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Chemistry 1A
FACULTY OF SCIENCE
Laboratory Manual
201030
*CHM104*
Chemistry 1A
Faculty of Science
Revised by
Dr Michael Antolovich
Dr John H. Beard
Dr Andrea Bishop
Educational designer
Jen Thompson
Produced by the Division of Learning and Teaching Services, Charles Sturt University, Albury -
Bathurst - Wagga-Wagga, New South Wales, Australia.
Revised 1986
Reprinted 1990, 1991, 1993
Revised 1994, 1995, December 1997, December 1998, December 1999,
December 2000, December 2001, November 2002, November 2003,
November 2004, November 2005
Reprinted November 2006
Revised November 2007
Reprinted November 2008
Revised January 2010
Previously published material in this book is copied on behalf of Charles Sturt University pursuant to
Part VB of the Commonwealth Copyright Act 1968.
ii
Contents
Page
General notes 1
The aims of the practical program 1
Learning outcomes 1
How to use the manual 1
Assessment of laboratory work 2
How to use the laboratory 3
Laboratory safety 3
Safety rules 5
iii
iv
General notes
Learning outcomes
When you have successfully completed this subject you should be able to:
Outline
Objectives
These list many of the concepts and skills which you should have mastered on
completing the exercise. If you have any difficulty with any of these objectives
you should discuss them with your demonstrator.
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Discussion
This section includes theory relevant to the practical exercise. It must be worked
through before attempting the practical work.
Procedure
The actual practical work to be undertaken is set out in stepwise fashion in this
section. It is essential that this be read and complete the preliminary
questions BEFORE attending the practical session. You should relate the
procedural steps to the discussion section and the objectives. You should then be
able to perceive the point of the exercise. The value in doing this is that your time
in the laboratory will be spent most efficiently and you will enjoy a sense of
purpose in your practical endeavours. Practical work should never reduce to
‘recipe-following’.
Result sheet
It is essential that you record your results in ink on the result sheet at the time
of the experiment. Marks will be deducted for use of pencil and liquid paper.
At any later stage you must be confident that the results recorded were honest,
not a later inclusion of what you thought may possibly have happened. The
result sheet must be signed and dated by your demonstrator at the conclusion of
the practical work.
Post work
In most cases this section of the exercise should be completed during the practical
session. In some cases, the calculations involved in an experiment take some time
which is best found outside the time allocated for practical work. In others, some
questions are set to test your understanding of the concepts involved in the
particular practical exercises.
Practical work is allocated 20% of the total assessment for Chemistry 1A. Details
are provided in the Subject Outline.
Attendance at practical sessions is compulsory. Any student who attends less than
80% of the time allocated to practical work without adequate explanation (e.g.
medical certificate for illness) will be automatically awarded an FL grade for
Chemistry 1A.
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The following points are listed to help you to work efficiently in the laboratory.
If you are at all unsure about any procedure, ask your demonstrator.
Laboratory safety
To help you become a safe laboratory worker, some hazards commonly found in
chemistry laboratories are mentioned below. These are followed by a set of rules
which must be obeyed at all times by students working in the chemistry laboratories.
Hazards
a. Laboratory equipment
• All unfamiliar equipment, e.g., distillation apparatus, gas cylinders,
should be regarded as hazardous. Check with a demonstrator
before use.
• Never use cracked or badly worn glassware. Obtain a replacement
from the service counter.
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b. Dangerous chemicals
Gases and vapours
• Entry routes for gases and vapours are through the lungs, eyes, skin
and mouth.
• Some which attack eyes and lungs are Cl2, Br2, NH3, NO2, SO2.
• Those which are toxic when inhaled include H2S, HCN, CO, Hg.
• Vapours of any flammable liquid and H2 and CO can form explosive
mixtures with air.
• Any reaction from which a gas issues should be performed under a
fume hood, as should any reaction known to involve even minute
amounts of the gases listed above.
Liquids
• Entry routes for liquids are through the skin, eyes and mouth.
• Liquids or solutions which are strongly acidic, strongly basic or
strongly oxidizing can cause external damage particularly to eyes.
Liquids containing a halogen often behave similarly.
• Affected areas of the body should be washed with copious quantities
of water.
• Some liquids decompose explosively when heated. A common
example is hydrogen peroxide H2O2.
