Analysis and Characterisation

Expert precision and exceptional reactivity

Specialists in the characterisation of fine and ultra-fine powders, SDTech Micro is equipped with a dedicated laboratory and an ever-increasing range of high precision apparatus.
We can offer our clients a wide range of different analyses:

Particle size analyses using laser diffraction
Particle size analyses using dynamic light scattering (DLS)
Particle size analyses by sieving (column of sieves)
Particle shape analyses
Measurements of specific surface area (BET) and porosity
Analyses using Scanning electron microscope (SEM) & Elemental mapping using Energy Dispersive X-Ray Spectroscopy (EDS)
Thermal analyses (DSC, TGA, DTA)
Density measurements
Humidity measurements
pH measurements

For all analyses undertaken, SDTech Micro guarantees its clients a prompt response and a swift turnaround at an optimal price.

Our analyses

Particle size analysis

Further information

Particle size analysis

Particle size analysis using laser diffraction

SDTech Micro has a solid experience in the particle size analysis of fine powders.

The firm is equipped with numerous laser particle size analysers including the Malvern Mastersizer MS 3000 and MS 2000 models.
These machines allow to measure a very wide range of particle sizes from 50 nanometres to 3 millimetres (50nm – 3mm). They are equipped with various different modules:

Dry dispersion unit
Standard wet dispersion unit

An analytical protocol is established for each product depending on its physical and chemical properties and its intended use: choice of module, choice of dispersion liquid (water, oil, ethanol…), choice of surfactants and/or ultrasound… For reading and comparison of results or deconvolution of the most complex data, the expertise of SDTech Micro is at your disposal. An analysis report is provided for each procedure undertaken.
SDTech Micro is also equipped with several Insitec laser particle analysers, allowing continuous on-line control of particle size during the micronisation process. Our aim is to provide our clients with the best possible service by guaranteeing traceability throughout our procedures.
SDTech Micro can also accompany its clients on their own sits using Insitec technology to control and optimise their processes. The firm uses a fully reliable and extremely mobile Insitec Voyager to provide this service.

Particle size analysis by Scanning Electron Microscopy

To complete the particle characterisation of fine powders, SDTech can also provide a visual examination by scanning electron microscopy (SEM) coupled with statistical analysis of the images, if required.

Function

Interaction of radiation with the powder enables the production of high resolution images at nanometer scale. An electron beam scans the surface which re-emits certain particles, which are then analysed by different detectors. This allows a three-dimensional image of the surface to be reconstructed.

Specifications

Visual examination by scanning electron microscopy can confirm the sizes of the particles present in the sample and assess whether they are primary particles, aggregates or agglomerates.
The images obtained can be analysed in order to quantify the size classes and obtain a particle size distribution curve.

Nano-scale particle size analysis

SDTech Micro can also provide expertise in the field of nano-powder characterisation. To this end, the firm has invested in a Malvern Nano ZS Zetasizer.
This device enables the measurement of size and Zeta potential of nano-particles by combining 3 different techniques:

Dynamic light scattering to measure particle and molecule size
Electrophoretic light scattering to measure Zeta potential
Static light scattering to determine the molar mass of proteins and polymers.

Using this device, SDTech Micro is able to measure sizes ranging from 0.3nm to 10µm in diameter.

Particle shape analysis

Further information

Particle shape analysis

The Morphologi G3, an automated particle characterisation system.

SDTech Micro is equipped with a Morphologi G3, an advanced particle characterisation system for measuring the size and shape of particles measuring 0.5 microns to several millimetres. This single instrument provides the necessary flexibility for R&D and problem diagnosis as well as user independent results and the validation required for automated QC analysis (Quality Control). This technique is frequently used in conjunction with laser particle analysis for a better understanding of the product or process behaviour.

Function

The Morphologi G3 measures particle size and shape via static image analysis. There are 3 main stages in the measurement process:

Preparation and dispersion of the sample

This step is critical for obtaining good results. The aim is to achieve the physical separation of individual particles and agglomerates. The Morphologi G3 has an integrated dry powder dispersion system, which renders dry powder sample preparation simple and repeatable. A range of accessories are also available enabling samples to be prepared in the form of liquid suspensions or on membrane filters.

Image capture

The instrument captures images of individual particles by passing the sample under the microscope lenses while maintaining the focus on the particles. The Morphologi G3 is able to cast a very precise amount of light on the sample from above or from below. Polarising filters can also be used in order to study birefringent materials.

Data Analysis

The instrument measures a wide range of morphological parameters for each particle. The software’s advanced graphical representation and data classification options enable relevant data extraction from all your measurement data through an intuitive visual interface which is as simple as possible. The grayscale images are stored individually for each particle, in order to allow qualitative verification of quantitative results.

