Sizing by filtration

There are numerous options for combining phospholipids with an aqueous phase, but two major methods are used to make liposomal systems for drug delivery. The first is simple hydration (swelling) of the phospholipid. This is followed by high-intensity agitation using sonication or a high-shear impeller. Liposomes are then sized by filtration, extrusion or elutriation. The second method is an emulsion... 

Particle sizing by filtration was unsuccessful because of pore clogging of the Nuclepore membrane. Results of filtration experiments confirm the results of work cited previously and lead to two major conclusions (1) vacuum membrane filtration is not an acceptable means of particle sizing and (2) membranes with pore sizes of 1 /xm or less should be used for suspended-solids analysis. 

Informative distribution patterns can be obtained using only two or three filters having different pore sizes if the membrane filtration is combined with acidification of water fractions. Thus, an analytical scheme for determining the speciation of aluminum in natural waters has been described. The scheme is based on sizing by filtration of acidified and unacidified water sample portions through 0.1 and 0.4 pm... 

Particulate interferents can be separated from dissolved analytes by filtration, using a filter whose pore size retains the interferent. This separation technique is important in the analysis of many natural waters, for which the presence of suspended solids may interfere in the analysis. Filtration also can be used to isolate analytes present as solid particulates from dissolved ions in the sample matrix. For example, this is a necessary step in gravimetry, in which the analyte is isolated as a precipitate. A more detailed description of the types of available filters is found in the discussion of precipitation gravimetry and particulate gravimetry in Chapter 8. 

Nutsche Filter. The nutsche filter (Fig. 8) is simply an industrial-scale equivalent of the laboratory Buckner funnel. Nutsche filters consist of cylindrical or rectangular tanks divided into two compartments of roughly the same size by a horizontal medium supported by a filter plate. Vacuum is apphed to the lower compartment, into which the filtrate is collected. It is customary to use the term nutsche only for filters that have sufficient capacity to hold the filtrate from one complete charge. The cake is removed manually or sometimes by reslurrying. 

In a suspension polymerization, monomer is suspended ia water as 0.1—5 mm droplets, stabilized by protective coUoids or suspending agents. Polymerization is initiated by a monomer-soluble initiator and takes place within the monomer droplets. The water serves as both the dispersion medium and a heat-transfer agent. Particle size is controlled primarily by the rate of agitation and the concentration and type of suspending aids. The polymer is obtained as small beads of about 0.1—5 mm in diameter, which are isolated by filtration or centrifugation. 

Filtered-Particle Inspection. Solids containing extensive inteiconnected porosity, eg, sintered metallic or fired ceramic bodies formed of particles that ate typically of 0.15-mm (100-mesh) screen size, are not inspectable by normal Hquid penetrant methods. The preferred test medium consists of a suspension of dyed soHd particles, which may be contained in a Hquid vehicle dyed with a different color. Test indications can form wherever suspensions can enter cracks and other discontinuities open to the surface and be absorbed in porous material along interior crack walls. The soHd particles that form test indications ate removed by filtration along the line of the crack at the surface where they form color or fluorescent indications visible under near-ultraviolet light (1,3). 

Equipment. Centrifugation equipment that separates by density difference is available in a variety of sizes and types and can be categorized by capacity range and the theoretical settling velocities of the particles normally handled. Centrifuges that separate by filtration produce drained soflds and can be categorized by final moisture, drainage time, G, and physical characteristics of the system, such as particle size and Hquid viscosity. 

Common names have been given to sodium sulfate as a result of manufacturiag methods. In rayon production, by-product sodium sulfate is separated from a slurry by filtration where a 7—10-cm cake forms over the filter media. Thus rayon cake was the term coiaed for this cake. Similarly, salt cake, chrome cake, phenol cake, and other sodium sulfate cakes were named. Historically, sulfate cakes were low purity, but demand for higher purity and controlled particle size has forced manufacturers either to produce higher quaUty or go out of busiaess. Sodium sulfate is mined commercially from three types of mineral evaporites thenardite, mirabilite, and high sulfate brine deposits (see Chemicals FROMBRINe). 

