Slurry analysis techniques

Solid foods in powder form can be analyzed directly by means of LA- or ETV-ICP-MS to eliminate time-consuming sample dissolution procedures (see Table 8.2). However, this requires the preparation of homogeneous powdered samples and the subsequent analytical determination is not as straightforward as the one based on liquid sample introduction. Another way to perform direct analysis of solid foods is to grind and suspend them into slurries. The viability of slurry nebulization relies on the ability to prepare samples of fine particle size in a reproducible manner and on the adoption of suitable (e.g., high-solids) nebulizers. Otherwise, slurries can be analyzed by ETV-ICP-MS resorting to the ultrasonic slurry sampling technique [72-74]. 

Finally, surface cleanliness is critical to proper dispersion of micron particles in slurry vehicles and mixing and retention with bond components. The identity and concentration of surface impurities can be determined by surface spectroscopic and bulk elemental analysis techniques down to the part-per-million level. 

A single multielement calibration standard is used to establish a relative sensitivity factor (R.) for each analyte (i) to be determined in the multielement analysis. For solution analysis, this multielement standard is usually prepared from high-purity metal salts dissolved in deionized water, with sufficient nitric acid added to stabilize their concentrations (pH 2 or less). Because this is only a semiquantitative analysis, matrix matching of the calibration standard to the matrix of the sample is not required. When using solid analysis techniques (i.e., slurry nebulization, laser ablation, etc.), an appropriate solid phase multielement calibration standard is most desirable however, novel approaches for the use of a solution standard have been used with some methods. 

Heat Exchangers Using Non-Newtonian Fluids. Most fluids used in the chemical, pharmaceutical, food, and biomedical industries can be classified as non-Newtonian, ie, the viscosity varies with shear rate at a given temperature. In contrast, Newtonian fluids such as water, air, and glycerin have constant viscosities at a given temperature. Examples of non-Newtonian fluids include molten polymer, aqueous polymer solutions, slurries, coal—water mixture, tomato ketchup, soup, mayonnaise, purees, suspension of small particles, blood, etc. Because non-Newtonian fluids ate nonlinear in nature, these ate seldom amenable to analysis by classical mathematical techniques. 

Different analytical procedures have been developed for direct atomic spectrometry of solids applicable to inorganic and organic materials in the form of powders, granulate, fibres, foils or sheets. For sample introduction without prior dissolution, a sample can also be suspended in a suitable solvent. Slurry techniques have not been used in relation to polymer/additive analysis. The required amount of sample taken for analysis typically ranges from 0.1 to 10 mg for analyte concentrations in the ppm and ppb range. In direct solid sampling method development, the mass of sample to be used is determined by the sensitivity of the available analytical lines. Physical methods are direct and relative instrumental methods, subjected to matrix-dependent physical and nonspectral interferences. Standard reference samples may be used to compensate for systematic errors. The minimum difficulties cause INAA, SNMS, XRF (for thin samples), TXRF and PIXE. 

Attempts have been made to expand the technique to include the analysis of soil biotransformations f23.29V While the hydrodynamic nature and physical structure of soil systems vary widely and are difficult to establish with certainty, two limiting conditions may be specified. The first is where the soil particles are suspended and all phases are well-mixed. This case is not typically found in nature, but is found in various types of engineered soil-slurry reactors. The reactors currently used in our systems experiments include continuous stirred tank reactors (CSTRs) operated to minimize soil washout. 

Purge-and-trap collection is well adapted to biological samples such as blood or urine that are soluble in water (Pellizzari et al. 1985a Peoples et al. 1979), and is readily adapted from techniques that have been developed for the analysis of carbon tetrachloride in water and wastewater. For water- insoluble materials, the purge-trap approach is complicated by uncertainty of partitioning the analyte between sample slurry particles and water. 

NMR imaging techniques were applied to the measurements of velocity field in opaque systems such as tomato juice and paper pulp suspensions [58-60]. In both cases, the particle concentrations are sufficiently high that widely applied techniques such as hot film and laser Doppler anemometry could not be used. The velocity profile for a 6 % tomato juice slurry clearly showed a power-law behavior [58, 59]. Row NMR images for a 0.5 % wood pulp suspension provided direct visual of three basic types of shear flow plug flow, mixed flow and turbulent flow as mean flow rate was increased. Detailed analysis of flow NMR image is able to reveal the complex interaction between the microstructure of suspensions and the flow [60]. 

The slurry technique is an attractive compromise offering simplicity of sample preparation along with the convenience of a permanent or semi-permanent sample solution for repetitive analysis. The application of higher powder concentrations is a practical possibility, at least as far as lead is concerned, and then lower detection limits are then feasible. 

One of the advantages of GFAAS is the direct analysis of solid samples without prior decomposition, this technique has been reviewed by Bendicho and de Loos-Vollebregt (1991). The solid samples can be introduced directly or as a slurry. Calibration can be with aqueous standards, synthetic solids, standard additions or with SRMs. SRMs have been used for calibration for solid sampling of plant material (Schmidt and Falk, 1987). Examples of the use of solid samples with ETAAS are shown in Table 9-4. In many cases a matrix modifier is used with the sample, this allows the matrix to be volatilised at the pyrolysis stage without analyte loss, particularly important with volatile analytes such as Cd and Pb. (Ure, 1990). 

In the preceeding sections, development of the measurement technique and analysis of gas-phase characteristics in a slurry bubble column have been made along with some comparison of the experimental data with other correlations from the literature. Up to this point, analysis of gas-phase characteristics has included only single or binary liquid components. Recently, a large effect on gas holdup and bubble size has been observed for multicomponent liquid mixtures that contain small concentrations of surface-active species (24). In their study, mixtures of alcohols and water at alcohol concentrations less than 0.1 percent caused a dramatic increase in gas holdup (up to a factor of 2) and a decrease in bubble size (up to a factor of 4) compared to those observed for the water system. The authors think the effect is the result of- interaction between molecules of different species, leading to an enrichment of one species in the interface. Therefore, in multicomponent liquid mixtures, it is necessary to have knowledge of the presence of surface-active species as well as the physical properties of the fluid. 

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