Particle size sampling technique

IAEA/AL/095 1996). Both methods were suitable, but needed to be repeated several times to produce the small particle size that was required. The particle size reduction, e.g. of IAEA-395 from a median size of 30 pm to 3.5 pm, improved the homogeneity of elements. Sampling constants (the minimum mass that can be used to achieve a random error of i % at the 65 % confidence level) improved from a factor of 1.2 for Sc, up to a factor of 800 for Au. The average improvement was about a factor of 2-10. (Ni Bangfa et al. 1996). From these initial experiences, it is dear that preparation of reference materials is critical with respect to the final particle size distribution, which should exhibit a low maximum (<50 pm) and a narrow range in particle sizes. Milling techniques to meet such criteria are available today, and materials that show intrinsic uniformity are particularly suitable to achieve the desired properties. 

To obtain representative samples from nonhomoge-neous sample materials, such as polymer compounds, particle-size reduction techniques need often to be applied (not for film) [50]. Also, for destructive inpolymer additive analysis it is advantageous to change the physical state of solid samples to provide a larger surface area per unit mass. Complete extraction is sometimes achieved only after grinding the sample. Typically, Perlstein [51] has reported recoveries of only 59 % for extraction of Tinuvin 320 from unground PVC after 16 h of Soxhlet extraction with diethyl ether while recoveries rise to 97 % for ground polymer. 

The DR technique lends itself to polymorph studies since the technique is noninvasive, the polymorph character remains intact due to limited sample handling, and the technique is quantitative (4). One disadvantage to diffuse reflectance IR is that it is a particle size-dependent technique (22). Development of quantitative polymorph assays require that the particle size of each component be limited to a specific range, including both components of a mixture, and the nonabsorbing matrix if the mixture is not sampled neat. It must also be kept in mind that for a quantitative assay, all calibration, validation, and subsequent samples to be assayed must fall within the particle size range otherwise, significant prediction errors may arise. 

It is very likely that a sample collected from the main production stream is going to be too large for most particle size analysis techniques the... 

Sedimentation (qv) techniques, whether based on gravitational forces or centrifugation, derive the particle size from the measured travel rates of particles in a Hquid. Before the particle analysis is carried out, the sample is usually dispersed in a medium to break down granules, agglomerates, and aggregates. The dispersion process might involve a simple stirring of the powder into a Hquid, but the use of an ultrasonic dispersion is preferred. 

The two techniques differ in that HDC employs a nonporous stationary phase. Separation is affected as a result of particles of different size sampling different velocities in the interstitial spaces. Size exclusion chromatography is accomplished by superimposing a steric selection mechanism which results from the use of a porous bed. The pore sizes may vary over a wide range and the separation occurs as a result of essentially the same processes present in the gel permeation chromatography of macromolecules. 

As an alternative approach towards the above requirement, Somorjai introduced the method of electron lithography [119] which represents an advanced HIGHTECH sample preparation technique. The method ensures uniform particle size and spacing e.g. Pt particles of 25 nm size could be placed with 50 nm separation. This array showed a uniform activity similar to those measured on single crystal in ethylene hydrogenation. The only difficulty with the method is that the particle size is so far not small enough. Comprehensive reviews have been lined up for the effect of dispersion and its role in heterogeneous catalysis [23,124,125]. 

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