Specifications

Particle size

Measuring range: 0.5 µm to 10 mm (depending on the sample)
Measuring principle: Static image analysis
Size parameters: CE diameter (circle equivalent), length, width, perimeter, surface area, maximum distance, SE Volume

Particle shape

Measuring range: 0.5 µm to 10 mm (depending on the sample)
Measuring principle: Static image analysis
Shape parameters: Aspect ratio, circularity, convexity, elongation, HS circularity, solidity, average intensity, standard deviation of intensity

Time-frame for analysis results

SDTech Micro is committed to completing your Morpho G3 analyses within 48-72 hours following receipt of your samples.

Scanning Electron Microscopy, a visual examination of particles

SDTech can provide scanning electron microscopy (SEM) analysis in order to visually examine the morphology of very fine powders (<1 µm).

Function

A three-dimensional image of the surface is reconstructed by analysing the secondary electrons emitted during the interaction of an electron beam with the matter.
Chemical microanalysis can also be performed using an energy dispersive x-ray probe (EDS). The impact of the electron beam on the sample produces X-rays which are characteristic of the elements present.

Specifications

A visual examination using scanning electron microscopy enables us to study the shape of very fine particles (<1 µm) present in the sample.
Surface defects and asperities, cracks and images after cutting of materials can also be studied.
Qualitative elemental analysis allows the detection of the elements of the periodic table starting from carbon.

Time-frame for analysis results

This type of analysis requires 1 to 2 weeks.

Thermal analysis

Further information

Thermal analysis

Differential Scanning Calorimetry (DSC)

SDTech is equipped with Differential Scanning Calorimetry (DSC). This technique is used to study the thermal transitions of a given material (fusion, crystallisation, melting point, glass transition temperature, degradation etc).

Function

The measurement involves determining the variation in heat flux emitted or received by a given sample when subjected to changes in temperature. During the heating or cooling process, any change in a material is accompanied by an endothermic or exothermic heat exchange. The DSC is able to pinpoint the temperature at which the changes take place and provide qualitative and quantitative information about these reactions.

Specifications

With DSC the following thermal reactions can be observed:

Glass transition point
Evaporation
Melting
Enthalpy relaxation
Crystallisation
Decomposition

Thermogravimetric analysis (TGA)

Thermogravimetric Analysis (TGA) measures the changes in mass of a sample as it is heated.
This technique is mainly used to characterize materials according to their composition.
It gives access to the mass composition of a mixture and to its thermal stability.
Its fields of application include thermoplastic materials, elastomers, thermosets, metals, ceramics, but also various cosmetic, food or pharmaceutical formulations…

Differential Thermal Analysis (DTA)

Complementary to DSC, Differential Thermal Analysis (DTA) allows the study of weak transitions at high temperatures (up to 1100°C).

Information on the thermal behaviour of the powder is obtained by following the evolution of the temperature difference between the sample studied and a reference sample.
The samples are placed in an enclosure subjected to a predefined programme of temperatures (heating or cooling). This enables us to obtain a differential thermal curve based on the change in the chemical composition or the crystal structure of the sample.

SDTech Micro is committed to completing your TGA analyses within 48 hours following receipt of your samples.
DSC and DTA analyses require 7 to 10 days.

Surface analysis

Further information

Surface analysis

The BET method provides better understanding of particle surface.

SDTech Micro provides its customers with expertise in the study of powder surface and in particular via :

Measurement of the specific surface area of particles
Evaluation of porosity (pore volume, pore size distribution).

SDTech Micro has a Micromeritics 3Flex Surface Characterization Analyzer for this purpose.

Function

This equipment measures the adsorption and desorption of an inert gas (e.g. nitrogen) on porous particles. The isotherm obtained enables the calculation of various parameters which characterise the surface of a powder:
Starting from the volume of gas forming a monomolecular layer on the surface of the particles, the device calculates the specific surface area of a sample. The volume of the pores can be calculated via capillary condensation.
This data makes it possible to evaluate the surface condition of a powder and to understand its behaviour. Physical and chemical properties such as solubility, adsorption, reactivity, formability and formulation in various dosage forms are all dependent on surface properties.

Specifications

The measurement of the specific surface area makes it possible to evaluate the entire surface available for interactions with other molecules.
The higher the specific surface area, the more the powder interacts with its environment and the more reactive it is.
The size distribution of the pores influences the rate at which molecules can penetrate the interior of the pores, the rate of adsorption and desorption and, therefore, the reactivity.