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Bulletin of the Korean Chemical Society (BKCS)

ISSN 0253-2964(Print)
ISSN 1229-5949(Online)
Volume 28, Number 10
BKCSDE 28(10)
October 20, 2007 

Determination of Si/Al Ratio of Faujasite-type Zeolite by Single-crystal X-ray Diffraction
Technique. Single-crystal Structures of Fully Tl+- and Partially K+-exchanged
Zeolites Y (FAU), |Tl71|[Si121Al
Sung Man Seo, Oh Seuk Lee, Hu Sik Kim, Dong Han Bae, Ik-Jo Chun, Woo Taik Lim*
Faujasite-type zeolite, Si/Al ratio, Crystal structure, Thallium, Potassium
Large colorless single crystals of faujasite-type zeolite with diameters up to 200 μm have been synthesized from gels with the composition of 3.58SiO2:2.08NaAlO2:7.59NaOH:455H2O:5.06TEA:1.23TCl. Two of these, colorless octahedron about 200 μm in cross-section have been treated with aqueous 0.1 M TlC2H3O2 and KNO3 in order to prepare Tl+- and K+-exchanged faujasite-type zeolites, respectively, and then determined the Si/Al ratio of the zeolite framework. The crystal structures of |Tl71|[Si121Al71O384]-FAU and |K53Na18|[Si121Al71O384]-FAU per unit cell, a = 24.9463(2) and 24.9211(16) A, respectively, dehydrated at 673 K and 1 × 10-6 Torr, have been determined by single-crystal X-ray diffraction techniques in the cubic space group Fd m at 294 K. The two single-crystal structures were refined using all intensities to the final error indices (using only the 905 and 429 reflections for which Fo > 4σ(Fo)) R1/R2 = 0.059/0.153 and 0.066/0.290, respectively. In the structure of fully Tl+-exchanged faujasite-type zeolite, 71 Tl+ ions per unit cell are located at four different crystallographic sites. Twenty-nine Tl+ ions fill site I' in the sodalite cavities on 3-fold axes opposite double 6-rings (Tl-O = 2.631(12) A and O-Tl-O = 93.8(4)o). Another 31 Tl+ ions fill site II opposite single 6-rings in the supercage (Tl-O = 2.782(12) A and O-Tl-O = 87.9(4)o). About 3 Tl+ ions are found at site III in the supercage (Tl-O = 2.91(6) and 3.44(3) A), and the remaining 8 occupy another site III (Tl-O = 2.49(5) and 3.06(3) A). In the structure of partially K+-exchanged faujasite-type zeolite, 53 K+ ions per unit cell are found at five different crystallographic sites and 18 Na+ ions per unit cell are found at two different crystallographic sites. The 4 K+ ions are located at site I, the center of the hexagonal prism (K-O = 2.796(8) A and O-K-O = 89.0(3)o). The 10 K+ ions are found at site I' in the sodalite cavity (K-O = 2.570(19) A and O-KO = 99.4(9)o). Twenty-two K+ ions are found at site II in the supercage (K-O = 2.711(9) A and O-K-O = 94.7(3)o). The 5 K+ ions are found at site III deep in the supercage (K-O = 2.90(5) and 3.36(3) A), and 12 K+ ions are found at another site III' (K-O = 2.55(3) and 2.968(18) A). Twelve Na+ ions also lie at site I' (Na-O = 2.292(10) and O-Na-O = 117.5(5)o). The 6 Na+ ions are found at site II in the supercage (Na-O = 2.390(17) A and O-Na-O = 113.1(11)o). The Si/Al ratio of synthetic faujasite-type zeolite is 1.70 determined by the occupations of cations, 71, in two single-crystal structures.
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