Sample Analysis
Rheology

Rheological Analysis

Rheology refers to the analysis of a fluid’s flow or plastic deformation properties relative to shear forces such as rotational torque. It measures the material transportation properties of liquids, solutions, and slurries under distinct mechanical conditions, and enables analysts to accurately plot flow curves and yield points for a range of fluidic materials. This information provides mechanical insights into the coating and flowing properties of numerous commercial and industrial products, from agrochemicals to personal cosmetics.

To assess the rheological properties of a sample, Meritics provides the RM200 PLUS rheometer. This easily-programmable rotational stress rheometer can intuitively measure flow curves of samples with a built-in thermocouple capable of assessing temperatures between -50°C – 300°C.

Rheometry

Rheology at your fingertips

Thanks to its large storage capacity and its easy programming, the RM200 PLUS allows you to realise all your measurements of flow curves, yield point, thixotropic, fitting without software.

Save your flow curves and calculate your rheological parameters directly without a computer (Plastic viscosity, flow limit, thixotropy, regression model according to Newton, Bingham, Casson and Ostwald). Choose your attachment system tailored to your product constraints.

Contact us for a quote or to discuss your rheological analysis needs.

Sample Analysis
Zeta Potential

Zeta Potential Analysis by Meritics Specialists

Zeta potential is also known as the electro-kinetic potential of a colloid. It refers to the charge repulsion / attraction of particles dispersed in a solution, and is measured by applying an electrical field to the dispersive medium. Researchers commonly perform zeta potential measurements to ascertain the longevity and mechanical stability of a particulate solution, and to establish particle agglomeration characteristics for pharmaceuticals, food products, and more. The DelsaMax Pro is a rapid zeta potential analyser capable of measuring sample volumes as small as 45 microliters (μL) in under a second. This speed of measurement is crucial for maintaining sample stability and supporting zeta potential characterisation of fast-moving consumer goods, as overlong exposure to electrical fields can cause analytes to degrade – reducing experiment throughput and results accuracy.

Dynamic Light Scattering

The BeNano Series is the latest generation of nanoparticle size and zeta potential analysers designed by Bettersize Instruments. Dynamic light scattering (DLS), electrophoretic light scattering (ELS), and static light scattering (SLS) are integrated into the system to provide accurate measurements of particle size, zeta potential, and molecular weight. The BeNano Series is widely applied in academic and manufacturing processes of various fields including but not limited to: chemical engineering, pharmaceuticals, food and beverage, inks and pigments, and life science, etc.

Contact us for a quote or to discuss your zeta potential analysis needs.

Sample Analysis
Particle Charge

Particle Charge Analysis by Meritics Specialists

Powders and granular materials can acquire an electrical charge on the surface of their particles due to contact and movement against handling equipment and containers. Contact and movement of particles within the material itself can also cause charge acquisition. This process is called tribocharging.

It is important to measure particle charge as charge acquisition can lead to problems and unstable behaviour. Charged materials stick to processing equipment and containers, can become airborne more easily, and can flow in different ways than materials with no charge. Many researchers believe that material electrical properties are the most important contributors to powder flow behaviour.

The Mercury Revolution and Volution powder analysers provide particle charge assessments of powdered solid particles during dynamic and stable states when in contact with many different surfaces, including stainless steel, glass, and aluminium.

Volution

Flowability is the capacity to move by flow that characterises powders, i.e. loose particulate solids, as well as fluids. If you need an affordable, easy-to-use method to measure the flow properties and bulk characteristics of your powder then you need to be aware of the Volution Powder Flow Tester.

The Volution Powder Flow Tester uses an annular shear cell to measure a powder’s response to consolidating pressure using the yield locus technique. This approach, in conjunction with the instrument’s heavy duty frame and drive system, allows the Volution Powder Flow Tester system to measure powder samples at pressures up to 250kPa (50kg force). This is around 6 times greater than other instruments, which are often more expensive as well.

Cohesion is a measure of particle to particle bonding strength that results from inter-particle forces generated by factors such as electrical charges, moisture and van der Waals forces.

The angle of internal friction is a measure of the force required to cause particles to slide or move or on each other and is influenced by many parameters including particle surface friction, particle shape, hardness, particle size, etc. distribution, etc. As well as the cohesion and angle of internal friction of the material the Volution Powder Flow Tester can also measure wall friction, time consolidation and unconfined yield strength.