• Liquids boiling in open containers can superheat and vaporise
explosively. A boiling chip (porous pot), placed in the liquid before
heating is commenced, reduces this hazard.
Solids
• Most solid chemicals are toxic to some extent.
• Entry routes for solids are through the lungs, eyes, skin and mouth.
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Safety rules
3. Report all accidents, however slight, to the supervisor or first aid officer .
To be handed in to supervisor:
---------------------------------------------------------------------------------
I have read and agree to abide by the rules set out above.
Signed: __________________________________
Date: ___________
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Outline
Objectives
Discussion
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The source emits all the colours of white light. The wavelength selector (a
monochromator or filter) selects a particular wavelength (really a very narrow band
of wavelengths) which it is known is absorbed by the sample (analyte). Some
fraction of that wavelength of light passing through the sample will be absorbed by
the sample. For a fixed source intensity, P0, the intensity of the light emerging from
the sample, P, is determined by the concentration of analyte. The higher the
concentration, the more light is absorbed by the sample and hence the lower is P.
The detector, a photomultiplier tube (PMT), converts the incoming light signal, P,
into an outgoing electrical signal which can be very precisely measured.
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X
X
X
A X
c
A calibration plot determined at a fixed analysis wavelength.
Clearly, colorimetry relies on the analyte being coloured. Many substances are
naturally coloured and so can be directly analysed by colorimetry. However, even
those that are not coloured (or are so feebly coloured that analysis is very
difficult) can often be made intensely coloured by reaction with another species.
This is the case in this experiment.
Aqueous CuSO4 solutions have a very pale colour at low concentrations and so
cannot be directly analysed spectrophotometrically. However, the complex ion
[Cu(NH3)4]2+ produces intensely coloured solutions in water that absorb light in
the visible region. The copper (II) ions in a copper sulfate solution can be
converted to the intensely coloured tetraamine complex by the addition of
concentrated aqueous ammonia.
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Procedure
After you have been shown how to use an analytical balance use it to weigh
approximately 1.2 g of solid CuSO4·5H20 into a beaker. Record the actual mass
to 0.0001 g.
Make up to the mark with deionised water, making sure the solutions are well mixed.
Label six 15 cm test tubes S0, S1, S2, S3, S4, S5 and pipette 5.00 mL of the
respective solutions from the volumetric flasks into them. S0 should contain
deionized water only.
Label three test tubes X1, X2 and X3. Pipette 5.00 mL of the same test water
sample into each of these test tubes.
Add 0.4 mL of concentrated ammonia solution, NH3(aq) †, to each test tube from
the dispenser. Caution: Avoid inhaling ammonia. Mix thoroughly by gently
agitating the test tubes (consult a demonstrator if you are unsure how to proceed).
Colorimetric analysis
Measure each of the standard solutions in turn, and record the absorbance values
directly in Table 1.1.
Measure each of the test solutions in turn, and record the absorbance values
directly in Table 1.2.
Confirm that the absorbance reading obtained for the samples fall within the range
of absorbance values recorded for your standard solutions. (If not, consult a
demonstrator).
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Data analysis
Calculate the molar (moles per litre) concentration of the stock standard solution
prepared. Record your working and answer on the result sheet.
The stock standard solution was diluted volumetrically to prepare the standards.
Use the concentration of the stock standard solution to calculate the concentration
of copper (II) in each of the 50 mL standard solutions, S0 to S5. Record your
answers in Table 1.1 of the result sheet.
On graph paper (available from the service hatch) prepare a properly labelled
calibration plot of absorbance against copper concentration for S0 to S5.
Using the absorbance values recorded for the water sample solutions and the
calibration plot to determine the copper concentration for each of X1,X2 and X3.
Record in Table 1.2 of the result sheet.
Calculate a mean value for [Cu2+] in your unknown. As the error, quote the
greatest absolute deviation from the mean.
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Outline
Objectives
Discussion
Before beginning this experiment you should read the section on solution
stoichiometry in Module 1.
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the reactant in the flask) is called the equivalence point. To know when we have
reached the equivalence point we use a substance called an indicator which
undergoes a colour change in the region of the equivalence point. The point at
which the indicator changes colour is called the end point of the titration. It is
important that we choose an indicator so that the end point coincides with the
equivalence point of the titration.
