Problem Statement:

How to determine the cation and anion of the substances.

Objective:
To determine the cation and anion of the substances.

Introduction:

A chemical substance is a material that has a definite chemical composition. It is

homogeneous so the same chemical composition is found uniformly throughout the
substance. A chemical substance may be an element or a chemical compound. A element is
a pure substance that cannot be broken down into different types of substance while a
chemical compound is a new substance that forms when atoms of two or more elements
react with one another.

According to Brown, Lemay and Bursten (2006), qualitative analysis is used to

determine the presence or absence of a particular metal ion whereas quantitative analysis is
used to determine the amount of substance presents. Nowadays, wet methods of qualitative
analysis have become less important as a means of analysis. They are frequently used in
general chemistry laboratory programs, with the aim of illustrating equilibria, teaching the
properties of common metal ions in solution or to develop laboratory skills.

A chemical reaction is a process that changes some chemical substances into

another chemical substances. Hence, chemical reaction can be used to separate
substances in the compound also. As chemical reactions are happening during the
qualitative analysis, hence chemical reactions that take place in aqueous solution will fall into
one of three general categories which include precipitation reactions, acid-base
neutralization reactions and oxidation-reduction reactions (McMurry, Fay and Robinson,
2016).

Ions are often being separated by their different solubility. A metal ion in a substance
may form a solid which is precipitate in the presence of a specific anion while the remaining
metal ions remain dissolved in aqueous form. After the precipitate is formed, the liquid
solution above the precipitate is carefully poured off into a separate container. The soluble
ions are in the liquid solution while the insoluble ions is in the solid precipitate. Thus they are
physically separated from each other and easier to test the presence of anion and cation.
 Typically, qualitative analysis proceeds in five steps. First, make initial observation of the
physical properties of the salt. Second, study the action of heat on the salt. Third, make
aqueous solution of the salt to test for anions and cations present. Fourth, carry out
confirmatory test for cations and anions. Confirmation test allows each ion has a unique
response to an added chemical such as solution colour change or the formation of a
precipitate to confirm the presence of particular ion.

Material:
Solid KA1 and KA2
Dilute hydrochloric acid
Dilute nitric acid
Aqueous solution of sodium hydroxide, approximately 50 g dm-3
Aqueous solution of iron(III) chloride, approximately 50 g dm-3
Aqueous solution of ammonia, approximately 50 g dm-3
Aqueous solution of ammonium chloride, approximately 50 g dm-3
Aqueous solution of silver nitrate, approximately 50 g dm-3
Aqueous solution of disodium hydrogen phosphate, approximately 50 g dm-3
Aqueous solution of potassium chromate (VI), approximately 50 g dm-3
Aqueous solution of potassium iodide , approximately 50 g dm-3
Aqueous solution of sodium carbonate , approximately 50 g dm-3

Apparatus:
1 test tube rack with 6 test tubes
1 test tube holder
1 spatula
1 filter funnel and two pieces of filter paper
1 Bunsen burner
Red and blue litmus papers
Wooden splint
1 wash bottle filled with distilled water
1 lighter
1 glass rod
beaker (50ml & 100ml)
wire gauze
asbestos sheet
tripod stand
Procedure:
1. Solid KA1 and KA2 were sample salts. The experiments were carried out with solid
KA1 and KA2 to identify its cation and anion.
2. In all experiments, the reagent is added gradually until no further changes is
observed.
3. The observation is recorded and the deduction is made from the result gained.
4. The observation had included details of colour changes, precipitates and test on
gases
5. KA1 and KA2 are deducted.
6. The experiment is repeated to identify the cation and anion present in solid KA2.

Precaution step:
 Use distilled water at all times
 Label test tubes to avoid confusion
 Do not put the solutions near the fire as ammonia solution causes burns and gives off
ammonia vapour which irritates eyes, lungs and respiratory system while
hydrochloric acid, sodium hydroxide, silver nitrate solution and nitric acid can cause
burns
 Dispose all waste and chemicals in an appropriate waste container
 Use separate graduated cylinders for the solutions and water to avoid mixture of
solutions which can cause imprecise in the experiment.

Safety step:
 Wear eye protection
 Wear disposable gloves
 Wear lab coat all the time when conducting the experiment
 Wash hands thoroughly with soap and water before leaving the laboratory
 Long hair is tied
Result (KA1) :
Table 1: result of test on KA1 (refer table 3)

Test Observation Inference

a. Add dilute hydrochloric acid, HCI to The colourless Ag+, Hg2+, Pb2+,
a small amount of solid KA1, then solution turned CH3C00- ions may
warm gently cloudy. present.
White precipitate
formed after heating
Bubbles released.
Gas produced.
Smell of vinegar
released.
Blue litmus paper
turned red.

