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  • 1965-1969  (2,843)
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  • 1
    Electronic Resource
    Electronic Resource
    New York : Wiley-Blackwell
    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 659-662 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
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  • 2
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The crystal structure of the α polymorph of nylon 4 has been determined from the x-ray diffraction patterns of uniaxially oriented monofilaments. In general the crystal structure of α nylon 4 is similar to that of α nylon 6. The unit cell is monoclinic with the following dimensions: a = 9.29 ± 0.05 A., b = 12.24 ± 0.05 A., c = 7.97 ± 0.05 A., and β = 114.5 ± 1.0°. There are eight monomeric units in the unit cell. The theoretical density is 1.37 g./cc. and the observed density 1.25 g./cc. The space group is P21. The nylon 4 chains are of the extended planar zigzag type, with the plane of the zigzag approximately parallel to the a axis of the unit cell. Along the a axis, every other chain is inverted - an antiparallel arrangement of chains - thus permitting complete hydrogen bonding and the formation of sheets of nylon 4 chains. Along the c axis of the unit cell, the second sheet is displaced by3/10 of the b axis, thus leading to a staggered arrangement of sheets. The sheets are held in place by van der Waals forces.
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  • 3
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    New York : Wiley-Blackwell
    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 599-610 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A method is described for the conversion of polystyrene to poly(styrenesulfonic acid) without change in the molecular weight distribution; the reaction is performed at room temperature in 100% H2SO4 and uses Ag+ catalyst. The resulting polyelectrolyte has solubility and other characteristics significantly different from those of previously investigated poly(vinylsulfonic acid). This permits a study of the influence of the aromatic group on the local and long range interactions in solution. The barium salt of poly(styrenesulfonic acid) is unusual in showing both upper and lower consolute temperatures in solution.
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  • 4
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    New York : Wiley-Blackwell
    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 611-629 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Epitaxial deposition of homopolymers from solution [polyethylene, isotactic polystyrene, poly-3,3-bischloromethyloxacyclobutane (Penton) and polypropylene] was found on the (001) faces of cleaved alkali halide single crystals. Electron and optical microscopy studies have shown that the polymer usually grew from small, rodlike crystallites which were oriented in (110) directions of the halide crystal. Large oriented, four-leaved, “rose” structures also were observed for polyethylene. Electron diffraction studies indicate that the polymer chain axes for polyethylene, isotactic polystyrene, and Penton generally lie parallel to the (001) faces of the halide crystal and are also oriented in the 〈110〉 directions of the crystal face. Investigations on the effect of various halide substrates upon the epitaxial crystallization habit of polyethylene inferes that lattice matching does not play the major role in orientation. Two possible explanations are offered for this epitaxial behavior.
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  • 5
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    New York : Wiley-Blackwell
    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 631-638 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The effect of basic aluminium dibenzoate upon the supercooling of polypropylene fractions of molecular weight 9.2 × 103-1.25 × 106 was determined by differential thermal analysis. The response to heterogeneous nucleation within the precision of the method used appears to be only slightly dependent, if at all, upon the molecular weight of the polymer.
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  • 6
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    New York : Wiley-Blackwell
    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 639-647 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Wideline NMR techniques have been applied to both singly and doubly oriented specimens of nylon 66. Variations in the spectra obtained are observed for different orientations of the specimens relative to the applied field. These variations demonstrate that the zigzag chain axis is essentially parallel to the draw direction and that motion occurs in all of the sample. The motion is of two types: random in the mobile regions and rotation of segments about the chain axis in the rigid regions.
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  • 7
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    New York : Wiley-Blackwell
    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 663-665 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
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  • 8
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    New York : Wiley-Blackwell
    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 649-657 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The crystallization kinetics of poly(n-octadecyl methacrylate) has been studied at the air-water interface. The rate of the crystallization has been measured by the decrease in the area of monolayers with time at various temperatures and surface pressures. The crystallization isotherms have been analyzed by the general mathematical treatment of the kinetics of phase changes, and the results show linear growth to be dominant. The variation of the rate constant with temperature and pressure has been illustrated by the difference in the supersaturation defined by introducing the equilibrium pressure-area isotherms.
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  • 9
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 668-672 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
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  • 10
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 673-684 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Specific heats of plasticized poly(vinyl chloride) can be readily obtained by means of the thin foil calorimeter when the polymer is fabricated into sheet or film. The effects of temperature and plasticizer content on the specific heat and of the plasticizer content on the glass temperature are readily observed. The data may be used to estimate the glass temperatures of plasticizers where those temperatures are not readily reached by normal techniques. The specific heat at the glass temperature is approximately 0.255 for the ranges of 0-30 phr plasticizer. A definite glass transition is not observed with 60 phr plasticizer. No other transitions were observed between 200 and 400°K. The previous history of the polymer is important, as it can change the specific heat of the polymer noticeably, especially above the glass temperature. Comparison of the values listed here with those obtained by others should be made with the understanding that these samples were fabricated by extrusion and were free of observable strain. The degree of crystallinity of these polymers is very small, probably less than 10%, since none was found by x-ray diffraction. The plasticizing effect of some stabilizers was noted.
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  • 11
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 697-704 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Depolarization currents were used to study the persistent polarization induced in polystyrene and poly(methyl methacrylate) by cooling with flow under pressure. These studies showed that the charge on electrets made by flow under pressure consists in part of a surface charge which leaks off rapidly in moist air and in part of a charge due to volume polarization which decays more slowly. The volume polymerization produced in poly(methyl methacrylate) by flow under pressure is of the same order as that produced by cooling under a voltage drop, but flow under pressure produces a larger surface charge.
