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Inorganic Chemistry Qualitative Analysis Guide

This document provides procedures for identifying common cations and anions through simple chemical tests. For cations, hydroxides are precipitated using sodium hydroxide or ammonium hydroxide, allowing identification based on color, solubility and other properties. Common cations that can be identified include aluminum, ammonium, calcium, chromium, copper, iron, manganese and zinc. Chemical tests for anions involve the precipitation of chloride, bromide, iodide or carbonate ions using silver nitrate and other reagents. Notes are provided on interpreting results and edge cases. A related YouTube video demonstrates several cation identification tests.

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0% found this document useful (0 votes)
120 views13 pages

Inorganic Chemistry Qualitative Analysis Guide

This document provides procedures for identifying common cations and anions through simple chemical tests. For cations, hydroxides are precipitated using sodium hydroxide or ammonium hydroxide, allowing identification based on color, solubility and other properties. Common cations that can be identified include aluminum, ammonium, calcium, chromium, copper, iron, manganese and zinc. Chemical tests for anions involve the precipitation of chloride, bromide, iodide or carbonate ions using silver nitrate and other reagents. Notes are provided on interpreting results and edge cases. A related YouTube video demonstrates several cation identification tests.

Uploaded by

Timothy Handoko
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd

CATHOLIC JUNIOR COLLEGE

H2 CHEMISTRY 9729

2019 PRACTICAL HANDBOOK – Part 6


Content
Page
10 Inorganic Chemistry
Inorganic Qualitative Analysis
10.1 Identification of Cations 2
10.2 Identification of Anions 4
10.3 Confirmatory test for Gases 6
10.4 Solubility of Salts in Water 7
10.5 Reappearing of Precipitate on adding acid 8
10.6 Techniques and Recording 10
10.7 Safety Precautions 13

Page 1
10 Inorganic Chemistry

10.1 Identification of Cations

Simple chemical tests to identify Cations:

Procedures for chemical test


Test for Add NaOH(aq) dropwise to 1 cm3 of unknown Add NH3(aq) dropwise to 1 cm3 of unknown
Cations solution till excess. Shake well after adding solution till excess. Shake well after adding
each drop of NaOH(aq). each drop of NH3(aq).
White ppt of Al(OH)3 is observed.
Al3+(aq) + 3OH- → Al(OH)3(s) White ppt of Al(OH)3 is observed.

aluminium,
White ppt of Al(OH)3 is soluble in excess White ppt of Al(OH)3 is insoluble in excess
Al3+(aq)
NaOH(aq) to form a colourless solution of NH3(aq).
Al(OH)4–(aq). Al3+(aq) + 3OH- → Al(OH)3(s)
Al(OH)3(s) + OH- → [Al(OH)4]-(aq)
No ppt is observed.
ammonium, Ammonia, NH3 is produced on heating.
NOT APPLICABLE
NH4+ (aq) NH3(g) turns moist red litmus paper blue.
NH4+ + OH- → NH3 + H2O
barium, No ppt is observed. No ppt is observed.
Ba2+(aq)
White ppt of Ca(OH)2 is observed.

calcium, No ppt is observed.


White ppt of Ca(OH)2 is insoluble in excess
Ca2+(aq)
NaOH(aq).
Ca2+(aq) + 2OH- → Ca(OH)2(s)
Grey-green ppt of Cr(OH)3 is observed.
Grey-green ppt of Cr(OH)3 is observed.
Cr3+(aq) + 3OH- → Cr(OH)3(s)
chromium(III), Grey-green ppt of Cr(OH)3 is insoluble in
Grey-green ppt of Cr(OH)3 is soluble in
Cr3+(aq) excess NH3(aq).
excess NaOH(aq) to form a dark green
Cr3+(aq) + 3OH- → Cr(OH)3(s)
solution of Cr(OH)63-(aq).
Cr(OH)3(s) + 3OH- → [Cr(OH)6]3-(aq)
Blue ppt of Cu(OH)2 is observed.
Cu2+(aq) + 2OH- → Cu(OH)2(s)
Blue ppt of Cu(OH)2 is observed.

