SYSTEMATIC ANALYSIS OF THE SIMPLE SALT ANALYSIS

PRELIMINARY TESTS
1 Colour: Note the colour of the salt Blue or Bluish green Cu2+ or Ni2+
Greenish Ni2+
Light green Fe2+
Dark brown Fe3+
Pink Co2+
Light pink, flesh colour or earthy colour Mn2+
White Shows the absence of Cu2+, Ni2+, Fe2+, Fe3+, Mn2+, Co2+

2 APPEARANCE AND SOLUBILITY: Appearance of the salt is noted and a little of the salt is shaken Crystalline and soluble May be sulphate, nitrate or chloride salts
well with distilled water
3 Odour: Take a pinch of the salt between your fingers and rub with a drop of water Ammoniacal smell NH4+
Vinegar like smell CH3COO–
Smell like that of rotten eggs S2–
4 Density: Judge the density of the salt by placing it in your palm. (i) Heavy Salt of Pb2+, or Ba2+
(ii) Light fluffy powder Carbonate
5 Deliquescence: Take a small amount of salt and expose it in the atmosphere Salt absorbs moisture and (i) If coloured, may be
becomes paste like Cu(NO3)2, FeCl3
(ii) If colourless, may be
Zn(NO3)2, chlorides of
Zn2+, Mg2+ etc.

6 Dry heating test: A pinch of the salt is heated strongly in a dry boiling tube Colourless and odourless gas which turns lime water milky Presence of CO32-
Colourless gas and smells like rotten egg Presence of S2-
Colourless gas with Pungent smell, white fumes when a glass rod dipped Presence of Cl-
aqueous NH3 is brought near the mouth of the test tube
Colourless gas with ammonia smell, white fumes when a glass rod Presence of NH4+
dipped dilute HCl is brought near the mouth of the test tube
Reddish brown fumes Presence of NO3-
Yellow when hot, white when cold Presence of Zn2+
Brown when hot, yellow on cold Presence of Pb2+
White residue, glows on heating Presence of Ba2+, Ca2+, Mg2+, Al3+
7 Flame test: To a pinch of the salt taken in a watch glass, added a drop of conc.HCl . Introduced the Brick red presence of Ca2+
paste into a non-luminous Bunsen flame using a charred match stick. Apple green presence of Ba2+
Green flashes Presence of Zn2+ or Mn2+
Bright bluish green Presence of Cu2+
Dull bluish white Presence of Pb2+
IDENTIFICATION OF ACID RADICAL
1 Action of dil. HCl: To a pinch of the salt added a few drops of dil. HCl 1. Colourless, odourless gas with brisk effervescence, which turns lime Presence of CO3 2–
water milky.
2. Colourless gas with smell like that of rotten eggs which turns lead Presence of S2–
acetate paper black.
3. No gas evolved. Absence of carbonate, sulphide
2 Copper turnings test: A small amount of salt is heated with copper turnings and conc. H2SO4 Reddish brown gas is evolved. Presence of NO3–

3 Chromyl chloride test: Mix a small quantity of the salt with a small amount of powdered A yellow precipitate was obtained. (if no red/orange vapours observed - Presence of Chloride is confirmed
potassium dichromate. Take the mixture in a test tube and add conc. H2SO4. Heat the tube and absence of Cl-)
pass the red vapours evolved into the gas detector containing NaOH solution. To the yellow
solution thus obtained, add dil. acetic acid and lead acetate solution.
4 Action of conc. H2SO4: To a pinch of the salt added a few drops of concentrated conc. H2SO4 1. Colourless gas with Pungent smell, white fumes when a glass rod Presence of Cl-
dipped aqueous NH3 is brought near the mouth of the test tube or
Colourless gas with pungent smell, white fumes with aqueous ammonia
(NH4OH), white ppt. with AgNO3 solution.

2. Reddish brown gas with pungent smell, turns FeSO4 solution black. Presence of NO3–

3. Colourless vapours with smell of vinegar, turns blue litmus red. Presence of CH3COO–

4. No gas/vapours evolve. Cl–, Br –, I–, NO3–, CH3COO– absent

PREPARATION OF SODIUM CARBONATE EXTRACT : A pinch of salt is mixed with double the amount of sodium carbonate and is boiled with distilled water for sometime. The suspension obtained is filtered.The filtrate is
sodium
1 carbonate extract.
Barium chloride test: To a few drops of extract add dilute HCl in a test tube and boil. Filter the A white ppt. insoluble in conc. HCl Presence of SO42-
contents, and to the filtrate add few drops of BaCl2 solution.