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  • 12
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The ability of various polymers to acquire persistent polarization (i.e., to become electrets) was investigated. Polarization was induced in the polymers by two methods: (a) by cooling under a voltage drop and (b) by cooling with flow under pressure. There was found to be an optimum temperature for electret formation by either method. This optimum temperature was roughly 37°C. above Tg when polarization was produced by application of a voltage drop and roughly 57°C. when polarization was produced by flow under pressure. Crystallinity and the nonhomogeneities present in blended polymers were harmful to electret formation, but a small critical amount of ionic impurity was helpful.
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  • 13
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 705-714 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The determinations of the number-average molecular weight of polyethylene by cryoscopy has been improved, permitting precise measurements with both linear and branched polyethylenes in the molecular weight range 4,000-30,000. Improvements include a cryometer of new design, a lower-melting cryoscopic solvent containing a nucleating agent to control supercooling and rate of crystallization of the solvent, and more precise measurement of freezing point depression. Polyethylene samples are dissolved in hexamethylbenzene admixed with 0.1% of cadmium iodide, and steady-state freezingpoint depressions are measured with a thermistor to a maximum sensitivity of 5 × 10-5°C. Molecular weight measurements are reproducible to within ±10%. The cryoscopic apparatus and procedure are described in detail, and results obtained with samples of linear and branched polyethylene are presented and discussed.
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  • 14
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 765-775 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The behavior of films of polyelectrolytes at the water-organic liquid interface depends on the nature of the interface and the pH of the substratum. The present paper investigates the influence of these two factors on the cohesive forces between monomer units. Two polyelectrolytes were studied: poly(methacrylic acid) (APM) and poly-2-vinylpyridine (2-PVP). In the case of uncharged films, the collapse pressure decreases when the polarity of the organic phase becomes more important, whereas the term ω/kT, which appears in the theory of Motomura and Matuura, increases. A quantitative relation between the parameter ω/kT and the collapse pressure may be deduced. The behavior of the ionized surface film at different pH values is modified by the choice of the interface. However, there exists a competition between two phenomena: the dissolution of ionized residues in the substratum and the electrostatic repulsion between charges in the surface plane. Depending upon whether the first or the second parameter is more important, we observed that the surface pressure decreased or increased with the degree of ionization.
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  • 15
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 731-743 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Gel permeation chromatography is an elution chromatographic process depending on the permeation of the solute through a bed of gel particles. This process is used in the estimation of molecular weight distributions of polymers, since elution occurs in decreasing order of molecular size. The eluting species, however, are not perfectly fractionated, and apparent broadening of the distribution occurs. This broadening results from an axial (longitudinal) mixing of the eluting species. Consideration of the accessible bed volume for each species permits a correction to be made for this axial dispersion. The concept was applied to heterodisperse distributions by solving the resulting simultaneous equations. A least-squares regression may be employed to utilize the experimental data most effectively. The experimental chromatogram can be described in terms of accessible bed volume and dispersion coefficient of each species together with flow rate, sample concentration, and chromatograph column geometry. The chromatogram corrected for the axial dispersion describes the molecular weight distribution more accurately than does the experimentally determined curve. The correction procedure was applied to a well-characterized polystyrene; the results of the gel permeation chromatography show excellent confirmation of the results of fractionation and of other instrumental analyses.
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  • 16
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Torsional creep measurements on four natural rubber vulcanizates, crosslinked to different degrees, were carried out in the temperature range from -50 to 90°C. This investigation complements the studies on identical samples of the stress relaxation behavior by Chasset and Thirion and of the dynamic mechanical response by Ferry, Mancke, Maekawa, Ōyanagi, and Dickie. The creep measurements reported are shown to be in agreement with the stress relaxation results. In addition to the usual temperature reduction, a superposed curve was obtained for the long time response using the apparent molecular weight between crosslinks, Mc, as a reduction variable. The variation in viscoelastic response with crosslink density is interpreted as a restrictive action of the chemical crosslinks on the transient entanglement network.
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  • 17
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Crystallization kinetics of crystalline fractions of propylene oxide polymers made with different catalysts have been studied by isothermal dilatometric and microscopical measurements. Isothermal microscopical measurements indicate that spherulite growth in these polymers proceeds from predetermined nuclei. The half time for spherulitic appearance is less than, but of the same order as, the half time for complete crystallization. Only by taking this factor into account can the dilatometric data be represented by the Avrami equation. The deviation of the crystallization isotherm from that predicted from the microscopical data using the Avrami theory is attributed to a secondary crystallization process taking place within the spherulite. Crystallization continues long after spherulites completely occupy the available volume in the polymer. By assuming that the secondary crystallization proceeds as a first-order process in the uncrystallized, but crystallizable, portions of the melt, it is shown that the crystallization isotherms can be completely described in terms of four parameters. These are: (1) the time constant for the primary crystallization process; (2) the time constant for nucleation; (3) the time constant for the secondary crystallization process, and (4) the extent of secondary crystallization. The important conclusions of these studies are: the rates of nucleation and of spherulitic growth are far more dependent on temperature than on stereoregularity; the ratio of the rate of the secondary crystallization process to that of the primary crystallization process is almost independent of temperature, but increases with increasing stereoregularity of the polymer.
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  • 18
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 777-788 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The structure of polypropylene crystallized at pressures up to 5000 atm. has been studied. Upon slow cooling from the melt at 320 atm., the γ modification, previously found only in low molecular weight and stereoblock fractions, begins to appear in small amounts in addition to the normal α monoclinic form. As the pressure is increased further, a larger proportion of the sample crystallizes in the γ form until, at 5000 atm., only the γ modification is present. X-ray and DTA studies show that the γ form of polypropylene transforms to the normal α modification at a temperature only slightly below the γ melting point. Evidence is presented which favors the occurrence of a solid-state transition as a model of transformation to the α form. Results from isothermal crystallizations at low supercoolings and annealing experiments under high pressure show that the melting point of the γ modification of polypropylene is very sensitive to crystallite perfection.
