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  • 1
    ISSN: 1520-5851
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology , Energy, Environment Protection, Nuclear Power Engineering
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1436-5073
    Keywords: organotin ; alkylation ; environmental ; fentin ; fenbutatinoxide
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A method for the preparation and purification of pentylated derivatives is described for nine organotin compounds that are relevant in environmental analysis (tributyltin acetate, dibutyltin dichloride, butyltin trichloride, triphenyltin chloride, diphenyltin dichloride, phenyltin trichloride, tricyclohexyltin hydroxide (cyhexatin), dicyclohexyltin dibromide and bis (trineophyltin) oxide (fenbutatinoxide)). The compounds are synthesized on a 100 mg scale and purified by column chromatography. Purity checks were performed with gas chromatography with mass selective detection. The mass spectrum of pentyltrineophyltin is presented.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 0173-0835
    Keywords: Capillary electrophoresis ; Dialysis ; Sample pretreatment ; Serum ; Sulfonamides ; Urine ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: A fully automated dialysis solid-phase extraction (SPE) sample preparation procedure is coupled on-line to capillary electrophoresis (CE) for the first time. The system is used to determine sulfonamides in serum and urine. The dialysis unit serves to remove proteins and particulate matter. Reconcentration of the analytes is performed with a small SPE column while (in)organic salts and other interferences are removed simultaneously. Finally, the analytes are desorbed and injected, via a homemade interface, into the CE system. Limits of detection (LOD) of 0.05-0.1 and 0.05-0.3 μg/mL are obtained in urine and serum, respectively. The within-day and between-day precisions are in the range of 2-6% and 3-8%, respectively, for a concentration of five times the LOD. The dialysis SPE-CE system was used over a period of six months for the analysis of over 500 serum and urine samples without problems such as clogging of the CE capillary or SPE column.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
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  • 4
    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.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995), S. 124-128 
    ISSN: 0935-6304
    Keywords: Large volume injection ; PTV injector ; PTV solvent split injection ; Packed inserts ; Thermal degradation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 6
    ISSN: 0935-6304
    Keywords: Capillary GC ; Continuous liquid-liquid extraction ; Environmental applications ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The applicability of a liquid-liquid extraction system which is coupled on-line with a capillary gas chromatograph was studied for environmental and ecotoxicological analyses. The optimized and automated system was used for the determination of apolar and rather non-volatile organic compounds in aqueous samples. Relevant aspects of sample introduction, phase separation and selection of extraction solvent are discussed. Three routine-tipe applications are described, viz. an improved method for the determination of hexachlorocyclohexanes in ground water and the determination of the so-called NCC-ether and ACC-ether in ecotoxicological studies. Depending on the application studied, the concentration levels varied from 0.1 to 6000 μg/I, using ECD and/or FID detection. Typical coefficients of variation obtained with the total extraction-GC procedure were 2-25%.The system was found to be rugged, it saves time compared with set-ups involving off-line liquid-liquid extraction and considerably reduces the manual work load.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 20 (1997), S. 363-368 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Solid-phase extraction ; Automation ; Water samples ; Acetylation ; Chlorophenols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An automated system for derivaatization was coupled on-line with solid-phase extraction-gas-chromatography (SPE-GC). The system was optimized for the determination of phenol and chlorinated phenols in aqueous samples. The test analytes were acetylated with acetic anhydride; proper buffering of the sample was a critical factor. Next, the phenol acetates were enriched on a SPE cartridge and transferred to a GC; two appraoaches were studied. In the first approach, the derivatives were enriched on disposable C18 cartridges (ASPEC type) and desorbed with methylacetate. Aan aliquot of the final eluate was injected on-line the GC by means of a loop-type interface. In the second approach, trace enrichment was performed on 10 × 2 mm i.d. LC-type precolumn packed with polystyrenedivinylbenzene copolymer (PLRP-S) this precolumn was dried with a mitrogen purge and the phenol acetates were desorbed with ethyl acetate which was injectedon-line into the retention gap of the GC under partially concurrent solvent evaporation (PCSE) conditions. The Derivatization-SPE-GC system which was based on the loop-type interface has the advantage of simplicity and easy operation, the main drawback is the impossibility to determine phenol acetates which elute prior to trichlorophenol acetates. With the derivatization-SPE-GC approach using PCSE-based desorption, even the most volatile analyte of the test series, phenol acetate, can be determined successfully. The entire procedure, including the derivatization step, was fully automated and integrated in one set-up. The precision data for the integrated on-line derivatization-SP-FID system were fully satisfactory, with RSD values of 1-12 % at the 1 μg/1 level. When a sample volume of 2.2 ml was analyzed, The detection limits for the chlorinated phenol acetates were in the 0.1-0.3 μg/1 range.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 8
    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.
    Type of Medium: Electronic Resource
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  • 9
    ISSN: 1040-7685
    Keywords: on-line extraction-GC ; open-tubular traps ; coiled tubes ; secondary flow ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The effect of geometrical deformation of open-tubular extraction columns on peak dispersion of retained solutes is evaluated. By coiling or stitching of the columns peak dispersion is decreased, with a factor of two and more than five, respectively, due to secondary flow enhanced radial dispersion. This enables the increase of sampling flow rates in on-line extraction-GC using open-tubular extraction columns up to 4 mL/min while still obtaining quantitative trapping of the analytes. © 1995 John Wiley & Sons, Inc.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
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  • 10
    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.
    Type of Medium: Electronic Resource
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