Preparation of Salts

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Preparation of Salts

Monosodium glutamate, or MSG, is the sodium salt of glutamic acid.

Glutamic acid is a non-essential amino acid, and is found naturally. MSG
can be found in almost all foods out on the shelves in supermarkets, from
instant noodles, to tomato sauce and canned beans.

Some foods profess to contain no MSG, but in actual fact, can be found in other forms, e.g., autolysed yeast extract.
Some other names which MSG goes under includes monopotassium glutamate (in which the sodium ion is replaced by
the potassium ion), glutavene, glutacyl, glutamic acid (often, supposedly "MSG-free" foods will contain this, and another
sodium salt, which will give us MSG), calcium caseinate, sodium caseinate, or E620-E625.

how true is this?

Learning Outcomes
1. Describe the techniques used in the preparation, separation and purification of salts.
2. Recall the general rules of solubility of common salts.
3. Suggest methods of preparing a given salt using suitable materials, given appropriate information.

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 Preparation of Salts

1. What are Salts?

 Recall: Salts are ionic compounds formed by replacing one or more hydrogen ions of an acid
with a metallic ion or an ammonium ion (NH4+).

metallic ion replaces H+ of acid

NaOH(aq) + HCl(aq)  NaCl(aq) + H2O(l)

acid salt

 By analysing the anion, we can deduce the acid that is used to make the salt.

Table 1.1 Salts and their originating acids

Acids Name of Salt Ions present Formula of Salt
Hydrochloric acid Ammonium chloride NH4+, Cl NH4Cl
HCl Magnesium chloride Mg2+, Cl MgCl2
Sodium chloride Na+, Cl NaCl
Nitric acid Silver nitrate Ag+, NO3 AgNO3
HNO3 Lead(II) nitrate Pb2+, NO3 Pb(NO3)2
Potassium nitrate K+, NO3 KNO3
Ammonium nitrate NH4+, NO3 NH4NO3
Sulfuric acid Sodium sulfate Na+, SO42 Na2SO4
H2SO4 Aluminium sulfate Al3+, SO42 Al2(SO4)3
Sulfurous acid Sodium sulfite Na+, SO32 Na2SO3
H2SO3
Carbonic acid Calcium carbonate Ca2+, CO32 CaCO3
H2CO3 Copper(II) carbonate Cu3+, CO32 CuCO3

2. Hydrated Salts

 Salt crystals are often formed by crystallisation from aqueous solutions, and thus often have
water molecules bonded to them. This water is known as water of crystallisation.

 Salts that contain water of crystallisation are known as hydrated salts.

 Heating a hydrated salt drives away the water, leaving the anhydrous salt.

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 Preparation of Salts

(1) Copper(II) sulfate

CuSO4.5H2O(s) CuSO4(s) + 5H2O(g)

hydrated copper(II) sulfate, also anhydrous copper(II) sulfate water vapour

known as copper(II) sulfate
pentahydrate

blue crystalline powder white powder water of

crystallisation
lost as water
vapour

(2) Cobalt(II) chloride

CoCl2.6H2O(s) CoCl2(s) + 6H2O(g)

hydrated cobalt() chloride, anhydrous cobalt(II) chloride water vapour

also known as cobalt(II)
chloride hexahydrate

pink blue water of

crystallisation
lost as water
vapour

 
Use: We use anhydrous cobalt(II) chloride paper to test for water. Water turns anhydrous cobalt(II)
chloride paper from blue to pink.

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 Preparation of Salts

3. Preparation of Salts

 Recall: Solubility table.

Table 3.1 Solubility table

Compounds Remarks
Na+, K+, NH4+ compounds All are soluble
Nitrates (NO3) All are soluble
Chlorides (Cl) All are soluble except AgCl, PbCl2
Sulfates (SO42) All are soluble except PbSO4, BaSO4, CaSO4
Carbonates (CO32) All are insoluble except those of Na+, K+, NH4+
Lead(II) compounds All are insoluble except Pb(NO3)2
Hydroxides (OH) All are insoluble except those of Na+, K+

 The method of preparation depends on three factors:

(1) Solubility of the salt.
(2) Reactivity of the metal.
(3) Chemicals being reacted together to make the salt.

