Qualitative Analysis Theory - E

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1
CHEMISTRY
QualitativeAnalysis
Introduction :
Qualitative analysis involves the detection of cation(s) and anion(s) of a salt or a mixture of salts.
The systematic procedure for qualitative analysis of an inorganic salt involves the following steps :
(a) Preliminary tests
Physical appearance (colour and smell).
Dry heating test.
Charcoal cavity test.
Charcoal cavity and cobalt nitrate test.
Flame test.
Borax bead test.
Dilute sulphuric acid test.
Potassium permanganate test.
Concentrated sulphuric acid test.
Tests for sulphate, phosphate and borate.
(b) Wet tests for acid radicals.
(c) Wet tests (group analysis) for basic radicals.
1. Physical Examination Of the Mixture :
The physical examination of the unknown mixture involves the study of colour, smell and density.
Table : 1
Physical Examination
Experiment Observations Inference
(a) Colour Blue or Bluish green Cu
2+
or Ni
2+
Greenish Ni
2+
Light green Fe
2+
Dark brown Fe
3+
Pink, violet Co
2+
Light pink, flesh colour or dull
earthy colour Mn
2+
White
Shows the absence of
Cu
2+
,Ni
2+
,Fe
2+
,Fe
3+
Mn
2+
, Co
2+
(b) Smell
Ammonical smell NH
4
+
Vinegar like smell CH
3
COO
Smell like that of rotten eggs S

2
(i) Heavy Salt of Pb
2+
or Ba
2+
(ii) Light fluffy powder Carbonate salts
(d) Deliquescence
Salt absorbs moisture and
becomes
paste like
(i) If coloured, may be
Cu(NO
3
)
2
,
FeCl
3
(ii) If colourless, may be
Zn(NO
3
)
2
, chlorides of
Zn
2+
, Mg
2+
etc.
Take a pinch of the salt between
your fingers and rub with a drop of
water
(.C) Density
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CHEMISTRY
2. Dry Heating Test :
This test is performed by heating a small amount of mixture in a dry test tube. Quite valuable information can
be generated by carefully performing and noting the observations here. On heating some salts undergo
decomposition thus evolving the gases or may undergo characteristic changes in the colour of residue.
These observations are tabulated belowalong with the inferences that you can draw.
Table : 2
Observation Inference
1. Gas evolved
(a) Colourless and odourless gas
CO
2
gas turns lime water milky CO
3
2
(b) Colourless gas with odour
(i) H
2
S gasSmells like rotten eggs, turns Hydrated S
2
lead acetate paper black.
(ii) SO
2
gasCharacteristic suffocating SO
3
2
smell, turns acidified potassium dichromate
solution or paper green.
(iii) HCl gas Pungent smell, white fumes with Cl
ammonia, white precipitate with silver nitrate solution.

(iv) Acetic acid vapoursCharacteristic vinegar CH
3
COO
like smell.
(v) NH
3
gas Characteristic smell, turns NH
4
+
Nessler's solution brown.
(c) Coloured gases Pungent smell
(i) NO
2
gas Reddish brown, turns ferrous NO
2
or NO
3
sulphate solution black.

(ii) Cl
2
gas Greenish yellow, turns starch Cl
iodide paper blue.

(iii) Br
2
vapours Reddish brown, turns starch Br
paper orange red.

(iv) I
2
vapours Dark violet, turns starch paper I
blue.
2. Sublimate formed
(a) White sublimate NH
4
+
(b) Black sublimate accompanied by violet I
vapours.
3. Fusion
The mixture fuses. Alkali metal salts or salt containing water of
crystallisation.
4. Swelling
The mixture swells up into voluminous mass. PO
4
3
, BO
3
3
indicated
5. Residue
(i) Yellow when hot, white when cold. Zn
2+
(ii) Brown when hot and yellowwhen cold Pb
2+
(iii) Original salt blue becomes white on heating Hydrated CuSO
4
indicated
(iv) Coloured salt becomes brown or black on Co
2+
, Fe
2+
, Fe
3+
, Cr
3+
, Cu
2+
, Ni
2+
, Mn
2+
heating. indicated.
Note :
Use a perfectly dry testtube for performing this test. While drying a testtube, keeps it in slanting
position with its mouth slightly downwards so that the drops of water which condense on the upper
cooler parts, do not fall back on the hot bottom, as this may break the tube.
3
CHEMISTRY
For testing a gas, a filter paper strip dipped in the appropriate reagent is brought near the mouth of
the test tube or alternatively the reagent is taken in a gasdetector and the gas is passed through it.
Figure : Detection of gas evolved.
Do not heat the tube strongly at one point as it may break.

3. Charcoal Cavity Test :
This test is based on the fact that metallic carbonates when heated in a charcoal cavity decompose to give
corresponding oxides. The oxides appear as coloured incrustation or residue in the cavity . In certain cases,
the oxides formed partially undergo reduction to the metallic state producing metallic beads or scales.
Example :
(a) ZnSO
4
+ Na
2
CO
3
ZnCO
3
+ Na
2
SO
4
ZnCO
3
ZnO (Yellow when hot, white when cold) + CO
2
|
(b) CuSO
4
+ Na
2
CO
3
CuCO
3
+ Na
2
SO
4
CuCO
3
CuO+ CO
2
|
CuO + C Cu (Reddish scales) + CO |
Table : 3
Inference
Incrustation or Residue Metallic bead
Yellow when hot, white when cold None Zn
2+
Brown when hot, yellow when cold
Grey bead which
marks the paper
Pb
2+
No characteristic residue Red beads or scales Cu
2+
White residue which glows on heating None Ba
2+
,Ca
2+
, Mg
2+
Black None
Nothing definitegenerally
coloured salt
Observation
4. Cobalt Nitrate Test :
In case the residue is white in colour after charcoal cavity test, add a drop of cobalt nitrate in the charcoal
cavity. Adrop of water is then added and the mass is heated in an oxidising flame using blowpipe. It is cooled
and one or two drops of cobalt nitrate solution is added and then again heated in the oxidising flame. Different
metal salts give different coloured mass as given in the table. To illustrate :
ZnSO
4
+ Na
2
CO
3
ZnCO
3
+ Na
2
SO
4
; ZnCO
3
ZnO+ CO
2
2Co (NO
3
)
2
2CoO + 4 NO
2
+ O
2
; ZnO+ CoO ZnO. CoO(or CoZnO
2
)
(Rinmann's green)
4
CHEMISTRY
Table : 4
S.No. Metal Colour of the mass
1. Zinc Green
2. Aluminium Blue
3. Magnesium
Pink
Tin 4. Bluish - green
5. Flame test :
The chlorides of the metals are more volatile as compared to other salts and these are prepared in situ by
mixing the compounds with a little concentrated hydrochloric acid. On heating in a non-luminous Bunsen
flame they are volatilized and impart a characteristic colour to the flame as these absorb energy from the
flame and transmit the same as light as characteristic colour .
Table : 5
Colour of Flame Inference
Crimson Red / Carmine Red Lithium
Golden yellow Sodium
Violet/Lilac Potassium
Brick red Calcium
Crimson Strontium
Apple Green/Yellowish Green Barium
Green with a Blue centre/Greenish Blue Copper
Figure : Flame test
6. Borax Bead test :
On Heating borax forms a colourless glassy bead of NaBO
2
and B
2
O
3 .
Na
2
B
4
O
7
.10H
2
O
A
Na
2
B
4
O
7

A
2NaBO
2
+ B
2
O
3
On heating with a coloured salt , the glassy bead forms a coloured metaborate in oxidising flame.
For example, in oxidising flame copper salts give blue bead.
CuSO
4
CuO + SO
3
; CuO + B
2
O
3
Cu(BO
2
)
2
(blue bead)
However, in reducing flame the colours may be different due to different reactions.
2Cu(BO
2
)
2
+ C 2CuBO
2
+ B
2
O
3
+ CO
2Cu(BO
2
)
2
+ 2C 2Cu (brown red/red and opaque bead) + 2B
2
O
3
+ 2CO.
5
CHEMISTRY
Table : 6
When Hot When Cold When Hot When Cold
Copper Green Blue Colourless Brown red
Iron Brown yellow Pale yellow/Yellow Bottle green Bottle green
Chromium Yellow Green Green Green
Cobalt Blue Blue Blue Blue
Manganese Violet/Amethyst Red/Amethyst Grey/Colourless Grey/Colourless
Nickel Violet Brown/Reddish brown Grey Grey
Colour in oxidising flame Colour in reducing flame
Metal
Non luminous flame is called oxidising flame.

Luminous flame is called reducing flame.
Figure : Borax bead test
All acid radicals which are in JEE syllabus are colourless and diamagnetic. Hence the colour of the
salts is only due to the basic radicals.
Table : 7
SOLUBILITY CHART
S.No. Anion Solubility / Exception
1. CO
3
2
Except carbonates of alkali metals and of ammonium, all other normal carbonates
are insoluble.
2. SO
3
2
Only the sulphites of the alkali metals and of ammonium are water soluble. The
sulphite of other metals are either sparingly soluble or insoluble.
3. S
2
The acid, normal and polysulphide of alkali metals are soluble in water. The normal
sulphides of most other metals areinsoluble; thoseof thealkaline earths aresparingly
soluble, but aregraduallychangedbycontact withwater intosolublehydrogensulphides.
4. NO
2
, NO
3
Almost all nitrites and nitrates are solublein water. AgNO

2
sparingly soluble. Nitrates
of mercury and bismuth give basic salts on treatment with water. These are soluble
in dilute nitric acid.
5. CH
3
COO
Acetates are water soluble except Ag(I) and Hg(II) acetates which are sparingly
soluble.
6. Cl
Most chlorides are soluble in water. PbCl

2
(sparingly soluble in cold but readily
solubleinboilingwater), Hg
2
Cl
2
, AgCl, CuCl, BiOCl, SbOCl andHg
2
OCl
2
areinsoluble
in water.
7. Br
Silver, mercury(I) andcopper(I), bromidesareinsoluble. Leadbromideissparinglysoluble

in cold but more soluble in boilingwater. All other bromides aresoluble in water.
8. I
Silver, mercury(I), mercury(II), copper(I), lead and bismuth(III) iodides are the least
soluble salts. All other iodides are water soluble.
9. SO
4
2
The sulphates of barium, strontiumand lead are insoluble in water, those of calcium
and mercury(II) are slightly soluble. Some basic sulphates of mercury, bismuth and
chromiumare also insoluble, but these dissolves in dilute hydrochloric or nitric acid.
10 PO
4
3
The phosphate of the alkali metals, with the exception of lithium and ammonium,
are soluble in water ; the primary phosphate of the alkaline earth metals are soluble.
All thephosphates of theother metals andalso thesecondary and tertiary phosphate
of the alkaline earth metals are sparingly soluble or insoluble in water.
6
CHEMISTRY
Analysis of ANIONS (Acidic Radicals) :
Analysis of anions (acidic radicals) can be broadly divided in to two groups.
(A) GROUP 'A' RADICALS : It involves those anions which are characterised by volatile products by reaction
with HCl/ H
2
SO
4
It is further subdivided in to two groups as given below.
(a) Dilute Sulphuric acid/Dilute Hydrochloric acid : The anions of this group liberate gases or acid
vapours with dilute sulphuric acid/hydrochloric acid.
Table : 8
Observation
Inference
Gas Radical
Effervescence with the evolution of a colourless CO
2
CO
3
2
and odourless gas which turns lime water milky.
Evolution of colourless gas having smell of rotten
egg which turns lead acetate paper black. H
2
S S
2
Colourless gas having suffocating odour (like burning SO
2
SO
3
2
sulphur) which turns acidified K
2
Cr
2
O
7
paper green.
Evolution of reddish brown pungent smelling gas which turns
(i) FeSO
4
solution brownish-black and NO
2
NO
2
(ii) wet starch iodide paper blue.

Colourless gas having smell of vinegar. HAC(g) CH
3
COO
No peculiar gas is evolved. All above are absent

(b) Concentrated Sulphuric acid group : The anions of this group liberate acid vapours or gases with
conc. H
2
SO
4
.
Table : 9
Observation
Inference
Gas Radical
Colourless gas with pungent smell which gives dense HCl Cl
white fumes with a glass rod dipped in NH

4
OH.
Reddish brown gas with pungent smell, intensity of Br
2
Br
reddish brown fumes increases on addition of a pinch

of solid MnO
2
. Also it turns starch paper orange red.
Evolution of violet vapours which turns starch paper blue. I
2
I
Evolution of reddish brown fumes which intensifies on NO

2
NO
3
addition of copper turnings or bits of filter paper.

Starch iodide paper develops a blueblack spot
due to the formation of a I
2
starch complex.
(NO
2
liberated acts as oxidising agent).
(B) GROUP 'B' RADICALS : Anions of this group do not give acid vapours or gases with dilute as well as
concentrated H
2
SO
4
but are characterised by their specific reactions in solutions. This group is further sub
divided into two groups based on the type of the reactions.
(a) Oxidation and reduction in solutions : CrO
4
2
, Cr
2
O
7
2
etc.
(b) Precipitation reactions : These are given by SO
4
2
, PO
4
3
etc.
Table : 10
Observation Inference
W.E. or S.E. + BaCl
2
(aq)

White precipitate insoluble SO
4
2
in dil. HCl and HNO
3.
W.E or S.E + conc HNO
3
(12 mL) + PO
4
3
ammonium molybdate and boil Canary yellow precipitate
7
CHEMISTRY
W.E. = Water extract. (Salt is dissolved in distilled water)
S.E. = Sodium carbonate extract

Preparation of sodium carbonate extract :
Take 1-2 g of salt/salts mixture and three times the amount of pure solid sodium carbonate in a borosil
conical flask. Add 20 mL of distilled water and boil the contents for 10 minutes. Cool the solution and then
filter. The Filtrate is termed as "Sodium carbonate extract".
Sodium carbonate reacts with the inorganic salt to form water soluble sodium salt of the acid radical.
BaCl
2
+ Na
2
CO
3

BaCO
3
+ (white) + 2NaCl (aq)
Cd
3
(PO
4
)
2
+ 3Na
2
CO
3
3CdCO
3
+ + 2Na
3
PO
4
(aq)
Sodium carbonate extract is used when
(a) salt is only partially soluble in water or insoluble
(b) cations interfere with the tests for acid radicals or the coloured salt solutions may be too intense in colour
that the test results are not too clear.
As sodium carbonate extract contains excess of sodium carbonate, it should be neutralised with a
suitable acid before proceeding for analysis of an anion.
Figure : Preparation of sodium carbonate extract
Individual tests :
(A) GROUP 'A' RADICALS :
(a) DILUTE SULPHURIC ACID/DILUTE HYDROCHLORIC ACID GROUP :
1. CARBONATEION(CO
3
2
) :
Dilute H
2
SO
4
test : Acolourless odourless gas is evolved with brisk effervescence.
CaCO
3
+ H
2
SO
4
CaSO
4
+ H
2
O + CO
2
|
Lime water/Baryta water (Ba(OH)
2
) test : The liberated gas can be identified by its property of
rendering lime water (or baryta water) turbid.
CO
2
+ Ca(OH)
2
CaCO
3
+
(milky) + H
2
O
On prolonged passage of CO
2
the milkiness disappears.
CaCO
3
+ CO
2
+ H
2
O Ca(HCO
3
)
2
(soluble)
A
CaCO
3
+ + H
2
O+ CO
2
Magnesium sulphate test (for soluble carbonates) :
CO
3
2
(aq) + MgSO
4
(aq) MgCO
3
+ (white) + SO
4
2
(aq)
Silver nitrate solution : White precipitate is formed
CO
3
2
+Ag
+
Ag
2
CO
3
+
White precipitate is soluble in HNO
3
and ammonia. The precipitate becomes yellowor brown upon
addition of excess reagent owing to the formation of silver oxide ; the same happens if the mixture is
boiled.
Ag
2
CO
3
Ag
2
O + + CO
2
|
Phenolphthaleinis turned pink bysoluble carbonates andcolourless bysoluble hydrogencarbonates.
8
CHEMISTRY
Mercury(II) chloride does not form precipitate with hydrogen carbonate ions, while in a solution of
normal carbonates a reddishbrown precipitate of basic mercury(II) carbonate (3HgO. HgCO
3
=
Hg
4
O
3
CO
3
) is formed.
CO
3
2
+ 4 Hg
2+
+ 3 H
2
O Hg
4
O
3
CO
3
+ + 6H
+
Lime water milky test is also shown by SO
2
but CO
2
does not turn the filter paper soaked in acidified
K
2
Cr
2
O
7
green.
Soluble bicarbonates give white precipitate with MgSO
4
(aq) / MgCl
2
(aq) only on heating.
Mg
2+
+ 2HCO
3
Mg(HCO
3
)
2

A
MgCO
3
+ + H
2
O+ CO
2
Action of heat :
Bicarbonates : 2NaHCO
3
Na
2
CO
3
+ H
2
O+ CO
2
Carbonates : Except carbonates of Na, K, Rb, Cs ; the Li
2
CO
3
and all alkaline earth metals
decompose as given below:
Li
2
CO
3
Li
2
O + CO
2
; MgCO
3
MgO + CO
2
; Ag Ag
2
CO
3
2Ag + CO
2
CaCO
3

