Chemistry Practicals First Years 87-3 PDF
Chemistry Practicals First Years 87-3 PDF
Chemistry Practicals First Years 87-3 PDF
201
[CHEMISTRY
LABARATORY MANUAL
FOR FIRST YEARS]
THIS MANUAL PROVIDES STUDENTS WITH BASIC KNOWLEDGE OF HANDLING
CHEMICALS AND PERFORMING EXPERIMENTS IN A CHEMISTRY LABORATORY.
JOMO KENYATTA UNIVERSITY OF AGRICULTURE AND TECHNOLOGY
DEPARTMENT OF CHEMISTRY
Introduction
Performing experiments with chemicals in the laboratory is one of the most
important and exciting aspects of chemistry. It is from the results of experiments
over years that the information presented in lectures has been discovered. The
search for further insight into the underlying principles of chemistry, for new
compounds, particularly of biological significance, for new uses of compounds,
and for information about the secrets of the chemistry of living organisms
continues in the laboratory.
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IMPORTANT TECHNICAL POINTS
1. Keep your working spaces neat at all times and clean up before you leave at
the end of the period.
2. When boring a cork do not bore against the palm of your hand.
3. When forcing glass tubing through a cork or stopper, do not use any part of
your body as a backstop for the tubing. Hold the tubing as close to the cork
or stopper as possible, preferably with a piece of cloth.
4. Use a flexible metal spatula to break up caked solids in bottles, not a glass
rod.
5. Use Erlenmer flask for re-crystallization not beakers.
6. Do not place volatile solvents (often indicated in solvents bottles) in an
open flask except for a very short period of time.
7. NEVER assemble apparatus over a sink or delivery distillate into a sink.
8. Do not evacuate a flat-bottomed flask unless it is a heavy-wall suction flask
9. Materials which give off noxious fumes should be handled in fume hood.
10. Dispose of organic solvents into the waste recovery bottle.
11. Always wash your hands before leaving the laboratory.
A WORD OF WARNING
Most of the apparatus used are expensive to buy so use them carefully. If you are
in doubt whatsoever as to how to assemble or use the apparatus, please consult a
Technician or Lecturer in charge. Practical write up must be handed in within the
specified time given and not later. Nobody should hand a report for a practical
that he/she never attended.
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UNIT SCH 2100:
INORGANIC CHEMISTRY ONE.
EXPERIMENT 1.
VOLUMETRIC ANALYSIS.
Introduction
A quantitative analysis based upon the measurement of volume is called
volumetric or titrimetric method. Volumetric methods are much more widely
used than gravimetric methods because they are usually more rapid and
convenient. In addition they are often as accurate.
Procedure
Weigh out accurately about 1.32 g of a substance which is a metal carbonate with
the formula X2CO3 into a 250 ml volumetric flask. Add about 100 ml of distilled
water and stir until the crystals dissolve. Adjust the volume of the solution in the
volumetric flask to the mark. Pipette 25 ml of this solution into a 250 ml conical
flask. Add 2-3 drops of methyl Red indicator and titrate with a standard 0.1
hydrochloric acid. Repeat the titrations until the titres agree to 0.05 cm 3. Record
your results in a table.
Calculations.
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EXPERIMENT 2.
Visual observations of Emission colors of some of the Alkali metals
Theory
When the alkali metals are heated their outermost electrons are easily excited to
higher energy states. When these excited electrons ‘drop back’ to the ground
energy states, each alkali metal emits a characteristic color (which occurs in the
visible region hence a visual observation).
Procedure
Make appropriate dilute solutions of the salts NaCl2, KCl, LiCl and use distilled
water to make the above solutions. Dip a platinum wire in each solution and
quickly remove it and put it on the flame. Note the color each sample produces.
Repeat the process in a tap water. Repeat the process in a solution CaCl2. In your
write up, identify the most dominant alkali in the tap water.
Exercises:
a) Draw an energy level diagram (sketch) which roughly explains how the
above colors are produced. Explain the process involved.
b) Draw a table showing the colors emitted by the elements Lithium, Sodium,
potassium, ceasium, and Calcium.
c) Explain the major difference between the colors produced by the alkali
metals and Calcium.
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EXPERIMENT 3:
Introduction
Procedure
Weigh out accurately about 1.3 g of primary standard sodium carbonate into a 250
ml volumetric flask, add about 100 ml of distilled water and shake until dissolved.
Adjust the volume to the mark and mix thoroughly. Pipette 25 ml of this solution
into a 250 ml conical flask, add 2-3 drops of methyl red and titrate with HCl
solution to be standardized until the solution turns brown red. Now boil the
solution for 30 seconds. The color of the solution should return to yellow. Cool
the solution and titrate until the red appears again. Boil the solution and if the
yellow color returns again, repeat the above procedure. The titration is complete
when the red color persists.
