Detection of cation and anion in inorganic sample.

Writeup for
one unknown sample is provided here.

This file also contains a general instruction for all cations and anions.

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EXPERIMENT NO.

DETECTION OF CATION AND ANION IN GIVEN UNKNOWN INORGANIC

Sample No - 1

Colour - White Crystalli

Solubility - Water soluble

Sl No. Experiment Observation Inference

1. Heated 0.5 g of the salt in a dry (i)No gas was - -
i) NO3 , NO2 , Br
-
test tube and noted the colour of evolved. (ii) No maybe absent.
the gas evolved and change in the particular ii) Zn2+ maybe absent.
colour of the residue on heating and change in colour of
cooling. the residue
is observed
when heated and
when
cooled.
2. Prepared a paste of the salt with conc. No distinct colour of Ca2+, Sr2+, Ba2+, Cu2+
HCl and performed the flame test. the flame seen. may be absent.
3. Borax bead test was not performed as - Cu2+, Ni2+, Mn2+,
the salt was white in colour. Fe3+ may be absent.
4. Treated 0.1 g of salt with 1 mL No effervescence CO32–, SO32–, S2–,
dil.H2SO4. and evolution of –
NO2–, CH3COO
vapours. absent.
5. Heated 0.1 g of salt with 1 mL No gas evolved. Cl–, Br–, I–, NO3–, C2O42–
conc. H2SO4. are absent.
6. Acidified 1mL of aqueous salt No yellow precipitate. PO43– absent.
solution with conc. HNO3. Warmed
the
contents and then added 4 - 5 drops of
ammonium molybdate solution.
7. Aqueous solution of the salt A white ppt. SO42– present and
acidified with dil. HCl and then is obtained which is confirmed.
added 2mL of BaCl2 solution. insoluble in conc.
HNO3 and conc. HCl.
8. Heated 0.1 g of salt with 2 mL Ammonia gas is not NH4+ absent.
NaOH solution. evolved.
9. Prepared original solution of the salt Clear solution formed Water soluble salt
by dissolving approximately 1g of it in is present.
20 mL water.
10. To a small part of the above salt No white precipitate Group– I absent.
solution added 2 mL of dil. HCl. formed.
11. Passed H2S gas through one No precipitate Group– II absent.
portion of the solution of step 10. formed.

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 12. Added about 0.2 g of solid ammonium No precipitate Group– III absent.
chloride and then added excess formed.
of ammonium hydroxide to the
solution of step 10.
13. Passed H2S gas through the above No precipitate Group– IV absent.
solution. formed.
14. Added excess of ammonium hydroxide No precipitate Group–V absent.
solution to the original solution and formed.
then added 0 .5 g of ammonium
carbonate.
15. To the original solution of salt added White precipitate. Mg2+ present and
ammonium hydroxide solution, confirmed
followed by disodium hydrogen
phosphate solution. Heated and
scratched the sides of the test tube.

Conclusion: The given unknown sample contains Mg2+ as cation and SO42- as anion.

e. g. for the sample identified above, you should write the following equations:

The following pages (Page No.4 to 12) contains the general instructions for writing unknown
inorganic sample, not to be copied to the lab notebook.

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Preliminary tests for Anions:

Experiment observation Inference

1. Sample + dilute H2SO4 i) Colourless, Odourless gas i) CO32- present.

evolved with brisk
effervescence which turned lime
water milky.
ii) S2- maybe present.
ii) Colourless gas with smell
of rotten egg which turned
lead acetate paper black.

iii) Colourless gas evolved which iii) SO32- maybe present.

turned acidified dichromate
paper green.
iv) CH3COO- maybe present.
iv) Colourless gas evolved
with smell of vinegar

v) Brown fumes evolved which v) NO2- maybe present.

turned acidified dichromate
paper green.
2. Sample + i) Colourless gas evolved, a i) Maybe Cl-.
concentrated H2SO4 → glass rod dipped in ammonium
heat hydroxide when held near
the issuing gas, dense fume is
observed.

