The gravimetric method is based on the quantitative precipitation of

SO42- by BaCl2 in a HCl medium, after removal of Si and suspended

solids (e.g. CaSO4 + BaCl2 = BaSO4 + CaCl2). The method is subject
to interferences from SO32-, S2-, Si, NO3-, certain heavy metals such as
Cr and Fe, and suspended matter. According to American Public
Health (1975), the gravimetric method is the most accurate method
for determining SO42- concentrations > 10mg SO42- l-1. However, the
method is time consuming and normally requires relatively large
volumes of samples. Moreover, the quality of results depends to
some large measure on the skill and experience of the analyst. The
relatively high detection limit of the method precludes its application
to waters containing < 10 mg SO42- l-1. American Public Health
Association (1975) reports a between-laboratory relative SD and
CV2 of 4.7% and 1.9% , respectively, for 32 laboratories analysing an
unknown synthetic sample with 259 mg SO42- l-1.
An ore is any rock from which a metal may be extracted. Ores usually contain a compound of the
metal, a mineral, together with waste material. To decide whether an ore is worth mining it is
necessary to find out how much of the useful mineral it contains, and how much is waste. This
experiment illustrates one way in which this might be done using a form of colorimetry in which
comparisons of depth of colour are made by eye without necessarily using a colorimeter.

This experiment depends on the making and use of a set of comparison solutions of known copper
concentration of the kind that might be used with a colorimeter. Here the comparison is made by eye
but, as an extension, the solutions could be used in a colorimeter and a proper calibration curve
drawn and used.
Purified (deionised or distilled) water
Dilute sulfuric acid, approx. 2 M (CORROSIVE), 40 cm3
Sample of powdered ore (see technical notes) (HARMFUL, DANGEROUS FOR THE
ENVIRONMENT), 10 g
Copper(II) sulfate solution, 1 M, 25 cm3(HARMFUL, DANGEROUS FOR THE ENVIRONMENT)
Refer to Health & Safety and Technical notes section below for additional information.
Eye protection
Each student or pair of students will require:

Beaker (250 cm3)

Beaker (100 cm3)
Volumetric flask (100 cm3)
Small filter funnel and filter paper, to fit volumetric flask
Test-tubes, 6 (Note 1)
Test-tube rack
Plastic weighing dish (boat)
Measuring cylinder (50 cm3)
Measuring cylinder (10 cm3)
Access to:
A balance (weighing to the nearest 0.1 g)

Read our standard health & safety guidance

Wear eye protection throughout.
Dilute sulfuric acid, H2SO4(aq), (CORROSIVE) - see CLEAPSS Hazcard and CLEAPSS Recipe
Book.
Sample of powdered ore - A simulated copper ore made up with a minimum of 30% by mass of
copper(II) carbonate, CuCO3(s), (HARMFUL - see CLEAPSS Hazcard) thoroughly mixed with dry
silver sand or washed and dried building sand.
Copper(II) sulfate solution, CuSO4(aq), (HARMFUL, DANGEROUS FOR THE ENIVORNMENT) see CLEAPSSHazcard and CLEAPSS Recipe Book.
1 Test-tubes must have a capacity of at least 10 cm3.
a Weigh out as exactly as possible 10 g of the ground ore and transfer it into a 250 cm 3 beaker.
b Add 40 cm3 of the dilute sulfuric acid a little at a time, allowing the effervescence to subside
between additions.
c When the reaction has finished filter the mixture into the volumetric flask.
d Add purified water until the total volume of liquid in the flask is exactly 100 cm 3.
e Using the copper(II) sulfate solution provided, prepare six tubes of diluted copper(II) sulfate,
according to the following table. Ensure the solutions are well mixed.

Tube number

Voume of copper(II) sulfate

solution/cm3

Volume of purified water/cm3

10

f Pour a 10 cm3 sample of the copper solution from your volumetric flask into another test-tube.
g Compare the colour of your tube from part f with those from part e. Which one matches the colour
best?
h Estimate the mass of copper mineral in 10 g of the ore using the following table:
Tube of best match

