Unraveling Pre-filled Syringe Needle Clogging: Exploring a Fresh Outlook Through Innovative Techniques.

OBJECTIVE: This study aimed to investigate the movement of liquid in the needle region of staked-in-needle pre-filled syringes using neutron imaging and synchrotron X-ray tomography. The objective was to gain insights into the dynamics of liquid presence and understand the factors contributing to needle clogging. METHODS: Staked-in-needle pre-filled syringes were examined using neutron radiography and synchrotron X-ray phase-contrast computed tomography. Neutron radiography provided a 2D visualization of liquid presence in the needle, while synchrotron X-ray tomography offered high-resolution 3D imaging to study detailed morphological features of the liquid. RESULTS: Neutron radiography revealed liquid presence in the needle region for as-received samples and after temperature and pressure cycling. Pressure cycling had a more pronounced effect on liquid formation. Synchrotron X-ray tomography confirmed the presence of liquid and revealed various morphologies, including droplets of different sizes, liquid segments blocking sections of the needle, and a thin layer covering the needle wall. Liquid presence was also observed between the steel needle and the glass barrel. CONCLUSIONS: The combination of neutron imaging and synchrotron X-ray tomography provided valuable insights into the dynamics of liquid movement in staked-in-needle pre-filled syringes. Temperature and pressure cycling were found to contribute to additional liquid formation, with pressure changes playing a significant role. The detailed morphological analysis enhanced the understanding of microstructural arrangements within the needle. This research contributes to addressing the issue of needle clogging and can guide the development of strategies to improve pre-filled syringe performance.

Towards spatially resolved magnetic small-angle scattering studies by polarized and polarization-analyzed neutron dark-field contrast imaging.

In the past decade neutron dark-field contrast imaging has developed from a qualitative tool depicting microstructural inhomogeneities in bulk samples on a macroscopic scale of tens to hundreds of micrometers to a quantitative spatial resolved small-angle scattering instrument. While the direct macroscopic image resolution around tens of micrometers remains untouched microscopic structures have become assessable quantitatively from the nanometer to the micrometer range. Although it was found that magnetic structures provide remarkable contrast we could only recently introduce polarized neutron grating interferometric imaging. Here we present a polarized and polarization analyzed dark-field contrast method for spatially resolved small-angle scattering studies of magnetic microstructures. It is demonstrated how a polarization analyzer added to a polarized neutron grating interferometer does not disturb the interferometric measurements but allows to separate and measure spin-flip and non-spin-flip small-angle scattering and thus also the potential for a distinction of nuclear and different magnetic contributions in the analyzed small-angle scattering.

Decomposing Magnetic Dark-Field Contrast in Spin Analyzed Talbot-Lau Interferometry: A Stern-Gerlach Experiment without Spatial Beam Splitting.

We have recently shown how a polarized beam in Talbot-Lau interferometric imaging can be used to analyze strong magnetic fields through the spin dependent differential phase effect at field gradients. While in that case an adiabatic spin coupling with the sample field is required, here we investigate a nonadiabatic coupling causing a spatial splitting of the neutron spin states with respect to the external magnetic field. This subsequently leads to no phase contrast signal but a loss of interferometer visibility referred to as dark-field contrast. We demonstrate how the implementation of spin analysis to the Talbot-Lau interferometer setup enables one to recover the differential phase induced to a single spin state. Thus, we show that the dark-field contrast is a measure of the quantum mechanical spin split analogous to the Stern-Gerlach experiment without, however, spatial beam separation. In addition, the spin analyzed dark-field contrast imaging introduced here bears the potential to probe polarization dependent small-angle scattering and thus magnetic microstructures.

Grain morphology reconstruction of crystalline materials from Laue three-dimensional neutron diffraction tomography.