A
CaO + CO
2
2. SULPHITE ION (SO
3
2
) :
Dilute H
2
SO
4
test : Decomposition of salt is more rapidly on warming, with the evolution of sulphur
dioxide.
CaSO
3
+ H
2
SO
4
CaSO
4
+ H
2
O + SO
2
|
SO
2
has suffocating odour of burning sulphur.
Acidified potassiumdichromate test : The filter paper dipped in acidified K
2
Cr
2
O
7
turns green.
Cr
2
O
7
2
+ 2H
+
+ 3SO
2
2Cr
3+
(green) + 3SO
4
2
+ H
2
O.
Bariumchloride/Strontiumchloride solution : White precipitate of barium(or strontium) sulphite
is obtained.
SO
3
2
+ Ba
2+
/Sr
2+
BaSO
3
/SrSO
3
+ (white).
White precipitate dissolves in dilute HCl, when sulphur dioxide is evolved.
BaSO
3
+ + 2H
+
Ba
2+
+ SO
2
| + H
2
O.
White precipitate (BaSO
3
) on standing is slowly oxidised to sulphate which is insoluble in dilute
mineral acids. This change is rapidly effected by warming with bromine water, a little concentrated
nitric acid or with hydrogen peroxide.
2 BaSO
3
+ + O
2
2 BaSO
4
+
BaSO
3
+ + Br
2
+ H
2
O 2 BaSO
4
+ + 2 Br
+ 2H
+
Hence, reddish brown colour of bromine water is decolourised.
3BaSO
3
+ + 2 HNO
3
3 BaSO
4
+ + 2NO | + H
2
O
BaSO
3
+ + H
2
O
2
BaSO
4
++ H
2
O
These reactions are not given by carbonates (distinction from carbonates).
Zinc and sulphuric acid test : Hydrogen sulphide gas is evolved.
SO
3
2
+ 3Zn
2+
+ 8H
+
H
2
S | + 3Zn
2+
+ 3H
2
O
Lime water test : Awhite precipitate is formed. The precipitate dissolves on prolonged passage of
the gas, due to the formation of hydrogen sulphite ions.
Ca(OH)
2
+ SO
2
CaSO
3
+ (milky) + H
2
O
CaSO
3
+ + SO
2
+ H
2
O Ca(HSO
3
)
2
(soluble)
A turbidity is also produced by carbonates ; sulphur dioxide must therefore be first removed when
testing for the latter. This may be affected by adding potassiumdichromate solution to the testtube
before acidifying. The dichromate oxidizes and destroys the sulphur dioxide without affecting the
carbon dioxide.
Lead acetate or lead nitrate solution : White precipitate of PbSO
3
is obtained.
SO
3
2
+ Pb
2+
PbSO
3
+
White precipitate gets soluble in dil. HNO
3
on boiling. The precipitate is oxidized by atmospheric
oxygen and PbSO
4
is formed.
2PbSO
3
+ + O
2
2PbSO
4
+
9
CHEMISTRY
3. SULPHIDE ION (S
2
) :
Dilute H
2
SO
4
test : Pungent smelling gas like that of rotten egg is obtained.
S
2
+ 2H
+
H
2
S |
Lead acetate test : Filter paper moistened with lead acetate solution turns black.
(CH
3
COO)
2
Pb + H
2
S PbS + (black) + 2CH
3
COOH.
Sodiumnitroprusside test : Purple coloration is obtained.
S
2
+[Fe(CN)
5
(NO)]
2
[Fe(CN)
5
NOS]
4
(violet).
It is a ligand exchange reaction not a redox.
No reaction occurs with solution of H
2
Sor free gas. If however, filter paper moistened with a solution
of the reagent is made alkaline with NaOHor NH
3
solution, a purple colouration is produced with free
H
2
S also.
H
2
Sdoes not provide sufficient concentration of S
2
ions so that it does not give sodiumnitroprusside
test. Solubility is low 0.1 M and K
1
is just 10
7
.
Cadmium carbonate suspension/ Cadmium acetate solution : Yellow precipitate is formed.
Na
2
S + CdCO
3
CdS + + Na
2
CO
3
Filter paper moistened with cadmium acetate when brought in contact with evolving gas it turns
yellow.
S
2
+ 2H
+
H
2
S ; H
2
S + Cd
2+
CdS + + 2H
+
.
Silver nitrate solution : Black precipitate is formed which is insoluble in cold, but soluble in hot,
dilute nitric acid.
Ag
+
+ S
2
Ag
2
S +
Methylene blue test : NNDimethylpphenylenediamine is converted by iron(III) chloride and
hydrogen sulphide in strongly acid solution into the watersoluble dyestuff, methylene blue. This is
a sensitive test for soluble sulphides and hydrogen sulphide.
4. NITRITE ION (NO
2
) :
Dilute H
2
SO
4
test : Solid nitrite in cold produces a transient pale blue liquid (due to the presence of
free nitrous acid, HNO
2
or its anhydride, N
2
O
3
) first and then
evolution of pungent smelling reddish brown vapours of NO
2
takes place.
NO
2
+ H
+
HNO
2
; (2HNO
2
H
2
O + N
2
O
3
);
3HNO
2
HNO
3
+ 2NO + H
2
O ; 2NO + O
2
2NO
2
|
Starch iodide test : The addition of a nitrite solution to a solution of potassium iodide, followed by
acidification with acetic acid or with dilute sulphuric acid, results in the liberation of iodine, which
may be identified by the blue colour produced with starch paste. A similar result is obtained by
dipping potassium iodidestarch paper moistened with a little dilute acid into the solution.
2NO
2
+ 3I
+ 4CH
3
COOH I
3
+ 2NO | + 4CH
3
COO
+ 2H
2
O
Starch + I
3
Blue (starch iodine adsorption complex)

Ferrous sulphate test (Brown ring test) : When the nitrite solution is added carefully to a
concentrated solution of iron(II) sulphate acidified with dilute acetic acid or dilute sulphuric acid, a
brown ring appears due to the formation of [Fe(H
2
O)
5
NO]SO
4
at the junction of the two liquids. If the
addition has not been made slowly and caustiously, a brown colouration results.
NO
2
+ CH
3
COOH HNO
2
+ CH
3
COO
3HNO
2
H
2
O + HNO
3
+ 2NO |
Fe
2+
+ SO
4
2
+ NO | [Fe, NO]SO
4
Thiourea test : When a dilute acetic acid solution of a nitrite is treated with a little solid thiourea,
nitrogen is evolved and thiocyanic acid is produced. The latter may be identified by the red colour
produced with dilute HCl and FeCl
3
solution.
NaNO
2
+ CH
3
COOH HNO
2
+ CH
3
COONa
HNO
2
+ H
2
NCSNH
2
(s) (thiourea) N
2
+ HSCN + 2H
2
O
FeCl
3
+ 3HSCN
HCl dil
Fe(SCN)
3
(blood red colouration) + 3HCl
10
CHEMISTRY
Acidified potassiumpermanganate solution : Pink colour of KMnO
4
is decolourised by a solution
of a nitrite, but no gas is evolved.
5 NO
2
+ 2 MnO
4
+ 6 H
+
5 NO
3
+ 2 Mn
2+
+ 3 H
2
O
Silver nitrate solution : White crystalline precipitate of silver nitrite from concentrated solutions.
NO
2
+Ag
+
AgNO
2
+
5. ACETATE ION (CH
3
COO)
With dilute H
2
SO
4
a vinegar like smell is obtained.
(CH
3
COO)
2
Ca + H
2
SO
4
2CH
3
COOH+ CaSO
4
Neutral ferric chloridetest : Adeepred/ bloodred colouration(no precipitate) indicates thepresence
of acetate.
6CH
3
COO
+ 3Fe
3+
+ 2H
2
O [Fe
3
(OH)
2
(CH
3
COO)
6
]
+
+ 2H
+
When solution is diluted with water and boiled, brownish red precipitate of basic iron (III) acetate is
obtained.
[Fe
3
(OH)
2
(CH
3
COO)
6
]
+
+ 4H
2
O
Boil
3Fe(OH)
2
CH
3
COO + 3CH
3
COOH+ H
+
Silver nitrate solution test : Awhite crystalline precipitate is produced in concentrated solution in the
cold.
CH
3
COO
+Ag
+
CH
3
COOAg +
Precipitate is more soluble in boiling water and readily soluble in dilute ammonia solution.
Example-1 An aqueous solution of salt containing an anion X
n
gives the following reactions :
(i) It gives the purple or violet colouration with sodium nitroprusside solution.
(ii) It liberates a colourless unpleasant smelling gas with dilute H
2
SO
4
which turns lead acetate
paper black. Identify the anion (X
n
) and write the chemical reactions involved.
Solution X
n
is S
2
because
(i) [Fe(CN)
5
NO]
2
+ S
2
[Fe(CN)
5
NOS]
4
(purple or violet colouration)
(ii) S
2
+ H
2
SO
4
H
2
S | (colourless unpleasant smelling) + SO
4
2
H
2
S + Pb(CH
3
COO)
2
PbS + (black) + 2CH
3
COOH
Example-2 Sulphite on treatment with dil. H
2
SO
4
liberates a gas which :
(A) turns lead acetate paper black (B) burns with blue flame
(C) smells like vinegar (D) turns acidified K
2
Cr
2
O
7
solution green
Solution SO
3
2
+ H
2
SO
4
SO
2
+ SO
4
2
+ H
2
O
SO
2
turns acidified K
2
Cr
2
O
7
solution green.
K
2
Cr
2
O
7
+ H
2
SO
4
+ 3SO
2
Cr
2
(SO
4
)
3
(Green) + K
2
SO
4
+ H
2
O
Therefore, (D) option is correct.
Example-3 Acolourless pungent smelling gas (X) is obtained when a salt is reacted with dil. H
2
SO
4
. The gas (X)
responds to the following properties.
(A) It turns lime water milky
(B) It turns acidified potassium dichromate solution green
(C) It gives white turbidity when H
2
S gas is passed through its aqueous solution.
(D) Its aqueous solution in NaOH gives a white precipitate with barium chloride which dissolves in
dil. HCl liberating (X).
Identify (X) and write the chemical equations involved.
Solution As gas X turns lime water milky it may be CO
2
or SO
2
. But CO
2
is colourless and odourless, so 'X'
may be SO
2
. This is further, confirmed by the following reactions :
SO
3
2
+ H
2
SO
4
SO
4
2
+ SO
2
+ H
2
O ; Ca(OH)
2
+ SO
2
CaSO
3
(milky) + H
2
O
K
2
Cr
2
O
7
+ H
2
SO
4
+ 3SO
2
K
2
SO
4
+ Cr
2
(SO
4
)
3
(green) + H
2
O
SO
2
+ 2H
2
S 3S + (white) + 2H
2
O ; SO
2
+ 2NaOH Na
2
SO
3
+ H
2
O
Na
2
SO
3
+ BaCl
2
BaSO
3
+ (white) + 2NaCl ; BaSO
3
+ 2HCl BaCl
2
(soluble) + SO
2
+ H
2
O.
11
CHEMISTRY
(b) CONC . H
2
SO
4
GROUP :
1. CHLORIDE ION(Cl) :
Concentrated H
2
SO
4
test : Colourless pungent smelling gas is evolved which gives fumes of NH
4
Cl
when a glass rod dipped in dil. HCl is brought in contact with evolving gas.
Cl
+ H
2
SO
4
HCl + HSO
4
NH
4
OH + HCl NH
4
Cl | (white fumes) + H
2
O.
2NaCl + MnO
2
+ 2H
2
SO
4
(conc.) Na
2
SO
4
+ MnSO
4
+ 2H
2
O + Cl
2
Silver nitrate test :
Cl
+ Ag
+
AgCl + (white)
With sodium arsenite it is converted into yellow precipitate (distinction from AgBr and AgI) but
insoluble in dilute nitric acid.
3AgCl + + AsO
3
3
Ag
3
AsO
3
+ + 3Cl
.
White precipitate is soluble in aqueous ammonia and precipitate reappears with HNO
3
.
AgCl + 2NH
4
OH [ Ag(NH
3
)
2
]Cl (Soluble) + 2H
2
O
[Ag(NH
3
)
2
]Cl + 2H
+
AgCl + + 2NH
4
+
.
Chromyl chloride test :
4Cl
+ Cr
2
O
7
2
+ 6H
+
(conc.) 2CrO
2
Cl
2
(deep red vapours) + 3H
2
O
When deep red vapours are passed into sodium hydroxide solution, a yellow solution of sodium
chromate is formed, which when treated with lead acetate gives yellowprecipitate of lead chromate.
CrO
2
Cl
2
+ 4OH
CrO
4
2
+ 2Cl
+ 2H
2
O
CrO
4
2
+ Pb
+2
PbCrO
4
+ (yellow)
Heavy metal chlorides such as Hg
2
Cl
2
, HgCl
2
, SnCl
2
, AgCl, PbCl
2
and SbCl
3
do not respond to this
test as they are partially dissociated. This test is given generally by ionic chlorides.
Test should be carried out in a dry test tube otherwise chromic acid will be formed.
CrO
2
Cl
2
+ 2H
2
O H
2
CrO
4
+ 2HCl
2. BROMIDE ION(Br) :
Concentrated H
2
SO
4
test : First a reddish-brown solution is formed, then reddish-brown bromine
vapour accompanies the hydrogen bromide (fuming in moist air) is evolved.
2NaBr + H
2
SO
4
Na
2
SO
4
+ 2HBr
2HBr + H
2
SO
4
Br
2
| + 2H
2
O + SO
2
2KBr + MnO
2
+ 2H
2
SO
4
Br
2
| + K
2
SO
4
+ MnSO
4
+ 2H
2
O
Silver nitrate test : Pale yellow precipitate is formed
NaBr + AgNO
3
AgBr + + NaNO
3
Yellowprecipitate is partially soluble in dilute aqueous ammonia but readily dissolves in concentrated
ammonia solution.
AgBr + 2NH
4
OH [Ag(NH
3
)
2
] Br + H
2
O
Lead acetate test : Bromides on treatment with lead acetate solution, gives a white crystalline
precipitate of lead bromide, which is soluble in boiling water giving colourless solution.
2Br
+ Pb
+2
PbBr
2
+
Chlorine water test (organic layer test) : When to a sodium carbonate extract of metal bromide
containing CCl
4
, CHCl
3
or CS
2
, chlorine water is added and the content is shaken and then allowto
settle down reddish brown colour is obtained in organic layer.
2Br
+ Cl
2
2Cl
+ Br
2
| .
Br
2
+ CHCl
3
/ CCl
4
Br
2
dissolve to give reddish brown colour in organic layer..
With excess of chlorine water, the bromine is converted into yellow bromine monochloride and a
pale yellow solution results.
Br
2
|+ Cl
2
| 2BrCl
Starch paper test : When starch paper is brought in contact with evolving bromine gas orange red
spots are produced.
Br
2
+ starch starch bromine adsorption complex (orange red)
Potassium dichromate and concentrated H
2
SO
4
: When a mixture of solid bromide, K
2
Cr
2
O
7
and concentrated H
2
SO
4
is heated and evolved vapours are passed through water, a orange red
solution is obtained.
6KBr + K
2
Cr
2
O
7
+ 7H
2
SO
4
3Br
2
| + Cr
2
(SO
4
)
3
+ 4K
2
SO
4
+ 7H
2
O
12
CHEMISTRY
3. IODIDE ION (I) :
Concentrated H
2
SO
4
test : Pungent smelling violet vapours are evolved.
2NaI + H
2
SO
4
Na
2
SO
4
+ 2HI
2HI + H
2
SO
4
I
2
| (dark violet) + 2H
2
O + SO
2
Evolution of dark violet fumes intensifies on adding a pinch of MnO
2
.
3I
+ MnO
2
+ 2H
2
SO
4
I
3
| + Mn
2+
+ 2SO
4
2
+ 2H
2
S
Starch paper test : Iodides are readily oxidised in acid solution to free iodine; the free iodine may
than be identified by deep blue colouration produced with starch solution.
3I
+ 2NO
2
+ 4H
+
I
3
+ 2NO | + 2H
2
O.
Silver nitrate test : Bright yellow precipitate is formed.
I
+ Ag
+
AgI +
Bright yellowprecipitate is insoluble in dilute aqueous ammonia but is partially soluble inconcentrated
ammonia solution.
Chlorine water test (organic layer test) : When chlorine water is added to a solution of iodide,
free iodine is liberated which colours the solution brown and on shaking with CS
2
, CHCl
3
or CCl
4
, it
dissolves in organic layer forming a violet solution, which settles below the aqueous layer.
2NaI + Cl
2
2NaCl + I
2
I
2
+ CHCl
3
I
2
dissolves to give violet colour in organic layer..
If excess of chlorine water is added, I
2
is oxidised to iodic acid (colourless).
I
3
+ 8Cl
2
| + 9H
2
O 3 I

3
O + 16Cl
+ 18 H
+
Lead acetate solution : A yellow precipitate is formed which is soluble in hot water forming a
colourless solution and yielding golden yellowplates ('spangles') on cooling.
2I
+ Pb
+2
PbI
2
+
Potassiumdichromate and concentrated sulphuric acid : Violet vapours are liberated, and no
chromate is present in distillate.
6I
+ Cr
2
O
7
2
+ 2H
2
SO
4
3I
2 +
Cr
3+
+7SO
4
2
+ 7H
2
O
Action of heat :
Most of halides are stable but few decompose as
2FeCl
3
2FeCl
2
+ Cl
2
; MgCl
2
. 6H
2
O MgO + 2HCl + 5H
2
O
Hg
2
Cl
2
HgCl
2
+ Hg ; NH
4
Cl NH
3
+ HCl
2CuI
2
Cu
2
I
2
+ I
2
(without heating)
4. NITRATE ION(NO
3
) :
Concentrated H
2
SO
4
test : Pungent smelling reddish brown vapours are evolved.
4NO
3
+ 2H
2
SO
4
4NO
2
| + O
2
+ 2SO
4
2
+ 2H
2
O
Addition of bright copper turnings or paper pellets intensifies the evolution of reddish brown gas.
2NO
3
+ 4H
2
SO
4
+ 3Cu 3Cu
2+
+ 2NO | + 4SO
4
2
+ 4H
2
O ; 2NO | + O
2
2NO
2
|
4 C (paper pellet) + 4HNO
3
2H
2
O + 4NO
2
+ 4CO
2
.
Brownringtest : When a freshly prepared saturated solution of iron (II) sulphate is added to nitrate
solution and then concentrated H
2
SO
4
is added slowly from the side of the test tube, a brown ring is
obtained at the junction of two layers.
NaNO
3
+ H
2
SO
4
NaHSO
4
+ HNO
3
6FeSO
4
+ 2HNO
3
+ 3H
2
SO
4
3Fe
2
(SO
4
)
3
+ 2NO + 4H
2
O
or 2NO
3
+ 4H
2
SO
4
+ 6Fe
2+
6Fe
3+
+ 2NO + + 4SO
4
2
+ 4H
2
O.
Fe
2+
+ NO | + 5H
2
O [Fe
I
(H
2
O)
5
NO
+
]
2+
(brown ring).
Figure : Brown ring test
13
CHEMISTRY
On shaking and warming the mixture, NOescapes and a yellowsolution of iron(iii) ions is obtained.
Bromides and iodides interfere in brown ring test as liberated halogens obscure the brown ring.
Nitrites also interfere the brown ring test and can be removed by adding a little sulphamic acid, or
urea.
H
2
NHSO
3
+ NO
2
N
2
+ + SO
4
2
+ H
+
+ H
2
O
NO
2
+ H
+

