Negative staining TEM or cryo-TEM for liposomal powders

The following analyses are included in this nanoparticle analysis package, intended to characterize nanoforms according to the REACH Regulation. Particle size distribution and aspect ratios by SEM-EDX Preparation with isopropanol, Sample dispersion on a slide, with centrifugation, SEM analysis and particle count by image analysis, Nanoparticle detection and classification according to the 2022 EC recommendation on the definition of nanomaterial, Reporting of PSD parameters for ~300 particles, including the following: PSD diagram, accumulated and individual., Feret min (min, d10, d25, d50, d75, d90, d95, max), Feret max (min, d10, d25, d50, d75, d90, d95, max), Equivalent circular diameter (min, d10, d25, d50, d75, d90, d95, max), Aspect ratio (calculated based on individual Feret min and Feret max measurements), Number based nano-fraction (%).. Crystal phase analysis by XRD/Rietveld method Sample preparation: drying, grinding, X-ray preparation, XRD analysis over an angular range extending from 10° to 90°, Identification of the crystalline phases present in the sample, Semi-quantitative analysis of phase distribution, using the Rietveld method, Interpretation of diffractograms. Chemical composition/purity by ICP-AES and CHNS analysis ICP-AES quantification of inorganic and metallic elements: Ag, Al, As, B, Ba, Be, Bi, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, S, Se, Sb, Si, Sn, Sr, V, Zn, Ti, and Tl, Determination of C, H, N, and S with an elemental analyzer. Volume-specific surface area (VSSA) and VSSA diameter calculations (optional) BET specific surface area measurement of powder by nitrogen adsorption, True (skeletal) density measurement by He pycnometry, excluding intergranular and intragranular porosity, Both analyses include sample preparation. You can request a quote for the analysis using the form below. Please note that the OECD 125 guideline does not apply to this analysis.

Particle size distribution (PSD) is determined from transmission electron microscopy (TEM) images. The method is most suitable for small particles of 50 nm or smaller. Depending on particle shapes, the method includes calculating the diameters or lengths and widths of particles. In addition to size, TEM provides qualitative information about the surface morphology of the particles. TEM is a good option for irregularly shaped and non-spherical particles such as fibers, rods, and crystals that cannot be characterized meaningfully with traditional methods, including laser diffraction (LD) and dynamic light scattering (DLS). As a result of the analysis, TEM images and the determined particle size distribution for diameter (or length and width) are delivered. Dry samples are suitable for TEM as is. If the particles are wet or dispersed in a solvent, the sample may be dried with a suitable sample preparation method before imaging.

Imaging of the sample using scanning electron microscopy (SEM). Typically, several images are taken with varying magnifications to get a good overview of the sample. Non-conductive samples can be prepared with a metallic coating to allow imaging. For cross-section measurement, additional preparation might be needed: FIB, BIB, or freeze fracturing. Cryo preparation is available for biological materials and other sensitive sample types. If compositional analysis is also needed, please see the SEM-EDX measurement. We also offer high-temperature SEM analyses at temperatures up to 1400 °C. Do not hesitate to ask for a quote.

Determination of volume-specific surface area (VSSA) for the identification of nanoparticles. VSSA can be calculated from the specific surface area obtained by N2 adsorption and the BET method, and the effective density obtained by He Pycnometry. The measurement is a part of the EC recommendation for the definition of nanomaterials (2022/C229/01). According to the recommendation, materials with a VSSA of < 6 m2/cm3 are not considered nanomaterials.

Imaging of the sample using a scanning electron microscope (SEM) with energy-dispersive X-ray spectroscopy (EDX or EDS). Typically, several images are taken with varying magnifications to get a good overview of the sample. An EDX mapping, line scan, or point measurement is collected to measure the sample composition (elemental at.% or wt.%). Non-conductive samples can be prepared with a metallic coating. For cross-section measurement, additional preparation might be needed: FIB, BIB, or freeze fracturing.

Particle size analysis with scanning electron microscopy (SEM). The analysis is performed in conformity with the 2022 European Commission recommendation on the definition of nanomaterials (2022/C 229/01). At least 300 particles are measured, the minimum Feret diameter is chosen as the dimensional parameter, and the particle size distribution histogram is reported. By default, the following data are reported: Mean, Median (d50), Number-based nano percentage according to 2022/C 229/01 definition . Please indicate if you want any other statistics reported. These projects are priced per population of similar particles. If the qualitative SEM analysis reveals multiple populations, the price needs to be adjusted according to the number of populations to be reported. This method can be used to establish the presence of small particles including nanoparticles according to EFSA novel food guidance (Particle-TR). In this case, the following statistics are also included in the report: mean and median, 10% value of the total particles, % of the particles that are smaller than 500 nm, % of the fraction of small particles that are smaller than 250 nm. For cosmetics applications, the following statistics are provided: mean and median, 10% value of the total particles, Number-based nano percentage according to 2022/C 229/01 definition . This analysis can be coupled with XRD analysis for crystallinity information, or with VSSA analysis for specific surface area information.

Nondestructive 3D analysis of internal structures by X-ray computed tomography. The method visualizes voids, cracks, density, and phase differences within solid structures. The analysis is suitable for powdered materials, such as pharmaceutical and cosmetic ingredients, as well as bulk solids and parts, such as machine parts and wafers. The voxel size can go down to 60 nm. Please contact us for more information about the analysis options for different materials and material dimensions. Some devices available for the analysis are as follows: Bruker SkyScan 1272 CMOS, Bruker SkyScan 2214 CMOS, Zeiss Xradia 515 Versa.

The particle size distribution (PSD) and shapes of the particles are determined using image analysis. The method is suitable for particles sized 10 to 3,000 µm. Image analysis characterizes particle shapes, such as fibers, rods, and crystals, that cannot be analyzed meaningfully with traditional devices, such as laser diffraction or dynamic light scattering. Depending on the particle shapes, results typically include size distribution for length, width, and equivalent circular area (ECA) diameter.

Test of 1 bottle at 20 °C with Malvern Spraytec to characterize particle sizes between 0.1 µm and 900 µm with a standard distance between the nozzle and the laser beam. The results are reported for 3 repeat shots. Particle size distribution histograms, percent finers (Dv10, Dv50, Dv90), and % of particles smaller than 5 µm, 10 µm, and 50 µm are reported. Providing two 100% charge spray bottles per analysis is recommended for aerosols. Contact us for a quote and more information on analyses under nonstandard conditions.

Imaging of the sample with a transmission electron microscope (TEM). Typically, several images with varying magnifications are taken to get a good overview of the sample. TEM allows nm-resolution images. Solid samples often require FIB preparation before analysis. HR-TEM and cryo-TEM can also be provided. Contact us for more details.