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  • 19
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 817-825 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The vapor pressure osmometry method for determining the molecular weight of polyamides has been studied by use of the newly developed solvents. Polymers used were polycaprolactams, polyenanthamides, and polypelargonamides. The measurements were carried out with 2,2,3,3-tetrafluoro-1-propanol and 2,2,3,3,4,4,5,5,6,6,7,7-dodecafluoro-1-heptanol as solvents at 50 and 130°C., respectively. Endgroup determinations on samples were also done in m-cresol by 0.1 N-hydrochloric acid. Reduced resistance differences (ΔR/C)0 obtained by vapor pressure osmometry at 50°C. were found to be in linear relation with the reciprocal of the number-average molecular weight determined by endgroup titrations; but anomalous results were obtained when dodecafluoroheptanol was used as the solvent at 130°C.
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  • 20
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 797-816 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The orientation behavior of stereoregular poly(vinyl alcohols) was investigated during stretching and after releasing the stress on the bulk polymers at relatively high humidity (80% R. H.) A structural model, differing from polyethylene, was proposed in which the crystallites were embedded in a considerably swollen amorphous matrix without any definite physical interaction so as to form an aggregation of crystallites, a superstructure. The crystal orientation followed, in principle, “the first borderline case” of Kratky, but with some difference from theory in orientation, while the noncrystalline orientation was represented by the freely jointed equivalent chain model of Kuhn and Grün with a value of N/γ as small as around 5. The difference between crystal orientation found and the theorietical orientation is discussed and some factors which prevented the crystal orientation are considered.
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  • 21
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 789-796 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Mechanical damping measurements were carried out in the range of 103-105 cps and between 60°K. and the softening point on some substituted Polystyrenes and poly(vinyl benzoates) containing different substituents (methyl groups, methoxy groups, and halogen atoms) either in the ring or in the main chain. The ortho and meta ring-substituted polystyrenes do not show any secondary mechanical relaxation in the glassy state, although all the other substituted polystyrenes, exhibit a low-temperature damping peak (δ process) (which is in some way connected with ring motions) whose height and temperature location depend on nature, position, and number of substituents. Substituents in the para position of the ring or in the α position in the backbone chain shift the δ peak of the unsubstituted polystyrene towards higher temperatures; this shift is accompanied by an increase of the apparent activation energy E*. Substitution in the β position, on the contrary, does not affect the δ peak. Analogous results are obtained for substituted poly(vinyl benzoates), which exhibit, in addition, a β relaxation effect, associated with carboxyl group motions. A very good correlation is found between the values of E* and the limiting relaxation time τ for the δ relaxation of polystyrenes and poly(vinyl benzoates), similarly substituted in the ring, indicating that the δ relaxation leads to absorption curves in the mechanical relaxation spectrum which are characteristic of the structure of the aromatic side chain.
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  • 22
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 827-829 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
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  • 23
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 830-831 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
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  • 24
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 835-844 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The second virial coefficients of amylose acetate fractions have been determined at different temperatures and have been analyzed according to recent theories of second virial coefficient.
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  • 25
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 845-854 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Dynamic viscoelastic properties of 10 and 20% aqueous solutions of sodium polyacrylate were studied by the electromagnetic transducer method at 500 cps in the temperature range of 0-50°C. These solutions distinctly showed a relaxation phenomenon in this temperature range which was also affected by addition of such compounds as sodium chloride, urea, and dioxane. An anomalous behavior that cannot be explained as due to the relaxation phenomenon was observed on the addition of small amounts of these agents. One of the causes of this behavior is ascribed to the ion association in the solution. The static viscosity of the solution was also measured by using a rotating cylinder viscometer and the results compared with the dynamic data.
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  • 26
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 855-868 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The glass transitions of an ionic polymer in bulk have been studied as a function of the counterion for various homo- and copolymers. It is shown that the glass transition temperature can vary by as much as 530°C., from -10°C. for the nonionic material to +520 for Ca2+ or Zn2+ substituted polymer. From simple electrostatic considerations, it is shown that a linear correlation should exist beween the glass transition and the ratio of the cation charge, q, to the internuclear distance, a, between cation and chain anion; for this particular material (the polyphosphate chain) the relation is Tg = 625(q/a) -12 where q is in units of one electron and a is in A. If the data are interpreted in the light of the Gibbs-DiMarzio theory, it is seen that both the chain stiffness and the intermolecular energy increase in an approximately parallel manner as q/a increases.
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  • 27
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 869-880 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The configurational entropy of the polyethylene chain at the melting points calculated in two ways. In both calculations, tetrahedral angles and discrete trans and gauche arrangements of all bonds are assumed, and trans bonds are assumed more stable than gauche by energy U1. First, calculations are made on chains of up to N = 18 bonds, disallowing all configurations having overlapping atoms, and the result is extrapolated to large N. Second, a calculation is made directly for long chains, with overlaps excluded only over every short chain segment. The results are in almost exact agreement, suggesting that the second method can be safely used with other molecules. The calculated configurational entropy is in line with that suggested by the entropy of fusion, assuming the chains to acquire a configurational freedom in the melt which approaches that of independent chains.