HCl
HNO
2
CO(NH
2
)
2
+ 2HNO
2
2N
2
| + CO
2
| + 3H
2
O
Diphenyl amine test : Blue ring is formed at the junction of two liquids (reagent and nitrate salt
solutions).
NaNO
3
+ H
2
SO
4
NaHSO
4
+ HNO
3
2HNO
3
H
2
O + 2NO
2
+ [O]
2C
6
H
5
NHC
6
H
5
+ [O] (C
6
H
5
)
2
N N (C
6
H
5
)
2
(blue ring) + H
2
O.
This test is also given by various oxidising agents like CrO
4
2
, Cr
2
O
7
2
, ClO
3
, BrO
3
, IO
3
, NO
2
etc.
TO distinguish Br
2
with NO
2
(both are reddish brown gases)
(a) Br
2
+ starchiodide paper Blue black colour spots do not develop immediately as Br
2
is a
weaker oxidising agent whereas NO
2
being strong oxidising agent develops the blue black colour
immediately.
(b) Bromine develops orangered colour spots on starch paper.
(B) GROUP'B' RADICALS:
Group of anions which do not give any gas with dilute as well as concentrated H
2
SO
4
in cold but
give precipitate with certain reagents :
These acid radicals are identified in inorganic salts by their individual tests as given below
1. SULPHATE ION(SO
4
2
) :
Barium chloride test :
W.E. or S.E. + Barium chloride (aq) White precipitate
Na
2
SO
4
+ BaCl
2
BaSO
4
+ (white) + 2NaCl.
White precipitate is insoluble in warm dil. HNO
3
as well as HCl but moderately soluble in boiling
concentrated hydrochloric acid.
Lead acetate test :
W.E. or S.E. + Lead acetate white precipitate
Na
2
SO
4
+ (CH
3
COO)
2
Pb PbSO
4
+ (White) + 2CH
3
COONa
White precipitate soluble in excess of hot ammonium acetate.
PbSO
4
+ 2CH
3
COONH
4
(CH
3
COO)
2
Pb (soluble) + (NH
4
)
2
SO
4
Match stick test :
(a) W.E. or S.E. + Barium chloride white precipitate
Na
2
SO
4
+ BaCl
2
2NaCl + BaSO
4
+ (white)
(b) White precipitate + Na
2
CO
3
(s) mix and apply the paste on the end of the carbonized match stick
or a wooden splinter. Put it in the reducing flame.
BaSO
4
(s) + Na
2
CO
3
(s) Na
2
SO
4
+ BaCO
3
+ (white)
Na
2
SO
4
+ 4C Na
2
S + 4CO
(c) Now dip the match stick in sodium nitroprusside solution, purple colour near the fused mass is
developed.
Na
2
S + Na
2
[Fe(CN)
5
NO] Na
4
[Fe(CN)
5
NOS] (purple)
Mercury II chloride test : Yellow precipitate is formed
SO
4
2
+ 3Hg
2+
+ 2H
2
O HgSO
4
. 2H
2
O (basic mercury II sulphate) + + 4H
+
Silver nitrate test : White precipitate is obtained.
SO
4
2
+ 2Ag
+
Ag
2
SO
4
+
14
CHEMISTRY
2. PHOSPHATE ION (PO
4
3
) :
Ammonium molybdate test :
Na
2
HPO
4
(aq) + 12(NH
4
)
2
MoO
4
+ 23HNO
3
(NH
4
)
3
PMo
12
O
40
+ (canary yellow) + 2NaNO
3
+ 21NH
4
NO
3
+ 12H
2
O
Some times ammoniumphosphomolybdate is also represented by the formula (NH
4
)
3
PO
4
. 12MoO
3
Magnesium nitrate or magnesia mixture test : W.E. or S.E + Magnesium nitrate reagent (3-4
mL) and allows to stand for 4-5 minutes, white crystalline precipitate is formed.
Na
2
HPO
4
(aq) + Mg(NO
3
)
2
(aq) + NH
4
OH(aq) Mg(NH
4
) PO
4
+ (white) + 2NaNO
3
+ H
2
O
Magnesia mixture is a solution containing MgCl
2
, NH
4
Cl and a little aqueous NH
3
.
PO
4
3
also gives BaCl
2
test due to the formation of white precipitate of Ba
3
(PO
4
)
2
. So phosphate
test should be carried out first and then conclude if PO
4
3
is present or absent before proceeding
with the test for SO
4
2
.
Silver nitrate solution : Yellow precipitate is formed which is soluble in dilute ammonia and in dilute
nitric acid.
PO
4
3
+ 3Ag
+
Ag
3
PO
4
+
Ag
3
PO
4
+ + 6NH
3
3[Ag(NH
3
)
2
]
+
+PO
4
3
; Ag
3
PO
4
+ + 2H
+
H
2
PO
4
+ 3Ag
+
Iron (III) chloride solution : Yellowish-white precipitate of FePO
4
is obtained
HPO
4
2
+ Fe
3+
FePO
4
+
3. BORATEION(BO
3
3
) :
Salt (0.2 g) + conc. H
2
SO
4
(1 mL) + Ethyl alcohol (4-5 mL) mix in a test tube and then heat. Ignite
the evolved vapours with the help of Bunsen flame, green edged flame is obtained.
2Na
3
BO
3
+ 3H
2
SO
4
3Na
2
SO
4
+ 2H
3
BO
3
3C
2
H
5
OH + H
3
BO
3
(C
2
H
5
)
3
BO
3
+ 3H
2
O
Example-4 Acompound (A) of S, Cl and Ohas vapour density of 67.5 (approx.). It reacts with water to formtwo
acids and reacts with KOHto formtwo salts (B) and (C) while (B) gives white precipitate withAgNO
3
solution and (C) gives white precipitate with BaCl
2
solution. Identify (A), (B) & (C).
Solution As mixture give white precipitate with BaCl
2
and AgNO
3
, it should contain SO
4
2
and Cl
ions. As
SO
2
Cl
2
when dissolved in water gives, a mixture of H
2
SO
4
&HCl which then react with KOHto form
KCl and K
2
SO
4
. Therefore, (A) is SO
2
Cl
2
and (B) & (C) are K
2
SO
4
and KCl respectively.
Vapour density of SO
2
Cl
2
= molecular weight / 2.
Vapour density of SO
2
Cl
2
= 135 / 2 = 67.2.
Example-5 Bromine vapours turn moist starch iodide paper :
(A) brown (B) red (C) blue (D) colourless
Solution 2I
+ Br
2
I
2
+ 2Br
; I
2
+ starch blue starch iodine adsorption complex.
Therefore, (C) option is correct.
Example-6 Na
2
S
2
O
3
+ I
2
NaI + .......... [X], [X] is :
(A) Na
2
S
4
O
6
(B) Na
2
SO
4
(C) Na
2
S (D) Na
3
ISO
4
Solution 2Na
2
S
2
O
3
+ I
2

2NaI + Na
2
S
4
O
6 .
Therefore, (A) option is correct.
Example-7 Column I and column II contains four entries each. Entries of column I are to be matched with some
entries of column II. Each entry of column I may have the matching with one or more than one entries
of column II.
Column I Column II
(A) Colourless gas evolved on addition of dil. H
2
SO
4
(p) Cl
(B) White precipitate on addition of AgNO

3
(q) S
2
(C) Precipitate with solution containing Pb
+2
ions. (r) NO
2
(D) Its acidified salt solution decolourises pink KMnO

4
solution. (s) SO
3
2
15
CHEMISTRY
Solution (A - p, q, s) ; (B - p, r, s) ; (C - p, q, s) ; (D - p, q, r, s)
(A) Cl
+ H
2
SO
4
HCl| (colourless) + HSO
4
; S
2
+ 2H
+
H
2
S | (colourless)
NO
2
+ 2H
+
NO
2
| (reddish brown) + H
2
O; SO
3
2
+ 2H
+
SO
2
| (colourless) + H
2
O
(B) Ag
+
+ Cl
AgCl + (white) ; Ag
+
+ S
2
Ag
2
S + (black)
Ag
+
+ NO
2
AgNO
2
+ (white) ; 2Ag
+
+ SO
3
2
Ag
2
SO
3
+ (white)
(C) Pb
2+
+ 2Cl
PbCl
2
+ (white) ; Pb
2+
+ S
2
PbS + (black)
Pb
2+
+ NO
2
PbNO
2
(soluble) ; Pb
2+
+ SO
3
2
PbSO
3
+ (white)
(D) 2MnO
4
+ 16HCl 5Cl
2
+ 2Mn
2+
+ 6Cl
+ 8H
2
O
2MnO
4
+ 5H
2
S + 6H
+
Mn
2+
+ 5S + + 8H
2
O
2MnO
4
+ 5NO
2
+ 6H
+
Mn
2+
+ 5NO
3
+ 3H
2
O
2MnO
4
+ 5SO
2
+ 2H
2
O 2Mn
2+
+ 5SO
4
2
+ 4H
+
Analysis of CATIONS (Basic Radicals) :
Table : 11
Group Group reagent Basic radical Composition and colour of
precipitate
Zero NaOH or Ca(OH)
2
, heat if required NH
4
+
Ammonia gas is evolved.
1. Dil HCl Ag
+
AgCl ; White
Hg
2
2+
Hg
2
Cl
2
; White
Pb
2+
PbCl
2
; White
2.(A) H
2
S in presence of dil HCl Hg
2+
HgS ; Black
(Insoluble in YAS) Pb
2+
PbS
;
Black
Bi
3+
Bi
2
S
3
; Black
Cu
2+
CuS ; Black
Cd
2+
CdS ; Yellow
2.(B) H
2
S in presence of dil HCl As
3+
As
2
S
3
; Yellow
(Soluble in YAS) Sb
3+
Sb
2
S
3
; Orange
Sn
2+
SnS ; Brown
Sn
4+
SnS
2
; Yellow
3. NH
4
OHin presence of NH
4
Cl Fe
3+
Fe(OH)
3
; Reddish brown
Cr
3+
Cr(OH)
3
; Green
Al
3+
Al(OH)
3
; Gelatinous white
4. H
2
S in presence of NH
4
OH Zn
2+
ZnS ; White
and NH
4
Cl Mn
2+
MnS ; Buff (or Pink)
Co
2+
CoS ; Black
Ni
2+
NiS ; Black
5. (NH
4
)
2
CO
3
in presence of NH
4
OH Ba
2+
BaCO
3
; White
Sr
2+
SrCO
3
; White
Ca
2+
CaCO
3
; White
6. Na
2
HPO
4
in presence of NH
4
OH Mg
2+
Mg(NH
4
)PO
4
; White
[YAS = Yellow ammonium sulphide. (NH
4
)
2
S
x
].
There are some important points which should be kept in mind while doing the analysis of cations.
1. Group 1
st
radicals (Ag
+
,
Pb
2+
,
Hg
2
2+
) are precipitated as chloride because the solubility product of these
chlorides (AgCl, PbCl
2
, HgCl
2
) is less than the solubility products of chlorides of all other metal ions, which
remain insolution. Lead chloride is slightly soluble in water and therefore, leadis never completely precipitated
by adding dilute hydrochloric acid to a sample ; the rest of the lead ions are precipitated with H
2
S in acidic
medium together with the cations of the second group.
16
CHEMISTRY
2. Group 2
nd
radicals are precipitated as sulphides because of their lowsolubility products whereas sulphides
of other metals remain in solution because of their high solubility products. HCl acts as a source of H
+
which
decreases the concentration of S
2
due to common ion effect. Hence, the concentration of S
2
ion is too low
that it exceeds only the solubility products of the metal sulphides of II
nd
group.
We can not use H
2
SO
4
inplaceof HCl because some cations of higher groups i.e. v
th
group will also precipitate
as their sulphates like BaSO
4
, SrSO
4
, CaSO
4
etc.
HNO
3
can't be used in place of HCl. HNO
3
is a powerful oxidising agent. HNO
3
will oxidize H
2
S forming
sulphur (yellowprecipitate) or colloidal solution causing confusion with CdS, As
2
S
3
even though Cd
2+
, As
3+
will be absent. The colloidal solution is white-yellowand that cannot be filtered causing unnecessary trouble.
3. Group 3
rd
radicals are precipitated as hydroxides and the addition of NH
4
Cl suppresses the ionisation of
NH
4
OH so that only the group 3 cations are precipitated as hydroxides because of their low solubility
products.
(i) Excess of NH
4
Cl should not be added, as manganese will precipitate as MnO
2
.H
2
O
(ii) (NH
4
)
2
SO
4
cannot be used in place of NH
4
Cl because the SO
4
2
will also give the precipitate of BaSO
4
,
SrSO
4
etc.
(iii) While proceeding for 3
rd
group from2
nd
group, the filtrate of 2
nd
group is boiled off to remove the dissolved
H
2
Sand then one drop of concentrated HNO
3
is added and again boil so that if Fe
2+
is present is oxidised to
Fe
3+
. The K
sp
of Fe
2+
is higher than Fe
3+
, therefore, it is partially precipitated and will thus interfere in the
analysis of 4
th
group radicals. In our scheme Fe
2+
is not there even if it is present, we shall report only Fe
3+
(Fe
2+
needs other special tests).
(iv) If the mediumremains acidic the hydroxides do not precipitate and we would think that Fe
3+
, Al
3+
, Cr
3+
are
absent even though they may be present.
(v) In place of NH
4
OH, NaOH solution can't be used for the precipitation as their hydroxides because in
excess of it we get soluble complexes of Al
3+
and Cr
3+
.
4. In 4
th
group, ammonium hydroxide increases the ionisation of H
2
S by removing H
+
from H
2
S as unionised
water.
H
2
S 2H
+
+ S
2
; H
+
+ OH
H
2
O
Nowthe excess of S
2
ions is available and hence the ionic products of group 4
th
group cations exceeds their
solubility products and will be precipitated. In case H
2
S is passed through a neutral solution, incomplete
precipitation will take place due to the formation of HCl, which decreases the ionisation of H
2
S. For example
MnCl
2
+ H
2
S MnS + 2HCl
5. In 5
th
group the reagent ammonium carbonate should be added in alkaline or neutral medium. In the
absence of ammonia or ammonium ions, magnesium will also be precipitated.
PREPARATION OF ORIGINAL SOLUTION (O.S) :
Original solution is used for the analysis of basic radicals except NH
4
+
. It is prepared by dissolving given salt
or mixture in a suitable solvent as follows :
H
2
O
dil HCl
conc. HCl
Salt or Mixt. + H
2
O
A
soluble (then H
2
O is suitable solvent)
If given salt or mixture is insoluble in H
2
O then it is dissolved in dil HCl.
Salt or Mixt. + dil HCl
A
soluble (then dil HCl is taken as solvent)
If given salt or mixture is insoluble in dilute HCl then it is dissolved in conc. HCl.
Salt or Mixt. + conc. HCl
A
soluble
In this way after selecting suitable solvent, given salt or mixture is dissolved in small quantity in the solvent
and filtered. Obtained filtrate is called as original solution (O.S.) and that is used for the detection of basic
radicals except NH
4
+
.
17
CHEMISTRY
ZERO GROUP :
1. AMMONIUM ION (NH
4
+
) :
Sodiumhydroxide solution : Ammonia gas is evolved on warming the solution containing ammonium salt
and sodium hydroxide.
NH
4
Cl + NaOH NH
3
+ H
2
O + NaCl
The gas can be identified by the following characteristics / reactions.
Its characteristics smell.
The evolution of the white fumes of ammoniumchloride when a glass rod dipped in dilute HCl is held
in the vapour.
NH
3
+ HCl NH
4
Cl | (white fumes)
Its ability to turn filter paper moistened with Hg
2
(NO
3
)
2
solution black.
2HgNO
3
+ 2NH
3

lack b
Hg NO ) NH ( Hg
3 2
+ + NH
4
NO
3
Its ability to turns filter paper moistened with CuSO
4
solution deep blue.
CuSO
4
+ 4NH
3
[Cu(NH
3
)
4
]SO
4
Filter paper moistened with a solution of manganese (II) chloride and hydrogen peroxide made
alkaline with ammonia gives a brown colour due to the oxidation of manganese.
2NH
3
+ Mn
2+
+H
2
O
2
+ H
2
O MnO(OH)
2
+ + 2NH
4
+
Nessler's reagent (Alkaline solution of potassiumtetraiodidomercurate(II) :
Brown precipitate or brown or yellowcolouration is obtained according to the amount of ammonia or
ammonium ions present. The precipitate is a basic mercury (II) amidoiodide.
NH
4
+
+ 2[HgI
4
]
2
+ 4OH
HgO Hg (NH
2
)I + + 7I
+ 3H
2
O
Sodium hexanitritoNcobaltate (III) solution :
NH
4
+
ions gives a yellow precipitate with the reagent.
3NH
4
+
+ [Co(NO
2
)
6
]
3
(NH
4
)[Co(NO
2
)
6
]+
Hexachloridoplatinate (IV) solution (i.e., hexachloroplatinic acid) :
NH
4
+
ions gives a yellow precipitate with the reagent .
2NH
4
+
+ [PtCl
6
]
(NH
4
)
2
[PtCl
6
]+ yellow
Saturated sodiumhydrogen tartrate solution (NaHC
4
H
4
O
6
) :
NH
4
+
ions gives a white precipitate with the reagent .
NH
4
+
+ HC
4
H
4
O
6
NH
4
HC
4
H
4
O
6
+
4-Nitrobenzene - diazonium chloride reagent : NH
4
+
gives red colouration with the reagent in
presence of sodiumhydroxide.
O
2
N N=NCl + NH
4
+
+ OH
O
2
N N=NONH
4
+ Cl
+ H
2
O
18
CHEMISTRY
I
st
GROUP (Pb
2+
, Hg
2
2+
, Ag
+
) :
1. LEAD ION (Pb
2+
) :
Dilute HCl solution : White precipitate is formed in cold solution.
Pb
2+
+ HCl PbCI
2
+ (white) + 2H
+
White precipitate is soluble in hot water. White precipitate is also soluble in concentrated HCl or concentrated
KCl.
PbCl
2
+ + 2Cl
[PbCl
4
]
2
(colourless)
Sodium hydroxide solution : White precipitate is formed which is soluble in excess of the reagent.
Pb
2+
+ 2OH
Pb(OH)
2
+ ; Pb(OH)
2
+ + 2OH
[Pb(OH)
4
]
2
[Pb(OH)
4
]
2
+ H
2
O
2
PbO
2
+ (black / brownish black) + 2H
2
O + 2OH
[Pb(OH)
4
]
2
+ S
2
O
8
2
PbO
2
+ + 2H
2
O + 2SO
4
2
Potassiumiodide solution : Ayellow precipitate is formed which is soluble in excess more concentrated
(6M) solution of the reagent. Yellowprecipitate of PbI
2
is moderately soluble in boiling water to giveacolourless
solution.
PbCl
2
+ 2KI PbI
2
+ + 2KCl ; Pbl
2
+ KI K
2
[PbI
4
] +
Yellowprecipitate reappears on dilution with water. Yellowprecipitate of PbI
2
does not dissolve in excess of
dilute solution of KI.
Potassium chromate solution (in neutral, acetic acid or ammonia solution) : A yellow precipitate is
formed.
PbCl
2
+ K
2
CrO
4
PbCrO
4
+ + 2KCl
Yellow precipitate is soluble in sodium hydroxide and HNO
3
(nitric acid).
2PbCrO
4
+ 2H
+
2Pb
2+
+ Cr
2
O
7
2
+ H
2
O
PbCrO
4
+ 4OH
[Pb(OH)
4
]
2
+ CrO
4
2
Both reversible reactions on buffering the solution with ammonia or acetic acid respectively, PbCrO
4
reprecipitates.
19
CHEMISTRY
Ammonia solution : With ammonia solution, Pb
2+
gives a white precipitate of lead hydroxide.
Pb
2+
+ 2NH
4
OH Pb(OH)
2
+ + 2NH
4
+
Dilute H
2
SO
4
: White precipitate is formed which is soluble in more concentrated ammonium acetate (6M)
solution or ammonium tartrate in the presence of ammonia.
PbCl
2
+ H
2
SO
4
PbSO
4
+ + 2HCl
PbSO
4
+ + 4CH
3
COO
[Pb(CH
3
COO)
4
]
2
+ SO
4
2
PbSO
4
+ + 2C
4
H
4
O
6
2
[Pb(C
4
H
4
O
6
)
2
]
2
+ SO
4
2
Hot concentrated H
2
SO
4
dissolves the precipitate due to the formation of PbHSO
4
.
PbSO
4
+ + H
2
SO
4
Pb
2+
+ 2HSO
4
2. MERCURY(I) ION(Hg
2
2+
) :
Dilute HCl solution : White precipitate is formed in cold solution.
Hg
2
2+
+ 2HCl Hg
2
Cl
2
+ (white) + 2H
+
Ammonia solution : Amixture of mercury metal (black precipitate) and basic mercury (II) amido chloride
(white precipitate) is formed.
2Hg
2
Cl
2
+ 4NH
4
OH