There are certain criteria to be met by a reaction for it to be successfully used for a
titration:
The discussion given below meets these criteria and introduces the remaining
aspects of volumetric analysis necessary for you to complete the experimental
work.
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If we accurately know the concentration of the hydrochloric acid, we can use the
HCl(aq) as a standard. For example, let us say that the concentration of
hydrochloric acid to be used in the experiment is 0.0894M HCl .
i.e. [HC1] = [H + ] = 0.0894 M
Note: Unless specified otherwise, square brackets around a substance means
concentration in moles per litre.
This will have been determined by the technical staff prior to the experiment,
using a primary standardization method.
Using a pipette, a precise volume of the standardized HCl, in this example 2.00
mL, is delivered into a conical flask and indicator added. Using a burette,
NaOH(aq) is run into the conical flask until the end point is reached. The volume
added from the burette in this example is 2.30 mL. Assuming that we chose an
indicator so that the end point coincided with the equivalence point, we can
calculate the concentration of the NaOH(aq) as follows:
2.00
Number of mole H+ added = L × 0.0894mol / L
1000
This amount was contained in the titre delivered from the burette, i.e. 2.30 mL.
2.30
∴ Concentration of NaOH = 1.79 × 10 − 4 mol ÷ L
1000
= 0.0778 mol/L
or 0.0778 M
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Acid-base titration
Procedure
Note - You will need this solution for both parts i and ii of this experiment.
Use a small volume of this approx. 0.1M NaOH solution to rinse a burette. Fill
this burette to somewhere near the 0 mL mark and record the reading to the
nearest 0.01 mL.
Place approximately 1 mL of the approx. 0.1M NaOH solution in a small test tube
and add 2 drops of bromothymol blue† indicator. Record the colour of the
indicator in base.
Repeat the titration precisely now, using a fresh 3.00 mL aliquot (sample) of the
acid but run the base in rapidly only until 0.5 mL less has been added than in the
rough titration. Continue adding the base dropwise until an indicator hue
intermediate between that found in acid and in base is obtained. Record the
burette reading. Calculate the volume of base used in this precise titration.
Perform a second precise titration and record your results. If the volumes of base
used in the two precise titrations are not concordant to within 0.02 mL, perform
further titrations until this repeatability is achieved. Calculate the molarity of the
sodium hydroxide†.
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Pipette accurately 3.00 mL of the acetic acid solution into a clean conical flask
and 2 drops phenolphthalein† indicator. Record the indicator colour in acid.
__________________________
† See MSDS
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Outline
Objectives
Discussion
Before beginning this experiment you should read the topic on Stoichiometry.
Substances are characterised (identified) by their properties. The properties of
substances can be classified as physical properties or chemical properties.
Physical properties of a substance are those which do not involve changing the
substance into another. For instance, the temperature at which ice melts to form
liquid water is a physical property of water since the change is a physical change;
both ice and liquid water have the same chemical composition, H2O. Chemical
properties of a substance are those which involve a chemical change, i.e. the
conversion of the substance to another substance. For instance, the ease with
which a substance burns is a chemical property since, in burning, the substance
chemically combines with oxygen.
In this experiment the metal, copper, is obtained by a series of chemical changes
from copper(II) chloride†.
__________________________
† See MSDS
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Quantitative transfer
Complete transfer of material without loss. Solids are often weighed on a weigh
boat or watch glass and transferred into a beaker or flask. There is no point
carefully weighing something to 4 decimal places only to tap most of it into a
beaker and then throwing the rest away.
If transferring into a volumetric flask, rinse a glass funnel and place it in the flask.
The solid is carefully transferred to the funnel and then any remaining material is
washed from the weigh boat into the funnel (a wash bottle may be used). Also
make sure that too much solvent is not used (an issue when using small
volumetric flasks).
To remove solids from a solution, filter through a glass funnel fitted with a fluted
filter paper (increases the rate of filtration). Use the following as a guide to
folding.
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Calculations of yields
The actual yield simply means the amount of purified product as weighed in the
laboratory. The theoretical yield is the maximum possible yield of product as
calculated based on the limiting reactant. Calculation of theoretical yield relies
simply on the laws of proportion.
