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Salt Analysis-2

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49 views7 pages

Salt Analysis-2

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Salt Analysis

I. Preliminary Tests

S.No Characteristic Inference


1. Physical Appearance
a. Crystalline Maybe- SO42-, NO3-, Cl-, CH3COO-
b. Amorphous Maybe- CO32- , S2-
2. Colour
a. Blue Maybe- CuSO4.5H2O
b. Green Maybe- Cu2+,Ni2+
c. Light green Maybe-Fe2+
d. Brown Maybe-Fe3+
e. Pink Maybe-Co2+
f. Fleshy Maybe-Mn2+
g. White Absence of Cu2+,Ni2+,Fe2+,Fe3+,Co2+,Mn2+
3. Smell
a. Ammoniacal Maybe-NH4+
b. Vinegar like Maybe-CH3COO-
c. Rotten eggs like Maybe-S2-
4. Solubility
a. Soluble in cold/hot water Maybe- SO42-, NO3-, Cl-, CH3COO-
b. Soluble in dil. HCl Maybe- CO32- , S2-

II. Dry Heating Test

S. No. Exp Observation Inference

1. A Colourless and odourless gas Maybe-


sm CO2 gas turning lime water milky CO32- , C2O42-
2. all Colourless gas with odour Maybe-
am H2S gas (rotten egg smell)–turns (CH3COO)2Pb paper black S2-
oun SO2 gas(suffocating smell)-turns acid. K2Cr2O7 paper green SO32-
t of HCl gas(Pungent smell)-white fumes with ammonia Cl-
salt CH3COOH vapours(vinegar like smell)- CH3COO-
is NH3 gas(pungent smell)-white fumes with glass rod dipped in HCl NH4+
3. tak Coloured gases- Pungent smell Maybe-
en NO2 gas- reddish brown NO2-, NO3-
in a Cl2 gas- greenish yellow Cl-
dry Br2 vapours-reddish brown Br-
test I2 vapours-dark violet I-
4. tub Sublimate formed Maybe-
e White sublimate NH4+
and Black sublimate I-
5. hea Decripitation Maybe-
ted Cracklng noise for those salts that do not have water of crystalisation Pb(NO3)2
6. Swelling Maybe-
The salt swells up into voluminous mass PO43-
7. Residue Maybe-
Yellow when hot white when cold Zn2+
Brown when hot yellow when cold Pb2+
White residue glows on heating Al3+
Original blue salt becomes white on heating CuSO4.5H2O
Coloured salt becomes brown or black on heating Co2+,Cu2+,Mn2+

III. Flame test

S. No. Experiment Observation Inference

1. A paste of the salt was made with conc. Flame colour Maybe-
HCl and introduced into the flame Brick red Ca2+
Crimson Sr2+
Grassy green Ba2+
Bluish green Cu2+
IV Test for Anions
3 Groups
i) Dil. H2SO4 /Dil. HCl group
ii) Conc. H2SO4 group
iii) Independent group

