Use of the Apparent Content Curves for the spectrophotometric identification of substances: identification of amphetamines

The possibility of identification of substances which have similar spectral behaviour by means of Apparent Content Curves has been studied. This study is carried out with absorption, excitation and emission spectra of several amphetamines of widespread pharmaceutical use. Results obtained show that amphetamine, phenylpropanolamine, pseudoephedrine, phenylephrine, epinephrine, dopamine and methoxyamphetamine can be identified with a probability of >95%.     

Determination of glycols by HPLC with refractive index detection

A simple and fast HPLC method for the determination of glycols is described. It is characterized by a reversed-phase separation using water as eluent and a refractive index detection. The method was applied to investigate the biodegradation of glycols in a laboratory activated sludge plant and to determine the content of glycols or alcohols in detergents. The detection limit is 4 mg/l ethylene glycol or propylene glycol in an aqueous sample.     

Raman spectroscopy of carbon fibres

Investigations of coated carbon fibres are reported using Raman spectroscopy. Relationships between different process parameters (for example precursor concentration, reactor temperature and various precursors) and the resulting types of carbon fibres are discussed.     

Comparison of four quantification methods for the determination of PCB in transformer oils

The analysis of PCB in transformer oils has been achieved with three HRGC/ECD based methods, proposed by the International Electrotechnical Commission (IEC/TC 10), by the Comité Européen de Normalisation (CEN/TC 19/WG 22) and by the Deutsches Institut für Normung (DIN 51 527). The same clean-up, described in the CEN/TC 19/WG 22, has been used for all the samples, allowing a comparison of the quantification procedure only. The total chlorine content has also been determined with X-ray fluorescence. These different methods of quantification are compared and their application for legislative purposes is discussed.Dedicated to Professor Dr Dieter Klockow on the occasion of his 60th birthday     

Preconcentration of trace antimony in tap and sea water on activated alumina. Determination by graphite furnace atomic absorption spectrometry

Summary A method is described for antimony preconcentration based on retention on a column of activated alumina. Recovery is 80% when no pH-control and 4 mol/l HCl as eluent are used. The preconcentration factor is 400. The method was applied to the determination of antimony in spiked tap and sea water. The analytical performance of the method is discussed.     

TEM investigations on PECVD-titanium carbide layers

TiC_x-PECVD-layers were characterized by TEM. EDX analysis and electron diffraction. TiC_x-layers deposited using benzene showed a columnar structure, at which the column size decreases with rising excess carbon content. TiC_x-layers deposited using n-heptane presented a lamellar structure, at which the lamellar thickness diminishes with an increasing excess carbon content. In dependence on the layer thickness a periodic progress of the element contents was observed, at which a maximum for Ti and Cl correlates with a minimum for C. It was found that the incorporated chlorine is bonded to titanium. The lattice parameter depends on the chlorine content. Using TiCl₄/H₂/Ar-gas mixtures without any hydrocarbon, layers containing TiH₂ are formed.     

Chemometric approaches in environmental problems concerning PCDD and PCDF. Data interpretation and source correlation. Mechanisms of formation and destruction in MSW combustion process

Summary The role of multivariate analysis methods in evaluating, rationalizing, and working out complex environmental problems is discussed. The discussion is organized in two sections; a literature analysis of the application of chemometric methods to PCDD/PCDF data interpretation and source correlation and a review of the role of chemometric methods in analysing the results obtained by the Authors studying PCDD/PCDF formation and destruction mechanisms in MSW combustion processes.     

Photochemistry of dibenzo-1,4-dioxins: intramolecular rearrangement-reduction through observable 2,2′-biphenylquinones

The photochemistry of dibenzo-1,4-dioxin (7) and 2,3,7,8-tetramethyldibenzo-1,4-dioxin (15) — both of which have the parent ring system of the well-known enrimental contaminant dioxin— has been studied in aqueous solution and in selected organic solvents. It is shown that a novel intramolecular photorearrangement is the major mode of reaction for 7 and the exclusive reaction for 15, giving rise to observable (by UV—Vis spectrophotometry) intermediate 2,2′-biphenylquinones. Subsequent reduction by the organic co-solvent gives rise to 2,2′-biphenols as major or exclusive product. Thus, photolysis of these compounds generates oxidizing agents in the biphenylquinones. Photolysis in the presence of added N_aBH₄ resulted is greatly enhanced yields of biphenols along with more than 90% material balance. These findings have relevance to dioxin photodecomposition, which can be used as a method for its destruction.     

Solvatochromic shifts of naphthalene and pyrene excimers

Solvatochromic shifts of pyrene (Py) and naphthalene (Np) excimers were obtained in polar and non-polar solvents. The observed shifts for both excimers are explained by changes in the polarizability between the excimer and the dissociative ground state. The magnitudes of the shifts in the pyrene excimer are larger, indicating that the pyrene excimer is more polarizable than the naphthalene excimer.     

Fourier transform IR product study of the reaction of CFO radicals with O2 at 298 K

Experimental results are presented of a Fourier transform IR product study at 298 K of the reaction system CFO+O₂ at oxygen pressures between 3 and 250 mbar. Pulsed photolysis of oxalyl fluoride (CFO)₂ or formyl fluoride (CHFO) at 193 nm was used to produce CFO. As stable products we detected bis-fluoroformyl peroxide, carbonyl fluoride and carbon dioxide. The yields of the peroxide and of CF₂O were measured as a function of [O₂]/[precursor] and are discussed qualitatively.