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  • 28
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 881-897 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The angular distribution function P(θ) for intensity of light scattered by a dilute solution of comblike branched molecules has been determined for three situations of some interest for evaluation of experimental data: (1) the molecules are identical with branches of equal length attached equidistantly along linear backbone chains; (2) the molecules are homogeneous in mass, with the same number of branches on each molecule, but the branches are distributed at random along the chain; (3) branches and main chains are still uniform, but the molecules are heterogeneous in mass with the number of branches per molecule distributed according to the binomial distribution and the branches in any molecule spaced randomly along the backbone. Examination of numerical results shows that the scattering functions for models (1) and (2) are not very different. The function for case (3) is somewhat different from the others when the mean number of branches per molecule is small but they contain a large fraction of the mass of the molecule. Over a limited range of the pertinent variables (corresponding roughly to observations on typical vinyl polymers of molecular weights up to 106) all three functions agree quite well with P(θ) for homogeneous linear chains with the same mean-square radius of gyration.
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  • 29
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 923-942 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A light-scattering study is presented of two isotactic polypropylene samples with broad molecular weight distributions (Mw/Mn = 8.1 and 8.7, respectively) dissolved in α-chloronaphthalene at 147°C. Incident radiation of 5460, 4358, and 3650 A. was used. The reciprocal intramolecular scattering function, P-1(u) is expressed as a function of the variable [sin(θ/2)/λ′]2. This provides a wider range of experimental values of the variable u = 16π2(b2/6) [sin(θ/2)/λ′]2 than is accessible by the usual technique of using only one wavelength. The shape of the function P-1(u) is closer to that predicted theoretically if the weight distribution function f(N) in the equation \documentclass{article}\pagestyle{empty}\begin{document}$ P(u) = \int_0^\infty {Nf(N)P_N (u)dN} /\int_0^\infty {Nf(N)dN} $\end{document} is given by the log-normal distribution rather than the distribution function of Schulz and Zimm. The method is applicable to polymer samples for which the average molecular weights are too low to be measured by the light-scattering method of Benoit and Loucheux.
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 571-586 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The changes in x-ray orientation brought about by the treatment of cotton and ramie with caustic soda of different concentrations have been studied. With ramie the effect of the treatment is to decrease the x-ray orientation, while with cotton the reverse is true. The cause of this difference is traced to a difference in the morphology of the two fibers rather than a difference in their fine structure.
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 559-569 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The dynamic mechanical properties of poly-4-methylpentene-1 have been measured in torsion in the temperature range from 25 to 160°C. at frequencies from 10-3 to 10 cps. Two transitions are found. The first, with a peak at 40°C. at 1 cps, appears as a normal glass transition. A broad high temperature peak appears at 130°C. The dynamic compliance-frequency data can be superposed by the conventional method of reduced variables for temperatures up to 100°C. The temperature dependence of the shift factors follows the WLF equation. Above this temperature, superposition can be achieved by applying horizontal and vertical shifts to both components of the dynamic compliance. When the vertical shift is permitted, the range of applicability of the WLF equation is extended to 160°C.
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  • 32
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 545-557 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Two sets of dynamic mechanical property data and some stress relaxation data for semicrystalline, linear polyethylene are treated by data reduction methods previously described. These data can be represented by a master plot of reduced modulus versus reduced frequency and two sets of temperature-dependent shift factors. The first of these factors reflects the change of viscoelastic relaxation times with temperature. The second represents a separable change of modulus with temperature which applies over the entire time or frequency range of the experiments. This change is larger and in the opposite direction to that found applicable in the behavior of noncrystalline plastics and rubbers. The two sets of dynamic data show the same frequency-temperature dependence which can be represented by an activation energy of 22 kcal./mole. Small differences in the modulus-temperature dependence are attributed to differences in molecular weight or annealing conditions. The stress relaxation data superposes to a curve in good agreement with the dynamic data but with a factor of 20 difference in time scale. This difference is attributed to the finite strains used in the stress relaxation measurements. Such strains might be expected to increase free volume in simple extension deformations and so accelerate the relaxation.
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    Journal of Polymer Science Part A-2: Polymer Physics 4 (1966), S. 587-598 
    ISSN: 0449-2978
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: NMR measurements on undrawn polyethylene (PE) samples in contact with a solvent such as C2Cl4 indicate an increase in the mobility of the mobile chain segments as compared to dry samples. Highly drawn PE shows no such effect. This is because Sa, the sorption per unit mass of noncrystalline material present, decreases from 20.9 wt.-% (dry basis), found for undrawn quenched PE, to 0.63 wt.-% after drawing (Sa determined at 25°C. and 0.80 vapor activity). Drawing also reduces the segment mobility according to the NMR spectrum. It is shown that these effects are caused by considerable structural changes occurring in the noncrystalline regions of PE upon drawing. Annealing of drawn PE samples at successively higher temperatures leads to a gradual relaxation of the noncrystalline regions towards the state characteristic of undrawn PE. With increasing annealing temperature Sa as well as the mobility approach values found with undrawn PE.
