Center for
Particulate Products
and Processes


Research


Our vision is to create new functionality, improve quality, and reduce the costs of particulate-based products


Our mission is to provide the knowledge, tools, and trained workforce needed to effectively design and manufacture particulate products

Facilities


Purdue University’s Particle, Powder, and Compact Characterization Laboratory

Purdue University has a dedicated 2000 ft2 facility located in POTR 205/277 for Particle, Powder, and Compact characterization. A description of the laboratory’s equipment is given below. In addition to these facilities, researchers have access to additional research equipment across campus, including numerous optical and scanning electron microscopes, atomic force microscopy, nanoindentation, x-ray computed microtomography, BET gas adsorption, differential scanning calorimetry, NIR spectroscopy, UV-Vis spectrophotometry, Raman spectroscopy, and other devices.

Our Lab Manager is available to help with your material characterization measurements - contact us for more information


Retsch PT100 sample divider

This device divides a sample so that the composition of each fraction of the sample corresponds to that of the original bulk sample. The material feed and dividing processes take place automatically.


Humboldt H-3985 sample splitter

Material poured into the splitter’s hopper is divided into two equal portions by a series of chutes that discharge the material alternately in opposite directions into separate pans. Chutes: (12), 0.75" (19mm) width; Hopper: 8.5" width x 14" length (171 X 356mm).


Gilson SP-1 sample splitter

A large-capacity sample splitter for materials with particle sizes up to 4 in. (102 mm). The device has a hopper capacity of 1 ft3 (28.3 l) and has 48 chutes, each with a width of 0.5 in. (13 mm). The sample splitter dimensions are WxDxH 29x19x39 in. (737x483x990 mm).


Malvern Mastersizer 3000 particle size analyzer

This analyzer uses Mie light scattering theory to measure the size distributions of particle populations. It is the state-of-the-art equipment for size measurement and has a broad measuring range from 10nm to 3500 µm. The Characterization Laboratory has two wet dispersion units: Hydro MV (100mL dispersant/run) can measure up to 1400µm, whereas Hydro SV (6 ml / run) is used for smaller quantities of dispersant and can measure up to size of 200 µm. In addition, the equipment also has a solvent-free air dispersion unit Aero S, which can measure up to 3500 µm. The equipment comes with real time size monitoring capability, allowing the study of agglomeration, dissolution etc.


Malvern Morphologi G3-ID

The Morphologi G3-ID utilizes automated static imaging features to measure the size and shape distribution of particles. It also offers a unique capability of chemical identification of individual particles using Morphologically-Directed Raman Spectroscopy. The measuring range, for both dry and wet dispersion, is 1 µm to 1000 µm. The particle size parameters that can be measured are circle equivalent (CE) diameter, length, width, perimeter, area, maximum distance, sphere equivalent (SE) volume, fiber total length, and fiber width; and the particle shape parameters that can be measured are aspect ratio, circularity, convexity, elongation, high sensitivity (HS) circularity, solidity fiber elongation, and fiber straightness.


Tyler Ro-tap Model E sieve shaker ASTM E-11 sieves

This sieve shaker holds up to six full-height or 13 half-height 8 in. diameter sieves, including a top cover and receiving pan. The shaker is actuated by a built-in, 99-minute digital timer with 0.1 second accuracy. The laboratory sieves can measure particle size distributions from 45 µm to 8 mm.


Nikon SMZ1500 microscope & Nikon Optiphot-2 microscope

Imaging software


Innopharmlabs Eyecon in-line/at-line image analysis system

This portable instrument uses real-time, direct imaging of particles to measure particle size distributions and 2D particle shape information for particle streams traveling at up to 10 m/s. Particle sizes between 50 and 3000 μm can be measured.


Skyscan X-ray MicroCT

Compact and powerful X-ray CT system with maximum resolution of 0.35 µm, to study microstructure of materials in a non-destructive manner. Can hold sample as large as 70 mm diameter x 75 mm height. Powerful software can reconstruct 2D images of internal microstructure in less than an hour, as well as calculate sample porosity. Movies to visualize internal 3D structure can also be created.