Calculations:
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EXPERIMENT 4:
STANDARDIZATION OF APPROXIMATELY 0.1 M SODIUM HYDROXIDE
USING AN ORGANIC ACID AS A PRIMARY STANDARD.
Introduction:
Procedure:
Weigh out accurately 2.04 g of the ordinary Analar (A.R) product of potassium
hydrogen phthalate into a 100 ml volumetric flask. Add distilled water and
dissolve the solid. Make up the solution to 100 ml (up the mark). Using 10 ml
portions of this solution titrate each of them with the sodium hydroxide solution
(approximately 0.1M already prepared) contained in a burette, using the
phenolphthalein or thymol blue indicator.
Note: Individual titrations should not differ by more than 0.1 ml.
Questions:
Reference:
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EXPERIMENT 5
a) Oxalic acid
In acid solution, permanganate oxidizes oxalic acid to carbon dioxide
with water. This reaction is slow at room temperature, but above 600 C
it is fast enough to be useful in analysis. The reaction catalyzed by the
manganese (II) ion, which is formed during the titration, autocatalysis.
b) Hydrogen peroxide
Hydrogen peroxide is oxidized to oxygen by the permanganate ion in
acid solution; the reaction is fast at room temperature unlike the
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reaction in (a). Note that very dilute solutions of hydrogen peroxide
decompose rather quickly.
c) Iron(II)
Perhaps the most important permanganate method is the analysis for
iron ores, steels and other alloys. Iron (III) in acid solution.
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TITRATION OF IRON (II) SOLUTION
Mohr’s salt, (NH4)2Fe (SO4), 6H2O, keeps well under storage (it does
not lose water or become air-oxidized). Weigh accurately 1 to 1.5g of the
salt into a 250 ml conical flask. Dissolve the salt in about 40 ml, 1M
sulphuric acid and titrate with standardized permanganate solution.
Repeat at least once. Calculate the percentage of iron in the salt and
compare your results with the theoretical, two more titrations.
References
1. A.I. Vogel, a textbook of Quantitative Inorganic Analysis,
Longman, London(1971)
2. L.B. Clapp, Investigating Chemical Systems II, Rhode Island(1971)
Exercises
1. Write net ionic equations (redox equations) for the three
reactions in part (a to c).
2. Calculate the concentration of iron(II) solutions and that of oxalic
acid in:
i) moles/litre ii)
grams/litre
3. Give two reagents you can use to reduce iron (III) to iron (II).
4. Explain briefly the use of redox titrations as an analytical method.
5. Write the equations for the oxidation reactions for potassium
permanganate in alkaline media.
6. Why is potassium permanganate not used as a primary standard?
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EXPERIMENT 6:
TITRATION OF ANTACIDS
Introduction
In the procedure below, excess acid is added to react with the antacid, the
solution is heated to remove CO2, and the excess acid is titrated with standard
base. Phenolphthalein can be used as an indicator and reasonably sharp end point
is obtained.
CO2 + H2O
Procedure:
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6. Add 4 drops of the indicator and titrate with standard base to the first
permanent pink color.
7. Calculate the grams of HCl neutralized by 1 g of antacid.
8. Assume that 0.1M HCl has density of 1.00g/ml
9. Calculate the grams of 0.1m HCl solution neutralized by 1g of the antacid.
Note:
There may be a small amount of white solid (filler), which does not dissolve
even after heating.
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EXPERIMENT 7:
You are provided with orange squash or commercial fruit juice that has been
diluted 50%. It is alleged to contain citric acid has indicated in the assay. The
Government National Laboratory wants to ascertain the concentration of citric
acid in the commercial juices. The aim of this experiment is to find the
concentration of the citric acid given that it reacts with NaOH by the equation:
COOH COONa
CH2 OH CH2 OH
Procedure.
Put the squash in the burette. Take 10ml aliquots of the 0.1M NaOH
provided into a conical flask. Add phenolphthalein indicator and titrate this
against the squash.
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Calculations
1. Calculate the number of moles of NaOH in 10cm3 of the 0.1M
NaOH 2. How many moles of citric do these moles of NaOH react with?
3. What is the volume of citric acid containing these moles?
4. What is the original undiluted volume of the squash that contained
these moles of citric acid?
5. Calculate the concentration of the original acid in moles per litre.
6. Calculate the concentration of the citric acid in grams per litre (C=12,
O=16, H=1).
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EXPERIMENT 8:
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EXPERIMENT 9
To find the equation for reaction by titration
Put potassium permanganate (0.02M) in the burette. Pipette 25cm 3 of
oxalic acid solution into a conical flask. (CARE: oxalates are poisonous)
and add 10cm3 of 1M sulphuric acid. Heat the mixture to about 60 0C and
then titrate against the permanganate solution until a permanent pink color
is obtained.