The Volution Powder Flow Tester also has built in temperature and relative humidity sensors, which means it will also automatically weigh the sample to provide density and compressibility measurements. Flow functions can be measured by testing the material at different pressures.

Meritics can provide this level of functionality at such low cost because design and engineering all takes place in house, thanks to their experience gained over 20 years in the industry. Due to the geometry of its test cell, the Volution can test granular materials as well as powders, which other shear testers cannot, as the test cells for other instruments are too small. With the ION Charge Module you can even measure powder charge too.

Contact us for a quote or to discuss your particle charge analysis needs.

Revolution

Powder flow property measurements generally fall into two main categories: dynamic analysis and static analysis. Dynamic instruments measure powder flow properties as the test material is moving or is about to move.

Static instruments measure powder that is not moving and typically has been exposed to pressure. For a complete picture of a material’s flow behaviour, both types of testers are required. For solving specific flow problems, usually one type of tester or test is required.

The Revolution Powder Analyser can measure your powder’s ability to flow, consolidate, granulate, cake, pack and fluidise by measuring the power, time and variances in power of your powder in a rotating drum. This data can be used to quantify your powder’s particle behaviour during process applications such as blending, tableting, mixing and transportation. The Revolution is both easy to load and automatic, eliminating the opportunity for human error.

The REVOLUTION Powder Analyser consists of a rotating drum that measures the flow properties of granular and fluidised materials. Several drum sizes are available, from drums requiring 10 cc’s of sample to drums using 500 cc’s.

A stepper motor turns high precision silicone rollers which in return rotates the drum. The operator can set the drum rotation rate (range 0.1 to 200 RPM) and prep time (range 0 to 999 seconds) of the analysis. A digital camera with the assistance of back-light illumination takes digital images of the powder during the rotation process. The images can be accumulated up to a rate of 30 frames per second.

Using patent pending algorithms, the software measures the behaviour of the powder from the images collected due to the drum rotation and how this behaviour changes over time. This data is then used to calculate various parameters representing the powder’s quality and process ability.

Contact us for a quote or to discuss your particle charge analysis needs.

Sample Analysis
Powder Flow

Powder Flow Analysis by Meritics Specialists

The flowability of bulk powdered solids is a crucial parameter for determining an analyte’s proclivity to conglomeration or fluidisation under distinct conditions.

Motion and pressure can cause bulk powders to undergo complex pseudo-phase transitions depending upon the molecular composition and particle geometry of the sample. Particle flow analysis is used to capture imagery of powders under defined mechanical conditions and to characterise the flow characteristics of the material as a proportion of potential energy to flow capacity, and cohesion relating to inter-particle forces.

Meritics supplies a broad range of powder flow analysers for determining the flowability and caking capacities of bulk powders. The Mercury Revolution is an advanced powder flow analyser for assessing the dynamic properties of samples at rotational speeds of up to 200 RPM. The Volution Powder Flow Tester uses an annular shear cell to assess a powder’s physical responses to consolidating pressures of up to 250 kPa.

Absolute density of solids and powders is commonly measured through pycnometry, which uses gas displacement to determine the particulate density and purity of compact and granulated solid samples. This method uses a test gas with minute atomic dimensions such as helium to permeate the porous structures of a dry powder or solid sample. The small atomic size of helium enables the test gas to diffuse through extremely narrow pores, providing a volumetric measurement that can be compared to the weight of the dried sample to characterise the real or absolute density of the sample.

Powder flow property measurements generally fall into two main categories: dynamic analysis and static analysis. Dynamic instruments measure powder flow properties as the test material is moving or is about to move.

Static instruments measure powder that is not moving and typically has been exposed to pressure. For a complete picture of a material’s flow behaviour, both types of testers are required. For solving specific flow problems, usually one type of tester or test is required.

Contact us for a quote or to discuss your powder flow analysis needs.

The Revolution Powder Analyser can measure your powder’s ability to flow, consolidate, granulate, cake, pack and fluidise by measuring the power, time and variances in power of your powder in a rotating drum. This data can be used to quantify your powder’s particle behaviour during process applications such as blending, tableting, mixing and transportation. The Revolution is both easy to load and automatic, eliminating the opportunity for human error.