Krüss K100MKII goniometer

This device measures the surface tension and the interfacial tension of liquids using the Wilhelmy plate method in a range from 1 to 1000 μN/m. Contact angles on solids of uniform geometry are measured using the dynamic Wilhelmy method. The dynamic contact angle and the adsorption behavior on powders and other porous materials are determined via the Washburn method. The instrument has a built-in ionizer, which eliminates electrostatic charges and increases the measuring accuracy. The surface energy on solids, powder, and fibers can also be measured with this device.


Photron FASTCAM-X 1024 PCI 100K high-speed video camera

This monochrome high-speed camera system is a full-size PCI camera with 4 GB of onboard memory. The equipment is capable of recording from 60 to 109500 frames per second and captures 1000 frames per second at a resolution of 1024x1024 pixels for up to 3.2 seconds. It is capable of an electronic shutter speeds down to 1.5 μs. The camera system also includes 25mm, 50 mm, and 100 mm lenses, lighting, and several tripods.


NovaStrobe DA115 strobe lamp

This device can be used for optical frequency estimation using 30 to 20000 flashes per minute in 0.1 fpm increments.


Carver Press Auto Series 3888

The equipment has a minimum and maximum clamp force of 700 lbf and 30000 lbf, respectively. It can be used to produce powder compacts of various solid fractions.

Micromeritics AccuPyc II 1340 pycnometer

This device measures the apparent volume and density of solids and powders using helium as the working gas. Sample capacities of 1, 10, 100, and 350 cm3 are available. Using multivolume kits, measurements can be performed for materials having volumes as small as 0.01 cm3. The Characterization Laboratory has a 10 cm3 sample cup and a multivolume kit enabling smaller sample sizes (1 and 3.5 cm3).


Micromeritics GeoPyc 1360 envelope and T.A.P. density analyzer

This device measures the envelope density of granules and compacts (even porous objects of irregular size and shape) using the displacement of a fine, free flowing powder. The Characterization Laboratory has all available sample chambers ranging from 1.27 to 5.08 cm inner diameter. The analyzer can also measure the Transverse Axial Pressure (T.A.P) density of powders and other solids.


Agilent Technologies 350 tapped bulk density tester

This tester provides a standardized, reproducible method for measuring the tapped or bulk density of powdered, granulated, or flaked materials. Two 100 ml funnel-top cylinders hold the samples to be tested.


Freeman FT-4 rheometer

This device measures a powder’s basic flowability energy, a measure of the powder’s flow properties. The FT4 also includes a shear cell for measuring the powder’s shear strength, and a wall friction kit to quantify how the powder shears against a boundary. Accessories for measuring other bulk properties, such as bulk density, compressibility, and permeability are also available.


Schulze RTS-XS ring shear tester

This ring shear tester measures a powder’s flow properties such as internal friction angle, effective friction angle, flow function, cohesion, and compressibility using small volumes of material (9 – 70 ml). The effects of time consolidation can also be measured, as well as wall friction measurements. The testing procedure is computer-controlled to eliminate bias due to operator’s handling.


Anton Paar MCR 502 Powder/Liquid Rheometer

This rheometer has a unique capability to analyze the flow properties of both powders and liquids. For liquid and gel samples analysis, the rheometer is equipped with Parallel plate and cup geometries. For powder samples analysis, there is a state of the art powder cell that measures powder flow properties under stationary or fluidized conditions.


PerkinElmer Thermogravimetric Analyzer (TGA)

The TGA measures the change in mass of a particulate sample as a function of temperature. The heating range of this instrument is from ambient to 1000 ºC. This instrument can be used to study the thermal behavior as it relates to product formulation and stability. This can also be used to quantify the mineral composition and moisture content of particulate materials.


Mettler Toledo HG63 moisture analyzer

A sample is weighed and heated with an infrared radiator (halogen lamp). The loss in weight is continuously recorded and drying ends once a defined criterion is reached.


