Anal. Chem. 1989, 61, 143R-152R
Particle Size Analysis Howard G.B a r t h *
D u Pont Company, Experimental Station, P.O. Box 80228, Wilmington, Delaware 19880-0228
Shao-Tang Sun
Hercules Incorporated, Research Center, Wilmington, Delaware 19894
INTRODUCTION
Table I. Review Contents
Particle size analysis is an extremely broad area that covers a wide range of applications and techniques. In past reviews (Al,A2),we have attempted to include as many major techniques as possible that could be of interest to analytical chemists and others involved in particle size analysis. In this paper, we have been more selective and have deleted sections on microscopy/image analysis and aerosol measurement devices, which are themselves highly specialized areas and include ancillary techniques that are outside the scope of this review. Methodologies that are included are listed in Table I. We continue to see a steady rise in the introduction and use of laser-light scattering instrumentation based on photon correlation spectroscopy, Fraunhofer diffraction, and classical scattering techniques. Of the chromatographic techniques, the number of papers in field-flow fractionation has continued to grow. Literature searches were based on Chemical Abstracts 1986, 105(23),through 1988, 109(24),for relevant papers dealing with new developments and advances in particle size analysis mainly in English, French, German, and Russian. Except for hydrodynamic chromatography and field-flow fractionation, papers dealing with macromolecules in solution and micelles were not covered. Because of the enormous breadth of topics, in terms of sample type, technique, and particle size range, different search strategies were used to include as many pertinent articles as possible. T o this end, we gratefully acknowledge Ruth Curtiss, Hercules Inc., and Neil Feltham, Du Pont Co., for their assistance and advice regarding search routines.
development. Luerkens et al. ( A l l ) presented an overview of particle size and shape characterization. Sheppard (Al2) gave a brief review of instruments for use in particle analysis.
GENERAL BOOKS AND REVIEWS
SCAlTER ING TECHNIQUES
Provder (A3)edited an ACS Symposium Series on particle size analysis with emphasis on measurement techniques, methodology, and application to a variety of particulate systems. Included are sections on image analysis, lightscattering measurements, disk centrifuge photosedimentometry, field-flow fractionation, and chromatographic techn iq u es. Svarovsky's book on methods of measuring physical properties of bulk powders (A4)is a guide to test methods for the Characterization of powders. Included are chapters on particle size analysis and characterization, behavior and properties of powders, and grinding of particles. A volume on particle analysis was recently written by Lloyd (A5). Muller (A6)reported on the Fifth Conference of Granulometrie which was organized by the Technische Universitat Dresden and the GDR Association of Engineers Kammer der Technik and held in December, 1987, in Dresden. Buttner (A7) summarized the Gesellschaft Verfahrenstechnik und Chemieingenieurwesen topical group on Particle Characterization held in Wurtzburg in May, 1987. A brief but informative biography of Rammler, who contributed to many as ects of particle science and technology, was written by Schugert and Wachtler (A8). Freshwater (A9) described the achievements of Heywood who had made significant contributions in the measurement of particle size and shape. Polke (AlO) summarized the characteristics of particles, with emphasis on particle shape, and its impact on product
Light, neutron, and X-ray scattering techniques have been used extensively to study the structure and dynamics of particles and macromolecules in multicomponent systems. In a typical experiment, an incident beam probes the medium of interest and the scattered radiation is analyzed with a suitable spectrometer. The momentum and energy differences between the scattered and the incident radiations characterize the structure and dynamics of the medium. In the case of classical light scattering, the radius of gyration of the particle is determined from the wave vector dependence or angular dependence of the time-averaged scattering intensity. With photon correlation spectroscopy (PCS),the size information is obtained from the time-dependent fluctuations resultin from Brownian motion of particles. The fiffusion coefficient of the Brownian particles is determined from the intensity autocorrelation function measured experimentally with a digital correlator. The hydrodynamic radius is then calculated from the diffusion coefficient by using the Stokes-Einstein relation. This method is used to probe cm. The power of PCS particle sizes ranging from lo-' to lies in its relative ease of use, rapid determination of diffusion coefficients with high precision ( 1 pm could be analyzed. Bauckhage and colleagues (H3, H4)developed a new laser-Doppler technique based on the phase Doppler difference method for simultaneous size and velocity measurements. Predictions of local particle fluxes and kinetic energy fluxes in multiphase flows could then be made. Preconditions for proper use of the method were carefully spelled out and discussed. Bachalo (H5)examined the theories for light scattering interferometry and phase Doppler method. The problem of combined light scattering with reflection and refraction was addressed. Monodisperse-drop streams were used to demonstrate the need for sophisticated instrumentation. Kliafas et al. (H6)analyzed the errors in particle sizing by laser Doppler anemometer due to flow turbidity in the incident laser beam. The random error increased as the diameter ratio of the laser beam and particulate phase decreased. Systematic errors corresponded to 10% underestimation of sizes. The root-mean-square error increased with increasing diameter. Horrocks and co-workers (H7) adapted a two-color laser Doppler particle monitoring system to measure the charge and size of particles in the wake region of a precipitator. Chevaillier et al. (H8) developed an apparatus combining a laser Doppler velocimeter and particle sizing system. Simultaneous measurements of size and velocity of sphereical particles in the range 10-500 pm and 1 cm/s to 5 m/s were achieved. Yianneskis (H9) reviewed the technique of laser-Doppler velocimetry for the determination of the velocities and/or of the sizes of particles in multiphase flows. The determination of particle concentration was also examined.
Khorramian et al. (J4) examined the usefulness of smallangle X-ray scattering in size analysis with a Kratky camera under a small entrance-slit/counter-slitcombination. Measurements on samples of high-molecular-weight polystyrene in methyl ethyl ketone were made and results were compared to those from light scattering. Kranold and Goecke (J5) characterized particle size and specific surface area of silicon nitride and Seiditz kaolin powders. The results obtained by scattering techniques were compared with those from gas adsorption and sedimentation analysis. The structure of partially crystalline maltodextrin gel was determined by Gernat et al. (J6)using wide-angle X-ray scattering. The presence of microcrystalline domains of polysaccharide chains was found at the junction zones of the network. The dimensions of the microcrystallites were calculated. De Angelis et al. (J7)applied synchrotron X-ray scattering to measure particle-size distributions of catalysts. The effect of calcination temperature on the particle size of nickel supported on silica was studied. Deslandes et al. (J8)investigated the average agglomerate sizes of carbon black dispersions in polystyrene and epoxy resins by using both small-angle X-ray scattering and transmission electron microscopy. The inner specific surface areas were deduced from X-ray data. The size distributions and shapes were determined by TEM. Stradomskii et al. (J9) characterized the particle size distribution of soot from kerosine combustion in a direct-flow chamber with SAXS and electron microscopy. The integral intensity of optical emission of the flame was obtaine and used to evaluate the thermal stress at the chamber walls.
