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The effect of a double hydrophilic block-copolymer additive (made of polyaspartic acid and polyethyleneglycol, pAsp(10)-b-PEG(110)) on the initial formation of calcium carbonate from a supersaturated salt solution has been studied in situ by means of time-resolved synchrotron small-angle X-ray scattering (SAXS). A stopped-flow cell was used for rapidly mixing the 20 mM aqueous reactant solutions of calcium chloride and sodium carbonate. In reference measurements without polymer additive the very rapid formation of primary, overall spherical CaCO3 particles with a radius of ca. 19 nm and a size polydispersity of ca. 26% was observed within the first 10 ms after mixing. A subsequent, very rapid aggregation of these primary particles was evidenced by a distinct upturn of the SAXS intensity at smallest angles. During the aggregation process the size of the primary particles remained unchanged. From an analysis of the absolute scattering intensity the mass density of these particles was determined to 1.9 g/cm3. From this rather low density it is concluded that those precursor particles are amorphous, which has been confirmed by simultaneous wide-angle X-ray diffraction measurements. Upon adding 200 pm of the block-copolymer no influence on the size, the size polydispersity and morphology of the primary particles, nor on the kinetics of their formation and growth, was found. On the other hand, the subsequent aggregation and precipitation process is considerably slowed down by the additive and smaller aggregates result. The crystalline morphology of the sediment was studied in situ by WAXS ca. 50 min after mixing the reactants. Several diffraction rings could be detected, which indicate that a transformation of the metastable, amorphous precursor particles to randomly oriented vaterite nanocrystallites has taken place. In addition, a few isolated Bragg spots of high intensity were detected, which are attributed to individual, oriented calcite microcrystals that nucleated at the wall of the capillary. [Copyright &y& Elsevier]

The texture of a yarn describes the orientation of individual fibers in a yarn group. This yarn structure is determined by the application. The OE-rotor spinning system is a very flexible solution among staple fiber spinning processes, since it allows yarn manipulation through the use of various spinning elements. For example, the design of the navel has a significant influence on the yarn structure. The opening roller and rotor are responsible for a large proportion of: the measured number of imperfections, the yarn uniformity, and damage to the fibers. The principal item however, the navel, is able to broadly manipulate yarn volume and hairiness, without necessarily having a negative effect on processing parameters, such as tenacity and elongation. The character of a textile product can be predominantly controlled by the navel.

A compact laboratory X-ray scattering platform that uniquely enables for high-performance ultra-small-angle X-ray scattering (USAXS), small- and wide-angle X-ray scattering (SAXS/WAXS), and total scattering (atomic pair distribution function analysis; PDF) experiments was developed. It covers Bragg spacings from sub-Angstroms to 1.7 μm, thus allowing the analysis of dimensions and complex structures in (nano-)materials on multiple length scales. The accessible scattering vector q-range spans over almost five decades (q min = 0.0036 nm -1 , q max = 215 nm -1 ), without any gaps. Whereas SAXS is suitable to characterize materials on a length scale of 1-100 nm, with USAXS, this range can be significantly extended to the micrometer range. On the other end, from WAXS and particularly from PDF measurements, information about the local atomic order and disorder can be obtained. The high performance, exceptional versatility, and ease-of-use of the instrument are enabled by a high-resolution 2-circle goniometer with kinematic mounts, a modular concept based on prealigned, quickly interchangeable X-ray components, and advanced detector technology. For USAXS measurements, a modified Bonse-Hart experimental setup with single crystal collimator and analyzer optics is used. SAXS/WAXS measurements are enabled by focusing optics, an evacuated beam path, and a 2D detector. For total scattering experiments, a high-energy X-ray source is used in combination with a hybrid pixel array detector that is based on a CdTe sensor for the highest counting efficiency. To ensure high resolution and sensitivity in these various applications, special care is taken to suppress any type of background scattering signal. The high resolution that can be achieved with the USAXS collimation system is demonstrated on a set of monodisperse, colloidal silica dispersions and derived colloidal crystals, with particle diameters in the range of hundreds of nanometers up to 1.6 µm. USAXS and SAXS results are shown to be consistent with those obtained by static light scattering (SLS) and dynamic light scattering. It is demonstrated that the obtainable USAXS data bridge the gap in q between SAXS and SLS. The capabilities of the instrument to acquire high-quality total scattering data for PDF analysis are demonstrated on amorphous SiO 2 nanoparticles as well as on NaYF 4 upconversion nanocrystals. To the best of our knowledge, it is for the first time that we present a single laboratory instrument that enables measurements of high-quality X-ray scattering data within such a wide q-range, by combining four complementary elastic X-ray scattering techniques. The modular design concept of the instrument allows for incremental improvements as well as to add more applications in the future.