Suspension Polymerization. At very low levels of stabilizer, eg, 0.1 wt %, the polymer does not form a creamy dispersion that stays indefinitely suspended in the aqueous phase but forms small beads that setde and may be easily separated by filtration (qv) (69). This suspension or pearl polymerization process has been used to prepare polymers for adhesive and coating appHcations and for conversion to poly(vinyl alcohol). Products in bead form are available from several commercial suppHers of PVAc resins. Suspension polymerizations are carried out with monomer-soluble initiators predominantly, with low levels of stabilizers. Suspension copolymerization processes for the production of vinyl acetate—ethylene bead products have been described and the properties of the copolymers determined (70). Continuous tubular polymerization of vinyl acetate in suspension (71,72) yields stable dispersions of beads with narrow particle size distributions at high yields. 

Grade 2 water to reverse osmosis or de-ionisation, followed by filtration through a membrane filter of pore size 0.2 jum to remove particulate matter. Alternatively, Grade 2 water may be redistilled in an apparatus constructed from fused silica. 

The physical nature of the precipitate must be such that it can be readily separated from the solution by filtration, and can be washed free of soluble impurities. These conditions require that the particles are of such size that they do not pass through the filtering medium, and that the particle size is unaffected (or, at least, not diminished) by the washing process. 

In general, fungal mycelia are filtered relatively easily, because mycelia filter cake has sufficiently large porosity. Yeast and bacteiia are much more difficult to handle because of thefr small size. Alternative filtration methods, which eliminate the filter cake, are becoming more acceptable for bacterial and yeast separation. Micro-filtration is achieved by developing large cross-flow fluid velocities across the filter surface while the velocity vector normal to the surface is relatively small. Build up of filter cake and problems of high cake resistance are therefore prevented. Micro-filtration is not discussed in this section. 

The sampling of solution for activity measurement is carried out by filtration with 0.22 pm Millex filter (Millipore Co.) which is encapsuled and attached to a syringe for handy operation. The randomly selected filtrates are further passed through Amicon Centriflo membrane filter (CF-25) of 2 nm pore size. The activities measured for the filtrates from the two different pore sizes are observed to be identical within experimental error. Activities are measured by a liquid scintillation counter. For each sample solution, triplicate samplings and activity measurements are undertaken and the average of three values is used for calculation. Absorption spectra of experimental solutions are measured using a Beckman UV 5260 spectrophotometer for the analysis of oxidation states of dissolved Pu ions. 

SWNTs (HiPco, Carbon Nanotechnologies Incorporated) were shortened by ultrasonication with a probe-type sonicator in mixed acids (H2SO4 and HNO3) under ice-cooling. After diluting the mixture with water (MiliQ), the shortened SWNTs were purified by filtration through a PTFE membrane filter (pore size 1 pm or 0.2 pm) or by chromatography (Sepadex G-50). 

Table 2.7 lists techniques used to characterise carbon-blacks. Analysis of CB in rubber vulcanisates requires recovery of CB by digestion of the matrix followed by filtration, or by nonoxidative pyrolysis. Dispersion of CB within rubber products is usually assessed by the Cabot dispersion test, or by means of TEM. Kruse [46] has reviewed rubber microscopy, including the determination of the microstructure of CB in rubber compounds and vulcanisates and their qualitative and quantitative determination. Analysis of free CB features measurements of (i) particulate and aggregate size (SEM, TEM, XRD, AFM, STM) (ii) total surface area according to the BET method (ISO 4652), iodine adsorption (ISO 1304) or cetyltrimethylammonium bromide (CTAB) adsorption (ASTM D 3765) and (iii) external surface area, according to the dibutylphthalate (DBP) test (ASTM D 2414). TGA is an excellent technique for the quantification of CB in rubbers. However, it is very limited in being able to distinguish the different types of... 

Method Polishing treatment after chemical precipitation and sedimentation by filtration through a bed of particles of several distinct size ranges. 

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