Blue ppt of Cu(OH)2 is insoluble in


copper(II) Blue ppt Cu(OH)2 is insoluble in excess
excess NH3(aq) to form a dark blue
Cu2+(aq), NaOH(aq).
solution.
Cu2+(aq) + 2OH- → Cu(OH)2(s)
Cu(OH)2(s) + 4NH3(aq)
→ [Cu(NH3)4]2+(aq) + 2OH-(aq)

Page 2
Green ppt of Fe(OH)2 is observed. It turns
Green ppt of Fe(OH)2 is observed. It turns to
to red-brown ppt of Fe(OH)3 on contact
red-brown ppt of Fe(OH)3 on contact with air.
with air.
iron(II),
Fe2+(aq) Green ppt of Fe(OH)2 is insoluble in excess
Green ppt of Fe(OH)2 is insoluble in
NaOH(aq).
excess NH3(aq)
Fe2+(aq) + 2OH- → Fe(OH)2(s)
Fe2+(aq) + 2OH- → Fe(OH)2(s)
Red-brown ppt of Fe(OH)3 is observed. Red-brown ppt of Fe(OH)3 is observed.

iron(III), Red-brown ppt of Fe(OH)3 is insoluble in Red-brown ppt of Fe(OH)3 is insoluble in


Fe3+(aq) excess NaOH(aq). excess NH3(aq).
3+ -
Fe (aq) + 3OH → Fe(OH)3(s) Fe3+(aq) + 3OH- → Fe(OH)3(s)

Off-white ppt of Mn(OH)2 is observed. Off-white ppt of Mn(OH)2 is observed.


Mn2+(aq) + 2OH- → Mn(OH)2(s) Mn2+(aq) + 2OH- → Mn(OH)2(s)

manganese(II), It turns to brown ppt of Mn(OH)3 rapidly on It turns to brown ppt of Mn(OH)3 rapidly on
Mn2+(aq) contact with air. contact with air.

Off-white ppt of Mn(OH)2 is insoluble in Off-white ppt of Mn(OH)2 is insoluble in


excess NaOH(aq). excess NH3(aq).
White ppt of Zn(OH)2 is observed. White ppt of Zn(OH)2 is observed.
Zn2+(aq) + 2OH- → Zn(OH)2(s) Zn2+(aq) + 2OH- → Zn(OH)2(s)

zinc, White ppt of Zn(OH)2 is soluble in excess White ppt of Zn(OH)2 is soluble in excess
Zn2+(aq) NaOH(aq) to form a colourless solution. NH3(aq) to form a colourless solution.
Zn(OH)2(s) + 2OH- → [Zn(OH)4]2-(aq) Zn(OH)2(s) + 4NH3(aq)
→ [Zn(NH3)4]2+(aq) + 2OH-(aq)

Points to note:
 NaOH is a precipitating agent by supplying high concentration of OH- as it is a strong base,
fully ionised in solution (NaOH → Na+ + OH-). So those insoluble hydroxides with low Ksp will
be normally be precipitated.
 NH3(aq) is also a precipitating agent by supplying lower concentration of OH- as it is a weak
base, only partially ionised in solution (NH3 + H2O NH4+ + OH-). So those insoluble
hydroxides with low Ksp will be normally be precipitated. In addition, NH3(aq) can also act as
ligands in the formation of coloured complex ions.
 Transition metal cations are easily identified as they give coloured precipitates.
 All ammonium salts react with NaOH(aq) to give NH3 gas.
 If no ppt is observed, possible cations present are either
 H+ (use Na2CO3 to confirm) OR
 NH4+ (warm with NaOH(aq) to test for NH3(g)) OR
+ +
 Group 1 metal ions, e.g. Na , K OR
2+
 Ba (although usually it will form a white Ba(OH)2 suspension due to impurities)

Qualitative Analysis | Test for Cations


[Link]
Duration: 4:21 min
This video shows: Zn2+, Al3+, Pb2+ (not in syllabus), Ca2+, Fe2+, Fe3+, Cu2+, NH4+

