Chapter 4 - Jacobs University

Chapter 9
Unpublished Results
9.1.5 Synthesis of K 9 Li 27 [Ni 4 (H 2 O) 16 (P 8 W 48 O 184 )(WO 4 ) 2 ]·44H 2 O(10a)
A sample of NiCl 2·6H 2 O (0.0784 g, 0.33 mmol) was dissolved in 0.5 M LiCH 3 COO buffer
solution (20 mL) at pH 4.0 then K 28 Li 5 [H 7 P 8 W 48 O 184 ]·92H 2 O (0.187 g, 0.0125 mmol) was added.
Then 6-10 drops of 30% H 2 O 2 was added to that solution. 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 2-3 days a green 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: 0.163g (79%). IR: 1139(s), 1088(s), 1020(m),
933(sh), 918(sh), 813(s), 685(s), 468 (sh) cm -1 .
50
45
40
%Transmittance
35
30
25
20
15
10
1200
1100
1000
900
800
Wavenumbers (cm-1)
700
600
500
Figure 9.12 FT-IR spectrum of 10a.
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