Sympatec GmbH

Laser Diffraction | Particle Size and Particle Size Distribution from below 0.1 µm to 8,750 µm

The proven HELOS laser diffraction series – with its classical parallel beam laser diffraction set-up – offers a powerful technology for reliable particle size distribution analysis of powders, granules, suspensions, emulsions, sprays and numerous other particulate systems. A size range from below 0.1 µm to 8,750 µm is mastered.

In the early 1980s, Sympatec introduced a breakthrough innovation which was leading laser diffraction to another dimension: dry powder dispersion for even the finest, cohesive powders came true with RODOS. And with the R series of our laser diffraction sensor HELOS new benchmarks for precision and accuracy have been achieved. Latest improvements comprise enhanced application of parameter-free Fraunhofer evaluation down to the submicron regime (below 1 µm), the greatest measuring signal frequency for best resolution with range combination technology and more powerful evaluation modes (Fraunhofer & Mie).

The modular HELOS system design together with a great variety of dispersing and dosing units provides a flexible adaptation to the most diverse industrial and research applications:

Dry applications

• RODOS | injection disperser for finest, even cohesive powders | 0.1 µm to 3,500 µm
• GRADIS | gravity disperser for coarser, even fragile dry particulate systems | 0.5 µm to 8,750 µm
• VIBRI | vibratory feeder for precise dosing and feeding of dry particulate systems (in combination with RODOS or GRADIS)
• ASPIROS | micro dosing system for feeding of small amounts of precious or toxic dry substances in encapsulated sample vials (in combination with RODOS)

Wet applications

• SUCELL | closed-loop flow-through cell for suspensions and emulsions | 0.1 µm to 1,750 µm | (50) 500ml cell
• QUIXEL | flow-through cuvette with pumping circuit for emulsions and suspensions, even with coarser, high density particles | 0.1 µm to 3,500 µm | heating option
• CUVETTE | stationary cuvette for precious or toxic emulsions and suspensions of small sample volume | 1 µm to 3,500 µm
• MULTISAMPLER | sample handling system for automated feeding of wet samples in 39 ml vials in batch operation (in combination with SUCELL or QUIXEL) | 70 vials per rack

Specialties

• OASIS | combined dry and wet disperser, consisting of RODOS & SUCELL
• SPRAYER | actuator for the analysis of aerosol clouds released by MDIs, pump sprays or sprays with propellants | 25 µm to 1,750 µm
• INHALER | adapter for the analysis of aerosols released by DPIs, MDIs, nebulizers, pump sprays or sprays with propellants | 25 µm to 1,750 µm
• LIQIBACK | Reprocessing unit for recycling of dispersion liquids (in combination with QUIXEL, SUCELL or OASIS) | 1 µm and 0.45 µm

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Laser Diffraction | Particle Size and Particle Size Distribution from 0.25 µm to 3,500 µm

Real-time measurement of particles in process environments
MYTOS integrates the established core technologies of HELOS laser diffraction and RODOS dry dispersion in a single robust body: a process-proven laser diffraction sensor for dry powders ranging from 0.25 µm to 3,500 µm. In combination with continuously operating sampling system TWISTER a complete integration into the processing pipe is realised making it a true in-line solution delivering representative results. Alternatively, MYTOS may be operated on-line either with TWISTER, MIXER, L-probes or existing sampling solutions. Integrated at-line operation in automated lab environments is succeeded with vibratory feeder VIBRI. For instance, typical applications comprise milling operations or spray granulation.

The process-specific laser diffraction sensor finds a wide range of applications from cement to pharmaceuticals, from roughest industrial conditions to GMP environments. If required, the system may be configured for ATEX zones.

• RODOS at MYTOS | injection disperser for finest, even cohesive powders | 0.25 µm to 3,500 µm
• VIBRI | vibratory feeder for precise dosing with adaption to proprietary sampler or for manual feeding (in at-line combination with MYTOS)
• TWISTER | dynamic, representative sampler for installation in process pipes (in-line or or on-line in combination with MYTOS)
• MIXER | static mixer for representative sampling behind screw feeder or feeding
• L-probes | compact sampler with blow back unit or with pivoting option

Innovative Superior Performance

MYTOS | TWISTER & Co. bundle innovative technologies for superior performance and foresighted capacity planning:

• Efficient dry dispersion ensuring complete dispersion for fine, even cohesive powders down to the submicron range with MYTOS
• Real-time particle size analysis with laser diffraction of perfectly dispersed powders with up to 2,000 measurements per second
• Representative sampling in or out of process pipes in the diameter range from 38 to 660 mm at product temperatures of up to 150°C with TWISTER
• Comparability to the established off-line laser diffraction system HELOS | RODOS that share the same core components for a valid method transfer

