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Qualitative tests for the anions CO32-, HCO3-, SO42-, 3

Using a dropping pipette add 2 cm of dilute hydrochloric acid to each


SO32-, Cl-, NO3- and PO43- in aqueous solution test tube. Record your observations in the table below.

Student Material Repeat steps 1 and 2 using the arrangement shown in the diagram.
Record your observations in the table below. Write equations for the
Theory reactions occurring in the table below.

Reactions of anions with certain reagents to produce characteristic 3


Add 2 cm of sodium carbonate solution to a clean test tube labelled C,
coloured precipitates or other easily identifiable results are 3
and 2 cm of sodium hydrogencarbonate solution to a clean test tube
employed to identify or confirm the presence of these anions in aqueous 3
labelled D. Using a dropping pipette add 2 cm of magnesium sulfate
solution and to distinguish the anions from one another. solution to each. Record your observations in the table below. Write
equations for any reactions occurring.
(a) To test for the carbonate and hydrogencarbonate
anions Carefully heat the contents of test tubes labelled C and D at the end of
the step 4. Record your observations in the table below. Write equations
for any reactions occurring.
Theory
Carbonate Hydrogencarbonate
Solutions containing hydrogencarbonate ions react with hydrochloric
Observations upon addition
acid, producing carbon dioxide gas. For example,
of HCl solution
NaHCO3 + HCl  NaCl + H2O + CO2↑
Observations and conclusion
Solutions containing carbonate ions also react with hydrochloric acid,
from limewater test
producing carbon dioxide gas. For example,
Na2CO3 + 2HCl  2NaCl + H2O + CO2↑ Equation for reaction
between the salt and HCl
It is possible to distinguish between solutions containing Observation upon addition
hydrogencarbonate ions and solutions containing carbonate ions using a of MgSO4 solution
further test. Carbonate ions in solution react with a solution containing Equation for reaction
magnesium ions, forming a precipitate of magnesium carbonate. between the salt and MgSO4
For example, Observation upon heating
Na2CO3 + MgSO4  Na2SO4 + MgCO3↓ Equation for reaction upon
No precipitate is formed when solutions containing hydrogencarbonate heating
ions are mixed with a solution of magnesium sulfate.
(b) To test for the sulfate and sulfite anions
However, if a mixture of a solution containing hydrogencarbonate ions
and a solution of magnesium sulfate is heated, a precipitate of
Theory
magnesium carbonate is formed. This is because hydrogencarbonate
Solutions containing sulfite ions react with barium chloride solution,
changes to carbonate on heating.
producing a white precipitate of barium sulfite. For example,
For example,
Na2SO3 + BaCl2 2NaCl + BaSO3↓
2NaHCO3  Na2CO3 + H2O + CO2
Na2CO3 + MgSO4  Na2SO4 + MgCO3↓
Solutions containing sulfate ions also react with barium chloride
solution, producing a white precipitate of barium sulfate For example,
Chemicals and Apparatus
Na2SO4 + BaCl2 2NaCl + BaSO4↓
 Solution of sodium carbonate
 Solution of sodium hydrogencarbonate
It is possible to distinguish between solutions containing sulfite ions and
 Deionised water
solutions containing sulfate ions using a further test. Hydrochloric acid is
 Dilute hydrochloric acid added to the white precipitates obtained using the barium chloride test.
Barium sulfite reacts and dissolves:

Limewater i BaSO3 + 2HCl  BaCl2 + H2O + SO2
 Solution of magnesium sulfate Barium sulfate does not dissolve.
 Test tubes
 Test tube rack Chemicals and Apparatus
 Test tube holder
 Stoppers for test tube fitted with plastic delivery tubing  Solution of sodium sulfate
 Labels  Solution of sodium sulfite
 Bunsen burner  Deionised water
 Dropping pipettes
 Beakers  Solution of barium chloride n
 Wash bottle
 Dilute hydrochloric acid
 Test tubes
Procedure
 Test tube rack
 Test tube holder
 Labels
NB: Wear your safety glasses.
3  Dropping pipettes
Add 2 cm of sodium carbonate solution to a clean test tube labelled A,
3  Beakers
and 2 cm of sodium hydrogencarbonate solution to a clean test tube
 Wash bottle
labelled B.

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3
Add 2 cm of dilute ammonia solution to the contents of the test tubes
Procedure at the end of the step 3. Record your observations in the table below.

NB: Wear your safety glasses.