Neutron Scatterlng
ELUTION TECHNIQUES
Hayter (11)surveyed small-angle neutron scattering. He focused on the analysis of particles size, charge, and polymer latex structures under shear flow. Fisher et al. (12) used small-angle neutron scattering (SANS) to study interfacially polymerized core-shell latexes. Deuterated methyl methacrylate and styrene formed a shell around performed poly(methy1 methacrylate) latexes via emulsion polymerization. The locus of polymerization of the deuterated monomers was thus at the latex surface. Feeney et al. (13)measured particle nucleation at an early stage of emulsion polymerization. Average radius of polystyrene particles of -6 nm was obtained. An interesting sample preparation technique was used which involved the use of polyacrylamide gels. Wai et al. (14) characterized the morpholo y of seeded emulsion-polymerized latex particles. A core-&ell structure was determined by SANS technique. Agamalyan and colleagues (15,16) studied radiation-grafted acrylic acid-ethylene copolymer. The grafted poly(acry1ic acid) in polyethylene showed phase-separated domains or particles with 3 nm in diameter determined from neutron scattering. Plestil et al. (17)investigated the morphology of collapsed gels of poly(NJV-diethylacrylamide)in deuterated water. Compact globular structures were found in both gel networks and solutions in the collapsed phase. The presence of charges on the polymer chains shifted the phase-transition temperature by 10-15 OC. Detailed comparison of SANS and X-ray diffraction was made on alloy precipitates by Spooner et al. (18). Size distribution of cobalbrich precipitates in c o p p e m b a l t alloy was characterized by both SANS and wide-angle X-ray diffraction methods. Murthy and Aharoni (19) described X-ray and neutron scattering studies of poly(ester carbonate) poly(ethylene terephthalate) alloys. Quenched blends of di ferent compositions were characterized. Complete phase separation took place upon annealing.
Elution techniques are those methods in which a sample is injected into a flowing stream and particles are separated by means of hydrodynamics or by the distribution between two phases. Techniques that utilize the former mechanism are hydrodynamic chromatography (HDC), field-flow fractionation (FFF),and more recently planetary coil centrifugation (also called angle-rotor-coil planet centrifuge which is really a subtechnique of FFF). Size exclusion chromatography is based on the latter mechanism.
4
X-ray Scatterlng
Frydrychowicz et al. (51)described the use of Tikhnov’s regularization orithm for the evaluation of X-ray diffraction data. The size istribution function of silver sulfide colloids in gelation was studied. The crystallite size distribution of magnesium oxide powder was characterized. Volodin and co-workers (52,53) developed a Monte Carlo method to calculate X-ray scattering intensity for multiphase heterogeneous slurry analysis. The scattered coherent X-ray intensity was calculated as a function of slurry particle size.
9.
Size Exclusion Chromatography
Hamielec and co-workers ( K I )reviewed the use of SEC and turbidity measurements to measure the particle-size distribution of latexes in the submicrometer range. This group (K2) also investigated the applicability of universal particle-size calibration for SEC of latexes using porous-glass packings with a number of different mobile phase compositions. Nunes and reported on the fractionation of a water-based ferYu (K3) rofluid, ranging in diameter from 73 to 165A, using Sepharose as the packing. Elution Centrlfugation
Sutherland (K4)reviewed the fundamental principles and applications of an angle-rotor-coil planet centrifuge for countercurrent chromatography of biological particles and biopolymers. Aoki et al. (K5) derived a simple relationship between the particle velocity along the tube length and operational parameters (tube radius, angular velocity, and sedimentation velocity) in a rotating tube used for particle separation. A patent was awarded to Ito (K6) for an angle-rotor-coil planet centrifuge for particle separation. Hydrodynamlc Chromatography
In hydrodynamic chromatography (HDC), the separation can take place in columns packed with either porous or nonporous packings, as well as in empty capillary columns. In packed columns, velocity gradients produced by the flow of mobile phase through the interstices of the packing are responsible for separations. Smaller particles will tend to sample velocity streamlines near the packing surface and will travel at a lower average velocity than larger particles, resulting in the elution of large particles first. With porous packings the separation mechanism is more complex. Not only are hydrodynamic processes occurring but also size exclusion effects can take place. In capillary HDC, also called tubuANALYTICAL CHEMISTRY, VOL. 61, NO. 12, JUNE 15, 1989
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to characterize the atomic bonding properties of these and related materials. IR measurements tend to emphasize the H bonding environments while Raman scattering emphasizes the Si network vibrational modes. IR spectroscopy has continued to be used to characterize the H environments in hydrogenated amorphous Si and alloy filmsunder various growth and processing conditions ( D l 13-01 19). Hydrogenated amorphous S i c alloys combined with a-SkH films could prove useful for photovoltaic applications, and a-SiC:H films grown under different conditions have been characterized with IR spectroscopy (0120,0121).The defects in the bandgap of the films have been measured by using the optical technique, photothermal deflection spectroscopy (0122).Raman spectroscopy has been used to characterize hydrogenated amorphous carbon, a-C:H (0123,0124),and S i c layers have been detected a t the interface of the a-C:H and the Si substrate (0123). The H environments of amorphous carbon nitride films have been characterized by IR (0125). IR measurements have been combined with Raman scattering to characterize a-Si:H films with microcrystalline structures (0126-0128).In a related material, Raman scattering has been used to study the oxidation of polycrystalline Si which results in semiinsulating polycrystalline Si or SIPOS (0129). Recent advances in CVD techniques have demonstrated the deposition of diamond filmson Si and other substrates. These films have many potential applications including optical coatings, use as wide band gap semiconductors, and X-ray windows. Raman scattering has proven particularly useful for distinguishing between diamond and graphitic structures in the films. The potential crystalline and amorphous C bonded structures that appear in CVD films have been described (0130). Raman spectroscopy has been used to characterize the diamond structures in films prepared by different CVD methods (0131-0136).While the films with a diamond structure show little H incorporation, IR spectroscopy has identified C-H vibrational modes (0137). Raman spectroscopy has also been used to characterize the surface of graphite (0138),and Raman and IR spectroscopies have also been used to characterize diamond-like films produced by pulsed laser evaporation (0139). BN and S i c crystalline films have been used to deposit these materials. IR spectroscopy has been used to characterize BN films (0140),and Raman spectroscopy has been applied to distinguish the different polytypes of S i c (0141). Several other oxide films have been characterized by Raman or IR spectroscopies. One of the most notable is high-temperature superconducting materials. Raman scattering has been used to describe the oxidation DroDerties (0142-0144). while IR has been used to measure ihe superconducting gap (071.0145. 