility of ppt separately in (i) dil. HNO3 (aq) (ii)NH3 (aq) and
discard product immediately!
(b) Add aqueous barium chloride. Divide ppt into three portions and test its solubility in (i) dil nitric acid,
(ii) dil ethanoic acid, (iii) dil aqueous ammonia.
(c) Add an equal volume of ammonium molybdate. Warm gently to accelerate formation of ppt.
(d) Add aqueous iron (III) chloride. Test solubility of ppt in (i) dilute nitic acid, (ii) dilute ethanoic acid.
3. Lead (II) cations
(a) Add aqueous sodium hydroxide until in excess
(b) Add dilute hydrochloric acid. Heat mixture and allow to cool.
(c) Add potassium chromate (VI). Divide mixture and add(i) dil nitric acid,(ii) dil ethanoic acid
(d) Add aqueous potassium iodide until in excess.
(e) Add aqueous sodium sulphide
.
QUESTIONS
(a) A sensitive test for cyanide ions ( concentration limit 1 in 50,000) involves their reaction with polysulphide
(S2 2- ) ions to form thiocyanate ions to which a solution of iron (III) chloride is then added. Suggest the colour
and formula of the final product.
(b) Cyanide ions react with dil HCl to liberate a poisonous gas which has the smell of bitter almonds. Identify
the gas and explain the reaction.
Do not write a full lab report. Tabular form of the result is suggested.
Phosphate ions and silver nitrate
yellow ppt (soluble in both acid and
ammonia)
phosphate ions and ammonium
molybdate with heating yellow ppt
page 16 of 20
MODULE 3
TITLE:
AIM: To compare the efficiency of separating ethanol from a sample of Unknown Barbados Rum by simple
distillation and fractional distillation.
INTRODUCTION: Methods of separation are never 100% efficient. However some methods are more
efficient than others. The separation technique which is more suitable is dependent on the type of mixture being
separated.
PROCEDURE:
Observe the demonstration for the simple distillation and the fractional distillation of the sample. Please note
the distillation rate and if you are careful waft the vapours from each type of distillate for your own
determination of alcohol present.
RESULTS
Table of comparison of simple and fractional distillation of a sample of Unknown Barbados Rum
Temperature of the
lower boiling point
fraction
Volume of
distillation after
demonstration was
completed
Smell of distillate
(state whether there
was a strong or
weak smell of
alcohol)
Simple distillation
Fractional
distillation
QUESTIONS:
1. Explain the process of simple distillation and fractional distillation. What areas in the demonstration that
could have been improved to obtain a purer distillate?
2. Even industrially not all the water can be removed from an alcohol water mixture via fractional
distillation. Suggest what can be done to remove the last traces of moisture from a distillate obtained from an
alcohol-water mixture.
3. Why would there be a difference in the volumes of distillate collected?
4. Based on the strong or weak smell of alcohol of the distillate, which seems to be the more efficient
separation technique?
page 17 of 20
MODULE 2
TITLE:
page 18 of 20
MODULE 3
TITLE: Qualitative analysis of sample X
SKILLS TESTED: M&M, A&I
PROCEDURE:
Carry out the following tests on the sample X. Carefully record all observable changes. Complete the table below. Do not
write a full lab report.
Tests
1. Add a heaped spatula load of the
solid X to 10 cm3 of distilled water in
a boiling tube and stir thoroughly.
Keep the contents of the tube for the
following tests.
2. To approximately 1 cm3 of solution,
add NaOH(aq) slowly until in excess.
Observations
Inferences
..
.
Ion(s) possibly present
Ion present
TREATMENT OF RESULTS
1.
2.
3.
4.
page 19 of 20
MODULE 2
TITLE:
AIM :
INTRODUCTION:
The ethanol content of a distillate may be determined by the following procedure:
1. A given volume of the distillate is treated with an excess of potassium dichromate of known concentration by
heating the mixture in a water bath for at least 2 hours or in an oven overnight.
2. The sample is then left to cool to room temperature.
3. Any excess dichromate is estimated by adding an excess of potassium iodide to the mixture. The dichromate will
oxidize the iodide to iodine.
4. The iodine can then be estimated using a standard solution of sodium thiosulphate.
This procedure was carried out up to the end of step 3 on the same volume of the two samples of alcohol collected by
fractional distillation and simple distillation from a previous practical. The iodine mixture obtained from the alcohol
sample collected by simple distillation is labeled A; and that from the alcohol sample collected by fractional distillation
is labeled B. You are required to determine which distillation method was the more efficient.
PROCEDURE:
Pipette 25cm3 of the iodine mixture into a clean conical flask. Fill the burette with a standard solution of sodium
thiosulphate. Titrate the iodine mixture until a pale yellow (straw) colour is obtained. Add 1 cm 3 of starch solution and
carefully continue the titration until the blue-black colour just disappears. Repeat the titration to obtain consistent results.
Record your results in an appropriate format.
TREATMENT OF RESULTS:
The following equations are useful in helping you to arrive at a conclusion re the relative alcohol content of the two
alcohol samples: The standard solution of sodium thiosulphate
I2(aq) + 2 S2O32- (aq) 2I- (aq) + S4O62- (aq)
2I- - 2e
I2 (aq)
page 20 of 20
MARGARINE VS BUTTER