Chloride
3
Add 2 cm of sodium sulfate solution to a Observations upon addition of
3
clean test tube labelled A and 2 cm of AgNO3 solution
sodium sulfite solution to a clean test tube Equation for reaction between the
labelled B. Using a dropping pipette add 1 salt and AgNO3
3
cm of barium chloride solution to each. Observation upon addition of NH3
Record your observations in the table solution
below. Write equations for any reactions
occurring.
3 (d) To test for the nitrate anion
Add 2 cm of dilute hydrochloric acid to the contents of the test tubes
labelled A and B at the end of Step 1. Record your observations in the
table below. Write equations for any reactions occurring. Theory
Solutions containing nitrate ions react with a mixture of iron(II) sulfate
solution and concentrated sulfuric acid. A brown ring develops slowly at
Sulfate Sulfite the interface of the sulfuric acid layer and the layer containing a mixture
Observation upon of nitrate and iron(II) sulfate solutions.
addition of BaCl2
solution
Equation for reaction Chemicals and Apparatus
between the salt and
BaCl2  Solution of potassium nitrate
Observation upon  Deionised water
addition of HCl  Cold saturated solution of iron(II) sulfate
solution
Equation for reaction  Concentrated sulfuric acid
upon addition of HCl
 Test tubes
 Test tube rack
 Test tube holder
 Labels
(c) To test for the chloride anion  Dropping pipettes
 Beakers
 Wash bottle
Theory
Procedure
Solutions containing chloride ions react with silver nitrate solution,
producing a white precipitate of silver chloride. For example: NB: Wear your safety glasses.
NaCl + AgNO3  NaNO3 + AgCl↓
3
This precipitate dissolves when dilute ammonia solution is added. Add 2 cm of potassium nitrate solution to a clean test tube. Using a
3
dropping pipette, add 3 cm of cold saturated iron(II) sulfate solution.
3
Chemicals and Apparatus Using a dropping pipette, carefully add 2 cm of concentrated sulfuric
acid slowly down the wall of the test tube. Do not mix the contents of
Solution of sodium chloride the test tube.
Deionised water
Solution of silver nitrate
Dilute ammonia solution

Test tubes
Test tube rack
Test tube holder
Labels
Dropping pipettes
Beakers
Wash bottle Allow the mixture to stand undisturbed for a few minutes. Record your
observations in the table below.
Procedure

NB: Wear your safety glasses. Nitrate


Observations upon addition of
3 FeSO4 solution
Add 2 cm of sodium chloride solution to a clean test tube. Using a
dropping pipette add a few drops of silver nitrate solution. Record your Observation upon addition of
observations in the table below. Write equations for any reaction concentrated H2SO4
occurring.

2
3
If no gas is evolved, take further 2 cm samples of the unknown in clean
(e) To test for the phosphate anion test tubes and test in turn with (i) barium chloride solution followed by
dilute hydrochloric acid, (ii) silver nitrate solution, (iii) cold saturated
iron(II) sulfate solution followed by concentrated sulfuric acid, and (iv)
Theory ammonium molybdate reagent, according to tests (b), (c), (d) and (e)
Solutions containing phosphate ions react on heating with an respectively, until a positive result is obtained.
ammonium molybdate reagent, forming a yellow precipitate, which
dissolves on addition of ammonia solution. Complete a results table for each unknown.
Unknown
Observations upon addition of HCl
Chemicals and Apparatus solution

 Solution of disodium hydrogen phosphate Conclusion from limewater test


 Deionised water on gas produced
Result from addition of MgSO4
 Ammonium molybdate reagent n
solution
 Dilute ammonia solution
Result from addition of BaCl2
 Warm water
solution followed by addition of
HCl solution
 Test tubes
Observation upon addition of
 Test tube rack
AgNO3 solution
 Test tube holder
 Labels Observation upon addition of
 Thermometer FeSO4 solution followed by
 Dropping pipettes concentrated H2SO4
 Beakers Observation upon addition of
 Wash bottle ammonium molybdate reagent
CONCLUSION
Procedure
Specimen Results
NB: Wear your safety glasses.
Carbonate Hydrogencarbonate
3
Add 2 cm of disodium hydrogenphosphate(V) solution to a clean test Observations upon Effervescence, Effervescence,
tube. addition of HCl colourless gas colourless gas evolved
solution evolved
3
Using a dropping pipette add approximately 6 cm of the clear Observations and Limewater Limewater becomes
ammonium molybdate reagent to the test tube. conclusion from becomes milky: CO2 milky: CO2 evolved.
limewater test evolved.
Warm gently by placing in a beaker of water at a temperature not Equation for Na2CO3 + 2HCl  NaHCO3 + HCl  NaCl +
exceeding 40 °C. Record any observations in the table below. reaction between 2NaCl + H2O + H2O + CO2↑
the salt and HCl CO2↑
Add an equal volume of ammonia solution to the contents of the test Observation upon White precipitate No change observed
tube at the end of step 2. Record your observations in the table below. addition of MgSO4 formed
solution
Equation for Na2CO3 + MgSO4  2 NaHCO3 + MgSO4 
Phosphate reaction between Na2SO4 + MgCO3↓ Na2SO4 + Mg(HCO3)2
Observations upon addition of the salt and MgSO4
ammonium molybdate reagent Observation upon No change White precipitate
and heating heating observed appears
Observations upon addition of Equation for None Mg(HCO3)2  MgCO3↓
ammonia solution reaction upon + H2O + CO2
heating

