Frank Babick

Dependence of ultrasonic attenuation on the material properties

Abstract Ultrasonic spectroscopy is a promising measurement technique for the characterisation of emulsions and suspensions over a wide range of particle size and concentration. It appears highly suitable for on-line applications, in particular for dense nano-sized particle systems, where the system stability may be very sensitive to changes in the concentration. In the case of colloidal dispersions the particle sizes are usually smaller than the sound wavelength. Then dissipative processes rather than scattering govern the acoustic behaviour of such systems. The dissipative processes, however, are affected by several material properties, whose significance for the overall acoustic behaviour depends on the type of the material system, e.g. thermal properties are important in the case of emulsions and non-watery suspensions but not for watery suspensions. Often the information on these parameters is incomplete and not sufficiently accurate. In this paper the stability of ultrasonic particle size measurement against incorrect values of the relevant material properties is investigated. This was done firstly by analytical consideration. From this, the degree of influence of the respective material properties on the analysis of spectrometric measurements was derived for oil-water-emulsions, watery and non-watery suspensions. It could be shown that the single properties affect the analysis very differently. In a second step, the conclusions obtained analytically could be confirmed by analysing experimental attenuation spectra with slightly changed material property data. The paper is intended to give users of ultrasonic spectroscopy a practical guide for deciding which material properties have to be obtained with high accuracy and which can be estimated.

How reliably can a material be classified as a nanomaterial? Available particle-sizing techniques at work

Currently established and projected regulatory frameworks require the classification of materials (whether nano or non-nano) as specified by respective definitions, most of which are based on the size of the constituent particles. This brings up the question if currently available techniques for particle size determination are capable of reliably classifying materials that potentially fall under these definitions. In this study, a wide variety of characterisation techniques, including counting, fractionating, and spectroscopic techniques, has been applied to the same set of materials under harmonised conditions. The selected materials comprised well-defined quality control materials (spherical, monodisperse) as well as industrial materials of complex shapes and considerable polydispersity. As a result, each technique could be evaluated with respect to the determination of the number-weighted median size. Recommendations on the most appropriate and efficient use of techniques for different types of material are given.Graphical Abstract

Polydisperse particle size characterization by ultrasonic attenuation spectroscopy for systems of diverse acoustic contrast in the large particle limit

Ultrasonic attenuation spectroscopy offers advantages over other spectrometric methods for the determination of suspension and emulsion size distributions. One advantage is the possibility of conducting measurements in highly concentrated or optically opaque dispersions. Models useable for the inversion of measured attenuation spectra to calculate particle size distributions are available and widely used, but their applied forms only allow for the characterization of particles smaller than 10μm. In this paper, a methodology using the Faran model for elastic scatterers is examined in the region of micrometer-sized particles with respect to its suitability for the prediction of measured attenuation spectra and size distributions of various material combinations. All selected particle fractions and fluid materials were characterized independently from ultrasonic attenuation spectroscopy with respect to their material properties, size distributions, and shape. A comparison of measured and calculated attenuation spectra shows an acceptable agreement. The chosen methodology for particle sizing applications is further confirmed if a fit of the model to the measurement data is performed. In this approach, the solids volume fraction is treated as the only fit parameter. The findings indicate that the methodology is suitable for polydisperse particle size characterization for a wide range of acoustic contrast.Ultrasonic attenuation spectroscopy offers advantages over other spectrometric methods for the determination of suspension and emulsion size distributions. One advantage is the possibility of conducting measurements in highly concentrated or optically opaque dispersions. Models useable for the inversion of measured attenuation spectra to calculate particle size distributions are available and widely used, but their applied forms only allow for the characterization of particles smaller than 10μm. In this paper, a methodology using the Faran model for elastic scatterers is examined in the region of micrometer-sized particles with respect to its suitability for the prediction of measured attenuation spectra and size distributions of various material combinations. All selected particle fractions and fluid materials were characterized independently from ultrasonic attenuation spectroscopy with respect to their material properties, size distributions, and shape. A comparison of measured and calculated attenuati...

Ultrasonic Spectrometry for Particle Size Analysis in Dense Submicron Suspensions

Ultrasonic spectrometry was applied to the particle size analysis of disperse systems. The investigations were made for acoustic conditions called the long-wavelength regime (LWR). In the LWR the acoustic behaviour is governed by dissipative effects rather than by scattering. Two principal theoretical approaches to ultrasonic spectrometry — scattering theory and coupled phase models — are introduced. A model based on a newly developed coupled phase model and the scattering theory (ECAH theory) is implemented in the ultrasonic spectrometer Acousto Phor. Experiments were carried out for several suspensions with a high density contrast. It could be demonstrated that the model successfully describes acoustic attenuation and that the inversion algorithm finds particle size distributions comparable to those given by other measurement techniques. With regard to the particle size, a lower and an upper limit for the applicability were determined, which include three decades. As a further result, the model was validated at concentrations up to 10 vol.%. The model is considered to be open to development to cover even higher concentrations.