0146). The oxidation process is due to chemical interactions a t semiconductor surfaces. For multiple component materials such as 111-V compounds, additional layers can often be observed at the interface. Raman spectroscopy has been used to characterize the oxidation of InGaAsP quaternary films, and crystalline As was detected a t the interface (0147).The technique has also been used to identify a thin layer of Te on the surface of CdTe after chemical treatment (0148). Reflectance spectra of electronic transitions can be enhanced by using surface differential reflectivity to study semiconductor surfaces, and this technique has demonstrated success for characterization of the oxidation of GaAs (0149). An important area of chemical processing is reactive-ion or dry etching processes. Raman scattering has been used to detect damaged regions on etched GaAs surfaces (0150,0151). Raman scattering has also been used to measure the surface carrier concentration after chemical passivation (0152). Surface films that form after CF4 plasma etch of Si3N4have been identified by using IR measurements (0153). One of the most common passivation methods of semiconductor surfaces includes the exposure to H or chemical etching resulting in H bonding at the surface. IR spectroscopy has been used to characterize the H bonding a t the surface of GaAs (0154)and Si (0155-0157).Raman spectroscopy has revealed that crystalline Si samples exposed to atomic H form internal defects (0158). In situ IR spectroscopy has also been used to measure the H bonding during the growth of a-Si:H (0159).The adsorption of 0 on Si has been studied by using differential reflectivity (0160))and 0 out diffusion from Si has been measured with IR (0161).The interactions
of organometallic molecules on Si surfaces were also studied (0162). IR spectroscopy has proven useful for characterizing molecular interactions on insulator surfaces. Measurements obtained include SiOz substrates, adsorption of CC14 (0163), H 2 0 (0164))and TiC14 (01651,and for NaCl substrates, adsorption of CO (0166)and C 0 2 (0167). The properties of molecules adsorbed on metal surfaces have been the subject of numerous studies, and IR measurements have proved particularly useful for identifying atomic structures. Some of these have been recently reviewed (0168,0169). One of the most studied single systems is that of CO on Pt. IR spectroscopy has been used on a series of CO absorbates on crystalline Pt with different processing conditions (D17O-0178). All of these studies focused on the strong IR active C-0 stretching mode. A feature has also been detected which is assigned to the metal-C stretch mode (0179).IR measurements of other molecules on Pt include ethylidyne (0180-0182),methanol (0138),and PF3 (0184). The properties of CO adsorbed on Ni have also been extensively studied using IR spectroscopy (0185-0188), and NO on Ni has also been reexamined (0189).The aspects of N2 on Si have focused on the N-N stretching mode (0190,0191). Stretching modes of other molecules on Ni have been related to atomic bonding and structure (0192-0195). Raman scattering results have also been observed for monolayer coverages of pyridine on Ni surfaces in UHV (0196). CO adsorption on Cu (0197,0198) and Ru (0199)crystalline surfaces have been measured. Copper deposited on Ru crystalline substrates with CO have also been studied (0200, 0201). Other molecules adsorbed on Cu have been detected with IR spectroscopy (0202-0204). An extensive study of H adsorbed on tungsten and molybdenum has shown derivative line shapes characteristic of Fano resonances (0205). While this review has addressed applications of Raman scattering, IR spectroscopy, and optical spectroscopy, there are new techniques which may lead to significant advances in the future for optical characterization of semiconductors. The technique of IR-visible sum generation holds promise of monolayer sensitivity for metal and semiconductor surfaces (0206).There have been several advances in Raman spectroscopy that could become more widely applied. Fourier transform Raman spectroscopy allows near-IR excitation to avoid luminescence background signals (0207).Use of a prism coupler in the Kretschmann geometry can give an enchancement by a factor of up to 1000 (0208).Interference enhanced Raman scattering can enhance the signal at metal surfaces and interfaces (0209).Optical characterization of electronic transitions in semiconductors and insulators could be greatly advanced by electroreflectance and modulation spectroscopy. While these techniques were demonstrated in the past, new understanding has led to a resurgence of their use (0210-0216).
E. DESORPTION TECHNIQUES-ELECTRONSTIMULATED DESORPTION (ESD), LASER-INDUCED DESORPTION (LID), AND THERMAL DESORPTION SPECTROSCOPY (TDS) Electron-Stimulated Desorption (ESD)
Electron-stimulated desorption work has continued to develop along several major lines, both experimental and theoretical. One review article on electron-stimulated desorption was published ( E l ) . Relevant experimental work is listed in Table 11. Angle-resolved ion distributions (ESDIAD) continue to provide information about the orientation of adsorbed structures on well-characterized single crystal surfaces. This is just the kind of information desperately needed in the development of surface chemical structural concepts and rules. There is also a developing interest in ESDIAD of coadsorbed layers which provides insight into how coadsorbates interact to alter each other’s surface bonding structure (E6,E7). Negative ion ESD has also been investigated and represents an important extension of stimulated desorption for examining surface structures as well as providing new kinds of experimental yield data against which various theoretical descriptions can be tested (E4).While theory continues to advance (E18-E20),the detailed description in terms of ab initio ANALYTICAL CHEMISTRY, VOL. 61, NO. 12, JUNE 15, 1989
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Schure (M45) used a random-walk Monte Carlo method to simulate the sedimentation FFF process. The results of the simulation suggest that large discrepancies exist between theory and simulation in the low retention region due to transient behavior which produces non-Gaussian zone shapes. Karaiskakis and Dalas (M46) used frontal sedimentation FFF to determine the particle-size distribution of polystrene latexes. Hoshino et al. (M47) investigated the effects of surfactants on the sedimentation FFF of polystrene and described the poly(vinylto1uene) latexes. Yonker et al. (M48) use of nonaqueous mobile phases for the separation of silica particles in sedimentation FFF. A patent was awarded to Keary and Shepherd (M49) for a sedimentation FFF apparatus. Sedimentation FFF was applied to the fractionation of gold and silver sols (M50),cartilage proteoglycans (M51),mitochondrial and microsomal membranes from corn roots (M52), and streptococcal cell wall particles (M53). Steric FFF. Giddings et al. (M54) reported on the use of gravity-augmented, high-speed flowlsteic FFF in which two fields, gravity and flow, were a plied to particles in the range of 5-50 l m . Seungho and GidJngs (M55) described the steric transition phenomena in sedimentation FFF. Dalas and Karaiskakis (M56) used steric FFF to characterize needleshaped stregite particles. Beckett (M57) applied steric FFF to the separation of silt-size particles in water. In addition, colloidal river-borne particles were characterized by using sedimentation FFF and humic acid and fulvic acid were analyzed by using flow FFF. Thermal FFF. Kirkland and co-workers (M58, M59) determined the molecular weight distribution of ~olvmersusine., time-delay, exponential-decay, thermal FFF: " Schimpf et al. (M60) used thermal FFF to determine the polydispersity of near-monodisperse polystyrene samples by measuring band broadening and its velocity dependence. This group (M61) used thermal FFF to study the thermal diffusion of polystyrene as a function of molecular weight and branching. Song et al. (M62) also measured the thermal diffusion coefficient of polystyrene and its dependency on molecular weight, concentration, and temperature. Gunderson et al. (M63) investigated the use of supercritical fluids as a carrier in thermal FFF. This group (M64) compared the resolution obtained in thermal FFF to that of SEC. Gao et al. (M65) also compared SEC with thermal FFF for the separation of linear and star-branched polystyrenes. Martin et al. (M66) used thermal FFF to characterize asphalts and asphaltenes.