Binder FED115 drying oven

Used for drying and sterilization applications up to 300 °C (572 °F) and storage at precisely controlled elevated temperatures. The internal volume is 4.1 ft3.


Instron ElectroPuls E1000 mechanical testing frame

This testing frame is used to measure the mechanical properties of wet granules and compacts. It is capable of performing static testing up to 710 N and dynamic testing up to 1000 N. The Characterization Laboratory has 250 N and 2000 N load cells, which are calibrated to measure loads down to 1 N and 20 N, respectively with an accuracy of ±0.5%. The calibrated maximum test stroke of the equipment is 50 mm (max. test stroke is 60 mm). The minimum and maximum speeds are 0.05 mm/min and 1700 mm/sec, respectively.


Mechanical Testing Systems (MTS) Model C43.504 testing frame

This testing frame is used to make powder compacts and measure the mechanical properties of powder compacts. It is capable of performing static testing up to 50 kN. The Characterization Laboratory has load cells ranging from 5N to 50 kN, which are calibrated to measure loads down to 0.15 N with an accuracy of ±0.5%. The calibrated maximum test stroke of the equipment is 1100 mm (max. test stroke is 60 mm). The minimum and maximum speeds are 0.005 mm/min and 750 mm/min, respectively.


Drucker-Prager Cap powder parameter and powder-surface adhesion instrumented punch-die set

This instrumented punch and die system is used to measure powder Drucker-Prager Cap constitutive model parameters and powder-die wall friction coefficients. The measurement system consists of a die with capacitive radial stress sensor, load cell to measure punch force, and displacement transducer to measure punch displacement. The output of the sensors enables simultaneous measurement of the powder density, die-wall friction, and the stress state of the powder. The variation in the material constitutive parameters is less than 10% depending on the material and applied stress. A novel punch design also allows us to measure powder adhesion against various surfaces as a function of compression force.



Purdue University’s Continuous Solids Processing Pilot Plant

Responsive image

Three-level platform with containment modules for housing powder processing equipment, with a negative pressure clean room equipped with HEPA filters


The Continuous Solids Processing Pilot Plant is a state-of-the-art high-bay facility with options for producing dry and wet granulated products. The line includes several Schenk Accurate continuous feeders, two Gerike continuous blenders, an Alexanderwerks roll compactor and mill, and RIVA and Natoli tablet presses. A Thermofisher continuous wet granulation/hot melt extrusion device is also available for inclusion into the continuous manufacturing line. Instrumentation for monitoring and controlling the process is also integrated into the facility (CDI-Solvias NIR spectrometers and probes, Sartorius microwaves sensor, CAMO ProcessPulse and Unscrambler signal acquisition and post-processing software, Emerson DeltaV control software). A dust collection system and dust isolation booths are present in order to minimize health and safety hazards. A laboratory manager is available for operator training, materials testing services, and research measurements.


Tote blender


Bin blender for batch mixing of API and excipients. Capacity of 5 L and 2-20 rpm speed.


Gilson SP-1 sample splitter


A large-capacity sample splitter for materials with particle sizes up to 4 in. (102 mm). The device has a hopper capacity of 1 ft3 (28.3 l) and has 48 chutes, each with a width of 0.5 in. (13 mm). The sample splitter dimensions are WxDxH 29x19x39 in. (737x483x990 mm).


Schenck AccuRate AP feeders (2)


Feed rates from 0.5 to 150 kg/hr. Made with 316L stainless steel and 32 microinch RA interior finishes provide smooth wipe down friendly surfaces. Low cost disposable flexible feed hoppers made from FDA-compliant EPDM also simplify the cleaning process and eliminate cross contamination concerns.


Gericke GCM 250/350 mixers (2)


The GCM mixer is designed as a continuous mixer with modular components. The residence time and the energy input can be varied. The output range for these mixers varies from 10 to 250 L/h.