3. Sample + Cu-turnings i) Reddish Brown fumes evolved. i) Maybe NO3-

+ conc. H2SO4 →heat

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Confirmatory tests for anions:
extract of the salt:
Experiment
1. 1 mL aqueous solution
+ drops of NaOH + sodium
nitroprusside solution.
2. 1 mL aqueous solution
+ dilute HCl + BaCl2
solution.
3. 1 mL aqueous solution
+ dilute HNO3 + AgNO3
solution.
4. 1 mL aqueous solution
+ freshly prepared FeSO4
solution + conc. H2SO4
added along the side
of the test tube
without shaking.
5. 1 mL aqueous solution +
few drops of acetic acid
(to acidify) + calcium
chloride solution.
6. 1 mL aqueous solution +
concentrated HNO3+
Ammonium molybdate
solution → heated to
boiling.
7. Aq. Soln. of sample +
neutral FeCl3 solution,
filtered and add dilute HCl
Wettestsfor anions are performed by using the
observation Inference
i) purple or violet i) S2- present and confirmed.
colouration observed.
i) White precipitate insoluble i) SO42- present and confirmed.
in concentrated HCl.
i) Curdy white ppt dissolves i) Cl-present and confirmed.
in excess NH4OH.
i) Brown ring formed at the i) NO3- present and confirmed.
junction of two liquid
layers.
i) white precipitate observed i) C2O42- (oxalate) present
which is insoluble in and confirmed.
ammonium oxalate and oxalic
acid but
soluble in dil HCl and dil HNO3.
i) Canary yellow precipitate is i) PO43-(phosphate) present
observed. and confirmed.
Reddish colour formed Acetate present and
which disappears confirmed.
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Preliminary (Dry) tests for cations (Dry heating test and Flame test).
Experiment
Dry heating test: 0.1g of
the dry salt was taken in
a dry test tube and
strongly heated.
Flame test: Small
amount of sample taken
at the tip of the platinum
wire with conc. HCl and
introduced into the flame.
observation Inference
i) Blue when cold and white i) Cu2+ maybe present.
when hot.
ii) White when cold and
ii) Zn2+ maybe present.
yellow when hot.
iii) Yellow when cold and
brown when hot. iii) Pb2+ maybe present.
iv) Coloured salt turned iv) Co2+, Cu2+, Mn2+
brown/blue on maybe present.
heating.
v) NH4+ maybe present.
v) White sublimate formed.
vi) Pb(NO3)2 maybe present.
vi) Decripitation with
brown fume.
vii) Yellow when hot. vii) Ni2+ maybe present.
viii) Fe3+ maybe present.
viii) Dirty white or yellow
i) Transient brick red flame. i) Maybe Ca2+.
ii) Persistent crimson red flame ii) Maybe Sr2+ .
iii) Apple green flame. iii) Maybe Ba2+.
iv) Bluish green flame. iv) Maybe Cu2+ .
v) Lambent blue flame. v) Maybe Pb2+.
vi) Green flashes. vi) Maybe Mn2+ .
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Borax bead/Charcoal Cavity/Cobalt nitrate, Preliminary (Dry) test for cations.

Experiment Observation Inference

Borax bead test: i) Blue in cold and Green in i) Maybe Cu2+ .

(only for coloured salt, no hot oxidising flame, Red
need to perform this test if opaque in cold and colourless
the salt is white) Borax was in hot in reducing flame.
heated in the loop of
ii) Yellow in cold and ii) Maybe Fe3+ .
platinum wire, it swelled
yellowish brown in hot in
and formed transparent
oxidising flame. Green in cold
colourless glassy bead,
and hot in reducing flame.
touched with small
amount of coloured salt iii) Light violet in cold and hot
and heated again, colour of iii) Maybe Mn2+ .
in oxidising flame. Colourless
the bead was observed. in cold and hot in reducing
flame.
iv) Maybe Co2+ .
iv) Deep blue in both
reducing and oxidising flame.

v) Brown bead in oxidising v) Maybe Ni2+ .

flame and grey bead in reducing
flame.
Charcoal cavity test: Pinch i) Yellow residue when hot i) Maybe Pb2+ .
of salt was mixed with and grey metal when cold.
sodium carbonate and
heated on a charcoal ii) White residue with the ii) Maybe As3+ .
cavity in the reducing odour of garlic.
flame.
iii) Yellow residue when hot
and white when cold. iii) Maybe Zn2+ .

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 Cobalt nitrate test: (only i) Green residue. i) Maybe Zn2+ .
if the sample leaves
ii) Pink residue. ii) Maybe Mg2+ .
white residue in a charcoal
block). White residue is iii) Blue residue. iii) Maybe Al3+ .
treated with 2 to 3 drops of
cobalt nitrate solution and
heated in an oxidising
flame.

Confirmatory test for cations (Group analysis by H2S).