ELECTROZONE SENSING Lines (N1)presented a review of particle size analysis using the Coulter counter. Lin and Briedis ( N 2 ) described a modified calibration procedure for the Elzone analyzer. These authors ( N 3 ) also discussed several limitations of the Elzone data system. Harfield and Wharton (N4) described a mathematical approach for the derivation of true size spectra for narrow-particle size distributions by deconvolution of the composite spectra resulting from the effect of the inhomogeneous electric field in the Coulter aperture. James and Welford (N5) compared results obtained from the Coulter counter with three other techniques for the analysis of coal and cyclone exhaust gas. Braun and Rieger (N6)discussed the effect of particle shape of fine wax powder on Coulter counter results. Sherwood (N7,N8) evaluated the use of a Coulter counter to determine the particle-size distribution of intravenous fat emulsions.
S I EVES/F ILTRATION Muller and co-workers ( 0 1 ) described approaches that can be taken to reduce errors during sieving. Scott ( 0 2 ) discussed sample preparation and procedures for determining particle-size distribution by sieving. A mathematical relation was derived by Tikhonov (03)for selecting the weight of a representative sample for sieve analysis. A method was proposed by Cernansky ( 0 4 ) for estimating the maximum size of particles that can pass through a filtration barrier of a given structure. Kaye and Clark (05) developed a confederate miniature sieve system as an alternative to nest sieving. Hoornstra and Dunn-Rankin ( 0 6 ) evaluated the size-distribution charac-
teristics of pulverized coal using dry sieving. Whiteman and Ridgway (07)evaluated sieves having rectangular and square apertures to separate particles according to their shape. Shape factors of fractonated material were calculated to evaluate the performance of the two types of apertures. Meloy et al. (08) studied the influence of particle shape on the rate a t which a particle passes through a screen. This group ( 0 9 ) also used an optical counter to monitor the rate of particles passing through a stack of identical sieves. This information was used to determine particle-shape distribution. Cieslicki (010) discussed whether a measurement of the relative flow rate of a suspension of spheres, flowing under a constant pressure drop through gaps of precisely defined geometry, may be utilized to measure the concentration and size distribution of particles. Orr (011) explored the use of gravity flow of powders through a vibrated column of loose glass spheres to determine the influence of particle size and shape on the rate of passage. A patent was awarded to Ho and Xanthopoulo (012) for determining the particle-size distribution of latexes by using a series of different pore-size filters.
CENTRIFUGATION/SEDIMENTATION Using osmocentrifugation and zonal centrifugation in density gradients, Costa et al. (PI)determined the particle-size distribution of latexes. This technique was applied to polystyrene latex particles in the 0.1-0.5 l m range (P2). These authors found that there was a significant amount of particles between successive bands caused by particleparticle reversible association. Kulvanich and Stewart (P3) measured the adhesion characteristics between particles using centrifugation. Dumm and Hogg (P4) discussed the mathematical treatment used or the evaluation of particle-size distribution from pipet-withdrawal centrifuge data. Shih and co-workers (P5) developed a one-dimensional hydrodynamic model for the sedimentation of multisize particles. The basic model and its modified form were programmed on a supercomputer to simulate settling of multisize particles. Disk Centrifugation
Coll and Searles (P6) compared the line-start with the homogeneous-start method in the Joyce-Loebl disk centrifuge usign colloidal AgBr and polystyrene latexes ranging from 0.3 to 1.2 km. This group (P7) also obtained improved results by using preformed density gradients in the rotor fluid rather than using the buffer-layer method. This was done by using an oil-covered density gradient in the rotor and correcting the optical signal with the help of light-scattering theory. Holsworth et al. (P8)developed an external-gradient-formation method in which the spin fluidldensity gradient is formed external to the disk cavity and injected into the disk cavity while the disk is spinning. This group (P9) also described an improved disk-centrifuge photosedimentometer and data system. Allen (PIO)presented a detailed evaluation of possible errors that may occur in the Joyce-Loebl disk centrifuge. These errors result from radial dilution of the sample and the breakdown in the laws of geometric optics as the particle size approaches the wavelength of the incident radiation. Photosedimentometry
Hostomsky et al. ( P I I ) evaluated theoretical relations for the sedimentation behavior of nonspherical particles by comparing results obtained by photosedimentometry and microscopy. Staudinger et al. (P12)developed and evaluated a photosedimentometer equipped with three sensors and interfaced to a personal computer. Somasundaran et al. (P13) reported on the use of CAT scanning to monitor and characterize sedimentation of particles.
OTHERTECHNIQUES Smith and Stermer (Q1) demonstrated that particle size and particle-size distribution information may be obtained from mercury intrusion measurements of powder compacts if the particle-size distribution is monodisperse and relatively narrow. A patent was awarded to Hauptmann et al. (Q2) for ANALYTICAL CHEMISTRY, VOL. 61, NO. 12, JUNE 15, 1989
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developing an acoustic method for detecting particle formation during emulsion polymerization. Emitted acoustic waves indicated the beginning and end of particle formation as an impulse number and density.
INTERCOMPARISON OF TECHNIQUES Koehler and Provder ( R I )determined the particle size of
a series of monodisperse poly(methy1 methacrylate) latexes by using disk centrifuge photosedimentometry, hydrodynamic chromatography, dynamic light scattering, turbidity, and transmission electron microscopy. Hoffman and Bernhardt (R2)presented data demonstrating that the technique used to measure particle size may be dependent on the characteristics of the sample. Surface-modified and porous particles were analysed by use of sedimentation and sieving and the results compared. Davies and Collins (R3) compared particle-size distributions of boron powders as determined from a Coulter counter and the Malvern diffractometer.
