Page 426 - Copper and Bronze in Art: Corrosion, Colorants, Getty Museum Conservation, By David Scott
P. 426

Using the method from Rahn-Koltermann and coworkers (i99i),  12 g of neutral copper ace­
            tate monohydrate was dissolved in 200 ml of water in a 500 ml beaker. Then 15.4 ml of a  16.6%
            solution of ammonia  was  added. An initial  precipitate formed and  redissolved  as  the  ammo­
            nia was  added. Next, 200 ml of a  6% neutral copper  acetate monohydrate  solution was  added,
            during which  time a gelatinous  precipitate  developed. The mixture was  allowed to stand  for
            48  hours  at  room  temperature.  Within  the  first  24 hours,  a blue  precipitate  developed  that
            turned green  over the remaining 24 hours. A gelatinous  layer appeared above this precipitate.
                                                        i
            The  contents  of the  beaker were  allowed to  stand  for s weeks.  The  green  material did not
            change,  but within  the  solution above  the  green  precipitate, a thin  layer of a blue substance
            developed. The precipitates were separated, washed with water, and dried. This yielded 9.17 g of
            a green material and 110.7 mg of a blue product.
               In  the  GCI Museum Research Laboratory, it was possible  to make  so many different basic
            copper acetates that another series of studies was undertaken, varying the conditions as follows:
            six flasks were made up containing 12 g of neutral copper acetate dissolved in 200 ml of distilled
            water. Six different concentrations and volumes of ammonium hydroxide were then added drop
            by drop to each flask. The volume per volume (v/v) hydroxide concentrations  were

               1.  15% v/v  NH 4 OH  using 15 ml solution
               2.  10% v/v  NH 4 OH  using 15 ml solution
               3.  20% v/v  NH 4 OH  using 15 ml solution
               4.  25% v/v  NH 4 OH  using 15 ml solution
               5.  30% v/v  NH 4 OH  using  15 ml solution
               6.  30% v/v  NH 4 OH  using 30 ml solution

               After  slowly mixing the solutions, the pH of the resultant mother liquor in each flask was,
            respectively,  (1) pH 5; (2) pH 6; (3) pH 8;  (4) pH 8.5;  (5) pH 9.5; and  (β) pH 10.
               The activity in each flask was  as  follows:

           Flask 1  Immediately after mixing, a light blue precipitate formed. This had turned light green
            24 hours  later. Eight days later, the solution had turned to a jelly and included some light blue
            needlelike  masses. Deep  green  crystals  of the  neutral  acetate formed  on  the  surface  of  the
            beaker. Two weeks later, the remianing bulk of the solution became gelatinous, and this gelati­
            nous mass was covered with light blue needle-shaped crystals. The pH was about 6. Three weeks
            later,  the  solution had  dried. The  upper  part  was  covered by neutral  copper  acetate, and  the
            lower region was  filled  with  light blue crystals that were partially covered with  a darker  blue
            deposit. The light blue and dark blue products were collected, washed,  and then dried over sil­
            ica gel under reduced pressure. X-ray diffraction  analysis of the blue materials showed very sim­
            ilar peaks to those found for compound Β by Schweitzer and Mühlethaler  (i968).






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