Applied Science BTEC Nationals/Chemical Laboratory Techniques/Qualitative organic analysis

=Qualitative Organic Analysis=

The experimental details given here are given in good faith and are believed to be safe and workable methods. However, the authors cannot take responsibility for the consequences of performing these experiments.

The experiments are written for experienced science teaching staff to use as instructions for a supervised class of students. The experiments are not designed for students or inexperienced members of the public to perform without supervision. If you wish to attempt the experiments, ensure that you have completed a legally adequate risk assessment beforehand and that you work within the constraints of the risk assessment.

Burning
Place a small amount of the test substance on a crucible lid on a heat resistant mat in the fume cupboard. Attempt to ignite it by playing a small Bunsen flame on it from above.

Reaction With Alkali
To about 0.5 g or 1cm3 in a test tube, add about 5 cm3 of bench sodium hydroxide solution, a little at a time, shaking after each addition. If there is no apparent reaction in the cold, warm and eventually boil the mixture. Test for gases with litmus paper but be careful not to touch the solution with test papers.

Reaction With Sodium Carbonate or Hydrogencarbonate
To about 0.5 g or 1 cm3 in a test tube add about 5 cm3 of sodium carbonate solution, a little at a time and with shaking. Look for evolution of gas and test for carbon dioxide with lime water.

Fehling's Solution
Mix equal volumes (about 3 cm3) of Fehling's A & B and add 1 cm3 or 1 g of the test substance. Warm, gently at first and then boil.

"Neutral" Iron (III) Chloride
To 1 g or 1 cm3 of the test substance add "neutral" iron III chloride dropwise until no further colour change - if any - occurs. If in doubt perform a control or blank test using water in place of the test sample.

Potassium Manganate (VII) ('Permanganate')
Use acidified potassium manganate (VII) - mix equal volumes of dil. sulphuric acid and potassium permanganate solution. To about 1 cm3 or 1 g of the test sample, add a few drops of reagent. If there is no immediate reaction, warm the mixture. If reaction does take place, then by adding reagent to slight excess and boiling, it may be possible to detect the odour of the product.

Note (i) A brown ppt. is sometimes observed, especially if insufficient acid is added to the manganate (VII). (ii) alkaline manganate (VII) is sometimes used as an alternative - the expected colour change is then from purple to green.

Potassium Dichromate (VI)
Experimental details are similar to the manganate (VII) test. The expected colour change is orange to blue/green.

Nitrous Acid (Nitric (III) Acid)
Into a test tube cooled in a beaker of crushed ice, place 1 g sodium nitrite (nitrate III) and dissolve it in 5 cm3 water. Add 5 cm3 dil. hydrochloric acid dropwise slowly. Dissolve 0.5 g or 0.5 cm3 of the test sample in a similarly cooled tube. Add the nitrous acid solution to this.

Iodine Or Potassium Iodide
To 0.5 cm3 sample add 3 cm3 iodine solution (or potassium iodide) and 1 cm3 sodium hypochlorite (chlorate I). Add aqueous sodium hydroxide until the brown colour just fades.

Phosphorus (V) Chloride
Place a small amount of the sample in a dry tube and add the phosphorus V chloride carefully - "spitting" may occur.

Bromine Water
NB - bromine is sometimes used in organic solvents such as tetrachloromethane - the following observations may be different.

Place 1 cm3 of the sample in a tube and add the aqueous solution of bromine dropwise with shaking. If decolourisation occurs continue to add it until it is in excess.

2,4-Dinitrophenylhydrazine (Brady's Reagent)
To 1 cm3 of reagent add several drops of the sample. Dissolve solid samples in the minimum volume of methanol.

Tollen's Reagent
To 5 cm3 of silver nitrate solution, add 2 drops sodium hydroxide to ppt. silver oxide. Decant as much of the supernatant liquid as possible. Add aqueous ammonia dropwise until the silver oxide just dissolves. To this solution add a few drops of the sample, or an aqueous solution of it, and place the tube in a beaker of hot water for a few minutes. Use a clean narrow test tube for best results.

NB Tollen's reagent must never be stored and must be disposed with copious amounts of water immediately.

Chlorate (I) - Hypochlorite
A very sensitive and specific test for aniline - blue or purple colouration produced.