Sample preparation size limitation

Several objective methods are available to determine the freshness of shrimp however, many require a) raw products for analysis, b) complex chemistry and equipment for testing, or c) highly trained technicians. Additionally, some of these methods require extensive analysis time making results meaningless if product has already spoiled or has been released to consumers. Results for the impedance method discussed in the present paper demonstrate that spoilage of raw or thermally processed shrimp can be detect in 30 min with easy sample preparation. The limitations of this method revolve around the requirement for authentic fresh frozen standards as a basis for comparison. Further research is necessary to define the effect of seasonal and geographical variations, and species and size difference. The sum of these factors will likely affect the reproducibility of this method. 

At X-ray fluorescence analysis (XRF) of samples of the limited weight is perspective to prepare for specimens as polymeric films on a basis of methylcellulose [1]. By the example of definition of heavy metals in film specimens have studied dependence of intensity of X-ray radiation from their chemical compound, surface density (P ) and the size (D) particles of the powder introduced to polymer. Have theoretically established, that the basic source of an error of results XRF is dependence of intensity (F) analytical lines of determined elements from a specimen. Thus the best account of variations P provides a method of the internal standard at change P from 2 up to 6 mg/sm the coefficient of variation describing an error of definition Mo, Zn, Cu, Co, Fe and Mn in a method of the direct external standard, reaches 40 %, and at use of a method of the internal standard (an element of comparison Ga) value does not exceed 2,2 %. Experiment within the limits of a casual error (V changes from 2,9 up to 7,4 %) has confirmed theoretical conclusions. 

Sample size and matrix Your choice of analytical method will also be dependent on the amount of sample you have, especially if the amount is limited and some of the methods under consideration are destructive to the sample. In the Bulging Drum Problem, sample size was not an issue. However, sampling the gas in the drum was challenging, since loss and contamination were quite likely. Getting the samples to the lab presented other challenges. Sample matrix is another important factor in method choice. As you know, some methods and instrumental techniques are not suitable for analysis of solids, without sample preparation. Table 21.8 lists some of the issues that must be considered for different sample matrices. 

Bogan MJ, Agnes GR. 2004. WaU-less sample preparation of micron-sized sample spots for femtomole detection limits of proteins from liquid based UV-MALDI matrices. J Am Soc Mass Spectrom 15 486. 

Infrared Spectroscopy. The use of IR (9.10.11.12) and FTIR (3.4) for coal mineralogy has been reported. Painter and coworkers (3) demonstrated that FTIR can provide a virtually complete analysis. Painter, Brown and Elliott (4), and others (9.10.11) discuss sample preparation, reference minerals, and data analysis. The advantages of IR are 1) high sensitivity to molecular structure, 2) unequivocal identification of a number of minerals, 3) small sample size (a few milligrams), and 4) rapid analysis time (once LTA is available). Disadvantages include 1) reliance on reference minerals, 2) requires careful attention to sample preparation, and 3) limited selectivity (discrimination among similar minerals). 

A newer approach for lipid analysis is electrospray ionization tandem mass spectrometry (ESI-MS/MS) (Welti et al., 2002). This method requires limited sample preparation and sample size to identify and quantify lipids. Fauconnier et al. (2003) used ESI-MS/MS to analyze phospholipid and galactolipid levels during aging of potato tubers. 

Fig. 2 Two methods of sample preparation selectivity by polarity or by molecular size. Fractionation by polarity, e.g., using Florisil (vertical fraction), selects a limited range of the pesticides but does not remove high-molecular-weight materials of similar polarity. GPC (horizontal fraction) removes primarily material of high molecular weight, leaving all the pesticides (and other compounds of similar molecular weight) in the fraction. (From Ref. 19.)...

Some of the disadvantages were overcome by the use of the colloidal probe technique to measure adhesion forces (review Ref. [216]). The colloidal probe technique offers the advantage that the same particle can be used for a series of experiments and its surface can be examined afterwards. The accessible range of particle size is typically limited to a range between 1 /zm and 50 pm. The tedious sample preparation, limits the number of different particles used within one study, for practical reasons. Therefore the colloidal probe and centrifugal methods complement each other. 

Microcline, albite and labradorite were obtained from Ward s Canada Limited. Cleaved crystal fragments and 60 mesh-sized samples were ultrasonically cleaned prior to use. Powdered samples (particle size < 25 ym) were prepared by grinding in a tungsten carbide ball mill, wet-sieving and washing in water. 

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