The macroscopic properties of advanced engineering and functional materials are highly dependent on their overall grain orientation distribution, size, and morphology. Here we present Laue 3D neutron diffraction tomography providing reconstructions of the grains constituting a coarse-grained polycrystalline material. Reconstructions of the grain morphology of a highly pure Fe cylinder and a Cu cube sample are presented. A total number of 23 and 9 grains from the Fe and Cu samples, respectively, were indexed and reconstructed. Validation of the grain morphological reconstruction is performed by post-mortem EBSD of the Cu specimen.

Visualization and quantification of inhomogeneous and anisotropic magnetic fields by polarized neutron grating interferometry.

The intrinsic magnetic moment of a neutron, combined with its charge neutrality, is a unique property which allows the investigation of magnetic phenomena in matter. Here we present how the utilization of a cold polarized neutron beam in neutron grating interferometry enables the visualization and characterization of magnetic properties on a microscopic scale in macroscopic samples. The measured signal originates from the phase shift induced by the magnetic potential. Our method enables the detection of previously inaccessible magnetic field gradients, in the order of T cm-1, extending the probed range by an order of magnitude. We visualize and quantify the phase shift induced by a well-defined square shaped uniaxial magnetic field and validate our experimental findings with theoretical calculations based on Hall probe measurements of the magnetic field distribution. This allows us to further extend our studies to investigations of inhomogeneous and anisotropic magnetic field distribution.

Laue three dimensional neutron diffraction.

This article presents a measurement technique and data analysis tool to perform 3D grain distribution mapping and indexing of oligocrystalline samples using neutrons: Laue three-dimensional neutron diffraction (Laue3DND). The approach builds on forward modelling used for correlation and multiple fitting of the measured diffraction spots relative to individual grains. This enables not only to identify individual grains, but also their position and orientation in the sample. The feasibility and performance of the Laue3DND approach are tested using multi-grain synthetic datasets from cubic (α-Fe) and tetragonal (YBaCuFeO5) symmetries. Next, experimental results from two data sets measured at the FALCON instrument of Helmholtz-Zentrum Berlin are presented: A cylindrical alpha iron (α-Fe) reference sample with 5 mm diameter and 5 mm height, as well as a 2 mm3 layered perovskite (YBaCuFeO5). Using Laue3DND, we were able to retrieve the position and orientation of 97 out of 100 grains from a synthetic α-Fe data set, as well as 24 and 9 grains respectively from the α-Fe and YBaCuFeO5 sample measured at FALCON. Results from the synthetic tests also indicate that Laue3DND is capable of indexing 10 out of 10 grains for both symmetries in two extreme scenarios: using only 6 Laue projections and using 360 projections with extremely noisy data. The precision achieved in terms of spatial and orientation resolution for the current version of the method is 430 µm and 1° respectively. Based on these results obtained, we are confident to present a tool that expands the capabilities of standard Laue diffraction, providing the number, position, orientation and relative size of grains in oligocrystalline samples.

Dynamic volume magnetic domain wall imaging in grain oriented electrical steel at power frequencies with accumulative high-frame rate neutron dark-field imaging.

The mobility of magnetic domains forms the link between the basic physical properties of a magnetic material and its global characteristics such as permeability and saturation field. Most commonly, surface domain structure are studied using magneto-optical Kerr microscopy. The limited information depth of approx. 20 nanometers, however, allows only for an indirect interpretation of the internal volume domain structures. Here we show how accumulative high-frame rate dynamic neutron dark-field imaging is able for the first time to visualize the dynamic of the volume magnetic domain structures in grain oriented electrical steel laminations at power frequencies. In particular we studied the volume domain structures with a spatial resolution of ∼100 µm and successfully quantified domain sizes, wall velocities, domain annihilation and its duration and domain wall multiplication in real time recordings at power frequencies of 10, 25 and 50 Hz with ±262.5 A/m and ±525 A/m (peak to peak) applied field.

X-ray phase microtomography with a single grating for high-throughput investigations of biological tissue.

