Chapter 4 - Jacobs University

Chapter 9
Unpublished Results
9.1.7 Synthesis of K 22 Li 14 [(VO 2 ) 4 (P 8 W 48 O 184 )]·22H 2 O (12a)
A sample of VOSO 4·5H 2 O (0.0348 g, 0.1375 mmol) was dissolved in 1M LiCH 3 COO buffer
solution (20 mL) at pH 5.30 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. Then the solution was layered
with 1M NH 4 Cl. The filtrate was allowed to evaporate in an open beaker at room temperature.
After 5-6 days a brown 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: 0.10g (15%). IR : 1141(s), 1090(s), 1021(m), 985(sh),
956(sh), 934(sh), 915(sh), 799(s), 697(s), 573(w), 526(sh), 465 (w) cm -1 .
70
65
60
55
50
45
%Transmittance
40
35
30
25
20
15
10
5
1200
1100
1000
900
800
Wavenumbers (cm-1)
700
600
500
Figure 9.18 FT-IR spectrum of 12a.
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