Mass of compound in 10 g or
ore/g

10

7.5

2.5

It is a good idea to set up the standard colour test-tubes in a rack, put white paper under the tubes
and observe by looking down through the solutions.
When students have completed this experiment they are probably going to ask two things:
1 What is the correct answer?
2 How does the arithmetic work?
For the answer to the first question, consult the person who made up the ore mixture it is best to
come clean and confess that the ore is not a real one. Samples of copper ore, such as malachite,
could be shown, if available.
For the second question, work out the concentration of copper in, say, test-tube 3:
Concentration Cu (as Cu2+) = 4/10 x 1 M = 0.4 M
Work out the concentration of copper ions when 5 g of copper carbonate is dissolved and made up
to 100 cm3 of solution: (Formula mass of CuCO3 = 124)
Concentration Cu = (5/124) x (1000/100) = 0.4 M

The two concentrations should be the same. However, this calculation works only approximately
because basic copper carbonate also contains an equimolar amount of copper hydroxide and some
water.
It should be stressed that copper ores are seldom as concentrated as this.

1.

What happens? Why is concentrated ethanoic acid called 'glacial'?

Concentrated acetic acid is often called glacial acetic acid. The origin of this name can be
attributed to acetic acids high freezing point. Acetic acid freezes into a solid at a temperature
very close to room temperature: 16.5 C, or 62 F. When it freezes, it kind of looks like ice; hence
the term glacial.

Cautiously smell the vapour from a bottle of concentrated ethanoicacid. Hold

the bottle at a distance, fill your lungs with air and waft thevapour towards
your nose.
2. Is the smell familiar? How did the original name 'acetic acid' come to
be used for what we now call ethanoic acid?
. On the other extreme, when used undiluted (anhydrous) its called glacial acetic acid.

Test the solubility of concentrated ethanoic acid in water.

3. Is the acid soluble in water? Explain your answer in terms of the
structure of the acid.
4. Would you expect octadecanoic acid, C17H35COOH to be soluble in
water? Explain your answer.
Experiment 2: To investigate the Acidic properties of ethanoic acid
Using a pH meter, measure thepH of 0.1 mol dm-3 solutions of:
a ethanol,
bethanoic acid,
C hydrochloric acid.
5. Record your results and list the three compounds in order of increasing
acid strength.
6. Would you classify ethanoic acid as a strong or a weak acid?
7. What explanation can you give for the difference In acid strength
between ethanol and ethanoic acid?
Measure the pH of a 0.1 mol dm-3 solution of sodium ethanoate.
8. Why might sodium ethanoate be expected to be neutral?
9. Is it neutral in fact? If not, why not?

Put 10 cm3 of 2 mol dm-3 sodium hydroxide solution in an evaporating

basin. Add 5 cm3 of 2 mol dm-3ethanoic acid and cautiously smell the
resulting mixture.
10.
Can ethanoic acid still be smelled? If not, why not?
Add a further 5 cm3 or so of 2 mol dm-3ethanoic acid to the evaporating
basin, until the acid is just in excess. (How can you test whether it is in
excess?) Evaporate the contents of the evaporating basin over a beaker of
boiling water until all the water has left the basin and white crystals
remain. (This may take some time. Get on with another part of the
practical while you are waiting.)
11.
Identify the white crystals and write an equation for the reaction
that has occurred.
Put a few of the crystals in a test tube and add a few cubic centimetres of
dilute hydrochloric acid. Gently warm the tube and cautiously smell the
vapour coming off.
12.
What has been formed? Explain the reaction that has occurred in
terms of your answer to question 5.
Experiment 3:Esterification
Put 2 cm3 of ethanol (ethyl alcohol) in a boiling tube and add 1 cm3
ofconcentrated sulphuric acid. Add a few drops of concentrated ethanoicacid
and warm the tube gently with shaking (CARE). Allow the tube tocool a little,
then pour the contents into a beaker containing about50 cm3 of cold water.
Cautiously smell thevapour.
13.
Describe the smell of the vapour.
14.
write the structural formula of the ester that has been formed.
15.
Write an equation for the reaction.
16.
What is the purpose of the sulphuric acid in this reaction?
17.
Why is the reaction mixture poured into cold water before
smelling?
18.
Give the names and structural formulae of the esters that would
have been formed if:
a)pentan-1-ol had been used instead of ethanol,
b)propanoic acid had been used instead of ethanoic acid.
Experiment 4:Oxidation
Put 2 cm3 of concentrated ethanoic acid in a test tube. Add a few drops of
potassium manganate(VII) solution and warm gently.
19.
Are there any signs of reaction?
20.
Is ethanoic acid easily oxidised?