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1、laParticle size analysis-Laser diffraction methods(ISO-13320-1)Introduction Laser diffraction methods are nowadays widely used for particle sizing in many different applications.The success of the technique is based on the tact that it can be applied to various kinds of particulate systems,is fast a
2、nd can be automated and that a variety of commercial instruments is available.Nevertheless,the proper use of the instrument and the interpretation of the results require the necessary caution.Therefore,there is a need for establishing an international standard for particle size analysis by laser dif
3、fraction methods.Its purpose is to provide a methodology for adequate quality control in particle size analysis.Historically,the laser diffraction technique started by taking only scattering at small angles into consideration and,thus,has been known by the following names:-fraunhofer diffraction;-(n
4、ear-)forward light scattering;-low-angle laser light scattering(LALLS).However,the technique has been broadened to include light scattering in a wider angular range and application of the Mie theory in addition to approximating theories such as Fraunhofer and anomalous diffraction.The laser diffract
5、ion technique is based on the phenomenon that particles scatter light in all directions with an intensity pattern that is dependent on particle size.All present instruments assume a spherical shape for the particle.Figure 1 illustrates the characteristics of single particle scattering patterns:alter
6、nation of high and low intensities,with patterns that extend for smaller particles to wider angles than for larger particles2-7,10,15 in the bibliography.Within certain limits the scattering pattern of an ensemble of particles is identical to the sum of the individual scattering patterns of all part
7、icles present.By using an optical model to compute scattering for unit volumes of particles in selected size classes and a mathematical deconvolution procedure,a volumetric particle size distribution is calculated,the scattering pattern of which fits best with the measured pattern(see also annex A).
8、A typical diffraction instrument consists of a light beam(usually a laser),a particulate dispersing device,a detector for measuring the scattering pattern and a computer for both control of the instrument and calculation of the particle size distribution.Note that the laser diffraction technique can
9、not distinguish between scattering by single particles and 名师资料总结-精品资料欢迎下载-名师精心整理-第 1 页，共 31 页 -scattering by clusters of primary particles forming an agglomerate or an aggregate.Usually,the resulting particle size for agglomerates is related to the cluster size,but sometimes the size of the primary
10、 particles is reflected in the particle size distribution as well.As most particulate samples contain agglomerates or aggregates and one is generally interested in the size distribution of the primary particles,the clusters are usually dispersed into primary particles before measurement.Historically
11、,instruments only used scattering angles smaller than 14,which limited the application to a lower size of about 1m.Thereason for this limitation is that smaller particles show most of their distinctive scattering at larger angles(see also annex Z).Many recent instruments allow measurement at larger
12、scattering angles,some up to about 150,for example through application of a converging beam,more or larger lenses,a second laser beam or more detectors.Thus smaller particles down to about 0.1 m can be sized.Some instruments incorporate additional information from scattering intensities and intensit
13、y differences at various wavelengths and polarization planes in order to improve the characterization of particle sizes in the submicrometre range.Particle size analysis Laser diffraction methods-Part 1:General principles 1 scope This part of ISO 13320 provides guidance on the measurement of size di
14、stributions of particles in any two-phase system,for example powders,sprays,aerosols,suspensions,emulsions and gas bubbles in liquids,through analysis of their angular light scattering patterns.It does not address the specific requirements of particle size measurement of specific products.This part
15、of ISO13320 is applicable to particle sizes ranging from approximately 0.1m to 3m.For non-spherical particles,an equivalent-sphere size distribution is obtained because the technique uses the assumption of spherical particles in its optical model.The resulting particle size distribution may be diffe
16、rent from those obtained by methods based on other physical principles(e.g.Sedimentation,sieving).3,terms,definitions and symbols For the purposes of this part of ISO 13320,the following terms,definitions and symbols apply.3.1 terms,definitions 3.1.1 absorption 名师资料总结-精品资料欢迎下载-名师精心整理-第 2 页，共 31 页 -i
17、ntroduction of intensity of a light beam traversing a medium through energy conversion in the medium 3.1.2 coefficient of variation(变异系数)Noative measure(%)for precision:standard deviation divided by mean value of population and multiplied by 100 or normal distributions of data the median is equal to