Questions
1. Find the number of moles of permanganate in the mean titre and hence
calculate the number of moles of oxalic acid that react with the
permanganate in the 25 cm3 of oxalic acid solution.
2. How many moles of oxalic acid react with one mole of permanganate?
3. How many moles of oxalic acid react with two moles of potassium
permanganate?
4. The half equation are:
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EXPERIMENT 10:
Since there is gain of electrons on the left hand side of the equation, the
dichromate ion, CrO2-7 is reduced. The corresponding species in the
titration will have to undergo oxidation to supply the electrons that are
taken up by the dichromate ion.
In this experiment iron (II) will be as the reducing agent, iron (II) is
oxidized to iron (III) by a suitable oxidizing agent, such as potassium
dichromate, according to the equation:
Fe2+ Fe3+ +e -
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Since one mole of dichromate ion requires six electrons, then six moles of
iron (II) will be required for every mole of dichromate ion. i.e.
6Fe2+ +
6Fe3+ 6e-
The overall balanced redox reaction is:
6Fe2+ + Cr O + 14H
2 2-7 + + +
Fe3+ 2Cr3+ 7H2O
The end point of dichromate titration is detected by using a suitable redox
indicator; a color change from deep green to intense violet-blue occurs with
barium dephanylamine sulphate.
Requirements
Procedure
Preparation of standard K2Cr2O7:
Weigh accurately 50.8g (to the nearest 0.001g) of dried K2Cr2O7 and empty the
contents into 1 litre volumetric flask. Add sufficient distilled water and mix well
to dissolve the K2Cr2O7. Add enough water to the 1 litre mark ().
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Preparation of standard solution of Ferrous ammonium
sulphate
Iron (II) is rather unstable in air and consequently the samples must not be
heated in oven to dry them.
Weigh accurately 390.g (the nearest 0.001g) of ferrous ammonium sulphate and
empty the contents into a 1 litre volumetric flask. Add sulphuric acid to dissolve
the solid and bring to 1 litre mark with distilled water. Use of sulphuric acid as a
solvent prevents hydrolysis and also provides the necessary acidic conditions for
the titrations.
Fill the burette with K2Cr2O7 solution. Pipette exactly 25ml of iron ammonium
sulphate solution into a 50 or 100 ml flask. Add about 0.5 ml of the indicator
solution and about 2ml of conc. Phosphoric acid which reacts with the iron (III)
ions, producing a complex which does not affect the indicator.
Carry out one rough titration and three accurate titrations. Results should agree
to within 0.05cm3.
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UNIT SCH 2101.
EXPERIMENT 1:
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Principles:
Apparatus
1. Pipette(10ml)
2. Burette(50ml)
3. Conical flask(250ml)
4. Small beakers(50ml)
5. White tiles
6. Burette stands.
Procedure:
1. Fill a clean burette with a standard solution of H2SO4
2. Pipette in triplicate 10ml of an alkali from a 50ml beaker into a clean conical
flask.
3. Add 2 drops of methyl red to an alkali.
4. Then run in the standard solution from a burette until the color changes
from yellow to red.
Calculate:
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a) 1. Molarity of the alkali
Note:
Name:………………………………………………………………………..Stream………………………………
Titration
1 2 3 Average
…………………………………………………………………………………………………………………………..
ml of H2SO4
……………………………………………………………………………………………………………………………
Calculation of results:
Calculate:
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a). 1. Molarity of the alkali
Note:
DATA SHEET
Name:………………………………………………………………………..Stream:……………………….
Titration 1 2 3 Average
…………………………………………………………………………………………………………………..
Ml of H2SO4
…………………………………………………………………………………………………………………………
Calculation of results:
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Report
1. Calculation of normality of NaOH
2. Calculation of wt. of NaOH per litre
3. Calculation of Molarity of NaOH
4. Calculation of purity of NaOH
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EXPERIMENT 2:
Acid-Base titration: The titration of weak acid with a strong base
Introduction:
This experiment involves the titration of a weak acid with a strong and the
selection of a suitable indicator for the titration. Acid-base titration forms one
branch of volumetric analysis. Other branches such as redox, precipitation, and
complex metrics, will be studied later.
Several tutorials have been or will be given on aqueous solutions containing acids
and bases and the calculation oh pH of these solutions. At the end of this exercise
you will find a problem which should test your understanding of these principles.
We will proceed on the basis that you have some understanding.
and the solution will have a “basic” pH i.e. >7. Similarly for the titration of a strong
acid with a weak base-hydrolysis occurs.
M+ + H2O = MOH +H i.e. MOH + H-
And the solution will have a pH >7. Titrations of weak acids with weak bases are
usually avoided. The reason for this will become apparent later.