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Photon Cross-Correlation Spectroscopy (PCCS) | Particle Size and Stability from 0.5 nm to 10,000 nm

In general, the acquisition of scattered light intensities of particles under thermal motion is deployed for nanoparticle characterisation (principle of dynamic light scattering (DLS)). The method known as Photon Correlation Spectroscopy (PCS) applies auto-correlation of scattered light intensities in order to determine particle size distribution. However, this conventional technology requires extremely diluted samples in order to deliver meaningful results.

NANOPHOX brings Photon Cross-correlation Spectroscopy (PCCS) to life, which allows for nanoparticle size analysis in turbid suspensions and emulsions ranging from 0.5 nm to 10,000 nm at up to a hundred times higher solid contents. The outstanding technological feature of NANOPHOX is the acquisition of two separately induced scattered light intensities which then are cross-correlated. This allows for robust measurement even at higher sample concentrations. In addition to size, the aggregation or sedimentation behaviour of nanosuspensions (i.e. stability) may be analysed. Typical applications comprise e.g., pharmaceutical emulsions, polymer emulsions, paints and inks, oxidized particles like aluminium (II) oxide (AIO) or titanium dioxide (TiO₂) in suspensions as well as research on nanodispersions in general.

PCCS advantages

• Robust method for research, development and quality control
• Concentration independent particle characterisation by elimination of multiple scattering effect
• Extension of conventional PCS provides concurrent measurements of particle size and stability in opaque suspensions and emulsions
• Easy sample preparation without undesired dilution series
• Insensitive to sample contamination
• No required cleanroom conditions
• Direct measurement of stability, agglomeration and sedimentation of slightly charged (electro-steric stabilised) to uncharged (steric stabilised) particles of turbid samples
• Premature detection of invisible destabilisation (micro agglomeration) of suspensions or emulsions
• High sensitivity for changes in size and measurement of bimodal distributions
• Solid-state measuring method for in-situ observation of changes in stability or size, e.g. growth and crystallisation processes
• Analysis of special effects such as particle-particle interactions and changes in viscosity in high-concentrated samples
• Wide concentration range by PCS and PCCS united

Nanoparticle measurement in primary conditions

As a professional pioneer of PCCS we are offering the first table top instrument based on Photon Cross-Correlation Spectroscopy (PCCS). With this we consequently follow our strategy of developing innovative instruments which measure the sample as close as possible to its original state. The NANOPHOX system together with its powerful control and evaluation software is fully compliant with FDA requirements and 21 CFR Rule 11.

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Ultrasonic Extinction | Particle Size and Concentration from below 0.1 µm to 3,000 µm 

Liquid dispersions with a high concentration of solid particles or droplets, often totally opaque, are typically found in production processes. For optical analysers, sampling of a small partial flow of the main product stream combined with a high degree of dilution is required. However, dilution not only causes an extensive preparation effort, but often changes the original state of the dispersion.

For such applications, whose typical range of concentration is between 5 and 50 % by volume, ultrasonic extinction (UE) provides an outstanding performance for particle size distribution analysis of suspension and emulsions. Even paste-like particulate systems with concentrations up to 70 % by volume can be analysed.

Instead of electromagnetic waves (light), ultrasonic extinction applies low energetic sound waves. These waves will be coupled into the sample and run through the sample layer of defined distance. Running through this dispersion layer, part of the sound energy gets absorbed and scattered depending on size and amount of particles or droplets. Sound energy that can pass freely through the sample gets captured by a piezo-electric RF-generator and detector setup. The relation between energy going in and coming out results into a so-called ultrasonic attenuation, which is recorded for 31 frequencies. This frequency dependent attenuation spectrum forms the basis for inverse calculation. This results into a 31 size classes particle size distribution for each of the, as well as information of solid or droplets volume concentrations.

Using sound instead of light waves, ultrasonic extinction is independent of the suspension’s or emulsion’s level of transparency. Hence, totally opaque samples like water droplets in crude oil, mineral slurries or coal particles in pitch can be analysed. Furthermore, materials and products which allow no sampling or dilution without facing destruction due to their stability, rank as standard application.

In addition, the ultrasonic extinction method allows a rugged and robust probe design that resists typical process conditions. The OPUS probe masters temperatures up to 120°C, pressures up to 40 bar and the entire range of pH-value. It is also resistant to aggressive media and abrasive materials. For applications in hazardous atmospheres, an ATEX compliant OPUS version is available.

