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  • 1
    ISSN: 1573-739X
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Normal phase gradient elution ; Polyester resins
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Polymers can be characterized by gradient elution techniques in order to obtain information on their chemical composition and molar mass. In this paper, features and applications of Normal Phase Gradient Polymer Elution Chromatography (NP-GPEC) for the characterization of (co)polyesters are investigated. Two polyesters were characterized, using various stationary and mobile phases. Separation was shown to be dominated by end groups in most cases, and to a lesser extent by molar mass. A distinct influence of both column type and mobile phase type was observed. A polymer based polyamine (PA) column povided the best results, although no complete separation between the mono- and di-acid fractions could be obtained. In all cases, separation was governed by sorption rather than by precipitation/redissolution. NP-GPEC was shown to be a potentially interesting technique for the characterization of copolyesters according to the chemical composition of the backbone, independent of end groups.
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  • 3
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Isotachophoresis ; Sample pretreatment
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This study focusses attention on the possibilities of preparative isotachophoresis (ITP) as a sample pretreatment technique prior to liquid chromatographic (HPLC) analysis. The increased demand for accurate and less time consuming analysis necessitates that sample pretreatment procedures, should be develop in parallel with other improvements (e. g. in detection and separation) which can be observed. The preparation isotachophoresis was performed on gel slabs and the zones of interest were subsequently cut out, desorbed and the desorbates analyzed by HPLC. In this study satisfactory recoveries of between 85–90% with a standard deviation of 1–5% were observed for blank experiments. For spiked serum and urine samples the recoveries in general decreased with decreasing spiked drug concentrations. These observations are discussed in this paper.
    Type of Medium: Electronic Resource
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  • 4
    ISSN: 1612-1112
    Keywords: Micellar electrochromatography ; Electroosmotic flow ; Column coatings
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An investigation was carried out to study the electroosmotic flow (EOF) in micellar electrokinetic capillary chromatography (MECC). Fused silica capillaries were treated with various reagents to investigate the parameters influencing the magnitude and reproducibility of the EOF. The results for untreated and treated columns were collected and compared under the same experimental conditions. Furthermore, experiments with and without sodium dodecylsulfate (SDS) addition to the buffer were carried out to elucidate the influence of this surfactant on the EOF. The mechanisms behind the effects of these modifications on the EOF and the stability of the coatings on the column wall are discussed.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 34 (1992), S. 25-30 
    ISSN: 1612-1112
    Keywords: Electrokinetic capillary chromatography ; Micellar agents ; Chlorophenoxy acids ; Herbicides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method for the separation of a number of herbicides consisting of chlorophenoxy acids by micellar electrokinetic capillary chromatography (MECC) was developed. Sodium dodecyl sulphate (SDS), Brij 35, cetyltrimethylammonium bromide (CTAB) and methanol were introduced into the buffers to investigate their effects on the separation of the herbicides. SDS combined with Brij 35 as the micellar agent was found to provide the best overall separation of these components.
    Type of Medium: Electronic Resource
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  • 6
    ISSN: 1612-1112
    Keywords: Reversed-phase HPLC ; Ageing processes ; Solid state NMR ; FTIR ; Chain dynamics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Laboratory use of HPLC columns packed with C8 and C18 bonded phases leads to changes in selectivities and retention volumes. FTIR,1H NMR of hydrolysed bonded phases and solid state13C- and29Si NMR were applied to characterize the materials. The results of the various techniques are in fair agreement except solid state NMR. Loss of silane and hydrolysis of surface siloxane groups have been observed for the C8 bondes phase, while for the C18 material the latter process seems to dominate. The solid state NMR results have been tentatively explained in terms of changing chain arrangements and mobilities.
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  • 7
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 23 (1987), S. 189-194 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Instrument bandbroadening by extrapolation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Methods to determine the contribution of the chromatographic equipment to the total band broadening which involve replacing the column by a union or a capillary tube are not suitable as they involve a fundamental change in the chromatographic system. The linear extrapolation method, based on the estimation of the relative influence of the instrument variance on solutes with different capacity factors, is a more attractive alternative method since the column remains in the chromatographic system. This method is only valid when a number of conditions are satisfied. By meeting these conditions the error in the instrument variance by using the linear extrapolation method was determined. At the same time, ways to minimise these errors were studied. Use of the linear extrapolation method in combination with conventional columns of 4.6 mm i.d. appears to yield inaccurate results. In combination with microbore columns the method can be used, provided the columns have a maximum length of 5cm and contain a packing material with a particle size of 2 or 3μm. The error in the determined instrument variance is then of the order of 2μl2.
    Type of Medium: Electronic Resource
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  • 8
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Stability of reversed phases ; Acid pretreatment of silica ; Solid state29Si NMR ; Crystalline regions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two stationary phases, identically modified and derived from the same experimental Chromspher substrate, but one of which has been pretreated with a hydrofluoric acid solution, are compared after ageing with various eluents under simulated routine conditions. The hydrothermal hydrofluoric acid treatment of the silica substrate prior to modification with dimethyloctadecyl-silane improved both the surface coverage and the stability of the resulting stationary phase compared to those of the original substrate. The stability of the silica-to-silane bonding after modification was characterized by means of chromatographic techniques and elemental analysis. Changes in the rigidity of the substrate were studied by means of solid state29Si NMR. The effect of the hydrothermal acid treatment on relevant substrate parameters, including formation of crystalline regions at the surface, is also discussed.
    Type of Medium: Electronic Resource
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  • 9
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Flame ionization detection ; Poly(styrene-co-methyl acrylate) ; Poly(methyl acrylate-co-n-butyl acrylate) ; Chemical composition distribution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This investigation is focused on the development of HPLC with subsequent flame ionization detection as a tool to determine the chemical composition distribution of non-or poorly UV absorbing copolymers. Experiments were carried out with poly(styrene-co-methyl acrylate) and poly(methyl acrylate-co-n-butyl acrylate) copolymers. HPLC combined with FID provided useful qualitative information. Quantitative information could be obtained after calibration.
    Type of Medium: Electronic Resource
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  • 10
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 23 (1987), S. 331-336 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Microbore columns ; Injection techniques
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This paper focuses attention on the potentially larger signal-to-noise ratios produced by microbore columns in comparison with conventional columns. The increased chromatographic signals by the application of microbore columns are due to the lower chromatographic dilution of elution profiles which are proportional to the square of the column inner radius. Generally less than 1μl sample should be injected into microbore systems to obtain the full benefit of the column performance. However, since more sample can be loaded on conventional columns compared to microbore columns the advantage of improved signal-to-noise ratio can only be realised in situations where very little sample is available. To inject more than 1μl sample, at the same time avoiding extra band-broadening effects, suitable injection techniques must be available. In this study three injection methods for microbore systems that meet this condition, are studied and compared.
    Type of Medium: Electronic Resource
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