1 Salt Analysis - 1

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Experiment 1 (a):

Aim: Determination of one cation and one anion in unknown salt.


Physical examination of the salt:
Experiment Observation Inference
2+
1. Colour: Blue or bluish green Cu
Light green Fe2+
Dark brown Fe3+
Green Ni 2+
Pink Co2+
Light pink, flesh colour or earthy colour Mn2+
white Absence of above cations
2. Smell: Ammonical smell NH4+
Vinegar smell CH3COO-
Rotten egg smell S2-
Preliminary tests:
Experiment Observation Inference
4. Dry heating test: Colourless and odorless gas. May be CO32-
A pinch of the salt was taken in a clean Brown color gas May be NO3- or Br-
and dry test tube and was heated Yellowish green gas with pungent smell May be Cl-
strongly for 4 to 5 min. in oxidizing Melts with Vinegar like smell May be CH3COO-
flame. White sublimate formed or volatile May beNH4+
White residue glows on heating Zn2+, Ca2+, Sr2+, Ba2+, Mg2+, Al3+
Yellow when hot, white when cold May be Zn2+
Brown when hot yellow when cold May be Pb2+
Salt swells up May be Ca2+, PO43-, Al3+
5. Charcoal cavity test: Completely volatile May beNH4+
A pinch of the salt was heated in a Yellow when hot, white when cold May be Zn2+
charcoal cavity in the non-luminous White infusible and incandescent mass May be Zn2+, Ca2+, Sr2+, Ba2+,
flame with the help of a blow pipe. Mg2+, Al3+
Swells up May be Ca2+, PO43-, Al3+
Melt and shrink May be CH3COO-
6. Cobalt nitrate test: Green May be Zn2+
1 -2 drops of cobalt nitrate solution Pink May be Mg2+
were dropped on the white residue left Blue May be Al3+ or PO43
after charcoal cavity test.
7. Flame test: Brick red May be Ca2+
A paste was prepared with salt and 1-2 Crimson red May be Sr2+
drops of conc. HCl in a watch glass. A
Grassy red May be Ba2+
clean Nichrome wire was used to pick
up the paste. Then it was shown to the Green flashes May be Zn2+, Mn2+
flame. Dull bluish white May be Pb2+

Identification of acid radicals (Dry test):

Experiment Observation Inference


8. Dilute sulphuric acid test: Colorless, odorless gas with brisk Gas Ion
A small amount of salt was treated effervescence turns lime water milky. Co2 CO32-
with 1-2 ml of dil. H2SO4. Colorless pungent smell, turns acidified SO2 SO32-
potassium dichromate solution green
Colorless rotten egg smell turns lead acetate H2S S2-
paper black
Reddish brown gas, pungent smell turns NO2 NO2-
ferrous sulphate solution black.
No observation CO32-, SO32-, S2-, NO2- Absent
9. Conc. sulphuric acid test: Color less gas with pungent smell HCL Cl-
Small amount of salt was treated with Reddish brown vapour with pungent smell Br2 Br-
1-2 ml of conc. sulphuric acid Deep violet vapour with pungent smell I2 I-
Reddish brown gas with pungent smell NO2 NO3-
Colorless vapours, vinegar smell, CH3COOH CH3COO-
Colourless and odorless gas, burns with blue CO C2O42-
flame
No observation Cl-, Br-, I-, NO3-, CH3COO-,
C2O42- Absent
10. Individual Test for sulphate
a. To the salt solution BaCl2 solution White ppt. obtained which was insoluble in dil.
was added. HCl.
b. To the salt solution lead acetate White ppt. was obtained which was soluble in SO42- conf.
was added. excess hot Amm. acetate solution

11. Individual Test for PO43-


To the salt solution conc. HNO3 was A canary yellow ppt was obtained
added and boiled. Then excess amm. PO43-Conf.
molybdate solution was added and
again boiled.
Confirmation (wet) test for acid radicals:

12. Test for CO32-


a. Dil. HCl test: To the solution of the Brisk effervescence and evolution of CO2 which
salt dil. HCl was added turns lime water milky. CO32- conf.
b. CaCl2 test: To the solution of the White ppt. was obtained
salt CaCl2 solution was added
13. Test for SO32-
a. BaCl2 test: To the salt solution few White ppt. was obtained which was dissolved
drops of BaCl2 solution was added. in dil. HCl with liberation of SO2 gas. SO32- conf
b. K2Cr2O7 test: To the salt solution Green coloration was obtained.
few drops of K2Cr2O7 solution was
added along with dil. sulphuric acid.
14. Test for NO2- :
a. FeSO4 test: To the salt solution few Dark brown coloration was obtained
drops of dil. acetic acid and FeSO4
solution was added.
b. Starch iodide test: To the salt Blue solution was obtained NO2- conf.
solution few drops of dil. H2SO4 and
few drops of KI was added followed
freshly prepared starch solution.
c. Diphenylamine test: To the salt Deep blue coloration obtained
solution few drops of diphenylamine
was added.
15. Test for S2- :
a. Sod. nitroprusside test: Few drops Purple coloration was obtained
sod. nitroprusside solution was added
to the salt solution. S2- conf.
b. Lead acetate test: A few drops of Black ppt. was obtained
lead acetate solution was added to
the salt solution
16. Test for Cl-
a. AgNO3 test: Salt solution was white ppt. was obtained and dissolved in amm.
acidified with dil. HNO3, boiled and Hydroxide.
cooled. AgNO3 solution was added
b. Chromyl Chloride test: Conc. H2SO4 Yellow ppt. was obtained
was added to a mixture of salt and Cl- conf.
solid pot. dichromate and then
heated. Red vapor evolved was passed
into NaOH solution and a yellow
solution was obtained. Then dil. Acetic
acid and lead acetate solution was
added.
17. Test for Br- Yellow ppt. was obtained and was dissolved in
a. AgNO3 test: Salt solution was amm. hydroxide. Br- conf.
acidified with dil. HNO3 , boiled and
cooled. AgNO3 solution was added
b. MnO2 test: Salt with solid A yellowish brown vapour turned starch paper
manganese dioxide and H2SO4 was yellow.
heated.
18. Test for I –
a. AgNO3 test: Salt solution was Yellow ppt. was obtained and was dissolved in
acidified with dil. HNO3 , boiled and amm. hydroxide.
cooled. AgNO3 solution was added I – conf.
b. MnO2 test: Salt with solid violet vapour turns starch paper blue.
manganese dioxide and H2SO4 was
heated.
19. Test for NO3-
a. Ring test: To the salt solution conc. A dark brown ring was formed.
H2SO4 was added and then freshly
prepared solution of FeSO4 was added
slowly along the side of the test tube. NO3- conf.
b. Copper chips test: The salt solution Reddish brown gas was evolved.
was heated with conc. H2SO4 and few
copper chips.