2 Brown ring test: To a few drops of extract add a small quantity of freshly prepared solution of A dark brown ring is formed at the junction of the layers of the acid and Presence of NO3-
ferrous sulphate and then pour concentrated sulphuric acid slowly along the sides of the test tube the solution.

PREPARATIONS OF ORIGINAL SALT SOLUTION: The salt is dissolved in water in cold, if the salt does not dissolve heat the contents and the solution is used to identify the group in which the basic radical is present
GROUP ANALYSIS
1 To the salt added Nesselrs reagent and excess of NaOH is added. brown precipitate Presence of ammonium(zero group)
2 To the salt solution, added dil. HCl white ppt. Presence of Pb2+(group 1)
3 To the salt solution, added dil. HCl and yellow ammonium sulphide black ppt. or yellow ppt. Presence of Cu2+ Or Cd2+(group II)
4 Take about 5 ml of the original solution and add 4–5 drops of conc. nitric acid. Boil the solution for gelatinous white ppt Presence of Al3+ (group III)
sometime. Add to it about 2 g of solid NH4Cl and boil again. Cool the solution under tap water.
Add excess of ammonium hydroxide to it and shake.
5 Take about 5 ml of the original solution and add 4–5 drops of conc. nitric acid. Boil the solution for dirty white ppt Presence of Zn2+( group IV)
sometime. Add to it about 2 g of solid NH4Cl and boil again. Cool the solution under tap water.
Add excess of ammonium hydroxide to it and shake. Now add yellow ammonium sulphide

6 To the O.S. add 2–3 gms of solid NH4Cl, boil, cool and add NH4OH till the solution smells of white ppt Presence of Ca2+,Ba2+,Sr2+ (group V)
ammonia. Then add (NH4)2CO3 solution.
7 To a part of the original solution add some solid NH4Cl and NH4OH in slight excess. Then add white ppt Presence of Magnesium (group VI)
ammonium phosphate solution
CONFIRMATORY TEST FOR ACID RADICALS
1 Confirmation of Chloride, Cl-
i) Silver nitrate test: Acidify a portion of aqueous solution (or sodium carbonate extract) with dil. A curdy white ppt. completely soluble in NH4OH and insoluble in dil. Presence of Chloride is confirmed
HNO3. Boil for some time, cool and add silver nitrate solution. HNO3
ii) Chromyl chloride test: Mix a small quantity of the salt with a small amount of powdered A yellow precipitate was obtained Presence of Chloride is confirmed
potassium dichromate. Take the mixture in a test tube and add conc. H2SO4.
Heat the tube and pass the red vapours evolved into the gas detector containing NaOH solution.
To the yellow solution thus obtained, add dil. acetic acid and lead acetate solution.

iii) Manganese dioxide test: Heat a pinch of the salt with a small quantity of manganese dioxide and Evolution of greenish yellow gas having a pungent irritating smell. Presence of Chloride is confirmed
conc. H2SO4.

2 Confirmation of Nitrate, NO3-

i) Brown ring test: To a part of the aqueous solution add a small quantity of freshly prepared A dark brown ring is formed at the junction of the layers of the acid Presence of Nitrate is confirmed
solution of ferrous sulphate and then pour concentrated sulphuric acid slowly along the sides of and the solution.
the test tube
ii) Copper chips test: Heat a small quantity of the original salt with concentrated sulphuric acid and a Dark brown fumes of nitrogen dioxide are evolved. Presence of Nitrate is confirmed
few copper chips.
3 Confirmation of Sulphate, SO42-
i) Barium chloride test: To a part of the aqueous solution of the salt add barium chloride solution. A white ppt. insoluble in dil. HCl Presence of Sulphate is confirmed

ii) Lead acetate test: To an aqueous solution added lead acetate solution A white ppt. soluble in NaOH ( or ammonium acetate) Presence of Sulphate is confirmed

4 Confirmation of Carbonate, CO32-

i) Dil HCl test: To the salt solution, added dil HCl Brisk effervescence with evolution of CO2 which turns lime water milky Presence of carbonate is comfirmed

ii) Magnesium sulphate test: To an aqueous solution added magnesium sulphate solution A white ppt. is formed Presence of carbonate is comfirmed

5 Confirmation of Sulphide, S2-

i) Silver nitrate test: To salt solution add silver nitrate solution black ppt. soluble in HNO3 Presence of sulphide is comfirmed
ii) Sodium nitroprusside test: Take a portion of aqueous solution (or sodium carbonate extract) in a A purple or violet colouration Presence of sulphide is comfirmed
test tube and add a few drops of sodium nitroprusside solution
iii) Lead acetate test: To a portion of aqueous solution (or sodium carbonate extract acidified with dil. Black percipitate is formed Presence of sulphide is comfirmed
Acetic acid) add lead acetate solution.