b. Dissolve solid KA1 in distilled water The colourless Mg2+ or Ca2+ ions may
and filter. Use separate portions of solution turned present.
the filtrate for tests (i) to (viii) cloudy.
White precipitate
i. Add aqueous sodium formed after NaOH
hydroxide, NaOH then in add in excess and it
excess is not insoluble.
ii. Add aqueous ammonia, The solution Mg2+, Al3+ or Pb2+ may
NH3 then in excess followed by remained colourless present.
aqueous ammonia chloride but white precipitate
NH3Cl formed after NH3
added in excess and
it is insoluble.
iii. Add aqueous iron (III) chloride, Light brown solution CH3C00- ions may
FeCl3 then warm turned reddish-brown present
after heating.
iv. Add aqueous silver nitrate, The solution No Br- , Cl-, I- ions.
followed by dilute nitric acid.  remained colourless.

v. Add aqueous disodium White precipitate Pb2+ ions may

hydrogen phosphate. formed and it is not present.
soluble.
vi. Add aqueous potassium Yellow solution Pb2+ ions may
chromate(VI) followed by dilute formed yellow present.
hydrochloric acid precipitate.

vii. Add aqueous sodium carbonate White precipitate Pb2+ ions may

formed. present

viii. Add 5-10 drops aqueous Yellow precipitate Pb2+ may present.
potassium iodide formed.

Identify of KA1:  Lead (II) acetate

Result (KA2) :

Table 2: result of test on KA2 (refer table 3)

Test Observation Inference

a. Add dilute hydrochloric acid to a Wooden splinter CO2 gas produced.
small amount of solid KA2, then extinguished CO32- ions may
warm gently Colourless and present.
odourless gas
released.
Blue litmus paper
turned red
b. Dissolve solid KA2 in distilled The solution Mg2+ or Ca2+ ions may
water and filter. Use separate remained colourless present.
portions of the filtrate for tests (i) to and white precipitate
(viii) formed in excess
sodium hydroxide
i. Add aqueous sodium hydroxide,
then in excess

ii. Add aqueous ammonia, then in The solution Ca2+ ions may

excess followed by aqueous remained colourless. present
ammonia chloride

iii. Add aqueous iron (III) chloride, Light brown solution No CH3COO- ions
then warm remained unchange

iv. Add aqueous silver nitrate, The solution remain No Br- , Cl-, I- ions.
followed by dilute nitric acid. colourless.

v. Add aqueous disodium The solution remain No Pb2+ ions

hydrogen phosphate. colourless

vi. Add aqueous potassium Yellow solution turned No Pb2+ ions

chromate(VI) followed by dilute orange
hydrochloric acid

vii. Add aqueous sodium The solution No Pb2+ ions

carbonate. remained colourless

viii. Add 5-10 drops aqueous The solution No Pb2+ ions

potassium iodide remained colourless.

Identify of KA2:  Calcium carbonate

Conclusion:
The anion presents in KA1 is acetate ions (CH 3COO-) and cation is lead (II) ions (Pb2+).
KA1 is lead (II) acetate. The anion presents in KA2 is carbonate ions (CO 32-) and cation is
calcium ions (Ca2+). KA2 is calcium carbonate.

Discussion:

For KA1, the colour of the given salt is white solid and is colourless during aqueous
state which had excluded the presence of copper, cobalt, iron, nickel and manganese as
these ions are coloured. The appearance of the given salt is crystalline which had excluded
the presence of carbonate salts (refer Figure 1).

When carrying out test (a), white precipitate is formed after heating (refer Figure 2). The
possible ions present are Group I (Ag+, Pb2+, Hg2+) cations as they produce insoluble
chlorides so they can be precipitated with dilute HCl, while all other cations remain in
solution. However, the blue litmus paper that turned red had indicated the presence of acidic
ions and a smell of vinegar had produced during heating. Hence it is acetate ions, CH 3COO-.
Equation below showed the chemical reaction: Pb ¿. According to the equation, we can
conclude that the gas produced during heating is CH 3COOH and the white precipitate is
PbCl2 as lead(II) chloride is insoluble in water.

When carrying out test b(i), theoretically, the white precipitate formed after NaOH is
added in excess should be soluble in water to indicate the possible presence of Al 3+, Zn2+ and
Pb2+ with the equation Pb ¿. The white precipitate formed should be lead (II) hydroxide.
However, in the experiment, the white precipitate turned out to be insoluble in water hence
the possible ions present are Mg2+ and Ca2+.

When carrying out test b(ii), white precipitate is formed after heating. The possible ions
present are Al3+, Zn2+ and Pb2+ as they are white precipitate insoluble in water when reacting
with NH3. Lead (II) ions is confirmed by reacting with aqueous ammonia to precipitate a
basic salt, P b2 O¿ . The basic salt is insoluble in excess ammonia chloride. The equation:

P b2+ ¿ (aq )+2 N H 3 ( aq ) +3 H 2 O ( l ) +2 N O3 → P b2 O ¿¿

When carrying out test b(iii), iron (III) chloride solution appears as a colorless to light
brown aqueous solution that has a faint hydrochloric acid odour. The iron (III) chloride
solution is added to the salt solution containing acetate to give a red colouration. The acetate
ion is confirmed by adding water to this mixture and warming till formation of red precipitate.
However, the solution remained as reddish-brown solution (refer Figure 3). The equation
when added to FeCl3 acetates produce a red coloration: FeC l 3 +3 C H 3 COOH →¿

When carrying out test b(iv), the solution remained colourless after adding aqueous
silver nitrate and dilute nitric acid because there is no any Br -, Cl-, I- ions present.
Theoritically, if either Br-, Cl-, I- ions presents, either yellow or white precipitate will be formed.

