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  • Chemistry  (58)
  • Inorganic Chemistry  (7)
  • Magnetism
  • Wiley-Blackwell  (58)
  • 1990-1994  (58)
  • 1993  (23)
  • 1992  (35)
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Materialwissenschaft und Werkstofftechnik 24 (1993), S. 86-90 
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Ziel der Untersuchungen war die Analyse der Schichtwachstumsprozesse bei der plasmaunterstützten CVD-Abscheidung (PACVD) von Titannitridschichten auf Stählen im Niedertemperaturbereich ≤ 500°C.Im Vordergrund standen werkstoffkundliche Untersuchungen der verschiedenen Schichtwachstumsstadien, die sich als Funktion der Beschichtungsdauer ergeben. Die Herstellung der Schichten erfolgte in einer Puls-Plasma-CVD-Anlage. Um den gesamten Wachstumsprozeß vom Beginn der Abscheidung bis zum Wachstum geschlossener Schichten zu untersuchen, wurden die Proben bei konstanten Abscheidungsbedingungen jeweils unterschiedlich lange dem Reaktionsgasfluß ausgesetzt. Der Abbruch des Beschichtungsprozesses für die entsprechende Probe nach einer festgelegten Beschichtungszeit wurde durch die Verwendung eines Probenwechslers gewährleistet.Die Bildung der TiN-Schichten wurde an Proben aus dem Schnellarbeitsstahl S 6-5-2 (DIN 1.3343) im vergüteten Zustand untersucht. Es wurde festgestellt, daß bei diesem Substratwerkstoff zwei Oberflächenqualitäten mit unterschiedlich guten Anlagerungsbedingungen für, während der Vorbehandlung entstehende, adhäsive Verbindungen vorliegen. Die Bildung von Keimen und das Wachstum von Agglomeraten wird wesentlich durch diese Sorptionsschichten beeinflußt. Die Zahl der gebildeten Agglomerate ist bei Proben, die einer Vorbehandlung im Plasma ausgesetzt wurden, um den Faktor 10 größer als bei Proben, die während dieser Vorbehandlung abgedeckt waren. Es wurden neue Modellvorstellungen für die Entstehung und das Wachstum von Schichten entwickelt.
    Additional Material: 15 Ill.
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  • 2
    ISSN: 0935-6304
    Keywords: Coupled LC-GC-MS ; Aqueous sample ; s-Triazine Herbicides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Liquid chromatographic (LC) type trace enrichment is coupled online with capillary gas chromatography (GC) with mass spectrometric (MS) detection for the analysis of aqueous samples. A volume of 1-10 ml of an aqueous sample is preconcentrated on a trace-enrichment column packed with a polymeric stationary phase. After cleanup with HPLC-grade water the precolumn is dried with nitrogen and subsequently desorbed with ethyl acetate. A fraction of 60 μl is introduced on-line into a diphenyltetramethyldisilazane-deactivated retention gap under partially concurrent solvent evaporation conditions and using an early solvent vapor exit. The analytes are separated and detected by means of GC-MS. The potential of the LC-GC-MS system for monitoring organic pollutants in river and drinking water is studied. Target analysis is carried out with atrazine and simazine as model compounds; the detection limits achieved under full-scan and multiple ion detection conditions are 30 pg and 5 pg, respectively. Identification of unknown compounds (non-target analysis), is demonstrated using a river water sample spiked with 168 pollutants varying in polarity and volatility.
    Additional Material: 6 Ill.
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  • 3
    ISSN: 0935-6304
    Keywords: Capillary GC ; On-line extractive alkylation ; On-line acylation ; Carboxylic acids ; Amines ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Gas chromatographic procedures are described for the determination of carboxylic acids and chlorinated anilines in water samples.Propionic acid and 2,6-difluorobenzoic acid in aqueous solution have been simultaneously alkylated and extracted by means of a continuous two-phase reaction system, and then quantitated by on-line coupled capillary gas chromatography; tetrahexyl-ammonium hydrogen sulfate was used as phase transfer catalyst and pentafluorobenzyl bromide as reagent.A factorial design approach was used to optimize on-line derivatization of aqueous propionic acid with regard to pH and concentration of phase transfer catalyst. Alkylation and extraction, under optimized conditions, followed by quantitation of the pentafluorobenzyl ester by flame ionization detection furnished a linear calibration for concentrations between 0.1 and 10 μg/ml. The relative standard deviation was 9-15 %.The continuous two-phase reaction system was also used to determine (chlorinated) anilines present in water at concentrations of 0.1-1 μg/ml; pentafluorobenzoyl chloride was used as reagent and analysis was performed by capillary gas chromatography with flame ionization or electron capture detection. The on-line acylation of p-chloroaniline was optimized with regard to pH, reagent concentration, and reaction time.The on-line reaction system worked satisfactorily for both applications, although excess reagent caused some problems with the chromatography.
