Chapter 4 - Jacobs University

Chapter 9
Unpublished Results
9.1.4 Synthesis of K 12 Li 16 Co 2 (H 2 O) 6 [Co 4 (H 2 O) 16 P 8 W 48 O 184 ]·54H 2 O
(9a)
A sample of CoCl 2·6H 2 O (0.0785 g, 0.33 mmol) was dissolved in 1M LiCH 3 COO buffer solution
(20 mL) at pH 5.3 then K 28 Li 5 [H 7 P 8 W 48 O 184 ]·92H 2 O (0.187 g, 0.0125 mmol) was added. The
solution was heated to 80 °C for 1h and filtered hot. The filtrate was allowed to evaporate in an
open beaker at room temperature. After 2-3days a red-pink crystalline product started to appear.
After that, the evaporation was allowed to continue until the solution level approached the solid
product which was then collected by filtration and air dried. Yield: 0.13g (73.86 %). IR :
1136(s), 1083(s), 1017(m), 931(sh), 911(sh), 793(s), 676(s), 525(w), 462 (w) cm -1 .
75
70
65
60
%Transmittance
55
50
45
40
35
30
25
1200
1100
1000
900
800
Wavenumbers (cm-1)
700
600
500
Figure 9.9 FT-IR spectrum of 9a.
150