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  • Analytical Chemistry and Spectroscopy  (45)
  • Wiley-Blackwell  (45)
  • 1980-1984  (45)
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 355-356 
    ISSN: 0935-6304
    Keywords: Gas-liquid chromatography (GLC) ; Open tubular glass capillary columns ; Blended stationary phases ; Liquid crystals ; Polycyclic aromatic hydrocarbons (PAH) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 634-640 
    ISSN: 0935-6304
    Keywords: HPLC ; Reverse-phase ; UV detection ; Fluorescence detection ; Polycyclic aromatic hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Modern liquid chromatographic (LC) conditions which effect a separation of polycyclic aromatic hydrocarbons (PAH) containing up to ten rings are described. The LC conditions include reverse-phase chromatographic columns in combination with a quaternary solvent system. Methanol and water are combined to form solvent system A, while tetrahydrofuran and acetonitrile form solvent system B. Solvent systems A and B are then combined in a linear gradient relationship to effect the separation. The separation of benzo(a)pyrene and perylene along with benzo(ghi)perylene and indeno (1,2,3-cd)pyrene is achieved. In the same chromatogram the PAHs, coronene, dibenzo(a,e), (a,i), (a,h)pyrene and tribenzo(a,e,i)pyrene are also separated. An increase in column temperature from 45°C to 55°C is shown to shorten the elution time and increase chromatographic resolution of many of the PAHs examined. At least 25 PAHs ranging in molecular weight from 178 to 536 are examined for their chromatographic behavior. As examples, the application of this method to samples from a coal liquefication process are included. The samples are examined with both a UV detector and fluouescence detector to demonstrate the utility of dual detectors when analyzing for PAHs in complex matrices. With minor modification of the gradient this method is applicable to PAHs containing ring systems other than those reported here.
    Additional Material: 8 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 444-445 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Open-tubular columns ; Reduced diameter ; High pressure ; Coating reservoir ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 333-336 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Liquid crystal ; N,Ń, Bis (p-phenylbenzylidene)-α, α′-bi-p-toluidine (BPhBT) ; Steroids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A gas-chromatographic separation of underivatized steroids is described, in which the liquid crystal N,Ń-bis(p-phenylbenzylidene)α,α′-bi-p-toluidine (BPhBT) was used isothermally at 265°C for the stationary phase. The nematic range of this crystal is 247 to 403°C. Use of the BPhBT crystal allowed operations in a temperature range where steroids are volatile and unlikely to display broad elution peaks and long retention times.With columns precoated with 2.5 weight percent of BPhBT, steroids containing minor structural differences in the ring system were readily differentiated. For example, 5-androsten-17α-ethinyl-3β, 17β-diol was found to elute more rapidly than its 3-keto analog, ethisterone. Ethisterone was distinguished readily also from its 19-nor analog, norethisterone. Additionally, differences in side-chain functionality and resultant molecular dimensions facilitated the separation of steroids of identical ring structure, as in the comparison of cholesterol with methyl 3β-hydroxy-5-cholenate and 25-hydroxycholesterol.An enhancement of separation according to the molecular length-to-breadth ratio was observed; in general, the larger this length-to-breadth ratio, the greater the retention period on the column.
    Additional Material: 4 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 4 (1981), S. 654-655 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Memory effects ; Sample solvent ; Peak broadening ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 6
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Preparation of deactivated capillaries for routine analysis ; Easy deactivation and pretreatment steps described in detail ; Comparison of different modes given ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new surface pretreatment for the preparation of wall-coated open tubular (WCOT) glass capillary columns has been evaluated. This technique involves the application of a non-extractable layer of Superox™-4, a 4,000,000 MW polyethylene glycol, to the glass surface as a pretreatment and deactivation agent. Unlike other polyethylene glycols, Superox-4 is stable at high temperatures (〉 300°C) in the absence of oxygen, coats smoothly onto a bare glass surface and resists droplet formation. WCOT columns (SE-54, Carbowax 20M, and SP-2250) prepared using this technique are compared to columns prepared using a modified Grob [2,3] BaCO3 procedure. The Superox-4 pretreated columns were equal or superior in quality to the BaCO3 pretreated columns, based on the appearance of an activity standard and the effective theoretical plates (Neff) per meter. Chromatograms showing practical application of the WCOT columns prepared using both methods is given.
    Additional Material: 12 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 4 (1981), S. 366-384 
    ISSN: 0935-6304
    Keywords: GC/MS ; Capillary columns, fused silica ; Priority pollutants ; Quantitation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Operational characteristics have been determined for fused silica capillary column (FSCC) GC/MS as applied to “extractable” priority polutants. Chromatographic data show excellent relative retention time (RRT) intralaboratory precision and interlaboratory accuracy when multiple internal standards are empolyed. Potential chromatographic problems, such as column overload and “double peaking”, are addressed. Response factor relative standard deviations (RSD) at 50 ng for most of the extractable priority pollutants over the long term indicated precise determination (i.e. RSD generally ≤ 10%). Linearity was demonstrated over two orders of magnitude for FSCC GC/MS analysis of compounds with relatively low and high RF (response factor) values. Potential quantitative problems, such as saturation, are discussed. For certain aromatic priority pollutants interlaboratory RF agreement was observed. This was noted as perhaps the most important property of FSCC GC/MS analysis when the multiple internal standard approach is utilized. Determinations of extractable priority pollutants are directly compared for paced column GC/MS and FSCC GC/MS analysis of separate and composited extracts. For six extracts analyzed in triplicate, the latter configuration was shown to produce more consistent results. In view of the superior analysis logistics of composite extract FSCC GC/MS analysis, this approach was established as the preferred method for the analysis of priority pollutants classified as extractable.
    Additional Material: 12 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 7 (1980), S. 294-300 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The mass spectra of the TMS derivatives of some 28 5-methoxyindoles, 5-hydroxyindoles and related compounds have been measured. Their retention times and methylene unit values on a 10% OV1/Chromosorb gas chromatography column linked to a Varian 311A double focusing mass spectrometer have been determined. Rf values of these compounds were also determined using 18 different solvents on thin layers of silica gel.
    Additional Material: 6 Ill.
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  • 9
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: As part of a study to make a comparative analysis of selected halogenated compounds in man and the environmental media, a quantitative gas chromatographic mass spectrometric analysis of the levels of the halogenated compounds found in the breath, blood and urine of an exposed population (Old Love Canal area, Niagara, New York) and their immediate environment (air and water) was undertaken. In addition, levels of halogenated hydrocarbons in air samples taken in the general Buffalo, Niagara Falls area were determined.
    Additional Material: 8 Ill.
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  • 10
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 8 (1981), S. 144-148 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Folic acid and several analogs have been characterized as their permethylated derivatives. These derivatives are readily evaporated from the solid probe and provide spectra with abundant molecular ions and characteristic fragment ions. This method has been used to confirm the identities of the two methotrexate metabolites, 7-hydroxymethotrexate and 4-amino-4-deoxy-N10-methylpteroic acid, which have been isolated from human urine. The permethylation products of the folate cofactors, dihydrofolic acid, tetrahydrofolic acid and leucovorin, are also characterized.
    Additional Material: 4 Ill.
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