Alexanderwerk WP-120V Roller Compactor


Roller compactor transforms cohesive powders into compacts that can be converted into granules upon milling. The WP-120V can work with as little as 5g and up to a maximum of 40kg/hour capacity. It can operate at maximal gap of 4 mm, maximum roll speed of 15 rpm and exert pressure force of 20 kN/cm. Available rolls are 120 mm in diameter and 25/40 mm in width.


16-Station Natoli BLP-16 Rotary Tablet Press


16-station rotary press with B-tooling.

Innopharmlabs Eyecon in-line/at-line image analysis system


This portable instrument uses real-time, direct imaging of particles to measure particle size distributions and 2D particle shape information for particle streams traveling at up to 10 m/s. Particle sizes between 50 and 3000 m can be measured.


Emerson DeltaV distributed control system


Widely used Distributed Control System (DCS) in pharmaceutical industry


Diosna P/VAC 10/60 High Shear Granulator/Mixer


The Diosna laboratory mixer is flexible laboratory/pilot scale high shear granulator. The machines can be equipped with 10, 25 and 60 liter high shear granulator bowls. Equipment has PLC with operating terminal.


Thermofisher Eurolab 16 Twin Screw Granulator Extruder


Twin screw melt extruder used for granulation research. Maximum output of 10 kg/hour can be achieved. The equipment operates up to 1000 pm screw speed and 400 C temperature. The extruder barrel is 16 mm in diameter with a L/D ratio of 40. Currently used for food and pharmaceutical research.


Dott. Bonapace & C. Model MP1 tumble mixer


Tumble mixer with 1 L, 2L and V-blender shells.


Coperion K-tron Model K-CV-KQX-4 volumetric feeder


Single screw volumetric feeder to handle free flowing materials such as pellets, glass beads and powders. 0.06 L/ hr to 184 L/hr capacity. Screw speed can be varied up to 1000 rpm.


Continuous Direct compression line for tablet manufacturing


The formulation is prepared by blending the API with all excipients in the continuous mixers. From the blender, the formulation enters the X-Ray system for mass flow rate measurement. It is then conveyed into the tablet press hopper using a Z-incline conveyor.

People


  • R.P. Kingsly Ambrose - Assistant Professor
    Agricultural and Biological Engineering

      SH 312
  • Stephen Beaudoin - Professor of Chemical Engineering
    Academic Director, Teaching and Learning Technology

      FRNY 1019

    Research interests: particle and thin film adhesion

  • Teresa Carvajal
    Agricultural & Biological Engineering Faculty


    Research interests: surface material science, including: investigation into surface energy, particle interactions, and functionality for dry powders; surface and interface of mobile phases, mechanical assessment of materials.

  • Srinivasan Chandrasekar - Professor
    Department of Materials Engineering

      MGL 337

    Research interests: manufacturing, materials processing, microsytems technology, nanostructured materials.

  • Weinong Chen - Aeronautics and Astronautics Associate Head for Graduate Education
    Reilly Professor of Aeronautics and Astronautics & Materials Engineering

  • Ivan C. Christov - Assistant Professor
    Mechanical Engineering

  • R. Edwin García - Professor
    Materials Engineering

  • Marcial Gonzalez - Assistant Professor
    Mechanical Engineering

      ME 3061M
  • Michael Harris - Associate Dean of Engineering for Undergraduate Education
    Robert B. and Virginia V. Covalt Professor of Chemical Engineering

      FRNY 1053

    Research interests: electrodispersion processes, dynamics of nanophase formation, impaction and drying of hydrosol and organosol drops on smooth and porous substrates, environmental control technology, materials synthesis using biotemplates.

  • Klein Ileleji - Associate Professor
    Agricultural & Biological Engineering

      ABE 309

    Research interests: biomass feedstock logistics, processing, particulate flows and handling, biofeedstock engineering systems for food, feed, fuel, and fiber production.