Example:
3C6H10 + 2KMnO4 + 4H2O → 3C6H10(OH)2 + 2KOH + 2MnO2
If the actual yield in this case had weighed 2.6 g, then the percentage yield
would have been:
actual yield 100 2.6
percentage yield = × = × 100 = 23%
theoretical yield 1 11.1
When reactants are measured by volume, rather than by weight, the conversion to
weight is required to calculate the number of moles
The art of the synthetic chemist lies in obtaining the highest possible yields of
pure products with the minimum of effort. Although the percent yield is a
criterion for efficiency in the laboratory, it is only one measure among several.
The cost of materials and special equipment must be calculated. Time is perhaps
the most precious commodity of all. Full realisation of the factors making for
success in the laboratory can only come with experience.
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Procedure
After you have been shown how to use an analytical balance, use it to weigh out,
in a 20-30 mL beaker, between 0.16 g and 0.18 g of CuCl2.2H2O† to 0.001 g.
Record the mass. Add approximately 10 mL of deionised water and stir to
dissolve. Write an ionic equation for this dissolution.
Using a bunsen burner, tripod and gauze, gently boil the contents of the beaker for
about 3-5 minutes while stirring constantly to prevent ‘bumping’ of the solution.
Any chemical change that occurs is the removal of a water molecule from
Cu(OH)2† to give copper(II) oxide, CuO†. Record your observations and write a
net ionic equation for any change.
Allow the precipitate to settle and carefully decant most of the supernatant
solution through a fluted filter paper. Then transfer the remaining solution and all
the solid to the filter paper. Using a washbottle rinse the beaker with deionised
water into the filter paper. Wash the precipitate on the filter paper with deionised
water and discard all the filtrate.
Place a clean, not necessarily dry, 20-30 mL beaker under the filter funnel, pierce
a small hole in the base of the filter paper with a pasteur pipette and wash the
precipitate through the hole with 3 mL of 5 M H2SO4† (sulfuric acid). If any solid
remains on the filter paper, wash it through with the filtrate (use a pasteur pipette).
When all solid dissolved, wash the filter paper with a little water (keep the filtrate
volume as low as possible). Record your observations and write a net ionic
equation.
__________________________
† See MSDS
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Do not commence this section unless it can be completed in the time available.
(Hint: Zinc† reacts with hydrochloric acid† to evolve H2† (hydrogen gas) but
copper does not.)
Using the analytical balance weigh a clean dry evaporating dish. Record the
mass. Transfer all the copper metal you have prepared to the evaporating dish
using small jets of water from the washbottle. Decant most of the water from the
evaporating dish and heat the dish on a steam bath until it appears dry. Place the
dish in the 100ºC oven for 10 minutes to remove any remaining water and allow
the dish to cool.
Weigh the dish plus the copper and record the mass. Complete the calculations on
the result sheet. Submit your copper sample to your demonstrator for inspection.
__________________________
† See MSDS
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Outline
Objectives
• define the terms: element, compound, covalent bond, ionic bond, cation,
anion, electrolyte, acid, base, carbonate, oxide, hydroxide;
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Discussion
Part A only will be conducted as a demonstration. Before the demonstration, you
should read the following topics in the Study Guides: classification of matter,
nomenclature and equations, atomic theory and bonding.
When the bonding electrons are equally shared we say the bond is a covalent
bond and the compound is made up of essentially neutral (uncharged) molecules,
e.g. methane comprises uncharged molecules of CH4 i.e. molecules of four
hydrogen atoms covalently bonded to one carbon atom. We sometimes depict a
molecule of methane as:
H
H C H
When the electrons essentially reside on the one atom, the solid compound exists
as a regular array of positively and negatively charged species which strongly
attract one another. This attraction (bond) is called an ionic bond since we call
the charged species, ions. Positively charged ions are called cations. Negatively
charged ions are called anions.
For example, table salt, sodium chloride, NaCl, is an ionic solid which consists of
a regular array of Na+ cations and Cl– anions, i.e. the sodium atom has lost an
electron and the chlorine atom has gained an electron.
The term electronegativity is used to describe the attraction by atoms for the
electrons forming bonds between them. Covalent bonds form between atoms of
equal electronegativity. When differences in electronegativity between two atoms
is great, the bond formed between them is ionic, the atom with the higher
electronegativity becoming the anion e.g. Cl has a much higher electronegativity
than Na.
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Laboratory Manual
δ+ δ−
H Cl
H : Cl or H – Cl or
The δ s are partial electronic charges and the shaded area represents the region
where the bonding electrons spend most of their time.
