Laser diffraction for particle sizing

Introduction: By far the most important physical property of particulate samples is particle size. Particle size measurement is routinely carried out across a wide range of industries and is often a critical parameter in the manufacture of many products. Particle size has a direct influence on material properties such as:

Reactivity or dissolution rate - e.g. catalysts, tablets Stability in suspension e.g. sediments, paints Efficacy of delivery e.g. asthma inhalers Texture and feel e.g. food ingredients Appearance e.g. powder coatings and inks Flowability and handling e.g. granules Viscosity e.g. nasal sprays Packing density and porosity e.g. ceramics

Measuring particle size and understanding how it affects your products and processes can be critical to the success of many manufacturing businesses. The link between particle size and product performance is well documented with regards to dissolution, absorption rates and content uniformity. Reducing particle size can aid the formulation of NCEs (New Chemical Entities) with poor water solubility. Proper matching of active ingredient and excipient particle size is important for several process steps. Particle size analysis is an integral component of the effort to formulate and manufacture many pharmaceutical dosage forms. Laser diffraction: Laser diffraction is the most popular particle size analysis technique used in the pharmaceutical industry. Laser diffraction is a widely used particle sizing technique for materials ranging from hundreds of nanometers up to several millimeters in size. The main reasons for its use are:

Wide dynamic range - from submicron to the millimeter size range. Rapid measurements - results generated in less than a minute. Repeatability - large numbers of particles are sampled in each measurement. Instant feedback - monitors and controls the particle dispersion process.

High sample throughput - hundreds of measurements per day. Calibration not necessary - easily verified using standard reference materials.

Principle Laser diffraction measures particle size distributions by measuring the angular variation in intensity of light scattered as a laser beam passes through a dispersed particulate sample. Large particles scatter light at small angles relative to the laser beam and small particles scatter light at large angles, as illustrated below. The angular scattering intensity data is then analyzed to calculate the size of the particles responsible for creating the scattering pattern, using the Mie theory of light scattering. The particle size is reported as a volume equivalent sphere diameter.

Scattering of light from small and large particles. Assumptions of Laser diffraction: Spherical, non-porous and opaque particles, Diameter d > wavelength l, Particles are distant enough from each other, Random motion, All the particles diffract the light with the same efficiency, regardless of their shape

Optical properties Laser diffraction uses Mie theory of light scattering to calculate the particle size distribution, assuming a volume equivalent sphere model.

Mie theory requires knowledge of the optical properties (refractive index and imaginary component) of both the sample being measured, along with the refractive index of the dispersant. Usually the optical properties of the dispersant are relatively easy to find from published data, and many modern instruments will have in-built databases that include common dispersants. For samples where the optical properties are not known, the user can either measure them or estimate them using an iterative approach based upon the goodness of fit between the modeled data and the actual data collected for the sample. Mie Theory: The Mie model takes into account both diffraction and diffusion of the light around the particle in its medium. To use the Mie model, it is necessary to know the complex refractive index of both the sample and the medium. This complex index has a real part, which is the standard refractive index, and an imaginary part, which represents absorption. Complex index = m m=a+b where a: real part, b: imaginary part. Instrumentation:

Photo courtesy (http://www.shimadzu.com) As shown in Figure, the diffracted/scattered light intensity distribution pattern is generated spatially when a measurement target particle group is irradiated with a laser beam. The light intensity distribution pattern of the forward scattered light is condensed by the lens, and a ringshaped diffracted/scattered image is formed on the detecting plane located at the focal distance. This is detected by a ring sensor comprising sensing elements placed concentrically. Side scattered light and backward scattered light are detected by side scattered light sensors and backward scattered light sensors, respectively. In this way, various sensing elements are used to

detect the light intensity distribution pattern to obtain light intensity distribution data. The light intensity distribution data changes according to the size of the particle. Because actual samples contain a mixture of different size particles, the light intensity distribution data generated from a particle group is the result of overlaid diffracted/scattered light from each respective particle. References: BASIC PRINCIPLES OF PARTICLE SIZE ANALYSIS Written by Dr. Alan Rawle,Malvern Instruments Limited, Enigma Business Park, Grovewood Road, Malvern, Worcestershire, WR14 1XZ, UK. Tel: +44 (0)1684 892456 Fax: +44 (0)1684 892789 illavenkatesa A, Dapkunas S J, Lin-Sien Lum, Particle Size Characterization, NIST Special Publication 960-1, 2001 Laser Diffraction Particle Size Measurement of Food and Dairy Emulsions Using Equipment from Malvern Particle size distributions in skim milk by C. Holt, D.G. Dalgleish, T.G. Parker Hannah Research Institute, Ayr, KA6 5HL Great Britain Received 12 June 1973. Available online 28 January 2003 Particle size distribution analysis of soils using laser diffraction S. Wanogho, G. Gettinby, B. Caddy Forensic Science Unit, University of Strathclyde, Royal College, 204 George Street, Glasgow G1 1XH UK Department of Mathematics, University of Strathclyde, Glasgow G1 1XH UK Received 20 November 1985. Revised 30 June 1986. Accepted 27 August 1986. Available online 2 April 2004. New developments in particle characterization by laserdiffraction: size and shape Zhenhua Ma, Henk G Merkus, Jan G.A.E de Smet, Camiel Heffels, Brian Scarlett 7 July 2000. Sivakugan N, Soil Classification, James Cook University Geoengineering lecture handout, 2000 Terence Allen, ed. (2003). Powder sampling and particle size determination (1st ed. ed.). Amsterdam: Elsevier. ISBN 978-0-444-51564-3. Retrieved 22 August 2011. Fieller, N.R.J; Gilbertson, D.D. and Olbricht, W (1984). "A new method for environmental analysis of particle size distribution data from shoreline sediments". Nature 311 (5987): 648651.