The REVOLUTION Powder Analyser consists of a rotating drum that measures the flow properties of granular and fluidised materials. Several drum sizes are available, from drums requiring 10 cc’s of sample to drums using 500 cc’s.

A stepper motor turns high precision silicone rollers which in return rotates the drum. The operator can set the drum rotation rate (range 0.1 to 200 RPM) and prep time (range 0 to 999 seconds) of the analysis. A digital camera with the assistance of back-light illumination takes digital images of the powder during the rotation process. The images can be accumulated up to a rate of 30 frames per second.

Using patent pending algorithms, the software measures the behaviour of the powder from the images collected due to the drum rotation and how this behaviour changes over time. This data is then used to calculate various parameters representing the powder’s quality and process ability.

Sample Analysis
Viscosity

Viscosity Analysis

Viscosity is a measure of a fluid’s resistance to flowing under varying temperature conditions.

It is typically associated with the concept of liquid density or thickness, and usually increases exponentially with decreased temperatures. This property is determined by friction between particles within the liquid or solution and is quantified as a measure of centipoise (cP). Viscosity measurements apply relatively weak thermodynamic forces to a liquid or solution to encourage the material to flow. Temperatures can be increased and torque can be applied to measure the material’s resistance to these conditions, with common applications in the food and beverage, cosmetics, and chemical sectors.

Meritics provides a substantial range of viscosity analysers suitable for a broad range of applications. The RM 100 Portable enables analysts to measure viscosity outside of laboratory conditions with a sustained accuracy of within 1% of the full scale. The First Plus is an ultra-sensitive viscosity analyser with a torque range as low as 0.005 mNm for outstanding precision..

Viscometers

Unique design removes the problems associated with spring type viscosity measurements. This makes the Lamy range very robust and replacing expensive springs and pointer assembles are a thing of the past!

For ultra-sensitive viscosity measurements, the First Touch features a torque range of 0.005 to 0.8 mNm

With its expanded programming possibilities and increased modularity, the FIRST PLUS will be the ideal tool for your application whether you use it alone or with its software.

Delivery as a single unit or with the spindle sets L1-L4 or R2-R7.

• Measurement at different speeds
• Viscosity range up to 240 000 000 mPas
• 7 “touch screen
• different measuring spindle sets
• easy to use
• wide range of applications
• stable stand

Contact us for a quote or to discuss your particle analysis needs.

Sample Analysis
Density

Density Analysis

Solid materials are regularly characterised relative to their density, which is expressed as the mass of a powder or solid material per unit volume. Density analysis is regularly acquired using a form of gas displacement, which can rapidly determine the real density and purity of solid materials such as ceramics, metals, and polymers.

The Thermo Scientific Pycnomatic is a comprehensive solution for performing density measurements of solid materials. It features a fully-integrated, high-precision temperature control for exceptional results reproducibility. It boasts a real multi-volume capability for utmost accuracy of results with different solid materials, including fine powders and foams.

BeDensi T Pro 

The BeDensi T Pro series is a reliable tapped density analyser that excels at intuitive operation while complying with the USP, EP, ASTM, and ISO standards. It can measure the bulk density and tapped density with less than 1% repeatability variation to help users to understand the flowability of a wide variety of powder materials.

Sample Analysis
Surface Area

Surface Area

Surface area analysis is a common particle measurement methodology that provides data relevant to a material’s adsorption and dissolution properties, as solid particles primarily interact with other media through their surface area. It is possible to determine multiple characteristics of solid materials by assessing the volume of an inert gas that it can adsorb, and the pressure required to push the gas into a porous structure. It is also possible to assess the interaction of gases with the free surfaces of powder particles. Both techniques provide critical insights for manufacturing of dosage form pharmaceuticals.

The Horiba SA-9600 series is suitable for both single- and multi-point surface area analysis with a range of 0.10 – 2,000 square meters per gram.

BET Surface Area

Brunauer-Emmett-Teller (BET) surface area analysis is the multi-point measurement of an analyte’s specific surface area (m2/g) through gas adsorption analysis, where an inert gas such as nitrogen is continuously flowed over a solid sample, or the solid sample is suspended in a defined gaseous volume. Small gas molecules adsorb to the solid substrate and its porous structures due to weak van der Waals forces, forming a monolayer of adsorbed gas. This monomolecular layer, and the rate of adsorption, can be used to calculate the specific surface area of a solid sample and its porous geometry, informing studies into the reactivity and bioavailability of pharmaceutical products.