Page 3
10.2 Identification of Anions
Simple chemical tests to identify Anions:
Chemical Test
Test for Anions
Procedures Observations
Effervescence observed.
Add 2 cm3 dilute acid to 1 cm3 of CO32-(aq) + 2H+(aq) → CO2(g) + H2O(l)
carbonate,
unknown solution.
CO32-(aq)
CO2 gas evolved forms a white ppt of
CaCO3 with Ca(OH)2(aq) / limewater.
White ppt of AgCl is formed.
Ag+(aq) + Cl-(aq) → AgCl(s)
chloride,
Cl-(aq) White ppt of AgCl is soluble in excess
NH3(aq) to form a colourless solution
AgCl(s) + 2NH3(aq) → [Ag(NH3)2]+(aq)
Add AgNO3(aq) to 1 cm3 of unknown Cream ppt of AgBr is formed.
bromide, solution dropwise, followed by excess Cream ppt of AgBr is insoluble in excess
Br-(aq) NH3(aq). NH3.
The ppt dissolves in conc. NH3.
Yellow ppt of AgI is formed.
iodide,
Yellow ppt of AgI is insoluble in excess
I-(aq)
NH3(aq).
3 3
Add 2 cm NaOH(aq) to 1 cm of unknown Effervescence observed upon heating with
solution. Al.

Then add Devarda’s alloy (mixture of Al NH3 gas evolved does not turn moist red
nitrate,
and Zn) or Al foil or powder to the test– litmus blue.
NO3-(aq)
tube. Warm gently.

Test the gas evolved using moist red


litmus paper at the mouth of test tube
without touching test tube.
Add 2 cm3 NaOH(aq) to 1 cm3 of unknown Effervescence observed upon heating with
solution. Al.

Then add Devarda’s alloy (Al foil or NH3 gas evolved does not turn moist red
powder) to the test–tube. Warm gently. litmus blue.

nitrite, Test the gas evolved using moist red


NO2-(aq) litmus paper at the mouth of test tube
without touching test tube.
AND/OR
AND/OR Brown fumes, NO2 evolved upon heating.
Add 1 cm3 dilute acid to 1 cm3 of Note:
unknown solution. Warm gently. NO2–(aq) liberates colourless NO gas which
oxidises to (brown) NO2 gas in air.

Test for Anions Chemical Test

Page 4
Procedures Observations
Add Ba(NO3)2(aq) dropwise to 1 cm3 of White ppt of BaSO4 is formed.
sulfate, unknown solution, followed by excess Ba2+(aq) + SO42-(aq) → BaSO4(s)
SO42-(aq) dilute acid.
White ppt of BaSO4 is insoluble in
excess dilute acid.
Add Ba(NO3)2(aq) dropwise to 1 cm3 of White ppt of BaSO3 is formed.
unknown solution, followed by excess Ba2+(aq) + SO32-(aq) → BaSO3(s)
dilute acid.
White ppt of BaSO3 is soluble in excess
sulfite, Test the gas evolved using paper strip dilute acid to form a colourless solution
SO32-(aq) dipped into purple acidified KMnO4(aq) at of Ba2+(aq).
the mouth of test tube without touching test SO32-(s) + 2H+(aq) → SO2(g) + H2O(l)
tube.
SO2 gas evolved decolourises purple
KMnO4.

Qualitative Analysis | Test for Anions


[Link]
Duration: 3 min

Note: In the video, lead(II) nitrate was used to test for the presence of iodide ions. Hence the
yellow ppt has a very intense colour. If silver nitrate was used, the yellow ppt is a lot paler.

Page 5
10.3 Confirmatory test for Gases: Simple chemical tests to identify gases:
Gas Test Observation Video
Experiment - Testing for Hydrogen
H2 gas evolved gives a Gas
H2 lighted or [Link]
‘pop’ sound with a
(neutral) burning splint
lighted splint.

Testing for Gas - Oxygen Gas


O2 gas evolved [Link]
glowing splint rekindles the glowing
O2 splint.
(neutral)
Note: O2 gas is usually accompanied by other gases. E.g.
 NO3– salt (solid) gives NO2 and O2 gas
 XO3– salt (solid) gives X2 and O2 gas (X is Cl, Br, I)
Testing for gas Carbon Dioxide
[Link]
(via delivery tube method)
CO2 gas evolved forms
a white ppt of CaCO3
CO2 1 cm3 to 2 cm3 of with Ca(OH)2.
(acidic) Ca(OH)2(aq) Test for Carbon Dioxide by Dropper
(Note: White ppt Method
dissolves with excess [Link]
CO2.)

Testing for gas - Ammonia gas


[Link]
NH3 moist red litmus NH3 gas evolved turns
moist red litmus
(alkaline) paper
paper blue.

