The synthesis of pure silica ZSM-5 has been modified to produce highly crys
talline material in the protonated form, necessary for catalytic activity,
directly from a low water fluoride gel. Tetrahedrally co-ordinated divalent
species of nickel and copper have been synthesised as salts of large organ
ic cations and increasing mole fractions incorporated into the zeolite gels
. The products have been analysed and characterised using simultaneous ther
mogravimetric and derivative thermogravimetric analysis (TG-DTG). The therm
al decomposition under nitrogen of the metal associated cations, tetraethyl
ammonium (TEA(+)), occluded within the zeolite channels is indicative and c
haracteristic of the incorporation of heteroatoms into the zeolite framewor
k. Anomalous losses in the systems can be explained by Jahn-Teller distorti
ons. The mass losses increased with increased metal loading and were consis
tent with those reported in full water system, analysis also confirmed that
the material was hydrophobic and thermally stable.
Analysis by X-ray diffraction (XRD), scanning electron microscope (SEM), X-
ray fluorescence (XRF), Fourier transform infrared spectroscopy (FTIR) and
Atomic Absorption Spectroscopy (AAS) has confirmed the reliability of TG-DT
G as a diagnostic tool. The maximum levels of substitution achieved were (m
ass%) Ni 3.93 and Cu 4.38.