The end point of an acid base titration will therefore be characterized by a definite
pH, the value depending on the nature of the acid and the base and as has been
discussed in tutorials, the concentration of the solution.
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The most important method of detecting the end point of an acid-base titration
involves the use of pH indicators. These are substance, either weak organic acids
or bases, which posses different colors according to the pH of the solution. Let us
consider the example of a weak acid type indicator Hin. In aqueous solution the
acid dissociates according to the equilibrium,
HIn + H- + In-
First note that the equilibrium is a function of pH. Now if Hin has a different
color from that of HIn, the color of a solution containing the indicator will change.
K2 = (H -) (In-) (1)
(HIn)
Or
In general, the eye will perceive the color of the molecule HIn when it is present to
the extent of ten times or more the amount of I-. Conversely the color of In- will be
perceived when it is present to the extent to ten times or more the amount of HIn.
I.e. In- color perceived at
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10
pH= pKa + log - -pKa + 1
1
If one form is more intensely colored than the other or if the eye is more sensitive
to one color than the other, then the middle tint will be highly displaced along the
pH range of the indicator.
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When doing a titration of a weak acid against a strong base, the end point cannot
be accurate since at the equivalence point, the solution contains excess of OHions
which will repress the hydrolysis of the salt.
As a general rule it may be stated that for a titration to be feasible, there should be
a change of approximately two units of ph at or near stoichiometric point
produced by the addition of a small volume of the reagent. The ph at the
equivalence point during titration of a weak acid and a strong base is calculated
from the equation:
NOTE: The pH range for acids with Ka 10 3 is 7 105; for weaker acids (K 10-5)
the range is reduced (8- 10). The pH range 8 10.5 will cover most of the
examples likely to be encountered; this permits the use of thymol blue,
thymolphthalein, or phenolphthalein.
The weak acid to be used in this experiment is glacial acetic against sodium
hydroxide being a strong base.
Objective (a):
Procedure:
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water and add the washings to the volumetric flask. Make up to the mark with
distilled water. Shake the flask well to ensure thorough mixing. Titrate 10ml
portions for the acid with 0.1 M standard sodium hydroxide solution using
phenolphthalein or thymol blue as the indicator.
Reaction:
QUESTIONS
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EXPERIMENT 3:
DETERMINATION OF THE CONCENTRATION OF
HYDROCHLORIC ACID PRESENT IN A GIVEN SOLUTION
The aims of the experiment.
REAGENTS REQUIRED
a) Oxalic acid
b) NaOH solution
c) Hydrochloric acid solution of unknown strength
d) Phenolphthalein as an indicator.
Introduction:
COOH C_OONa
+2NaOH (aq)
COOH (aq C_OONa (aq)
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Procedure
Indicator: Phenolphthalein
Pipette 25ml of the given hydrochloric acid into a conical flask and add 23
drops of phenolphthalein. Titrate the contents of the flask with NaOH
solutions taken in a burette. A light pink color (permanent) appears. Repeat
the experiment or titration until two concordant volume values are obtained.
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EXPERIMENT 4: WATER
OF HYDRATION
Introduction:
Water has a strong attraction for many compounds because of its polar
character and electronic structure. Because water is a normal component of
our atmosphere, most compounds will contain some dissolved or absorbed
water. In some cases, water molecules become chemically bound in a
compound, usually an ionic salt, so that the water molecules become part of
the crystal lattice.
In such compounds called hydrates, the water molecules are in e definite
proportion relative to the other atoms and must be included as part of the
chemical formula.
Copper (II) Sulphate pent hydrate is such a compound. It may be written
either as CuSO4 (H2O) 5 or CuSO4.5H2O.
The water in hydrates often is loosely bound and may be driven off by heating
the solid. If CuSO4 (H2O)5 is heated until all the water is driven off, the
remaining CuSO4 are called anhydrous Copper (II) Sulphate. If the anhydrous
crystals are allowed to stand in the air, they will absorb water from the air
continuously, until the pent hydrate is formed. If an aqueous solution of Cu2+
and SO42- ions is evaporated, CuSO4 (H2O) 5 will crystallize directly. The
behavior described for CuSO4 (H2O) 5 is typical of many other hydrates. Some
examples are NiSO4 (H2O) 7, NaCO3 (H2O) 2 and CoCl2(H2O)6. At any given
pressure, the temperature at which a particular hydrate will lose its water
completely is difficult for each salt.
Some hydrates lose their water at room temperature and atmospheric pressure;
these are called efflorent. Hydrates which are stable at room temperature and
one atmosphere, but are not yet saturated with water to stoichiometric limit
will absorb water from the atmosphere; these are called hygroscopic.
Hygroscopic salts often are used as drying agents, called desiccants.