    Additional Material: 6 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 16 (1993), S. 459-463 
    ISSN: 0935-6304
    Keywords: LC-GC ; Aqueous samples ; Large volume injection ; PTV injector ; Solid-phase extraction ; Thermal desorption ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A system is described that allows the introduction of large volumes of water samples in capillary GC. Water elimination is carried out in the solvent split mode in a PTV injector with a packed liner. Two ways of separating water and analytes, i.e. evaporative and non-evaporative (solid-phase extraction), are compared. Sampling in the solid-phase extraction mode is favorable both in terms of recovery as well as with regard to sampling time. Quantitative recovery is obtained for priority pollutants ranging in volatility from dimethyl-phenol to phenanthrene. Losses occur for more volatile compounds, but even for these compounds the repeatability of the recoveries remains acceptable. With the system described here, water samples up to at least 1 ml of water can be directly analyzed. The detection limits are in the sub-ppb range.
    Additional Material: 4 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 785-790 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Derivatization ; (Chloro)alkyl chloroformates ; Non-aqueous reaction media ; Aqueous reaction media ; Fatty acids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fatty acids can be conveniently derivatized in less than one minute with (chloro)alkyl chloroformates such as methyl chloroformate, 2-chloroethyl chloroformate and 2,2,2-trichloroethyl chloroformate. 2,2,2-Trichloroethyl chloroformate is the most reactive reagent, and yields a reaction product which can be sensitively detected by GC ECD (detection limit 50 ng/ml, i.e. 25 pg/injection, for C8, C10, and C12 acids).In non-aqueous media 3-picoline, N-methylpiperidine, and dimethylaminopyridine show catalytic activity comparable with that of pyridine and can, therefore, replace it. N-methylpiperidine is the best basic catalyst in aqueous media (i.e. media containing up to 40 % water).
    Additional Material: 7 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 5 (1993), S. 303-315 
    ISSN: 1040-7685
    Keywords: capillary GC ; solid phase extraction ; membrane disks ; water samples ; automation ; nitrogen-phosphorus detection ; mass selective detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An automated procedure for the analysis of aqueous samples by membrane disk extraction coupled on-line to capillary gas chromatography (GC) is presented. Organophosphorus pesticides are preconcentrated from aqueous samples on three 0.5 mm thick, 4.0 mm diameter XAD-2 membrane extraction disks which are mounted in a polymer holder for use in a PROSPEKT sample processor. The layers are dried by a stream of nitrogen (30 min at ambient temperature). Desorption of the analytes is carried out with ethyl acetate which is directly introduced into a retention gap under partially concurrent solvent evaporation conditions, using an early solvent vapor exit. The method is a fully software-controlled automated system, and includes sample preparation, sample transfer and GC analysis. The final analysis is carried out by GC with nitrogen-phosphorus (NPD) or mass-selective detection. The technique is applied to the determination of a series of organophosphorus pesticides in tap water and water from European rivers. With a sample volume of only 2.5 mL, the detection limits achieved with the NPD were 20-50 ng L-1 in tap water and 20-100 ng L-1 in river water.
    Additional Material: 9 Ill.
