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2.2. General characterization, Papers A-F 15 Table 2.2: Type and molar composition of synthesis mixtures used for NaX and MFI film growth. Zeolite Type of type synthesis solution NaX gel clear solution ZSM-5 gel clear solution Molar composition of the synthesis solution 14Na2 O:Al2 O3 :10SiO2 :800 H2 O 80Na2 O:Al2 O3 :9SiO2 :5000H2 O 100SiO2 :Al2 O3 :30Na2 O:4000H2 O 12TPAOH:100SiO2:Al2O3:4Na2O:6400H2O:400EtOH 2.2 General characterization, Papers A-F The weight gain (gzeolite/gsample) was determined by measuring the weight of the support before and after hydrothermal treatment of rinsed and dried samples. A Philips XL30 scanning electron microscope (SEM) equipped with a LaB6 emission source was used for studies of surface morphology of the structured adsorbents and also to measure film thicknesses. The monoliths were cut in the channel direction prior to SEM investigation. Images were recorded on samples covered with a thin layer of gold (about 10 nm) deposited by sputtering. X-ray diffraction data (XRD) in the 2θ range 5-35◦ were recorded with a Siemens D5000 powder X-ray diffractometer (XRD) running in Bragg-Brentano geometry. Nitrogen adsorption/desorption isotherms at liquid nitrogen temperature were mea- sured with a Micromeritrics ASAP 2010 instrument after outgassing at 300 or 350 ◦C for 12 h or 24 h prior to analysis. The surface area was calculated from the adsorption isotherm using the Brunauer-Emmet-Teller (BET) equation. The surface area was used to calculate the zeolite loading (gzeolite/gsample) as the ratio between the surface area of the zeolite film sample and the surface area of a powder of zeolite crystals grown in the same synthesis mixture as that used for film growth. The pore size distribution was de- termined by the Barrett-Joyner-Halenda (BJH) method applied to the desorption branch of the isotherm. A Micromeritrics ASAP 2020 instrument was used to determine carbon dioxide or nitrogen adsorption/desorption isotherms at 0, 20 or 40◦ C for NaX samples. A water bath was used to control the temperature. Mercury Intrusion Porosimetry (MIP) data were recorded using a Micromeritics Au- topore 9220 V1.04 mercury porosimeter, operated between 0.1 and 3500 bar. The Si/Al and Na/Al ratios of the discrete ZSM-5 crystals was determined by induc- tively coupled plasma-atomic emission spectrometry (ICP-AES, Analytica AB, Sweden) by using an ARL-3560 spectrometer. The surface Si/Al and the Na/Al ratios of the ZSM-5 zeolite films were determined by X-ray photoelectron spectrometry (XPS) using a KRATOS Axis ultra electron spectrometer.PDF Image | Structured Zeolite Adsorbents for PSA Applications
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