The process adaptation of OPUS to vessels or to large pipes is simple and typically uses a 100 mm adapter-flange. For smaller pipes or bypass-lines, specific process adapters are available: e.g., flow-through (FT) or bypass (BP). The sensor may be positioned in a standby (SB) rack.

The control and evaluation software using intuitive and high-performance methods provides calculation and display of all relevant and characteristic size distribution values. The OPUS system is fully compliant with FDA requirements and 21 CFR Rule 11. Adaptation to process control systems is natively supported by Modbus®, OPC-UA, Profibus®, TCP/IP digital or analogue PLC signals.

For many years, OPUS is successfully operating in crystallization, grinding or homogenization processes and proves ultrasonic extinction’s manifold performances. With various applications, OPUS is repeatedly revealing new insights – not only in production lines but also in pilot plants and lab settings.

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Dynamic Image Analyse | Particle Size and Particle Shape from below 1 µm to 34,000 µm 

The modular image analysis sensor QICPIC combines size and shape analysis of disperse particle systems within a size range of < 1 µm to 34,000 µm. Flexible sensor adaptation for analysis of powders, granules, fibres, suspensions and emulsions is provided by a wide range of dispersing and dosing units. Numerous implementations in pharmaceutical and chemical industry, food and beverage technology or soil science just denote the array of applications in industry and research.

Using a pulsed light source with illumination times in the nanosecond range the particles are optically frozen while a high-resolution, high-speed camera captures the razor-sharp particle projections with a frequency of up to 500 frames per second. The extremely short exposure times ensure capturing and clear imaging of even fastest singular particles. With powerful algorithms QICPIC is evaluating millions of particles in shortest time and guarantees outstanding statistically relevant results. The unrivalled, high speed RODOS dispersion empowers image analysis to master fine, dry and even agglomerating powders as fine as 1.8 µm and above. Most prominent features are reproducibility and comparability of measurement results at optimized sample quantities. Powerful evaluation software supports the simultaneous determination of all relevant size and shape characteristics.

Due to modular placed disperser and dosing units the analyser fits flexible for dry and wet applications generating product-specific characterisation:

Dry Applications

• RODOS | Injection disperser for finest, even cohesive dry powders | 1.8 µm to 4,000 µm
• GRADIS | Gravity disperser for coarser, even fragile dry particulate systems | 5 µm bis 10,000 µm
• VIBRI | Vibratory feeder for precise dosing and feeding of dry particulate systems (in combination with RODOS, GRADIS or OASIS)
• ASPIROS | Micro dosing system for feeding of small amounts of precious or toxic substances in encapsulated sample vials (in combination with RODOS or OASIS) | 1.8 µm to 500 µm
• FIBROS | Pre-disperser for gentle separation and feeding of dry, even curly fibres (in combination with GRADIS) | Fibre thickness 5 µm to 5,000 µm, fibre length 500 µm to 30,000 µm

Wet applications

• SUCELL/L | Closed-loop flow-through cell for suspensions and emulsions | < 1 µm to 2,000 µm | (50) 500 ml cell
• FLOWCELL | Open-loop cell for high volume with mid-size or coarse particles | 10 mm cell: 11 µm to 5,000 µm or 20 mm cell: 17 µm to 10,000 µm
• LIXELL + LIQXI | Dispersing and dosing combination for suspensions and emulsions | < 1 µm to 500 µm
• MULTISAMPLER | Sample handling system for automated feeding of wet samples in 39 ml vials in batch operation (in combination with SUCELL/L) | 70 vials per rack

Specialties

• OASIS | Combined dry and wet disperser consisting of RODOS & SUCELL/L | < 1 µm to 4,000 µm
• LIQIBACK | Reprocessing unit for recycling of dispersion liquids (in combination with SUCELL/L or OASIS) | 1 µm and 0.45 µm

Process-related particle size and shape characterisation is opened up by integrated image analysis sensors PICTOS, PICTIS & PICCELL covering a size range from 1.8 µm to 20,000 µm.

PICTOS integrates QICPIC dynamic image analysis and RODOS dry dispersion technology in a robust body, which was specifically developed for on-line applications. PICTIS combines image analysis and gentle gravitational disperser GRADIS, allowing at-line or on-line applications in process environments. And PICCELL with its flow-through cuvette finally transfers wet dispersion to on-line operations of image analysis.

For the connection of our analysis systems to a process line, we offer a wide range of different samplers for obtaining representative analysis samples.

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