Experiment Observation Inference

i) A small amount of salt i) Gas with smell of ammonia i) Group 0 may be present.
was taken in test tube and evolved, a glass rod dipped in
added HCl brought near the mouth of
1 to 2 ml of NaOH the
and heated. test tube, white fumes observed.
ii) NH4+ present and confirmed.
ii) The gas evolved on ii) Brown precipitate observed.
heating with NaOH was
passed through Nessler’s
reagent.
Preparation of original solution (O.S.): A small amount of salt was dissolved in distilled water; the
following tests were performed with this solution. [The salt may dissolve on heating and if it does
not dissolve on heating,a few ml of dil. HCl would be added to fresh salt taken in a test tube, if
the salt dissolves this will be treated as original solution (O.S.)]

1. To a small part of 1. White precipitate (ppt). 1. Group I (Pb2+) present.

the above salt solution,
added 2ml of dil. HCl.

2. If no ppt. for group 2. Black/yellow ppt. 2. Group II (Pb2+/Cu2+) if

I, Passed H2S gas through black ppt, (As3+) if yellow ppt.
one portion of above present.
solution.

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 3. If no ppt. for group II, 3. Brown or green/white 3. Group III (Fe3+) if brown
to another portion of gelatinous ppt. or green ppt. and (AI3+) if
salt solution, added 2 to 3 white gelatinous ppt.
drops of conc. HNO3 (if present.
sample is coloured) and
boiled, cooled and then
added NH4CI solid and
NH4OH solution.
4. If no ppt. for group 4. White/flesh coloured/black 4. Group IV (Zn2+) if
III, passed H 2S through ppt. white, (Mn2+) if flesh
the solution. coloured,
(Ni2+/Co2+) if black ppt.
present.
5. If no ppt. for group IV, 5. White ppt. 5. Group V
To the O.S. added NH4CI (Ba2+/Sr2+/Ca2+) present.
solid and NH4OH
solution, followed by
(NH4)2CO3 solution.

6. If no ppt. for group 6. White ppt. 6. Group VI (Mg2+) present.

V, added Na2 HPO4 solution.

Confirmatory test (Wettest) / Treatment of precipitate (ppt.).

GR. I(Pb2+)

White precipitate was dissolved in

hot water.

i) To one part, Added KI solution.

i) Yellow ppt. Pb2+ present and confirmed.
ii) To other part, Added K2Cr2O4.
ii) Yellow ppt.

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Group
Experiment observation Inference

Black precipitate boiled

with dil. HNO3.

1. i) To one part, Added

1. i) Deep blue colouration.
excess of NH4OH soln.
1. Cu2+ present and
confirmed.
ii) To other part, Added ii) Chocolate brown ppt.
K4 [Fe(CN)6] soln.

Group III

Experiment Observation Inference

Brown or green/white gelatinous

ppt. dissolves in dil. HCl.
1. i) A Blood
1. i) To one part, NH4SCN was added. red colouration.
1. Fe3+ present and confirmed.
ii) To other part, K4 [Fe(CN)6] ii) A Prussian
was added. blue ppt.

2. Add dil. NaOH drop wise. 2. A white

gelatinous ppt. 2. Al3+ present and confirmed.
soluble in excess of
NaOH.

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Group IV (Zn2+/Ni2+/Co2+/Mn2+).

Experiment Observation Inference

White/flesh/black ppt.
dissolves in dilute HCl.
i) Added NaOH or NH4OH i) White ppt. soluble in i) Zn2+ present and confirmed.
soln. in excess. excess of NaOH or NH4OH.

ii) Added NH4OH soln. + ii) Bright red ppt. ii) Ni2+ present and confirmed.
Dimethyl Glyoxime solution.
iii) Added diethyl ether + iii) Ether layer turns blue. iii) Co2+ present
NH4SCN solid. and confirmed.

iv) Added NaOH soln. iv) Flesh coloured ppt. iv) Mn2+ present
and confirmed.

2+/ 2+ 2+
Group (Ba Sr /Ca )
Experiment Observation Inference

White ppt. dissolves in

dilute acetic acid and 3 parts.

i) To 1st part added K2CrO4 soln. i) Yellow ppt. i) Ba2+ present

ii) To 2nd part added and confirmed.
(NH4)2SO4 soln.
ii) White ppt. ii) Sr2+ present
and confirmed.

iii) To 3rd part added iii) White ppt. iii) Ca2+ present
(NH4)2C2O4 soln. and confirmed

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Gr VI(Mg2+)

Experiment Observation Inference

Take O.S.(original solution). White ppt. Mg2+ present and confirmed.

Added
NH4CI+NH4OH+Na2 HPO4.

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