Sample preparation contamination

See alsa Chromatography Multidimensional Techniques. Environmental Analysis. Extraction Solid-Phase Extraction. Food and Nutritional Analysis Sample Preparation Contaminants Pesticide Residues. Forensic Sciences Drug Screening in Sport Illicit Drugs. Herbicides. Liquid Chromatography Instrumentation Clinical Applications Food Applications. Mass Spectrometry Peptides and Proteins. Pesticides. Pharmaceutical Analysis Sample Preparation. Proteomics. Sample Handling Automated Sample Preparation. Water Analysis Organic Compounds. 

The very low Hg concentration levels in ice core of remote glaciers require an ultra-sensitive analytical technique as well as a contamination-free sample preparation methodology. The potential of two analytical techniques for Hg determination - cold vapour inductively coupled plasma mass spectrometry (CV ICP-SFMS) and atomic fluorescence spectrometry (AFS) with gold amalgamation was studied. 

Theoretical and applied aspects of microwave heating, as well as the advantages of its application are discussed for the individual analytical processes and also for the sample preparation procedures. Special attention is paid to the various preconcentration techniques, in part, sorption and extraction. Improvement of microwave-assisted solution preconcentration is shown on the example of separation of noble metals from matrix components by complexing sorbents. Advantages of microwave-assisted extraction and principles of choice of appropriate solvent are considered for the extraction of organic contaminants from solutions and solid samples by alcohols and room-temperature ionic liquids (RTILs). 

The performance of microwave-assisted decomposition of most difficult samples of organic and inorganic natures in combination with the microwave-assisted solution preconcentration is illustrated by sample preparation of carbon-containing matrices followed by atomic spectroscopy determination of noble metals. Microwave-assisted extraction of most dangerous contaminants, in particular, pesticides and polycyclic aromatic hydrocarbons, from soils have been developed and successfully used in combination with polarization fluoroimmunoassay (FPIA) and fluorescence detection. 

One of trends of development of thin-layer chromatography implies that replacement of aqueous-organic eluents by micellar surfactants solution. This is reduces the toxicity, flammability, environmental contamination and cost of the mobile phases, reduce sample prepar ation in some cases. 

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. 

PL measurements are generally nondestructive, and can be obtained in just about any configuration that allows some optically transparent access within several centimeters of the sample. This makes it adaptable as an in situ measurement tool. Little sample preparation is necessary other than to eliminate any contamination that may contribute its own luminescence. The sample may be in air, vacuum, or in any transparent, nonfluorescing medium. 

There are advantages to direct solid sampling. Sample preparation is less time consuming and less prone to contamination, and the analysis of microsamples is more straightforward. However, calibration may be more difficult than with solution samples, requiring standards that are matched more closely to the sample. Precision is typically 5% to 10% because of sample inhomogeneity and variations in the sample vaporization step. 

Most of the transition elements that are of primary interest in the semiconductor industry such as Fe, Cr, Mn, Co, and Ni, can be analyzed with very low detection limits. Second to its sensitivity, the most important advantage of NAA is the minimal sample preparation that is required, eliminating the likelihood of contamination due to handling. Quantitative values can be obtained and a precision of 1-5% relative is regularly achieved. Since the technique measures many elements simultaneously, NAA is used to scan for impurities conveniently. 

Large quantities of solvents are employed for sample preparation, in particular, and these are then concentrated down to a few milliliters. So particularly high quality materials that are as free as possible from residual water and especially free from nonvolatile or not readily volatile impurities ought to be employed here such impurities are enriched on concentration and can lead to gross contamination. The same considerations also apply to preparative chromatography. Special solvents of particular purity are now available. 

Although SFE and SFC share several common features, including the use of a superaitical fluid as the solvent and similar instrumentation, their goals are quite distinct. While SFE is used mainly for the sample preparation step (extraction), SFC is employed to isolate (chr-omatography) individual compounds present in complex samples (11 -15). Both techniques can be used in two different approaches off-line, in which the analytes and the solvent are either vented after analysis (SFC) or collected (SFE), or on-line coupled with a second technique, thus providing a multidimensional approach. Off-line methods are slow and susceptible to solute losses and contamination the on-line coupled system makes possible a deaease in the detection limits, with an improvement in quantification, while the use of valves for automation results in faster and more reproducible analyses (16). The off-line... 