20. Test for CH3COO-


a. Oxalic acid test: A paste was Vinegar smells
prepared by mixing solid oxalic acid
and salt with few drops of water,
rubbed and smelled.
b. Ferric chloride test: neutral ferric Reddish color solution obtained. CH3COO- conf.
chloride solution was added to the salt
solution and divided into two parts.
1.To 1st part of the solution dil. HCl Reddish color fades up.
was added.
2.To the 2nd part of the solution Reddish brown ppt. obtained.
water was added and boiled.
21. Test for oxalate
a. The salt soln was added to dil. H2SO4 Purple color of KMnO4 decolorized.
and heated. then KMnO4 solution was C2O42- conf.
added drop by drop.
b. the salt solution was added to CaCl2 Curdy white ppt.
solution.
Identification of basic radicals
22. Test for ammonium (zero group):
The salt was heated with conc. NaOH Gas evolved with ammoniacal smell. NH4+ present
Confirmation test for NH4+ .
a. Dil. HCl test: A glass rod dipped in White fumes were obtained
dil. HCl was brought near the mouth of NH4+ confirmed
the test tube.
b. The gas was passed through Brown ppt. was obtained.
Nessler’s reagent
Preparation of ORIGINAL SOLUTION (O.S):
Small amount of salt was taken in a test tube. Suitable solvent (cold/hot water, dil. HCl) was added and shaken well.
GROUP ANALYSIS:
Experiment Observation Inference
1.To a part of O.S, dil. HCL was added. White ppt. formed Gr. 1 radicals (Pb2+)
2.To a part of O.S, H2S gas was passed. Coloured/yellow ppt formed Gr. 2 radicals (Cu2+ As3+)
3. To a part of O.S, NH4Cl and NH4OH were added. Reddish brown/white ppt. Gr.3 radicals (Fe3+, Al3+)
formed
4.To a part of O.S, H2S gas was passed. Black/white/buff coloured ppt. Gr.4 radicals (Mn2+, Ni 2+, Zn2+,
formed Co2+)
5.To a part of O.S, (NH4)2CO3 and NH4OH were White ppt. formed Gr.5 radicals (Ca2+, Sr2+, Ba2+)
added.
24. Group-I analysis: The original solution was divided into three parts.
To the 1st part KI was added. Yellow ppt. was obtained (PbI2)
To the 2nd part K2CrO4 soln was added. Yellow ppt. was obtained (PbCrO4) Pb2+ conf.
rd
3 part was cooled. White ppt. was reappeared (PbCl2)
25. Group-II analysis (if coloured ppt): The original solution was two parts.
To the 1st part CH3COOH was added followed by KSCN Chocolate brown ppt. was obtained. Cu2+ conf.
To the 2nd part CH3COOH was added followed by KI White ppt. was obtained.
Group-II analysis (if yellow ppt): The original solution was two parts.
To the 1st part, ammonium molybdate{(NH4)2S} solution Yellow ppt. was obtained
was added and then heated As3+ conf.
To the 2nd part NH4OH and magnesia mixture (1:1:1 ratio White ppt. was obtained
of MgSO4, NH4Cl and NH4OH) was added.
26. Group-III analysis (if reddish brown ppt):The original solution was divided into two parts:
To the 1st part potassium ferrocyanide [K4Fe (CN)6] soln Prussian blue colored ppt. obtained
was added. Fe3+ conf.
nd
To the 2 part potassium thiocyanate (KSCN) was added. Red blood coloration obtained.
Group-III analysis (if gelatinous white ppt.): The original solution was divided into two parts.
To the 1st part, dil. NaOH was added. White ppt. obtained which was dissolved
in excess of NaOH solution. Al3+ conf.
To the 2nd part, few drops of blue litmus solution was Bluish white ppt. floating like lake formed.
added. Then NH4OH soln was added in drop wise.
27. Group-IV analysis (if buff colored):
To the original solution NaOH was added. Then bromine White ppt. turned brown.
(Br2) water was added and shaken well. Mn2+ conf.
The ppt. of gr-IV was treated with conc. HNO3 and then Pink colored solution was obtained.
lead peroxide (PbO2). Solution was boiled and then
cooled.
The ppt. of gr-IV (if dirty white colored): The original solution was divided into two parts.
To the first part, NaOH solution was added drop wise. White ppt. was obtained. Zn2+ conf.
nd
To the 2 part potassium ferrocyanide was added. White/Bluish white ppt. was obtained.
The ppt. of group-IV (if black colored ppt and O.S is greenish): The original solution was divided into two parts.
To the 1st part NH4OH solution was added. Then few
drops of dimethyl glyoxime. Rose red ppt. was obtained.
To the 2nd part NaOH solution was added followed by Ni2+ conf.
bromine water and then boiled. Black ppt. was obtained.
The ppt. of group-IV (if black colored ppt and O.S is purple or violet): The original solution was divided into two parts.
To the 1st part NH4OH solution was added followed by dil. Yellow ppt. was obtained.
CH3COOH. then was warmed by adding solid KNO3.
To the 2nd part ether was added followed by solid Blue colored was obtained. Co2+ conf.
ammonium thiocyanate(NH4CNS).