S. No. Experiment Observation Inference

I. Dil. H2SO4 /Dil. HCl group


1. A small amount of salt was treated Colourless odourless gas with brisk Maybe CO32-
with dil. HCl effervescence
CaCO3 + HCl →CaCl2 + H2O + CO2↑
Conf. The colourless gas was passed through Lime water turned milky CO32-
Test lime water confirmed
CO2 + Ca(OH)2 → CaCO3↓ + H2O
2. A small amount of salt was treated Colorless gas with pungent smell Maybe SO32-
with dil. HCl
CaSO3 + 2HCl →CaCl2 + H2O + SO2↑
Conf. The colourless gas was passed through Orange paper turns green SO32-
Test acidified K2Cr2O7 paper confirmed
K2Cr2O7 + 4H2SO4 →K2SO4 +Cr2(SO4)3 + 4H2O + 3[O]
Na2SO3 + [O] → Na2SO4
3. A small amount of salt was treated Colorless gas with rotten egg smell Maybe S2-
with dil. HCl
ZnS + 2HCl → ZnCl2 + H2S↑
Conf. The colourless gas was passed through Paper turns black S2- confirmed
Test (CH3COO)2Pb paper
Na2S + (CH3COO)2Pb → PbS↓ + 2CH3COONa
II. Conc. H2SO4 group
1. A small amount of salt was treated Colourless gas with pungent smell, Maybe- Cl-
with conc. H2SO4 gives white fumes with glass rod
dippen in NH4OH
NaCl + H2SO4 → NaHSO4 + HCl↑
HCl + NH4OH → NH4Cl↓ + H2O
Conf. To the salt solution added AgNO3 sol. White ppt. soluble in NH4OH Cl- confirmed
Test 1
NaCl + AgNO3 → AgCl ↓+ NaNO3
AgCl + 2NH4OH → [Ag(NH3)2]Cl + 2H2O
Conf. To smal amount of salt added a pinch Orange red fumes which on passing Cl- confirmed
Test 2 of solid K2Cr2O7 and added conc. H2SO4 through (CH3COO)2Pb solution
turns yellow
4NaCl + K2Cr2O7 + 3H2SO4 → 2Na2SO4 + K2SO4 + 2CrO2Cl2↑ + 3H2O
CrO2Cl2↑ + 4NaOH → Na2CrO4 + 2H2O + 2NaCl
Na2CrO4 + (CH3COO)2Pb → PbCrO4↓ + 2CH3COONa
Conf. Heated a pinch of salt with a small amt. Greenish yellow gas having pungent Cl- confirmed
Test 3 of MnO2 and added conc. H2SO4 smell
2NaCl + MnO2 + 3H2SO4 → 2Na2SO4 + MnSO4 +H2O + Cl2↑
2. A small amount of salt was treated Reddish brown vapous with pungent Maybe- Br-
with conc. H2SO4 smell
NaBr + H2SO4 → NaHSO4 + HBr↑
2HBr + H2SO4→ SO2 + 2H2O + Br2↑
Conf. To the salt solution added AgNO3 sol. Light yellow ppt. sparingly soluble in Br-confirmed
Test 1 NH4OH
NaBr+ AgNO3 → AgBr↓+ NaNO3
Conf. Heated a pinch of salt with a small amt. Yellowish brown vapours which turn Br-confirmed
Test 2 of MnO2 and added conc. H2SO4 starch paper yellow
2NaBr+ MnO2 + 3H2SO4 → 2Na2SO4 + MnSO4 +H2O + Br2↑
3. A small amount of salt was treated Deep violet vapous with pungent Maybe- I-
with conc. H2SO4 smell
NaI+ H2SO4 → NaHSO4 + HI↑
2HI + H2SO4→ SO2 + 2H2O + I2↑
Conf. To the salt solution added AgNO3 sol. yellow ppt. insoluble in NH4OH I- confirmed
Test 1
NaCI+ AgNO3 → AgI↓+ NaNO3
