Page 425 - Copper and Bronze in Art: Corrosion, Colorants, Getty Museum Conservation, By David Scott
P. 425

and a fine white sediment  settled out at the bottom of the beaker. The blue crystals were sepa­
         rated from  the solution and formed into two small cakes that were allowed to air dry.  An efflo­
         rescence of neutral verdigris formed on the outside of the  cakes and was removed. It can  take
         as many as  14 days for the cakes to dry sufficiently. The cakes were then crushed, and the green-
         blue crystals were washed and dried. This synthesis  was not particularly successful  because the
         cakes were too small to produce  a discrete  surface  efflorescence.  A second  synthesis  was made
         by  dissolving 5.9  g of neutral verdigris in 65 ml  of water in  a 300  ml  Erlenmeyer flask. Then 1.91 g
         of freshly precipitated cupric hydroxide was stirred into the solution, and the flask was covered
                                                    °
         and maintained at a temperature  between  60 C and  63 C. The chemical changes were followed
                                            °
        by  observing the color changes of the salt. The sediment was agitated occasionally. The reaction
         took from  8 to 10 days to go to completion. The precipitate was washed  first with  a  3%  neutral
        verdigris solution and then with water and alcohol and dried at  30  °C.
            In  the  preparation  by  Rahn-Koltermann  and  coworkers  (i99i),  100 g of neutral  copper
         acetate monohydrate  (0.5  mol) was dissolved in  750  g of water. The solution was stirred vigor­
         ously and heated just until the boiling point was reached. After the solution cooled, 3 ml  of a  24%
         ammonia solution was  added  drop by drop until  a light green precipitate developed. This was
        filtered  and then dried for 2 days under phosphorus  pentoxide and a reduced pressure of  10 torr
         (1333.22  Pa).
                                                                  °
            The  filtrate  was next placed in a beaker under  ethylene glycol at 40 C. After 48-64  hours,
         a cloudy light blue precipitate appeared. The solution was decanted,  and the residue centrifuged
        for  10  minutes, washed with water, and centrifuged again until a stable pH of 6.5  was  reached.
        This  step had  to  be  done  rapidly; otherwise  the  layered product would  turn brown between
        solid and liquid phase after  15 minutes of standing. The products were dried in the usual way
        and produced  1.39  g of light blue product and  3.75  g of light green precipitate.


        RECIPE  11  VERDIGRIS COMPOUND D
        A  laboratory experiment  to replicate  Schweitzer  and Mühlethaler's  (i968)  method of making
        compound D, U ( C H 3 C O O ) 2 [ C U ( O H ) 2 ] 3 - 2 H 2 0 ,  is as follows: In a 31 beaker, 2000 ml of water
                   C
        was stirred while  127.7  g of neutral verdigris was added. The solution was then divided into two
        equal portions. To one portion, concentrated  NH 3  solution was added drop by drop while stir­
        ring. After  about  13 ml of the  N H 3 had been added,  a sediment formed that, when about  30 ml
        of  the  N H 3 solution had been added,  was highly viscous; further  additions dissolved it again.
        When  about  80 ml of the  N H 3 had been added,  everything was in solution again. While  this
        solution was vigorously stirred, the second portion of neutral verdigris was added. This homog­
        enized  the precipitating gel-like sediment. The mixture was  left  to stand,  and  after  about 4 to
        5 days,  beautiful deep green  crystals  formed  at the bottom of the  beaker. The  solution above
        them was clear. The crystals were washed with water and alcohol.





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