Neutron Backscattering Research Articles

Accessing self-diffusion on nanosecond time and nanometre length scales with minute kinetic resolution.

Neutron spectroscopy uniquely and non-destructively accesses diffusive dynamics in soft and biological matter, including for instance proteins in hydrated powders or in solution, and more generally dynamic properties of condensed matter on the molecular level. Given the limited neutron flux resulting in long counting times, it is important to optimize data acquisition for the specific question, in particular for time-resolved (kinetic) studies. The required acquisition time was recently significantly reduced by measurements of discrete energy transfers rather than quasi-continuous neutron scattering spectra on neutron backscattering spectrometers. Besides this reduction in acquisition times, smaller amounts of samples can be measured with better statistics, and most importantly, kinetically changing samples, such as aggregating or crystallizing samples, can be followed. However, given the small number of discrete energy transfers probed in this mode, established analysis frameworks for full spectra can break down. Presented here are new approaches to analyze measurements of diffusive dynamics recorded within fixed windows in energy transfer, and these are compared with the analysis of full spectra. The new approaches are tested by both modeled scattering functions and a comparative analysis of fixed energy window data and full spectra on well understood reference samples. This new approach can be employed successfully for kinetic studies of the dynamics focusing on the short-time apparent center-of-mass diffusion.

Quasielastic neutron scattering study on low-hydrated myoglobin inside silica nanopores

In this study, nanosecond-scale dynamics of low-hydrated myoglobin (Mb) encapsulated in mesoporous silica (MPS) with 7.8 nm pores was investigated by using high resolution (energy resolution: 1 μeV) neutron backscattering spectroscopy. The apparent hydration level of the encapsulated myoglobin was 0.06, which was deduced by assuming a uniform distribution of water within myoglobin encapsulated mesoporous silica. The mean square displacement of myoglobin derived from an elastic fixed-window scan was essentially proportional to temperature in the range 120–300 K, indicating the absence of dynamical transition induced by the onset of translational diffusion in the hydration D2O. Since the width of quasielastic neutron scattering (QENS) peaks of the encapsulated Mb was Q-independent at 220, 240, and 265 K, the observed nanosecond-scale dynamics was attributed to internal motions of the encapsulated Mb, such as slow motions of amino acid groups or side chains. The fraction of immobile H-atoms in Mb was estimated to be above 0.8, which was larger than that for a free protein with a similar molecular weight to Mb. The large immobile fraction indicates that the nanosecond-scale motions of amino acid residues and side chains in the vicinity of the pore wall are restricted by the interfacial interactions with the rigid pore wall.

Characterization of heterogeneities in the sandy facies of the Opalinus Clay (Mont Terri underground rock laboratory, Switzerland)

SUMMARY This contribution is presenting a multidisciplinary investigation of heterogeneities in a clay rock formation, based on seismic tomography, logging and core analysis, as a reconnaissance study for a diffusion experiment. Diffusion experiments in clay rock formations provide crucial experimental data on diffusive transport of radionuclides (RN) in extremely low hydraulic conductivity media. Previous diffusion experiments, conducted, for example, in the Mont Terri underground rock laboratory within the relatively homogeneous shaly facies of Opalinus Clay, and modelling studies of these experiments have demonstrated that the clay rock could sufficiently well be described as a homogeneous anisotropic medium. For other lithofacies, characterized by larger heterogeneity, such simplification may be unsuitable, and the description of heterogeneity over a range of scales will be important. The sandy facies of the Opalinus Clay exhibits a significantly more pronounced heterogeneity compared to the shaly facies, and a combined characterization and RN diffusion study has been initiated to investigate various approaches of heterogeneity characterization and subsequent diffusion in a heterogeneous environment. As an initial step, two inclined exploratory boreholes have been drilled to access the margins of the experiment location. These boreholes have been used to acquire a cross-hole tomographic seismic data set. Optical, natural gamma and backscattering logging were applied and rock cores were analysed. The integrated results of these investigations allowed the identification of an anomalous brighter layer within the investigated area of the sandy facies of approximately 1 m thickness and with its upper bound at roughly 10 m depth within the inclined exploratory wells. Mineralogical analyses revealed only slight variations throughout the rock cores and indicated that the anomalous layer exhibited a slightly higher quartz content, and locally significantly higher calcite contents, accompanied by a lower content of clay minerals. The anomalous layer was characterized by reduced natural gamma emissions, due to the lower clay content, and increased neutron backscattering likely indicating an increased porosity. Seismic P-wave velocities, derived from anisotropic tomography, exhibited a maximal gradient near the top of this layer. The transition from the overlaying darker rock matrix into this layer has been identified as an appropriate location for the setup of a tracer diffusion experiment in a heterogeneous environment.