Conf. Heated a pinch of salt with a small amt. Violet vapours which turn starch I- confirmed
Test 2 of MnO2 and added conc. H2SO4 paper blue
2NaI+ MnO2 + 3H2SO4 → 2Na2SO4 + MnSO4 +H2O + I2↑
4. A small amount of salt was treated Reddish brown gas with pungent Maybe- NO3-
with conc. H2SO4 smell
Pb(NO3)2 + H2SO4 → PbSO4 + 2HNO3↑
4HNO3↑+heat→2H2O + 4NO2 ↑+ O2
Conf. Copper chips test Dark brown fumes of NO2 NO3-
Test 1 Heated a small amount of salt with confirmed
conc. H2SO4 and Cu turnings
2KNO3 + H2SO4 →K2SO4 + 2HNO3
4HNO3 + Cu → Cu(NO3)2 + 2NO2↑ +2H2O
Conf. Brown Ring Test
Test 2 Added small amount of freshly A dark brown ring is formed at the NO3-
prepared FeSO4 sol. to original solution junction of the acid and the solution. confirmed
and added conc. H2SO4 along the sides
of the test tube
KNO3 + H2SO4 → KHSO4 + HNO3
6FeSO4 + 3 H2SO4 +2 HNO3 → 3Fe(SO4)3 + 4H2O + 2NO
FeSO4 + NO + 5 H2O → [Fe(NO)(H2O)5]SO4
5. A small amount of salt was treated Colourless vapour having vinegar Maybe-
with conc. H2SO4 smell CH3COO-
CH3COONa + H2SO4 → NaHSO4 + CH3COOH
Conf. Oxalic Acid Test
Test 1 A small quntity of Oxalic acid(solid) and Smell of vinegar CH3COO-
salt(solid) was rubbed on a watch glass confirmed
with few drops of water and smelled
(COOH)2 + 2CH3COONa → (COONa)2 + 2CH3COOH
Conf. FeCl3 Test
Test 2 To the salt solution added FeCl3 Reddish brown filtrate
solution. The filtrate was divided into
two parts
i) To one part added Dil. HCl Reddish colour disappears CH3COO-
ii) To second part added confirmed
water and boiled Reddish brown ppt.
3CH3COONa + FeCl3 → (CH3COO)3Fe + 3NaCl
(CH3COO)3Fe + 2H2O → (CH3COO)(OH)2Fe↓ + 2CH3COOH
III. Independant group
1. To salt solution added BaCl2 solution White ppt Maybe SO4 2-
Na2SO4 + BaCl2 → BaSO4↓ + 2NaCl
Conf. To the white ppt. added Dil. HCl ppt. insoluble in Dil. HCl SO4 2-
Test 1 confirmed
2. Added conc. HNO3 to the salt in the
test tube and boiled. Added excess of Yellow ppt Maybe PO4 3-
ammonium molybdate solution
K3PO4 + 3(NH4)2MoO4 → 2(NH4)3PO4 + 3K2MoO4
K2MoO4 + 2HNO3 → H2MoO4 + 2KNO3
H2MoO4 → MoO3 + H2O
(NH4)3PO4 + 12Moo3 + 6H2O →(NH4)3PO4.12MoO3.6H2O↓
Conf. Magnesia mixture test
Test 1 To the salt solution added magnesia
mixture(mixture of solid NH4Cl and PO4 3-
White ppt confirmed
MgCl2 solution boiled and cooled and
added excess of NH4OH) and allowed
to stand.
Na2HPO4 + MgCl2 +NH4OH → Mg(NH4)PO4↓ + 2NaCl + H2O
V. Test for cations
A clear solution of the salt in distilled water should be made before doing the tests.This is said to be
the original solution. If the salt is not soluble in distilled water than dil. HCl/dil. HNO 3 is added and
heated to remove the evolving gas completely.

