A method to quantify crystallinity in amorphous metal alloys: A differential scanning calorimetry study.

We developed and describe a differential scanning calorimetry method for calculating the initial crystallinity, change of crystallinity and crystallinity percentage of amorphous metal alloys as a function of temperature. Using thermodynamic enthalpies of amorphous, crystalline and partially devitrified specimens, our methodology is capable of determining crystallinity percentages as low as a few percent. Moreover, the linear relationship between the set (pre-determined) and calculated crystallinities of experimental samples indicates that there is no need to prepare calibration samples before measuring the crystallinity percentage of target samples. This technique also eliminates the need for expensive in situ accessories, such as those required in electron microscopy. Thus, the technique is highly relevant as a primary technique for characterization of devitrification behavior in amorphous materials.

Segmental Mobility in the Non-crystalline Regions of Semicrystalline Polymers and its Implications on Melting.

Detailed knowledge on chain mobility in polymers is of fundamental interest in order to understand their mechanical properties. As a specific example, the melting behavior of semicrystalline polyethylene can be studied by thermal analysis and NMR spectroscopy. In ultra high molecular weight polyethylene (UHMW-PE) crystallised via different routes, i.e., directly during polymerisation, from solution, or from the melt, and melted under different protocols, different melting processes involving detachment of stems from the crystals and cluster melting can be distinguished. Melting by the consecutive detachment of chain stems from the crystal substrate ultimately results in a melt state where chain dynamics for entanglement formation are much more restricted.

NC100150 Injection, a preparation of optimized iron oxide nanoparticles for positive-contrast MR angiography.

A preparation of monocrystalline iron oxide nanoparticles with an oxidized starch coating, currently in clinical trials (NC100150 Injection; CLARISCAN), was characterized by magnetization measurements, relaxometry, and photon correlation spectroscopy. By combining the results with a measure of iron content, one can obtain the size and magnetic attributes of the iron cores, including the relevant correlation times for outer sphere relaxation (tau(SO) and tau(D)), and information about the interaction of the organic coating with both core and solvent. The results are 6.43 nm for the iron oxide core diameter, a magnetic moment of 4.38x10(-17) erg/G, and a water-penetrable coating region of oxidized oligomeric starch fragments and entrained water molecules. The latter extends the hydrodynamic diameter to 11.9 nm and lowers the average diffusivity of solvent about 64% (which increases tau(D) accordingly). The nanoparticles show little size-polydispersity, evidenced by the lowest value of r(2)/r(1) at 20 MHz reported to date, an asset for magnetic resonance angiography.

'NC100150', a preparation of iron oxide nanoparticles ideal for positive-contrast MR angiography.

A laboratory-scale synthesis of NC100150 (iron oxide particles with an oxidized starch coating) was characterized by magnetization measurements (vibrating sample magnetometry, VSM), relaxometry (1/T1 NMRD profiles and 1/T2 at 10 and 20 MHz), and dynamic light scattering (photon correlation spectroscopy, PCS). The results were related to give a self-consistent physical description of the particles: a water-impenetrable part making up 12% of the total particle volume, 82% of this volume consisting of an iron oxide core and the remaining 18% consisting of an oxidized starch rind; and, a water-penetrable part making up 88% of the total particle volume, consisting of oxidized starch polymers and entrained water molecules. Relating the magnetization to the relaxometry results required that the oxidized starch coating slows the diffusivity of solvent water molecules in the vicinity of the iron oxide cores. The effect of the organic coating on water diffusivity, not previously considered in the application of relaxation theory to iron oxide nanoparticles, is supported by the much greater (factor of about 2) diameter obtained from the dynamic light scattering measurements in comparison to that obtained from the magnetization measurements. The present work shows that three physical techniques--VSM, relaxometry, and PCS--are needed for properly assessing iron oxide nanoparticles for use as contrast agents for magnetic resonance angiography (MRA). It is also shown that NC100150 has a narrow range of diameters and the smallest value of r2/r1 reported to date, an asset for MRA.

Inactivation of photosensitizing merocyanine dyes by plasma, serum and serum components.

Merocyanine dyes with an oxygen in the electron donor heterocycle were rapidly degraded by plasma, serum and serum components. Replacement of the oxygen by a sulfur or selenium atom rendered the dyes refractory to degradation. The degradation of labile merocyanine dyes was temperature dependent and oxygen independent. The plasma component that was responsible for the degradation of merocyanine dyes was sensitive to heat and detergent, suggesting an enzymatic process. The identification of the structural requirements for sensitivity/resistance to degradation provides the experimenter with a simple means to manipulate the stability of merocyanines in high serum or plasma environments and may expand the clinical utility of merocyanine photosensitizers beyond their traditional role in the extracorporeal purging of bone marrow grafts.