18、 the mean 3.1.3complex refractive index（）Refractive index of a particle,consisting of a real and an imaginary(absorption)part.Np=np-ikp3.1.4 relative refractive index（m）complex refractive index of a particle,relative to that the medium。3.1.5 deconvolution Mathematical procedure whereby the size dist
19、ribution of a particle ensemble is inferred from measurements of their scattering pattern.3.1.6 diffraction Spreading of light around the contour of a particle beyond the limits of its geometrical shadow with a small deviation from rectilinear propagation 3.1.7 extinction Attenuation of a light beam
20、 traversing a medium through absorption and scattering.3.1.8 model matrix Matrix containing light scattering vectors for unit volumes of different size classes,scaled to the detector s geometry,as derived from model computation.3.1.9multiple scattering Subsequent scattering of light at more than one
21、 particle,causing a scattering pattern that is no longer the sum of the patterns from all individual particles(in contrast to single scattering)3.1.10 obscuration Optical concentration Percentage or fraction of incident light that is attenuated due to extinction(scattering and/or absorption)by the p
22、articles 3.1.11 optical model Theoretical model used for computing the model matrix for optically homogeneous spheres with,if necessary,a specified complex refractive index,e.g.Frauhofer diffraction,anomalous diffraction,Mie scattering 3.1.12 reflection Return of radiation by a surface,without chang
23、e in wavelength 3.1.13 refraction 名师资料总结-精品资料欢迎下载-名师精心整理-第 3 页，共 31 页 -Change of the direction of propagation of light determined by change in the velocity of propagation in passing from one medium to another,in accordance with Snell s law Nmsinm=npsinp3.1.14 scattering General term describing the c
24、hange in propagation of light at the interface of two media 3.1.15 scattering pattern Angular or spatial pattern of light intensitiesI()and I(r)respectively originating from scattering,or the related energy values taking into account the sensitivity and the geometry of the detector elements 3.1.16 s
25、ingle scattering Scattering whereby the contribution of a single member of variation(relative percentage)of the size distribution NOTE for normal distributions about 95%of the population falls within 2 standard deviations from the mean value and about 99.7%within 3 standard deviations from the mean
26、value.3.2 symbols 4 principle A representative sample,dispersed at an adequate concentration in a suitable liquid or gas,is passed through the beam of a monochromatic light source,usually a laser.The light scattered by the particles at various angles it measured by a multi-element detector and numer
27、ical values relating to the scattering pattern are then recorded for subsequent analysis.These numerical scattering values are then transformed,using an appropriate optical model and mathematical procedure,to yield the proportion of total volume to a discrete number of size classes forming volumetri
28、c particle size distribution.Laser diffraction instrument In the conventional set-up,a light source(typically a laser)is used to generate a monochromatic,coherent,parallel beam.This is followed by a beam processing unit,usually a beam expander with integrated filter,producing a extended and nearly i
29、deal beam to illuminate the dispersed particles.A representative sample,dispersed at an adequate concentration is passed through the light beam in a measuring zone by a transporting medium(gas or liquid);this measuring zone should be within the working distance of the lens used.Sometimes,the particl
30、e stream in a process is illuminated directly by the laser beam for measurement,as in 名师资料总结-精品资料欢迎下载-名师精心整理-第 4 页，共 31 页 -the case of sprays,aerosols and air bubbles in liquids.In other cases(such as emulsions,pastes and powders),representative samples can be dispersed in suitable liquids(see annex
31、 C).Often dispersants(wetting agents:stabilizers)and/or mechanical forces(agitation;ultrasonication)are applied for deagglomeration of particles and stabilization of the dispersion.For these liquid dispersions a recirculating system is most commonly used,consisting of an optical measuring cell,a dis
32、persion bath usually equipped with stirrer and ultrasonic elements,a pump and tubing.Dry powders can also be converted into aerosols through application of dry powder dispersers,which apply mechanical forces for deagglomeration.Here a dosing device feeds the disperser with a constant mass flow of sa
33、mple.The disperser uses the energy of a compressed gas or the differential pressure to a vacuum to disperse the particles It outputs an aerosol that is blown through the measuring zone,usually into the inlet of a vacuum pipe that collects the particles.There are two positions in which the particles