DATA ANALYSIS Popplewell et al. ( S I )demonstrated that populations which can be described by the normal, log-normal, and RosinRammler distributions can also be described by a modified version of the beta distribution function. In a subsequent paper (S2), these authors compared a modified beta and a modified normal distribution function for describing populations with a finite size range. Yu and Gentry (S3) compared representative inversion algorithms for characterizing particle-size distributions. Groves and Wong (S4)described a simple numerical index for measuring the size distribution of particles in small-volume parenteral solutions. Slaney (S5) advocated the use of a log-geometric mean and log-standard geometric deviation to specify the particle-size distribution of atomized and crushed powders. Alderliesten (S6) presented an excellent review of the current nomenclature used to describe mean particle diameters. Recommendations were made for a systematic nomenclature for describing mean particle diameters to avoid confusion. Particle Shape
Reviews of particle shape analysis were presented by Beddow (S7) and Meloy et al. (S8). Luerkens (S9) described a general, three-dimensional, mathematical method of particle representation. Wange (S10) introduced a simple mathematical expression to generate two-dimensional polygonally symmetrical shapes to improve methods for particle shape and size characterization. Staniforth and Hart ( S I I )used image processing and bulk powder measurements for shape analysis of microcrystalline cellulose particles. Clark et al. (SI2)used polygonal harmonics of silhouettes for particle-shape analysis and also presented a scheme for the characterization of particle shape based on fractal harmonics and fractal dimensions (S13). Meloy ( S I 4 ) reported on a n approach for describing the idealized or fundamental shape of fractured particles. Pandit and Joshi (SI5) presented a method for determining the volumetric-shape factor of particles by measuring the flow rate of a liquid draining through a bed packed with nonspherical particles. Feruuchi and co-workers (SI6)determined the particle shape of nonconducting particles of various shapes from the electric conductivity of suspensions.
PARTICLE SIZE STANDARDS Small et al. ( T I )studied different methods of producing micrometer and submicrometer particle standards. These methods included the production of ground-glass shards, fibers, microspheres, metal and metal-alloy particles, and doped-ceramic particles. Blackford (7'2) evaluated the use of polystyrene spheres ( 5 7 , 10, and 15 mm) as calibrants for scanning electron microscopy, Coulter counter, and image analysis. Thioye et al. (T3)described standards of dispersed particles for the calibration of light scattering instruments. The standards are useful for applications in the determination of particle-number density and particle-size distribution. 150R
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A patent was awarded to Timm (2'4) for the preparation of uniform-size spherical polymer beads. This was accomplished by polymerizing uniformly sized monomer droplets formed by the vibratory excitation of a laminar flowing jet of monomer in a liquid medium containing a suitable suspending agent. LITERATURE CITED GENERAL BOOKS AND REVIEWS
( A l ) Barth, H. G.; Sun, S. T. Anal. Chem. 1985, 5 7 , 151R-175R. (A2) Barth, H. G.; Sun, S.T.; Nickol, R. M. Anal. Chem. 1987, 5 9 , 142R162R. (A3) Particle Size Distribution: Assessment and Characterization; Provder, T., Ed.; ACS Symp. Ser. 332; American Chemical Society: Washington, DC, 1987. (A4) Svarovsky, L. Powder Testing Guide; Elsevier: Amsterdam, 1987. (A5) Lloyd Particle Size Analysis, 1988; Wiley: Chichester, 1988. (AB) Muller, S. Powder Technol. 1988, 5 5 , 229-230. (A7) Buttner, H. Part. Part. Syst. Charact. 1988, 5 , 144-149. (A8) Schubert, H.; Wachtler, E. Part. Charact. 1987, 4 , 45-48. (A9) Freshwater, D. C. Powder Techno/. 1987, 5 0 , 295-299. (A10) Polke, R. Part. Charact. 1987, 4 , 54-62. ( A l l ) Luerkens, D. W.; Beddow, J. F.; Vetter, A. F. Powder Technol. 1987, 5 0 , 93-101. (A12) Sheppard. L. M. Am. Ceram. Soc.Bull. 1988, 6 7 , 878-883. SCATTERING