Microscopic molecular mobility of high-performance polymers of intrinsic microporosity revealed by neutron scattering - bend fluctuations and signature of methyl group rotation.

Polymers of intrinsic microporosity exhibit a combination of high gas permeability and reasonable permselectivity, which makes them attractive candidates for gas separation membrane materials. The diffusional selective gas transport properties are connected to the molecular mobility of these polymers in the condensed state. Incoherent quasielastic neutron scattering was carried out on two polymers of intrinsic microporosity, PIM-EA-TB(CH3) and its demethylated counterpart PIM-EA-TB(H2), which have high Brunauer-Emmett-Teller surface area values of 1030 m2 g-1 and 836 m2 g-1, respectively. As these two polymers only differ in the presence of two methyl groups at the ethanoanthracene unit, the effect of methyl group rotation can be investigated solely. To cover a broad dynamic range, neutron time-of-flight was combined with neutron backscattering. The demethylated PIM-EA-TB(H2) exhibits a relaxation process with a weak intensity at short times. As the backbone is rigid and stiff this process was assigned to bend-and-flex fluctuations. This process was also observed for the PIM-EA-TB(CH3). A further relaxation process is found for PIM-EA-TB(CH3), which is the methyl group rotation. It was analyzed by a jump-diffusion in a three-fold potential considering also the fact that only a fraction of the present hydrogens in PIM-EA-TB(CH3) participate in the methyl group rotation. This analysis can quantitatively describe the q dependence of the elastic incoherent structure factor. Furthermore, a relaxation time for the methyl group rotation can be extracted. A high activation energy of 35 kJ mol-1 was deduced. This high activation energy evidences a strong hindrance of the methyl group rotation in the bridged PIM-EA-TB(CH3) structure.

Backscattering silicon spectrometer (BASIS): sixteen years in advanced materials characterization.

Quasielastic neutron scattering (QENS) is an experimental technique that can measure parameters of mobility, such as diffusion jump rate and jump length, as well as localized relaxations of chemical species (molecules, ions, and segments) at atomic and nanometer length scales. Due to the high penetrative power of neutrons and their sensitivity to neutron scattering cross-section of chemical species, QENS can effectively probe mobility inside most bulk materials. This review focuses on QENS experiments performed using a neutron backscattering silicon spectrometer (BASIS) to explore the dynamics in various materials and understand their structure-property relationship. BASIS is a time-of-flight near-backscattering inverted geometry spectrometer with very high energy resolution (approximately 0.0035 meV of full width at half maximum), allowing measurements of dynamics on nano to picosecond timescales. The science areas studied with BASIS are diverse, with a focus on soft matter topics, including traditional biological and polymer science experiments, as well as measurements of fluids ranging from simple hydrocarbons and aqueous solutions to relatively complex room-temperature ionic liquids and deep-eutectic solvents, either in the bulk state or confined. Additionally, hydrogen confined in various materials is routinely measured on BASIS. Other topics successfully investigated at BASIS include quantum fluids, spin glasses, and magnetism. BASIS has been in the user program since 2007 at the Spallation Neutron Source of the Oak Ridge National Laboratory, an Office of Science User Facility supported by the U.S. Department of Energy. Over the past sixteen years, BASIS has contributed to various scientific disciplines, exploring the structure and dynamics of many chemical species and their fabrication for practical applications. A comprehensive review of BASIS contributions and capabilities would be an asset to the materials science community, providing insights into employing the neutron backscattering technique for advanced materials characterization.

