Page 221 - Vogel's TEXTBOOK OF QUANTITATIVE CHEMICAL ANALYSIS
P. 221

ACTION OF  ION EXCHANCE RESINS   7.2

         It should be noted  that large-size ions rnay  not be  absorbed by  a medium
       cross-linked  resin so that its effective capacity is seriously reduced. A resin with
       larger pores should be used for such ions.

       Changing the ionic form: some widely used resins.  It is frequently necessary to
       convert a resin completely from one ionic form to another. This should be done
       after regeneration, if  this is being practised to 'clean'  the resin (for example, if
       the  'standard'  grade  of  ion  exchanger  is  used).  An  excess  of  a  suitable  salt
       solution should be  run  through  a column  of  the  resin. Ready conversion will
       occur if  the ion to be introduced into the resin has a higher, or only a slightly
       lower, affinity than that actually on the resin. When replacing  an ion of lower
       charge number on the exchanger by one of higher charge number, the conversion
       is  assisted  by  using  a  dilute  solution of  replacing  salt  (preferably  as  low  as
       0.01 M), while to substitute a more highly charged ion in the exchanger by one
       of lower charge number, a comparatively concentrated solution should be used
       (say, a  1 M solution).
         Strongly acidic cation  exchangers are usually  supplied in  the  hydrogen  or
       sodium forms, and strongly basic anion exchangers in the chloride or hydroxide
       forms; the chloride form is preferred to the free base form, since the latter readily
       absorbs carbon  dioxide  from  the  atmosphere  and  becomes  partly  converted
       into the carbonate form. Weakly acidic cation exchangers are generally supplied
       in the hydrogen  form, while weakly basic anion exchange resins are available
       in the hydroxide or chloride forms.
         The resins are available in  'standard'  grade, in  a purer  'chromatographic'
       grade, and in some cases in a more highly purified 'analytical'  grade: 'standard'
       grade materials should be subjected to a preliminary 'cleaning' by a regeneration
       procedure (see Section 7.8).

       Strongly  acidic  cation exchangers  (polystyrene  sulphonic  acid  resins).  These
       resins (Duolite C225, Amberlite  120, etc.) are usually marketed in the sodium
       form* and to convert  them into the  hydrogen  form (which, it  rnay be noted,
       are also available commercially) the following procedure rnay be used.
         The cleaned standard grade resin (which rnay of course be replaced  by  one
       of  the purer grades) is treated with 2M or with  10 per cent hydrochloric acid;
       one bed  volume of  the  acid  is  passed  through the column in  10-15  minutes.
       The effluent should  then  be  strongly  acid  to methyl orange indicator; if  it  is
       not, further acid must be used (about three bed volumes rnay be required). The
       excess of  acid  is drained  to almost  bed  level and  the  remaining acid  washed
       away  with  distilled  or de-ionised  water,  the  volume  required  being  about  six
       times that of the bed. This operation occupies about 20 minutes: it is complete
       when  the  final  100mL of  effluent  reauires  less  than  1 mL  of  0.2M  sodium
       hydroxide to neutralise its acidity using methyl orange as indicator. The resin
       can now be employed for the exchange of its hydrogen ions for cations present
       in a given solution. Tests on the effluent show that its acidity, due to the exchange,
       rises to a maximum, which is maintained until  the capacity is exhausted when
       the acidity of  the treated  solution falls. Regeneration is then necessary  and is
       performed, after backwashing, with 2M hydrochloric acid as before.

       *The resin is supplied in moist condition, and should not be allowed to dry out; particulate fracture
       rnay occur after repeated drying and re-wetting.
   216   217   218   219   220   221   222   223   224   225   226