C12 Chemical analysis and investigation

In this chapter we will learn about:

- Testing for anions and cations
- Testing for gases and water
- Collecting gases
- Testing pH
- How to test for unsaturated hydrocarbons
- The use of chromatography as a test for purity and to analyse a mixture
- Aspects of experimental work and the scientific method.

C12.01 Chemical analysis

One of the most important jobs for a chemist is to be able to analyse chemical compounds
and materials and be able to figure out what they are. Chemical analysis is widely used in
research institutions and industrial processes:
- Checking the contents of foods to make sure they do not contain harmful chemicals
- Checking the purity of the air and water
- Checking the gases and waste products emitted by cars and factories
- Making sure that the medicines we use are safe
- Making new medicines
- Analysing materials found in crime scenes.
There are of course thousands of more applications that we could add to this list. Before a
chemist does any chemical analysis they must be sure that they have a series of protocols
decided upon before they start the analysis.

C12.02 Inorganic analysis

The first type of analysis that we will look at is called qualitative analysis.

This type of analysis will tell us whether a substance is present or not but does not tell us
how much of the substance is present nor does it tell us the purity of that substance.

For this type of analysis we need to identify a reaction that will clearly show us that particular
ion is present and can not be confused with another one.

The most useful reactions for us are ones which produce a precipitate, this is where two
solutions are mixed together and an insoluble precipitate is formed.

Testing for anions.

The characteristic tests for the presence of anions (Remember: anion is a negative ion) are
listed below.
 Negative ion Test Test result

Carbonate (CO32-) Add dilute HCl to solid effervescence , carbon

dioxide produced (further
tested with limewater to
confirm CO2 gas)

Chloride (Cl-) in solution Acidify solution with dilute White precipitate of silver
nitric acid, the add aqueous chloride is formed, further
silver nitrate tested and soluble in
ammonia solution

Sulphate (SO42-) in solution Acidify solution with dilute White precipitate of barium
nitric acid, the add barium sulphate is formed
nitrate solution

Nitrate (NO3-) in solution Make solution alkaline with Ammonia gas is released,
sodium hydroxide solution, test with moist red litmus
then add aluminium foil and paper.
warm carefully

Testing for cations

Once we have identified the anion present in our unknown substance we then need to figure
out what cation is present (Remember: cation is a positive ion).

As we saw in a previous chapter metal ions when tested using a flame give off different
colours. This is an easy way to identify the cation.

The precipitation tests for metal ions are based on the fact that most metal hydroxides are
insoluble. Some of these are coloured as we can see in the table further below but many of
them are white in colour. We also must be very careful when we are adding sodium
hydroxide to the solution that we are testing as we may miss the formation of the precipitate
if it re-dissolves in excess sodium hydroxide. Therefore we should add the sodium hydroxide
drop by drop and quite slowly.

This is the case for the hydroxides of aluminium and zinc. As they are amphoteric
hydroxides they will re-dissolve in excess sodium hydroxide.

The hydroxides of the other metals do not re-dissolve because they are basic hydroxides-
reacting only with acids in neutralisation reactions.

Metal ion Formula Colour of flame

Sodium Na+ Yellow

Potassium K+ Lilac

Lithium Li+ Crimson

 Copper Cu+ Blue-green
Flame test colours

The strategy behind testing for metal ions in salts.

Positive ion Effect of adding sodium hydroxide Effect of adding ammonia solution
(in solution)

Ammonium Ammonia produced on warming -

(NH4+) (test with damp red litmus paper)

Copper(II) Light blue gelatinous precipitate of Light blue gelatinous precipitate,

(Cu2+) copper hydroxide, insoluble in dissolves in excess ammonia, giving
excess of sodium hydroxide a deep blue solution

Iron (II) Green gelatinous precipitate of Green gelatinous precipitate,

(Fe2+) iron (II) hydroxide, insoluble in insoluble in excess.
excess

Iron (III) Rust-brown gelatinous precipitate Rust-brown gelatinous precipitate,

(Fe3+) of iron (III) hydroxide, insoluble in insoluble in excess
excess

Calcium White precipitate of calcium White precipitate, soluble in excess

(Ca2+) hydroxide, insoluble in excess

Zinc (Zn2+) White precipitate of zinc White precipitate, soluble in excess

hydroxide, soluble in excess,
 giving a colourless solution

Aluminium White precipitate of aluminium White precipitate, insoluble in excess

(Al3+) hydroxide, soluble in excess,
giving a colourless solution

Tip: It is very important that you know the tests in the table in this chapter. They are very
common questions in exam papers and you will not have a copy of this information in the
exam.

Tip: It is very important to use the correct wording in your answers- you must use the word
colourless- to describe the results. Many students use the word “clear” and this is wrong-
clear and colourless do not mean the same thing in science.

The tests for gases

As we have already seen some of the tests for anions and cations require the collection of
gases for further testing. The gas tests are another very important part of analytical
chemistry, the table below we can see the tests for five important gases.