Testing for gas sulphur dioxide gas


Use filter paper [Link]
SO2 gas evolved
strip dipped into
SO2 decolourises purple
purple acidified
(acidic) KMnO4.
KMnO4(aq)

2MnO4-(aq) + 5SO2(g) + 2H2O(l) → 2Mn2+(aq) + 5SO42-(aq) + 4H+(aq)


Testing for gas - chlorine gas
Greenish yellow Cl2 gas [Link]
Cl2
moist blue evolved turns moist
(greenish
litmus paper blue litmus paper red
yellow gas)
and then bleached it.

Reddish brown Br2 gas


Br2
moist blue evolved turns moist
(reddish brown
litmus paper blue litmus paper red
gas/liquid)
and then bleached it.
I2
Purple I2 gas evolved
(Purple gas starch iodide
turns starch iodide
condenses to a paper
paper blue-black.
black crystals)

Page 6
10.4 Solubility of Salts in water

Salt Solubility

Carbonate , CO32– All are insoluble except those of Na+, K+ and NH4+

Hydroxide , OH– All are insoluble except those of Na+, K+ and NH4+

Chloride , Cl– All are soluble except PbCl2 and AgCl

Iodide , I– All are soluble except PbI2; and AgI

Sulfate , SO42– All are soluble except PbSO4 and BaSO4

Nitrate , NO3– All are soluble


Sodium, Na+, Potassium, K+
All are soluble
& Ammonium, NH4+

Page 7
10.5 Reappearing of Precipitate on adding acid.

An example of a Qualitative Analysis question that involves reappearing of precipitate by adding


acid to solution of soluble complexes

Example
FA 7 containing two cations were reacted with excess NaOH and followed by a filtration.
Dilute sulfuric acid was added to the filtrate.

Tests Observations Deductions


2+
(a) Add aqueous sodium Off-white ppt formed. ppt is Mn ions present.
hydroxide to FA 7. insoluble in excess NaOH (aq). Mn(OH)2 ppt oxidised to
form brown Mn(OH)3 .
Filter the mixture obtained. Ppt turned brown of standing.
Collect the filtrate
produced and retain it for Colourless filtrate obtained.
test (b).
(b) Add dilute sulfuric acid to White ppt formed. Al(OH)3 or Zn(OH)2 ppt
the filtrate from (a). may be formed.
Ppt is soluble in excess Al3+ or Zn2+ ions may be
H2SO4(aq) to form a colourless present.
solution. (See equations below)

Excess NaOH is added followed by filtration and addition of H2SO4 to the filtrate:

OR

Page 8
Further tests using NH3(aq) are required to identify if the cation present is
Al3+ or Zn2+.

Tests Observations Deductions

(c) Add aqueous ammonia to Off-white ppt formed. ppt is Mn2+ ions present.
FA 7. insoluble in excess NH3
(aq).
Filter the mixture obtained. Mn(OH)2 ppt oxidized to
Collect the filtrate Ppt turned brown of form brown Mn(OH)3 .
produced and retain it for standing.
test (b). Mn2+ ions present
Colourless filtrate obtained.

(d) Add dilute sulfuric acid to White ppt formed. ppt is Zn(OH)2 ppt is formed.
the filtrate from (c). soluble in excess excess
H2SO4(aq) to form a Zn2+ ions is present.
colourless solution.

Deductions:
 Zn2+ is present if the ppt reappears when dilute acid is added because Zn(NH3)42+ is
formed
 Al3+ is present if no ppt reappears when dilute acid is added because Al(OH)3 is not
soluble in excess NH3(aq).

Chemical reactions:

Page 9
10.6 Techniques & Recording

1 Techniques
(A) Handling reagents

1. Put on safety googles at all times when handling reagents, especially during heating.
2. Read the label before use.
3. It is essential that all reagents are free from contamination - hold the reagent bottle
such that the mouth of the dropper is just above the mouth of the test tube (not
touching!) and allow the reagent to drop into the test tube.
4. Should not follow instructions blindly.
 Think about nature of reagent being used and what is a positive test (e.g. ppt
formed or ppt formed soluble in excess or NH3 gas evolved),
 Be prepared to test for any gases that may be produced before adding the
reagent.

(B) Preparation of solution


1. Unless specified, use enough solid sample to cover the hemisphere of the test tube
followed by solvent to make up 2/3 test tube full of solution.
2. Stir with a clean glass rod.

(C) Filtration
 Fold your filter paper in a “fluted” manner to increase the surface area that is in contact
with your filtrate. This allows the filtration process to be faster.