The Horiba SA-9600 can measure BET surface area at a range of 0.10 to > 2,000 m2/g for intervals of just 6 minutes.

Contact us for a quote or to discuss your particle sizing needs.

Sample Analysis
Particle Shape

Particle Shape Analysis

Particle morphology refers to its form, shape, and its physiochemical or biochemical structure. Analysing particle shape and morphology can provide significant insights into the characteristics of a material and its practical applications, as well as its genesis.

There are numerous applications for the observation of particle shape and morphology, including the assessment of drug efficacy and quality control of industrial surface treatments. The FlowCam series of particle counters is equipped to perform particle shape and morphology analysis, with additional parameter considerations for application-specific purposes. Sub-visible proteins of below 10 micrometers (μm) can be quantified using the FlowCam Biologics, while larger particles of between 50 µm – 5000 µm can be morphologically measured using the FlowCam Macro.

Dynamic Imaging

Today microscopic examination and counting and sizing of small particles is commonplace, Meritics work with Yokogawa Fluid Imaging Technologies (YFIT) and their FlowCam Image Analyser range can size from 300nm to 5mm in range, this takes the tedium involved away and frees up the scientist to analyse data comprehensively.

Electron microscopes probe the size range below the limit of optical microscopy and a scanning technique enables pictures of the surface features of even very delicate surfaces to be made in exquisite detail.

Most recently our scientists have been sizing sugar samples on the FlowCam 8000 to measure the size and to give an image of the particles.

Contact us for a quote or to discuss your image analysis needs.

Sample Analysis
Particle Count

Particle Count Analysis

Particle Count Analysis is a broad field of particle analysis, using multiple techniques and methodologies to acquire data about the density and concentration of solid, liquid, or gaseous particles in a sample. High-sensitivity imaging technology, electrical sensing zone (ESZ) techniques, and light obscuration methods are all used to measure the concentration or volume of particles, with proven applications in material characterisation and environmental studies.

At Meritics, we provide Laboratory Analysis using a range of particle counters, including the Multisizer 4e which uses Electrical Sensing Zone analysis; the Spectradyne nCS2 uses resistive pulse sensing to count and size from 2um down to 50nm and the FlowCam range which uses Dynamic Imaging.

Electrical Sensing Zone

Beckman Coulter Multisizer 4e, with a range of 0.2µm to 1600µm is widely used in many areas: Life Sciences such stem cells, cell biology, and Industrial such as toner, ceramics, sediments etc. as well as Pharmaceutical applications.

The Coulter Principle (also known as ESZ – Electrical Sensing Zone) is hailed as probably the most significant advance in the field of particle technology, and tens of thousands of Coulter Counter instruments are in regular use worldwide.

Most recently our scientists have been running a lot of water samples on the Multisizer 4e to measure contaminants.

Contact us for a quote or to discuss your particle sizing needs.

Resistive Pulse Sensing

The Spectradyne’s nCS2 ^TM has taken the Coulter Counter method and re-engineered the principle, it is now possible to count and size individual particles down to 50nm.

The Spectradyne nCS2^TM instrument provides a unique platform for the rapid quantitative measurement of Nanoparticle size in solution.

The instrument measures individual nanoparticles to produce particle size distributions with quantitative concentration information for particles from 40nm to 2000nm in size. Not relying on optical technology, the Spectradyne system can be used for protein aggregation studies, extracellular vesicle analysis, nanomedicine, virus studies etc.

Disposable microfluidic cartridges eliminate cross contamination and make operation simple and straightforward from just 2-3µl of sample.

Spectradyne’s nCS1 instrument and associated analysis cartridges, are based on Spectradyne’s patented nanoparticle analyzer (NPA) technology. The heart of the instrument is the microfluidic cartridge, which allows the electrical detection of nanoparticles as they pass one by one through a nanoconstriction. Particles larger than the nanoconstriction are removed before reaching it by filters that are built into the cartridge.

No pre-filtering of the sample is required by the user.

Contact us for a quote or to discuss your particle sizing needs.

Dynamic Imaging

Today microscopic examination and counting and sizing of small particles is commonplace, Meritics work with Yokogawa Fluid Imaging Technologies (YFIT) and their FlowCam Image Analyser range can size from 300nm to 5mm in range, this takes the tedium involved away and frees up the scientist to analyse data comprehensively.

