Droppers, pipette

If reaction does not occur when a little allyl bromide is first introduced, further addition must be discontinued until the reaction has commenced. Remove 2-3 ml. of the Grignard solution with a dropper pipette, add about 0-5 ml. of allyl bromide and warm gently to start the reaction after this has reacted well, add the solution to the main portion of the Grignard reagent. 

Reflux 1 ml. of the ether with 5 ml. of freshly distilled, constant boiling point hydriodic acid (Section 11,49,2), b.p. 126-128°, for 2-3 hours. Add 10 ml. of water, distil and collect about 7 ml. of liquid. Decolourise the distillate by the addition of a httle sodium bisulphite, and separate the two layers by means of a dropper pipette (Fig. 11,27,1). Determine the b.p. of the resulting iodide by the Siwoloboff method (Section 11,12) and prepare a crystalline derivative (Section 111,42). 

Hydrolysis (or saponification) of n-butyl acetate. Boil 4-5 g. of n-butyl acetate (Section 111,95) with 50 ml. of 10 per cent, sodium hydroxide solution under reflux until the odour of the ester can no longer be detected (about 1 hour). Set the condenser for downward distiUation and coUect the first 10 ml. of distillate. Saturate it with potassium carbonate, aUow to stand for 5 minutes, and withdraw all the Uquid into a small pipette or dropper pipette. AUow the lower layer of carbonate solution to run slowly into a test-tube, and place the upper layer into a small test-tube or weighing bottle. Dry the alcohol with about one quarter of its buUr of anhydrous potassium carbonate. Remove the alcohol with a dropper pipette and divide it into two parts use one portion for the determination of the b.p. by the Siwoloboff method (Section 11,12) and convert the other portion into the 3 5-dinitrobenzoate (Section III, 27) and determine the m.p. 

A liquid may be transferred from one vessel to another with a dropper pipette (Fig. XII, 1, 2, a or b). If the dropper pipette is calibrated, it may be employed for measuring out a definite volume of liquid. 

A cyUndrical or, preferably, a pear-shaped separatory funnel (Fig. II, 1, 5, e and d) of 10-15 ml. capacity is usually employed for the separation of immiscible liquids. For separations on a smaller scale, a dropper pipette may be used the upper layer is best removed with a bent pipette as in Fig. XII, 1,3. For liquids which tend to emulsify, centrifugation (a hand centrifuge is satisfactory) will usually produce a clean line of demarcation between two immiscible liquids. 

Alternatively, add pure aqueous ammonia solution (1 1) by means of a dropper pipette until a definite precipitate of iron(III) hydroxide just begins to form. Now add concentrated hydrochloric acid dropwise, stirring and allowing to stand for a minute or two after each 2-3 drops, until a clear solution is obtained then add 1.5 mL of concentrated hydrochloric acid and mix well. 

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