How to Make Fluted Filter Paper


[Link]
Duration 1:21 min

 Filtrate must be clear (either colourless or coloured). If not clear, filter again.
 Filter into a fairly dry test tube.
 Do not shake the filtrate upon addition (slowly) of reagent in order to observe the
appearance of ppt, if any.
 Continue with the addition of the reagent to the filtrate to confirm the solubility of the ppt
in excess.

(D) Lighting a bunsen burner


 Close air hole.
 Turn on gas tap.
 Light.
 Adjust gas tap to required rate.
 Adjust air hole.

Page 10
(E) Warming

1. For heating liquid sample, use about '1.5 cm depth' of liquid sample.
2. For heating liquid sample, heat gently at the meniscus of the solution, move the test
tube left and right to distribute the heat evenly and to avoid spurting of the solution.
3. For testing of gas during heating or warming of solution using litmus paper, do not let
the litmus paper or any other filter paper touched the test tube.
4. Warming using delivery tube to test for gases:
 Fix delivery tube to the test-tube
 Heat the test-tube.
 Submerge delivery tube into test
solution while still heating.
To stop
 Remove test solution.
 Remove tube from flame.

(F) Heating Solid Sample


 Use dry test tube.
 Point mouth of test tube away from other people.
 For heating solid salt, use about 1.5 cm depth of
solid sample. Test tube should be held in an almost
horizontal position and heat should be applied gently
initially to the whole length of tube and both sides
(to prevent condensation of water vapour on cold
parts of the test tube and subsequently cracking of
test tube).
 Heat the sample strongly, continue heating even if the sample appears to have melted
(especially hydrated salt)

1.3.3 Heating of a solid sample


[Link]
(Yishun JC, 2014)

Page 11
2 Recording

(G) Observations
1. All observations should be useful in determining the anion or cation present or absent.
2. Do not record observations that are not necessary – e.g. ‘solution turns warm when
heated’ is redundant.
3. If ppt is expected to be formed, record as:
 ‘(colour) ppt formed’ or ‘no ppt formed’
 If ppt expected cannot be clearly observed, mixture can be left aside for a while
to allow ppt to settle to bottom of test tube.
4. If ppt formed can be soluble in excess reagent added, (e.g. in aqueous NaOH, NH3,
H2SO4 ) record as:
 ‘(colour) ppt formed soluble in excess of (name of reagent added) to give colour
of solution’
 ‘(colour) ppt formed insoluble in excess of (name of reagent added)’
5. If gas is expected to be evolved from a solution, observation to be recorded as
‘effervescence evolved which (test for gas, if any)’.

If gas is evolved from heating of solid, the term ‘fume’ or gas’ should be used instead of
‘effervescence’.)
6. Do not use term such as milky, chalky or limewater.
7. Be aware of possibility of more than one coloured ion.

(H) Evidences and Deductions


1. Deductions are to be written either next to observations or under the evidence section.
2. Deductions must be specific!
Suppose unknown substance W given is stated to be a compound and you found that
copper(II) ions is present in W:
 Under deductions, you may write: ‘W contains copper(II) ions / Cu2+ ions’ or ‘W is
a salt of copper(II)’.
3. If you are not required to identify the unknown, your deductions could be to state the
nature of unknown.
For example:
‘W is an acid or alkali’ or ‘W is acidic or basic in nature’. or ‘W is a reducing or oxidizing
agent’.
4. In writing evidences to support a deduction, the following should be present:
 Identity of ppt, e.g. the blue ppt formed is Cu(OH)2
 Identity of soluble complex formed, e.g. the blue ppt dissolves in excess NH3 to
give a deep blue complex [Cu(NH3)4(H2O)2]2+.
 Identity of gas evolved
 Chemical reactions involved, e.g. the H2O2 oxidised the Fe(II) to Fe(III).

Page 12
10.7 Safety Precautions

1. If acidic fumes e.g. HCl or HBr are liberated, perform the experiment in the fume cupboard
and wear goggles to protect eyes from the fumes.

2. If alkaline gas is liberated, wear goggles to protect eyes from the fumes. Take care not to
bring the mouth of test tube too close to your nose.

3. Take care when handling corrosive chemicals; e.g. concentrated acids. Wear gloves so as
to avoid direct contact.

4. Take care when handling chemicals that are “harmful/irritant” as they may cause reddening
or blistering of the skin. Avoid direct contact.

Page 13

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