Electron microscopes probe the size range below the limit of optical microscopy and a scanning technique enables pictures of the surface features of even very delicate surfaces to be made in exquisite detail.

Most recently our scientists have been sizing sugar samples on the FlowCam 5000 to measure the size and to give an image of the particles.

Contact us for a quote or to discuss your particle sizing needs.

Sample Analysis
Particle Size

Particle Size Analysis

In all product development, the particle size of products and materials is a critical parameter in their manufacture. Changing the particle size distribution of a material has a massive impact on its characteristics and behaviour either during manufacture, within the final product or on its effects within the environment.

The Meritics Lab offer a range of measurement techniques and particle size analysis testing methods that cover virtually all materials — wet or dry, ranging from >1 nm to 5 mm in size. Our expert scientists can help select the most appropriate test for your material/system from the following:

• Laser Diffraction
• Dynamic Light Scattering
• Electrical Sensing Zone
• Dynamic Imaging
• Sieve

Depending on the technique used, we can report:

• Particle size distribution – weighted to volume, number or surface area
• Polydispersity

Additionally, Meritics offer a fully validated method development service.

Get in touch for a quote or to find out more about how we can support you ….

Laser Diffraction

Laser diffraction analysis is based on the Fraunhofer diffraction theory. The intensity of light scattered by a particle is directly proportional to the particle size. The angle of the laser beam and particle size have an inversely proportional relationship, where the laser beam angle increases as particle size decreases and vice versa. The particles are placed in a flow cell between the laser and its focal point. The material is analysed using its laser scatter pattern.

The technique of laser diffraction requires the ability to measure the angle of diffraction of the laser light in order to ascribe a size to the particle. For relatively large particles such as 20µm, this is relatively easy as the intensity minima are well defined, see below:

However, once the size gets below 1µm, there is little or any discernible shape to the intensity ‘curve’ making the discernment of any angular variation virtually impossible below approx. 0.4µm.

Some manufacturers take the intensity data down to this size level and then make effectively; an educated guess; at the data below in order to show something down to 0.1µm. Beckman Coulter developed a patented detection system ‘Polarisation Intensity Differential Scattering’ (PIDS) to overcome the limitations of laser diffraction in this region. Particles scatter polarised light by differing amounts. By combining vertically and horizontally polarised light with multi-wavelength measurements, a much more accurate and reliable measurement can be made below 0.4µm.

The approach has been validated by many of the other manufacturers trying to partially copy this by adding additional wavelength measurements.
The most Modern Beckman Coulter LS 13320 XR system can now produce real data down to 10nm using the Patented PIDS system.

Our scientists work with clients across many industries and are experienced in measuring a variety of samples from dry powders such as sugars, soils and sediments to emulsions. If your samples are soluble in water we can measure them in a non-aqueous dispersant, or use a surfactant if it wets poorly. Additionally, we can report means weighted results according to volume, number or surface area.

For submicron particles, the principle of Brownian Motion can be used, as in the Beckman Coulter DelsaMax. Particles suspended in a liquid are in a constant state of random movement or vibration due to the molecular bombardment.

The smaller the particle, the faster it will move. Analysis of the frequency change of scattered laser light pattern is made by auto-correlation spectroscopy, from which average particle size and particle distribution are calculated, the only contestants with this method are the liquids refractive index and viscosity or temperature need to be known. DLS has an overall effective size range of 0.4nmm to 10m.

Our most recent work has been with a lot of university establishments working with crude oil.

Contact us for a quote or to discuss your particle sizing needs.

Electrical Sensing Zone

Beckman Coulter Multisizer 4e, with a range of 0.2µm to 1600µm is widely used in many areas: Life Sciences such stem cells, cell biology, and Industrial such as toner, ceramics, sediments etc. as well as Pharmaceutical applications.

The Coulter Principle (also known as ESZ – Electrical Sensing Zone) is hailed as probably the most significant advance in the field of particle technology, and tens of thousands of Coulter Counter instruments are in regular use worldwide.

Most recently our scientists have been running a lot of water samples on the Multisizer 4e to measure contaminants.

Contact us for a quote or to discuss your particle sizing needs.

Spectradyne’s nCS2^TM has taken the Coulter Counter method and re-engineered the principle, it is now possible to count and size individual particles down to 50nm.