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(H6) Kiiafas, Y.; Taylor, A. M. K. P.; Whitelaw, J. H. Exp. fluids 1987,5, 159-76. (H7) Horrocks, J. K.; Corbin, R. G.; Towell, D. E.; Hemsley, D. J.; Gillespie, R. F.; Yeoman, M. L. Inst. Chem. Eng. Symp. Ser., 99 (GasClean. High Temp.) 1986. 101-16. (HE) Chevaillier, J.-P.; Fabre, J.; Hamelin, P.; Lesne, J.-L. Part. Part. Syst. Charact. 1988,5,9-12. (H9) Yianneskis, M. Powder Technol. 1987,4 9 , 261-9. Neutron Scalterlng (11) Hayter, J. B. Mater. Res. SOC. Symp. Proc. 1987,7 9 , 241-50. (12) Fisher, L. W.; Melpolder, S. M.; O'Reilly, J. M.; Ramakrishnan, V.; Wignall, G. D. J. Colloid Interface Sci. 1988, 123, 24-35. (13) Feeney, P. John; Geissler, Erik; Gilbert, Robert G.; Napper, Donald H. J. Colloid Interface Sci. 1988, 121, 508-13. (14) Wai, M. P.; Gelman, R. A.; Fatica, M. G.; Hoerl, R. H.; Wignall, G. D. Polymer 1987,2 8 , 918-22. (15) Agamalyan, M. M.; Babkin, I.Yu.; Burukhin, S. B.; Evmenenko, G. A. Khim. Vys. Energ. 1987, 2 1 , 418-21 (Russian); Chem. Abstr. 1987, 107, 218344q. (16) Agamalyan, M. M.; Evmenenko, G. A,; Babkin, 1. Yu.; Burukhin, S. B.; Duarev, V. Ya.; Noifekh, A. I.Vysokomol. Soedin., Ser. A . 1987,2 9 , 888-92 (Russian); Chem. Abstr. 1987, 106, 197051d. (17) Plestii, J.; Ostanevich, Yu. M.; Borbely, S.; Stejskal, J.; Ilavsky, M. Polym. Bull. (Berlin) 1987, 17, 465-72. (18) Spooner, S.; Iida, S.; Larson, B. C. Mater. Res. SOC. Symp. Proc. 1987,82, 79-84. (19) Murthy, N. S.; Aharoni, S. M. Polymer 1987,2 8 , 2171-5. X-ray Scatterlng ( J l ) Frydrychowicz, J.; Kojdecki, M.; Swillo, R. Conf. Appl. Crystallogr., (Proc.) 1988, 12, 134-47. (J2) Volodin, S. A.; Revenko, A. G. Metody Rentgenospektr. Anal. 1988, 41-6 (Russian); Chem. Abstr. 1987, 106, 130757~. (J3) Volodin, S. A.: Revenko, A. G.; Afonin, V. P. Zavod. Lab. 1987,5 3 , 24-7 (Russian); Chem. Abstr. 1987, 108, 30619q. (J4) Khorramian, B. A.; Stivala, S. S.; Patel, A. Polym. Prepr. 1987, 2 8 , 274-5. (J5) Kranold, R.; Gcscke, W. Silikattechnik 1987,38, 313 (German); Chem. Abstr. 1987, 108, 4 2 6 4 8 ~ . (J6) Gernat, Ch.; Reuther. F.; Damaschun, G.; Schierbaum, F. Acta Polym. 1987,3 8 , 603-7. (J7) De Angelis, R. J.; Dhere, A. G.; Maginnis, M. A.; Reucroft, P. J.; Ice, G. E.; Habenschuss, A. Adv. X-Ray Anal. 1987,3 0 , 389-94. (J8) Deslandes, Yves; Whitrnore, Mark D.; Bluhm, Terry L.; J. Dispersion sci. Technol. 1988,9 , 235-57. (J9) Stradomskii, M. V.; Maksimov, E. A.; Plita, A. G.; Efremova, E. A. Prom. Teplotekh. 1988, 10, 84-8 (Russian); Chem. Abstr. 1988, 109, 131717f. ELUTION TECHNIQUES ( K l ) Kourti, T.; Penlidis, A.; MacGregor, J. F.; Hamielec, A. E. ACS Symp. Ser. 1987,No. 332 (Part. Size Distrib.), 242-55. (K2) Styring, M. G.; Honig, A. J.; Harnielec, E. J. Llq. Chromatogr. 1988,9 , 3505-41. (K3) Nunes, A. C.; Yu, 2 . C. J. Magn. Magn. Mater. 1987,6 5 , 265-8. (K4) Sutherland, I.A. Chromatogr. Sci. 1988,44(Countercurrent Chromatogr.), 617-52. (K5) Aoki, I.;Shirane, K.; Tokimoto. T.; Kimura, M. Rev. Sci. Instrum. 1988,5 9 , 484-5. (K6) Ito, Y. US. Patent 4,753,734 A, 28 June 1988. Hydrodynarnlc Chromatography (Ll) Secchi, B. M.; Visioii, D. L.; Silebi, C. A. ACS Symp. Ser. 1987,No. 332 (Part. Size Distrib.), 267-98. (L2) Molina, L. F.; Velilla, P. A.; Enguidanos, S. S. An. Quim., Ser. A 1988, 84, 84-8 (Span.); Chem. Abstr. 1988, 109, 116692a. (L3) Thornton, W.; Olivier, J. P.: Smart, C. G.; Gilman, L. B. ACS Symp. Ser. 1987,No. 332 (Part. Size Distrib.), 256-71. (L4) Van Gilder, R. L.; Langhorst, M. A. ACS Symp. Ser. 1987, No. 332 (Part. Size Distrib.), 272-86. (L5) Hoagland, D. A.; Prud'homme, R. K. J. Appl. Polym. Sci. 1988,3 8 , 935-55. (LE) Tazaki. M.; Maruyama, I.; Takase, S.; Homma, T. Kobunshi Ronbunshu 1988,4 5 , 19-23 (Jpn.); Chem. Abstr. 1988, 108, 142518~. (L7) Ploehn, H. J. I n t . J. Multiphase Flow 1987, 13, 773-84. (LE) De Jaeger, N. C.; Trappers, J. L.; Lardon, P. Part. Charact. 1988,3, 187-9 1. (L9) Elk, P.; Renaud, M. Entropie 1987,23(136), 33-40 (Fr.); Chem. Abstr. 1988, 108, 96427s. Fleld-Flow Fractionation (Ml) Du Pont Sedimentation Field Flow Fractionator, Du Pont Co., Instrument Systems, North Walnut St., P.O. Box 10, Kennet Sq., PA 19348. (M2) FFFractionation, Inc., P.O. Box 8718, Salt Lake City, UT 84108. (M3) Janca, J. Field Now Fractionation; Dekker: New York, 1988. (M4) Caidweil, K. D. Anal. Chem. 1988, 6 0 , 959A-960A, 962A-966A. 9 - 6- 6-.A., 9- 7. O- .A.- 9-7.1 A.. .. (M5) Janca, J. Chem. Listy 1987, 8 1 , 1034-57 (Czech.); Chem. Abstr. 1987. 107. 2377470. (M6) Janca, J. TrAC, 'Tends Anal. Chem. (Pers. Ed.) 1987, 6, 147-52. (M7) Andreev, V. P.; Reifman, L. S. Nauchn. Appar. 1986, 1 ( 3 ) , 3-36 (Russ.); Chem. Abstr. 1987, 107, 117502j. (ME) Kirkland, J. J.; McCormick, R. M. Chromatographia 1987,2 4 , 58-76. (M9) Giddings. J. C. J. Chromatogr. 1987,395, 19-32. ANALYTICAL CHEMISTRY, VOL. 61, NO. 12, JUNE 15, 1989
151 R