34、can enter the laser beam.In the conventional case the particles enter the parallel beam before and within the working distance of the collecting lens see Figure 3-a.In the so-called reversed Fourier optics case the particles are entered behind the collecting lens and,thus,in a converging beam see Fi
35、gure 3-b.The advantage of the conventional set-up is that a reasonable path length for the sample is allowed within the working distance of the lens.The second set-up allows only small path lengths but enables measurement of scattered light at larger angles,which is useful when submicrometre particl
36、es are present.The interaction of the incident light beam and the ensemble of dispersed particles results in a scattering pattern with different light intensities at various angles(see annex a for theoretical background of laser diffraction),the total angular intensity distribution I(),consisting of
37、 both direct and scattered light,is then focused by a positive lens or an ensemble of lenses onto a multi-element detector.The lens(es)provide(s)for a scattering pattern which,within limits,is not dependent upon the location of the particles in the light beam.So,the continuous angular intensity dist
38、ribution I()is converted into a discrete spatial intensity distribution I(r)on a set of detector elements.It is assumed that the recorded scattering pattern of the particle ensemble is identical to the sum of the patterns from all individual single scattering particles presented in random relative p
39、ositions.Note that only a limited angular range of scattered light is collected by the lens(es)and,thus,by the detector.The detector generally consists of a number of photodiodes;some instruments apple one photodiode in combination with moving slits.The photodiodes convert the spatial intensity dist
40、ribution I(r)into a set of 名师资料总结-精品资料欢迎下载-名师精心整理-第 5 页，共 31 页 -photocurrents In,subsequent electronics then convert and digitize the photocurrents into a set of intensity or energy vectors Ln.Representing the scattering pattern.A central element measures the intensity of the non-scattered light and
41、,thus,with a calculation,provides a measure of optical concentration or obscuration.Some instruments provide special geometries of the central element in order to automatically re-centre or re-focus the detector by moving the detector or the lens.It is desirable that the detector elements are positi
42、oned so as to prevent the light reflected from the surface from re-traversing the optical system.A computer controls the measurement and is used for storage and manipulation of the detected signals,for storage and/or calculation of a proper form of the optical model(usually as a model matrix contain
43、ing light scattering vectors per unit of volume per size class,scaled to the detector s geometry and sensitivity)and calculation of the particle size distribution(see annex a for theoretical background of laser diffraction).Also it may provide automated instrument operation.Several significant diffe
44、rences exist,both in hardware and software,not only between instruments from different manufacturers but also between different types from one company.The instrument specifications should give adequate information for proper judgement of these differences.In annex B recommendations are presented for
45、 the specifications of laser diffraction instruments.6 operational procedures 6.1 requirements 6.1.1 instrument location The instrument should be located in a clean environment that is free from excessive electrical noise,mechanical vibration,and temperature fluctuations and is out of direct sunligh
46、t.The operating area should be well ventilated.The instrument should either contain a rigid internal optical bench or be installed on a rigid table or bench to avoid realignment of the optical system at frequent intervals.Warning：the radiation of instruments equipped with a low power laser can cause
47、 permanent eye damage.Never look into the direct path of the laser beam or its reflections.Avid cutting the laser beam with reflecting surfaces.Observe the local laser radiation safety regulations.6.1.2 dispersion liquids Any optically transparent liquid of known refractive index may be used.Thus,a
48、variety of liquids is available for preparation of liquid dispersions of powders.Annex c provides requirements for the dispersion liquids.If an organic liquid is used for dispersion,observe the local health and safety regulations.Use a cover for the ultrasonic bath when using 名师资料总结-精品资料欢迎下载-名师精心整理-
49、第 6 页，共 31 页 -liquids with a high vapour pressure in order to prevent the formation of hazardous vapour concentrations above the bath and/or the generation of low-temperature zones with fluctuating refractive indices in the fluid by evaporation.6.1.3 dispersion gases For dry dispersion and spray app
50、lications a compressed gas is sometimes used.If used,it is essential that it is free from oil,water and particles.To achieve this,a dryer with a filter is required.Any vacuum unit should be located apart from the measurement zone,so that the output of the hot air does not reach the measuring zone,dr