Chapter 4 - Jacobs University

Chapter 9
Unpublished Results
9.1.9 Synthesis of K 21 RbLi 12 [(UO 2 ) 3 WO(H 2 O)(P 8 W 48 O 186 )]·29H 2 O
(14a)
A sample of UO 2 (NO 3 ) 2·6H 2 O (0.0417 g, 0.0825 mmol) was dissolved in 1M LiCH 3 COO buffer
solution (20 mL) at pH 4.1 then K 16 Li 2 [H 6 P 4 W 24 O 94 ]·33H 2 O (0.182 g, 0.025 mmol) was added.
The solution was heated to 50 o C for 1h and filtered hot. The resulting solution was layered with
0.5 mL of 1 M KCl. The filtrate was allowed to evaporate in an open beaker at room
temperature. After 4-5 days a yellow 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: 0.07g (10%). IR : 1138(s), 1084(s),
1017(m), 951(sh), 928(sh), 909(sh), 864(w), 812(s), 684(s), 570(w), 478 (w) cm -1 .
60
58
56
54
52
50
48
46
%Transmittance
44
42
40
38
36
34
32
30
28
26
24
22
20
18
1200
1100
1000
900
800
Wavenumbers (cm-1)
700
600
500
Figure 9.22 FT-IR spectrum of 14a.
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