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35
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19544376183
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note
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4. The total volume of the solution was made up to 100 mL, and nitrobenzene (2.46 g, 20 mmol) as an internal standard, was added. A sample of the resultant solution was then drawn out and analyzed by GLC using a Packard instrument Model 417, equipped with F.I.D. coupled to an SP4290 integrator. The glass column (6 ft, 1.5 mm) was packed with 10% SP2401 on Supelcoport 100/120. The operating conditions were: detector temp 250°C, injector temp 250°C, carrier gas argon, oven temp 70°C, ramp rate 5°C/min, final temp 220°C and sample size 0.2 μL. Products were identified by comparing retention times with those of authentic samples. Nitrobenzene was used as the internal standard. The compound were eluted in the following order: CB, nitrobenzene, p-BCB and o-BCB
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36
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19544390205
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note
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Preparation of cation-exchanged clays and zeolites: The sodium form of the clay or the zeolite (10 g), was suspended in an aqueous solution (100 mL, 1.0 M) of the metal salt. The mixture was stirred at 25°C for 24 h. The solid was separated by centrifugation and washed several times with deionized water. The resulting solid was dried overnight at 110°C and calcined at 400°C for 12 h
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38
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19544394302
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note
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2 (20 mmol) at 25°C. The mixture was stirred at this temperature for 24 h. Workup of the reaction mixture and GLC analysis were performed as described in note 35
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