Aluminium phosphate adjuvants prepared by precipitation at constant pH. Part I: composition and structure.
Aluminium phosphate adjuvant was precipitated under constant pH conditions in an effort to characterize materials formed at defined precipitation conditions. A reaction vessel was designed to provide a continuous steady-state process. An aqueous solution containing aluminium chloride and sodium dihydrogen phosphate was pumped into the reaction vessel at a constant rate. A second pump infused a sodium hydroxide solution at the rate required to maintain the desired pH. Precipitations were performed between pH 3.0 and 7.5, at intervals of pH 0.5. The adjuvants were characterized using 27Al NMR, FTIR, Raman and X-ray diffraction methods along with elemental analysis. The results of this study indicate that a continuum of amorphous aluminium hydroxyphosphates were formed having properties that changed as a continuous function of the precipitation pH. The phosphate content decreased as the pH of precipitation increased. 27Al NMR spectra revealed that the majority of the aluminium was octahedrally coordinated, with a small percentage of tetrahedrally coordinated aluminium. The density of the adjuvants was directly related to the pH of precipitation. The most prominent feature of the IR and Raman spectra is the P-O stretching vibration of the structural PO(4) groups. The positions of these bands decreased linearly as the precipitation pH increased. The results of selective deuteration FTIR experiments are consistent with high surface area materials as most of the OH groups were exposed near the surface of the adjuvant.
Burrell
L S
LS
Department of Industrial and Physical Pharmacy, Purdue University, West Lafayette, IN 47907, USA.
Johnston
C T
CT
Schulze
D
D
Klein
J
J
White
J L
JL
Hem
S L
SL
D000276:Adjuvants, Immunologic / Q000737:chemistry*; D017607:Aluminum Compounds / Q000737:chemistry*; D011232:Chemical Precipitation; D006863:Hydrogen-Ion Concentration; D009682:Magnetic Resonance Spectroscopy; D010710:Phosphates / Q000737:chemistry*; D017550:Spectroscopy, Fourier Transform Infrared; D013059:Spectrum Analysis, Raman
D000276:Adjuvants, Immunologic; D017607:Aluminum Compounds; D010710:Phosphates; C012714:aluminum phosphate