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  • 34
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    Journal of High Resolution Chromatography 5 (1982), S. 311-320 
    ISSN: 0935-6304
    Keywords: Chromatography theory, GC and LC ; Chromatography plate concept, “theoretical” and “discontinuous” ; Partial differential contributions ; Variance addition rule ; Theoretical band shapes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: It is shown theorectically that the classical formula for calculating the theoretical plate number from squared first central moment, tms2, and second central moment, σ2, according to ntheor = tms2/σ2 is valid only when the capacity ratio, k approaches infinity. The general relation between the classical experimental HETP value, H = L/nmtheor, and the underlying true theoretical plate height, ΔL, is found to be\documentclass{article}\pagestyle{empty}\begin{document}$$ {\rm H' = }\frac{{{\rm L(\sigma ')}^{\rm 2} }}{{\overline {\rm t}_{{\rm ms}}^{\rm 2} }}{\rm = }\frac{{{\rm 2}\overline {\rm D} _{\rm m} }}{{\overline {\rm u} }}{\rm + }\overline {\rm k} \frac{{{\rm 2}\overline {\rm D} _{\rm s} }}{{\overline {\rm u} }}{\rm + \Delta L}\frac{{\overline {\rm k} }}{{{\rm 1 + }\overline {\rm k} }} $$\end{document} when (σ′)2 is the total column contribution to band broadening, L is the column length, Dm is the average diffusion coefficient of the sample component in the mobile phase, Ds is its value in the stationary phase, and u is the average linear velocity of the mobile phase. The mobile phase displacement, as well as the mass exchange process, is assumed to be continuous, but the application of the plate concept conditions leads to a mass balance equation that can be interpreted as belonging to a modified discontinuous plate model. The contributions 2Dm/u and k 2 Ds/u from longitudinal sample diffusion in the mobile and stationary phases, respectively, are consistent with the assumption that the processes are statistically independent, although the common solution technique of the differential equations does not take full account of this independence.
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    Journal of High Resolution Chromatography 5 (1982) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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  • 36
    ISSN: 0935-6304
    Keywords: Thin-layer chromatography, TLC ; Binary solvent mixtures ; New solvent polarity ranking ; Optimization ; Window diagram ; Cluster center ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ΔRf, the separation between a pair of compounds on a thin layer chromatographic plate, can be predicted as a function of solvent composition for certain binary systems. This allows the prediction of optimum solvent composition for separating a mixture of compounds by thin layer chromatography. A new solvent polarity ranking, based on calculation of ΔRf is described.
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    Journal of High Resolution Chromatography 5 (1982), S. 382-384 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Trapping by active charcoal ; Thermal desorption system ; Microwave oven ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 3-12 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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  • 39
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    Journal of High Resolution Chromatography 5 (1982), S. 31-37 
    ISSN: 0935-6304
    Keywords: Gas-liquid chromatography ; Plasma determination ; Midazolam ; Pharmacokinetic study ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A sensitive gas liquid chromatographic (GLC) assay was developed for plasma determinations of 8-chloro-6-(2′ -fluorophenyl)-1-methyl-4H-imidazo[1,5 α][1,4]benzodiazepine (compound I) and its hydroxymethylimidazo metabolite (compound II). The internal standards used were 8-chloro-6-(2′ -chlorophenyl)-1 -methyl-4H-imidazo[1,5 α][1,4]benzodiazepine (compound VI) and 7-chloro-5-(2′ -fluorophenyl)-1, 3-dihydro-1-(hydroxyethyl)-2H-1,4-benzodiazepin-2-one (compound VII) for compounds I and II, respectively. Following extraction, and silylation for compound II, compounds I and II were analyzed by GLC using a glass column packed with 5% OV-101 on Gas-Chrom Q, and a 63Ni electron-capture detector. The GLC method was validated by a CI-GC/MS technique. The detection limit of the assay is approximately 4-5 ng/ml for compound I and 3 ng/ml for compound II. The method was used in comparative pharmacokinetic studies of the distribution of the two compounds in arterial and venous blood.
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    Journal of High Resolution Chromatography 5 (1982), S. 50-51 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass, fused silica ; Connection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 58-58 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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  • 42
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, fused silica ; Effluent splitter ; Selective detectors: NPD, Hall™ electrolytic conductivity detector ; Chloro- and chloronitroanilines ; POTW sludge extracts ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Simultaneous detection with a 700-A Hall™ and an NPD detector is an effective technique for characterizing chloro-and chloronitroanilines in highly complex Publicly Owned Water Treatment Works (POTW) sludges. The utilization of a modified Varian effluent splitter and a SE-54 fused silica capillary column permitted the detection of mid-picogram quantities of the polar chloroanilines without sacrificing peak shape. The response of the Hall™ detector in the halogen mode was roughly proportional to the number of chlorine atoms present, while the response of the Hall™ in the nitrogen mode and the NPD was less predictably influenced by the presence of one or more nitro groups. When combined with retention time data, the ratio of the NPD response to the Hall™ response has been found to substantiate the presence of chloro- and chloronitroanilines in sludge extracts.
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    Journal of High Resolution Chromatography 5 (1982), S. 98-99 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Polyaromatic hydrocarbons ; Airborn Particulates ; Aircraft turbines ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 106-107 
    ISSN: 0935-6304
    Keywords: RM values in HPTLC ; A-ring derivatives of 5α-cholestane ; trans-Decalin derivatives as reference compounds ; ΔRM values for C/D rings and side chain in 5α-cholestanes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 113-113 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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  • 46
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; High temperature silylation ; C2-C6 fatty acids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 134-138 
    ISSN: 0935-6304
    Keywords: Thin-layer chromatography ; Reversed phases ; Preloading with solvent vapors ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The chromatographic behavior of some hydrocarbons and some of their nitro derivates after preconditioning with solvent vapors has been investigated. After preloading with cyclohexane or hexane an improved separation of some sample pairs is observed. Furthermore, inversion of Rf values takes place. The preloading of the reversed-phase plates permits utilization of mobile phase with higher water content, thus leading to a significant shortening of developing time.
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    Journal of High Resolution Chromatography 5 (1982), S. 150-150 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 5 (1982), S. 139-142 
    ISSN: 0935-6304
    Keywords: Thin-layer chromatography, TLC ; TLC with mixed mobile phases ; Adsorption chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Considerations of TLC process optimization have been based on the thermodynamic theory of adsorption from multicomponent solvents using experimental and theoretical RM1, 2 = f (Φ1) relationships. It was found that a relationship exists between the Az parameter (log k1,2∞ where k1,2∞ is the partition coefficient of the substance chromatographed) of the above theory and pKa values of substances as well as the solubility parameter δ of the mobile phase components. Analysis of the Az values of substances shows that a slight variation therein is associated with lower selectivity of chromatographic separation.
