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Aim: To identify the cation and anion in a mixture.

Theory;

All matter can be classified into two categories: pure substances and mixtures. A pure
substance consists of a single element or compound. Iron is formed only of iron (Fe) atoms;
table salt is formed only of sodium chloride (NaCl) molecules. A mixture, however, is made up
of different compounds or elements. A mixture contains two or more substances that have not
reacted chemically with each other. Despite that there are no chemical changes to its
constituents, the physical properties of a mixture, such as its melting point, may differ from
those of the components. Some mixtures can be separated into their components by physical
(mechanical or thermal) means.

Qualitative analysis is a chemical technique used to determine the identities of


chemical substances present in a mixture but not their quantity. In this case, qualitative
analysis of a compound is a scheme of test to identify the cation and anion present in the
compound. There are many types of qualitative analysis including observing the colour of salt
or aqueous solution, observing the solubility of salt in water, observing the effect of heat on
the salt, identifying the gases evolved when a test is performed on the salt and identifying the
precipitate formed when a chemical reagent is added to the aqueous solution. And of course
solubility of compound should be test first as they are quick and reliable and use only a small
amount of sample.

To identify the cations and anions exactly in an unknown compound as well as a


mixture, we can actually use the analysis flowcharts below.

FC 1

FC 2

Apparatus:

Beaker, test tube, measuring cylinder, test tube holder, spatula, Bunsen burner, glass rod,
dropper, wooden splint, litmus paper, delivery tube with rubber stopper, conical flask, tripod
stand with wore gauze.
Materials:
S3 mixture powder, 2M sodium hydroxide, 3M ammonium hydroxide, 6M hydrochloric acid,
0.2M barium chloride, 6M nitric acid, 0.2M silver nitrate, distilled water, potassium iodide, lime
water.
Procedure:

1. The steps in the experiment which are supplied in table 1,2 and 3 are carried out.
2. The observation for the test are recorded.
3. Analysis based on the observation are made.

Table 1

1. Observe the appearance of the S3mixture. (Physical properties)


O: White powder
Odourless
Coarse
A: Na+ K NH4 Mg ca ba Al Pb Zn may be present.
2. Place one small spatula of the S3 mixture in about 30ml of water. Stir it.
O: Slightly soluble in water
A: 1 compound is soluble in water, 1 compound is insoluble in water.
3. Separate 2 compounds:
Put all the S3 mixture powder in a beaker,
Pour about 300ml of water in the beaker and stir it.
Filter the mixture solution using a filter funnel and filter paper.
O: The filtrate is collected in a beaker.
The residue left on the filter paper.
Ana: The filtrate solution is a soluble salt.
The residue is an insoluble salt.
Table 2
Compound 1 ( Soluble salt )
1. Put 5ml of the filtrate into a test tube and add NaOH dropwise. Shake the solution and
observe any reaction. If a precipitate forms, continue adding excess NaOH. Stir or
shake the solution.
O: No precipitate form after dropwise of NaOH. Ana; NH4+ ions present.

2. Put 5ml of the fitrate into a test tube and add NH4OH dropwise. Shake the solution
and observe any reaction. If a precipitate forms, continue adding excess NH4OH. Stir
or shake the solution.
O: No precipitate Ana: NH4+ ions present
3. Heat the filtrate and test the gas released with a moist red litmus paper.
O: Red litmus paper turns blue Ana: NH4+ ions present.
4. Put 5 ml of the filtrate solution into a test tube and add a few drops of 6M HCl. Then
add a few drops of 0.2 M BaCl2 solution. Shake the solution and observe any reaction.
O: No precipitate, A: SO42- ions is absent.
5. Put 5 ml of the filtrate solution into a test tube and add a few drops of 6M HNO3. Then,
add a few drops of 0.2 M AgNo3 solution. Shake the solution and observe any reaction.
O: White precipitate formed. Ana: Cl-ions present.

