QUALITATIVE SEMI MICRO ANALYSIS

Analysis: It deals with the process of detection of various components present in a substance Qualitative analysis: To identify the nature of the components Quantitative analysis: To identify the amount of the components

MACRO ANALYSIS: Quantity of the substance is 0.1 to 10grams

MICRO ANALYSIS: Quantity of the substance is 10 to 100 mg

SEMI MICRO ANALYSIS: Quantity of the substance is 1 to 10 mg

Systematic Qualitative Semi micro Analysis

1. PRELIMINARY EXAMINATION 2. ANALYSIS OF ANIONS 3. ANALYSIS OF CATIONS

Colour test: By observing the colour of the substance we can predict the presence of some ions Ex. Light pink colour Mn+2 blue colour Cu+2 etc

1. PRELIMINARY EXAMINATION

PHYSICAL STATE: Crystalline or Amorphous

COLOUR:

SOLUBILITY: Water soluble or water insoluble

FLAME TEST:

Flame test: Take little amount of salt in a watch glass, add 2 to 3 drops of con. HCl and make it as a paste, take small amount of the paste on the loop of a platinum wire and introduce into the side of the busen flame

Flame colorations Barium (Ba+2 ) apple green

Strontium (Sr+2 ) crimson red

ANALYSIS OF ANIONS

Classification of anions
I. II. Carbonate(CO3-2), Sulphite(SO3-2), Sulphide (S-2) Chloride (Cl- ), Bromide(Br- ), Iodide (I- )

III. Sulphate (SO4-2), Phosphate (PO4-3). IV. Nitrate (NO3-), Acetate (CH3COO-)

ANALYSIS OF GROUP I ANIONS

Group reagent dil. HCl Experiment: Take little amount of dry salt in a clean & dry test tube, to this add few drops of dil. HCl. If first group anions are present you will observe a colourless gas coming out with effervesces

Observation and Inference

1. Colourles Odorless, gas turns lime water into milky white 2. Colourless gas with burning sulpher smell, turns the orange coloured potassium dichromate into green 3. Colourless gas with rotten egg smell, turns lead acetate into black

Carbonate(CO3-2)

Sulphite(SO3-2)

Sulphide (S-2)

ANALYSIS OF GROUP II ANIONS (wet test) Group reagent Silver Nitrate (AgNO3) Take few drops of salt solution in a test tube and add few drops of silver nitrate

Observation and Inference

1. A curdy white ppt appears immediately, the ppt is soluble in ammonia and it will be re obtained on adding dil. HNO3

Chloride (Cl- )

2. A pale yellow colored ppt is formed, it is insoluble in ammonia.

Bromide(Br- )

3. A bright yellow coloured ppt is formed, it is insoluble in ammonia

Iodide (I- )

ANALYSIS OF GROUP II ANIONS (dry test) Group reagent con. H2SO4

Experiment: Take little amount of dry salt in a clean & dry test tube, to this carefully add few drops of con. H2SO4

Observation and Inference

1. A colourless gas with pungent smell, which gives dense white fumes when a rod dipped in ammonium hydroxide is brought near the mouth of the test tube. 2. Reddish brown gas with a pungent Odour is evolved

Chloride (Cl- )

Bromide(Br-)

3. Violet vapours, which turn starch paper blue and a layer of violet sublimate is formed on the sides of the tube.

Iodide (I- )

ANALYSIS OF GROUP III ANIONS Group reagent Barium-Calcium Nitrate (Barium nitrate & Calcium nitrate)

Experiment: Take few drops of salt solution in a test tube and add few drops of Barium-Calcium Nitrate reagent with stirring

Observation and Inference

A white precipitate is obtained which remains undissolved after adding dil. HCl and heating.

sulphate (SO4-2) ion

A white precipitate is obtained which will get dissolved in dil. HCl

Phosphate (PO4-3) ion

ANALYSIS OF GROUP IV ANIONS

Test for Nitrate (NO3-) : i) Brown ring test: Take few drops of salt solution in a test tube and add few drops of freshly prepared saturated ferrous sulphate solution and stir. keep the test tube in inclined position and add few drops of con.H2SO4 with a dropper slowly along the side of the tube A brown ring forms at the junction of two liquids indicates the presence of Nitrate (NO3-) ion

Test for Acetate (CH3COO-)

Experiment: Take few drops of salt solution in a test tube and add few drops of neutral ferric chloride solution. You observe deep red colouration on dilution and upon boiling a brown coloured ppt will be formed. This indicates the presence of Acetate (CH3COO-) ion

ANALYSIS OF CATIONS Classification of cations into groups