CH 502 : Experimental & Analytical Methods in Chemical Engineering

Particle Size Analysis

Material Science
Material Synthesis

Polymer Science & Engineering

Nucleation, Polymerization

Environmental Engineering
Size distribution of colloids in the environment Atmospheric Aerosols

Catalysts Aerosol Science

Laser Diffraction
Fraunhofer Theory
Scattering of light on large particles compared to the wavelength of incident light Spherical , non-porous and opaque particles

http://www.cilasus.com/theory/

Laser Diffraction
Mie Theory
Diffraction on particles with relatively larger particles compared to the wavelength of incident light (d = 1-10 ) Diffraction and Diffusion Necessary to know refractive index of particle and medium

http://www.cilasus.com/theory/

Laser Diffraction
Mie Theory

http://www.sympatec.com/LaserDiffraction/LaserDiffraction.html

Laser Diffraction

Intensity Distribution of Diffraction from a small particle on a semi-circular photo-detector

Multi-Element Photo Detector Simultaneous Diffraction Superposition of Diffraction Patterns If Particles are moving the- diffraction between particles are evened out

http://www.sympatec.com/LaserDiffraction/ LaserDiffraction.html

http://www.microtrac.com/laserdiffraction .cfm

Laser Diffraction

Single Wavelength Laser e.g.: HeNe laser at 632.8 nm Algorithms to calculate the particle size from simultaneous spectra Particle Size Range: 0.1 micron to 1000 micron

http://www.sympatec.com/LaserDiffraction/ LaserDiffraction.html

http://www.microtrac.com/laserdiffraction .cfm

Dynamic Light Scattering

Light Scattering in all Directions when Light hits Small Particles
Brownian Motion Rayleigh Scattering Particles smaller than the wavelength (< 250 nm)

Laser
Coherent and Monochromatic Source Known Frequency

Interception with moving particles

Light Scattering occurs at different frequency Doppler Shift

Doppler Shift
Related to Particle Size Smaller particles are moving at higher velocity and cause higher shift Difference in frequency used to calculate the sizes of particles present Photomultiplier Tube Detector to measure photons

Typical particle size ranges in commercial instruments: 1 nm 1micron

Dynamic Light Scattering

http://www.brookhaveninstruments.com/DLSBasics.html

Dynamic Light Scattering

Auto-Correlation Function is an exponential decay in time Each monodisperse particle collection has a characteristic exponential decay A mixture of particle size produce a sum of exponentials Mathematical algorithms used to extract particle size information from these curves

http://www.brookhaveninstruments.com/ DLSBasics.html

Particle Size Analyzers

Provide an Equivalent Spherical Diameter Particle shape is usually not taken into consideration Output calculations include
Mean diameter Cut-off diameters ( e.g: 10%, 50%, 90% ) Standard deviations

Analysis depends on the concentration of particles

Optimum concentration required for reliable readings

Particle Size Analyzers

Provide an Equivalent Spherical Diameter Particle shape is usually not taken into consideration Particle shape is analyzed using Microscopy
Light or Electron Light Microscopy can be performed with static or flowthrough systems Pulsed light source and High speed Video Camera Image Analysis Some modern instruments combine particle size and shape in one instrument

Output calculations include

Mean diameter Cut-off diameters ( e.g: 10%, 50%, 90% ) Standard deviations

Analysis depends on the concentration of particles

Optimum concentration required for reliable readings

Microscopy for Particle Size Analysis

Direct Method Image Acquisition
Optical Microscopy (microns) Electron Microscopy
SEM (micron to submicron) TEM (nano particles)

Image Analysis
Based on contrast difference Projected area of particles Distribution

Microscopy for Particle Size Analysis

http://www.fyslab.hut.fi/nanomat/EM_pages_Rdrive

Electrostatic Separation
Differential Mobility Analyzer
Particles pass through a radioactive bipolar charger Differential Charging Electric field inside affects flow trajectory of charged particles Negatively charged particles go towards the outer wall Particles with narrow range of electrical mobility exit the system

Condensation Nuclei Counter (CNC)

Particles are considered as nucleus Growth of particles by condensation of vapor on the surface When particle reaches a certain state, measurement is performed by either diffraction or scattering technique DMA + CNC = SMPS (Scanning Mobility Particle Sizer) Primary application in Aerosol Science

Flow field Fractionation

http://www.wyatt.com/solutions/hardware/Field-Flow-Fractionation-Theory.cfm

Surface Area / Porosity Measurement

BET Isotherm

Nitrogen or Krypton at 77K is used in the experiment Filling of micropores, mesopores and macropores with increasing pressure Surface area calculated from the monolayer coverage Pore size distribution needs entire isotherm Differential pressure measurements are used to estimate the volume at each pore volume Macro pore size distribution
Hg Intrusion Porosimetry Surface area of N2 is known

Applicable for surface area measurements and micropore size distribution http://www.refiningonline.com

www.micromeritrics.com

Velocity Field
Hot Wire Anemometers A wire (e.g. tungsten) is heated above ambient temperature As flow occurs through the wire, it cools Affects the electrical resistance in the wire Temperature/Resistance calibrated to wind velocity

www.efunda.com www.inotek.com

Velocity Field
Cup Anemometer The counter records the number of turns and converts to windspeed Used in meteorology Micro versions are used for small speeds Windmill Anemometers

wikipedia

Velocity Field Pressure Anemometers

Pitot Tube Measures pressure and correlates to velocity Applicable in very high flow conditions e.g: Wind tunnel, aircrafts

www.efunda.com

Velocity Field LDV

Laser Doppler Velocimetry Velocity of fluid particles Two beams of collimated monochromatic lasers Microscopic pattern of bright and dark stripes form in the intersection volume Small particles coming this region reflect light towards a detector Frequency of light is affected by the velocity through the Doppler effect Unreliable near solid surfaces

http://www.lavision.de/images/techniques/ldv_pdi.jpg

Velocity Field PIV

Particle Image Velocimetry Double pulsed laser source Optics to convert laser to light sheet Digital Camera Tracer Particles that do not disturb the flow field are used Scattering from the particles Scattered light captured by camera
http://www.tfhrc.gov/pubrds

http://www.tfhrc.gov/pubrds

Temperature
Thermocouples Thermoelectric or Seebeck effect Thermal gradient applied to a conductor voltage Types K Ni-Cr/Ni-Al ( -200C 1200 E - Ni-Cr/Ni-Cu (cryogenic) J Fe/Cu-Ni (-40C 750C) N Ni-Cr-Si/Ni-Si (>1200C)
www.efunda.com

Solid-state Infra-red sensors

http://www.allqa.com/probes