A dose calculation algorithm for boron neutron capture therapy using convolution/superposition method

The convolution/superposition (C/S) method originally designed for photon dose calculation was first applied for developing a treatment planning system for boron neutron capture therapy. The original concept of TEGMA (total energy generated per unit mass) was proposed to represent distinctive dose components from neutron reactions with the elements in the patient's tissue. First, neutron fluence distributions in a homogeneous brain phantom irradiated with an energy-groupwise pencil beam of 2.5 × 2.5 mm2 were calculated using the MCNP6.2 code. Then, a library of energy-groupwise TEGMA and KERMA were generated and stored in the developed C/S code. As a benchmark, dose distributions in a cuboid phantom and a human head phantom were calculated using the developed C/S and PHITS Monte Carlo codes. A neutron beam having a continuous epithermal spectrum and a square field of 22.5 × 22.5 mm2 or a circle field of 22.5 mm in diameter was assumed to be incident on the phantoms. The human head phantom was created by the pre-processing including the voxelization and transformation of test DICOM CT images. The differences in boron doses between C/S and MC ranged from 2% to 6%. In nitrogen doses, the differences were from 4% to 9%. A large discrepancy observed in hydrogen lateral dose profiles could be explained by the differences in cross-section data and recoil-proton transport algorithms of MCNP6.2 and PHITS. With isodose curves normalized at the center of the tumor in the human head phantom, they were almost identical in the range of 60%–110% for both cases. The C/S have underestimated the backscattering neutron and showed a larger absorbed dose gradient around 40% region. The calculation time of C/S using Intel i7-10700 processor was less than 1 min for both phantoms. The calculation time of PHITS using three Intel Xeon E5-2640 v4 processors was 15.5 min for the cuboid phantom and ∼380 min for the human head phantom. The proposed algorithm has the advantages of high speed while promising fair accuracy in BNCT dose calculations.

Sludge interface measurement in the storage tank utilizing neutron backscattering technique: A field experiment

Modern industrial plant operations commonly necessitate a measurement system of the liquids level interface in the oil storage tank. Various advanced-level indicators almost meet the demand, but these may not be in online condition and are less accurate due to sedimentation in the bottom tank. Sedimentation or sludge known as a petroleum hydrocarbons complex emulsion, contained water and solid particles generated during distribution, storage, or even production. The neutron backscatter technique can help the maintenance system of the tank or vessel by measuring sludge levels from outside the wall. This paper presents a non-intrusive method for identifying the interface between two materials in the crude oil storage system. A fast neutron source (241Am–Be) with activity 1 Ci (Ci) and a portable backscattering neutron detector are used for storage tank measurement. The storage tank has an outer diameter (OD) of 34 m and a height of 11 m. Time measurement is 2 s for each position, starting from 0 m to 11 m. The slow neutron intensity can be correlated to the hydrogen concentration inside chemical compounds. The interface between sludge and oil is identified at 27 cm from the bottom plate. The method has the potential for non-destructive measurement of sludge in a refinery facility.

Domain-induced dynamics in phase-separating lipid membranes.

Lipid membranes have a significant role in cells, not only defining the boundaries of cells and cell organelles but also playing an active role in cell functions, including the partitioning of proteins and the spatiotemporal regulation of signaling clusters. This is facilitated by the rich lipid diversity in cell membranes, which often results in unideal mixing and subsequent lipid phase-separation into lateral compositional heterogeneities or domains. Over the past few decades, structural measurements on such membranes have shed important light on the molecular mechanisms underlying domain formation. However, major information gaps still exist in our understanding of how domain formation affects the dynamics of lipid membranes, whether in the form of collective fluctuations or molecular motions. To address this outstanding question, we use neutron spectroscopy and molecular dynamics (MD) simulations that can selectively investigate the matrix dynamics in domain-forming membranes. Specifically, our studies are performed on binary mixtures of 1,2-dimyristoyl-sn-glycero-3-phosphocholine (DMPC) and deuterated 1,2-distearoyl-sn-glycero-3-phosphocholine (DSPC). Experimental results, obtained by neutron spin-echo spectroscopy and neutron backscattering spectroscopy, show that the formation and growth of rigid DSPC domains causes an effective slowdown in the bending fluctuations and diffusional dynamics of the otherwise fluid DMPC matrix. MD simulations on cognate bilayers suggest that the measured changes in the matrix dynamics are mediated by interfacial DMPC lipids that experience constrained diffusional jumps and longer residence times at the domain boundaries. Our findings present striking evidence of dynamic coupling between lipid domains and their surrounding lipid environment. More importantly, this interplay occurs on the nanosecond time scales of protein conformational changes and signaling events. Put together, the results suggest an intriguing mechanism by which domain formation can play a regulatory role in functional membrane processes.