The high-throughput 3D visualisation of biological specimens is essential for studying diseases and developmental disorders. It requires imaging methods that deliver high-contrast, high-resolution volumetric information at short sample preparation and acquisition times. Here we show that X-ray phase-contrast tomography using a single grating can provide a powerful alternative to commonly employed techniques, such as high-resolution episcopic microscopy (HREM). We present the phase tomography of a mouse embryo in paraffin obtained with an X-ray single-grating interferometer at I13-2 Beamline at Diamond Light Source and discuss the results in comparison with HREM measurements. The excellent contrast and quantitative density information achieved non-destructively and without staining using a simple, robust setup make X-ray single-grating interferometry an optimum candidate for high-throughput imaging of biological specimens as an alternative for existing methods like HREM.

Sub-pixel correlation length neutron imaging: Spatially resolved scattering information of microstructures on a macroscopic scale.

Neutron imaging and scattering give data of significantly different nature and traditional methods leave a gap of accessible structure sizes at around 10 micrometers. Only in recent years overlap in the probed size ranges could be achieved by independent application of high resolution scattering and imaging methods, however without providing full structural information when microstructures vary on a macroscopic scale. In this study we show how quantitative neutron dark-field imaging with a novel experimental approach provides both sub-pixel resolution with respect to microscopic correlation lengths and imaging of macroscopic variations of the microstructure. Thus it provides combined information on multiple length scales. A dispersion of micrometer sized polystyrene colloids was chosen as a model system to study gravity induced crystallisation of microspheres on a macro scale, including the identification of ordered as well as unordered phases. Our results pave the way to study heterogeneous systems locally in a previously impossible manner.

Visibility simulation of realistic grating interferometers including grating geometries and energy spectra.

The performance of X-ray and neutron grating interferometers is characterised by their visibility, which is a measure for the maximum achievable contrast. In this study we show how the real grating geometry in a grating interferometer with three gratings impacts the interference and self projection that leads to visibility in the first place. We quantify the individual contributions of wavelength distributions and grating shapes in terms of visibility reduction by determining the absolute as well as relative effect of each contribution. The understanding of the impact of changed geometry and wavelength distributions on the interference of neutrons/X-rays allows us to present the first fully quantitative model of a grating interferometer setup. We demonstrate the capability of the simulation framework by building a model of the neutron grating interferometer at the ICON beamline and directly comparing simulated and measured visibility values. The general nature of the model makes it possible to extend it to any given grating interferometer for both X-rays and neutrons.

Toward clinical X-ray phase-contrast CT: demonstration of enhanced soft-tissue contrast in human specimen.

OBJECTIVES: X-ray computed tomography (CT) using phase contrast can provide images with greatly enhanced soft-tissue contrast in comparison to conventional attenuation-based CT. We report on the first scan of a human specimen recorded with a phase-contrast CT system based on an x-ray grating interferometer and a conventional x-ray tube source. Feasibility and potential applications of preclinical and clinical phase-contrast CT are discussed. MATERIALS AND METHODS: A hand of an infant was scanned ex vivo at 40 kVp tube voltage. The simultaneously recorded attenuation and phase-contrast CT images were quantitatively compared with each other, by introducing a specific Hounsfield unit for phase-contrast imaging. RESULTS: We observe significantly enhanced soft-tissue contrast in the phase images, when compared with the attenuation data. Particularly, tendons and ligaments appear with strongly increased contrast-to-noise ratio. CONCLUSIONS: Our results demonstrate the huge potential of phase-contrast CT for clinical investigations of human specimens and, potentially, of humans. Because the applied technique works efficiently with conventional x-ray tubes and detectors, it is suitable for the realization of preclinical and clinical phase-contrast CT systems.

Phase-contrast imaging and tomography at 60 keV using a conventional x-ray tube source.

Phase-contrast imaging at laboratory-based x-ray sources using grating interferometers has been developed over the last few years for x-ray energies of up to 28 keV. Here, we show first phase-contrast projection and tomographic images recorded at significantly higher x-ray energies, produced by an x-ray tube source operated at 100 kV acceleration voltage. We find our measured tomographic phase images in good agreement with tabulated data. The extension of phase-contrast imaging to this significantly higher x-ray energy opens up many applications of the technique in medicine and industrial nondestructive testing.