S. No. Experiment Observation Inference

I. Zero group – NH4+


1. To the solid salt added NaOH solution Gas with smell of ammonia and it Maybe-NH4+
gives white fumes with a glass rod
dipped in dil. HCl
NH4Cl + NaOH→ NaCl + H2O + NH3↑
NH3 + HCl → NH4Cl (white fumes)
Conf. To the salt solution added NaOH Brown ppt. NH4+
Test 1 solution and Nessler’s reagent (K2HgI4) confirmed
2K2[HgI4] + NH3 +3KOH →H2N.HgO.HgI↓ + 7KI + 2H2O
II. group I (Silver group)– Pb2+,Ag+,Hg22+
1. To the salt solution added dil. HCl White ppt. Maybe-Pb2+
Pb(NO3)2 + 2HCl → PbCl2↓ + 2HNO3
Conf. To the salt solution added KI solution Yellow ppt. Pb2+
Test 1 confirmed
PbCl2 + 2KI → PbI2↓ + 2KCl
Conf. To the salt solution added K2CrO4 Yellow ppt. Pb2+
Test 2 solution confirmed
PbCl2 + K2CrO4 → PbCrO4↓ + 2KCl
III. group II (Copper group)– Pb2+, Cu2+, As3+
1. To the salt solution added dil. HCl and Black ppt. Maybe- Pb2+
passes H2S gas or Cu2+
PbCl2 + H2S → PbS ↓ + 2HCl
Note: As Pb2+ would have been already precipitated in first group, proceed to confirm Cu 2+
Conf. To the salt solution added NH4OH Deep blue coluration Cu2+
Test 1 confirmed
CuSO4 + 4NH4OH → [Cu(NH3)4]SO4
Conf. To the salt solution added Pot. Chocolate brown ppt Cu2+
Test 2 Ferrocyanide sol. confirmed
CuSO4 + K4[Fe(CN)6]→ Cu2[Fe(CN)6]↓ + 2K2SO4
2. To the salt solution added dil. HCl and yellow ppt. Maybe- As3+
passes H2S gas
2AsCl3 + 3H2S → As2S3↓ + 6HCl
Conf. Dissolved the yellow ppt in conc. HNO3 yellow ppt. As3+
Test 1 and added ammonium molybdate confirmed
solution and heated
As2S3 + 10HNO3 → 2H3AsO4 + 10NO2 + 3S + 3H2O
H3AsO4 + 12 (NH4)2MoO4 + 21 HNO3→(NH4)3AsO4 .12MoO3↓ + 21NH4NO3 + 12H2O
IV. group III (Iron group)– Fe2+, Fe3+, Al3+, Cr3+
1. To the salt solution added solid NH4Cl White ppt Maybe- Al3+
and excess of NH4OH
AlCl3 + 3NH4OH → 3NH4Cl + Al(OH)3↓
Conf. Blue Lake Test
Test 1 The white ppt was dissolved in dil. HCl Blue ppt. floating in the colourless Al3+ confirmed
and to it was added a few drops of blue solution.
litmus solution.
Al(OH)3 + 3HCl → AlCl3 + 3H2O
AlCl3 + 3NH4OH → 3NH4Cl + Al(OH)3↓
2. To the salt solution added solid NH4Cl Brown ppt Maybe- Fe3+
and excess of NH4OH
FeCl3 + 3NH4OH → 3NH4Cl + Fe(OH)3↓
Conf. Dissolved the brown ppt in dil. HCl Prussian blue coloration Fe3+ confirmed
Test 1 and added pot. Ferrocyanide
FeCl3 + 3K4[Fe(CN)6]→ Fe4[Fe(CN)6]3↓ + 12KCl
Conf. Dissolved the brown ppt in dil. HCl Blood red colouration Fe3+ confirmed
Test 2 and added pot. Sulphocyanide
FeCl3 + 3KCNS → 3KCl + Fe(CNS)3
3. For Fe2+,conc. HNO3 is added in the analysis of group III which serves to oxidise it to Fe3+
Fe2+ gives green ppt with NH4Cl and NH4OH. FeCl2 + 2NH4OH → 2NH4Cl + Fe(OH)2↓
V. group IV (Zinc group)– Zn2+, Co2+, Ni2+, Mn2+
1. To the salt solution added solid NH4Cl Dull white ppt. Maybe- Zn2+
and excess of NH4OH and passed H2S
gas
Zn(OH)2 + H2S → 2H2O + ZnS↓
Conf. To the salt solution added few Bluish white ppt. Zn2+
Test 1 drops of Dil. HCl to acidify it and confirmed
then added pot. Ferrocyanide
2ZnCl2 + K4[Fe(CN)6] → Zn[Fe(CN)6]↓ + 4KCl
Conf. To the salt solution added NaOH White ppt. soluble in excess Zn2+
Test 2 solution confirmed
ZnCl2 +2NaOH → Zn(OH)2↓ + 2NaCl
Zn(OH)2 + 2NaOH → Na2ZnO2 ↓ + 2H2O
2. To the salt solution added solid NH4Cl Black ppt Maybe- Ni2+ or
and excess of NH4OH & passed H2S gas Co2+
Ni(OH)2 + H2S → 2H2O + NiS↓
As salt is greenish colour, confirmatory test for Ni2+ is done.
Conf. To salt solution added ammonium Rose red ppt. Ni2+ confirmed
Test 1 hydroxide solution and few drops of
dimethyl glyoxime.