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    Journal of High Resolution Chromatography 5 (1982), S. 206-207 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; cis, trans, positional isomers of C22 esters separated on OV-73 ; Numerous arguments favor nonpolar columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 213-214 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Electron capture detection ; Time constant, purge flow ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 222-222 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 5 (1982), S. 218-220 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 5 (1982), S. 236-244 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Rotary valve ; Cold trap ; Reinjection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This paper describes a cold trap/reinjection system for capillary columns which utilizes a flow switching rotary valve. Sample enrichment is performed in a liquid nitrogen-cooled glass trap attached to the valve. Evaporation of enriched compounds is carried out with the aid of an electric heating coil. Parameters such as cryogenic trapping efficiency, reinjection rates, transference of sample, and adsorption, as well as overall performance, are examined. In addition, a comparison is made between the cold trap/reinjection technique and injection with a gas-tight syringe.
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    Journal of High Resolution Chromatography 5 (1982), S. 265-266 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; Helium ionization detector ; Aroma ; Coffee ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 56
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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  • 57
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    Journal of High Resolution Chromatography 5 (1982), S. 13-18 
    ISSN: 0935-6304
    Keywords: Gas chromatography, capillary ; Column preparation ; Immobilization of stationary phases ; Procedure for polar phases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Whereas the immobilization of apolar silicone phases is essentially understood and mastered, the corresponding treatment of even moderately polar phases remains problematical. Upon attack by peroxide radicals, these phases respond by forming active transformation products rather than by bonding to the support surface or to neighboring molecules. OV-1701 is at present the most polar stationary phase which can reasonably be immobilized. An essential feature of the practical procedure is the prevention of film breakage after coating the inert support surface and before immobilization. Two ways of overcoming this problem are presented.
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    Journal of High Resolution Chromatography 5 (1982), S. 45-47 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Fast screening of drugs and adulterants ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 55-56 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Non-uniformity of distribution of stationary phase confirmed ; Chemistry ; Analytical Chemistry and Spectroscopy
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    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 60-60 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 5 (1982) 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 5 (1982), S. 19-26 
    ISSN: 0935-6304
    Keywords: Gas chromatography, glass capillary ; Selective detection ; Nitrated polycyclic aromatic hydrocarbons ; Carbon black ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Glass capillary gas chromatography has been investigated as a method for the analysis of nitrated polycyclic aromatic hydrocarbons (nitro-PAH) using both splitless and on-column injection techniques. The nitro-PAH showed good chromatographic performance and thermal stability under the GC conditions used. Retention times and response factors of several nitro-PAH were compared to those of conventional PAH.Simultaneous flame ionization and thermionic nitrogen selective detection was used to facilitate identification of nitro-PAH in complex samples. The feasibility of the method is demonstrated on two samples of commercial carbon black. Besides 1-nitropyrene several isomeric dinitropyrenes have been identified.
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    Journal of High Resolution Chromatography 5 (1982), S. 27-30 
    ISSN: 0935-6304
    Keywords: Gas chromatography/mass spectrometry ; Capillary columns, fused silica ; Response factors, interlaboratory ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A quality control procedure for Fused Silica Capillary Column Gas Chromatography/Mass Spectroscopy (FSCC GC/MS) was tested and shown to produce similar response factors at five Spectroscopy (FSCC GC/MS) was tested and shown to produce similar response factors at five laboratories. The average relative standard deviation (RSD) of interlaboratory response factors for fifty three compounds of environmental interest determined at each laboratory at nominal injected weights of 20, 100, and 200 ng was found to be 18.9% for four of the five laboratories which participated in this work. These data demonstrate that similar response factors can be attained in routine GC/MS measurements when adequate quality control is maintained.
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  • 64
    ISSN: 0935-6304
    Keywords: Chromatography theory, GC and LC ; Statistical independence of various band broadening processes ; Variance addition rule for statistically independent processes ; Random walk description of longitudinal diffusion ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The total length-based second moment contribution from longitudinal sample diffusion in both phases on a column, σc,2D, is derived by adding individual partial differential contributions to a partial differential equation accounting for the longitudinal diffusion processes only. Although each diffusion-dispersed sample part is equilibrated between two phases, the resulting σc,2,D (= 2Dmtm + 2Dsts) can be interpreted as the sum of two independent contributions in accordance with the variance addition rule. (Dm and Ds are the mean diffusion coefficients and tmand ts the mean residence times of the sample in the mobile and stationary phases, respectively.) The same σc,2D expression is derived from the random walk model of Giddings by treating the diffusional process in each phase as statistically independent of the other processes. Under these conditions the broadening contribution from longitudinal diffusion in the mobile phase is shown to be independent of the velocity profile.
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    Journal of High Resolution Chromatography 5 (1982), S. 53-55 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, fused silica ; Thermal aging regeneration of fused silica capillaries ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary ; SD-E enrichment ; Pesticide residues ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A simple method is described for the quantitative determination of organochlorine pesticides and polychlorinated biphenyls (PCB's) in water at the sub-ppb level. A micro gas-phase extractor advantageously replaces other preconcentration and purification techniques. The extract is analyzed by capillary gas chromatography without further enrichment. The recovery at the ppb level was nearly 100% for organochlorine pesticides and more than 80% for PCB's. The complete procedure including sample preparation, steam distillation-extraction, and capillary gas chromatographic analysis is carried out in less than four hours.