28. Group-V analysis: The original solution was divided into three parts.
1st part was treated potassium chromate {K2CrO4} Yellow ppt. was obtained Ba2+ conf.
solution.
2nd part was treated with ammonium sulphate{(NH4)2SO4} White ppt. was obtained Sr2+ conf.
solution and warmed.
3rd part was treated with ammonium oxalate {(NH4)2C2O4} White ppt. was obtained Ca2+ conf.
solution.
29. Group-VI analysis
To the salt solution, solid NH4Cl, NH4OH and ammonium White ppt. was obtained Mg2+ conf.
phosphate solution was added and the side of the test
tube was rubbed with a glass rod.

Name: ___________________

Class: ___________________

Section: ___________________

Roll no: ___________________

Group: ___________________

Experiment 1 (b):
Aim: Determination of one cation and one anion in the given salt no: 102
Physical examination of the salt:
Experiment Observation Inference
2+ , 2+ ,
1. Colour: White/ colourless Cu Fe Fe Ni 2+ , Co2+ Mn2+ are
3+ ,

absent.
2. Smell: Ammonical smell May be NH4+
3. Structure of the salt: Crystalline
4. Solubility: Soluble in cold water
Preliminary tests:
Experiment Observation Inference
5. 5. Dry heating test: white sublimate formed. May beNH4+
A pinch of the salt was taken in a clean
and dry test tube and was heated
strongly for 4 to 5 min. in oxidizing
flame.
6. Charcoal cavity test: Completely volatile. May beNH4+
A pinch of the salt was heated in a
charcoal cavity in the non-luminous
flame with the help of a blow pipe.
7. Cobalt nitrate test: No observation. Zn2+, Mg2+, Al3+ or PO43—
1 -2 drops of cobalt nitrate solution absent.
were dropped on the white residue left
after charcoal cavity test.
8. Flame test: No observation. Ca2+, Sr2+, Ba2, Zn2+, Mn2+ ,Pb2+
A paste was prepared with salt and 1-2 are absent.
drops of conc. HCl in a watch glass. A
clean Nichrome wire was used to pick
up the paste. Then it was shown to the
flame.
9. Borax bead test: Borax bead test is not required as the salt is colorless.

Identification of acid radicals (Dry test):

Experiment Observation Inference


10. Dilute sulphuric acid test: No observation CO32-, SO32-, S2-, NO2- Absent
A small amount of salt was treated
with 1-2 ml of dil. H2SO4.
11. Conc. sulphuric acid test: Colorless gas with pungent smell May be Cl-
Small amount of salt was treated with
1-2 ml of conc. sulphuric acid.
Confirmation (wet) test for acid radicals:

12. Test for Cl-


a. AgNO3 test: Salt solution was white ppt. was obtained and dissolved in amm.
acidified with dil. HNO3, boiled and Hydroxide.
cooled. AgNO3 solution was added
b. Chromyl Chloride test: Conc. H2SO4 Yellow ppt. was obtained
was added to a mixture of salt and Cl- conf.
solid pot. dichromate and then
heated. Red vapor evolved was passed
into NaOH solution and a yellow
solution was obtained. Then dil. Acetic
acid and lead acetate solution was
added.

Identification of basic radicals


13. Test for ammonium (zero group):
The salt was heated with conc. NaOH Gas evolved with ammoniacal smell. NH4+ present
Confirmation test for NH4+ .
a. Dil. HCl test: A glass rod dipped in White fumes were obtained
dil. HCl was brought near the mouth of NH4+ confirmed
the test tube.
b. The gas was passed through Brown ppt. was obtained.
Nessler’s reagent

Result: The cation and anion present in the supplied salt are found to be NH4+ and Cl- respectively.