  • Tonglei Li - Associate Dean of Graduate Programs
    Allen Chao Chair and Professor of Industrial and Physical Pharmacy

      RHPH 124B

    Research interests: solid-state organic chemistry, computational chemistry, formulation, drug delivery.

  • Amy Marconnet - Assistant Professor
    Mechanical Engineering

  • Aaron Morris - Assistant Professor
    Mechanical Engineering

  • Zoltan Nagy - Professor
    Chemical Engineering

      FRNY G027D

    Research interests: crystallization systems engineering, control for intelligent manufacturing systems of particulate, process analytical technologies and composite sensor arrays.

  • Martin Okos - Professor
    Agricultural and Biological Engineering/Biochem and Food Processing Engineering

      FS 1171

    Research interests: food and bioprocess engineering, rheological, heat and mass transfer properties, dehydration shrinkage and swelling, compaction of viscoelastic materials, computer-aided process design.

  • Dhananjay Pai - Laboratory Manager
    Mechanical Engineering

  • Rodolfo Pinal - Director, Dane O. Kildsig Center for Pharmaceutical Processing Research
    Associate Professor of Industrial and Physical Pharmacy

      RHPH 124C

    Research interests: drug solubility and solubilzation, strategies for enhancing the bioavailability of poorly soluble drugs, prefabricated film-based dosage forms, and polymer based composites.

  • Gintaras Reklaitis - Burton and Kathryn Gedge Distinguished Professor of Chemical Engineering
    Deputy Director, NSF ERC on Structured Organic Composites

      FRNY G027B

    Research interests: application of computing, information, and systems technology for supporting complex decisions in the design and operation of processing systems, enterprise-wide optimization.

  • Fernanda San Martin - Associate Professor
    Department of Food Sciences

  • Steven Son - Professor
    Mechanical Engineering

      130 Chaffee Hall, Zucrow

    Research interests: multiphase combustion, particularly related to propellants, explosive, and pyrotechnics, nanoscale composite energetic materials, advanced energetic materials, microscale combustion.

  • Kevin Trumble - Professor
    Materials Engineering

      ARMS Room 2333

    Research interests: microstructure development in materials processing, metal-ceramic interfaces and composites.

  • Lynne S. Taylor - Professor
    Pharmacy

      RHPH 124E

    Research interests: phase transformations, physical and chemical stability, water-solid interactions, amorphous systems, solid dispersions.

  • Arvind Varma - Professor
    Chemical Engineering

      FRNY 1060C

    Research interests: hydrogen for fuel cells, underground coal gasification, carbon sequestration, combustion synthesis, chemical and catalytic reaction engineering, trickle-bed reactors.

  • Carl Wassgren - Professor
    Mechanical Engineering/Industrial and Physical Pharmacy

      ME 3003J

    Research interests: dynamics and characterization of particulate materials applied to feeding, blending, granulation, tableting, and coating.

  • Janelle P. Wharry - Assistant Professor
    Nuclear Engineering

      NUCL 132C
  • Yoon Yeo - Associate Department Head
    Industrial and Physical Pharmacy

  • Qi (Tony) Zhou - Assistant Professor
    Industrial and Physical Pharmacy

      RHPH 308B

Education


Chemical Engineering Bachelors Degree

Concentration in Pharmaceutical Engineering

Biological and Food Processing Unit Operations (ABE 55500)

Analysis and design of operations, such as sterilization, freezing, dehydration, fermentation, and separation processes. Integration of pilot plant results into the design and scale-up process systems. Emphasis on how the properties of biological materials influence the quality of the processed product.


Physical Properties of Biomaterials (ABE 305)

Course topics include physical attributes (size, density, porosity, etc.), statistical distribution of attributes; moisture measurement techniques, equilibrium moisture, moisture relationships; composition and microscopic structure related to texture, density, thermal properties and other attributes; water activity, chemical potential and water potential; coefficient of friction, angle of repose, internal angle of friction, flow patterns, flow through orifices, Rankine and Janssen equations; aerodynamic properties; thermal properties and freezing of foods and biological materials; electromagnetic properties; and force-deformation properties.