3. To the salt solution added solid NH4Cl Black ppt Maybe- Ni2+ or
and excess of NH4OH & passed H2S gas Co2+
Co(OH)2 + H2S → 2H2O + CoS↓
As salt is purple or deep violet, confirmatory test for Co2+ is done.
Conf. To the salt solution added NaoH Blue ppt. changing to light pink Co2+
Test 1 solution. confirmed
Co(NO3)2 + 2 NaOH →Co(OH)2↓+ 2 NaNO3
Conf. To the salt solution added NH4OH Yellow ppt Co2+
Test 2 solution.Add CH3COOH and a crystal of confirmed
KNO2.
CoCl2 +2KNO2 → 2KCl +Co(NO2)2
KNO2 +CH3COOH → CH3COOK + HNO2
Co(NO2)2 +HNO2→ Co(NO2)3 + H2O + NO
Co(NO2)3 + 3KNO2 → K3[Co(NO2)6] ↓
4. To the salt solution added solid NH4Cl Buff(flesh/earth colour) ppt Maybe- Mn2+
and excess of NH4OH & passed H2S gas
Mn(OH)2 + H2S → 2H2O + MnS↓
Conf. To the salt solution added NaoH White/ Cream-Peach ppt which do Mn2+
Test 1 solution. not dissolve in excess confirmed
Add Br2 water On standing a characteristic brown
ring at the surface exposed to air
Mn(NO3)2 + 2 NaOH → Mn(OH)2↓+ 2 NaNO3
Br2 + H2O → 2HBr +[O]
Mn(OH)2 + [O]→ MnO(OH)2↓
VI. group V (Calcium group)– Ba2+, Sr2+, Ca2+
1. To the salt solution added NH4Cl solid, White ppt Maybe
NH4OH in excess and (NH4)2CO3 solution Ca2+ ,Sr2+ ,Ba2+
BaCl2 + (NH4)2CO3 → BaCO3↓ + 2NH4Cl
SrCl2 + (NH4)2CO3 → SrCO3↓ + 2NH4Cl
CaCl2 + (NH4)2CO3 → CaCO3↓ + 2NH4Cl
To the white ppt added CH3COOH and boiled off CO2 . It was then divided into three parts.
BaCO3 + 2CH3COOH → (CH3COO)2Ba + CO2↑ + H2O
SrCO3 + 2CH3COOH → (CH3COO)2Sr+ CO2↑ + H2O
CaCO3 + 2CH3COOH → (CH3COO)2Ca + CO2↑ + H2O
Conf. To one part of the solution added Yellow ppt Ba2+
Test 1 K2CrO4 solution confirmed
(CH3COO)2Ba + K2CrO4 → 2CH3COOK + BaCrO4↓
Conf. To second part added (NH4)2SO4 White ppt Sr2+
Test 2 solution confirmed
(CH3COO)2Sr+ (NH4)2SO4 → 2CH3COONH4 + SrSO4↓
Conf. To second part added (NH4)2C2O4 White ppt Ca2+
Test 3 solution confirmed
(CH3COO)2Ca + (NH4)2C2O4 → 2CH3COONH4 + CaC2O4 ↓
VI. group VI (Magnesium group)– Mg2+
1. To the salt solution added NH4Cl solid, White ppt. Maybe
NH4OH in excess and (NH4)2HPO4 Mg2+
solution and scratched the sides of the
test tube with a glass rod
MgCl2 + NH4OH + (NH4)2HPO4 → Mg(NH4)PO4↓ + 2NH4Cl + H2O
Conf. To the salt solution added NaOH A violet colouration changing to Mg2+
Test 1 solution and added a few drops of green confirmed
Magneson reagent

IV. Result:
The given salt contained Cation:_____________ and Anion:____________

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