Filtering crucibles

Procedure for filtering through a filtering crucible. The trap is used to prevent water from a water aspirator from backwashing into the suction flask. 

Filter crucibles with a porous filter base are available in porcelain (porosity 4), in silica (porosities 1,2,3,4), and in alumina (coarse, medium and fine porosities) these have the advantage as compared with sintered crucibles, of being capable of being heated to much higher temperatures. Nevertheless, the heating must be gradual otherwise the crucible may crack at the join between porous base and glazed side. 

This operation is the separation of the precipitate from the mother liquor, the object being to get the precipitate and the filtering medium quantitatively free from the solution. The media employed for filtration are (1) filter paper (2) porous fritted plates of resistance glass, e.g. Pyrex (sintered-glass filtering crucibles), of silica (Vitreosil filtering crucibles), or of porcelain (porcelain filtering crucibles) see Section 3.24. 

Although precipitates which require ignition will usually be collected in porcelain or silica filtering crucibles, there may be some occasions where filter paper has been used, and it is therefore necessary to describe the method to be adopted in such cases. The exact technique will depend upon whether the precipitate may be safely ignited in contact with the filter paper or not. It must be remembered that some precipitates, such as barium sulphate, may be reduced or changed in contact with filter paper or its decomposition products. 

Pipette 25.0 mL of the bromide ion solution (0.01-0.02M) into a 400 mL beaker, add excess of dilute silver nitrate solution, filter off the precipitated silver bromide on a sintered glass filtering crucible, and wash it with cold water. Dissolve the precipitate in a warm solution prepared from 15 mL of concentrated ammonia solution, 15 mL of 1M ammonium chloride, and 0.3 g of potassium tetracyanonickelate. Dilute to 100-200 mL, add three drops of murexide indicator, and titrate with standard EDTA (0.01 M) (slowly near the end point) until the colour changes from yellow to violet. 

The precipitate may be filtered through paper or any variety of filtering crucible. 

The precipitate, collected in a sintered-glass (porosity No. 4) or porcelain filtering crucible, may be weighed more rapidly as follows. Wash the copper(I) thiocyanate five or six times with ethanol, followed by a similar treatment with small volumes of anhydrous diethyl ether, then suck the precipitate dry at the pump for 10 minutes, wipe the outside of the crucible with a clean linen cloth and leave it in a vacuum desiccator for 10 minutes. Weigh as CuSCN. 

Precipitate about 0.1 g potassium (present as potassium chloride in 50 mL water) with 40 mL of the sodium TPB solution added slowly and with constant stirring. Allow to stand for 30 minutes, filter through a sintered-glass filtering crucible, wash with distilled water, and dry for 1 hour at 120 °C. Shake 20-25 mg of the dry precipitate with 200 mL distilled water in a stoppered bottle at 5-minute intervals during 1 hour. Filter through a Whatman No. 40 filter paper, and use the filtrate as the wash liquid. 

B. Determination of tellurium Procedure. The solution should contain not more than 0.2 g tellurium in 50 mL of 3M hydrochloric acid (ca 25 per cent by volume of hydrochloric acid). Heat to boiling, add 15 mL of a freshly prepared, saturated solution of sulphur dioxide, then 10 mL of a 15 per cent aqueous solution of hydrazinium chloride, and finally 25 mL more of the saturated solution of sulphur dioxide. Boil until the precipitate settles in an easily filterable form this should require not more than 5 minutes. Allow to settle, filter through a weighed filtering crucible (sintered-glass, or porcelain), and immediately wash with hot water until free from chloride. Finally wash with ethanol (to remove all water and prevent oxidation), and dry to constant weight at 105 °C. Weigh as Te. 

C. Determination of mixtures of selenium and tellurium Procedure. Dissolve the mixed oxides (not exceeding 0.25 g of each) in 100 mL of concentrated hydrochloric acid, and add with constant stirring 50 mL cool concentrated hydrochloric acid which has been saturated with sulphur dioxide at the ordinary temperature. Allow the solution to stand until the red selenium has settled, filter through a weighed filtering crucible (sintered-glass or porcelain) and complete... 

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