Sample preparation methods method

This sample preparation method (Method 1) is the result of several experiments. An attempt was also made to extract the deproteinated sample with alkali (Method 2) without previously extracting with toluene. As a comparison, an experiment was carried out in which the toluene phase was evaporated to dryness and then acetylated (Method 3). The results are given in Table 9-5. The criterion was again the recovery rate. 

The following experiments introduce students to the importance of sample preparation and methods for extracting analytes from their matrix. Each experiment includes a brief description of the sample and analyte, as well as the method of analysis used to measure the analyte s concentration. 

Sample preparation methods vary widely. The very first procedure for characterizing any material simply is to look at it using a low-power stereomicroscope often, a material can be characterized or a problem solved at this stage. If examination at this level does not produce an answer, it usually si ests what needs to be done next go to higher magnification mount for FTIR, XRD, or EDS section isolate contaminants and so forth. 

The coupling of supercritical fluid extraction (SEE) with gas chromatography (SEE-GC) provides an excellent example of the application of multidimensional chromatography principles to a sample preparation method. In SEE, the analytical matrix is packed into an extraction vessel and a supercritical fluid, usually carbon dioxide, is passed through it. The analyte matrix may be viewed as the stationary phase, while the supercritical fluid can be viewed as the mobile phase. In order to obtain an effective extraction, the solubility of the analyte in the supercritical fluid mobile phase must be considered, along with its affinity to the matrix stationary phase. The effluent from the extraction is then collected and transferred to a gas chromatograph. In his comprehensive text, Taylor provides an excellent description of the principles and applications of SEE (44), while Pawliszyn presents a description of the supercritical fluid as the mobile phase in his development of a kinetic model for the extraction process (45). 

Mark, H. "Use of Mahalanobis Distances to Evaluate Sample Preparation Methods for Near-Infrared Reflectance Analysis", Anal. Chem. 1987 (59) 790-795. 

Second, the properties of micro/nano friction and wear/ scratch of several representative films are introduced. These films include from organic molecular films, solid films, to multilayers. The experiments were designed reasonably to understand the behaviors of micro/nano friction and wear of the films. The sample preparation methods were also de-... 

Several methods are available for the analysis of trichloroethylene in biological media. The method of choice depends on the nature of the sample matrix cost of analysis required precision, accuracy, and detection limit and turnaround time of the method. The main analytical method used to analyze for the presence of trichloroethylene and its metabolites, trichloroethanol and TCA, in biological samples is separation by gas chromatography (GC) combined with detection by mass spectrometry (MS) or electron capture detection (ECD). Trichloroethylene and/or its metabolites have been detected in exhaled air, blood, urine, breast milk, and tissues. Details on sample preparation, analytical method, and sensitivity and accuracy of selected methods are provided in Table 6-1. 

How critically interdependent matrix and analytical methods can be is illustrated in the example of the analysis of a soil sample. Table 7.1 shows the method dependent certified values for some common trace elements. The soil had been subjected to a multi-national, multi-laboratory comparison on a number of occasions (Houba et al. 1995) which provided extensive data. The data was subjected to a rigorous statistical program, developed for the USEPA by Kadafar (1982). This process allowed the calculation of certified values for a wide range of inorganic analytes. Uniquely, for the soil there are certified values for four very different sample preparation methods, as follows ... 

Dai, Y., Whittal R.M., and Li, L., Two-layer sample preparation a method for MALDI-MS analysis of complex peptide and protein mixtures, Anal. Chem., 71, 1087, 1999. 

Sample matrix Sample preparation Analytical method Detection limit Accuracy Reference... 

Of the radioassays that are commonly used to quantify americium, a-spectroscopy is used when isotopic analyses of americium must be conducted (e.g., 241Am and 243Am). 243Am is often added as a tracer to estimate the efficiency of the sample preparation method when quantifying 241Am in biological matrices. 

The preponderance of analytical sample preparation methods employs some type of extraction. Traditionally, these methods were liquid-liquid, liquid-solid, and hot... 

In order to increase the overall extraction efficiency during SFE sonication has been applied [352]. Ultrasound creates intense sinusoidal variations in density and pressure, which improve solute mass transfer. Development of an SFE method is a time-consuming process. For new methods, analysts should refer the results to a traditional sample preparation method such as Soxhlet or LLE. 

P.D. McDonald and E.S.P. Bouvier, Solid Phase Extraction Applications Guide and Bibliography, A Resource for Sample Preparation Methods Development, Waters, Milford, MA... 

L.G. RandaU, W.S. Miles, F. Rowland and C.R. Knipe, Designing a Sample Preparation Method Which Employs Supercritical Fluid Extraction (SFE), Hewlett-Packard Publ. 435091-2102E, Wilmington, DE (1994). 

Table 4.15 Sample preparation methods used in GC analysis ...

Berger [340] has examined the use of pSFC in polymer/additive analysis. As many polymer additives are moderately polar and nonvolatile SFC is an appropriate separation technique at temperatures well below those at which additives decompose [300,341,342], SFC is also a method of choice for additives which hydrolyse easily. Consequently, Raynor et al. [343] and others [284,344] consider that SFC (especially in combination with SFE) is the method of choice for analysing polymer additives as a relatively fast and efficient sample preparation method. Characterisation of product mixtures of nonpolar to moderately polar components encompassing a wide range of molecular masses can be accomplished by cSFC-FID. Unknown polymer additives may be identified quite adequately by means of cSFC-FID by comparison with retention times of standards [343], However, identification by this method tends to be time-consuming and requires that all the candidate compounds are on hand. SFC-FID of some low-to-medium polarity additives on reversed-phase packed columns... 

Standard practices for GC-IR analysis have been described (ASTM E 1642-94). Griffiths [200] has discussed GC-FTIR designs. Sample preparation methods for hyphenated infrared techniques, in particular GC-FTIR, have been reported [201]. The technique has been reviewed repeatedly [167,183,201-204] a monograph [205] has appeared. 

Destructive solid sample preparation methods, such as digestion and mineralisation, are well known as they have been around for some time they are relatively cheap and well documented [13-15]. Decomposition of a substance or a mixture of substances does not refer so much to the dissolution, but rather to the conversion of slightly soluble substances into acid- or water-soluble (ionogenic) compounds (chemical dissolution). 

Indeed, a bDNA assay for diagnosis of African trypanosomiasis was developed and compared with buffy coat microscopy for detection of T brucei in human blood samples (Harris etal., 1996). Two repetitive DNA sequences found only in the T. brucei complex, a 177-bp satellite repeat and the ribosomal mobile element, were selected as targets in the bDNA assay. The assay used the standard bDNA components capture probes, target probes, amplifier molecules, and alkaline phosphatase-labeled probes. Various blood fractions and sample preparation methods were examined. Ultimately, buffy coat samples resulted in the highest sensitivity. Although typanosomes do not infect leukocytes, they cosediment with them. 

It needs to be pointed out, that the investigation of some technically important polymers like polyolefines has not been very successful so far. Owing to their inert nature they are difficult to dissolve and also difficult to ionize. Typically one needs for the ionization process some heterogeneities or double bonds in the polymer. For some insoluble substances a solvent-free sample preparation method has been developed that allows a characterization by MALDI-TOF mass spectrometry [93]. 

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