The Spectradyne nCS2^TM instrument provides a unique platform for the rapid quantitative measurement of Nanoparticle size in solution.

The instrument measures individual nanoparticles to produce particle size distributions with quantitative concentration information for particles from 40nm to 2000nm in size. Not relying on optical technology, the Spectradyne system can be used for protein aggregation studies, extracellular vesicle analysis, nanomedicine, virus studies etc.

Disposable microfluidic cartridges eliminate cross contamination and make operation simple and straightforward from just 2-3µl of sample.

Spectradyne’s nCS2 instrument and associated analysis cartridges, are based on Spectradyne’s patented nanoparticle analyser (NPA) technology. The heart of the instrument is the microfluidic cartridge, which allows the electrical detection of nanoparticles as they pass one by one through a nanoconstriction. Particles larger than the nanoconstriction are removed before reaching it by filters that are built into the cartridge.

No pre-filtering of the sample is required by the user.

Contact us for a quote or to discuss your particle sizing needs.

Dynamic Imaging

Today microscopic examination and counting and sizing of small particles is commonplace, Meritics work with Yokogawa Fluid Imaging Technologies (YFIT) and their FlowCam Image Analyser range can size from 300nm to 5mm in range, this takes the tedium involved away and frees up the scientist to analyse data comprehensively.

Electron microscopes probe the size range below the limit of optical microscopy and a scanning technique enables pictures of the surface features of even very delicate surfaces to be made in exquisite detail.

Most recently our scientists have been sizing sugar samples on the FlowCam 8000 to measure the size and to give an image of the particles.

Contact us for a quote or to discuss your particle sizing needs.

Sieves

For the characterisation of bulk goods of different forms and sizes, the knowledge of their particle size distributions is essential. The particle size distribution, i.e. the number of particles of different sizes, is responsible for important physical and chemical properties such as solubility, flowability and surface reaction.

In many industries such as food, pharmaceuticals and chemistry traditional sieve analysis is the standard for production and quality control of powders and granules. Advantages of the sieve analysis include easy handling, low investment costs, precise and reproducible results in a comparably short time and the possibility to separate the particle size fractions. Therefore, this method is an accepted alternative to analysis methods using laser light or image processing.

Contact us for a quote or to discuss your particle sizing needs.

Industry Information
Chemicals

Why particle characterisation is important in chemical industries

Particle characterisation is a crucial process in the automotive industry that involves the analysis and understanding of the properties and behaviour of particles present in various automotive components. These particles can be found in engine lubricants, brake pads, fuel, and many other materials used in cars.

By characterising these particles, engineers can gain valuable insights into their size, shape, composition, and distribution. This information helps them in designing and developing more efficient and reliable automotive parts. For example, understanding the particle size distribution in engine lubricants can help engineers create lubricants that provide better protection and reduce friction, leading to improved engine performance and fuel efficiency.
Particle characterisation also plays a vital role in ensuring the safety of automotive components. By analysing the particles in brake pads, engineers can determine their wear rate and composition, helping them develop brake pads that offer optimal stopping power and durability.
Overall, particle characterisation in the automotive industry is a crucial science that enables engineers to create better-performing and safer automotive components, resulting in a smoother driving experience for all.

Case study

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Instruments to support chemical manufacturing

Applications to support chemical manufacturing

Affinite
ezSPR

Benchtop SPR

• Core technology
• Flexible design
• Rapid data processing

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Core Technology

Basic thin film SPR found in most benchtop devices capable of detection in complex media such as serum, plasma, cell lysates, or wastewater.

Flexible Design

Adaptable from injection to sensor. Comes with two injection models with multiple options to meet your research needs

Rapid Data Processing

Intuitive software providing key data for biosensing and protein interaction characterization in real time.

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Technology
BET Surface Area

Gas adsorption: Determination of the specific surface area (BET surface area)

The determination of specific surface areas represents a major task regarding the characterization of porous and finely-dispersed solids. Gas adsorption is the appropriate method to solve this task. If a gas gets in contact with a solid material a part of the dosed gas molecules is being adsorbed onto the surface of this material. The adsorbed amount of gas depends on the gas pressure, the temperature, the kind of gas and the size of the surface area. After choosing the measuring gas and temperature, the specific surface area of a solid material can be reliably and comparably calculated from the adsorption isotherm. Due to practical reasons the adsorption of Nitrogen at a temperature of 77 K (liquid Nitrogen) has been established as the method for the determination of specific surface areas.

