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Paragraph 3

Changes not yet applied. Later legislation changes this provision in ways not yet written into the text below:

REAGENTS

  • Note: The suitability of a batch of aluminium oxide and of the other reagents should be tested before use by analysing a blank feed to which a known amount of meticlorpindol has been added.

    1. 3.1.

      Aluminium oxide for column chromatography, 100 to 250 mesh, alkaline, Brockman activity 1.

    2. 3.2.

      Ammonia (density 0.88g per ml).

    3. 3.3.

      Anion exchange resin, AG1-X8 or Dowex 1-X8, 100 to 200 mesh—To convert Dowex resin in the chloride form to the acetate form add 1 litre of 6M hydrochloric acid to 350g of resin in a 3 litre beaker, and heat the mixture on a steam bath for 2 to 3 hours. Pour the slurry into a glass Buchner funnel, and wash the resin with water until the washings are free from chloride (about 6 litres of water are required). Transfer the resin to a 50mm diameter glass column having a coarse sintered-glass disc at the bottom end, and wash with sodium acetate solution (5g sodium acetate, anhydrous, dissolved in water and diluted to 100ml) until the column effluent gives only a cloudy solution on addition of silver nitrate solution. Return the resin to the glass Buchner funnel, and wash with water. Transfer the resin to a 3 litre beaker, add 1 litre of 40% v/v acetic acid solution (3.4) and heat on a steam bath for 3 hours or longer. Filter, and wash the resin again with water until the washings are free from chloride. Store the resin in water.

    4. 3.4.

      Acetic acid solution 40% v/v.

    5. 3.5.

      Methanol.

    6. 3.6.

      Methanol solution 80% v/v.

    7. 3.7.

      Ammoniacal methanol solution: dilute 1 volume of ammonia (3.2) with 19 volumes of methanol (3.5).

    8. 3.8.

      Meticlorpindol standard solution: weigh, to the nearest 0.1mg, 125mg of meticlorpindol into a beaker, add 25ml of sodium hydroxide solution (2g sodium hydroxide dissolved in water and diluted to 100ml) to dissolve the meticlorpindol, transfer the solution to a 500ml graduated flask, and dilute to the mark with water. This solution contains 250μg per ml meticlorpindol.