Page 105 - Vogel's TEXTBOOK OF QUANTITATIVE CHEMICAL ANALYSIS
P. 105

surface caused  by  rubbing,  and (c) by  its temperature  being different from
         that of the balance case. These errors may be  largely eliminated by  wiping
         the vessel gently with a linen cloth, and allowing it to stand at least 30 minutes
         in proximity  to the balance before weighing. The electrification,  which may
         cause a comparatioely large error, particularly  if both the atmosphere and  the
         cloth are dry, is slowly dissipated on standing; it may be removed by subjecting
         the vessel to the discharge from an antistatic gun. Hygroscopic, efflorescent,
         and  volatile  substances  must  be  weighed  in  completely  closed  vessels.
         Substances which  have  been  heated  in an air oven or ignited  in a crucible
         are generally  allowed  to cool  in  a  desiccator  containing  a  suitable  drying
         agent. The time of  cooling in a desiccator cannot be exactly specified, since
         it will depend upon the temperature and upon the size of the crucible as well
         as  upon  the  material  of  which  it  is  composed.  Platinum  vessels  require  a
         shorter time than those of  porcelain, glass, or silica. It has been customary
         to leave platinum crucibles in the desiccator for 20-25  minutes, and crucibles
         of other materials for 30-35  minutes before being weighed. It is advisable to
         cover crucibles and  other open vessels.
       2.  When a substance is immersed in a fluid, its true weight is diminished by the
         weight of the fluid which it displaces. If  the object and the weights have the
         same density, and consequently the same volume, no error will be introduced
         on this account. If, however, as is usually  the case, the density of  the object
         is different from  that  of  the weights, the volumes  of  air displaced  by  each
         will be different. If  the substance has a lower density  than the weights, as is
         usual in analysis, the former  will displace a greater volume of  air than the
         latter, and it will  therefore weigh less in air than in a vacuum. Conversely,
         if  a denser material (e.g. one of  the precious metals) is weighed, the weight
         in a vacuum will be less than the apparent weight in air.
            Consider the weighing of  1  litre of  water, first  in  oacuo, and then in air.
         It is assumed that the flask containing the water is tared by an exactly similar
         flask, that the temperature of  the air is 20 OC  and the barometric pressure is
         101 325 Pa (760 mm of mercury). The weight of 1 litre of water in oacuo under
         these conditions is 998.23 g. If  the water is weighed in air, it will  be  found
         that  998.23 g  are too  heavy.  We  can  readily  calculate  the  difference. The
         weight  of  1  litre  of  air  displaced  by  the  water  is  1.20g. Assuming  the
         weights to have a density of 8.0, they will displace 998.2318.0 = 124.8 mL, or
         124.8 x  1.20/1000 = 0.15 g of  air. The net difference in weight will therefore
         be  1.20 - 0.15 = 1.05 g. Hence the weight in air of  1 litre of water under the
         experimental  conditions named  is  998.23 - 1.05 = 997.18 g,  a  difference of
         0.1 per cent from the weight in  oacuo.
           Now  consider the case of  a solid, such as potassium  chloride, under  the
         above conditions. The density of potassium chloride is 1.99. If  2 g of the Salt
         are  weighed,  the  apparent  loss  in  weight  (= weight  of  air  displaced)  is
         2 x 0.0012/ 1.99 = 0.0012 g.  The  apparent loss  in  weight  for the  weights  is
         2 x 0.0012/8.0 = 0.000 30 g.  Hence  2 g  of  potassium  chloride  will  weigh
         0.0012 - 0.000 30 = 0.000 90 g  less  in  air  than  in  oacuo,  a  difference  of
         0.05 per cent.
            It must be pointed out that for most analytical purposes where it is desired
         to express the results in the form of  a percentage, the ratio of the weights in
         air, so far as solids are concerned, will give a result which is practically  the
         same as that which would be given by the weights in oacuo. Hence no buoyancy
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