Determination of stainless steel constituents in plastics

Summary Instrumental neutron activation analysis (INAA), atomic absorption spectrometry (AAS), and X-ray fluorescence analysis (XRF) were tested for the determination of the abrasion effect in plastics processing equipment. As optimal solution measurement of Fe by XRF in cylindrical samples was found.     

Thin-layer chromatography combined with diode laser desorption/atmospheric pressure chemical ionization mass spectrometry

The desorption of an analyte by a continuous wave diode laser from a porous surface of a thin-layer plate covered with a graphite suspension is presented. The thermally desorbed analyte molecules are ionized in the gas phase by a corona discharge at atmospheric pressure. Therefore, both essential processes--the desorption and the ionization of analyte molecules, which are often performed in one step--are separated. The target preparation is easy and fast since no additional extraction process is required. The mass spectrometric background signal was mostly limited to the low mass range showing no interference with typical compounds of interest. In this study, the calmative and antihypertensive drug reserpine was chosen as model analyte, which is often used for specification of mass spectrometers. No fragmentation was observed because of efficient collisional cooling under atmospheric pressure. The influence of diode laser power and the composition of the graphite suspension were investigated, and a primary optimization was performed.     

Characterisation of humic substances using atmospheric pressure chemical ionisation and electrospray ionisation mass spectrometry combined with size-exclusion chromatography

Humic substances were analysed by atmospheric pressure chemical ionisation (APCI) and electrospray ionisation (ESI) mass spectrometry in positive and negative modes. Using APCI the average m/z range of humic substances was reduced 5-fold compared to ESI. High-resolution time-of-flight mass spectrometry revealed the formation of multiply charged molecules in the ESI mode. Moreover, it was possible to obtain daughter ion mass spectra of humic substances by nanospray tandem mass spectrometry. The size-exclusion chromatography elution profile of humic substances was highly influenced by the pH of the analyte solution. By contrast, the pH had no significant influence on the observed mass spectra of humic substances.     

Analysis of volatile organic compounds in human urine by headspace gas chromatography-mass spectrometry with a multipurpose sampler.

A multipurpose sampler (Gerstel MPS), designed for liquid large volume, gaseous and headspace samples was used for the GC-MS analysis of organic volatiles in human urine. Headspace sampling with a volume-, temperature- and speed-controlled gas-tight syringe was combined with a temperature-controlled cold injection system (CIS) for cold trapping, enrichment and focusing of analytes. Regular 2-ml GC vials filled with 1 ml acidified urine were used as headspace sampling vials. A 100-vial autosampler tray was equipped with an additional temperature and heating time controlled "preheating station" for five vials. Profiles of organic volatiles in human urine were determined and 34 components identified. Trimethylamine (TMA) and 4-heptanone as two metabolites of medical interest were quantified. Calibration curves and intra assay imprecision for 4-heptanone concentrations in the range of 40 to 800 ng/ml showed a correlation coefficient of r = 0.9980 and a relative standard deviation (RSD) between 3.0 and 3.4%. Calibration curves and intra-assay imprecision for TMA concentrations in the range of medical interest from 0.5 to 20 micrograms/ml showed a correlation coefficient of r = 0.9968 and a RSD between 4.1 and 6.8%. The high practicability of the multipurpose sampler for both gaseous and liquid samples together with the here shown good reproducibility and sensitivity make this single CIS-GC-MS system very attractive for routine clinical use in metabolic profiling of organic volatiles (headspace) and non-volatiles (liquid).     

On the use of Helmholtz resonators as sound attenuators

Summary In the present paper a nonlinear acoustic theory is proposed, to accurately describe the properties of a generalized type of Helmholtz resonators. The theory may be used as a layout tool to design sound attenuators for combustion facilities. The present investigation shows that, in addition to the nonlinear effects, the effects due to thermoacoustic boundary layers and the first frequency correction to the Helmholtz approximation should be taken into account, in order to predict the frequency-dependent attenuation properties of Helmholtz attenuators with the accuracy required by typical technical applications. A series of experiments is presented which is used to validate the theoretical predictions.

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Zusammenfassung In der vorliegenden Abhandlung wird eine nichtlineare akustische Theorie vorgeschlagen, mit der das Verhalten einer verallgemeinerten Art von Helmholtzresonatoren beschrieben werden kann. Die Theorie kann als Werkzeug zur Auslegung von Schalldämpfern für Verbrennungsanlagen benutzt werden. Die vorliegende Arbeit zeigt, dass neben den nichtlinearen Effekten auch die Einflüsse der thermoakustischen Grenzschichten und der ersten Frequenzkorrektur zur Helmholtzapproximation berücksichtigt werden müssen, damit die frequenzabhängigen Eigenschaften von Helmholtzdämpfern mit technisch ausreichender Genauigkeit beschrieben werden können. Mit einer Reihe von Experimenten werden die theoretischen Ergebnisse untermauert.

     

Determination of aromatic sulfonic acids in industrial waste water by ion-pair chromatography

A method for the identification and quantification of aromatic sulfonic acids in industrial waste water has been developed. The preparation of the samples comprises a clean-up step and an enrichment step, utilizing i) reversed-phase extraction and ii) ion-pair solid phase extraction. The aromatic sulfonic acids are separated by ion-pair chromatography with diode-array detection. An advantage of the developed ion-pair chromatographic method is the separation of linear alkylbenzenesulfonic acids (LAS), lignosulfonic acids and aromatic sulfonic acids in one chromatographic run. Also described is an optimized clean-up procedure for collected fractions of a preparative chromatographic run to identify monosulfonic acids with GC/MS after methylation. The detection limits for aromatic sulfonic acids in industrial waste waters are at the g/l level.     

Quantitative determination of chloride by means of flow injection analysis with spectrophotometric detection in the UV/VIS range

Chloride is determined indirectly by Spectrophotometric flow injection analysis. Two systems are compared, both based on the principle of ion exchange of easily detectable anions versus chloride from suitable mercury salts. The first method is based on the exchange of chloride with chloranilate which is detected at 332 nm or at 306 nm in neutral or in acidic medium respectively. In the second case, chloride reacts with Hg(SCN)₂. The liberated thiocyanate forms a strongly coloured complex with Fe(III) in acidic solution with an absorption maximum at 460 nm. Both methods have a detection limit of about 5 mol Cl^–/l (175 ng/ml). In the case of the thiocyanate method, the relative standard deviation is about 2% (7 measurements) in the range of 5 to 150 mol/l and decreases significantly to a value of approximately 0.2% at higher concentrations; for the chloranilate method it is 10% for lower and about 1% for higher concentrations respectively.     

An invariant trace formula for the universal covering group of SL(2,ℝ)

Automorphic forms of arbitrary real weight can be considered as functions on the universal covering group of SL(2, ). In this situation, we prove an invariant form of the Selberg trace formula for Hecke operators. For this purpose, the Fourier transforms of weightet orbital integrals, obtained by J. Arthur, R. Herb and P. Sally, jr., are explicitly calculated. Our formula does not follow from Arthur's invariant trace formula, since the group has infinite centre, and vector-valued automorphic forms with respect to non-congruence lattices are considered.