Measuring method

Speaking about the BET method, actually means the analysis of isotherm data by a method developed by Brunauer, Emmett and Teller. By means of the BET equation the amount of adsorbed gas, which build up one monolayer on the surface, can be calculated from the measured isotherm. The amount of molecules in this monolayer multiplied by the required space of one molecule gives the BET surface area. Besides the adsorption of Nitrogen at 77 K, Krypton adsorption at 77 K is recommended for the determination of very small surface areas.

Technology
Closed Cell Content

Closed cell content in foams

The determination of closed and open cell content in foams is based on the determination of the samples volume by means of gas pycnometry, which is an analytical method for density and volume analysis described separately on this homepage. When investigating foams, the most common challenge is to determine the amount of vesicular polymer cells completely closed, as these cells determine the insulation capacities of rigid foams commonly used in the thermal insulation of housing.

Measuring principle

The measurement is carried out as stated per DIN ISO 4590 „Determination of the volume fraction of open and closed cells in rigid foams“. Initially, a geometrically exact sample body will be cut (cube, cuboid or cylinder) and its exact dimension will be determined by means of a micrometer in order to calculate the geometric volume. Afterwards, the sample body will be analyzed in the pycnometer at a low pressure of roughly 0.25 bar. The analytical gas employed here is nitrogen, as helium will penetrate into the walls of the closed cells in the foam. This first measurement includes the volume of the sample body yielding the closed volume, into which the analysis gas cannot penetrate and from which the amount of closed cells will be derived. The so-called uncorrected method terminates here, the quotient from closed volume to geometric volume multiplied by 100% determines the percentage of closed cell content in the sample.

In the so-called corrected method relates to the fact that by cutting through the sample cells previously closed will be opened. This can be corrected by an additional measurement. For this, the sample body will be cut into smaller parts and all parts obtained after cutting will be measured in the pycnometer again. The amount and position of cuts as well as the equation for results depend on the geometry of the original sample body and can either be determined by DIN ISO 4590 or by measuring.

Product

Technology
Gas Pycnometry

Determination of density by means of gas pycnometry

In general terms density is defined as the quotient from mass by volume. Mass can be determined with ease by a scale. The determination of volume is more challenging, usually due to samples having irregular shapes or being powders of varying degree. Additionally, it needs to be noted that volume, and thus density, may be defined differently if pores are included (raw density) or excluded (true / absolute density) into the solid samples volume. The density is based on the solid samples volume excluding the pore volume of porous solids.

With a pycnometer (Greek, „gauged vessel”) the amount of a certain medium (liquid or Helium or other analytical gases) displaced by a solid can be determined. Examples for the use of density determinations for finely ground or bulky solids include, but are not limited to, for example the differentiation between solids, quality insurance, determination of open and closed pore volume in foams and determination of so-called vacuolar volume in the quality control of milk powders. These fields illustrate the versatility of gas pycnometry and exceed the limits of liquid pycnometry. The main advantages of the gas pycnometry are:

• fast
• precise
• requires no organic liquids
• low user expense
• automatisation

Product

Technology
Laser Diffraction

Introduction

The particle size distribution is a crucial parameter in many applications that involve powders or dispersions. These include construction materials like cement and sand, pharmaceuticals, ceramics, colored pigments, fertilizers, emulsions, and more. As the range of applications expands, so do the requirements for measuring methods in terms of size range, measurement time, and reproducibility.

Measuring particles close to the range limits and simultaneously detecting particle sizes of both small (nanometer range) and large particles (lower millimeter range) for polymodally or broadly distributed samples is particularly challenging. However, modern laser diffraction particle size analyzers such as the Bettersizer S3 Plus overcome these challenges through innovative optical system design that detects backscattered light of very small particles and captures large particles with an integrated high-speed CCD camera or a combination of laser diffraction method and image analysis method.

Measuring Method

Laser diffraction method of particle sizing involves the interaction of laser (monochromatic and coherent light) with particles that need to be measured in terms of their size. The diffraction of light waves by the particles follows a distinct pattern depending on their size: larger particles scatter more light in the forward direction. For particles smaller than 100 nm, the scattering intensity is almost the same in all directions.

