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Determination of pentachlorphenol (PCP) in waste wood - method comparison by a collaborative trial
(2002)
Two independently developed and validated procedures for the determination of pentachlorophenol (PCP) in waste wood were compared by means of a collaborative trial. Both methods foresee quantification of PCP by gas chromatography (GC-ECD) after acetylation and differ with regard to the use of methanol or toluene/sulphuric acid, respectively, as solvent in the sonication extraction step. Test samples with established analyte homogeneity were prepared from a ground real life starting material. A total of 23 participating laboratories with experience in wood preservative analysis were instructed to apply both methods to three levels of content in the range of 0.520 mg PCP/kg. In case of the toluene/sulphuric acid extraction, lower recoveries and higher interlaboratory dispersion of results at the higher PCP contents were observed. Seen against the background of the Horwitz equation a reproducibility standard deviation of not, vert, similar19% for the methanol extraction at the 4.5 mg/kg level meets the requirement for a sound analytical method. Thus, the sonication extraction procedure with methanol has been annexed as a reference method to the German waste wood regulation.
Due to the utilisation of 1,1,2-trichlorotrifluoroethane (CFE) as extraction solvent the IR-spectrometric determination of total petrol hydrocarbon (TPH) in soil according to ISO/TR 11046 has been replaced by gas chromatography/flame ionisation detection (GC/FID) after extraction with a halogen-free solvent according to ISO/DIS 16703:2001. The results obtained with both methods by field laboratories in three proficiency testing (PT) rounds are compared. The consensus means obtained with GC/FID are typically 10%-20% (ranging between 0% and 25%) higher than those found with IR-spectroscopy. On the contrary, coefficients of variation (CV) are roughly double in case of GC/FID and are briefly discussed against the background of the Horwitz equation.
Für Korrosionsprüfungen stehen eine ganze Reihe bewährter und standardisierter Verfahren zur Verfügung, die eine weite Verbreitung gefunden haben. Dazu gehören die Sprühnebelverfahren, Klimaprüfverfahren, Auslagerungsversuche in spezifisch wirkenden Prüfmedien und die elektrochemische Polarisationsmesstechnik. Dennoch bleiben eine ganze Reihe von Fragen und Wünschen offen. Insbesondere die Anfangsprozesse der Korrosion lassen sich häufig nur unzureichend untersuchen. Auch über den zeitlichen Verlauf der Korrosion geben die eingesetzten Verfahren keine ausreichenden Informationen. Weiterhin führt der Wunsch nach möglichst praxisnahen Prüfbedingungen bei vertretbarem Aufwand und die Suche nach Möglichkeiten zur Verkürzung von Prüfzeiten zur ständigen Weiterentwicklung der Prüf- und Untersuchungsmethoden.
In der Korrosionsforschung steht mit der Rauschdiagnostik bei der Untersuchung von Korrosionsprozessen ein einfaches, empfindliches und nahezu zerstörungsfreies Messverfahren zur Beurteilung der Korrosionsneigung metallischer Werkstoffe zur Verfügung. Mit dem heutigen Kenntnisstand über das elektrochemische Rauschen bei Korrosionsprozessen können die Einsatzmöglichkeiten sowohl auf die Lösung von Messaufgaben im Labor, als auch auf spezielle Probleme bei der Korrosionsüberwachung in der Praxis erweitert werden. Des Weiteren findet diese Methode auf Grund ihrer spezifischen Vorteile auch immer mehr Anwendung zur Unterstützung bzw. Verbesserung herkömmlicher Korrosionsprüfungen. Der Zugewinn wichtiger Erkenntnisse, die Verkürzung von Prüfzeiten sowie die damit verbundene Schonung von Ressourcen (Arbeitskraft, Energieaufwand, chemische Hilfsmittel etc.) sind einige der Vorteile, die eine moderne Korrosionsprüfung heute kennzeichnen.
Translated Abstract
Electrochemical noise measurements - Innovation in corrosion testing
There are a lot of approved and standardized methods available for corrosion testing which have found wide application. Salt-spray testing, electrochemical polarization techniques and exposure tests in specific test media belong to these. Nevertheless, some questions remain unanswered and requirements unsatisfied. In particular, both the start of corrosion and the way it proceeds with time can often be examined only to an insufficient extent. Furthermore, the requirements of practical test conditions, acceptable effort and expenditure and shorter test durations lead to continuous development of these test methods.
Within corrosion research, the analysis of electrochemical noise offers a simple, sensitive and virtually non-destructive measuring technique for assessment of the corrosion susceptibility of metallic materials and for the investigation of corrosion processes. The present status of knowledge concerning noise diagnostics in corrosion processes permits the application of this method not only to experimental tasks in the laboratory, but also to special problems in the context of practical corrosion monitoring. Furthermore, specific advantages of the technique enable its use to an increasing extent in supporting or improving conventional corrosion testing. The advantages here include obtaining additional information and shortening testing times (together with associated savings in resources such as manpower, energy, chemical reagents, etc.), thus resulting in state-of-the art corrosion testing.
Poly(methyl methacrylate) (PMMA) surfaces have been modified by dynamic plowing lithography. The resulting modified structures, presenting regions of different densities and stiffnesses, have been studied by forcedisplacement curves. The elasto-plastic response, the stiffness, and the adhesion of the modified samples have been characterized. Forcedisplacement curves are able to distinguish between unmodified PMMA and two different structures resulting from the lithography, i.e. compressed PMMA and low density PMMA. In particular, the low density regions are made up of cluster-like globular particles, whose elasto-plastic response and adhesion are measured and whose contribution to the total elasto-plastic response and to the adhesion has been studied in detail.
The adhesion of poly(methyl methacrylate) (PMMA) and polystyrene (PS) films, whose surface has been previously structured by dynamic plowing lithography (DPL), has been measured by means of forcedisplacement curves. The different adhesion of modified and unmodified PS leads to the assumption that polymer chains are broken during DPL. After measuring the energy dissipated by the tip during DPL, in order to check that the transferred energy is sufficient to break covalent bonds, the polymer chain scission caused by the lithographic process has been definitely confirmed by size exclusion chromatography measurements of the lithographed films.