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    Journal of High Resolution Chromatography 5 (1982), S. 360-363 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Microbore columns ; Reverse-phase mode ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A procedure for packing reverse-phase microbore columns using moderate pressure is described. Columns packed from different manufacturer's tubing are compared with commercially available columns. A method for coupling the column to the injection valve is suggested. The effect of detector cell volume on overall efficiency of the system is also examined.
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    Journal of High Resolution Chromatography 5 (1982), S. 377-378 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Glass capillary columns ; Headspace analysis ; Alcohols in blood ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 381-381 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 5 (1982), S. 692-693 
    ISSN: 0935-6304
    Keywords: Liquid-liquid partition chromatography, HPLC ; Liquid-liquid distribution ; Toluoylglycines, methylhippuric acids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 158-160 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Reversed-phase mode ; Good separation of preservatives from matrix and from each other at optimum pH and mobile phase ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 165-166 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Pulse flow reaction chromatography ; Two-detector system ; Reactions in a two-detector system ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 73
    ISSN: 0935-6304
    Keywords: Gas chromatogarphy ; Capillary columns ; Headspace analysis ; Both headspace and essential oil chromatograms required for evaluation of herbs ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: GC headspace analyses of various aromatizing herbs have been compared with those relating to the essential oils, obtained by steam distillation, of the same plants. In this way it was possible to establish the most significant differences between the composition of a herb flavor and that of its essential oil. In particular, we observed some very volatile compounds in the headspace samples which were absent from the essential oil; these components may make an important contribution to the herb flavor. The identification of these substances is still in progress.
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    Journal of High Resolution Chromatography 5 (1982), S. 285-290 
    ISSN: 0935-6304
    Keywords: Gas chromatography, capillary ; Column preparation ; Neutral and amino sugars, alditol acetates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The development of improved high resolulation glass capillary columns for separating the alditol acetates of neutral and amino sugars is described. Different capillary column treatments were evaluated for their activity toward amino sugar derivatives and for their effect on the efficiency of the completed column. The simple two-step procedure of leaching with aqueous hydrochloric acid and dynamic coating with SP-2330 was found to produce efficient and inert columns.
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    Journal of High Resolution Chromatography 5 (1982), S. 321-321 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, fused silica ; Pyrolysis studies ; Cryofocusing device ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 349-354 
    ISSN: 0935-6304
    Keywords: Gas chromatography, capillary ; Persilylated, apolar columns ; Immobilized coatings ; Determination of column bleeding ; Re-silylation of fresh and used columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The bleeding of apolar high temperature columns may well be the critical factor limiting their applicability for GC/MS-coupling, and for high temperature analyses. Therefore, a bleeding determination procedure has been designed as a basis for a systematic approach to the production of low-bleed columns. Re-silylation is a traditional method of reducing column bleeding. Increased efficiency of re-silylation becomes feasible with immoblized coatings. Experience gained so far shows that resilylation of immoblized coatings may indeed result in the expected strongly reduced bleed rates and in improved overall column quality. Re-silylation may also contribute to column washing by enhancing the solubility of adsorbed contaminants.
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    Journal of High Resolution Chromatography 5 (1982), S. 80-84 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Triglycerides in cocoa butter, hazelnut oil ; Separation according to the number of unsaturated fatty acids (N.U.F.A.) ; Ozonolysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Structure determination of triglycerides according to their number of unsaturated fatty acids (N.U.F.A.) is more easily achieved after ozonolysis of their mixtures (fats and oils) than by capillary gas chromatographic analysis of the mixture as such. Analyses performed before and after ozonolysis of cocoa buttel, hazelnut oil, and a mixture of both fats illustrate the potential of this approach to the structure elucidation of triglycerides by chromatographic techniques.
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    Journal of High Resolution Chromatography 5 (1982), S. 100-101 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; High performance thin-layer chromatography ; Lipid analysis ; Quantitative interpretation ; High-temperature transesterification by tetramethylammonium hydroxide ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 102-103 
    ISSN: 0935-6304
    Keywords: Micro HPLC ; Isotope separation ; Packed micro glass capillary ; Reversed phase mode ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 109-112 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 5 (1982), S. 150-150 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 5 (1982), S. 156-157 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; Cold trapping ; Use of ABT concept in evaluating effect of trapping on peak ; shape ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 83
    ISSN: 0935-6304
    Keywords: Chromatography theory, GC and LC ; Revised “stage” model of Said ; Revised relaxation-time model of Giddings ; Statistically independent partial differential contributions ; Relation between HETP and true theoretical plate height ΔL ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The mass balance changes of Said's so-called “stage” model, based on the movement of the mobile phase with mean velocity ū (=L/tm), are synchronized by introduction of the relaxation time of Giddings, tr=1/(km+ks) where km and ks are the general overall mass rate constants for sample transfer to and from the stationary phase, respectively. This makes the “stage” length equal to the true theoretical plate height, ΔL, related to the classical HETP contribution due to non-equilibrium, H(α), according to the “discontinuous-ΔL” relation \documentclass{article}\pagestyle{empty}\begin{document}$$ {\rm H}_{{\rm (\alpha)}} {\rm =}\frac{{{\rm L\sigma}^{\rm 2} _{{\rm (\alpha)}}}}{{\overline {\rm t} _{{\rm ms}}^{\rm 2}}}{\rm = \Delta L}\frac{{\overline {\rm k}}}{{{\rm 1 + k}}} $$\end{document} Here k= (tms - tm)/tm is the central moment-based capacity ratio, L the column length, and σ2(α) the second moment contribution from the non-equilibrium only. Correct application of the relaxation-time model to chromatography requires that the real sample concentration in the stationary phase at a given position and time, Cs,l,t, is in a continuous equilibrium with the real sample concentration in the mobile phase, Cm,l+ΔL/2,t at that time displaced down the column by a distance \documentclass{article}\pagestyle{empty}\begin{document}$$ \frac{{{\rm \Delta L}}}{{\rm 2}}{\rm = t}_{\rm r} \overline {\rm u} {\rm =}\frac{{\rm L}}{{k_{\rm m} \overline {\rm t} _{\rm m}}}\frac{{\overline {\rm k}}}{{{\rm 1 +}\overline {\rm k}}} $$\end{document} This leads to the classical HETP contribution \documentclass{article}\pagestyle{empty}\begin{document}$$ {\rm H}_{{\rm (\alpha)}} {\rm =}\frac{{{\rm 2L}}}{{k_{\rm m} \overline {\rm t} _{\rm m}}}\frac{{\overline {\rm k}}}{{{\rm (1 +}\overline {\rm k})^2}} $$\end{document} obtained from various other continuous models, which implies that ΔL is a good estimation of the true theoretical plate height.