The scattering intensity is determined by stationary detectors depending on the angle. State-of-the-art laser diffraction systems such as the Bettersizer S3 Plus laser diffraction particle size analyzer guarantee the determination of scattering intensities in a continuous angular range of 0.02 – 165°, i. e. in the forward, side, and backward direction. This is achieved by means of the unique Dual Lens and Oblique Incidence (DLOI) optical system: Fourier lenses (collective lens) are positioned between the laser and particles as well as between particles and detectors. The particles will interact with the light within a parallel laser beam. This offers the advantage that the scattered light can also be detected at very large angles (in the backward scattering direction) and thus even very small particles can be detected and measured precisely. Thanks to DLOI technology, the problems of conventional measurement setups can also be avoided. Therefore, neither the suitable lenses for the corresponding particle size measurement range have to be selected prior to the measurement (in comparison to the Fourier optics), nor do measurement inaccuracies result from different particle-to-detector distances if not all particles lie in one plane (in comparison to the inverse Fourier optics).

To calculate the particle size distribution from the measured scattering spectra, the theory of either FRAUNHOFER or MIE is applied. The FRAUNHOFER theory is based on the hypothesis of opaque and spherical particles: the scattered pattern corresponds to a thin opaque two-dimensional plate – diffraction only occurs at the edges. Therefore no additional optical input constants of the material are necessary for this calculation. In contrast, the MIE theory uses the hypothesis of virtually translucent and spherical particles, meaning that light permeates the matter and is scattered elastically at the atoms of the particle. The knowledge of the complex refractive index of the particles and the liquid as well is necessary. This theory is applicable to particles of all sizes.

The following figure shows an example of a volume-weighted particle size distribution of a calcium carbonate powder – measured with a Bettersizer S3 Plus. The cumulative throughput curve (blue line) and the resulting histogram (black bar) can be seen.

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Technology
Image Analysis

What is image analysis?

The term “image analysis” is describing the mechanism: the image analyzer will capture an image of a 3-D particle first, then do the analysis based on the 2-D particle projection image. Depending on the movement state of particles during the measurement, the image analysis method is divided into 2 kinds: one is the dynamic image analysis method (DIA), and another is the static image analysis method (SIA).

Why Image Analysis?

Today, particle size alone may not be sufficient to get qualified products out the door. Many industries are turning to particle size and shape analysis. This is where the image analysis method comes in. The necessity for size and shape analysis of every single particle, combined with ever-increasing PC processing power, ensures that automated imaging methods are becoming increasingly more relevant to a market which is taking advantages of non-spherical particles.

Automated imaging methods for the determination of the particle size distribution of a material offers a fundamental advantage over alternative methods such as static light scattering, sedimentation or sieving: Each particle is photographed and thus analyzed individually! In addition, the individual photography of the particles gives the opportunity to make statistical calculations of not only the particle size but also the particle shape, this results in several important advantages for the determination of the particle size (shape) distribution:

• Realistic proportional values also at the edges of the size distribution, i. e. detection of oversized particles or fine particles
• More meaningful size and shape parameters of each single particle, instead of diameter of ideal spheres. e. g. geodetic length or elongation for fibers.
• For more information, please check the particle size and shape parameter guidebook
• Flexible changeovers between distribution types (volume / area / number) depending on the particular task
• Visual assessment of the dispersing state of a sample (dispersing quality, presence of agglomerates)
• Further differentiation of materials. For example, in addition to the particle size distribution, the roughness of the particle surface plays an important role for the success of shaping or polishing.

How to Image Analysis?

The determination of the particle size and shape by image analysis method includes 4 basic steps:

1. Image taking

The image taking process is the base of the image analysis method. Special digital cameras are ultilized to ensure a clear vision contains sharp images of particles. If necessary, the camera can be in combination to a microscope.

2. Image processing and particles detection

Appropriate software processes captured pictures: signal noise, isolated pixels and edging particles are eliminated, brightness is adjusted to strengthen the contrast between the particle and the background, etc.

Particles are then separated from the background. Depending on the application, special requirements will be employed to filter out part of particles, such as agglomerates, bubbles, or reflecting metal powders.

3. Particle size and shape calculation

Size and shape parameters of every single particle will be calculated with the software.

4. Statistical calculations and classification

The particles are arranged in classes (e.g. size equivalent classes) on the basis of their attributed features (size and shape parameters).

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