Particle distribution, resolution

The slopes of the calibration curves for the HDC and Fractosil systems are 0.512 and 0.289, respectively. This indicates that the "resolution of the peak separation" for the Fractosil system is superior to that of HDC, since resolution is considered to be inversely proportional to the slope of the log particle diameter - AV calibration curve (26). However when peak spreading is taken into account, the actual relative resolution between particle populations is less for the Fractosil system 2k) a result which indicates that overall, for size distribution resolution, the HDC system is superior. 

The latter approach—completely drying the aerosol— while valid, is diffi-cnlt to perform experimentally (29). The low solids content of pharmaceutical nebulizer solutions results in dry aerosols that are too fine for reliable enough measurements to be made to allow back calculation with any accuracy. For example a typical nebulizer droplet distribution with a mass median diameter of 3 pm generated from a 0.1% drug solution would result in a dry particle distribution with a mass median diameter of 0.1 pm. Obtaining size distribution data with any reasonable resolution at this size is very problematic. A further issue is that the solids content of the original droplets must be known in order to perform the calculation, and this can vary considerably during the course of nebulization. This technique has therefore not been used extensively. 

Figure C2.17.4. Transmission electron micrograph of a field of Zr02 (tetragonal) nanocrystals. Lower-resolution electron microscopy is useful for characterizing tire size distribution of a collection of nanocrystals. This image is an example of a typical particle field used for sizing puriDoses. Here, tire nanocrystalline zirconia has an average diameter of 3.6 nm witli a polydispersity of only 5% 1801.

The electrical aerosol analyzer and the optical counter are used to measure particle size distributions. Describe the size range and resolution characteristics of each of these instruments. 

Because a FIXE spectrum represents the int al of all the X rays created along the particle s path, a single FIXE measurement does not provide any depth profile information. All attempts to obtain general depth profiles using FIXE have involved multiple measurements that varied either the beam energy or the angle between the beam and the target, and have compared the results to those calculated for assumed elemental distributions. Frofiles measured in a few special cases surest that the depth resolution by nondestructive FIXE is only about 100 nm and that the absolute concentration values can have errors of 10-50%. 

The Mattauch-Herzoggeometry (Fig. 3.20) enables detection of several masses simultaneously and is, therefore, ideal for scanning instruments [3.49]. Up to five detectors are adjusted mechanically to locations in the detection plane, and thus to masses of interest. Because of this it is possible to detect, e. g., all isotopes of one element simultaneously in a certain mass range. Also fast, sensitive, and precise measurements of the distributions of different isotopes are feasible. This enables calculation of isotope ratios of small particles visible in the image. The only commercial instrument of this type (Cameca Nanosims 50) uses an ion gun of coaxial optical design, and secondary ion extraction the lateral resolution is 50 nm. 

Two-phase suspension systems produce beaded products with broader particle-size distribution (e.g., 1-50 /rm). The microspherical particles usually need to be classified repeatedly to reduce the particle-size distribution in order to improve the resolution and efficiency in the separation for use in chromatography. The actual classification process depends on the size range involved, the nature of the beaded product, and its intended applications. Relatively large (>50 /rm) and mechanically stable particles can be sieved easily in the dry state, whereas small particles are processed more conveniently in the wet state. For very fine particles (<20 /rm), classification is accomplished by wet sedimentation, countflow setting, countflow centrifugation, or air classification. 

The advantages of monosized chromatographic supports are as follows a uniform column packing, uniform flow velocity profile, low back pressure, high resolution, and high-speed separation compared with the materials of broad size distribution. Optical micrographs of 20-p,m monosized macroporous particles and a commercial chromatography resin of size 12-28 p,m are shown in Fig. 1.4. There is a clear difference in the size distribution between the monodispersed particles and the traditional column material (87). 

All packing materials produced at PSS are tested for all relevant properties. This includes physical tests (e.g., pressure stability, temperature stability, permeability, particle size distribution, porosity) as well as chromatographic tests using packed columns (plate count, resolution, peak symmetry, calibration curves). PSS uses inverse SEC methodology (26,27) to determine chromatographic-active sorbent properties such as surface area, pore volume, average pore size, and pore size distribution. Table 9.10 shows details on inverse SEC tests on PSS SDV sorbent as an example. Pig. 9.10 shows the dependence... 

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