Before we look at them we need to see the different methods for collecting gases:
- Downward delivery: is used for the collection of gases that are denser than air.
- Upward delivery: is used for the collection of gases that are less dense than air.
- Collection over water: is used for gases that are not very soluble in water.
- Collection in a gas syringe: this method is used when the volume of gas needs to be
measured.
Gas Colour and smell Test Test result

Ammonia (NH3) Colourless and Hold damp red Indicator paper turns
pungent smell litmus paper in gas blue

Carbon dioxide Colourless and Bubble gas through White precipitate of

(CO2) odourless limewater (Calcium calcium carbonate is
hydroxide solution) formed, the
limewater turns
milky colour

Chlorine (Cl2) Pale green and Hold damp litmus Indicator paper is
choking smell paper in gas bleached white

Hydrogen (H2) Colourless and Hold a lighted splint Hydrogen burns

odourless in the gas quickly making a
pop sound

Oxygen (O2) Colourless and Hold a glowing splint The splint re-ignites
odourless in the gas
Sometimes it is necessary to produce a gas by heating a test tube and then it is collected
over water. This method may cause a dangerous effect that is called suck back. This is
where the heat source is removed from the test tube and the delivery tube starts to cool
down. This will cause the gas to contract and suck water back through the delivery tube and
into the hot test tube. This sudden cooling and presence of water may cause the test tube to
crack or explode. To avoid this a bunsen valve must be used at the end of the delivery tube.
This will stop the water flowing in the reverse direction. To further avoid problems you should
remove the delivery tube first from the water before removing the heat source.

Other tests
These may include testing the pH of the substance either by using litmus paper, universal
indicator or an electronic pHmeter.

The presence of water may also be tested for by using cobalt chloride paper which turns
from blue to pink in the presence of water.

To show that the water being tested in pure water then you will have to check its boiling
point. Pure water has a boiling point of 100℃. Remember from previous chapters we have
seen that the boiling point of a substance will be affected by the presence of impurities. A
pure substance has a known and sharp boiling point.
Questions
C12.01 Why can many metal ions be identified by using sodium hydroxide solution?
C12.02 Which metal hydroxides will dissolve in excess sodium hydroxide solution?
C12.03 Why can iron ions give two different coloured precipitates with sodium hydroxide?
C12.04 What gas is produced when acid is added to a solution of carbonate ions?
C12.05 What solution will give a precipitate with chloride ions?
C12.06 What must be added before barium nitrate when testing for sulphate ions?
C12.07 Which gas is tested with a glowing splint?
C12.08 Name a cation which is not a metal ion.
C12.09 The table below shows the results of practical tests on substance A to E.

Choose from, A to E, the substance that is likely to be :

a. Distilled water
b. Sodium chloride solution
c. Chlorine gas
d. Hydrochloric acid.

For e. Name a suitable candidate.

Substance Action on universal Action on Action on silver

indicator solution hydrochloric acid nitrate solution

A Goes red then No reaction No reaction

bleaches

B Goes blue Fizzes White precipitate

C Goes red No reaction White precipitate

D Stays green No reaction No reaction

E Stays green No reaction White precipitate

C12.03 Organic analysis

There are also some characteristic tests for certain organic chemical compounds. You need
to be familiar with the test for unsaturated hydrocarbons.

Remember that unsaturated hydrocarbons are ones which contain at least one double bond.
The simplest test for an unsaturated hydrocarbon such as an alkene (for example ethene) is
to use bromine water. If the unknown compound is a liquid then they can be mixed together
directly or if it is a gas then it may be bubbled through it. The bromine water is initially an
orange-brown colour. If the gas or liquid being tested is an unsaturated hydrocarbon then it
will make it colourless. Alkanes for example are saturated hydrocarbons and would have no
effect on the bromine water.
Chromatography
Chromatography was initially used as a method for separating coloured substances,
however, it can also be used for analysis in helping to identify substances.
The components of a mixture, for example food colouring, can be compared to the positions
of known compounds. These known compounds are called standards. This will allow us to
confirm whether or not certain suspect substances have been added to the food colour.

Summary.
You should know:
- How to identify inorganic compounds:
- Test for cations
- Test for anions using flame tests
- Test anions using sodium hydroxide and aqueous ammonia
- Test gases
- Test pH
- Test for the presence of water.
- How to test for unsaturated hydrocarbons
- How to use chromatography.

End of chapter questions.

1. Why is it important for chemists to be able to tests to discover what elements and
compounds substances contain?
2. A student reacted dry ammonia gas with hot copper (II) oxide. The apparatus used is
shown below. The equation for the reaction is:

2NH3 + 3CuO → 3Cu + N2 + 3H2O

 a. On a copy of the diagram indicate where we should heat the apparatus. (1)
b. The colour of the copper (II) oxide would change from __________ to _________ (2)
c. Draw a diagram of how we should capture the water vapour as it leaves the
experimental apparatus. (2)
d. Suggest the effect that the nitrogen would have on a lighted splint. (1)

3. Electricity was passed through aqueous copper (II) sulphate solution using inert
electrodes as shown in the the diagram below.

a. Why have carbon electrodes been used in this experiment? (1)

b. At which electrode will the copper be deposited? (1)
c. Give one other observation seen during this experiment. (1)

The electrode at which the copper was deposited was removed, washed , dried and weighed
periodically during the experiment. . The results are shown in the table below.

Time (minutes) Mass of electrode (g) Total increase in mass (g)

0 3.75 0.00

10 4.00 0.25

20 4.25 0.50

30 4.50

40 4.75

50 4.90

60 4.90

70 4.90
 d. i. Suggest how the electrode was washed. (1)
ii. How could the electrodes be dried quickly? (1)

e. Copy and complete the table above by calculating the total increase in the mass for
the remaining time intervals. (1)
f. Plot the points on a copy of the grid paper below. Draw a graph, remember to
correctly label your axes.

(3)
g. Suggest why the last three readings were the same. (1)

(Cambridge IGCSE Chemistry 0620 paper 61 Q2 November 2012)

4. The diagram below shows the results of an experiment to separate and identify the
colours present in two coloured mixtures, A and B.

Substances C,D,E and F are single colours.