Particulate Systems (CHE 53600)

A broad overview of the fundamental concepts in particulate systems including particle characterization, particle size measurement, sedimentation, fluidization, gas and liquid conveying, particle storage, fluid-particle separation, particle size enlargement and reduction, particle mixing and hazards associated with the handling of particulate solids. Practical applications are emphasized, with a focus on how particles behave differently than fluids.


Design and Processing of Particulate Products (CHE 53800)

Characterization of particulate systems, use of population balances to describe processes that make or transform particles, applications in important unit processes including crystallization, granulation, milling, aerosol processes.


Principles of Pharmaceutical Engineering (CHE 55100)

This course is designed to provide engineering, science and pharmacy students with an understanding of the structure, economic and regulatory context, product discovery and development pipeline dynamics, intellectual property considerations and common manufacturing technology of the global pharmaceutical industry.


Pharmaceutical Process, Development, and Design (CHE 55300)

This course introduces the engineering methodologies involved in translating a laboratory recipe for a drug compound produced via synthetic organic chemistry methods to an industrial process. The basic features of common unit operations used in the pharmaceutical industry will be reviewed, including batch reaction, solid-liquid separation, crystallization, drying, mixing, batch distillation and other separation systems. Both dedicated and multi-product production system design and batch and semi-continuous operating modes will be covered.


Colloidal and Interfacial Phenomena (CHE 66800)

Preparation, characterization, and stability of emulsions, aerosols, and other multiphase dispersions. Interparticle forces, electrokinetics, thermodynamics and kinetics of coagulation. Techniques for determining size, shape, orientation, and charge of particles. Capillary and wetting phenomena. Thermodynamics of interfacial tension and adsorption. Applications to surfactants, polymers, biodispersions, flotation, separations, oil recovery, etc.


Introduction to Pharmaceutical Manufacturing Processes (IPPH 56200)

A course intended to provide the student with basic understanding of both the theoretical and practical aspects of pharmaceutical manufacturing by combining a thorough classroom treatment of the underlying principles of each pharmaceutical unit operation with hands-on execution of these activities in the laboratory.


Spray Applications and Theory (ME 52600)

Theory of spray formation and evolution as well as treating a host of spray applications. Topics include drop size distributions, breakup of liquid sheets and ligaments, drop formation and breakup, drop motion and the interaction between a spray and its surroundings, drop evaporation, nozzle internal fluid mechanics, external spray characteristics, nozzle performance, and experimental techniques relevant to these subjects. Applications include: (1) agricultural sprays, (2) consumer products, (3) gas turbine combustion, (4) heat transfer, (5) internal combustion engines, (6) paints and coatings, (7) pharmaceutical and medicinal sprays, and (8) spray drying.


Particle, Powder, and Compact Characterization (ME 53100)

The goal of this course is to familiarize students with the properties and methods used to characterize the mechanical behavior of particles, powders, and compacts, with the intention of using these properties for process and performance design. Students will work with a subset of the measurement methods in a laboratory setting. Students successfully completing the course will be able to: (1) define and describe the significant properties of particles, powders, and compacts; (2) describe and demonstrate techniques used to measure these properties; and (3) demonstrate how these properties are useful in product and manufacturing performance.


Powder Processing (MSE 51200)

Processing of engineering materials from powders. Synthesis of metals, ceramics, and polymers in powder form. Characteristics of particulates. Behavior of collections of particles; surface forces, particle agglomeration and dispersion, gelation, particle packing. Consolidation of powders; mechanics of dry flow and compaction, slurry rheology, shaping processes. Densification and microstructural development; geometry, thermodynamics, and kinetics of sintering, liquid-phase sintering, reaction densification, infiltration. Powder processing of composites.


Collaborating Centers


Contact

Center for Particulate Products and Processes
Dr. Carl Wassgren
585 Purdue Mall
ME 3003J (Office)
West Lafayette, IN
47907-2088
wassgren@purdue.edu