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    Journal of High Resolution Chromatography 5 (1982), S. 163-164 
    ISSN: 0935-6304
    Keywords: High performance thin-layer chromatography, HPTLC ; HPTLC bonded phases ; 3-Aminopropyltriethoxysilane-treated plate ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 175-181 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Discrimination factor non-vaporizing on-column/vaporizing splitless injection for underivatized steroids ; Quantitation feasible for most underivatized steroid hormones except corticosteroids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Recent developments in the preparation of capillary columns by persilanization of the glass surfaces have resulted in highly inactive, heat-stable columns. With this type of column certain steroid hormone classes can be analyzed without derivatization; these include the 17-keto steroids, 11-oxo compounds, estrogens, and progesterone metabolites. It has been found that good quantitative analysis calls for non-vaporizing, on-column injection, as normal vaporizing injection results in breakdown of thermolabile compounds such as estriol and 17-OH progesterone metabolites. The gas chromatographic method described was used to obtain urinary steroid profiles.
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    Journal of High Resolution Chromatography 5 (1982), S. 208-209 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Liquid chromatography ; Capillary glass ; Capillary columns with inside splitting of eluent ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 211-212 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; On-column injection ; Elimination of discrimination ; Sliding sample inlet ; Cooling column system ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 245-249 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; High resolution ; Spherical silica gel ; Column coupling ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In order to justify its classification as a “high resolution” technique, HPLC should show an improvement in efficiency by a factor of at least 10, should be easily achievable with separation times of less than 1 h, preferably in the reversed phase mode. This is accomplished by coupling three 25 × 0.46 cm columns packed with 5 μm spherical ROSiL-C18-D silica gel. Details of the method and some typical chromatograms are given.
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    Journal of High Resolution Chromatography 5 (1982), S. 107-108 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Static coating ; Closing glass capillaries ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 115-116 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 5 (1982), S. 119-123 
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    Keywords: Gas chromatography ; Capillary, glass ; Static coating ; Filling with mechanical closure ; Description of an easy and safe technique ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The static technique is commonly accepted as the most universal and scientific method of coating. At the same time, however, it is said to be experimentally demanding. Great efforts have therefore been made to render the method easier and safer, resulting in a wealth of recommendations confusing non-experts. Over a period of two years we have practically applied most of the reported procedures with the aim of studying their practical convenience. We do not doubt that most procedures are comparably suitable in the hands of expert users, i. e. once the initiation efforts have been forgotten, or are otherwise of little interest. We have attempted to describe a method which is specifically suited for easy and quick introduction to beginners. The method is based on mechanical column closure. The principles of the method are discussed, and a comprehensive description of its practical application is given.
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    Journal of High Resolution Chromatography 5 (1982), S. 167-168 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 5 (1982) 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 5 (1982), S. 331-335 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 5 (1982), S. 91-92 
    ISSN: 0935-6304
    Keywords: Ultra-micro-HPLC ; LC-Ms coupling ; EIMS ; Chemistry ; Analytical Chemistry and Spectroscopy
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    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 104-105 
    ISSN: 0935-6304
    Keywords: Thin-layer chromatography ; Effect of relative humidity ; Phospholipids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 5 (1982), S. 108-108 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 5 (1982) 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 5 (1982), S. 227-235 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Van Deemter curve ; GC column selection ; GC carrier gas ; Capillary column length ; Capillary column diameter ; Film thickness in capillary columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of computer-constructed van Deemter curves that permits evaluation of a number of variables in capillary gas chromatography is presented. The graphs permit the comparison of inter-related parameters, including the choice of carrier gas (hydrogen vs helium vs nitrogen), column length (10-100 m), column diameter (0.20, 0.25, 0.32, 0.4 mm), solute partition ratios (0-10), and liquid phase film thickness (0.1, 0.25, 0.5, 1.0 μm). The curves are evaluated, both in terms of the relative magnitude of the optimum average linear carrier gas velocity, and in terms of the significance of the sharpness of the curve.
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    Journal of High Resolution Chromatography 5 (1982), S. 255-260 
    ISSN: 0935-6304
    Keywords: Liquid chromatography HPLC ; High-speed HPLC ; Oil spill identification ; Polynuclear aromatic hydrocarbons ; Crude oils ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The use of high-speed HPLC in oil spill identification problems has been evaluated in terms of analysis time and reliability. The aromatic fraction was analyzed by reverse-phase chromatography on a 3 μm packing, with detection at 210 and 287 nm, in less than 20 minutes. The profiles exhibited by several Spanish and Middle East crude oils were differentiated by simple statistical parameters. The effect of environmental weathering on the samples has also been investigated. An Arabian light crude oil was still identifiable after four months' simulated marine weathering.
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