Covalent compounds
Solid Liquid
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Ionic compounds
Consider a solid ionic compound. If we heat the solid until it melts we supply
enough energy for the oppositely charged ions to slide over one another.
Ionic compound
Solid Liquid
Electrolytes
We have seen that liquids and solutions can contain essentially none, some, or a
high proportion of the compound as ions and that the extent of ionization can give
an indication of the bond type in the molecules of the compound.
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Procedure
The conductivity meter supplied has the electrodes immersed in deionised water.
Test the conductivity of the deionised water by pressing the button and record the
scale reading. To measure the conductivity of other liquids or solutions, immerse
the electrodes to a uniform depth each time, record the meter reading, rinse the
electrodes with deionised water after each test and store them in deionised water.
Avoid handling the electrodes and take care not to contaminate the solutions.
2. Fusion of solids
Test the conductivity of solid and fused
i. magnesium nitrate hexahydrate, Mg(NO3)2.6H2O, and
ii. camphor, C10H16O.
To do this, place about one teaspoonful of the solid in a porcelain crucible on a
clay triangle on a tripod stand. Hold the electrodes with a pair of tongs and
immerse them in the solid. Record the conductivity reading. Heat the solid
carefully with a bunsen burner until a melt is obtained. Immerse the electrodes
again and record the conductivity of the melt.
Make sure the electrodes are dry before immersing them in the prepared solution
of hydrogen chloride (HCl) gas in toluene (stored in fume cupboard). Record the
conductivity.
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Discussion
It is not a simple matter to predict which ionic compounds are soluble and which
are insoluble in water. A knowledge of solubility rules obviates the need for
lengthy calculations and provides a body of factual knowledge by which several
important operations can be performed. Table 2.1 below lists the common
solubility rules.
Compounds formed from the combination of ions have widely differing water
solubilities. The borderline between soluble and insoluble is therefore arbitrary.
Typically:
Barium sulfate, BaSO4, is insoluble so these two ions combine and precipitate out
of solution.
Copper (II) chloride, CuCl2, is soluble so does not precipitate out of solution. A
reaction has occurred so we can write an equation. We could write
However if we look more closely at the reacting species and the products we see
that ions were involved. This leads to the idea of a net ionic equation.
BaSO 4(s ) + Cu (2aq+ ) + 2C1(−aq ) . No change occurred with the Cu (2aq+ ) or 2 C1(−aq ) ions.
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These ions are called spectators, they took no part in the reaction. The net
overall reaction was the precipitation of barium sulfate from solution. The net
ionic equation is therefore
Ba (2aq+ ) + SO 42−(aq ) → BaSO 4(s )
Procedure
You are supplied with a series of sodium solutions and a series of nitrate
solutions.
On the surface supplied (previously rinsed with deionised water and dried), add
approximately 1 drop of the appropriate sodium solution, then 1 drop of the
appropriate nitrate solution to confirm the water solubility of each of the
compounds listed in the results section Table 2. Write net ionic equations where
appropriate.
2+
Acetates: : soluble, except Ag+, Hg2 slightly soluble
2+
Bromides: : soluble except Ag+ , Hg2 and Hg2+ and Pb2+ (slightly)
2+
Chlorides: : soluble except Ag+, Hg2 and Pb2+ (slightly)
2+
Iodides: : soluble except Ag+, Hg2 and Hg2+, Pb2+.
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Discussion
( )
Practically all metal carbonates CO 32− , oxides (O2-) and hydroxides (OH–) are
insoluble in water. However they all dissolve when treated with acids (H+). The
generalised ionic equations for divalent metal ions (M2+) can be written as:
MO (s ) + 2H (+aq ) → M (2aq+ ) + H 2 O (l )
Procedure
i. Carbonates
ii. Oxides
iii. Hydroxides
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Outline
This experiment involves imposing various changes to chemical systems at
equilibrium, and applying Le Chatelier’s Principle to predict and explain the shift
in the chemical equilibria that these changes cause.
Objectives
• To study some examples of chemical equilibria qualitatively.
• To use Le Chatelier’s Principle to explain what happens when a system at
equilibrium is subjected to a change.
Discussion
Le Chatelier’s Principle tells us that, if a system at equilibrium is subjected to a
change, processes occur that tend to neutralise the imposed change. This enables
us to explain (or even to predict) what happens when we cause a change in the
concentration of a reactant (or product) which is present in chemical equilibrium
with other reactants and products.