When a hydrate is heated, it may lose its water in several stages, forming a
series of hydrates with regular crystalline structures that contain progressively
smaller proportions of water. Color changes often accompany a change in
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degree of hydration. For example, CoCl2 (H2O) 2 is violet and anhydrous CoCl2
is blue. Intermediate species such as CoCl2 (H2O) 3 are unstable and do not
form regular crystal structures.
At anytime particular temperature, the degree of stable hydration is well
defined, and the stable form of the hydrate has a definite formula.
Plan of experiment
First you examine the behavior of a group of compounds when they are heated,
to determine which hydrates are and which are not. Then you drive all the
water from unknown hydrate, to determine the mole ration of water in its
stable structure.
Procedure
A. Testing of hydrates
1. Obtain several different samples from the following group of compounds.
Your instructor will tell you how many.
Sodium chlorideCobalt chlorideMagnesium
Potassium chlorideSodium tetrasulphate
Write the names of your compounds into the table on the data sheet. The
degree of hydration for these compounds ranges from zero to twelve water
molecules.
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2. Place about 0.2g of each compound into separate small dry test tubes. Mark
the test tubes for identification.
3. Gently heat each sample, in turn, over a burner flame and observe the
results. Write your observations in the table on the data page. Try to infer
which of the compounds hydrates are, using the criteria below are.
Questions
1. The formula for a hydrate of sodium phosphate is Na 3PO4(H2O)12
(a) If all the water were driven off by heating, how much mass would
be lost from a sample which weighed 2.5433g before heating? (b)
What is the mass % of water in the hydrate?
2. A hydrate of Cobalt chloride, CoCl2 (H2O) x is heated until it reached a
constant mass. The original sample weighed 1.6884g before heating. After
heating, its mass was 1.0856g. What is the formula of the hydrate?[use
relative atomic mass: Na=23, P=31, H=1, O=16, Co=59, Cl=35.5]
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UNIT SCH 2102.
PHYSICAL CHEMISTRY ONE
EXPERIMENT 1:
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Procedure:
Reaction (1):
1. Weigh a clean dry 250cm3 Erlenmeyer flask to 0.1g
2. Pour 200cm3 of 0.25M HCl into the flask
3. Measure and record the temperature to 0.50c
4. Quickly weigh about 2g of dry NaOH pellets to the nearest 0.01g
5. Place the solid NaOH into the flask and swirl to dissolve
6. Record the maximum temperature reached.
7. Record the weights of the solution.
Reaction (a):
1. Wash out the flask used to reaction (1)
2. Repeat the procedure for reaction(1) using 200cm3 of water in
place of 0.25M HCl Reaction (b):
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Where M (f) =weight of the flask
4. Calculate the total heat absorbed.
H=H(s) + H (f)
5. Calculate the number of moles of NaOH in the reaction(=N)
6. Heat evolved per mole of NaOH
H=H/N Jmol-1
EXPERIMENT 2
TO FIND THE HEAT OF NEUTRALIZATION OF VARIOUS
ACIDS AND BASES
Questions
1. Why was polystyrene cup used instead of a glass container and why
was it placed in the beaker?
2. Work out the enthalpy of neutralization of each acid, i.e. the heat
that would be evolved on neutralizing 1 mole of H+ (aq) ions from it.
Set out your calculations as shown below;
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You may assume that the density of each solution is 1 gcm3 and that
its specific heat capacity is the same as that of water, i.e. 4.2Jg -1k-1
No. of moles of HCl (aq) in 50cm3 of
2M hydrochloric acid = 50/100 X 2=0.1
Total mass of solution=100g
Initial temperature=T1
Final temperature =T2
Temperature= (T2-T1)
Heat produced when 0.1 mol of HCl(aq)= mass of solution X specific
heat capacity/temperature rise.= 100X 4.2X (T 2-T1)J
Heat produced when 1 mol of HCl(aq)=10 X 100 X 4.2 X (T2-T1)J
Is neutralized by NaOH (aq)
i.e. Heat of neutralization of hydrochloric acid by sodium hydroxide
solution= 10/100 X 100 X 4.2 X (T2-T1) kJ mol-1
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EXPERIMENT 3:
DETERMINING A SOLUBILITY PRODUCT.
Aim
Introduction
The equilibrium between calcium hydroxide and its ions in an aqueous solution is
Ca (OH)2 (s) =Ca2+ (aq) +2OH- (aq)
Requirements
Safety spectacles
4 stoppered bottles, 250cm3
Spatula
Calcium hydroxide
Measuring cylinder, 100cm3
Distilled water
Small funnel
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Hydrochloric acid solution, 0.1M standardized
Phenolphthalein indicator solution
Procedure
1. Into each of 4 bottles put about 2g of powdered calcium hydroxide and
about 100cm3 of distilled water. Stopper securely.
