Introduction to Quantitative Ultramicroanalysis by I. M. Korenman

By I. M. Korenman

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30. Heating the solution in a cone inserted into a capillary PRINCIPAL TECHNIQUES OF OPERATION diameter. and 47 The capillary is first filled with about 1 jul of water, sealed at one end by the microburner flame (Fig. 3 0 ) . The water is transferred by centrifuging to the sealed end, and a cone containing 0 . 1 - 1 jul of the liquid to be heated is inserted into the capillary. heating water. The open end of the operation is carried out capillary is sealed off and the in a test tube containing s o m e The high water vapor concentration in the capillary p r e - vents evaporation of the drop in the conical v e s s e l .

If the tested solution is taken in a volume of 1 ixl or m o r e , a s m a l l H 2S generator is employed. The apparatus (Fig. 31) basically consists of a test tube 1 (diameter, 4 - 6 m m ; length, 2 0 - 3 0 m m ) into which about 2 0 - 3 0 m g of pyrite of FeS is introduced together with 0 . 1 - 0 . 2 m l of a 2 N solution of H C 1 . A rubber tube 2 connects test tube 1 to a bent tube 3 drawn to a tapering capillary end. A wad of cotton 4 , stuffed into the wide portion of tube 3 , prevents FIG.

When the is turned on, the vibrating thread mixes the liquid. The amplitude of the vibrations created by the clapper must obviously be limited to about 0 . 5 - 0 . 7 of the height of the liquid column in the cone. It is set with the aid of a s c r e w adjustment connected with the interrupter. 5 m m from the bell clapper and the current is turned on. The vibrating vessel clapper strikes the repeatedly so that the liquid becomes mixed. Alternative mixing techniques are described in this book (see Chapter IV, Sects.

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