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  • 1
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 6 (1973), S. 148-152 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: A general procedure for determination of the crystallinity in polymers from the X-ray diffraction pattern was developed by modifying the method described by Ruland [Acta Cryst. (1961), 14, 1180–1185] on two points. One of these modifications furthermore permits substantial reduction of the required number of experimental data without a serious loss of accuracy being involved.
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  • 2
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 4 (1971), S. 340-342 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: A computer procedure for slit-height correction of X-ray small-angle scattering curves is described, which Ij based on direct calculation of the desmeared intensity values Ij from the equations Ĩi = ∑jai,jIj where Ĩi is the observed smeared intensity at point i and ai,jIj represents the contribution from a point j along the trace of the primary beam. However, the number of unknown Ij values is reduced by a factor 1/n (n = 3 to 5), and the equations are solved by the method of least-squares. The performance of the method is tested on the diffraction curve of isolated spheres.
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  • 3
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 14 (1981), S. 8-16 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Various sources of random deviations occurring in the determination of X-ray intensities with the aid of film methods are discussed and corresponding mathematical expressions are derived. From a comparison with experimental values of the standard deviations obtained from measurements on homogeneously exposed films, it follows that the deviations are primarily caused by the variations of the X-ray photon flux due to the stochastic nature of the X-ray emission process. The accuracy attainable with most X-ray films is found not to be limited by saturation of the number of excited AgBr particles occurring at increasing exposures, but at low exposures film methods are at a disadvantage because of the presence of fog. If, however, small signals superimposed on a high sample background have to be measured, relatively high exposures are required; in this case film registration is found to be much faster than methods involving step-scanning counters, and in general little slower than registration with the aid of a position-sensitive counter. It is also shown that the dynamic range of the film method may be extended without sacrificing accuracy by resorting to slower films.
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  • 4
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 6 (1973), S. 81-86 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The mean square of the electron-density gradient, 〈|grad η|2〉 in isotropic structures is shown to be proportional to the fourth moment of the SAXS intensity distribution in reciprocal space ∫s4I(s)ds, as well as to the second derivative of the correlation function in the origin. In the case of two-phase structures with unsharp phase boundaries, these relations may be used to find the thickness E of the transition regions. As was shown by Ruland [J. Appl. Cryst. (1971). 4, 70–73] E can also be determined by analysis of the intensity in the tail of the SAXS pattern. This approach is used here to investigate the effect of E on the one-dimensional correlation function. In the application of both methods, separation of the SAXS intensity from the continuous background of liquid scattering constitutes a critical step. A procedure in which the background is represented by a curve of the type a + bsn, where n is an even number, is found to work well for a number of polymers.
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  • 5
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 9 (1976), S. 433-440 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The total X-ray intensity as a function of h (h is the radial coordinate in reciprocal space), scattered by an isotropic system of particles of equal shapes but of different sizes R, can, under certain conditions, be expressed as an integral over the particle size distribution function D(R), multiplied by a common single-particle function of hR which can be calculated from the assumed particle shape. In the first method D(R) is calculated from this relation by the method of least squares, in which values of D at a limited number of particle sizes are the unknowns. To avoid oscillations in the D curve, constraints are imposed on the D values. The proper weight to be assigned to these constraints must be determined by trial and error. The method has been adapted to suit various assumptions and requirements as to the shape of the particles, the type of distribution function to be calculated, and experimental conditions (slit or pinhole focusing). The second method is essentially the one described by Schmidt, Weil & Brill [X-ray & Electron Methods of Analysis, pp. 86–100. (1968), New York: Plenum], which, however, is adapted to the use of slit-smeared intensities. Both methods may give rise to artefacts in the calculated distribution functions in the range of the smallest particle sizes, which are sensitive to the setting of the various parameters and to experimental errors. However, the position and shape of the main maxima can usually be determined quite well. The agreement between the results obtained by the two methods is satisfactory.
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  • 6
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 33 (2000), S. 1422-1429 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The conventional method to measure small induced changes in integrated intensity utilizes a zero-dimensional detector, which greatly limits the data collection speed. This paper shows that the use of an area detector in combination with an X-ray chopper decreases the data collection time significantly. A monochromatic diffraction setup using a charge-coupled device (CCD) detector coupled to an X-ray image intensifier was constructed and tested. The setup proved to be sufficiently stable to measure changes in integrated intensity well below 0.1%. Subsequently, a data set of a piezoelectric KD2PO4 crystal in an external electric field was collected. The data were merged to yield 77 unique reflections. The induced structural changes were determined by a least-squares refinement. The results agree very well with experiments in which a zero-dimensional detector was used. The major improvement is the decrease in data collection time by one order of magnitude, without any degradation of the data quality, offering new possibilities for this type of perturbation study.
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  • 7
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 8 (1975), S. 340-341 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The program comprises a main program for inspection and correction of the intensity data, and a number of subroutines covering specific operations. These subroutines can be called upon in any desired sequence.
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  • 8
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 11 (1978), S. 541-546 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The effects of deviations from an ideal lamellar structure (infinite-size clusters of parallel layers of alternating electron densities) on the small-angle scattering curve are treated with the aid of the correlation function. If surrounded by a matrix of the average electron density, reduction of the size of the clusters in the direction of the layer normals leads to a simple modification of the one-dimensional correlation function. Distortions giving rise to structures containing concentric layers have little effect on this function, whereas corrugation of the surfaces causes minor modifications. Second-order defects are shown to reduce the three-dimensional correlation function of the ideal structure γ°(r) according to γ(r) = γ°(r) exp (−2r/d), where d is the `distortion length'. This is the average length of the vectors for which the number of intersections with lamellar interfaces has changed by ±1 as a consequence of the distortions. Calculated diffraction curves show that the effects of reducing the cluster size and of increasing the width β of the lamellar thickness distribution function are very similar. However, changes in d and β affect the scattering curves in a different way, which, other conditions being favourable, may enable these parameters to be determined from observed scattering curves.
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  • 9
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 16 (1983), S. 274-276 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The method of Ruland [Acta Cryst. (1961). 14, 1180–1185] for the determination of crystallinity has been modified in order to take account of a difference in chemical composition of the crystallized and non-crystallized fractions, such as occurs in glass-ceramic materials. Application to two samples leads to higher crystallinities than found by other X-ray methods, and shows a large increase of disorder with decreasing crystallinity.
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  • 10
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Acta crystallographica 12 (1959), S. 859-866 
    ISSN: 0001-5520
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences
    Type of Medium: Electronic Resource
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