2. Shake well for about a minute. Label each bottle with your name.
3. Rinse and fill the burette with standardized HCl
4. Filter the contents of one bottle, allowing the first 5cm3 to run to and
collecting the rest in a dry conical flask. (The first few cm3 are rejected
because they are less concentrated in solute than the rest.).The filter paper
absorbs solute until it attains equilibrium with the solution. Yet another
equilibrium!)
Step 5 and 6 should be done as quickly as possible (with due care) and with
only the minimum shaking that will ensure mixing.
5. Rinse the pipette with the calcium hydroxide solution and transfer 25cm 3
to a conical flask (this need not be dry).
6. Add two drops of phenolphthalein to the flask and titrate the solution until
the pink color just disappears. Record your burette readings in a copy of
results Table 2.
7. Record the temperature.
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Table 2: Results
Solution in flask mol dm3 cm3
Volume used
Mean titre
Calculation
1. Calculate the concentration of hydroxide ion in a saturated solution of
calcium hydroxide.
2. From the equilibrium concentration of hydroxide ion calculate the
equilibrium concentration of calcium ion.
3. Calculate the solubility of calcium hydroxide at the temperature of your
experiment. Compare your result with the value listed in your data
book.
4. Calculate the solubility product from:
a) Your list
b) The solubility of Ca (OH) 2 given in your data book.
5. Suggest a reason for the speed of working advised for steps 5 and 6
above.
(Hint: slow working with much shaking of the flask, gives a smaller
titre).
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EXPERIMENT 4:
A PH OF A WEAK ACID AT VARIOUS
CONCENTRATIONS
Aim:
The purpose of this experiment is to examine the effect of dilution on
the pH of ethanoic acid, a weak acid.
Introduction:
Ethanoic acid dissociates according to the following equation:
CH3CO2H (aq) = CH3CO2- (aq) + H+(aq)
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Results in Table 4a:
Concentration of Observed pH of Calculated pH of
acid(mol/dm3) solutions of ethanoic solutions of
acid hydrochloric acid
0.00010
0.0010
0.010
0.10
Questions:
1. Compare the pH of ethanoic acid with HCl at each concentration
a) In which of the two acids is the concentration of hydrogen ions
greater?
b) What does this tells you about the extent of dissociation of
ethanoic acid compared to hydrochloric acid?
2.
a) What happens to the difference between the pH of the two acids
as concentration decreases?
b) Use Le Chateliers principle to explain the effect of dilution on the
extent of dissociation of ethanoic acid.
Wash your hands with soap or detergent and water after
handling chromium solutions and the reaction mixtures.
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EXPERIMENT 5:
Introduction:
When aqueous solutions of HCl and NaOH are mixed, a reaction takes place, the
products being a salt and water only.
NaOH (aq) + HCl (aq) NaCl (aq) + H2O (l)
I.e. OH- + H+ H2O
This is a neutralization reaction since the H+ ion which is responsible for acidic
properties has reacted with the hydroxide ion which is responsible for basic
properties. The purpose of this experiment is to determine the heat change for the
neutralization reaction between NaOH and HCl.
0.5M HCl
0.5M NaOH
0.5M HNO3.
Procedure:
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Using NaOH as the base and HCl and HNO3 as the acids, proceed as follows
performing the neutralization as duplicate.
1. Pour 40cm3 of 0.5M NaOH into one measuring cylinder and 40 ml of the
acid into the other.
2. Measure accurately and record the temperature of each solution
3. Pour the acid and base together into the beaker simultaneously.
4. Stir gently with the thermometer and record the highest temperature
reached.
5. Wash the beaker and do the duplicate.
6. Repeat the above procedure but now use HNO3 as the acid
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EXPERIMENT 6:
RATE OF THE REACTION BETWEEN- SODIUM
THIOSULPHATE AND HYDROCHLORIC ACID
Introduction:
This experiment is designed to examine the kinetics of the reaction
between sodium thiosulphate and hydrochloric acid.
S2O3 (aq) + 2H+ (aq )S (s) + SO2 (g) + H2O (l)
This rate is determined from the time it takes a fixed amount of sulpur to
precipitate. By varying the concentrations of thiosulphate and then acid,
it is possible to determine the order of the reaction with respect to
thiosulphate and acid respectively.
Apparatus:
Graduated cylinder, 10cm3, 100cm3
Beaker, 50cm3. Stop watch.
Reagents:
3M hydrochloric acid.
0.15M sodium thiosulphate.
Procedure:
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cm3 of 0.15M NaSO3 cm3 of H2O cm3 of 3M HCl
solution
25 0 4
20 5 4
15 10 4
10 15 4
5 20 4
10 0 5
10 1 4
10 2 3
10 3 2
10 4 1
Results and Calculations:
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EXPERIMENT 7:
Procedure
Set up the same apparatus as in the previous experiment, pour
50cm3 of distilled water into the cup and measure its temperature.