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  • 7
    ISSN: 1040-7685
    Keywords: micro-LC ; flame photometric detection ; thermionic detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Microcolumn liquid chromatography (micro-LC) with on-line flame photometric (FPD) or thermionic detection (TID) has been used for the determination of a series of organophosphoric and organophosphonic acids isolated from various sample matrices. Silica-based ion-exchange materials and polymer packings have been used as stationary phases. In order to improve the sensitivity (expressed in concentration units) of the technique, trace enrichment via a miniaturized precolumn (4 mm × 1 mm i.d.) and direct large-volume injections (1-10 μL) of aqueous samples have been studied. As an application, the verification of nonproduction of chemical warfare agents and their alleged use have been investigated by analyzing their hydrolysis products in spiked surface water and soil samples. The application of both the precolumn technique and large-volume injections permit the detection of organophosphorus acids in water and soil at the low ppm level.
    Additional Material: 8 Ill.
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  • 8
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A benzenesulphonic acid-type cation exchanger (pKa 〈 1) is used as trapping-column material in a phase-system switching for the on-line coupling of column liquid chromatography and thermospray mass spectrometry. Phase-system switching is used to remove non-volatile constituents from the mobile phase, so that eluents containing non-volatile buffers and ion-pairing agents can be used without contaminating the mass spectrometer. The total analytical system is optimized using four benzalkonium test compounds (quaternary ammonium compounds). The reversed-phase separation of the test compounds as well as the parameters involved in the sorption on and desorption from the trapping column are studied. Important parameters during sorption are the concentration of the phosphate buffer and the percentage of acetonitrile in the mobile phase. During desorption of the test compounds from the ion-exchanger the percentage of acetonitrile in the desorption eluent and the pH are the most important factors. As an example, the analysis of domiphen in nasal drops is shown.
    Additional Material: 10 Ill.
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  • 9
    ISSN: 1040-7685
    Keywords: solid phase extraction ; thermal desorption ; on-line ; aqueous samples ; gas chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A module for combined solid-phase extraction and thermal desorption (SPETD) was incorporated into a system for automated GC analysis. Solid-phase extraction of analytes from water could be carried out after injection of an aqueous sample of 100 μL either by a loop using the carrier gas for sample introduction or manually with a syringe. After drying of the stationary phase by the carrier gas at a high flow rate, thermal desorption could be carried out at temperatures up to 300-350°C. Suitable packing materials for the liner in the SPETD module, i.e., materials which efficiently trap the organic compounds from an aqueous solution and are sufficiently thermostable, include Tenax and carbon-based phases, as well as a silylated alkylmodified silica. With the latter, however, the problem of efficient drying after sorption still must be solved. Each phase has its own application range which, from among the analytes which are trapped during sorption, is determined at the volatile end by losses occurring during drying by helium purging, and at the nonvolatile end by losses due to incomplete release during thermal desorption. From this study (using n-alkanes, chlorobenzenes, and chlorophenols as test solutes), it appears that the Tenax phases, Tenax-TA and Tenax-GR, have the widest application range; essentially quantitative recoveries were obtained for C10 through C26 n-alkanes. The carbon-based phases appear to be useful for relatively volatile compounds, i.e., up to C19 n-alkanes. Each phase gave good recoveries for two test mixtures containing chlorobenzenes and chlorophenols dissolved in 100 μL of water at the 10 ppb level.
    Additional Material: 4 Ill.
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  • 10
    ISSN: 1040-7685
    Keywords: micro-LC ; large-volume injections ; flame photometric detection ; organo-phosphates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The sensitivity and separation performance of microcolumn liquid chromatography coupled with a flame photometric detector were considerably improved by the direct injection of large sample volumes (approximately 10 μL) and by peak compression. Extremely narrow peaks can be obtained by adding displacers such as hydrochloric acid (ion-exchange mode) or n-butanol (reversed-phase mode) to the sample.The system was used for the determination of ethyl methylphosphonic acid, isopropyl methylphosphonic acid, and pinacolyl methylphosphonic acid which are the hydrolysis products of the super-lethal nerve agents VX, sarin, and soman, respectively, and of the final degradation product, methylphosphonic acid. The detection limits for the alkyl methylphosphonic acids and sarin in water were 1-20 ppb.Two examples were used to demonstrate the practicality of the present procedure. Sarin and the much more polar isopropyl methylphosphonic acid were simultaneously determined in a spiked surface water sample used for verification studies. Low-ppb levels of phosphorous acid were identified in mustard gas.
    Additional Material: 6 Ill.
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