Detection of cation and anion in inorganic sample.

Write up 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 SAMPLES

Sample No – 1

Colour – White Crystalline

Solubility – Water soluble

Sl No. Experiment Observation Inference

1. Heated 0.5 g of the salt in a dry test (i)No gas was evolved. i) NO3-, NO2-, Br- may be
tube and noted the colour of the gas (ii) No particular absent.
evolved and change in the colour of change in colour of ii) Zn2+ may be absent.
the residue on heating and 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+, Fe3+
the salt was white in colour. may be absent.
4. Treated 0.1 g of salt with 1 mL No effervescence and CO32–, SO32–, S2–, NO2–,
dil.H2SO4. evolution of vapours. CH3COO– absent.
5. Heated 0.1 g of salt with 1 mL conc. No gas evolved. Cl–, Br–, I–, NO3–, C2O42–
H2SO4. are absent.
6. Acidified 1mL of aqueous salt solution No yellow precipitate. PO43– absent.
with conc. HNO3. Warmed the
contents and then added 4-5 drops of
ammonium molybdate solution.
7. Aqueous solution of the salt acidified A white ppt. is SO42– present and
with dil. HCl and then added 2mL of obtained which is confirmed.
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 is
by dissolving approximately 1g of it in 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 of formed.
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 note book.

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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- may be present.
ii) Colourless gas with smell of
rotten egg which turned lead
acetate paper black.

iii) Colourless gas evolved which

2-
turned acidified dichromate paper iii) SO3 may be present.
green.

iv) Colourless gas evolved with

iv) CH3COO- may be present.
smell of vinegar

v) Brown fumes evolved which

turned acidified dichromate paper v) NO2- may be present.
green.

2. Sample + concentrated i) Colourless gas evolved, a glass i) May be Cl-.

H2SO4→heat rod dipped in ammonium
hydroxide when held near the
issuing gas, dense fume is
observed.

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

conc. H2SO4→heat

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Confirmatory tests for anions: Wet tests for anions are performed by using the aqueous
extract of the salt:

Experiment observation Inference

1. 1 mL aqueous solution + i) purple or violet colouration i) S2- present and confirmed.

drops of NaOH + sodium observed.
nitroprusside solution.

2. 1 mL aqueous solution + i) White precipitate insoluble in i) SO42- present and confirmed.

dilute HCl + BaCl2 solution. concentrated HCl.

3. 1 mL aqueous solution + i) Curdy white ppt dissolves in i) Cl-present and confirmed.

dilute HNO3 + AgNO3 excess NH4OH.
solution.

4. 1 mL aqueous solution + i) Brown ring formed at the i) NO3- present and confirmed.
freshly prepared FeSO4 junction of two liquid layers.
solution + conc. H2SO4
added along the side of
the test tube without
shaking.

5. 1 mL aqueous solution + i) white precipitate observed i) C2O42- (oxalate) present and

few drops of acetic acid (to which is insoluble in ammonium confirmed.
acidify) + calcium chloride oxalate and oxalic acid but
solution. soluble in dil HCl and dil HNO3.

6. 1 mL aqueous solution + i) Canary yellow precipitate is i) PO43-(phosphate) present

concentrated HNO3+ observed. and confirmed.
Ammonium molybdate
solution → heated to
boiling.

7. Aq. Soln. of sample + Reddish colour formed which Acetate present and
neutral FeCl3 solution, disappears confirmed.
filtered and add dilute HCl