Compound 2 ( Insoluble salt )

1. Pour about 50 ml of 6 M nitric acid in a conical flask. Put small amount of the unknown
residue (S3)(insoluble salt) into the conical flask and then close it with a delivery tube
stopper. Channel the tube into the lime water and observe the changes.
O: Lime water turns chalky Ana: CO32- ions present
2. Pour about 50 ml of 6 M nitric acid in a conical flask. Put small amount of the unknown
residue into the conical flask. TEST the gases evolved with a burning wooden splinter.
O: Put off the burning splinter Ana: CO32- ions present
3. Put about 30cm3 of 6M nitric acid in a beaker and heat it.
Add the unknown residue compound a little at a time into the acid using spatula while
stirring continuously with a glass rod. The addition of the compound is stopped when
some solid remain undissolved.
The mixture is filtered to remove excess compound. Pour the filtrate into a beaker
O: filtrate is a colourless solution Ana: Na+ K NH4 Mg ca ba Al Pb Zn
may be present.

4. Put 5ml of the filtrate into a test tube and add NaOH dropwise. Shake the solution and
observe any reaction. If a precipitate forms, continue adding excess NaOH. Stir or
shake the solution.
O: White precipitate does not dissolve
A: Ca 2+ , Mg 2+ may be present.
5. Put 5m l of the fitrate into a test tube and add NH4OH dropwise. Shake the solution
and observe any reaction. If a precipitate forms, continue adding excess NH4OH. Stir
or shake the solution.
O: No precipitate
A: Ca2+ present
Discussion:

In this experiment, we have to identify the cation and anion in an unknown mixture.
Throughout the test, there are many aspects and precautions that required us to pay more attention.
Firstly, I washed all the apparatus with distilled water in order to prevent the dust or microorganisms
from affecting the outcome. All of the apparatus are wiped with a filter paper as we all know that
heating the apparatus with wet surface probably causing it to crack.

Besides, the addition of a reagent to the solution should be carried out drop by drop while
shaking the test tube until no further change occurs. Then, we must make sure to label all tubes and
solutions because these accumulate rapidly, and it is very easy to get tubes mixed up. All observations
must be recorded carefully and immediately after every test. The inferences are then recorded as soon
as possible.

Based on the experiment, I have identified that there are 1 soluble and 1 insoluble compound
present in the mixture. Both compound can be separated easily by dissolving and filtering it because
they do not chemically bond together. The soluble compound is NH4Cl. In this case, the presence of
NH4+ ions can be identified by the positive result (no precipitate fomed) came out when the addition
of NaOH solutions. The red litmus paper turns blue showing presence NH4+ ions as it shows basic
properties. Meanwhile, the presence of Cl- ions in the compound can be identified by the addition of
HNO3 and AgNO3 solution to it while white precipitate is produced.

As we all know, insoluble compound cannot react directly to the reagent. Hence, it had to
react with nitric acid to produce nitrate salt which are soluble and able to react when tested with
certain reagent. During this process, excess insoluble salt is added and then filtered to ensure all of
the ions in the nitric acid had completely reacted.

On the other side, the insoluble compound is CaCO3. The presence of Ca2+ ions are confirmed
from the test which shows no precipitate after testing with excess NH4OH. Then, the presence of
CO32- ions is confirmed through the results such as turns lime water chalky and put off a
burning wooden splinter. This is because the chemical reaction between an acid with any
carbonate salts will definitely release carbon dioxide at the end. In this experiment, we have
to redo the test for a few times as some outcome are not the thing we expected. This can be
happened by some error or mishandling the chemical substances such as mixing the solution with
other chemicals.

Throughout the process, we have to extra careful as there are some ions have similar
characteristics and reaction to certain reagents. After the experiment, I realised there are many
aspects which I need to improvise afterwards. For instance, I should wear a pair of rubber glove while
handling high corrosive chemicals such as hydrochloric acid. Secondly, I should wear eye protection
and mask. Because ammonia solution can cause burns and released pungent gases in the reaction
which then will affect our eyesight and respiratory system.

In short, this experiment emphasizes the importance of accurate observations, properly


recording them, and the use of deductive logic to draw conclusions from those observation.

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