Accurately weigh about 1.6g of anhydrous copper (II) sulphate on
a watch glass, tip the solid into the water and stir gently with the
thermometer until dissolution is complete. Note the maximum
temperature change. (Again, the use of a thermometer calibrated
in steps of 0.1 0C id desirable)
Repeat the experiment, using about 2.5g of copper (II) sulphate in
place of the anhydrous salt.
Questions
1. What are the possible sources of error in this experiment?
2. Calculate the enthalpies of solution of the two forms of the salt
as shown below. Assume that the densities and the specific
heat capacities of the solutions are the same as those of water
and that the salt and water were both at the same temperature
at the beginning of the experiment.
Temperature change =T
Heat produced by mass of copper (II) =Mass of solution X specific heat capacity
X temp rise
=50 X 4.2 X T J
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Heat produced by 1 mol (159.5g) of =159.5 X 50 X 4.2 X T J
Copper (II) sulphate dissolves in water M i.e.
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EXPERIMENT 8:
O or (oo)
Weak electrolytes, such as acetic acid, are characterized by a rapid non-linear fall
of Δ with increase in √C. This rapid decrease is due to a reduction in dissociation
of the molecules, whose bonding is predominantly covalent: The degree of
dissociation decreases approximately with the square root of concentration. The
slight fall of Δ with increase of √C for strong electrolytes is due to long range
electrostatic interaction of ions which reduces their ability with increase of
concentration.
Materials required
Conductance bridge and dip-type cell, 250ml 0.1 M solutions of potassium
chloride and acetic acid, 5.0, 10.0, 25.0 ml pipettes, 100ml graduated flask.
Procedure
Evaluate the cell constant from the measured resistance of the cell when dipping
in 0.01M potassium chloride solution.
Prepare 0.05, 0.05, 0.025, 0.01, 0.005, 0.0025, 0.001, 0.0005, and 0.0001 M solutions
of potassium chloride by accurate dilutions from the 0.1M solution of potassium
chloride using appropriate pipettes and graduated flask. Good quality distilled or
de-ionized water of specific conductance less than 1.5 X 10-6 ohm-1 should be
used for this dilutions. Determine the resistance of the cell when dipping into
each of the prepared solutions. Wash out the beaker and cell at least twice with
each solution, before taking a measurement. Repeat the dilutions and resistance
measurements using acetic acid. If possible, all measurements should be made on
the same day to minimize the effects of changes in room temperature. The results
obtained using acetic acid solutions also provide the data required for experiment
7.3.
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Results.
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UNIT SCH 2103
REACTIONS OF HYDROCARBONS
Introduction:
The limited chemical reactivity of the alkanes is indicated by the alternative name,
‘paraffins’ which means ‘little affinity’.
On the other hand, due to the presence of carbon carbon double bond, alkenes
are quite reactive.
In this experiment you will examine some simple reactions of alkanes and alkenes.
EXPERIMENTS:
1.Take three dry test tubes. To one, put 5 drops of an alkane, to the second put 5
drops of an alkene and to the other, 5 drops of benzene. To each of the three
test tubes, add ten drops of alkaline potassium permanganate solution.
Tabulate your results. [1% KMnO4 (aq) is made alkaline by the addition of
0.3-0.5 K2CO3(s)].
2. Repeat experiment 1 using 10 drops of acidified potassium
permanganateinstead of alkaline KMnO4 solution [H2SO4 is used to acidify].
3. To 1ml of an alkane in a test tube, add 10- 15 drops of bromine if
tetrachloromethane, drop by drop. Shake the test tube to ensure thorough
mixing after addition of each drop. Note any changes in color.
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Compare the color of the two test tubes. Test for the presence of HBr by holding a
moist blue litmus paper above the top of the test tube.
Finally add 1 ml of distilled water to each test tube, shake and separate the
aqueous layer using teat pipettes. Test each aqueous layer with aqueous silver
nitrate.
Questions:
1. On the basis of the above experiments, how would you distinguish between
cyclopentane and cyclopentene?
2. What kind of reaction occurs when:
i) An alkene decolorizes bromine in tetra chloromethane.
ii) An alkene decolorizes bromine in tetra chloromethane in the
presence of sunlight?
3. Indicate whether the following statements are true or false.
i) There is free rotation about the carbo carbon double bond of the
alkenes.
ii) Alkenes are isometric with cycloalkanes.
iii) The melting points of unsaturated fats and oils are increased by
catalytic hydrogenation. iv) The hybridization of the carbon
atoms in ethane is changed by an addition reaction.
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EXPERIMENT 2:
Introduction:
Alkyl halides have the general formula R-X (X=halogen). The halogen
is the functional group.