Sound attenuation by small spheroidal particles due to visco-inertial coupling

The sound attenuation at ultrasonic frequencies caused by small spheroidal particles in a fluid is examined with regard to the size parameters that determine the shape of the attenuation spectrum. Our investigations are based on a coupled phase model for spheroids with arbitrary orientation, thus facilitating the calculation of average attenuation for a given orientation distribution. Since the model just considers the visco-inertial coupling, its applicability is restricted to small solid particles with high density contrast. The calculated attenuation spectra of mono-sized, randomly aligned spheroidal particles are compared with the attenuation spectra of mono-sized spheres. When the latter approximate the former to a reasonable degree the size of the spheres is called attenuation equivalent diameter. It is shown that the concept of attenuation equivalent diameter can be applied only to slightly elongated prolates. Oblates and very stretched prolates yield considerably broader attenuation spectra than m...

Information Content of Acoustic Attenuation Spectra

In recent years ultrasonic attenuation spectroscopy has gained much attention as a method for the characterisation of concentrated dispersions. Several publications have shown, that this method allows the accurate determination of particle size. In particular for submicron dispersions there is, however, some uncertainty to which degree the details of a size distribution can be resolved by acoustic attenuation measurements. Ideally the inversion of an attenuation spectrum into a size distribution would yield as much distribution parameters as sound frequencies. In practice, however, the measurement errors affect the inversion very strongly and may result in multiple solutions for the size distribution. The maximum number of distribution parameters, for which a unique solution exists, can be therefore regarded as the information content. For a given ultrasonic spectrometer and material system it is possible to quantify the information content. Such an information analysis has been conducted with selected material systems in the submicron range. The investigation shows that the information content of acoustic attenuation spectra with regard to particle size analysis in the submicron range is relatively low. On the other hand, the results imply that the number of frequencies can be reduced significantly without loss of information content or stability of inversion algorithms.

Impact of ultrasonic dispersion on the photocatalytic activity of titania aggregates

Summary The effectiveness of photocatalytic materials increases with the specific surface area, thus nanoscale photocatalyst particles are preferred. However, such nanomaterials are frequently found in an aggregated state, which may reduce the photocatalytic activity due to internal obscuration and the extended diffusion path of the molecules to be treated. This paper investigates the effect of aggregate size on the photocatalytic activity of pyrogenic titania (Aeroxide® P25, Evonik), which is widely used in fundamental photocatalysis research. Well-defined and reproducible aggregate sizes were achieved by ultrasonic dispersion. The photocatalytic activity was examined by the color removal of methylene blue (MB) with a laboratory-scale setup based on a plug flow reactor (PFR) and planar UV illumination. The process parameters such as flow regime, optical path length and UV intensity are well-defined and can be varied. Our results firstly show that a complete dispersion of the P25 aggregates is not practical. Secondly, the photocatalytic activity is not further increased beyond a certain degree of dispersion, which probably corresponds to a critical size for which UV irradiation can penetrate the aggregate without significant obscuration.

Fundamentals in Colloid Science

The macroscopic behaviour of colloidal suspensions is directly related to the fineness of their particles, but is also affected by the interfacial properties and the interaction between neighbouring particles. Specific effects are encountered for nanosized particles, which weakly interact with light and for which surface curvature is relevant. A profound understanding of the physical phenomena prevailing in colloidal suspensions facilitates their preparation, handling, use and characterisation. This chapter addresses the physico-chemical properties of single colloidal particles as well as the processes at the interface and the structure of the interfacial layer. It further examines the non-viscous interactions that occur between colloidal particles.

Physico-chemical separation process of nanoparticles in cosmetic formulations

Understanding the world of nanoparticles, especially their interactions with the environment, begins with their correct detection and successive quantification. To achieve this purpose, one needs to perform correctly developed standard operating procedures (SOPs). Furthermore, the study of nanoparticles frequently requires their characterisation in complex media (e.g. in cosmetic formulations). In this study, a set of sample preparation procedures for the detection and extraction of NMs in emulsion-based formulations is proposed and their performance for model and real-life products is discussed. A separation or extraction of lipid phases is achieved by means of organic solvents. The polarity of the lipid phases is decisive for selecting an optimum solvent. The use of the Hansen Solubility Parameters (HSP) may clearly support this decision.

Characterisation of Colloidal Suspensions

Techniques for particle characterisation are inherently needed when preparing or processing colloidal suspensions. The challenge consist in finding an appropriate technique for the specific analytical task, which may ask for mean particle sizes, size distribution, particle shape, aggregate morphology or interfacial properties. A profound knowledge of the characteristics of relevant measurement techniques supports such a decision. The chapter provides a survey on analytical techniques for the quantification of particle size and morphology as well as interfacial properties.