black
2
Hg Cl ) HgO.Hg(NH + + + + 3NH
4
Cl + 3H
2
O
Dissolution of white precipitate (Hg
2
Cl
2
) in aquaregia :
3Hg
2
Cl
2
+ 2HNO
3
+ 6HCl 6HgCl
2
+ 2NO+ 4H
2
O
(a) Stannous chloride test : White precipitate is formed which finally turns to black.
2HgCl
2
+ SnCl
2
Hg
2
Cl
2
+ + SnCl
4
; Hg
2
Cl
2
+ SnCl
2
2Hg + (black) + 2SnCl
4
(b) Potassium iodide test : Scarlet/red precipitate is formed which is soluble in excess of the reagent.
HgCl
2
+ KI HgI
2
+ + 2KCl ; HgI
2
+ KI (excess) K
2
[HgI
4
] (soluble)
(c) Copper chips test : Shining grey deposition of mercury on copper chips is formed.
HgCl
2
+ Cu Hg+ (grey) + CuCl
2
Potassiumiodide solution : Agreen precipitate is formed.
Hg
2
2+
+ 2I
Hg
2
I
2
+
Green precipitate in excess of reagent undergoes disproportionation reaction and a soluble [HgI
4
]
2_
ions and
black mercury are formed.
Hg
2
I
2
+ + 2I
[HgI
4
]
2
+ Hg+ (finely divided)
Boiling the mercury (I) iodide precipitate with water, disproportionation takes place and a mixture of red
mercury (II) iodide precipitate and black mercury is formed.
Hg
2
I
2
+ HgI
2
+ + Hg+
Potassium chromate solution : Ared crystalline precipitate is formed which turns black when solution of
sodium hydroxide is added.
Hg
2
2+
+ CrO
4
2
Hg
2
CrO
4
+; Hg
2
CrO
4
+ + 2OH
Hg
2
O + + CrO
4
2
+ H
2
O
Potassium cyanide solution : Ablack precipitate of mercury is obtained
Hg
2
2+
+ 2CN
Hg+ + Hg(CN)
2
(soluble).
3. SILVER ION (Ag
+
) :
Dilute hydrochloric acid/soluble chlorides : White precipitate is formed.
Ag
+
+ HCl

AgCl + + H
+
The precipitate obtained after filtration is soluble in concentrated HCl.
AgCl + +Cl
[AgCl
2
]
On dilution with water, the equilibrium shifts back to the left and the precipitate reappears. Dilute ammonia
solution dissolves the precipitate forming a soluble complex.
AgCl+ + 2NH
3
[Ag (NH
3
)
2
]
+
+ Cl
Dilute nitric acid or hydrochloric acid neutralizes the excess ammonia and the precipitate reappears because
the equilibrium is shifted backwards.
[Ag(NH
3
)
2
]Cl + 2HNO
3
AgCl + (white) + 2NH
4
NO
3
.
Potassium iodide solution : Abright yellow precipitate is formed which is insoluble in dilute ammonia
but partially soluble in concentrated ammonia.
Ag
+
+ I
AgI+
The yellow precipitate is soluble in KCN and in Na
2
S
2
O
3
.
AgI + + 2CN
[Ag(CN)
2
]
+ I
; AgI+ + 2S
2
O
3
2
[Ag(S
2
O
3
)
2
]
3
+ I
20
CHEMISTRY
Potassiumchromatesolution: Redprecipitateis formedwhichissolubleindiluteHNO
3
andinammoniasolution.
2Ag
+
+ CrO
4
2
Ag
2
CrO
4
+
2Ag
2
CrO
4
+ + 2H
+
4Ag
+
+ Cr
2
O
7
2
+ H
2
O
2Ag
2
CrO
4
+ + 4NH
3
2[Ag(NH
3
)
2
]
+
+ CrO
4
2
Disodiumhydrogen phosphate solution : Inneutral solution a yellowprecipitateis formed withthe reagent.
3Ag
+
+ HPO
4
2
Ag
3
PO
4
+ + H
+
The yellow precipitate is soluble in nitric acid and ammonia solution.
Hydrazine sulphate (saturated) : With diammineargentate (I) reagent forms finely divided silver which
adheres to the cleaned glass walls of the test tube forming an attractive mirror.
4[Ag(NH
3
)
2
]
+
+ H
2
N
NH
2
.H
2
SO
4
4Ag + + N
2
|+ 6NH
4
+
+ 2NH
3
+ SO
4
2
Ammonia solution : Brown precipitate is formed.
2Ag
+
+ 2NH
3
+ H
2
O Ag
2
O + + 2NH
4
+
Precipitate dissolves in ammonia.
Ag
2
O+ + 4NH
3
+ H
2
O 2[Ag(NH
3
)
2
]
+
+ 2OH
Example-8 Acompound on heating with an excess of caustic soda solution liberates a gas (B) which gives white
fumes on exposure of HCl. The resultant alkaline solution thus obtained after heating again liberates
thesamegas (B) whenheatedwith zinc powder. Compound(A) onheatingalonegives aneutral oxide
of nitrogen not nitrogen gas. Identify(A) and (B) and give the relevant chemical reactions.
Solution As NH
3
gives whitefumes withHCl, therefore, (B) shouldbeNH
3
and(A) shouldbethesalt of ammonium.
Further we knowthat nitrite of ammonium gives NH
3
with Zn and alkali and when heated alone gives
neutral oxide (N
2
O) not N
2
. Hence the salt should be ammonium nitrate not ammonium nitrite.
NH
4
NO
3
(A) + NaOH

NaNO
3
+ H
2
O + NH
3
| (B) ; NH
3
+ HCl

NH
4
Cl (white fumes)
NaNO
3
+ 8[H]
NaOH Zn
NaOH + 2H
2
O + NH
3
; NH
4
NO
3

N
2
O(neutral) + 2H
2
O
Example-9 A certain metal (A) is boiled with dilute HNO
3
to give a salt (B) and an neutral oxide of nitrogen (C).
An aqueous solution of (B) gives a white precipitate (D) with brine which is soluble in ammonium
hydroxide. An aqueous solution of (B) also gives red / brick red precipitate, (E) with potassium
chromate solution. Identify (A) to (E) and write the chemical reactions involved.
Solution As solution of (B) gives white precipitate with NaCl (aq) and precipitate is soluble in ammonium
hydroxide, it may be of silver salt. Further it gives brick red precipitate with K
2
CrO
4
, therefore, metal
(A) may be silver.
3Ag (A) + 4HNO
3
3AgNO
3
(B) + NO(C) + 2H
2
O;
AgNO
3
+ NaCl AgCl + (white) (D) + NaNO
3
AgCl + 2NH
4
OH [Ag(NH
3
)]
2
Cl (soluble) + 2H
2
O
2AgNO
3
+ K
2
CrO
4
Ag
2
CrO
4
+ (red / brick red) (E) + 2KNO
3
Example-10 Which of the following salt will give white precipitate with the solution containing Pb
2+
ions ?
(A) Na
2
CO
3
(B) NaCl (C) Na
2
SO
3
(D) All of these
Solution Pb
2+
+ CO
3
2
PbCO
3
+ (white)
Pb
2+
+ 2Cl
PbCl
2
+ (white)
Pb
2+
+ SO
3
2
PbSO
3
+ (white)
Therefore, (D) option is correct.
21
CHEMISTRY
II
nd
Group (Hg
2+
, Pb
2+
, Bi
3+
, Cu
2+
, Cd
2+
, As
3+
, Sb
3+
, Sn
2+
)
On the basis of the solubility of the precipitates of the sulphides of II group cations in yellow ammonium
sulphide, they have been classified into two subgroups as given below:
IIA : HgS, PbS, CuS, Bi
2
S
3
, all black but CdS is yellow. All insoluble in yellow ammonium sulphide.
IIB : SnS
2
, As
2
S
3
are yellow, Sb
2
S
3
is orange & SnS is dark brown All soluble in yellow ammonium sulphide.
IIA Group (Hg
2+
, Pb
2+
, Bi
3+
, Cu
2+
, Cd
2+
)
1. MERCURY (II) ION (Hg
2+
) :
Precipitation with H
2
S in acidic medium : Black precipitate is formed. Precipitate insoluble in water,
hot dilute HNO
3
,alkali hydroxides, or colourless ammonium sulphide.
Hg
2+
+ H
2
S
+
H
HgS + + 2H
+
Na
2
S (2M) dissolves the precipitate forming soluble complex.
HgS + S
2
[HgS
2
]
2
Aqua regia dissolves the precipitate.
3 HgS + 6 HCl + 2HNO
3
3 HgCl
2
+ 3S
+
+ 2NO | + 4 H
2
O
22
CHEMISTRY
Under these circumstance HgCl
2
is undissociated. When solution is heated white precipitate of sulphur
dissolves forming H
2
SO
4
.
2 HNO
3
+ S + SO
4
2
+ 2 H
+
+ 2NO |
Stannous chloride solution : When added in moderate amounts silky white precipitate is formed.
2HgCl
2
+ SnCl
2
SnCl
4
+ Hg
2
Cl
2
+
If more reagent is added, Hg (I) chloride is reduced to black precipitate of mercury.
Hg
2
Cl
2
+ SnCl
2
SnCl
4
+ 2Hg +
Potassium iodide solution : On slow addition red precipitate is formed.
Hg
2+
+ 2I
HgI
2
+
Precipitate dissolves in excess of KI forming colourless soluble complex.
HgI
2
+ 2I
[HgI
4
]
2
KCNdoes not have any effect.

Copper chips , sheet or coin : Ablack precipitate of mercury is formed.
Hg
2+
+ Cu Hg + + Cu
2+
Sodiumhydroxidesolution: Whenaddedinsmall quantitybrownishredprecipitateof varyingcomposition
is formed and in stoichiometric amounts precipitate turns to yellow when Hg (II) oxide is formed.
Hg
2+
+ 2OH
HgO + + H
2
O
Precipitate is insoluble in excess reagent but dissolves readily in acids and this can be used to differentiate
Hg (I) fromHg (II).
Ammonia solution : White precipitate of mixed composition (Mercury (II) oxide + Mercury (II) amido
nitrate) is formed with metal nitrate.
2 Hg
2+
+ NO
3
+ 4NH
3
+ H
2
O HgO.Hg (NH
2
)NO
3
+ + 3 NH
4
+
Cobalt (II) thiocyanate test : When reagent is added to an aqueous solution of Hg
2+
ions and the walls
of the test tube is stirred with a glass rod, deepblue crystalline precipitate is formed.
Hg
2+
+ Co
2+
+ 4 SCN
Co
+2
[Hg(SCN)
4
]
2
+
Inplace of Cobalt (II) thiocyanate, Co(CH

3
COO)
2
and NH
4
SCNcan beadded to the aqueous solution
of Hg
2+
ions.
2. COPPER ION (Cu
2+
) :
2
S in acidic medium : Black precipitate is formed.
Cu
2+
+ H
2
S
+
H
CuS + + 2 H
+
Precipitate is insoluble in boiling dilute (M) H
2
SO
4
(distinction from cadmium), in NaOH, Na
2
S and (NH
4
)
2
S.
Precipitate dissolves in hot concentrated HNO
3
3 CuS + 8HNO
3

3Cu(NO
3
)
2
(blue) + 2NO + 4H
2
O + 3S
When boiled for longer S is oxidised to H
2
SO
4
and a clear solution of Cu(NO
3
)
2
is obtained.
KCN dissolves the precipitate forming a clear solution.

2 CuS + + 8 CN

2 [Cu(CN)
4
]
3
+ S
2
2
(disulphide ion)
Ammonia solution : When added sparingly a blue precipitate of basic salt (basic copper sulphate) is
formed with CuSO
4
.
2Cu
2+
+ SO
4
2
+ 2 NH
3
+ 2H
2
O Cu(OH)
2
.CuSO
4
+ + 2NH
4
+
It is soluble in excess of reagent forming a deep blue colouration.
Cu(OH)
2
.CuSO
4
+ + 8NH
3
2[Cu(NH
3
)
4
]
2+
+ SO
4
2
+ 2 OH
Sodium hydroxide in cold solution : Ablue precipitate is formed.

Cu
2+
+ 2 OH
Cu (OH)
2
+
Cu(OH)
2
+
Heat
CuO+ (red) +H
2
O

Potassiumiodide : It gives a white precipitate of Cu(I) iodide but the solution is intensely brown because
of the formation of triiodide ions (or iodine).
2 Cu
2+
+ 5 I
Cu
2
I
2
+ + I
3
The solution becomes colourless and a white precipitate is visible when excess of sodium thiosulphate
solution is added.
I
3
+ 2 S
2
O
3
2
3 I
+ S
4
O
6
2
23
CHEMISTRY
These reactions are used in quantitative analysis for the iodometric determination of copper.
Potassiumferrocyanide (Potassiumhexacyanidoferrate(II) ) solution: Cu
2+
ions gives brown/chocolate
brown precipitate.
2Cu
2+
+ K
4
Fe(CN)
6

Cu
2
[Fe(CN)
6
] + + 4K
+
2 [Fe(CN)
6
]
3
+ 3 Cu
2+

Cu
3
[Fe(CN)
6
]
2
+ (green)
(vi) Potassiumcyanide : When added sparingly forms first a yellow precipitate.
Cu
2+
+ 2CN

Cu(CN)
2
+ (yellow)
Precipitate quickly decomposes into CuCN and cyanogen.
2 Cu(CN)
2
+

2CuCN+ (white) + (CN)
2
| (highly poisonous)
Excess reagent dissolves the precipitate forming a colourless soluble complex.
CuCN + + 3 CN

[Cu(CN)
4
]
3
Complex is so stable that H
2
S cannot precipitate Cu (I) sulphide (distinction from cadmium).
Potassium thiocyanate solution : The Cu
+2
ions solution initially gives a black precipitate which then
slowly decomposes to give white precipitate of Cu(I) thiocyanate.
Cu
2+
+ 2 SCN

Cu(SCN)
2
+
2 Cu(SCN)
2
+

2 CuSCN+ + (SCN)
2
|
Cu (II) thiocyanate can be immediately converted into Cu(I) thiocyanate by adding a suitable reducing
agent like saturated solution of sulphur dioxide.
2 Cu(SCN)
2
+ + SO
2
+ 2 H
2
O 2 CuSCN + + 2 SCN
+ SO
4
2
+ 4H
+
3. BISMUTH ION (Bi
3+
) :
2
S in acidic medium : Black precipitate is formed which is insoluble in cold dilute
HNO
3
and yellowammoniumsulphide.
2Bi
3+
+ 3H
2
S
+
H
Bi
2
S
3
+ (black) + 6H
+
Bi
2
S
3
+ 8HNO
3
2Bi (NO
3
)
3
+ 2NO + 3S + 4H
2
O
Bi
2
S
3
+ + 6 HCl (boiling concentrated) 2 Bi
3+
+ 6 Cl
+ 3 H
2
S
Sodium hydroxide : White precipitate is formed with the reagent.
Bi
3+
+ 3 OH
Bi(OH)
3
+
Very slightly soluble in excess reagent in cold solution but soluble in acids.
Bi(OH)
3
+ + 3H
+
Bi
3+
+ H
2
O
Precipitate on boiling loses water and turns yellowish white which is oxidised to BiO
3
by H
2
O
2
.
Bi(OH)
3
BiO.OH+ + H
2
O
BiO.OH + H
2
O
2
BiO
3
+ H
+
+ H
2
O
Ammonia solution : White basic salt of variable composition is formed. Approximate chemical reaction is :
Bi
3+
+ NO
3
+ 2 NH
3
+ 2 H
2
O Bi(OH)
2
NO
3
+ + 2 NH
4
+
Alkaline sodiumstannite (Sodiumtetrahydroxidostannate (II)) : Ablack precipitate of metallic bismuth
is obtained.
Bi
3+
+ 3 OH

Bi(OH)
3
+
2Bi(OH)
3
+ + [Sn(OH)
4
]
2

2Bi + + 3 [Sn(OH)
6
]
2
(OA) (RA)
The reagent must be freshly prepared and test must be carried out in cold solution.
Dilution with water : Solution of bismuth salts gives white precipitate when water is added in larger
quantity.
Bi
3+
+ NO
3
+ H
2
O

BiO(NO
3
) + + 2H
+
Bi
3+
+ Cl
+ H
2
O

BiOCl + (bismuth oxychloride or bismuthyl chloride) + 2H
+
Soluble in mineral acids (dilute) but insoluble in tartaric acid (distinction fromantimony) and in alkali hydroxide
(distinction from tin).
24
CHEMISTRY
Potassium iodide : When the reagent is added dropwise to a solution containing Bi
3+
ions , a black
precipitate is formed.
Bi
3+
+ 3I

BiI
3
+
The precipitate dissolves in excess KI forming orange coloured soluble complex.
BiI
3
+ I
[BiI
4
]
On dilution the reaction is reversed and black BiI

3
is reprecipitated.
On heating with water black precipitate of BiI

3
turns orange.
BiI
3
+ + H
2
O

BiOI + + 2H
+
+ 2I
4. CADMIUM ION (Cd

2+
) :
2
S in acidic medium : Yellow precipitate is formed which dissolves in hot dilute
HNO
3
.
Cd
2+
+ H
2
S
+
H
CdS + + 2H
+
CdS + 8HNO
3

3Cd (NO
3
)
2
+ 4H
2
O + 2NO + 3S
Precipitate does not dissolve in KCN.