Name: ___________________

Class: ___________________

Section: ___________________
Roll no: ___________________

Group: ___________________

Experiment 1 (c):
Aim: Determination of one cation and one anion in the given salt no: 512
Physical examination of the salt:
Experiment Observation Inference
2+ , 2+ ,
1. Colour: White/ colourless Cu Fe Fe Ni 2+ , Co2+ Mn2+ are
3+ ,

absent.
2. Smell: No characteristics smell. NH4+, CH3COO- & S2- are absent
3. Structure of the salt: Crystalline
4. Solubility: Soluble in cold water

Preliminary tests:
Experiment Observation Inference
5. Dry heating test: Brown color gas May be NO3- or Br-
A pinch of the salt was taken in a clean
and dry test tube and was heated
strongly for 4 to 5 min. in oxidizing
flame.
6. Charcoal cavity test: White infusible and incandescent mass May be Zn2+, Ca2+, Sr2+, Ba2+,
A pinch of the salt was heated in a Mg2+, Al3+
charcoal cavity in the non-luminous
flame with the help of a blow pipe.

7. Cobalt nitrate test: No observation. Zn2+, Mg2+, Al3+ or PO43—


1 -2 drops of cobalt nitrate solution absent.
were dropped on the white residue left
after charcoal cavity test.
8. Flame test: Crimson red May be Sr2+
A paste was prepared with salt and 1-2
drops of conc. HCl in a watch glass. A
clean Nichrome wire was used to pick
up the paste. Then it was shown to the
flame.
9. Borax bead test: Borax bead test is not required as the salt is colorless.

Identification of acid radicals (Dry test):

Experiment Observation Inference


10. Dilute sulphuric acid test: No observation CO32-, SO32-, S2-, NO2- Absent
A small amount of salt was treated
with 1-2 ml of dil. H2SO4.
11. Conc. sulphuric acid test: Reddish brown gas with pungent smell May be NO3-
Small amount of salt was treated with
1-2 ml of conc. sulphuric acid

12. Confirmation (wet) test for acid radicals:


Test for NO3-
a. Ring test: To the salt solution conc. A dark brown ring was formed.
H2SO4 was added and then freshly
prepared solution of FeSO4 was added
slowly along the side of the test tube. NO3- conf.
b. Copper chips test: The salt solution Reddish brown gas was evolved.
was heated with conc. H2SO4 and few
copper chips.

13. Identification of basic radicals:


Test for ammonium (zero group):
The salt was heated with conc. NaOH No Gas evolved with ammoniacal smell. NH4+ absent
14. Preparation of ORIGINAL SOLUTION (O.S):
Small amount of salt was taken in a test tube. Suitable solvent (cold/hot water, dil. HCl) was added and shaken well.
GROUP ANALYSIS

Experiment Observation Inference


1.To a part of O.S, dil. HCL was added. No ppt. formed Gr. 1 radicals (Pb2+) absent
2.To a part of O.S, H2S gas was passed. No ppt. formed Gr. 2 radicals (Cu2+ As3+) absent
3. To a part of O.S, NH4Cl and NH4OH were added. No ppt. formed Gr.3 radicals (Fe3+,Al3+) absent
4.To a part of O.S, H2S gas was passed. No ppt. formed Gr.4 radicals (Mn2+,Ni 2+ ,Zn2+,
Co2+) absent
5.To a part of O.S, (NH4)2CO3 and NH4OH were White ppt. formed Gr.5 radicals (Ca2+,Sr2+,Ba2+)
added. present

15.Group-V analysis: The original solution was divided into three parts.
1st part was treated potassium chromate {K2CrO4} No ppt. was obtained Ba2+ conf.
solution.
2nd part was treated with ammonium sulphate{(NH4)2SO4} White ppt. was obtained Sr2+ conf.
solution and warmed.

Result: The cation and anion present in the supplied salt are found to be Sr2+ and NO3- respectively.

Name: ___________________

Class: ___________________

Section: ___________________

Roll no: ___________________

Group: ___________________

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