Figure 3.1 Flowchart for salt preparation method

 The key to the salt preparation method is to use the simplest reactions and recovery processes
to obtain the salt.

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 Preparation of Salts

3.1 Preparation of Insoluble Salt

 Insoluble salts can be prepared by precipitation. Because the salt is insoluble, we will start
with two aqueous solutions (soluble) to produce the insoluble salt, which can be obtained by
doing a simple filtration, e.g.,

Preparation of barium sulfate, an insoluble salt

Step 1 Barium sulfate, BaSO4, is insoluble in water  use

Identify solubility of salt precipitation

Step 2 BaSO4 contains the sulfate anion  use sulfuric acid,

Identify acid to be used H2SO4

Step 3 We will need to replace the H+ in sulfuric acid with Ba2+.

Identify the other reactant
Because the salt that we want (BaSO4) is insoluble in
water, we must ensure that at the end of the reaction,
there is only one insoluble compound, BaSO4.

Hence, we can choose barium chloride, BaCl2(aq)

Step 4
Prepare the salt by following the steps

BaCl2 H2SO4
ppt: BaSO4

(1) Add excess BaCl2(aq) with 100 cm3 of dilute H2SO4(aq) until no more precipitate (ppt)
forms.
(2) The resulting mixture is filtered to obtain the precipitate in the filter paper.
(3) The precipitate is washed with a small volume of cold distilled water to remove any
impurities present.
(4) The precipitate is pressed dried between sheets of filter paper, and left to dry.

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 Preparation of Salts

Chemical equation:

Ionic equation for the formation of the ppt:

Checkpoint 1

Suggest the two reactants that can be used to produce the following salts:
a) Silver chloride, AgCl

b) Lead(II) sulfate, PbSO4

c) Lead(II) chloride, PbCl2

d) Calcium sulfate, CaSO4

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 Preparation of Salts

3.2 Preparation of Soluble Salts

 There are a few ways to prepare a soluble salt:

(1) Reacting an acid with a metal - however, note that we must never use reactive metals (e.g.,
Na, K) in the reaction as it will be explosive.
(2) Reacting an acid with an insoluble base.
(3) Reacting an acid with an insoluble carbonate.
(4) Reacting an acid and an alkali (i.e., a soluble base) via titration

(1) Reacting an acid with a metal

 Only moderately reactive metals such as zinc and magnesium are suitable for this method, e.g.,

Preparation of zinc sulfate, a soluble salt

Step 1 Zinc sulfate, ZnSO4, is soluble in water

Identify solubility of salt

Step 2 ZnSO4 contains Zn2+, which can be derived from Zn

Identify method of preparation metal. Zinc is a moderately reactive metal.

SO42- can be derived from H2SO4.

Hence, an acid-metal reaction will be used.

Step 3
Prepare the salt by following the steps

(1) Add excess Zn powder to a warm dilute H2SO4(aq). This will ensure that all the acid has
reacted.

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 Preparation of Salts

(2) Remove the excess unreacted Zn by filtration. ZnSO4 is obtained in the filtrate.

Zn(s) + H2SO4(aq)  ZnSO4(aq) + H2(g)

(3) The filtrate is heated to evaporate off excess water. The solution is heated until it is
saturated.
(4) The saturated solution is allowed to cool and crystals of ZnSO4 will form.

(5) The ZnSO4 crystals are filtered off an recovered as residue in the filter paper.
(6) Wash the crystals with a small volume of cold distilled water.
(7) The crystals are then pressed dry between sheets of filter paper and left to dry.

Chemical equation: Zn(s) + H2SO4(aq)  ZnSO4(aq) + H2(g)

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 Preparation of Salts

Checkpoint 2

Why are the crystals not heated to dryness in an oven?

(2) Reacting an acid with an insoluble base

 Most metal oxides (base) are insoluble in water.

 We can still use them to prepare soluble salts by reacting them with acids, e.g.,

CuO(s) + H2SO4(aq)  CuSO4(aq) + H2O(l)

 The same method of preparation as (1) acid-metal preparation, is used.

(3) Reacting an acid with an insoluble carbonate

 Most carbonates are insoluble in water.