Ammonia solution (Dropwise addition) : Ammonium hydroxide first gives white precipitate of Cd(OH)
2
which gets dissolve in excess of reagent forming a soluble complex.
Cd
2+
+ 2 NH
3
+ 2 H
2
O Cd(OH)
2
+ + 2 NH
4
+
Cd(OH)
2
+ + 4 NH
3

[Cd(NH
3
)
4
]
2+
+ 2 OH
.
Potassiumcyanide : Initially a white precipitate of Cd(CN)
2
is formed which in excess of reagent dissolves
forming a soluble complex.
Cd
2+
+ 2 CN

Cd(CN)
2
+
Cd(CN)
2
+ + 2 CN

[Cd(CN)
4
]
2
The colourless soluble complex is not too stable, therefore, reacts with H
2
Sgas forming a yellowprecipitate
of CdS.
[Cd(CN)
4
]
2
+ H
2
S

CdS + + 2 H
+
+ 4 CN
KI forms no precipitate (distinction from Copper)

Sodium hydroxide : White precipitate is obtained which is not soluble in excess of sodium hydroxide.
Cd
2+
(aq) +2NaOH(aq)

Cd(OH)
2
+ + 2Na
+
5. LEAD ION (Pb
2+
) :
2
S in acidic medium : Black precipitate is formed which is soluble in hot dilute
HNO
3
.
Pb
2+
+ H
2
S

PbS + (black) + 2H
+
3PbS + 8HNO
3

3Pb(NO
3
)
2
+ 2NO + 4H
2
O + 3S
Dilute H
2
SO
4
: White precipitate is formed which is soluble in ammonium acetate.
Pb(NO
3
)
2
+ H
2
SO
4

PbSO
4
+ (white) + 2HNO
3
PbSO
4
+ 2CH
3
COONH
4

(CH
3
COO)
2
Pb + (NH
4
)
2
SO
4
Potassium iodide : Yellow precipitate is formed which is soluble in excess more concentrated (6M)
solution of the reagent. Yellow precipitate of PbI
2
is moderately soluble in boiling water to give a colourless
solution.
(CH
3
COO)
2
Pb + 2KI

2CH
3
COOK + PbI
2
+ (yellow)
Potassium dichromate : Yellow precipitate is formed.
(CH
3
COO)
2
Pb + K
2
CrO
4

2CH
3
COOK + PbCrO
4
+ (yellow)
25
CHEMISTRY
IIB Group (As
3+
, Sb
3+
, Sn
2+
, Sn
4+
)
1. ARSENIC ION(As
3+
) :
2
S in acidic medium : Yellow precipitate is formed which is soluble in warm
concentrated nitric acid, sodiumhydroxide solution and yellowammonium sulphide.
2As
3+
+ 3H
2
S
+
H
As
2
S
3
+ + 6H
+
3 As
2
S
3
+ + 28 HNO
3
+ 4 H
2
O 6 AsO
4
3
+ 9 SO
4
2
+ 36 H
+
+ 28 NO |
As
2
S
3
+ + 6OH
AsO
3
3
+ AsS
3
3
+ 3 H
2
O
As
2
S
3
+ +4 S
2
2
2 AsS
4
3
+ S
3
2
Silver nitrate : Yellow precipitate of silver arsenite in neutral solution is formed with AsO
3
3
ions.
AsO
3
3
+ 3 Ag
+
Ag
3
AsO
3
+
AsO
4
3
+ 3 Ag Ag
3
AsO
4
+ (brownish red)
The precipitate is soluble in both nitric acid and ammonia.
Magnesia mixture : White crystalline precipitate of magnesium ammonium arsenate Mg(NH
4
)
AsO
4
.6 H
2
O is formed from neutral or ammonical solution. Upon treating the white precipitate with silver
nitratesolutioncontaining afewdrops of acetic acid, redsilver arsenate is formed(distinction fromphosphate).
H
3
AsO
4
+ MgSO
4
+ 3NH
4
OH Mg(NH
4
)AsO
4
+ + (NH
4
)
2
SO
4
+ 3H
2
O
MgNH
4
AsO
4
+ + 3 Ag
+
Ag
3
AsO
4
+ + Mg
2+
+ NH
4
+
Marsh's test : This test is based on the fact that all soluble compounds of arsenic are reduced by 'nascent'
hydrogen in acid solution to arsine (AsH
3
), a colourless, extremely poisonous gas with a garlic-like odour. If
the gas, mixed with hydrogen, is passed through a heated glass tube, it is decomposed into hydrogen and
metallic arsenic, which is deposited as a brownish-black 'mirror' just beyond the heated part of the tube.
Zn + H
2
SO
4
ZnSO
4
+ 2 [H] ; AsCl
3
+ 3 [H] AsH
3
| + 3 [Cl]
AsO
4
3
+ 4 Zn + 11 H
+
AsH
3
| + 4 Zn
2+
+ 4H
2
O ; AsH
3
|
Heat
As + + 3/2 H
2
|
Ammoniummolybdate test : Solution of AsO
4
3
ion containing considerable excess of HNO
3
on boiling
with reagent gives a yellow crystalline precipitate.
H
3
AsO
4
+ 12(NH
4
)
2
MoO
4
+ 21HNO
3
(NH
4
)
3
AsO
4
. 12MoO
3
+ + 21NH
4
NO
3
+ 12H
2
O
or AsO
4
3
+ 12MoO
4
2
+ 3NH
4
+
+ 24H
+
(NH
4
)
3
AsMo
12
O
40
+ + 12H
2
O.
2. ANTIMONY ION(Sb
3+
) :
2
Sin acidic medium: Aorange red precipitate is formed from mildly acidic solutions.
Sb
3+
+ 3H
2
S
+
H
Sb
2
S
3
+ (orange) + 6H
+
Precipitate is soluble in warm concentrated HCl, in ammonium polysulphide and in alkali hydroxides.
Sb
2
S
3
+ + 6 HCl 2 Sb
3+
+ 6 Cl
+3 H
2
S |
Sb
2
S
3
+ + 4 S
2
2
2 SbS
4
3
+ S
3
2
Sb
2
S
3
+ + 4 OH
SbO
2
+ 3 SbS
2
+ 2 H
2
O
26
CHEMISTRY
Dilution with water : When water is poured in a solution of soluble SbCl
3
, a white precipitate of antimonyl
chloride (SbOCl) is formed, soluble in HCl. With a large excess of water, the hydrated oxide Sb
2
O
3
.xH
2
Ois
produced.
SbCl
3
+ H
2
O SbOCl + 2 HCl
SbO
+
Cl
is soluble in tartaric acid but BiO

+
Cl
is insoluble in tartaric acid.

Sodiumhydroxide or Ammonia solution : White precipitate of hydrate of antimony (III) oxide Sb
2
O
3
.xH
2
O
is soluble in concentrated (5M) solution of caustic alkalies forming antimonites.
2 Sb
3+
+ 6 OH
Sb
2
O
3
+ + 3 H
2
O ; Sb
2
O
3
+ 2 OH
2 SbO
2
+ H
2
O
Potassium iodide solution : Yellow colouration is obtained owing to the formation of a complex salt.
Sb
3+
+ 6 I
[SbI
6
]
3
Reduction with zinc or tin : Sb
3+
ions give black precipitate of metal.
2 Sb
3+
+ 3 Zn 2 Sb + + 3 Zn
2+
; 2 Sb
3+
+ 3 Sn 2 Sb + + 3 Sn
2+
3. TIN (II) ION (Sn
2+
) AND TIN (IV) ION (Sn
4+
) :
2
S in acidic medium :
Brown precipitate is obtained with Sn
2+
which is soluble in concentrated HCl and yellowammoniumsulphide
forming thiostannate but not in colourless ammonium sulphide.
Sn
2+
+ H
2
S SnS + (brown) ; SnS + + S
2
2
SnS
3
2
(thiostannate)
Sn
4+
+ 2H
2
S SnS
2
+ (yellow) + 4 H
+
Precipitate is soluble in concentrated HCl (difference fromAs
3+
and Hg
2+
) and in alkali hydroxide, and also in
ammoniumsulphide and yellowammoniumsulphide.
Sodium hydroxide solution : White precipitate of Sn(OH)
2
is formed which is soluble in excess of
reagent.
Sn
2+
+ 2OH
Sn(OH)
2
+ ; Sn(OH)
2
+ + 2OH
[Sn(OH)
4
]
2
With ammonia solution, white tin (II) hydroxide is precipitated, which cannot be dissolved in excess
ammonia.
Reduction of stannic chloride to stannous chloride by iron filling or granulated zinc :
SnCl
4
+ Zn SnCl
2
+ ZnCl
2
Mercuric chloride solution :
SnCl
2
+ 2HgCl
2
Hg
2
Cl
2
+ (silky white) + SnCl
4
SnCl
2
+ Hg
2
Cl
2
2Hg + (black or grey) + SnCl
4
HNO
3
is not used because it acts as an oxidising agent and in solution it oxidises H
2
S to S according to the
following reaction.
H
2
S + [O]

H
2
O + S + (Yellow)
Example-11 When NaOHsolution is mixed with aqueous solution of a salt 'A', and warmed, a black precipitate is
formed. Black precipitate is filtered and dissolved in concentrated HNO
3
by boiling. The resulting
solution gives a chocolate brown coloured precipitate with potassium ferrocyanide solution. The
filtrate obtained after filtering off the black precipitate, upon warming with Zn and NaOH evolves an
alkaline pungent smelling gas. The resulting solution also responds to the brown ring test. The
filtrate does not evolve N
2
gas when it is boiled with urea in the presence of H
2
SO
4
. Identify the cation
and anion present in the salt 'A'.
Solution Cu(NO
3
)
2
+ NaOH Cu(OH)
2
+(blue) + 2NaNO
3
Cu(OH)
2
+
A
CuO+ (black) + H
2
O
4Zn + NaNO
3
+ 7NaOH 4Na
2
ZnO
2
+ 2H
2
O+ NH
3
| (pungent smelling alkaline gas).
CuO+ 2HNO
3

A
Cu(NO
3
)
2
+ H
2
O
2Cu(NO
3
)
2
+ K
4
[Fe(CN)
6
] Cu
2
[Fe(CN)
6
] + (chocolate brown) + 4KNO
3
27
CHEMISTRY
Example-12 Select the correct statements from the following.
(A) Bi
3+
iongives black precipitatewithKI whichdissolves inexcess of KI formingorangecolouredsolution.
(B) Chloride of Cd
2+
is not soluble in excess of NaOH but soluble in excess of aqueous ammonia.
(C) Lead sulphate is soluble in ammonium acetate solution.
(D) The Co
2+
gives green coloured solution with KNO
2
and acetic acid.
(E) The red colour solution of ferric acetate turns to reddish brown precipitate when it is diluted with
water and then boiled.
Solution (A) Bi
3+
+ 3KI

BiI
3
+ (black) + 3K
+
; KI + BiI
3

K [BiI
4
] (orange)
(B) CdCl
2
+ 2NaOH

Cd(OH)
2
+ (white) + 2NaCl ; Cd(OH)
2
+ + NaOH

no reaction
CdCl
2
+ 2NH
4
OH

Cd(OH)
2
+ (white) + 2NH
4
Cl
Cd(OH)
2
+ 4NH
4
OH

[Cd(NH
3
)
4
] (OH)
2
(soluble) + 4H
2
O
(C) PbSO
4
+ 2CH
3
COONH
4

(CH
3
COO)
2
Pb (soluble) + (NH
4
)
2
SO
4
(D) CoCl
2
+7KNO
2
+ 2CH
3
COOH

K
3
[Co(NO
2
)
6
] +(yellow) + 2KCl +2CH
3
COOK+ NO+H
2
O
(E) Fe (CH
3
COO)
3
+ 2H
2
O
Boil
Fe (CH
3
COO) (OH)
2
+ (reddish brown) + 2 CH
3
COOH
Therefore, A, B, C and E are correct statements.
Example-13 Assertion : In aqueous solution, HgCl
2
and SnCl
2
can exist as Hg
2+
and Sn
2+
ions.
Reason : SnCl
2
acts as strong oxidising agent.
(A) BothAssertion and Reason are true and Reason is the correct explanation of Assertion.
(B) Both Assertion and Reason are true but Reason is not correct explanation of Assertion
(C) Assertion is true but Reason is false
(D) Assertion is false but Reason is true
(E) Assertion and Reason both are false.
Solution Sn
II
Cl
2
(excess) + Hg
II
Cl
2

Hg
0
+ (black) + Sn
IV
Cl
4
SnCl
2
and HgCl
2
can not exist together in aqueous solution because SnCl
2
acts as strong reducing
agent because Sn showinert pair effect.
Therefore, (E) option is correct.
III
rd
Group (Al
3+
, Cr
3+
, Fe
3+
)
28
CHEMISTRY
Concentrated HNO
3
is added to oxidise Fe
2+
to Fe
3+
if present.
Solid NH
4
Cl should be added in excess other wise cations like Zn, Mn, Mg may be precipitated here.
To much excess of NH
4
Cl should be avoided other wise Cr is not precipitated andAl may form a
colloidal solution.
1. ALUMINIUM ION (Al
3+
) :
Precipitation with NH
4
OH in presence of NH
4
Cl : White gelatinous precipitate is formed which is
slightly soluble in excess reagent. The solubility is decreased in the presence of ammonium salt. A small
portion of the precipitate passes into the solution as colloidal Al(OH)
3
(Aluminium hydroxide sol), the sol is
coagulated on boiling the solution or upon the addition of soluble salt yielding a precipitate of Al(OH)
3
, known
as Al(OH)
3
gel. For complete precipitation, add ammonia solution in excess and the mixture is boiled until,
the solution has a slight odour of NH
3
.
Al
3+
+ 3NH
4
OH
Cl NH
4
Al(OH)
3
+ + 3NH
4
+
Sodium hydroxide : A solution containing Al
+3
ions give a white precipitate with the reagent.
Al
3+
+ 3OH
Al(OH)
3
+
White precipitate dissolves in excess sodium hydroxide according to following reaction.
Al(OH)
3
+ OH
[Al(OH)
4
]
The reaction is reversible and any reagent, which will reduce the hydroxyl ion concentration sufficiently
shouldcausethe reactiontoproceedfromright toleft with theconsequent precipitationof aluminiumhydroxide.
This may be effected with a solution of ammoniumchloride (the hydroxyl ion concentration is reduced owing
to the formation of the weak base ammonia , which can be readily removed as ammonia gas by heating) or
by the addition of acid ; in the latter case, a large excess of acid causes the precipitated hydroxide to
redissolve.
[Al(OH)
4
]
+ NH
4
+
Al(OH)
3
+ + NH
3
| + H
2
O
[Al(OH)
4
]
+ H
+
Al(OH)
3
+ + H
2
O
Al(OH)
3
+ 3H
+
(excess) Al
3+
+ 3 H
2
O
Lake test :
AlCl
3
+ 3NH
4
OH Al(OH)
3
+ (white) + 3 NH
4
Cl
The precipitation of aluminium hydroxide is done in presence of blue litmus. Originally the solution will
appear red when the group precipitate is dissolved in HCl as blue litmus turns red in acid medium. On adding
large excess of NH
4
OH, Al(OH)
3
will be reprecipitated and will adsorb the litmus as it is flocculent by nature.
After a while a blue mass will be seen floating in a colourless solution as all the colour from the solution will
adsorbed.
Sodiumacetate solution : No precipitate is obtained in cold , neutral solution but on boiling with excess
reagent, a voluminous precipitate of basic aluminium acetate is formed.
Al
3+
+ 3 CH
3
COO
+ 2 H
2
O Al(OH)
2
CH
3
COO+ (white basic salt) + CH
3
COOH
Disodiumhydrogen phosphate solution : Awhite gelatinous precipitate is formed.
Al
3+
+ HPO
4
2
AlPO
4
+ + H
+
The reaction is reversible; strong acids dissolves the precipitate. However, the precipitate is insoluble in
acetic acid (difference from phosphates of alkaline earths, which are soluble). The precipitate can also be
dissolved in sodiumhydroxide.
Dry test : Aluminiumcompounds when heated with sodiumcarbonate upon charcoal gives a white infusible
solid, which glows when hot. If the residue is moistened with a little cobalt nitrate solution and again heated,
a blue infusible mass is obtained.
2 Al
2
O
3
+ 2 Co
2+
+ 4 NO
3
2 CoAl
2
O
4
(thenard blue) + 4NO
2
| + O
2
|
Use of excess cobalt nitrate solution should be avoided since this will produce black cobalt oxide (Co
3
O
4
)
upon ignition, which will mask the blue colour.
29
CHEMISTRY
2. IRON ION (Fe
3+
) :
4
OHin presence of NH
4
Cl : Gelatinous reddish brown precipitate is formed which
is insoluble in excess reagent but soluble in acids.
Fe
3+
+ 3NH
4
OH
Cl NH
4
Fe(OH)
3
+ + 3NH
4
+
Precipitation of iron(II) hydroxide occurs with ammonia solution. If larger amounts of ammoniumions
are present, the dissociation of NH
4
OHis suppressed and the concentration of OH
ions is lowered
to such an extent that solubility product of iron (II) hydroxide, Fe(OH)
2
is not attained and precipitation
does not occur.
K
sp
of iron(III) hydroxide is so small (3.8 10
38
) that complete precipitation take place even in the
presence of ammonium salts.
Fe(OH)
3

Heat
Fe
2
O
3
+ 3 H
2
O
Oxide is soluble with difficulty in dilute acids but dissolves on vigorous boiling with concentrated HCl.
Fe
2
O
3
+ 6 H
+

2 Fe
3+
+ 3 H
2
O
Sodiumhydroxide solution : Reddish brown precipitate is formed insoluble in excess reagent (distinction
fromaluminiumand chromium).
Fe
3+
+ 3OH

Fe(OH)
3
+
H
2
S gas in acidic solution : Fe
3+
reduces to Fe
2+
.
2 Fe
3+
+ H
2
S

2 Fe
2+
+ 2H
+
+ S + (milky-white)
If a neutral solution of iron (III) chloride is added to a freshly prepared saturated solution of H
2
S , bluish
colouration appears first, followed by precipitation of sulphur. The blue colour is due to a colloidal solution of
sulphur of extremely small particle size.
This reaction can be used to test the freshness of H
2
S solution.
Ammoniumsulphide solution : Black precipitate consisting of Fe(II) sulphide and sulphur is formed.
2 Fe
3+
+ 3 S
2