PARTICLE SIZE ANALYSIS (M10) Giddings, J. C.; Schure, M. R. Chem. Eng. Sci. 1987, 4 2 , 1471-9. (M11) Caldwell, K. D.; Brimhall, S. L.; Gao, Y.; Giddings, J. C. J . Appl. Polym. Sci. 1988, 3 6 , 703-19. (M12) Hansen. M. E.; Giddlngs, J. C.; Schure, M. R.; Beckett, R. Anal. Chem. 1988, 6 0 , 1434-42. (M13) Williams. P. S.; Giddings, J. C. Anal. Chem. 1987, 5 9 , 2038-44. (M14) Tomida, T.; McCoy, B. J. AIChE J . 1988. 3 4 , 341-6. (M15) Berthod, A.; Armstrong, D. W. Anal. Chem. 1987, 5 9 , 2410-13. (M16) Berthod, A.; Armstrong, D. W.; Myers, M. N.; Giddings, J. C. Anal. Chem. 1988, 6 0 . 2138-41. (M17) Van den Broeck. C.; Mass, D. Sep. Scl. Technol. 1987, 2 2 , 1269-80. (M18) Ugrozov, V. V. Zh. f i r . Khim. 1988, 6 2 , 1091-3 (Russ.); Chem. Abstr. 1988, 108, 2 2 3 6 6 6 ~ . (M19) Andreev, V. P.; Semenov, S.N.; Kuznetsov, A. A.; Relfman. L. S.Zh. f i z . Khim. 1987, 6 1 , 1-12 (Russ.); Chem. Abstr. 1987. 106, 126563m. (M20) Semyonov, S.N.; Kononenko. V. L.; Shimkus, Ya. K. J . Chromatogr. 1988, 446, 141-50. (M21) Semyonov, S. N.; Maslow, K. I . J . Chromatogr. 1988, 446, 151-6. (M22) Semyonov, S.N. J . Chromatogr. 1988, 446, 131-9. (M23) Davis, J. M.; Fan, F. R. F.; Bard, A. J. Anal. Chem. 1987, 5 9 , 1339-48. (M24) Janca. J. Mkromol. Chem., RapidCommun. 1987, 8 , 233-6. (M25) Wahlund, K. G.; Giddings, J. C. Anal. Chem. 1987, 5 9 , 1332-9. (M26) Beckett, R.; Jue, 2.; Giddings, J. C. Envlron. Scl. Technol. 1987, 2 1 . 289-95. (M27) Granger, J.; Dodds, J.; Leclerc. D.: Midoux, N. Chem. Eng. Scl. 1986, 4 1 , 3119-28. (M28) Giddings, J. C.; Chen. X.; Wahlund, K. G.; Myers, N. Anal. Chem. 1987, 5 9 , 1957-62. (M29) Mori, S. Chromatograph& 1986, 2 1 , 642-4. (M30) Giddings, J. C.; Caldwell, K . D.; Jones, H. K. ACS Symp. Ser. 1987, N o . 332 (Part. Size Dlstrib.). 215-30. (M31) Levy, G. 8. Am. Lab. (falrfieM. Conn.) 1987, 79(6), 84, 86. 88. 90, 92, 94-5. (M32) Levy, G. B.; Fox, A. Am. BiOt8ChnOl. Lab. 1988, 6(1), 14, 16-7, 20- 1, (M33) Lee, S.;Myers, M. N.; Beckett, R.: Giddings, J. C. Anal. Chem. 1988, 6 0 , 1129-35. (M34) Giddings, J. C.; Williams, P. S.;Beckett, R. Anal. Chem. 1987, 5 9 , 28-37. (M35) Williams, P. S.; Giddings. J. C.; Beckett, R. J . Liq. Chromafogr. 1987, 10, 1961-68. (M36) Williams, P . S.;KeHner, L.; Beckett, R.; Gddings, J. C. Ana/yst (London) 1988, 173, 1253-9. (M37) Springston, S.R.; Myers, M. N.;Giddings, J. C. Anal. Chem. 1987, 5 9 , 344-50. (M38) Jones, H. K.; b h n , K.; Myers, M. N.;Glddings. J. J . Colloid Interface Sci. 1987, 120, 140-52. (M39) Janca. J.; Pribylova, D.; Jahnova, V. J . Llq. Chromatogr. 1987, 10, 767-82. (M40) Jahnova, V.; Matulik, F.; Janca, J. Anal. Chem. 1987, 5 9 , 1039-43. (M41) Janca. J.; Pribylova. D.; Konak. C.; Sedlacek, B. Anal. Sci. 1987, 3 , 297-300. (M42) Janca, J. J . Chromafogr. 1987, 404, 23-32. (M43) Wicar, S. J . Chromatogr. 1988, 448, 456-7. ( M U ) Janca, J.; Novakova, N. J . Liq. Chromatogr. 1987, 10, 2869-76. (M45) Schure, M. R. Anal. Chem. 1988, 6 0 , 1109-19. (M46) Karaiskakis, G.; Dalas, E. J . Chromatogr. Scl. 1988, 2 6 , 29-33. (M47) Hoshino, T.; Suzuki, M.; Ysukawa, K.; Takeuchi. M. J . Chromatogr. 1987, 400, 361-9. (M48) Yonker, C. R.; Jones, H. K.; Robertson, D. M. Anal. Chem. 1987, 5 9 , 2574-9. (M49) Keary, C. M.; Shepherd, D. U S . Patent 4,657,676 A, 14 Apr 1987. (M50) Oppenheimer, L. E.; Smith, G. A. Langmuir 1988, 4 , 144-7. (M51) Schallinger, L. E.; Arner, E. C.; Kirkland, J. J. Blochim. Biophys. Acta 1988. 966, 231-8. (M52) Mozersky, S.M.; Caldwell, K. D.; Jones, S. B.; Maleeff, B. E.;Barford, R. A. Anal. Biochem. 1988, 172, 113-23. (M53) Gilbart, J.; Wells, A. F.; Hoe, M. H.; Fox, A. J . Chromatogr. 1987, 387, 428-33. (M54) Chen, X.; Wahlund, K. G.; Giddings, J. C. Anal. Chem. 1988, 6 0 , 362-5. (M55) Lee, S.;Giddings, J. C. Anal. Chem. 1988, 6 0 , 2328-33. (M56) Dalas, E.; Karalskakis, G. Collokls Surf. 1987, 28, 169-83. (M57) Beckett, R. Environ. Technol. Lett. 1987, 8 , 339-54. (M58) Kirkland, J. J.; Yau. W. W. Znt. GPC Symp. '87 1987, 199-224; Millipore Corp.; Milford, MA. (M59) Kirkland, J. J.; Rementer, S.W.; Yau, W. W. Anal. Chem. 1988, 6 0 , 610-1 6. (M60) Schimpf, M. E.; Myers, M. N.; Giddings, J. C. J . Appl. Polym. Scl. 1987, 3 3 , 117-35. (M61) Schimpf, M. E.; Giddings, J. C. Macromolecules 1987, 2 0 , 1561-3. (M62) Song, K. C.; Kim, E. K.; Chung, I.J. Korean J . Chem. Eng. 1986, 3 , 171-5. (M63) Gunderson, J. J.; Myers, M. N.; Gddings. J. C. Anal. Chem. 1987, 59, 23-8. (M64) Gunderson, J. J.; Giddings, J. C. Anal. Chim. Acta 1986, 789. 1-15. (M65) Gao, Y.; Wang. J.; Shen, J. Gaofenzi Tongxun 1986, (3), 231-5 (Chinese); Chem. Abstr. 1988, 105, 227656d. (M66) Martin, M.; Ignatiadis, I.; Reynaud, R. fuel 1987, 6 6 , 1436-44. ELECTROZONE SENSING
(NI) Lines, R. W. Anal. R o c . (London) 1987. 2 4 , 272-6. (N2) Lin, S. H.; Briedis, D. M. Rev. Sci. Instrum. 1988, 5 9 , 386-8. (N3) Lin, S. H.; Briedis, D. M. Rev. Sci. Instrum. 1988, 5 9 , 383-6.
152R * ANALYTICAL CHEMISTRY, VOL. 61, NO. 12, JUNE 15, 1989
(N4) Harfieid, J. G.; Warton. R. A. Part. Part. Syst. Charact. 1988. 5 , 29-37. (N5) James, R. G.; Weiford. G. Anal. Proc. (London) 1987, 2 4 , 38. (N6) Braun, R.; Rieger, K. farbe Lack 1988, 9 4 , 37-9 (Ger.); Chem. Abstr. 1988. 108. 57898b. (N7) Sherwood, J. D. Anal. Proc. (London) 1087, 2 4 , 277-9. (N8) Sherwood, J. D. Anal. Proc. (London) 1987, 2 4 , 279-81.