 We can still use them to prepare soluble salts by reacting them with acids, e.g.,

CuCO3(s) + H2SO4(aq)  CuSO4(aq) + H2O(l) + CO2(g)

 The same method of preparation as (1) acid-metal preparation, is used.

 Effervescence is observed during the reaction, with CO2 released. We know the carbonate is in
excess when no more effervescence is observed; or when excess carbonate is seen in the
mixture.

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 Preparation of Salts

(4) Reacting an acid with an alkali - via titration

 We can prepare a soluble salt by reacting an acid with an alkali. However, because both
reactants are usually colourless, and the products are also colourless and soluble in water, we
have no way of determining when all the acid has completely reacted with all the alkali. Hence,
we use titration.

Preparation of sodium sulfate, a soluble salt

Step 1 Sodium sulfate, Na2SO4, is soluble in water

Identify solubility of salt
Step 2
Identify method of preparation
Na2SO4 contains the sulfate anion  use sulfuric acid,
The Na+ ion cannot be obtained by reacting Na with
H2SO4. Na is too reactive and reaction will be explosive
and dangerous  we use a reactant containing Na+.

We use NaOH(aq), an alkali.

Step 3
Prepare the salt by following the steps

(1) Using a pipette, transfer 25.0 cm3 of dilute H2SO4(aq) into a clean conical flask.
(2) Add 2-3 drops of methyl orange indicator. Methyl orange turns red in acid, but yellow in
alkali.
(3) Fill a burette with NaOH(aq). Release the alkali into the conical flask slowly, swirling the
conical flask at the same time.
(4) Continue until 1 drop of the alkali turns the indicator from red to yellow-orange. This is the
end-point.
(5) Read the volume of acid used from the burette.
(6) Repeat steps 1 to 5, but do not add indicator now.
(7) The resulting solution in the conical flask will contain Na2SO4(aq) and water.
(8) The solution is heated to evaporate off excess water or until it is saturated.

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 Preparation of Salts

(9) The saturated solution is allowed to cool and crystals of Na2SO4 will form.
(10) The crystals are filtered off and collected as residue on the filter paper.
(11) Wash the crystals with a small volume of cold distilled water.
(12) The crystals are pressed dried between sheets of filter paper and left to dry.

Chemical equation:

Checkpoint 3

1. We do not need to use an indicator when we use acid-metal, acid-carbonate or acid-oxide

reactions to prepare soluble salts. Give a reason why.

2. Each of the following substances react together to produce a salt:

i. Copper(II) oxide and dilute hydrochloric acid

ii. Aqueous barium nitrate and aqueous sodium sulfate
iii. Aqueous sodium hydroxide and dilute nitric acid
iv. Calcium carbonate and dilute nitric acid
v. Dilute sulfuric acid and aqueous lead(II) nitrate

a) Give the formula of each salt formed.

b) Which salt must be prepared by titration?
c) Which salt is prepared by precipitation?
d) Write a balanced chemical equation for each reaction

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 Preparation of Salts

3. Which of the following pairs of aqueous reagents is not suitable for preparing insoluble salts?
A. Sulfuric acid and calcium chloride.
B. Aluminium chloride and silver nitrate.
C. Lithium carbonate and iron(II) sulfate.
D. Barium hydroxide and copper(II) sulfate.

4. Which of the following methods is most suitable for preparing potassium chloride?
A. Add excess potassium metal to hydrochloric acid.
B. Add excess solid potassium carbonate to hydrochloric acid.
C. Add equal volumes of aqueous potassium nitrate and aqueous sodium chloride together.
D. Add equal volumes of 0.1 mol dm3 potassium hydroxide and 0.1 mol dm3 hydrochloric acid
together.

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 Preparation of Salts

4. Uses of Salts

 Some uses of salts are listed below:

Table 4.1 Uses of salts

Name of Salt Formula Use
Ammonium nitrate NH4NO3 Nitrogenous fertiliser
Barium sulfate BaSO4 X-ray meals in hospital
Lead(II) chromate(VI) PbCrO4 Yellow paint for lines on road
Silver bromide AgBr Photographic films and emulsions
Magnesium sulfate MgSO4 Epsom salts
Zinc sulfide ZnS Luminous paints
Tin(II) fluoride SnF2 Toothpaste
Calcium sulfate CaSO4 Plaster of Paris, to make casts for broken limbs

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