2 FeS + S +
In HCl, the black precipitate of Fe(II) sulphide dissolves and white precipitate of sulphur becomes visible.
FeS + + 2H
+

H
2
S | + Fe
2+
The damp iron (II) sulphide precipitate, when exposed to air, is slowly oxidised to brown iron(III)
hydroxide.
4 FeS + + 6 H
2
O + 3 O
2

4 Fe(OH)
3
+ + 4S +
Fromalkaline solutions of ammonium sulphide, black iron(III) sulphide is obtained.
2 Fe
3+
+ 3S
2
Fe
2
S
3
+
On acidification with hydrochloric acid, iron (III) ions are reduced to iron (II) ions and sulphur is formed.
Fe
2
S
3
+ + 4H
+
2 Fe
2+
+ 2 H
2
S | + S +
Potassium ferrocyanide (Potassium hexacyanidoferrate(II) ) : Intense blue precipitate (Prussian
blue) of iron(III) hexacyanidoferrate(II) is formed.
4Fe
3+
+ 3 [Fe(CN)
6
]
4

Fe
4
[Fe(CN)
6
]
3
+
This is insoluble in dilute acids but decomposes in concentrated HCl. Alarge excess of the reagent dissolves
it partly or entirely, when an intense blue solution is obtained. Sodium hydroxide turns the precipitate red.
Fe
4
[Fe(CN)
6
]
3
+ + 12 OH

Fe(OH)
3
+ + 3[Fe(CN)
6
]
4
Oxalic acid also dissolves Prussian blue forming a blue-solution.
Important :
If iron(III) chloride is added to an excess of potassiumhexacyanidoferrate (II), a product with the composition
of K Fe[Fe(CN)
6
] is formed. This tends to form colloidal solutions ("soluble Prussian blue") and can not be
filtered.
Potassium ferricyanide (Potassium hexacyanidoferrate(III)) : Abrown colouration is formed.
Fe
3+
+ [Fe(CN)
6
]
3

Fe[Fe(CN)
6
]
Upon adding hydrogen peroxide or some tin(II) chloride solution, the hexacyanidoferrate(III) part of
the compound is reduced and Prussian blue is precipitated.
Fe
2+
gives dark blue precipitate with potassiumferricyanide. First hexacyanidoferrate(III) ions oxidise
iron(II) to iron(III), when hexacyanidoferrate(II) is formed.
Fe
2+
+ [Fe(CN)
6
]
3

Fe
3+
+ [Fe(CN)
6
]
4
and these ions combine to form a precipitate called Turnbull's blue.
4 Fe
3+
+ 3 [Fe(CN)
6
]
4

Fe
4
[Fe(CN)
6
]
3
30
CHEMISTRY
Note : Composition of this precipitate is identical to that of Prussian blue. Earlier the composition suggested was
Fe
3
[Fe(CN)
6
]
2
, hence different name.
3Fe
2+
+ 2K
3
[Fe(CN)
6
] Fe
3
[Fe (CN)
6
]
2
(ferrous ferric cyanide) + 6K
+
Turnbull's blue
Fe(II) in ammonical solution gives red solution with DMG colouration fades on standing due to the
oxidation of the iron(II) complex. Fe (III) does not give such complex.
Incompleteabsenceof air, Fe(II) ions produces whiteprecipitatewithpotassiumhexacyanidoferrate(II).
Fe
2+
+ 2K
+
+ [Fe(CN)
6
]
4
K
2
Fe [Fe(CN)
6
] +
Under ordinary atmospheric conditions a paleblue precipitate is formed.
Potassiumthiocyanate (Potassiumsulphocyanide) : In slightly acidic medium, a deep red colouration
is produced due to the formation of a non-dissociated iron(III) thiocyanate complex.
Fe
3+
+ 3 SCN
Fe(SCN)
3
This neutral molecule can be extracted by ether or amyl alcohol.
With pure Fe(II) ions no colouration is obtained.
Fluorides and Hg(II) ions bleach the red colour.
Fe(SCN)
3
+ 6F
[FeF
6
]
3
+ 3 SCN
2 Fe(SCN)
3
+ 3Hg
2+
2 Fe
3+
+ 3 Hg (SCN)
2
Sodium acetate solution : A reddishbrown colouration is obtained owing to the formation of
[Fe
3
(OH)
2
(CH
3
COO)
6
]
+
. The reaction becomes complete only if the strong acid which is formed, is removed
by the addition of an excess of the reagent, which acts as a buffer.
3 Fe
3+
+ 6 CH
3
COOH+ 2 H
2
O [Fe
3
(OH)
2
(CH
3
COO)
6
]
+
+ 2H
+
This reddishbrown coloured solution on dilution with water and boiling gives reddish brown precipitate of
basic ferric acetate.
[Fe
3
(OH)
2
(CH
3
COO)
6
]
+
+ 4 H
2
O 3 Fe(OH)
2
CH
3
COO+ + 3 CH
3
COOH+ H
+
The excess of acetate ion acts as a buffer and the reaction goes to completion.
Disodiumhydrogen phosphate solution : Ayellowishwhite precipitate is formed.
Fe
3+
+ HPO
4
2
FePO
4
+ + H
+
The reaction is reversible, because a strong acid is formed which dissolves the precipitate. It is advisable to
add small amounts of sodium acetate, which acts as a buffer.
3. CHROMIUMION(Cr
3+
) :
4
OH in presence of NH
4
Cl : A grey-green to green gelatinous precipitate is
formed.
Cr
3+
+ 3 NH
3
+ 3 H
2
O Cr(OH)
3
+ + 3 NH
4
+
Precipitate is slightly soluble in excess of reagent in cold forming pink or violet coloured solution. On boiling
the solution, chromium hydroxide is reprecipitated.
Cr(OH)
3
+ + 6 NH
3
[Cr(NH
3
)
6
]
3+
+ 3OH
Sodium hydroxide solution : Agreen precipitate is formed.

Cr
3+
+ 3 OH
Cr(OH)
3
+
The reaction is reversible. On addition of acids the precipitate dissolves. In excess of reagent the precipitate
dissolves readily forming chromites, the solution is green. The reaction is reversible ; on (slight) acidification
and also on boiling green precipitate of chromium(III) hydroxide is obtained.
Cr(OH)
3
+ OH
[Cr(OH)
4
]
On adding H
2
O
2
to the alkaline solution of [Cr(OH)
4
]
, a yellow solution is obtained.

2 [Cr(OH)
4
]
+ 3 H
2
O
2
+ 2 OH
2 CrO
4
2
+ 8 H
2
O
The green precipitate of Cr(OH)
3
can be dissolved by using any of the following methods.
(A) Fusion with fusion mixture (Na
2
CO
3
+ KNO
3
)
2 Cr(OH)
3
+ 2Na
2
CO
3
+ 3 KNO
3
2 Na
2
CrO
4
+ 3 KNO
2
+ 2 CO
2
+ 3 H
2
O
Fused mass on extraction with water gives yellow solution of Na
2
CrO
4 .
31
CHEMISTRY
(B) 2 Cr(OH)
3
+ 3 Na
2
O
2
2Na
2
CrO
4
+ 2NaOH + H
2
O
(C) Precipitate is heated with NaOHand bromine water.
2NaOH + Br
2
NaOBr + NaBr + H
2
O ; NaOBr NaBr + [O]
2Cr(OH)
3
+ 4NaOH + 3[O] 2Na
2
CrO
4
+ 5H
2
O.
The yellow solution of Na
2
CrO
4
gave the following reactions with lead acetate, barium chloride and silver
nitrate solutions.
(a) Lead acetate solution : Yellow precipitate is formed.
CrO
4
2
+ Pb
2+

OOH CH
3
PbCrO
4
+
(b) Barium chloride solution : Yellow precipitate is formed owing to the formation of barium chromate
which is insoluble in acetic acid.
CrO
4
2
+ Ba
2+
BaCrO
4
+
(c) Silver nitrate solution : Red/Brick red precipitate is formed owing to the formation of silver chromate
which is soluble in ammonia solution and its acidified solution turns to orange because of the formation of
dichromate.
Na
2
CrO
4
+ 2AgNO
3
Ag
2
CrO
4
+ + 2NaNO
3
.
Acidified H
2
O
2
test : On acidifying the yellow solution with dilute sulphuric acid and adding few drops of
ether or amyl alcohol to the mixture and finally adding some hydrogen peroxide, blue colouration is formed
which can be extracted into the organic layer by gently shaking.
Na
2
CrO
4
+ H
2
SO
4
Na
2
SO
4
+ H
2
CrO
4
; H
2
CrO
4
+ 2H
2
O
2

alcohol Amyl
CrO
5
(blue colouration) + H
2
O
Blue colouration fades slowly due to the decomposition of perchromic acid (or chromium peroxide ) with the
liberation of oxygen.
4CrO
5
+ 6H
2
SO
4
2Cr
2
(SO
4
)
3
+ 7O
2
+ 6H
2
O
1,5Diphenylcarbazide test : In dilute mineral acid solution the reagent produces a soluble violet colour
with chromate. During the reaction, chromate is reduced to chromium(III) and diphenylcarbazone is formed;
these reaction products in turn produce a complex with the characteristic colour.
Phenanthroline test : Green precipitate dissolved in dilute HCl (minimum quantity) gives red colouration
with the reagent.
Example-14 A black coloured compound (A) on reaction with dil. H
2
SO
4
gives a gas (B) and a yellow colour
solution. The gas (B) on passing in a solution of an acid (C) gives a white/yellow turbidity (D). Gas
(B) when passed in acidified solution of (E) gives a precipitate (F) soluble in dil HNO
3
. After boiling
this solution when excess of NH
4
OH is added, a blue coloured compound (G) is formed. To this
solution on addition of acetic acid and aqueous potassium ferrocyanide a chocolate coloured
precipitate (H) is obtained. On addition of an aqueous solution of BaCl
2
to an aqueous solution of (E),
a white precipitate insoluble in HNO
3
is obtained. Yellowcolour solution on reaction with ammonium
hydroxide in presence of air gives reddish brown precipitate. Identify (A) to (H).
Solution FeS (A) + H
2
SO
4
FeSO
4
+ H
2
S (B)
HNO
3
(C) NO
2
+ H
2
O + O ; H
2
S + O H
2
O + S + (D)
CuSO
4
(E) + H
2
S CuS + (F) + H
2
SO
4
.
3CuS + 8HNO
3
3Cu(NO
3
)
2
+ 2NO | + 4H
2
O + 3S +
Cu
2+
+ 4NH
3
[Cu(NH
3
)
4
]
2+
(G).
32
CHEMISTRY
2Cu
2+
+ K
4
Fe(CN)
6

Cu
2
[Fe(CN)
6
] + (H) + 4K
+
Ba
2+
+ SO
4
2

BaSO
4
+ (white)
Fe
2+
+ 2H
+
+ O

Fe
3+
+ H
2
O
Fe
3+
+ 3NH
3
+ 3H
2
O

Fe(OH)
3
+ (reddish brown) + 3NH
4
+
Hence, (A) = FeS; (B) = H
2
S; (C) = HNO
3
; (D) = S ; (E) = CuSO
4
; (F) = CuS ; (G) [Cu(NH
3
)
4
](NO
3
)
2
;
(H) Cu
2
[Fe(CN)
6
]
Example-15 Thenard's blue is :
(A) CoAl
2
O
4
(B) Fe
4
(Fe(CN)
6
)
3
(C) Fe
2
[Fe(CN)
6
]
3
(D) [Ni(NH
3
)
6
](OH)
2
Solution CoO+Al
2
O
3

A
CoO. Al
2
O
3
(Thenard's blue or cobalt meta-aluminate)
It is cobalt nitrate test.
Therefore, (A) option is correct.
IV
th
GROUP (Zn
2+
, Mn
2+
, Ni
2+
, Co
2+
) :
33
CHEMISTRY
1. MANGANESEION(Mn
2+
) :
2
S in presence of NH
4
OH + NH
4
Cl : A buff coloured (light pink) precipitate is
formed.
Mn
2+
+ S
2
MnS +
It is readily soluble in mineral acids (distinction with Ni and Co) and even in acetic acid (distinction with Ni,
Co and Zn).
MnS + + 2H
+
Mn
2+
+ H
2
S| ; MnS + + 2 CH
3
COOH Mn
2+
+ H
2
S | + 2 CH
3
COO
Ammonia solution : Partial precipitation of white manganese(II) hydroxide takes place.

Mn
2+
+ 2 NH
3
+ 2H
2
O Mn(OH)
2
+ + 2 NH
4
+
The precipitate is soluble in ammonium salts when the reaction proceeds towards left.
Sodium hydroxide solution : Initially white precipitate of Mn(OH)
2
is formed which is insoluble in
excess reagent and rapidly oxidised on exposure to air, becoming brown.
Mn
2+
+ 2 OH
Mn(OH)
2
+
Mn(OH)
2
+ + O
2
2 MnO(OH)
2
+ (hydrated manganese dioxide).
With sodium hydroxide and bromine water initially a white precipitate is formed which immediately
turns to black owing to the formation of MnO
2
.
Mn(OH)
2
+ + Br
2
+ 2NaOH MnO
2
+ (black) + 2NaBr + 2H
2
O
Mn(OH)
2
+ + H
2
O
2
MnO(OH)
2
+ (brown) + H
2
O
Lead dioxide(PbO
2
) and concentrated nitric acid : On boiling a dilute solution of manganese(II) ions
with lead dioxide and a little concentrated nitric acid and allowing the suspended solid containing unattacked
lead dioxide to settle, the supernatant liquid acquired a violet-red (or purple) colour due to permanganic acid.
5 PbO
2
+ 2 Mn
2+
+ 4H
+
2 MnO
4
+ 5Pb
2+
+ 2 H
2
O
Sodiumbismuthate (NaBiO
3
) solution : When sodium bismuthate (NaBiO
3
) is added to a cold solution
of manganese(II) ions in dilute nitric acid or in dilute sulphuric acid and the mixture stirred and then excess
reagent filtered off, a violetred (or purple) solution of permanganate is produced.
2 Mn
2+
+ 5 NaBiO
3
+ 14 H
+
2MnO
4
+ 5 Bi
3+
+ 5 Na
+
+ 7 H
2
O
2Mn(NO
3
)
2
+ 2Pb
3
O
4
+ 26HNO
3

A
2HMnO
4
(violetred/purple) + 15Pb(NO
3
)
2
+ 12H
2
O
Disodium hydrogen phosphate solution : A pink precipitate of Mn(NH
4
) PO
4
. 7 H
2
O is formed in
presence of ammonia or ammoniumions.
Mn
2+
+ NH
3
+ HPO
4
2
Mn(NH
4
)PO
4
+
If ammonium salts are absent, pink precipitate of manganese(II) phosphate is formed.
3 Mn
2+
+ HPO
4
2
Mn
3
(PO
4
)
2
+ + 2 H
+
Both precipitates are soluble in acids.
2. ZINCION(Zn
2+
) :
2
S in presence of NH
4
OH + NH
4
Cl : A white precipitate is formed. In neutral
solutions, precipitation is partial as H
+
ions concentration produced depressed the ionisation of H
2
S .
Zn
2+
+ H
2
S ZnS +
The precipitate is soluble in dilute HCl.
ZnS + 2H
+
Zn
2+
+ H
2
S |
Sodium hydroxide solution : A white gelatinous precipitate is formed.
Zn
2+
+ 2 OH
Zn(OH)
2
+
The precipitate is soluble in acids as well as in excess of the reagent.
Zn(OH)
2
+ 2 H
+
Zn
2+
+ 2 H
2
O
Zn(OH)
2
+ 2 OH
[Zn(OH)
4
]
2
Thus, zinc hydroxide is amphoteric in nature.
[Zn(OH)
4
]
2
+ S
2
ZnS + (white) + 4 OH
Ammonia solution : A white gelatinous precipitate is formed which is readily soluble in excess of the
reagent and in solutions of ammonium salts forming the tetraamminezinc(II).
Nonprecipitation of Zn(OH)
2
by ammonia solution in the presence of NH
4
Cl is due to the lowering of OH
ion
concentration to such a value that the K
sp
of Zn(OH)
2
is not attained.
Zn
2+
+ 2 NH
3
+ 2 H
2
O Zn(OH)
2
+ + 2 NH
4
+
Zn(OH)
2
+ + 4 NH
3
[Zn(NH
3
)
4
]
2+
+ 2 OH
34
CHEMISTRY
Disodiumhydrogen phosphate solution : White precipitate of zinc phosphate is formed.
3 Zn
2+
+ HPO
4
2
Zn
3
(PO
4
)
2
+ + 2H
+
In presence of ammoniumions zinc ammonium phosphate is formed.
Zn
2+
+ NH
4
+
+ HPO
4
2
Zn(NH
4
) PO
4
+ + H
+
Both precipitates are soluble in dilute acids, when the reactions are reversed.
Both precipitates are soluble in ammonia :
Zn
3
(PO
4
)
2
+ 12 NH
3

3 [Zn(NH
3
)
4
]
2+
+ 2 PO
4
3
Zn(NH
4
)PO
4
+ 3 NH
3

[Zn(NH
3
)
4
]
2+
+ HPO
4
2
Potassiumferrocyanide (Potassiumhexacyanidoferrate(II)) solution : Awhite precipitate of variable
composition is formed. If excess reagent is added, the composition of precipitate is K
2
Zn
3
[Fe(CN)
6
]
2
.
3 Zn
2+
+ 2 K
+
+ 2 [Fe(CN)
6
]
4

K
2
Zn
3
[Fe(CN)
6
]
2
+
The precipitate is insoluble in dilute acids, but dissolves in sodium hydroxide readily.
K
2
Zn
3
[Fe(CN)
6
]
2
+ 12 OH

2 [Fe(CN)
6
]
4
+ 3 [Zn(OH)
4
]
2
This reaction can be used to distinguish zinc from aluminium.
Ammonium tetrathiocyanatomercurate(II) copper sulphate test : Test solution faintly acidic with a
fewdrops of MH
2
SO
4
or 2MCH
3
COOHand 0.1 mL of 0.25 MCuSO
4
solution followed by2 mL of the reagent
produces a violet precipitate. Zinc ions alone forms a white precipitate with the reagent in the absence of
copper ions.
Zn
2+
+ [Hg(SCN)
4
]
2

Zn [Hg(SCN)
4
] + .
In the presence of the copper ions, the copper complex coprecipitated with that of zinc and the violet (or
blackishpurple) precipitate consists of mixed crystals of Zn[Hg(SCN)
4
] + Cu[Hg(SCN)
4
].
Diphenylthiocarbazone (dithizone) test : Dithizone forms complexes with a number of metal ions,
which can be extracted with chloroform. The zinc complex, formed in neutral, alkaline or acetic acid solutions,
is red in colour.
3. COBALT ION (Co
2+
) :
2
S in presence of NH
4
OH + NH
4
Cl : A black precipitate is formed. The black
precipitate of CoS is insoluble in dilute HCl or acetic acid but hot concentrated HNO
3
or aquaregia dissolves
it and white sulphur remains. On longer heating the mixture becomes clear as because sulphur is oxidised
to sulphate.
2[Co(NH
3
)
6
]
3+
+ 3S
2

2CoS + + 12NH
3
+ S
or CoCl
2
+ H
2
S
OH NH
4
CoS + + 2HCl
3 CoS + 2 HNO
3
+ 6 H
+
3 Co
2+
+ 3 S + + 2NO | + 4 H
2
O
2CoS + 6HCl + 2HNO
3
3CoCl
2
+ 2NO + 3S + 4H
2
O
Solution on evaporation to dryness gives blue residue (CoCl
2
) which turns pink on adding water.
Potassiumnitrite solution : Ayellow precipitate is formed from neutral solution of cobalt(II) ions.
CoCl
2
+ 7KNO
2
+ 2CH
3
COOH

K
3
[Co(NO
2
)
6
] + + H
2
O+ 2KCl + 2CH
3
COOK + NO|
or Co
2+
+ 7NO
2
+ 2H
+
+ 3K
+

K
3
[Co(NO
2
)
6
] + + NO | + H
2
O.
Ammoniumthiocyanate solution : Aneutral or acid solution of cobalt(II) gives a blue colouration in amyl
alcohol or ether layer when a few crystals of ammonium thiocyanate are added.
Co
2+
+ 4 SCN

[Co(SCN)
4
]
2
In amyl alcohol or ether, the free acid H
2
[Co(SCN)
4
] is formed and dissolved by the organic solvent
(distinction from nickel)
Sodium bicarbonate and bromine water test : To the test solution sodium bicarbonate is added in
excess followed by the bromine water. The mixture is slightly heated, the solution turns apple green.
CoCl
2
+ 2NaHCO
3
Co(HCO
3
)
2
+ 2NaCl
Co(HCO
3
)
2
+ 4 NaHCO
3
Na
4
[Co(CO
3
)
3
] + 3H
2
O+ 3CO
2
Br
2
+ H
2
O 2HBr + [O]
2Na
4
[Co(CO
3
)
3
] + H
2
O+ [O] 2Na
3
[Co(CO
3
)
3
] (green) + 2NaOH.
Green solution of sodium cobalticarbonate is obtained.