Small-angle X-ray scattering (SAXS) is a well-established, versatile technique for the analysis of nanoscale structures and dimensions, e.g., in liquid dispersions, thin solid objects or powder samples. When combined with wide-angle X-ray scattering (WAXS), complementary information about the atomic structure can be obtained. SAXS experiments traditionally require dedicated instruments to achieve the desired angular resolution, sensitivity, stability, and speed of measurement. Here we demonstrate how a multi-functional laboratory goniometer platform, as widely being used for powder X-ray diffraction and for a variety of related techniques, can be configured with pre-aligned X-ray modules that enable advanced SAXS/WAXS experiments, without compromising the exceptional versatility of the instrument. Line and point collimation setups, as well as quick and easy switching between them, are readily possible. Key components are a detachable, evacuated beam path and a high-resolution, low-noise hybrid pixel area detector, in combination with a hardware interface design that allows to configure the instrument with different X-ray modules without the need for re-alignment. Software for SAXS data reduction and analysis was developed. The good SAXS/WAXS performance and the derived analytical results were verified on various test samples, such as gold nanoparticles, colloidal silica, liposomes, dilute protein solutions, and solid polymer samples. It is believed that this novel approach to SAXS/WAXS instrumentation will help to make this powerful structure analysis technique more widely accessible and affordable for multi-user laboratories.

Synchrotron X-ray reflectivity and grazing incidence diffraction were applied to study the structures of phospholipid Langmuir-Blodgett films under controlled humidity. Distearoylphosphatidylethanolamine (DSPE) and DSPE-PEO lipopolymers, in which a poly(ethylene oxide) chain with n = 8, 17, or 45 EO units is covalently linked to the polar headgroup of DSPE, were used. When the relative humidity was changed from below 2 to 97%, the phosphate headgroup in a DSPE film was hydrated with a concomitant thickness increase of 4.2 A and an electron density decrease. The swelling of the monolayer was found to be a reversible process without any significant roughening of the film. Subtle differences in the film thickness could be detected for DSPE monolayers transferred under various lateral pressures. The degree of lateral ordering of the alkyl chains in DSPE monolayers increased considerably when the humidity was raised. In the case of DSPE-PEO with eight EO units, the hydration of the monolayer was also found to be reversible, but the water uptake was larger due to the presence of the hydrophilic polymer interlayer, which is located between the substrate and the DSPE moieties. Under high humidity, the lipopolymer monolayer with n = 17 exhibited a well-defined, layered structure similar to that of DSPE-PEO with n = 8. In the case of n = 45, however, there are indications for a significant intermixing of the polymer with the DSPE moieties, probably resulting in the formation of hydrophobic nanodomains of closely packed alkyl chains that are immersed into the hydrated polymer.

With reference to an observation, thirty-four cases of systemic mastocytosis with intestinal malabsorption are reviewed. The most characteristic intestinal anomalies are the steatorrhea, partial villous atrophy and deficiency in secretory IgA. Routine investigations for mastocytosis may be warranted in patients with malabsorption. A markedly telangiectatic and angiomatous aspect of cutaneous lesions may be suggestive of the association.