Alkyl halides can be divided into three classes, according to how
many alkyl groups are attached to the carbon atom which is bonded
to the halogen.
H H R
R C X R C X R C X
H R R
Primary (10) Secondary (2 0) Tertiary (30)
Most important reactions of alkyl halides are those in which the
halogen atom, X, is replaced by another group.
R X R OH + NaX
A Carbonation
Followed by
R + OH-
+
R OH
(The double barbed curly arrow represents movement of two
electrons)
The presence of the X- ion can be detected by reaction of silver nitrate
solution to form insoluble silver halide.
Not all alkyl halides form carbocations easily. The ease of formation
depends upon the structure of the halide. The following are some
classes of alkyl halides with indication of the ease with which they
form carbocation.
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Type of halide Ease of formation of carbocation Primary; Difficult
Cl
Tertiary; Easy
E.g. CH3 CH3
C
CH3 C CH3 CH3 CH3
Cl CH3
Alkyl; Easy
EXPERIMENT:
1. To compare the rate of hydrolysis of chloro-bromo- and
iodoalkanes.
-Place 2 ml of ethanol in each of the three test tubes, to act as a solvent.
Add to the solvent 5 drops of 1-chloro butane, to the second 5 drops of
1bromo butane and to the third, 5 drops of 1-iodo butane.
Put 5 ml of silver nitrate solution 0.1M in another test tube and stand
all four in a beaker of water at about 600C for about 10 minutes.
Transfer 1 ml of the silver nitrate solution to each of the other three
test tubes, shake them to mix their contents and put them back into
the warm water. Observe
a) The order in which the precipitate appears
b) The color and density of the precipitate
Record your observations in tabular form headed experiment,
observation and conclusion.
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2. To compare the rate of hydrolysis of 10, 20, 30alkyl
halides
Questions:
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EXPERIMENT 3:
REACTIONS OF ALCOHOLS
Introduction:
Tertiary R C OH
R
b) Elimination
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Examples in which oxygen is retained: Primary and secondary alcohols can
be oxidized by several methods to give aldehydes and ketons respectively.
(The aldehydes may be further oxidized to carboxylic acids under some
conditions).
Na2Cr7O7 O
CH3CH2OH CH3 C H
H2SO4 ethanal. (Aldehyde)
EXPERIMENT:
1. Reaction with Sodium
a) Put about 1 ml of the alcohol in a dry test tube and add a small piece of
sodium (rice grain size). Note the effervescence and test the gas with
a lighted splint.
b) When the sodium has all dissolved, carefully evaporate the solution to
dryness and add 3 drops of water. Test the solution with litmus
paper. 2. Reaction with carboxylic acid (Esterification)
Warm a mixture of 5 drops of an alcohol and 5 drops of an ethanoic acid
with one drop of concentrated sulphuric acid (CARE). Note the
characteristic smell of the product.
3. To 5 drops of an alcohol in a test tube add 2-3 drops of ethanoyl
chloride.
4. Oxidation reactions
a) Place 5 drops of the alcohol in a test tube, add 10 drops of dilute
sulphuric acid and 2 drops of potassium dichromate (0.1%).
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Warm gently noting i) the color of the solution ii) the smell of the
product
Questions:
1. Give the IUPAC name for each of the following alcohols
a) CH3CH2CH2CH2OH
b)OH
CH3 C CH2CH3
CH3
c)OH
CH3CHCH2CH2CH3
d)CH2CH3
CH3 CH2 CH2CCH3
OH
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2. Name the four alcohols represented by the molecular formula
C4H9OH and write their structural formula.
What is the effect of oxidation upon each of these compounds?
EXPERIMENT 4:
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Perform the following series of experiments to investigate the
reactions of aldehydes and ketons.
2. Fehling’s solution
To 1ml of the aldehyde or ketone, add 1ml of 10%
sodium carbonate solution followed by 1ml of
Fehling’s solution and boil the mixture for 1 minute.
Note down your observation.
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concentrated sulphuric acid (Care: corrosive).
Warm the mixture gently.
For an aldehyde R=H and hence only ethanol CH3 C=O gives
positive results.
Alcohol which on oxidation gives R C=CH3 also give positive
iodoform reaction.
• Add 3 4 drops of the aldehyde or ketone to 2ml of water
and add 2ml of 10% sodium hydroxide solution.
• Add drop wise with shaking a 10% solution of iodine in
20% potassium iodide solution until a dark brown color
persists.
• Allow to stand and warm if necessary.
A positive result is indicated by the presence of yellow crystals.
Record down your observations.
7. Addition-Elimination(Condensation)reactions with
2,4- Dinitrophenylhydrazine
Most aldehydes and ketones react with
2, 4 Dinitrophenylhydrazine (2, 4 DNPH) whose structure is
NO2
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NO2 H2NNH
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