Sodium hydroxide solution : Cobalt(II) nitrate in cold gives a blue basic salt.
Co
2+
+ OH
+ NO
3

Co(OH)NO
3
+
Upon warming with excess alkali, the basic salt is converted into a pink precipitate of Co(II) hydroxide.
Co(OH)NO
3
+ + OH

Co(OH)
2
+ + NO
3
35
CHEMISTRY
Ammonia solution : In absence of ammonium salt, its small amount precipitates a blue basic salt.
Co
2+
+ NH
3
+ H
2
O + NO
3

Co(OH)NO
3
+ + NH
4
+
The excess of the reagent dissolves the precipitate, when hexaamminecobalt(II) ions are formed.
Co(OH)NO
3
+ + 6 NH
3

[Co(NH
3
)
6
]
2+
+ NO
3
+ OH
Potassium cyanide solution :

Co
2+
+ 2 CN

Co(CN)
2
+ (reddish brown / buff coloured)
In excess of reagent, a brown solution of a soluble complex is formed.
Co(CN)
2
+ + 4 CN

[Co(CN)
6
]
4
On acidification precipitate reappears.
[Co(CN)
6
]
4
+ 4 H
+
(cold and dilute)

Co(CN)
2
+ + 4HCN |
If brown solution is boiled for a longer time in air or some H

2
O
2
is added and solution is heated it
turns yellow.
4 [Co(CN)
6
]
4
+ O
2
+ 2 H
2
O

4 [Co(CN)
6
]
3
(yellow solution) + 4 OH
2 [Co(CN)
6
]
4
+ H
2
O
2

2 [Co(CN)
6
]
3
(yellow solution) + 2 OH
4. NICKEL ION(Ni
2+
) :
2
S in presence of NH
4
OH + NH
4
Cl :
A black precipitate is formed which is insoluble in cold dilute HCl and CH
3
COOH but dissolves in hot
concentrated HNO
3
and in aquaregia.
NiCl
2
+ H
2
S
OH NH
4
NiS + (Black) + 2HCl
3 NiS + + 2 HNO
3
+ 6 H
+

3 Ni
2+
+ 2 NO | + 3 S + + 4 H
2
O
NiS + HNO
3
+ 3HCl

Ni
2+
+ S + + NOCl | + 2Cl
+ 2H
2
O.
Solution on evaporation to dryness gives yellowresidue (NiCl

2
) which turns green on adding water.
Dimethylglyoxime reagent : A red precipitate is obtained from the solution just made alkaline or acid
solutions buffered with sodium acetate.
NiCl
2
+ 2NH
4
OH+ 2CH
3
C= NOH (C
4
H
7
N
2
O
2
)
2
Ni + + 2NH
4
Cl +2H
2
O
(red) |
CH
3
C = NOH
Fe(II) ions give red colouration, bismuth gives yellowprecipitate and cobalt gives brown colouration
with DMG in ammonical solutions.
Bromine water test (alkaline medium) : A black precipitate of Ni
2
O
3
is formed.
NiCl
2
+ 2NaOH (excess) Ni(OH)
2
+ (green) + 2 NaCl
Green precipitate is formed which gradually turns black on adding bromine water.
Br
2
+ H
2
O 2HBr + [O] ; 2Ni(OH)
2
+ H
2
O+ [O] 2 Ni(OH)
3
+
A
Ni
2
O
3
+ + 3H
2
O
(black)
Ni
2+
gives black precipitate (Ni
2
O
3
) with sodium bicarbonate and bromine water on heating where as
Co
2+
gives green coloured solution, this is the point of difference.
NiCl
2
+ 2NaHCO
3
NiCO
3
+ 2NaCl + H
2
O ; 2NiCO
3
+ [O] Ni
2
O
3
+ (black) + 2CO
2
Cyanide test : A green precipitate is formed which dissolves in excess of reagent forming a yellow
coloured solution.
NiCl
2
+ 2KCN Ni(CN)
2
+
+ 2KCl ;
Ni(CN)
2
+ 2KCN K
2
[Ni(CN)
4
] ;
Complex on heatingwithsodiumhypobromite(NaOH+Br
2
water) solutiongives ablack precipitate(distinction
fromcobalt).
NaOH + Br
2
NaBrO + HBr
2K
2
[Ni(CN)
4
] + 4NaOH + 9NaBrO
boil
4NaCNO+ 9NaBr + Ni
2
O
3
+
(black) + 4KCNO+2H
2
O
36
CHEMISTRY
V
th
Group (Ba
2+
, Sr
2+
, Ca
2+
) :
IVGroup filtrate

Boil off H
2
S then add (NH
4
)
2
CO
3
(aq), NH
4
OH & NH
4
Cl (s)
White precipitate Filtrate,
(BaCO
3
, SrCO
3
or CaCO
3
). move for VI group.

+
Dissolve in CH
3
COOHand divide into three parts
and test in the sequence given below.
I part + K
2
CrO
4
. II Part + (NH
4
)
2
SO
4
. III part + (NH
4
)
2
C
2
O
4
.
+ + +
Yellowprecipitate White precipitate White precipitate
(BaCrO
4
insoluble in CH
3
COOH). (SrSO
4
). (CaC
2
O
4
).
1.BARIUM ION ( Ba
2+
) :
Precipitation with (NH
4
)
2
CO
3
in presence of NH
4
OH + NH
4
Cl : Awhite precipitate is formed which is
soluble in acetic acid and dilute mineral acids
BaCl
2
+ (NH
4
)
2
CO
3
BaCO
3
+ + 2NH
4
Cl
BaCO
3
+ 2CH
3
COOH Ba (CH
3
COO)
2
+ H
2
O+ CO
2
Potassium chromate test : Ayellow precipitate is formed, practically insoluble in water
Ba(CH
3
COO)
2
+ K
2
CrO
4
BaCrO
4
+ + 2CH
3
COOK
Precipitate is insoluble in dilute acetic acid (distinction from strontium and calcium) but readily
soluble in mineral acids.
Addition of acid to K
2
CrO
4
changes the yellow colour of the solution to reddishorange due to the
formation of dichromate.
2 H
+
+ 2 CrO
4
2
Cr
2
O
7
2
+ H
2
O
The solubility products of SrCrO
4
and CaCrO
4
are much larger than for BaCrO
4
and hence they
require a larger CrO
4
2
ion concentration to precipitate them. The addition of acetic acid to the
K
2
CrO
4
solution lowers the CrO
4
2
ion concentration sufficiently to prevent the precipitation of SrCrO
4
and CaCrO
4
but it is maintained high enough to precipitate BaCrO
4
.
2. STRONTIUMION(Sr
2+
) :
4
)
2
CO
3
in presence of NH
4
OH + NH
4
Cl :
A white precipitate is formed which is soluble in acetic acid.
SrCl
2
+ (NH
4
)
2
CO
3
SrCO
3
+ + 2NH
4
Cl
SrCO
3
+ 2CH
3
COOH Sr(CH
3
COO)
2
+ H
2
O+ CO
2
Ammonium sulphate solution : A white precipitate is formed which is slightly soluble in boiling
hydrochloric acid.
Sr(CH
3
COO)
2
+ (NH
4
)
2
SO
4
SrSO
4
+ + 2CH
3
COONH
4
The solubility of the precipitate in water is low but not negligible.
The precipitate is insolublein ammoniumsulphate solution even on boiling (Distinction fromcalcium
forms a soluble complex (NH
4
)
2
[Ca(SO
4
)
2
]) and slightly soluble in boiling HCl.
It is almost completely converted into the corresponding carbonates by boiling with a concentrated
solution of sodium carbonate.
SrSO
4
+ CO
3
2
SrCO
3
+ + SO
4
2
37
CHEMISTRY
3. CALCIUMION (Ca
2+
) :
4
)
2
CO
3
in presence of NH
4
OH + NH
4
Cl : A white precipitate is formed. The
precipitate is soluble in water which contains excess carbonic acid (e.g freshly prepared soda water) because
of the formation of soluble hydrogen carbonate. On boiling precipitate reappears again, as CO
2
is removed.
The precipitate is also soluble in acetic acid.
CaCl
2
+ (NH
4
)
2
CO
3
CaCO
3
+ + 2NH
4
Cl
CaCO
3
+ 2CH
3
COOH Ca(CH
3
COO)
2
+ H
2
O+ CO
2
Ammoniumoxalate solution (concentrated) : Awhite precipitate is formed. The precipitation is facilitated
by making the solution alkaline. The precipitate is practically insoluble in water (K
sp
= 2.6 10
9
), insoluble
in acetic acid but readily soluble in mineral acids.
Ca(CH
3
COO)
2
+ (NH
4
)
2
C
2
O
4
CaC
2
O
4
+ +2CH
3
COONH
4
Potassium hexacyanidoferrate (II) solution : White precipitate of a mixed salt is produced.
Ca
2+
+ 2 K
+
+ [Fe(CN)
6
]
4
K
2
Ca[Fe(CN)
6
] +
In presence of ammonium chloride the test is more sensitive and in this case K
+
is replaced by NH
4
+
ions in
the precipitate.
This test can be used to distinguish , calcium from strontium, barium and magnesium ions.
The confirmatory test for the basic radicals of (V) group have to be done in the order of Ba
2+
, Sr
2+
then Ca
2+
(i.e BSC) because Ba
2+
give positive test with all the reagents used in the confirmatory
test of these group radicals, K
2
CrO
4
, (NH
4
)
2
SO
4
& (NH
4
)
2
C
2
O
4
. So performs the test for Sr
2+
with
(NH
4
)
2
SO
4
only whenBa
2+
is absent. SimilarlySr
2+
gives thetest withboth(NH
4
)
2
SO
4
and(NH
4
)
2
C
2
O
4
.
So proceeds with Ca
2+
only when Sr
2+
is absent otherwise it will respond to ammonium oxalate test.
VI
th
GROUP :
1. MAGNESIUM ION(Mg
2+
) :
Disodium hydrogen phosphate solution : To the filtrate of V group or Mg
2+
ions solution add 1 ml
(NH
4
)
2
C
2
O
4
solution and heat if white precipitate is formed then filter it. Now to filtrate add a solution of
disodium hydrogen phosphate. Awhite crystalline precipitate is formed in the presence of NH
4
Cl (prevent
precipitation of Mg(OH)
2
) and ammonia solution.
Mg
2+
+ NH
3
+ HPO
4
2
Mg(NH
4
)PO
4
+
Precipitate is sparingly soluble in water, soluble in acetic acid and in mineral acids.
The precipitate separates slowly fromdilute solutions because of its tendency to formsupersaturated
solution. This may be overcome by cooling and by rubbing the test tube beneath the surface of the
liquid with a glass rod.
A white flocculent precipitate of magnesium hydrogen phosphate is obtained in neutral solutions.
Mg
2+
+ HPO
4
2
MgHPO
4
+
Ammonium phosphate can also be used.

Ammonia solution : Awhite gelatinous precipitate is formed.
Mg
2+
+ 2 NH
4
OH Mg(OH)
2
+ + 2 NH
4
+
The precipitate obtained is sparingly soluble in water but readily soluble in ammonium salts.
Mg(OH)
2
Mg
+2
+ 2 OH
NH
4
Cl NH
4
+
+ Cl
; NH
4
+
+ OH
NH
4
OH (weak base)
NH
4
+
ions 'remove' OH
causing the hydroxide to dissolve more. Not possible with NaCl.

Ammonium carbonate solution : A white precipitate of basic magnesium carbonate is obtained in the
absence of NH
4
+
salts.
5 Mg
2+
+ 6 CO
3
2
+ 7 H
2
O 2 MgCO
3
. Mg(OH)
2
. 5 H
2
O + + 2HCO
3
38
CHEMISTRY
In the presence of NH
4
+
salts no precipitation occurs, because the equilibrium
NH
4
+
+ CO
3
2
NH
3
+ HCO
3
is shifted towards the formation of HCO

3
ions. K
sp
of the precipitate being high (K
sp
of pure MgCO
3
is
1 10
5
), the concentration of carbonate ions necessary to produce a precipitate is not attained.
4(4Nitrophenyl azo resorcinol) or Magneson I : Precipitate is dissolved in dilute HCl (minimum
quantity) and to this sodium hydroxide solution is added followed by addition of 0.5 mL of magnesonI
reagent. Ablue lake is formed.
MgCl
2
+ 2NaOH Mg(OH)
2
+ 2NaCl
Magneson reagent is p-nitrobenzene-azo resorcinol a dye stuff which is adsorbed over Mg(OH)
2
to produce
a blue coloured lake.
Titan yellow(a water soluble yellowdyestuff) : It is adsorbed by Mg(OH)
2
producing a deep red colour or
precipitate.
Dissolved the precipitate in dilute HCl (minimum quantity) and to 1 drop of this add 1 drop of NaOH solution
(2 M) followed by 1 drop of titan yellow solution a deep red colour solution or precipitate is obtained.
Ba
2+
and Ca
2+
do not react but intensify the colour.
Example-16 Explain the following.
(a) Reaction between NiCl
2
and excess KCN solution.
(b) Reaction between cobalt chloride and sodiumbicarbonate and bromine water.
(c) When manganese nitrate, sodium bismuthate (NaBiO
3
) solution and concentrated HNO
3
is boiled.
(d) When precipitate of Zn(NH
4
)PO
4
reacts with ammonia.
Solution (a) A green precipitate is formed which dissolves in excess of reagent forming a yellow coloured
solution.
NiCl
2
+ 2KCN Ni(CN)
2
+
+ 2KCl ;
Ni(CN)
2
+ 2KCN K
2
[Ni(CN)
4
]
(b) When sodiumbicarbonate is added in excess to cobalt chloride solution followed by the bromine
water and then mixture is slightly heated, the solution turns apple green.
CoCl
2
+ 2NaHCO
3
Co(HCO
3
)
2
+2NaCl
Co(HCO
3
)
2
+ 4 NaHCO
3
Na
4
[Co(CO
3
)
3
] + 3H
2
O+ 3CO
2
Br
2
+ H
2
O 2HBr + [O]
2Na
4
[Co(CO
3
)
3
] + H
2
O+ [O] 2Na
3
[Co(CO
3
)
3
] (green) + 2NaOH
(c) 2 Mn
2+
+ 5 NaBiO
3
+ 14 H
+
2MnO
4
(violetred/purple) + 5 Bi
3+
+ 5 Na
+
+ 7 H
2
O
(d) Zn(NH
4
)PO
4
+ + 3NH
3
[Zn(NH
3
)
4
]
2+
+ HPO
4
2
.
Example-17 Column I and column II contains four entries each. Entries of column I are to be matched with some
entries of column II. Each entry of column I may have the matching with one or more than one entries
of column II.
Column I Column II
(A) Forms coloured precipitate on addition of CrO
4
2
ions but precipitate (p) Ag
+
dissolves in ammonia solution.
(B) Forms coloured precipitate with ammonia solution but dissolves forming (q) Cu
2+
coloured solution in excess of precipitant.
(C) Forms coloured precipitate on addition of I
ions but in excess of (r) Ni