Study of water intrusion in admixture concrete using neutron backscattering technique

This work aims to study the water infiltration in ordinary concrete with different percentages of super-plasticizer (SP) varied from 0.25% to 1.5% of cement weight. It was performed by measuring thermal neutrons backscattered from the investigated samples. Dynamic measurements were carried out by fixing the sample on a transfer table in front of the neutron beam exit. A slit collimated beam of neutrons emitted from 252Cf was hit on which surface of the sample water did not infiltrate through it and along the flow direction.Further, static measurements were made using collimated neutron beams of thermal and fast neutrons emitted from sources of 252Cf and Pu-Be with strength of 1.3 × 107 and 5 × 106 n/s respectively. These beams of neutron incident on the other side of sample which water allowed infiltrating for 7, 14, 21, 28, and 35 days. The backscattered thermal neutrons were measured by BF3 detector which fixed on the same side of the incident neutron beam. The obtained results show clearly the dependence of water infiltration on the percentages of SP and the submerged time. As well as, the measuring sensitivity depends on the main energy of the incident neutrons, submerged time, and SP% was given and discussed. The results indicated that samples with SP below 1.5% show an improvement in resistivity to water infiltration and therefore prolong the concrete durability for marine constructions. The best percentage of SP is 1%, for more percentages, there is a negative effect on the permeability and diffusivity. As well as, the obtained results indicated that, NBS is a powerful, nondestructive, and fast method to observe water infiltration in porous materials. In addition, these results lead to improve concrete properties to prevent fluid intrusion. Further investigation should be done with different recycled additives to achieving the optimization between waste reuse and engineering properties of porous concrete.

A Molecular Description of Hydrogel Forming Polymers for Cement-Based Printing Paste Applications

This research endeavors to link the physical and chemical characteristics of select polymer hydrogels to differences in printability when used as printing aids in cement-based printing pastes. A variety of experimental probes including differential scanning calorimetry (DSC), NMR-diffusion ordered spectroscopy (DOSY), quasi-elastic neutron scattering (QENS) using neutron backscattering spectroscopy, and X-ray powder diffraction (XRD), along with molecular dynamic simulations, were used. Conjectures based on objective measures of printability and physical and chemical-molecular characteristics of the polymer gels are emerging that should help target printing aid selection and design, and mix formulation. Molecular simulations were shown to link higher hydrogen bond probability and larger radius of gyration to higher viscosity gels. Furthermore, the higher viscosity gels also produced higher elastic properties, as measured by neutron backscattering spectroscopy.

Neutron backscatter edges as a diagnostic of burn propagation

High gain in hotspot-ignition inertial confinement fusion (ICF) implosions requires the propagation of thermonuclear burn from a central hotspot to the surrounding cold dense fuel. As ICF experiments enter the burning plasma regime, diagnostic signatures of burn propagation must be identified. In previous work [A. J. Crilly et al., Phys. Plasmas 27(1), 012701 (2020)], it has been shown that the spectral shape of the neutron backscatter edges is sensitive to the dense fuel hydrodynamic conditions. The backscatter edges are prominent features in the ICF neutron spectrum produced by the 180° scattering of primary deuterium–tritium fusion neutrons from ions. In this work, synthetic neutron spectra from radiation-hydrodynamics simulations of burning ICF implosions are used to assess the backscatter edge analysis in a propagating burn regime. Significant changes to the edge's spectral shape are observed as the degree of burn increases, and a simplified analysis is developed to infer scatter-averaged fluid velocity and temperature. The backscatter analysis offers direct measurement of the increased dense fuel temperatures that result from burn propagation.

Data Collection for Dilute Protein Solutions via a Neutron Backscattering Spectrometer

Understanding protein functions requires not only static but also dynamic structural information. Incoherent quasi-elastic neutron scattering (QENS), which utilizes the highly incoherent scattering ability of hydrogen, is a powerful technique for revealing the dynamics of proteins in deuterium oxide (D2O) buffer solutions. The background scattering of sample cells suitable for aqueous protein solution samples, conducted with a neutron backscattering spectrometer, was evaluated. It was found that the scattering intensity of an aluminum sample cell coated with boehmite using D2O was lower than that of a sample cell coated with regular water (H2O). The D2O-Boehmite coated cell was used for the QENS measurement of a 0.8 wt.% aqueous solution of an intrinsically disordered protein in an intrinsically disordered region of a helicase-associated endonuclease for a fork-structured type of DNA. The cell was inert against aqueous samples at 283–363 K. In addition, meticulous attention to cells with small individual weight differences and the positional reproducibility of the sample cell relative to the spectrometer neutron beam position enabled the accurate subtraction of the scattering profiles of the D2O buffer and the sample container. Consequently, high-quality information on protein dynamics could be extracted from dilute protein solutions.

