| 1. |
- Minelli, Caterina, et al.
(författare)
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Versailles project on advanced materials and standards (VAMAS) interlaboratory study on measuring the number concentration of colloidal gold nanoparticles
- 2022
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Ingår i: Nanoscale. - : Royal Society of Chemistry (RSC). - 2040-3372 .- 2040-3364. ; 14, s. 4690-4704
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Tidskriftsartikel (refereegranskat)abstract
- We describe the outcome of a large international interlaboratory study of the measurement of particle number concentration of colloidal nanoparticles, project 10 of the technical working area 34, "Nanoparticle Populations" of the Versailles Project on Advanced Materials and Standards (VAMAS). A total of 50 laboratories delivered results for the number concentration of 30 nm gold colloidal nanoparticles measured using particle tracking analysis (PTA), single particle inductively coupled plasma mass spectrometry (spICP-MS), ultraviolet-visible (UV-Vis) light spectroscopy, centrifugal liquid sedimentation (CLS) and small angle X-ray scattering (SAXS). The study provides quantitative data to evaluate the repeatability of these methods and their reproducibility in the measurement of number concentration of model nanoparticle systems following a common measurement protocol. We find that the population-averaging methods of SAXS, CLS and UV-Vis have high measurement repeatability and reproducibility, with between-labs variability of 2.6%, 11% and 1.4% respectively. However, results may be significantly biased for reasons including inaccurate material properties whose values are used to compute the number concentration. Particle-counting method results are less reproducibile than population-averaging methods, with measured between-labs variability of 68% and 46% for PTA and spICP-MS respectively. This study provides the stakeholder community with important comparative data to underpin measurement reproducibility and method validation for number concentration of nanoparticles.
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| 2. |
- Eberbeck, D., et al.
(författare)
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Magneto-structural characterization of different kinds of magnetic nanoparticles
- 2023
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Ingår i: Journal of Magnetism and Magnetic Materials. - 0304-8853. ; 583
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Tidskriftsartikel (refereegranskat)abstract
- Using well-established measurement techniques like transmission electron microscopy (TEM), dynamic light scattering (DLS), small and wide angle X-ray scattering (SAXS, WAXS), susceptometry, and magnetorelaxometry, the distribution of the physical and magnetic size (magnetic moments) and magnetic anisotropy of a variety of structurally different magnetic nanoparticle samples (MNPs) is analyzed and compared. A term which accounts for the presence of weak magnetic areas (WMAs) within the MNPs was introduced to the widespread analysis model for M(H) data, enabling a consistent interpretation of the data in most of the systems. A comparison of the size distributions as obtained for the physical and the magnetic diameter suggests a multidomain structure for three single core systems under investigation, in all probability evoked by the presence of a wustite phase, as identified by WAXS. Analyzing the relationship d < dm < dc between the average single core diameter d, the effective magnetic (domain) size dm and the cluster diameter dc quantitatively, two qualitatively different magnetic structures in multicore MNP (MCMNP) systems were identified: (i) The magnetic moments of single cores within the MCMNP of fluidMAG tend to build flux closure structures, driven by dipole–dipole interaction. (ii) The magnetic behavior of Resovist® was attributed to the presence of domain sizes of about 12 nm within MCMNP, exceeding the single core diameters of 5 nm. Thereby, WAXS revealed a bimodal crystallite size distribution suggesting a crystallite merging process within the MCMNP. The value of the effective magnetic moment of these MCMNP could be explained within the presented “random moment cluster model” (RMCM). We conclude that the combination of physical and magnetic structure parameters obtained from complementary measurement methods allows a reliable assessment of the magnetic structure of single and multicore MNPs.
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| 3. |
- Nass, Karol, et al.
(författare)
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Indications of radiation damage in ferredoxin microcrystals using high-intensity X-FEL beams
- 2015
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Ingår i: Journal of Synchrotron Radiation. - 0909-0495 .- 1600-5775. ; 22:2, s. 225-238
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Tidskriftsartikel (refereegranskat)abstract
- Proteins that contain metal cofactors are expected to be highly radiation sensitive since the degree of X-ray absorption correlates with the presence of high-atomic-number elements and X-ray energy. To explore the effects of local damage in serial femtosecond crystallography (SFX), Clostridium ferredoxin was used as a model system. The protein contains two [4Fe–4S] clusters that serve as sensitive probes for radiation-induced electronic and structural changes. High-dose room-temperature SFX datasets were collected at the Linac Coherent Light Source of ferredoxin microcrystals. Difference electron density maps calculated from high-dose SFX and synchrotron data show peaks at the iron positions of the clusters, indicative of decrease of atomic scattering factors due to ionization. The electron density of the two [4Fe–4S] clusters differs in the FEL data, but not in the synchrotron data. Since the clusters differ in their detailed architecture, this observation is suggestive of an influence of the molecular bonding and geometry on the atomic displacement dynamics following initial photoionization. The experiments are complemented by plasma code calculations.
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| 4. |
- Schavkan, Alexander, et al.
(författare)
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Number concentration of gold nanoparticles in suspension : SAXS and spICPMS as traceable methods compared to laboratory methods
- 2019
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Ingår i: Nanomaterials. - : MDPI AG. - 2079-4991. ; 9:4
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Tidskriftsartikel (refereegranskat)abstract
- The industrial exploitation of high value nanoparticles is in need of robust measurement methods to increase the control over product manufacturing and to implement quality assurance. InNanoPart, a European metrology project responded to these needs by developing methods for the measurement of particle size, concentration, agglomeration, surface chemistry and shell thickness. This paper illustrates the advancements this project produced for the traceable measurement of nanoparticle number concentration in liquids through small angle X-ray scattering (SAXS) and single particle inductively coupled plasma mass spectrometry (spICPMS). It also details the validation of a range of laboratory methods, including particle tracking analysis (PTA), dynamic light scattering (DLS), differential centrifugal sedimentation (DCS), ultraviolet visible spectroscopy (UV-vis) and electrospray-differential mobility analysis with a condensation particle counter (ES-DMA-CPC). We used a set of spherical gold nanoparticles with nominal diameters between 10 nm and 100 nm and discuss the results from the various techniques along with the associated uncertainty budgets.
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