2+
precipitant precipitate dissolves forming coloured solution.
(D) Forms white precipitate, when salt (chloride or nitrate) is poured into a (s) Bi
3+
large volume of water.
39
CHEMISTRY
Solution (A - p) ; (B - q, r) ; (C - s) ; (D - s)
(A) 2Ag
+
+ CrO
4
2
Ag
2
CrO
4
+ (red)
Ag
2
CrO
4
+ 4NH
3
2[Ag(NH
3
)
2
]
+
+ CrO
4
2
(B) 2Cu
2+
+ SO
4
2
+ 2NH
3
+ H
2
O Cu(OH
2
)
2
. CuSO
4
+ (blue) + 2NH
4
+
Cu(OH)
2
. CuSO
4
+ + 8NH
3
2 [Cu(NH
3
)
4
]
2+
]SO
4
2
(intense blue) + 2OH
Ni
2+
+ 2NH
3
+ 2H
2
O Ni(OH)
2
+ (green) + 2NH
4
+
Ni(OH)
2
+ + 6NH
3
[Ni(NH
3
)
6
]
2+
(deep blue) + 2OH
(C) Bi
3+
+ 3I
BiI
3
+ (black)
BiI
3
+ I
[BiI
4
]
(orange colouration)
(D) Bi
3+
+ NO
3
+ H
2
O BiO(NO
3
) + (white) + 2H
+
basic salt
MISCELLANEOUSSOLVEDPROBLEMS(MSPs)
1. BaCl
2
solution gives a white precipitate with a solution of a salt, which dissolves in dilute hydrochloric acid
with the evolution of colourless, pungent smelling gas. The gas as well as the salt both are used as bleaching
agent in the textile industries. The salt contains:
(A) sulphite (B) sulphide (C) acetate (D) carbonate
Ans. (A)
Sol. Ba
2+
+ SO
3
2
BaSO
3
+
(white)
BaSO
3
+ 2HCl BaCl
2
+ SO
2
(colourless pungent smelling gas) + H
2
O
SO
3
2
and SO
2
both act as bleaching agent.
2. Which of the following precipitate(s) does / do not dissolve in excess of ammonia solution ?
(A) Zn(OH)
2
(B) Ni(OH)
2
(C) Al(OH)
3
(D) (B) and (C) both
Ans. (C)
Sol. (A) Zn(OH)
2
+ 4 NH
3
[Zn(NH
3
)
4
]
2+
(colourless solution) + 2OH
(B) Ni(OH)
2
+
+ 6NH
3
[Ni(NH
3
)
6
]
2+
(deep blue solution) + 2OH
(C) Al(OH)
3
+ NH
3
No reaction.
3. Chocolate brown precipitate is formed with :
(A) Cu
2+
ions and [Fe (CN)
6
]
3
(B) Cu
2+
ions and [Fe(CN)
6
]
4
(C) Fe
2+
ions and [Fe (CN)
6
]
4
(D) Fe
2+
ions and dimethylglyoxime
Ans. (B)
Sol (A) Cu
3
[Fe(CN)
6
]
2
+ (green) ; (B) Cu
2
[Fe(CN)
6
] + ( chocolate brown)
(C) Fe
4
[Fe(CN)
6
]
3
+(Prussian blue) ; (D) red solution of iron(II) dimethylglyoxime.
4. Pink colour of acidified KMnO
4
is decolourised but there is no evolution of any gas. This may happen with the
compound containing the following acid radical.
(A)
2
3
SO (B)

2
NO (C) S
2
(D) All of these
Ans. (D)
Sol. (A) 5SO
3
2
+ 2MnO
4
+ 6H
+
2Mn
2+
+ 5SO
4
2
+ 3H
2
O
(B) 2MnO
4
+ 5NO
2
+ 6H
+
2Mn
2+
+ 5NO
3
+ 3H
2
O
(C) 2MnO
4
+ H
2
S + 6H
+
2Mn
2+
+ 5S + + 8H
2
O
5. Which of the following gives a precipitate with Pb(NO
3
)
2
but not with Ba(NO
3
)
2
?
(A) Sodium chloride (B) Sodium acetate
(C) Sodium nitrate (D) Disodiumhydrogen phosphate
Ans. (A)
Ans. (A) Pb
2+
+ 2Cl

PbCl
2
+ (white) ; Ba
2+
+ 2Cl

BaCl
2
(water soluble)
(B) (CH
3
COO)
2
Pb and (CH
3
COO)
2
Ba both are water soluble salts.
(C) Nitrates are mostly soluble in water
(D) 3Pb
2+
+ 2HPO
4
2

Pb
3
(PO
4
)
2
+ (white) + 2H
+
; Ba
2+
+ HPO
4
2

BaHPO
4
+ (white)
40
CHEMISTRY
6. Colour of cobalt chloride solution is :
(A) pink (B) black (C) colourless (D) green
Ans. (A)
Sol. Anhydrous Co(II) salts are blue in colour while hydrated Co(II) salts are pink/red.
7. A red colouration or precipitate is not obtained when :
(A) Fe
3+
reacts with potassium thiocyanate (B) Fe
2+
reacts with dimethylglyoxime.
(C) Hg
2+
reacts with potassium iodide. (D) None
Ans. (D)
Sol. (A) Fe
3+
+ 3SCN
Fe(SCN)
3
(red solution)
(B) Red solution of iron(II) dimethylglyoxime.
(C) Hg
2
+ 2I
HgI
2
+
(red).
8. When H
2
S gas is passed through an ammonical salt solution X, a slightly white precipitate is formed. The X
can be :
(A) a cobalt salt (B) a lead salt (C) a zinc salt (D) a silver salt
Ans. (C)
Sol. Zn
2+
+ H
2
S ZnS + (white) + 2H
+
9. Consider the following statement :
S
1
: Cu
2+
ions are reduced to Cu
+
by potassium iodide and potassium cyanide both, when taken in excess
S
2
: H
2
S will precipitate the sulphide of all the metals from the solutions of chlorides of Cu, Zn and Cd if the
solution is aqueous.
S
3
: The presence of magnesium is confirmed in qualitative analysis by the formation of a white crystal
line precipitate of MgNH
4
PO
4
.
S
4
: Calomel on reaction with potassium iodide gives red precipitate.
and arrange in the order of true /false.
(A) TTFF (B) TFTF (C) TTTT (D) TTTF
Ans. (D)
Sol. S
1
, S
2
and S
3
are correct statements.
S
4
: Hg
2
2+
+ 2I

2 2
I Hg
+
(green)
10. Statement - 1 : Addition of NH
4
OH to an aqueous solution of BaCl
2
in presence of NH
4
Cl (excess) precipi-
tates Ba(OH)
2
.
Statement - 2 : Ba(OH)
2
is water soluble.
(A) Both Statement-1 and Statement-2 are true and Statement-2 is the correct explanation of Statement-1.
(B) Both Statement-1 and Statement-2 are true but Statement-2 is not correct explanation of Statement-1.
(C) Statement-1 is true but Statement-2 is false.
(D) Statement-1 is false but Statement-2 is true
Ans. (D)
Sol. Ba
2+
ions does not give any precipitate with NH
4
OH solution in excess of NH
4
Cl because product formed,
Ba(OH)
2
is soluble in water
11. Statement - 1 : Sodiummeta aluminate on boiling with ammonium chloride produces white gelatinous pre-
cipitate.
Statement - 2 : Aluminium hydroxide is formed which is not soluble in water
(A) Both Statement-1 and Statement-2 are true and Statement-2 is the correct explanation of Statement-1.
(B) Both Statement-1 and Statement-2 are true but Statement-2 is not correct explanation of Statement-1.
(C) Statement-1 is true but Statement-2 is false.
(D) Statement-1 is false but Statement-2 is true
Ans. (A)
Sol. [Al(OH)
4
]
boil
Cl NH
4
Al(OH)
3
+ + OH
41
CHEMISTRY
12. Which of the following statement(s) is (are) incorrect?
(A) Fe
2+
ions give a dark blue precipitate with potassium hexacyanidoferrate (III) solution.
(B) Fe
3+
ions give intense blue precipitate with potassium hexacyanidoferrate (II) solution.
(C) Fe
3+
ions give a brown colouration with potassium hexacyanidoferrate (III) solution.
(D) Fe
2+
ions give a deep red colouration with ammonium thiocyanate.
Ans. (D)
Sol. (A) Fe
2+
+ [Fe(CN)
6
]
3
Fe
3+
+ [Fe(CN)
6
]
4
4Fe
3+
+ 3 [Fe(CN)
6
]
4
Fe
4
[Fe(CN)
6
]
3
(turnbull's blue)
(B) 4Fe
3+
+ 3[Fe(CN)
6
]
4
Fe
4
[Fe(CN)
6
]
3
+ (intense blue)
(C) Fe
3+
+ [Fe(CN)
6
]
3
Fe[Fe(CN)
6
] (brown colouration)
(D) Fe
3+
+ 4SCN
Fe (SCN)
3
(deep red colouration)
Fe
2+
+ 4 SCN
No reaction
13. Which of the following pair (s) of ions would be expected to form precipitate when dilute solutions are mixed?
(A) NH
4
+
, [Co(NO
2
)
6
]
3
(B) NH
4
+
, CO
3
2
(C) Fe
3+
, OH
(D) Ba
2+
, SO
4
2
Ans. (A,C,D)
Sol. (A) NH
4
+
+ [Co(NO
2
)
6
]
3
(NH
4
)
3
[Co(NO
2
)
6
]
+
(yellow)
(B) Ammonium and alkali metal carbonates are water soluble.
(C) Fe
3+
+ OH

Fe(OH)
3
+
(reddish - brown)
(D) Ba
2+
+ SO
4
2

BaSO
4
+
(white)
Comprehension (Q.14 to Q.16)
Aqueous solution of salt (A)
NaOH(aq)/warm
Gas(B)
Solution of salt (C)
FeSO
4
conc. H SO
2 4
Gas(B)
Zn/NaOH /heat
Brown ring (D)
at the junction
of the two layers
Colourless gas which is
alkaline in nature
White fumes
dil.HCI
Salt (A) on heating gives a colourless neutral gas which supports combustion.
From the aforesaid, flowdiagram, answer the following questions.
14. The compound (A) contains the following acid radical.
(A) NO
2
(B) NO
3
(C) Br
(D) SO
3
2
Ans. (B)
Sol. NO
3
and NO
2
both give brown ring test and reduction of NO

3
and NO
2
both give ammonia which with dilute

HCl gives dense white fumes.
if NH
4
NO
3

A
N
2
O+ 2H
2
O; N
2
O supports the combustion
but NH
4
NO
2

A
N
2
+ 2H
2
O ; Nitrogen does not supports combustion.
Hence, the anion is NO
3
.
15. The basic radical of salt (A) and gas Bboth gives brown precipitate with Nesslers reagent. The composition
of the brown precipitate is :
(A) (NH
4
)
2
[HgI
4
] (B) Hg(NH
2
) NO
3
(C) HgO. Hg (NH
2
)I (D) (NH
4
)
3
[Co(NO
2
)
6
]
Ans. (C)
Sol. NH
4
+
+ 2[HgI
4
]
2
+ 4OH
HgO. Hg (NH
2
)I + + 7I
+ 3H
2
O
Hence the cation is NH
4
+
.
42
CHEMISTRY
16. Which of the following statement is correct ?
(A) Salt (A) gives yellow precipitate with chloroplatinic acid as well as with sodium cobaltinitrite.
(B) The brown ring is formed due to the formation of nitroso ferrous sulphate [Fe(NO)]
2+
SO
4
.
(C) Salt C reacts with silver nitrate solution to form white precipitate.
(D) (A) and (B) both.
Ans. (D)
Sol. (A) 2NH
4
+
+ [PtCI
6
]
4
(NH
4
)
2
[PtCl
6
] + (yellow)
3NH
4
+
+ [Co(NO
2
)]
3

(NH
4
)
3
[Co(NO
2
)
6
] + (yellow)
(B) 2NO
3
+ 4H
2
SO
4
+ 6Fe
2+
6Fe
3+
+ 2NO | + 4SO
4
2
+ 4H
2
O
SO
4
2
+ Fe
2+
+ NO [Fe(NO)]
2+
SO
4
2
(C) Ag NO
3
+ NaNO
3
No reaction.
If the anion is NO
2
then Ag
+
+ NO
2
Ag NO
2
+ (white)
Reactions :
NH
4
NO
3
+ NaOH NH
3
| + NaNO
3
(A) (B) (C)
NH
3
+HCI NH
4
CI|(White)
NO
3
+ 4Zn + 7OH
+ 6H
2
O NH
3
+ 4[Zn(OH)
4
]
2
True/False :
17. Magnesium is precipitated from its salt solution as only magnesium ammonium phosphate by adding diso-
dium hydrogen phosphate solution in absence of ammonium chloride and aqueous ammonia.
Sol. (False) Precipitation is carried out in presence of ammoniumchloride and aqueous ammonia as they prevent
precipitation of magnesium hydroxide.
Mg
2+
+ NH
3
+ HPO
4
2
Mg (NH
4
) PO
4
+ (white)
18. When a solution of nitrite acidified with dilute hydrochloric acid is treated with solid urea, the nitrite is
decomposed, and nitrogen and carbon dioxide are evolved.
Sol. (True) CO(NH
2
)
2
+ HNO
2

2N
2
| + CO
2
| + 3H
2
O.
19. Solution of alkali metal cyanide containing freshly prepared iron (II) sulphate solution and dilute H
2
SO
4
on
exposure to air produces prussian blue precipitate
Sol. (True) Fe
2+
+ 2 CN
Fe(CN)
2
+ ; Fe(CN)
2
+ + 4CN

[Fe(CN)
6
]
4
4Fe
2+
+ O
2
+ 4H
+
4Fe
3+
+ 2H
2
O; Fe
3
+ [Fe(CN)
6
]
4
Fe
4
[Fe(CN)
6
]
3
+
Subjective :
20. What happens when ?
(A) Aqueous solution of CrCl
3
is added to ammonia solution.
(B) Ammonium carbonates reacts with MgCl
2
(i) in absence of ammonium salts and (ii) in presence of
ammonium salts :
Sol. (A) Cr
3+
+ 3NH
3
+ 3H
2
O Cr(OH)
3
+ (green) + 3NH
4
+
Cr(OH)
3
precipitate formed becomes slightly soluble in excess of precipitant in cold forming a violet
or pink solution containing [Cr(NH
3
)
6
]
3+
complex ions.
Cr(OH)
3
+ + 6 NH
3
[Cr(NH
3
)
6
]
3+
+ 3OH
(B) (i) 5Mg

2+
+ 6
2
3
CO + 7H
2
O 4MgCO
3
. Mg(OH)
2
. 5 H
2
O + + 2HCO
3
White precipitate of basic magnesium carbonate is formed.

(ii) In presence of ammonium salts no precipitation occurs, because the equilibrium
NH
4
+
+ CO
3
2
NH
3
+ HCO
3
is shifted towards the formation of HCO

3
ions.
43
CHEMISTRY
21. Salts given in column (I) reacts with the excess of reagents given in column (II) and form white /coloured
precipitates. Select the correct options for the salts given in column (I) with the reagent(s) given in the
column (II)
Column - I Column - II
(A) Zn(NO
3
)
2
(p) Sodiumhydroxide
(B) Cu(NO
3
)
2
(q) Ammonia solution
(C) Fe(NO
3
)
3
(r) Disodiumhydrogen phosphate
(D) Ag(NO
3
)
2
(s) Potassiumferrocyanide
Ans. (A - r, s) ; (B - p, r, s) ; (C - p, q, r, s) ; (D - p, q, r, s)
Sol. (A) Zn
2+
+ 2OH
Zn(OH)
2
+ (white) ;
Zn (OH)
2
+ 2OH
[Zn(OH)
4
]
2
(colourless soluble complex)
Zn
2+
+ 2NH
3
+ 2H
2
O Zn (OH)
2
+ (white) + 2NH
4
+
Zn(OH)
2
+ + 4NH
3
[Zn(NH
3
)
4
]
2+
(colour less soluble complex) + 2OH
3Zn
2+
+ 2HPO
4
2
Zn
3
(PO
4
)
2
+ (white) + 2H
+
3 Zn
2+
+ 2K
+
+ 2[Fe(CN)
6
]
4
K
2
Zn
3
[Fe(CN)
6
]
2
+ (bluish white)
(B) Cu
2+
+ 2OH
Cu(OH)
2
+ (blue)
Cu
2+
+ 4NH
3
[Cu(NH
3
)
4
]
2+
(deep blue soluble complex)
Cu
2+
+ 2HPO
4
2
Cu
3
(PO
4
)
2
+ (blue) + 2H
+
Cu
2
+[Fe(CN)
6
]
4
Cu
2
[Fe(CN)
6
] + (chocolate brown)
(C) Fe
3+
+ 3OH
Fe (OH)
3
+ (reddish brown)
Fe
3+
+ 3NH
3
+ 3H
2
O Fe(OH)
3
+ (reddish brown) + 3NH
4
+
Fe
3+
+ HPO
4
2
FePO
4
+ (yellowish-white) + H
+
4Fe
3+
+ 3 [Fe(CN)
6
]
4
Fe
4
[Fe(CN)
6
]
3
+ (intense blue)
(D) 2Ag
+
+ 2OH
Ag
2
O + (brown) + H
2
O
2Ag
+
+ 2NH
3
+ H
2
O Ag
2
O + (brown) + 2NH
4
+
4Ag
+
+ HPO
4
2
Ag
3
PO
4
+ (yellow) + H
+
4Ag
+
+ 3 [Fe(CN)
6
]
4
Ag
4
[Fe(CN)
6
] + (white)

Qualitative Analysis Theory - E

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Droits d'auteur :

Qualitative Analysis Theory - E

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Droits d'auteur :

"manishkumarphysics.

Smell like that of rotten eggs S

ammonia, white precipitate with silver nitrate solution.

sulphate solution black.

iodide paper blue.

paper orange red.

Do not heat the tube strongly at one point as it may break.

Non luminous flame is called oxidising flame.

Almost all nitrites and nitrates are solublein water. AgNO

Most chlorides are soluble in water. PbCl

Silver, mercury(I) andcopper(I), bromidesareinsoluble. Leadbromideissparinglysoluble

(ii) wet starch iodide paper blue.

No peculiar gas is evolved. All above are absent

white fumes with a glass rod dipped in NH

reddish brown fumes increases on addition of a pinch

Evolution of reddish brown fumes which intensifies on NO

addition of copper turnings or bits of filter paper.

W.E. = Water extract. (Salt is dissolved in distilled water)

S.E. = Sodium carbonate extract

Blue (starch iodine adsorption complex)

(B) White precipitate on addition of AgNO

(D) Its acidified salt solution decolourises pink KMnO

KCNdoes not have any effect.

Inplace of Cobalt (II) thiocyanate, Co(CH

KCN dissolves the precipitate forming a clear solution.

Sodium hydroxide in cold solution : Ablue precipitate is formed.

On dilution the reaction is reversed and black BiI

On heating with water black precipitate of BiI

4. CADMIUM ION (Cd

Precipitate does not dissolve in KCN.

KI forms no precipitate (distinction from Copper)

is soluble in tartaric acid but BiO

is insoluble in tartaric acid.

Sodium hydroxide solution : Agreen precipitate is formed.

, a yellow solution is obtained.

Ammonia solution : Partial precipitation of white manganese(II) hydroxide takes place.

Green solution of sodium cobalticarbonate is obtained.

Potassium cyanide solution :

If brown solution is boiled for a longer time in air or some H

Solution on evaporation to dryness gives yellowresidue (NiCl

Ammonium phosphate can also be used.

causing the hydroxide to dissolve more. Not possible with NaCl.

is shifted towards the formation of HCO

ions but in excess of (r) Ni

both give brown ring test and reduction of NO

both give ammonia which with dilute

(B) (i) 5Mg

White precipitate of basic magnesium carbonate is formed.

is shifted towards the formation of HCO

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