Powdered sample methods

Absorption of x-rays by a powdered sample of soHd fat has been a useful method for determination of polymorphic character as discussed eadier. The a, and P forms may be distinguished however, interpretation is made more difficult because subsets of the P and P forms have often been encountered. Also, a fat may contain mixtures of polymorphic forms and properties may therefore be difficult to relate to the spectra. 

Colorimetric Method. A finely powdered sample treated with sulfuric acid, hydrobromic acid [10035-10-6] and bromine [7726-95-6] gives a solution that when adjusted to pH 4 may be treated with dithi one [60-10-6] ia / -hexane [110-54-3] to form mercuric dithi2onate [14783-59-6] (20). The resultant amber-colored solution has a color iatensity that can be compared against that of standard solutions to determine the mercury concentration of the sample. Concentrations below 0.02 ppm have been measured by this method. 

The capillary tube method initially involves packing a powdered sample into a glass capillary tube of uniform diameter and length, carefully sealed at one end so that it forms a rounded tube of uniform thickness. The tube is then attached to a standardized thermometer so that the end of the tube reaches the middle of the thermometer reservoir bulb. This assembly is then inserted into a vessel contg a suitable liq which is uniformly heated so that the temp rises at a rate of about 1° per minute. Ref 1 discusses in detail equipment design and thermometer calibration. It should be noted that this technique is the method most widely used by organic chemists... 

Porous materials, such as silica and alumina, have thermal diffusion lengths of approximately 10 m, which is much less than the typical thickness of pressed discs. The small thermal diffusion length gives photoacoustic spectroscopy a larger dynamic range than transmission methods when applied to powdered samples. An additional advantage is the ease of sample preparation, since photoacoustic spectroscopy uses powdered samples with no special preparation required. 

Traditionally, the penetration of chlorides and sodium is measured destructively by grinding layers of concrete and chemically analyzing the powder samples. These data are used to calculate diffusion coefficients for the ions. This procedure is very slow, has low spatial resolution, and is destructive. The measured data are critically important for the development of service life models and therefore a rapid, high-resolution method to monitor the ingress of these ions is desirable. 

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. 

Chatterjee et al. [20] quantitatively separated primaquine from amodiquine by a selective precipitation method. A powdered sample containing primaquine and amodiaquine was dissolved in 0.01 N hydrochloric acid 4 N ammonia was added to precipitate amodiaquine. The mixture was filtered and the combined filtrate and washings containing primaquine was diluted with water and 0.1 N hydrochloric acid. The absorbance of this solution was measured at 282 nm versus a solvent blank. 

Porosity characteristics were determined by N2 adsorption-desorption at 77 K (Dubinin method) with a Thermoquest Sorptomatic 1990. Powder samples were outgassed (10 4 Torr) and heated to 450°C before each test. 

Property measurements of fullerenes are made either on powder samples, films or single crystals. Microcrystalline C6o powder containing small amounts of residual solvent is obtained by vacuum evaporation of the solvent from the solution used in the extraction and separation steps. Pristine Cgo films used for property measurements are typically deposited onto a variety of substrates (< . , a clean silicon (100) surface to achieve lattice matching between the crystalline C60 and the substrate) by sublimation of the Cr,o powder in an inert atmosphere (e.g., Ar) or in vacuum. Single crystals can be grown either from solution using solvents such as CS and toluene, or by vacuum sublimation [16, 17, 18], The sublimation method yields solvent-free crystals, and is the method of choice. 

The simplest method of XRD analysis, used in early studies and described by Tite (1972 286), is the powder diffraction method. A small sample, typically 5-10 mg, is removed from the artifact, either by scraping the surface, cutting... 

Figure 6.13. Experimental arrangement of the hot-explosive compaction method for the preparation of consolidated Ni-Al alloys (after Kecskes etal. 2004). (a) Precursor powder sample inside a steel-tube container placed in, (b) an asbestos thermal insulation sheet (c) a concentric card-box filled with the powdered explosive (80% NH4NO3 + 20% TNT) (d) threaded steel plugs serving as contacts for the preliminary heating and to be lifted off just before detonating the explosive (e) detonating cords.

Different sampling methods often result in collection of different components of the element or compound of interest. Most seawater samples are collected in bottles, filtered to remove particles and analyzed directly or after preconcentration of minor components. Particulate matter from the water column is collected by filtration or with sediment traps. Sediment samples are collected in cores that recover intact chronological sequences and are commonly subsampled, dried and ground to a powder. Pore waters are extracted from sediments by squeezing or suction, dialysis, and centrifugation. 

Spectra of powder samples can be measured using different methods which have been described and discussed in detail elsewhere 234, 235). It needs only to be indicated here that the technique used has a decided influence on the resulting spectrum. 

---