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By Garth Gilmour

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A solution of hexamethonium hydroxide [ (ΜββΝΟ^Η-^ΝΜββ) (0H) ] was prepared from the bromide s a l t (ex Sigma) and Ag20. Quantitative chemical trapping of the s i l i c a t e i n solution was performed by the t r i m e t h y l s i l y l a t i o n method by using an i n t e r n a l standard as described e a r l i e r (4,11). The results thus obtained were reproducible to within 20% r e l a t i v e . Si-NMR spectra were recorded on a Bruker WM-250 ( l i q u i d ) or a Bruker CXP-300 Fourier transform magic-angle-spinning (FT MAS) s o l i d state spectrometer.

Elevated temperatures were used (70-90 °C) to p a r t i a l l y depolymerize the D4R species to smaller fragments, from which i t would be possible to observe any exchange. Moreover, the rate of exchange would then be expected to be closer to that p r e v a i l i n g under synthesis conditions. In Figures 3 and 4 the main results are shown. Figure 3a shows the Si-NMR spectrum, including the precise composition and the assignments of the various peaks, of a s i l i c a t e solution of the organic base hexamethonium hydroxide at 70 °C.

Synthesis times are indicated i n Table I. Samples 10-17 were prepared i n s t i r r e d , Teflon-lined auto­ claves at 190 °C s t a r t i n g from a homogenized mixture of molar composition: 40 S i 0 (ex Ketjen s o l 40 AS), 1 A l 0 (ex NaA10 ; ex ICN, dried at 120 °C), 5 Na 0, 1000 H 0, and X, with X and the synthesis times indicated i n Table I I . ; ACS Symposium Series; American Chemical Society: Washington, DC, 1989. 2 KEUSPER AND POST Figure 1. Precursors in Zeolite Synthesis Formation of ZSM-5, including possible 'missing Τ s i t e s ' defects (·), s t a r t i n g from D5R s i l i c a t e s only.

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An Iron Age II Pictorial Inscription from Jerusalem Illustrating Yahweh and Asherah by Garth Gilmour


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