You may have already studied the reaction between silver ions, Ag+, and chloride
ions, Cl–. When you finished mixing these reactants in a test tube, you had an
‘equilibrium system’.
We might need to explain what would happen if some Ag+(aq) were somehow
removed from the solution (i.e. the imposed change is that [Ag+] has been
decreased). Le Chatelier’s Principle helps us to do this (i.e. predict or explain the
change).
For this example we can say that the position of equilibrium has been shifted (or
changed) to the right (i.e. more product, less reactant present). Other equilibrium
systems can be dealt with in a similar manner.
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Procedure
We can test the effect of removing Ag+ from the silver chloride equilibrium
mixture by adding potassium thiocyanate, KSCN†. This gives a high
concentration of the thiocyanate ion, SCN–, which reacts with Ag+ to give the
soluble complex silver thiocyanate ion, [Ag(SCN)2]–, as follows:
The silver thiocyanate ion, [Ag(SCN)2]–(aq), is quite soluble, and its formation
reaction has a very large equilibrium constant, i.e. it is formed easily.
a. Prepare the silver chloride equilibrium system by mixing small (~1 mL),
equal volumes of 0.2M AgNO3† and 0.2M NaCl† in a test tube.
b. Very slowly add 4M KSCN† solution until you can see that some of the
AgCl(s)† has dissolved. Shake the tube. Now we have a new equilibrium.
c. What happens if more thiocyanate ions are added? Explain why this
happens.
a. Balance this equation for the equilibrium between the dichromate and
chromate complex ions.
Cr2O72–(aq) + H2O CrO42–(aq) + H+(aq)
b. Observe the two solutions (Cr2O72–(aq) and CrO42–(aq)) and record their
colours below your equation (on the results sheet).
c. i. Test what happens if you increase [H+]. Do this by adding 2M HCl†
drop by drop to ~ 1 mL of 0.1M K2CrO4† until the colour is noticeably
changed. Record your observations.
ii. Use Le Chatelier’s Principle to explain these observations.
d. i. Test what happens if you increase [OH–]. Do this by adding 2M
KOH† drop by drop to about 1 mL of 0.1M K2Cr2O7.
ii. Record and explain these observations (Le Chatelier’s Principle).
Note: Increasing [OH–] decreases [H+] by reaction to form H2O.
e. Write an equation for the reaction by which OH–(aq) removes H+(aq).
__________________________
† See MSDS
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b. We can test the effect of removing heat from the KNO3† equilibrium system
by allowing the hot solution to cool.
i. Put the test tube in a rack to cool
ii. Record your observations
iii. Observe the shape of the crystals formed.
__________________________
† See MSDS
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__________________________
† See MSDS
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Outline
Objectives
On completing this experiment you should be able to:
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Discussion
Hydrolysis of ions
The reactions of ions with water are explored by monitoring the pH of solutions
formed when a range of salts are dissolved. Hydrolysis is a reaction with water
whereby water is cleaved. Depending upon the reaction, the resulting solution
contain OH-(aq) or H3O+(aq). For example, sodium phosphate creates a basic
solution in water.
Dissolution) Na3PO4 (s) → 3Na+(aq) + PO43-(aq)
Hydrolysis of ions Na+(aq) + H2O(l) → no reaction
PO43-(aq) + H2O(l) → HPO42-(aq) + OH-(aq)
Buffer solutions
Addition of a small amount of H3O+ to the solution causes the above equilibrium
to shift towards reactants, increasing [HA] and decreasing [A–]. However, since
these two components are initially present in high concentrations, the relative
change in concentrations is quite small.
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Other significant features of these titration curves will become apparent from the
experiments and the post work.
Acid-base indicators
Acid-base indicators are simply weak acids which have a markedly differently
coloured conjugate base. If we denote the indicator by HInd and suppose HInd is
red and Ind– is yellow, then in aqueous solution we have
HInd + H2O Ind– + H3O+
Red Yellow
In strongly acidic solutions, the indicator will exist predominantly as HInd (red).
In strongly basic solutions, the indicator will exist as predominantly Ind–
(yellow). (Confirm this by applying Le Chatelier principle.)