SIEVES/F ILTRATION (01) Mulier, H.; Kubier, B.; Rudolph, L. Part. Charact. 1987. 4 , 74-77. (02) Nushart, S. Powder Bulk Eng. 1987. 7(8), 14-19. (03) Tikhonov, 0. N. I z v . Vyssh. Uchebn. Zaved., Tsvetn. Metall. 1988, (3), 2-8 (Russian); Chem. Abstr. 1988, 109, 1 9 4 2 4 5 ~ . (04) Cernansky, A. Chem. Prum. 1986, 3 6 , 626-31 (Czech.); Chem. Abstr. 1987, 106. 5 2 3 5 5 ~ . (05) Kaye, B. H.; Clark, G. G. Part. Charact. 1988, 3 , 145-50. (06) Hoornstra, J.; Dunn-Rankin, D. Coal Sci. Technol. 1987, ll(Int. Conf. Coal Sci., 1987), 949-52. (07) Whiteman, M.; Ridgway, K. Drug Dev. Znd. Pharm. 1986. 12, 1995-20 13. ( 0 8 ) Meloy, T. P.; Pitchumani. 8.; Clark, N. Indian Chem. Eng. 1987, 2 9 , 43-9. (09) Clark, N. N.; Meloy, T. P. Powder Technol. 1988, 5 4 , 271-7. (010) Cieslicki, K. Part. Part. Syst. Charact. 1988, 5. 94-99. (011) Orr. C. Powder Technol. 1987, 5 0 , 217-220. (012) Ho, S. M.; Xanthopoulo, G. U S . Patent 4,747,959 A, 31 May 1988. CENTRIFUGATIONlSEDlMENTATION
(Pl) Costa, M. C.; Hechenleitner, A. A.; Nunes, S.; Galembeck, F. Synth. Po/ym. Membr ., Proc . Mlcrosymp . Macromol.; Sedlacek, B., Kahovec, J., Eds.; Gruyter: Berlin, Fed. Rep. Ger. 1987; pp 581-9. (P2) Costa, M.; Galembeck, F. Colloids Surf. 1988, 3 3 , 175-84. (P3) Kulvanich, P.; Stewart, P. J. Int. J . Pharm. 1987. 3 5 , 111-20. (P4) Dumm. T. F.; Hogg, R. Part. Charact. 1986, 3 , 122-8. (P5) Shih, Y. T.; Gidaspow, D.; Wasan. D. T. Powder Technol. 1987, 5 0 , 201-215. (P6) Coll, H.; Searies, C. G. J . Colloid Znferface Sci. 1987, 715, 121-9. (P7) Coll. H.; Oppenheimer, L. E. ACS Symp. Ser. 1987, No. 332 (Part. Size Distrib.), 202-14. (Pa) Holsworth, R. M.; Provder. T.; Stansbrey, J. J. ACS Symp. Ser. 1087, No. 332 (Part. Size Distrib.), 191-201. (P9) Koehler, M. E.; Zander, R. A.; Gill, T.; Provder, T.; Niemann, T. F. ACS Symp. Ser. 1987, No. 332(Part. Size Distrib.), 180-90. (PIO) Allen, T. Powder Technol. 1987, 5 0 , 193-200. (P11) Hostomsky. J.; Halasz, 2.; Liszi, I.; Nyvlt, J. Powder Technol. 1986, 4 9 , 45-51. (P12) Staudinger, G.; Hangl, M.; Pechtl, P. Part. Charact. 1988, 3 , 158-62. (P13) Somasundaran, P.; Huang, Y. B.; Gryte, C. C. Powder Technol. 1987, 5 3 , 73-77. OTHER TECHNIQUES
(Ql) Smith, D. M.; Stermer. D. L. Powder Technol. 1987, 5 3 , 23-30. ((22) Hauptmann, P.; Hergeth, W. D.; Wartewig, S.;Ranachowski, J.; Ranachowski, 2.; Adamczyk. E. East German Patent DD 241,480 A I 10 Dec. 1986 (German); Chem. Abstr. 1987, 107, 97311r. INTERCOMPARISON OF TECHNIQUES ( R I ) Koehler, M. E.; Provder, T. ACS Symp. Ser. 1987, No. 332 (Part. Size Distrib.), 231-9. (R2) Hoffmann. B.; Bernhardt, C. Part. Charact. 1988, 3 , 163-7. (R3) Davies, J. A.: Collins, D. L. Part. Part. Syst. Charact. 1988, 5 , 116-21.
DATA ANALYSIS
(S1) Popplewell, L. M.; Campanella, 0. H.; Normand, M. D.; Peleg, M. Powder Technol. 1988, 5 4 , 119-25. (S2) Popplewell, L. M.; Campanella, 0. H.; Peleg, M. Powder Techno/. 1988, 5 4 , 157-60. (S3) Tu, P.-Y.; Gentry, J. Powder Technol. 1987, 5 0 , 79-89. 6 4 ) Groves, M. J.; Wong, J. Drug Dev. Ind. Pharm. 1987, 13, 193-206. (S5) Slaney, J. S.Mod. Dev. Powder Metall. 1984, 17, 719-30. (536) Alderliesten, M. Anal. Proc. 1984, 2 1 , 167-72. (S7) Beddow, J. K. ACS Symp. S8r. 1987, No. 332 (Part. Size Dist.). 2-29. (S8) Melow, T. P.; Mani, B. P.; Clark, N. N. J . Powder Bulk Solids Technol. 1986, 10, 15-20. (S9) Luerkens, D. W. Part. Charact. 1987, 4 , 118-21. (SIO)Wang, P. K. J . Colloid Znferface Scl. 1987, 777, 271-81. (S11) Staniforth, J. N.;Hart, J. P. Anal. Proc. (London) 1987, 2 4 , 78-80. (S12) Clark, N. N.; Diamond, H.; Gelles, G.; Bocoum, 8.; Meloy, T. P. Part. Charact. 1987, 4 , 38-43. (S13) Clark, N. N. Powder Technol. 1987, 5 1 , 243-9. (S14) Meloy, T. P. Powder Technol. 1988, 5 5 , 285-91. (S15) Pandit, A. B.; Joshi, J. B. Indian J . Technol. 1986, 2 4 . 587-90. (S16) Furuuchi, M.; Ikeuchi, A.; Fukagawa, T.; Gotoh, K. J . Chem. Eng. Jpn. 1988, 21 528-33. ~
PARTICLE SIZE STANDARDS
( T l ) Small, J. A.; Ritter, J. J.; Sheridan, P. J.; Pereles, T. R. J . Trace Mlcroprobe Tech. 1986, 4 , 163-83. (T2) Blackford, D. B. Aerosol Scl. Technol. 1987, 6 , 85-9. (T3) Thioye. M.; Le Toulouzan. J. N.; Gouesbet, G.; Gougeon, P.; Chabot, F. J . Aerosol Sci. 1988, 19, 105-12 (French); Chem. Abstr. 1988, 109, 39824r. (T4) Timm, E. E. U.S.Patent 4,666,673 A, 19 May 1987.