6 Confirmatory test for acetate ion:

i) Oxalic acid test: Take a small quantity of the salt on a watch glass. Mix it with solid oxalic acid. Smell like that of vinegar Presence of acetate is confirmed
Prepare paste of it with a few drops of water. Rub the paste and smell.
ii) Ester test: Take a small quantity of the salt in a test tube. Add conc. H2SO4 (2 ml) and heat. Now Pleasant fruity smell of ester Presence of acetate is confirmed
add ethyl alcohol (1 ml). Shake and pour the contents of the tube in a beaker full of water. Stir.

iii) Ferric chloride test: Take water extract of the salt. Add neutral ferric chloride solution. Filter and Reddish coloured filtrate. Presence of acetate is confirmed
divide the filtrate into two portions. Reddish colour disappears.
(i) To one part, add dil. HCl. Reddish brown ppt.
(ii) To second part, add water and boil.

CONFIRMATORY TEST FOR BASIC RADICAL

1 Confirmation of ammonium, NH4+
i) Conc. NaOH test: The salt solution was heated with Conc. NaOH solution. A glass rod dipped in dil. Gas evolved with Characteristic ammoniacal smell. The gas gives white Presence of Ammomium (group 0) is confirmed
HCl was brought near the test tube in which gas was evolved fumes
ii) Nesseler’s test: To the salt added a few ml of nessler's reagent and excess of NaOH is added Brown ppt. was obtained Presence of ammonium (group 0) is confirmed

2 Confirmation of lead, Pb+

Dissolve the ppt. in hot ammonium acetate solution. Divide the solution into two parts :
i) Potassium iodide test Yellow ppt. is formed. The ppt. dissolves in boiling water and on Presence of lead (group I) is confirmed
To one part add pot. iodide solution. cooling recrystallises.
ii) Potassium chromate test Yellow ppt. is formed which dissolves in NaOH solution. Presence of lead (group I) is confirmed
To another part add pot. chromate solution.

3 Confirmation of Aluminum, Al3+

Dissolve the ppt. in dilute HCl, and divide the solution into three parts.
i) NaOH test: To the above solution added NaOH solution Gelatinous white ppt soluble in excess NaOH solution. Presence of Aluminium (group III) is confirmed
ii) Aluminium lake test: Add to it two drops of blue litmus solution. To this, add NH4OH dropwise till Blue ppt. floating in the colourless solution. Presence of Aluminium (group III) is confirmed
blue colour develops.
iii) Aluminion test: To another part of the solution added aluminon reagent A red lake was obtained. Presence of Aluminium (group III) is confirmed
4 Confirmation of zinc, Zn2+
i) Sodium hydroxide test: To one part of O.S. add sodium hydroxide solution dropwise. A white ppt which dissolves in excess of NaOH is formed Presence of Zinc (group IV) is confirmed
ii) Potassium ferrocyanide test: To another part, add pot. ferrocyanide soln. White or bluish white ppt. is formed. Presence of Zinc (group IV) is confirmed

5 Confirmation of Calcium, Ca2+

Filter and wash the ppt. with water. Dissolve the ppt. in hot dil. acetic acid
i) Ammonium oxalate test: To the third portion of the solution, add 1–2 ml of amm. oxalate A white ppt was obtained Presence of Calcium (group V) is confirmed
solution. Add a little amm. hydroxide
ii) Potassium Ferrocyanide test: To the salt solution added potassium Ferrocyanide solution. A white ppt was obtained Presence of Calcium (group V) is confirmed
iii) Flame test: Make a paste of the salt with the conc HCl. Introduce this paste to the flame A brick red flame Presence of Calcium (group V) is confirmed

6 Confirmation of Barium, Ba2+

Dissolve the ppt. in hot dil. acetic acid
i) Potassium chromate test: To one part of the solution,add a few drops of potassiumchromate A yellow ppt was obtained Presence of Barium (group V)is confirmed
solution.
ii) Flame test: To a pinch of the salt taken in a watch glass, added a drop of conc.HCl. Introduced Apple green flame Presence of Barium (group V) is confirmed
the paste into a non-luminous Bunsen flame

7 Confirmation of Magnesium, Mg2+

i) Ammonium phosphate test: To the original salt solution added NH4OH and NH4Cl in slight excess. A white ppt. was obtained Presence of Magnesium (group VI)is confirmed
Then added ammonium phosphate solution and scratch the side of the test tube with a glass rod

ii) Magneson reagent Presence of Magnesium (group VI)is confirmed

RESULT
The given acid radical is _______________
The given basic radical is _______________
The given simple salt is ________________