When carrying out test b(v), insoluble white precipitate formed is lead (II) hydrogrn
phosphate indicate the presence of lead (II) ions. The equation: Pb ¿.

When carrying out test b(vi), chromate (VI) ions gave a bright yellow precipitate of lead
2−
(II) chromate (VI) which shown by equation: P b2+ ¿(aq)+CrO 4 (aq )→ PbCr O4 (s)¿
.

When carrying out test b(vii), insoluble white precipitate formed is lead (II) carbonate
indicate the presence of lead (II) ions. The equation: Pb ¿.

When carrying out test b(viii), a yellow precipitate is formed as iodide ion from
potassium iodide combines with lead (II) ions to form a yellow precipitate of lead (II) iodide
−
(refer Figure 4). It can be shown by equation: P b2+ ¿(aq)+2 I (aq)→ Pb I 2(s )¿
.

Hence, the anion present in the given salt is acetate (CH 3COO-) and cation is lead (II)
(Pb2+). The salt is lead (II) acetate.

For KA2, it is same as KA1 in which the colour of the given salt is white solid and is
colourless during aqueous state which had excluded the presence of copper, cobalt, iron,
nickel and manganese as these ions are coloured. The appearance is fine and
microcrystalline powder.

Gases are often produced from reactions carried out during laboratory tests on salt.
Gases can be evolved when salts are heated or when salts are reacted with acids or alkalis.
When carrying out test (a), KA2 are being heated and carbon dioxide gas are released as
carbonate ions decomposed when heated which shown by equation :
CaC O3 ( s )+ ℎeat →CaO ( s )+ C O2 ( g ) . KA2 also reacted with acids and carbon dioxide gas
are released as carbonate ions produced carbon dioxide when reacted with dilute acid. The
release of gas can be proved by bubble releasing and the burning wooden splinter
extinguished as carbon dioxide did not support combustion. It can be shown by equation:
C O3 ( aq ) +2 H +¿ ( aq ) →C 0 ( g )+H
2 2 O (l ) ¿
. Moreover, the turning of blue litmus paper to red had
indicated the gas released is acidic and carbon dioxide is acidic gas.

For test b(i), insoluble white precipitate formed after adding excess NaOH had indicated
the presence of Mg2+ and Ca2+. The equation: CaCO 3 +2 NaOH → Ca¿ .

For test b(ii), there is no reaction between KA2 and ammonia which indicated that Ca 2+
is present.

For test b(iii), there is no reaction occur as the light brown solution remained
unchanged after heating which indicated the absence of CH3COO-.

For test b(iv), a precipitate will form with certain cations that form insoluble silver
compounds, but because of the acidic environment, some insoluble silver salts (e.g. salts
containing CO32-, S2-, and PO43- ions) are being destroyed. Hence, the solution formed
remained colourless as carbonate ions present cannot react with the silver ions and
insoluble silver salts did not form. Cl -, Br-, and I- form insoluble compounds when reacts with
silver ions but since there is no any precipitate formed hence Cl-, Br-, and I-  is absent.

For test b(vi), the yellow solution turned orange after the dilute hydrochloric acid is
added (refer Figure 5). It did not form precipitate which indicated the absence of Pb 2+. The
solution turned yellow because of the reaction of H + present in the dilute hydrochloric acid
2−

which shown by equation: 2 Cr O 24 − +2 H +¿→ C r O 2 7 +H 2 O ¿

.

For test b(v), b(vii) and b(viii), there are no reaction occur as the solution remained
colourless which indicated the absence of Pb2+.

Hence, the anion present in the given salt is carbonate (CO 3-) and cation is calcium
(Ca2+). The salt is calcium (II) carbonate.

Reference:
8.2 Qualitative analysis of salts. (n.d.). Retrieved September 18, 2020, from
http://onelearningsolution.blogspot.com/2015/02/82-qualitative-analysis-of-salts.html

Birk, J. P. (2020, August 15). Characteristic Reactions of Lead Ions (Pb²⁺). Retrieved
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https://chem.libretexts.org/Bookshelves/Analytical_Chemistry/Supplemental_Modules
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Characteristic_Reactions_of_Select_Metal_Ions/
Characteristic_Reactions_of_Lead_Ions_%28Pb%C2%B2%E2%81%BA%29

Brown, T. L., LeMay, H. E., & Bursten, B. E. (2006). Chemistry: The central science (10th
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Attachment:
 Figure 1
KA2 at the left is fine and microcrystalline powder.
KA1 at the right is crystalline salt.

Figure 2
White precipitate formed after heating (KA1, test (a))
 Figure 3
Light brown solution turned reddish-brown indicated the presence of acetate ions in
KA1, test b(iii)

Figure 4
Yellow precipitate formed indicated the presence of Pb2+ in KA1, test b (viii)

Figure5
Yellow solution turned orange after the dilute hydrochloric acid is added indicated the
absence of Pb2+ in KA2, test b (vi)