However, when there are equal concentrations of HInd and Ind–, the solution will
be orange. We have seen this will occur when pH (solution) = pKA(HInd). In a
titration, if so little of an indicator is used that the pH of the solution is governed
by the acid-base titration itself, the end point (colour change) will be observed
when the pH equals the pKA of the indicator. For a particular titration, a suitable
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Laboratory Manual
indicator is one whose pKA approximately equals the pH of the solution at the
equivalence point.
Note: Because the eye can detect hues of a particular colour, an indicator has a
useful pH range of approximately ± 1 pH unit about its pKA.
The direction of the colour change is also important. It is easier to see the change
from colourless → pink (base added to acid using phenolphthalein) than pink →
colourless (acid added to base).
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Procedure
A. Hydrolysis of ions
1. Thoroughly clean 12 small test tubes and rinse them finally with deionised
water. Set them up in a test tube rack.
2. Add about 2 mL of the supplied, deionised water to each of the test tubes.
3. To each of the test tubes add 1 drop of ‘universal indicator’.
(Note: Universal indicator is a mixture of different indicators which give
colour changes over the pH range 4 to 11.
4. Check that the colour is the same in all the test tubes and by reference to the
colour chart, that the pH of the water is 7. If any tests tubes are
contaminated, discard their contents, clean them again and repeat steps 2
and 3 until all twelve test tubes contain water at pH 7.
5. Keep the first tube as reference and to separate tubes add a small amount
(a few crystals) of each of the salts listed in Table 6.1 on the result sheet.
6. Agitate each tube gently to dissolve the salt and record the pH of the
solution from the colour of the indicator.
B. Buffer solutions
1. Set up ten clean test tubes in a test tube rack and label them 1 to 10.
2. You are supplied with solution A: a solution which is 0.315 M with respect
to HPO 24− † and 0.50 M with respect to H 2 PO −4 †.
4. Into the first four test tubes, transfer, by pasteur pipette, 1.0 mL of
solution A.
5. Into the second four test tubes, transfer 1.0 mL of solution B.
6. Into the remaining two test tubes, transfer 1.0 mL freshly boiled deionised
water.
7. To each of the ten test tubes add one drop of universal indicator.
8. To test tubes 1, 5 and 9 add, 1 drop of 1.0 M HCl.
To test tubes 2, 6 and 10 add, 1 drop of 1.0 M NaOH.
To test tubes 3 and 7 add, 1 drop of 5.0 M HCl.
To test tubes 4 and 8 add, 1 drop of 5.0 M NaOH.
In Table 6.2 on the result sheet record the pH of each solution from the
colour of the indicator.
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Laboratory Manual
Titration 1
100 mL beaker
3. Using a pipette, transfer 2.00 mL stock NaOH† solution into the clean
100 mL beaker, add 40-50 mL of deionised water and add 2-3 drops of
bromothymol blue indicator. Add just enough water to ensure that the bulb
of the electrode is immersed in the solution, stir the solution gently using
the magnetic follower and record the pH of the solution in Table 6.3 of the
result sheet.
4. Use a little of the supplied HCl† to rinse a burette. Fill this burette to
somewhere near the 0 mL mark and record the reading to the nearest 0.01
mL.
5. Run the acid in from the burette rapidly until the solution becomes slightly
acidic. Record the burette reading.
7. Repeat the titration using a fresh 2.00 mL aliquot (sample) of the base,
deliver the appropriate volumes of stock HCl† solution and record the pH
and indicator colour after each addition in the corresponding square in Table
6.3 on the result sheet.
8. Discard the solution, rinse and dry the apparatus and reassemble as in step
1.
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Laboratory Manual
Titration 2
2. Fill the burette to somewhere near the 0 mL mark with the approx. 1.0 M
hydrochloric acid solution and record the reading to the nearest 0.01 mL.
4. Run the acid in from the burette rapidly until the solution becomes slightly
acidic. Record the burette reading.
6. From the burette, deliver the appropriate volumes of stock HCl† solution
and record the pH and the indicator colour after each addition, in the
corresponding square in Table 6.4 on the result sheet.
Titration 3
The following is a simulated experiment, the data has been supplied in Table 6.5.
3. Empty the beaker and the burette and rinse all the apparatus, including the
electrode, with tap water. Give the electrode a final rinse with deionised
water.
__________________________
† See MSDS
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Laboratory Manual
44