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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 in to the flame.
observation
i) Blue when cold and white when
hot.
ii) White when cold and yellow
when hot.
iii) Yellow when cold and brown
when hot.
iv) Coloured salt turned
brown/blue on heating.
v) White sublimate formed.
vi) Decripitation with brown
fume.
vii) Yellow when hot.
viii) Dirty white or yellow
i) Transient brick red flame.
ii) Persistent crimson red flame
iii) Apple green flame.
iv) Bluish green flame.
v) Lambent blue flame.
vi) Green flashes.
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Inference
i) Cu2+ may be present.
ii) Zn2+ may be present.
iii) Pb2+ may be present.
iv) Co2+, Cu2+, Mn2+ may be
present.
v) NH4+ may be present.
vi) Pb(NO3)2 may be present.
vii) Ni2+ may be present.
viii) Fe3+ may be present.
i) May be Ca2+.
ii) May be Sr2+.
iii) May be Ba2+.
iv) May be Cu2+.
v) May be Pb2+.
vi) May be Mn2+.
Borax bead/Charcoal Cavity/Cobalt nitrate, Preliminary (Dry) test for cations.
Experiment
Borax bead test: (only
for coloured salt, no need to
perform this test if the salt is
white) Borax was heated in
the loop of platinum wire, it
swelled and formed
transparent colourless glassy
bead, touched with small
amount of coloured salt and
heated again, colour of the
bead was observed.
Charcoal cavity test: Pinch of
salt was mixed with sodium
carbonate and heated on a
charcoal cavity in the
reducing flame.
Observation Inference
i) Blue in cold and Green in hot i) May be Cu2+.
oxidising flame, Red opaque in
cold and colourless in hot in
reducing flame.
ii) Yellow in cold and yellowish ii) May be Fe3+.
brown in hot in oxidising flame.
Green in cold and hot in reducing
flame.
iii) Light violet in cold and hot in
iii) May be Mn2+.
oxidising flame. Colourless in
cold and hot in reducing flame.
iv) Deep blue in both reducing iv) May be Co2+.
and oxidising flame.
v) Brown bead in oxidising flame
v) May be Ni2+.
and grey bead in reducing flame.
i) Yellow residue when hot and i) May be Pb2+.
grey metal when cold.
ii) White residue with the odour
ii) May be As3+.
of garlic.
iii) Yellow residue when hot and
white when cold. iii) May be Zn2+.
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 Cobalt nitrate test: (only if i) Green residue. i) May be Zn2+.
the sample leaves white
ii) Pink residue. ii) May be Mg2+.
residue in a charcoal block).
White residue is treated with iii) Blue residue. iii) May be Al3+.
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 was i) Gas with smell of ammonia i) Group 0 may be present.
taken in test tube and added evolved, a glass rod dipped in HCl
1 to 2 ml of NaOH and brought near the mouth of the
heated. test tube, white fumes observed.

ii) The gas evolved on heating ii) Brown precipitate observed. ii) NH4+ present and confirmed.
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 the 1. White precipitate (ppt). 1. Group I (Pb2+) present.

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

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

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

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 3. If no ppt. for group II, to 3. Brown or green/white 3. Group III (Fe3+) if brown or
another portion of salt gelatinous ppt. green ppt. and (AI3+) if white
solution, added 2 to 3 drops gelatinous ppt. present.
of conc. HNO3 (if sample is
coloured) and boiled, cooled
and then added NH4CI solid
and NH4OH solution.

4. If no ppt. for group III, 4. White/flesh coloured/black 4. Group IV (Zn2+) if white,

passed H2S through the ppt. (Mn2+) if flesh coloured,
solution. (Ni2+/Co2+) if black ppt.
present.

5. If no ppt. for group IV, To 5. White ppt. 5. Group V (Ba2+/Sr2+/Ca2+)

the O.S. added NH4CI solid present.
and NH4OH solution,
followed by (NH4)2CO3
solution.

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

added Na2HPO4 solution.

Confirmatory test (Wet test) / 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 II(Cu2+)

Experiment observation Inference

Black precipitate boiled with

dil. HNO3.

1. i) To one part, Added excess

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

Group III (Fe3+/Al3+)

Experiment Observation Inference

Brown or green/white gelatinous ppt.

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

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

ppt. soluble in excess 2. Al3+ present and confirmed.
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 soln. i) White ppt. soluble in i) Zn2+ present and confirmed.
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 di ethyl ether + iii) Ether layer turns blue. iii) Co2+ present and
NH4SCN solid. confirmed.

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

Group V (Ba2+/Sr2+/Ca2+)

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

iii) To 3rd part added (NH4)2C2O4 iii) Ca2+ present and

iii) White ppt.
soln. 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+Na2HPO4.

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