(f) To identify 'unknown' anions Sulfate Sulfite


Observation upon White precipitate White precipitate
Procedure addition of BaCl2 formed formed
solution
NB: Wear your safety glasses.
3
Add 2 cm of each unknown solution to a clean test tube labelled with Equation for reaction Na2SO4 + BaCl2  Na2SO3 + BaCl2 
the same number as the unknown sample. between the salt and 2NaCl + BaSO4↓ 2NaCl + BaSO3↓
BaCl2
3
Using a dropping pipette add 2 cm of dilute hydrochloric acid to the test Observation upon No change observed White precipitate
tube. Record any observations in the table below. addition of HCl disappears
solution
If a gas is evolved establish with limewater whether it is CO2 or not. If the Equation for reaction None BaSO3 + 2HCl 
gas is CO2, proceed to test (a) and determine whether the unknown is a upon addition of HCl BaCl2 + H2O + SO2
carbonate or a hydrogencarbonate.

3
3
Take another 2 cm sample of the mixture. Test with AgNO3 solution. If
chloride ion is present a white precipitate is formed. This precipitate
Chloride dissolves in dilute ammonia solution.
Observations upon addition of White precipitate appears
3
AgNO3 solution Take another 2 cm sample of the mixture. Test with FeSO4 solution and
Equation for reaction between NaCl + AgNO3  NaNO3 + AgCl↓ concentrated sulfuric acid. A brown ring is observed if nitrate ion is
the salt and AgNO3 present.
Observation upon addition of White precipitate dissolves 3
NH3 solution Take another 2 cm sample of the mixture. Test with ammonium
molybdate reagent. If phosphate ion is present a yellow precipitate is
formed. This precipitate dissolves in dilute ammonia solution.
3
Nitrate Take another 2 cm sample of the mixture. If there is no phosphate ion
Observations upon addition of Nothing observed present, add BaCl2 solution and a precipitate will appear if either sulfite
FeSO4 solution or sulfate is present. Add dilute hydrochloric acid dropwise. If all the
Observation upon addition of A brown ring appears at precipitate dissolves only the sulfite anion was present. If there is a
concentrated H2SO4 the boundary between mixture of sulfite and sulfate anions some of the precipitate will remain
the liquid layers but some will dissolve producing sulfur dioxide gas, which has a
distinctive smell.

Which of these anions might be expected to be found in treated tap


Phosphate
water? Give a possible source of each anion you mention.
Observations upon addition of Yellow precipitate appears
ammonium molybdate reagent
Hydrogencarbonate anion from water hardness.
and heating
Sulfate ion from flocculating agents or water hardness.
Observations upon addition of Precipitate dissolves
Chloride ion from water hardness or sterilisation treatment.
ammonia solution
How would you distinguish two unlabelled samples, one of which is a
carbonate and the other which is a hydrogencarbonate, from each
Unknown (e.g. carbonate) other?
Observations upon addition of Gas evolved
HCl solution 3
Take a 2 cm sample of each sample. Add MgSO4 solution. If a precipitate
Conclusion from limewater test CO2 forms, it confirms the carbonate anion is present. Heat the other test
on any gas evolved tube and a precipitate appears upon heating a sample with the
Result from addition of MgSO4 White precipitate formed hydrogencarbonate ion.
solution
Result from addition of BaCl2 nothing observed How would you distinguish two unlabelled samples, one of which is a
solution followed by addition of sulfate and the other which is a sulfite, from each other?
HCl solution
Observation upon addition of nothing observed 3
Take a 2 cm sample of each sample. Add BaCl2 solution and a
AgNO3 solution precipitate will appear in each test tube. Add dilute hydrochloric acid
Observation upon addition of nothing observed dropwise. If all the precipitate dissolves the sulfite anion was present. In
FeSO4 solution followed by the case of the sulfate anion, the precipitate is insoluble.
concentrated H2SO4
Observation upon addition of nothing observed Industrial, Environmental & Social Links
ammonium molybdate reagent
CONCLUSION Carbonate Industry, medicine, and environmental science are more concerned with
quantitative measurement of these anions than with just identifying
student questions their presence.

Describe the appearance of pure samples of each of the following salts: Simple home soil test kits are an application of these types of test to
sodium carbonate, sodium hydrogencarbonate, sodium sulfate, sodium establish the presence of nitrogen, phosphorus and the cation potassium
sulfite, sodium chloride, sodium nitrate, disodium hydrogen phosphate. in soil extract and crudely estimate the quantity present.
They are all white crystalline solids. The samples used in the experiment
are aqueous solutions of the salts.

Explain the steps you would take to identify which of these anions are
present in a mixture of salts.
3
Take a 2 cm sample of the mixture. Add dilute hydrochloric acid solution
and collect any gas evolved and test with limewater. If carbon dioxide
gas was evolved then either a carbonate or a hydrogencarbonate or both
anions are present.
3
Take another 2 cm sample of the mixture. Add MgSO4 solution. If a
precipitate forms, carbonate anion is present. Filter off the precipitate
and heat. If further precipitate appears after heating,
hydrogencarbonate ion is also present.

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