Assessing the environmental risk posed by a legacy tanker wreck: a case study of the RFA War Mehtar

The ocean floor is littered with thousands of wrecks containing hazardous fuels, lubes, armaments and cargoes that have polluted, are polluting, or will pollute the marine environment. The UK Ministry of Defence manages the environmental risk associated with its ∼5,700 military wrecks through the Wreck Management Programme. This paper explores the methods used to assess the environmental risk associated with the wreck of the Royal Fleet Auxiliary (RFA) tanker RFA War Mehtar, which lies at approximately 39 m depth, 15 nm east of Great Yarmouth, United Kingdom. The methods employed include archival research, computational oil spill modelling combined with sensitivity mapping, environmental sampling and hydrocarbon concentration analysis, multibeam echosounder sonar surveys and neutron backscatter probe measurements. Each method is described, and its efficacy discussed. The archival research was essential to determine what fuel and cargo the RFA War Mehtar sank with; but only when high-resolution multibeam sonar images were combined with the ship’s plans and neutron backscatter measurements from individual tanks could one confidently conclude that the wreck does not pose a significant pollution risk.

High-resolution Neutron Spectroscopy to Study Picosecond-nanosecond Dynamics of Proteins and Hydration Water.

Neutron scattering offers the possibility to probe the dynamics within samples for a wide range of energies in a nondestructive manner and without labeling other than deuterium. In particular, neutron backscattering spectroscopy records the scattering signals at multiple scattering angles simultaneously and is well suited to study the dynamics of biological systems on the ps-ns timescale. By employing D2O-and possibly deuterated buffer components-the method allows monitoring of both center-of-mass diffusion and backbone and side-chain motions (internal dynamics) of proteins in liquid state. Additionally, hydration water dynamics can be studied by employing powders of perdeuterated proteins hydrated with H2O. This paper presents the workflow employed on the instrument IN16B at the Institut Laue-Langevin (ILL) to investigate protein and hydration water dynamics. The preparation of solution samples and hydrated protein powder samples using vapor exchange is explained. The data analysis procedure for both protein and hydration water dynamics is described for different types of datasets (quasielastic spectra or fixed-window scans) that can be obtained on a neutron backscattering spectrometer. The method is illustrated with two studies involving amyloid proteins. The aggregation of lysozyme into µm sized spherical aggregates-denoted particulates-is shown to occur in a one-step process on the space and time range probed on IN16B, while the internal dynamics remains unchanged. Further, the dynamics of hydration water of tau was studied on hydrated powders of perdeuterated protein. It is shown that translational motions of water are activated upon the formation of amyloid fibers. Finally, critical steps in the protocol are discussed as to how neutron scattering is positioned regarding the study of dynamics with respect to other experimental biophysical methods.

Evolution of texture in Alloy 80A during initial ingot breakdown

Abstract This paper presents details on the evolution of texture in Alloy 80A during the initial ingot break-down process by means of repeated hot-working (cogging). The ingot was produced by vacuum arc re-melting showing equiaxed and columnar grains. Compression tests were performed with a Gleeble system covering the range of temperatures, strains, and strain rates experienced during processing on an industrial scale. Texture analysis (neutron and electron backscatter diffraction) was applied to all specimens before and after hot deformation to reflect the thermo-mechanical history. The ingot exhibited a well pronounced <100>-fiber texture of the initial microstructure. Low deformation ratios did not change the type of texture, but the degree of the preferred orientation. High strains partially result in the destruction of the fiber texture and lead to the appearance of additional texture components, such as cube- and Goss-components. With continued deformation, recovery and recrystallization become predominant.

Comparative optimization of Be/Zr(BH4)4 and Be/Be(BH4)2 as 252Cf source shielding assemblies: Effect on landmine detection by neutron backscattering technique

