PubMed Health⌕ Search

Biomedical subjects

P Surmann

Publications and source records attributed to P Surmann.

10 recordsLinked to original sources
PubMed2000

Surface characterization of polydimethylsiloxane treated pharmaceutical glass containers by X-ray-excited photo- and Auger electron spectroscopy.

The siliconization of pharmaceutical glass containers is an industrially frequently applied procedure. It is done by spreading an aqueous silicone oil emulsion film on the inner surface and successive heat curing treatment at temperatures above 300 degrees C for 10-30 min. It was often proposed that a covalent bonding of PDMS to the glass or branching of the linear PDMS occurs during heat treatment. The present study was performed for a detailed investigation of the glass and silicone (polydimethylsiloxane = PDMS) chemical state before and after heat-curing treatment and analysis of the bond nature. Combined X-ray excited photoelectron (XPS) and Auger electron spectroscopy as well as angle resolved XPS-measurements were used for analysis of the glass samples. The silicon surface atoms of the borosilicate container glass were transformed to a quartz-like compound whereas the former linear PDMS had a branched, two-dimensional structure after the heat curing treatment. It was concluded that the branching indicates the formation of new siloxane bonds to the glass surface via hydroxyl groups. Further evidence for the presence of bonded PDMS at the glass surface can be found in the valence band spectra of the siliconized and untreated samples. However, this bond could not be detected directly due to its very similar nature to the siloxane bonds of the glass matrix and the organosilicon backbone of PDMS. Due to the high variation of data from the siliconized samples it was concluded, that the silicone film is not homogeneous. Previously raised theories of reactions during heat-curing glass siliconization are supported by the XPS data of this investigation. Yet, the postulation of fixing or baking the silicone on the glass surface is only partially true since the bonded layer is very thin and most of the silicone originally on the surface after heat curing can be removed by suitable solvents. This fraction can therefore still interact with drug products being in contact to the siliconized container wall.

Carbon↗
PubMed1999

Differential pulse polarography and electron spin resonance spectroscopy of nitroxyl free radicals used as ESR-spin probes.

Differential pulse polarography (DPP) and electron spin resonance (ESR) were used to study the influence of substituents and of the pH of the medium on DPP peak potentials (electrochemical reduction) resp. kreduction (chemical reduction) of nitroxyl free radicals. The DPP peak potentials can be used to select the appropriate nitroxide spin label for relevant biochemical and biophysical applications.

Algorithms↗
PubMed1996

Simulation of titration curves indicated with two indicator electrodes (biamperometry).

A rigorous method to simulate titration curves with indication using two indicator electrodes (biamperometry) is presented. Computer simulations can be carried out for reversible as well as for irreversible systems. The different parameters like the area of the individual electrodes, applied potential difference, heterogeneous rate constant, and the kinetic parameter alpha were varied and investigated as to their influence upon the shape of the titration curves. The theoretically derived effects match with the effects obtained by experiment. Considering the effects described here, it is possible to tailor the shape of the titration curve by the experimental conditions for specific applications in order to get an optimum shape at the end point of the titration.

Journal Article↗
PubMed1996

Bivoltametric titrations using electrodes with innovative geometry.

Electrodes with different surface areas were investigated for the determination of reversible, quasireversible, irreversible or electroinactive substrates. Two kinds of electrodes were constructed, a helical electrode with a given asymmetry and a platinum array electrode with a variable area. These electrodes were applied for the cerimetry of ammonium iron(II) sulfate and for the bromatometry of various organic substances. The theoretically derived effects on the shape of the voltametric titration curve are verified experimentally. It is possible to sharpen one side of the peak and to broaden the other side, depending on the system and the side of the peak one is interested in. It is possible to improve the bivoltametric determination of hydroquinone, benzocaine and sulfaguanidine by bromatometry by the directed employment of electrodes of different areas. For the bromatometric determination of electrochemically irreversible substrates the use of the electrode geometries proposed is a way to obtain a sharp bend and a steep decrease of titration curves with low values of the constant current which is a basic requirement for the accuracy.

Journal Article↗
PubMedDate not supplied

The fate of silicone oil during heat-curing glass siliconization--changes in molecular parameters analyzed by size exclusion and high temperature gas chromatography.

The siliconization of pharmaceutical glass containers, usually for parenteral formulations, is performed in a so-called heat-curing process using diluted aqueous emulsions of medical grade silicone oils. To do this, the emulsion film is spread on the inner container surface, followed by an application of dry heat at temperatures above 300 degrees C. Water and surfactants are removed by degradation and vaporization, while the thermostable poly(dimethylsiloxane) (PDMS) is left on the surface. In the present study, heat-cured siliconized glass containers of two different types were solvent-extracted to obtain material of heat-treated PDMS. These samples were analyzed by size exclusion chromatography (SEC) and high-temperature gas chromatography (GC) with special respect to low molecular-weight siloxanes (LMWS). By comparison with the untreated starting materials, significant changes in the molecular weight distribution (MWD) of the silicone oil were revealed. Almost all of the LMWS present in untreated materials were not detectable in the heat-cured extract of a 100 cSt. Baysilone silicone oil. Small amounts of PDMS-molecules, with chain lengths of 25 up 45 siloxane units, were traceable. The examination of a second product of higher viscosity yielded unexpected results. The heat-treated extract contained none of the siloxanes that were detected in the starting material. Siloxanes of chain lengths of up to 45 units having molecular weights of over 3000 g/mol could not be found after the siliconization process. This led to the conclusion that not only vaporization effects must be responsible for their absence, but also that silicone suffers from a heat-induced degradation. The results of SEC and GC analysis were supported by each other. The whole molecular weight distribution and four distinct fractions were characterized by SEC, while the GC analysis was capable of a high-resolution view into the LMWS fraction below 3500 g/mol. In conclusion, the benefit of the heat treatment is that no LMWS, a source of toxicological concern, remain in the respective containers. On the other hand, an increase in molecular weight and viscosity of the silicone oil, and thus a possible change of the lubricating properties, is likely to happen through removal of LMWS. But these changes probably have no impact on the hydrophobic surface behavior of silicone-treated glass.

Chromatography, Gas↗