A SAXS study of the nanostructural characteristics of TEOS-derived sonogels upon heat treatment up to 1100 °C

Xerogels obtained from the acid-catalyzed and ultrasound stimulated hydrolysis of TEOS were submitted to heat treatment at temperatures ranging from 60 to 1100 °C and studied by small-angle X-ray scattering (SAXS). The SAXS intensity as a function of the modulus of the scattering vector q was obtained in the range from q₀=0.19 to q_m=4.4 nm⁻¹. At 60 °C the xerogels exhibit an apparent surface fractal structure with a fractal dimension D_S∼2.5 in a length scale ranging from 1/q₁∼1 to 1/q_m∼0.22 nm. This structure becomes extremely rough at 120 °C (D_S∼3) and at 150 °C, it apparently converts to a mass fractal with a fractal dimension D∼2.4. This may mean an emptying of the pores with preservation of a share of the original mass fractal structure of the wet aged gel, for it had presented a mass fractal dimension D∼2.2. A well characterized porous structure formed by 2.0 nm mean size pores with smooth surface of about 380 m²/g is formed at 300 °C and remains stable until approximately 800 °C. At 900 °C the SAXS intensity vanishes indicating the disappearance of the pores in the probed length scale. The elimination of the nanopores occurs by a mechanism in which the number of pores diminishes keeping constant their mean size. The xerogels exhibit a foaming phenomenon above 900 °C and scatter following Porod's law as does a surface formed by a coarse structure.     

Liquid chromatographic analysis of prednisolone, prednisone and their 20-reduced metabolites in perfusion media

A reversed-phase liquid chromatographic assay was developed to quantitate prednisolone, prednisone and the 20 alpha-dihydro and 20 beta-dihydro reduced metabolites of both parent compounds in tissue culture media from in vitro perfusions of the human placental lobule. Steroids were extracted from perfusate, using reversed-phase cartridges, with average recoveries of 95.2% or greater. The internal standard for the analyses was 6 alpha-methylprednisolone. In this assay cortisol coelutes with prednisolone, however, no other significant interferences were found. Assay of each steroid was linear in the range 0-1 microgram/ml. Intra-assay coefficients of variation were measured at 10 and 750 ng/ml with ranges of 3.4% (20 alpha-dihydroprednisone) to 8.8% (20 beta-dihydroprednisolone) and 4.1% (20 beta-dihydroprednisone) to 8.8% (prednisone). The corresponding inter-assay coefficients of variation were 3.3% (20 alpha-dihydroprednisone) to 9.1% (20 beta-dihydroprednisolone) and 1.9% (prednisolone) to 3.5% (prednisone). The analyses utilized two C18 columns which were linked together and maintained at 40 degrees C.     

Thin-layer chromatography of radioactively labelled cholesterol and precursors from biological material

Summary The investigation methods of the action of xenobiotics on sterol biosynthesis from ¹⁴C-acetate in rat hepatocyte cultures can be developed, with regard to extraction using Extrelut and the separation of the sterol pattern by thin-layer chromatography, in such a way that they are suitable for wider application, e.g., screening. Good visualisation and recognition of changes in the sterol pattern are possible using autoradiography of the thin-layer chromatogram.

---

Dünnschicht-Chromatographie von radioaktiv markiertem Cholesterin und Vorstufen aus biologischem Material. Eine einfache und empfindliche Methode zur Untersuchung einer Beeinflussung des Sterolbiosynthesewegs

---

Dedicated to Dr. E. Roesch on occasion of his 65th birthday     

N2O emission in the 4.5 μM region: high excitation of the bending mode transitions v1v2v3→v1v2(v3−1) with (2v1+v2)=5

Eight emission spectra of pure N₂O and N₂O + N₂ + He mixtures excited by a radio frequency discharge were recorded by Fourier Transform Spectroscopy at a resolution of 0.005 and 0.004 cm⁻¹ in the 4.5 μm region. Results (wavenumbers, band centers, and spectroscopic constants) concerning nine new vibrational transitions which have not been observed before, and which occur between highly excited levels of the bending mode are reported. The derived spectroscopic parameters allow us to reproduce the experimental wavenumbers with an RMS error lower than 4.5 × 10⁻⁴ cm⁻¹.     

Magnetic structure of the interface between ferromagnet and antiferromagnet with parallel anisotropy axes

The structure of a spin spiral arising in the vicinity of the interface between a ferromagnet and a compensated antiferromagnet is studied in the case where the anisotropy axes of the layers are parallel to each other, and the evolution of this spiral in an external magnetic field is investigated.     

Thermochemistry of potassium morpholinodithiocarbamate

Results of thermochemical studies of a new compound, potassium morpholinodithiocarbamate, are presented. The enthalpies of its solution in water at various dilutions and the specific heat at 173–348 K were examined by the experimental methods of isothermal and dynamic calorimetry.     

The preparation and structure of 1,4,5,6,7,7-hexachloro-2-endo-ferrocenylhydroxymethyl-3-endo-hydroxymethyl-5-norbornene

The crystal structure of a novel ferrocene derivative with potential flame-retardant/smoke-suppressant activity, 1,4,5,6,7,7-hexachloro-2-endo-ferrocenyl-hydroxymethyl-3-endo-hydroxymethyl-5-norbornene, has been determined. Some of the carbon–carbon bonds within the chlorendic residue are unusually long, and there is no interaction between the hydroxyl groups and the iron atom. There is evidence of intramolecular hydrogen bonding between the two hydroxyl groups.