Monte Carlo simulations were used to model a portable Neutron backscattering (NBT) sensor suitable for detecting plastic anti-personnel mines (APMs) buried in dry and moist soils. The model consists of a 100 MBq 252Cf source encapsulated in a neutron reflector/shield assembly and centered between two 3He detectors. Multi-parameter optimization was performed to investigate the efficiency of Be/Zr(BH4)4 and Be/Be(BH4)2 assemblies in terms of increasing the signal-to-background (S/B) ratio and reducing the total dose equivalent rate. The MCNP results showed that 2 cm Be/3 cm Zr(BH4)4 and 2 cm Be/3 cm Be(BH4)2 are the optimal configurations. However, due to portability requirements and abundance of Be, the 252Cf-2 cm Be/3 cm Be(BH4)2 NBT model was selected to scan the center of APM buried 3 cm deep in dry and moist soils. The selected NBT model has positively identified the APM with a S/B ratio of 886 for dry soils of 1 wt% hydrogen content and with S/B ratios of 615, 398, 86, and 12 for the moist soils containing 4, 6, 10, and 14 wt% hydrogen, respectively. The total dose equivalent rate reached 0.0031 mSv/h, suggesting a work load of 8 h/day for 806 days within the permissible annual dose limit of 20 mSv.

Influence of molecular weight on the distribution of segmental relaxation in polymer grafted nanoparticles

The segmental dynamics of one-component nanocomposites (OCNC) is significantly influenced by the molecular weight $({M}_{w})$ of the grafted polymer. Neutron backscattering shows that compared to the neat polymer the OCNCs exhibit a shift from slower segmental dynamics at low ${M}_{w}$ to faster dynamics at high ${M}_{w}$. We model the local relaxation as distribution of exponential diffusers. This approach reveals the presence of fast and slow segments in both OCNCs. However, their fractional contribution varies with ${M}_{w}$ leading to different average relaxation times. Our results present important insights into the origin of segmental mobility in OCNC and address the inconsistencies in different literature reports.

Conceptual design of a radial collimator for MIRACLES, the time-of-flight backscattering spectrometer at the European Spallation Source

A parametrized conceptual design for a radial collimator in a neutron backscattering instrument is presented, with application to the characteristic geometry of the MIRACLES spectrometer, that will be constructed at the European Spallation Source (ESS). The analytic development of this design has considered both the forward scattering (sample-analyzer) and backscattering (analyzer-detectors) pathways. All the characteristic dimensions (internal and external radii, slit angle) and figures of merit (such as transmission and estimated background reduction) of the device are calculated as a function of the focal points. Finally, the estimated performance of the final concept has been validated by Monte Carlo simulations.

Recent Progress on DNA ToF Backscattering Spectrometer in MLF, J-PARC

DNA is a time-of-flight backscattering neutron spectrometer installed at the Materials and Life Science Experimental Facility in J-PARC. After opening user program, we have been developing and upgrading DNA. The energy resolution is improved and achieved the designed value of 1.4 μeV by renewing the disks of the pulse shaping chopper that can rotate at max 300 Hz instead of 225 Hz of the previous disks. The installation of Si311 analyser mirrors has been almost accomplished, which extends momentum transfer region up to 3.7 Å-1. We demonstrate the effect of this extension by measuring and analysing methyl rotation dynamics in solid toluene at 10 K and 40 K. We also report variety of sample environment available at DNA and their remote handling.

A sample holder for simultaneous neutron and dielectric spectroscopy – dielectric tests with glycerol, glycerol-water, water and phosphoric acid

We report on dielectric test measurements of a rectangular flat sample holder which serves as capacitor and which is aimed for simultaneous neutron and dielectric (n-DE) spectroscopy of acidic liquid samples. We describe technical details of the sample holder assembly and the dielectric and neutron equipment as well as the sample preparation procedure of the air sensitive acidic samples. The sample holder was characterised off-line from the neutron spectrometer by dielectric spectroscopy, but using the standard IN16B cryofurnace with a dielectric sample stick with 4-wire connection and a Novocontrol equipment, previously setup by a collaborative effort between ILL and Roskilde University. Temperature-dependent dielectric scans on standard samples (glycerol, glycerol-water, and Milli-Q water) were measured in the frequency range between 0.27 Hz and 1 MHz. Step-like temperature changes allowed to probe the temperature equilibrium conditions and continuous temperature changes were made to mimic typical IN16B backscattering neutron fixed window scans. Both type of scans were carried out in cooling and in heating. The standard samples show that our dielectric setup with flat sample holder is well suited for simultaneous n-DE-experiments. On the other hand, the dielectric scan on phosphoric acid reveals the limitations of our setup in case of high sample conductivities, but also shows that the DC-conductivity can still be accessed in a sufficiently wide low temperature range where the onset of conductivity can be simultaneously probed with the change in proton dynamics as seen by neutron spectroscopy.