The aspect of sample preparation and characterization is usually hidden in the smallprint of articles and many details are often not mentioned at all. It is, however, a very crucial point, especially with surface and interface investigations since there might be many unknown parameters with respect to surface contaminations, surface conformations, built-in stresses, lateral sample inhomogeneities, roughness, interfacial contact etc. This is in particular important when surfaces and interfaces are investigated on a molecular scale where those effects may be quite pronounced. Thus special care has to be taken to prepare well defined and artifact free specimens, which is of course not always simple to check. Many of these points are areas of... 

Sample preparation will involve extraction techniques, concentration procedures and methods for removing solid contaminants that may damage the sample valve, column or some other part of the... 

The relatively impure crude Ca obtained from both thermal reduction and electrolytic sources (97-98%) is distilled to give a 99% pure product. Volatile impurities such as the alkali metals are removed in a predistillation mode at 800°C subsequent distillation of the bulk metal at 825-850°C under vacuum removes most of the involatile impurities, such as Al, Cl, Fe and Si. The N content is often not reduced because of atmospheric contamination after distillation. Unfortunately, these commercial methods have no effect on Mg, which is the major impurity (up to 1 wt%). Typical analytical data for Ca samples prepared by electrolysis, thermal reduction (using Al) and distillation are collated in Table 1. 

Kinetic Analysis. Gas chromatographic analysis of the headspace gases confirms that the predominant reaction product is CO.. The negligible presence of N and 0 are probably due, at least in part, to air contamination during sample preparation for the GC analysis. The results of the GC analysis are shown in Table II. 

The 1970 s demonstrated a trend chemistry is going out of analytical chemistry . However, what was not used anymore up-ffont for analysis came bade in the form of sample preparation techniques. For example, lUPAC devoted as much attention as ever before, but now to the chemistry needed to prepare the sample for measurement and to avoid losses and contamination. 

During the last few years, miniaturization has become a dominant trend in the analysis of low-level contaminants in food and environmental samples. This has resulted in a significant reduction in the volume of hazardous and expensive solvents. Typical examples of miniaturization in sample preparation techniques are micro liquid/liquid extractions (in-vial) and solvent-free techniques such as solid-phase microextraction (SPME). Combined with state-of-the-art analytical instrumentation, this trend has resulted in faster analyses, higher sample throughputs and lower solvent consumption, whilst maintaining or even increasing assay sensitivity. 

Solubilizing all or part of a sample matrix by contacting with liquids is one of the most widely used sample preparation techniques for gases, vapors, liquids or solids. Additional selectivity is possible by distributing the sample between pairs of immiscible liquids in which the analyte and its matrix have different solubilities. Equipment requirements are generally very simple for solvent extraction techniques. Table 8.2 [4,10], and solutions are easy to manipulate, convenient to inject into chromatographic instruments, and even small volumes of liquids can be measured accurately. Solids can be recovered from volatile solvents by evaporation. Since relatively large solvent volumes are used in most extraction procedures, solvent impurities, contaminants, etc., are always a common cause for concern [65,66]. 

Industrial analytical laboratories search for methodologies that allow high quality analysis with enhanced sensitivity, short overall analysis times through significant reductions in sample preparation, reduced cost per analysis through fewer man-hours per sample, reduced solvent usage and disposal costs, and minimisation of errors due to analyte loss and contamination during evaporation. The experience and criticism of analysts influence the economical aspects of analysis methods very substantially. 

In general, new sample preparation technologies are faster, more efficient and cost effective than traditional sample preparation techniques. They are also safer, more easily automated, use smaller amounts of sample and less organic solvent, provide better target analyte recovery with enhanced precision and accuracy. Attention to the sample preparation steps has also become an important consideration in reducing contamination. A useful general guide to sample preparation has been published [3]. A recent review on sample preparation methods for polymer/additive analysis is also available [4]. 

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