Soil, biological analysis

S. D. Siciliano and J. J. Germida, Biolog analysis and fatly acid methyl ester profiles indicate that pseudormonad inoculants that promote phytoremediation alter the root-as.sociated microbial community of Bromus hiehersteinii. Soil Biol. Biochem. 30 1717 (1998). 

Schmid, O. (1984) Chemical soil analysis methods in biological husbandry. In Lampkin, N. and Woodward, L. (eds) The Soil Assessment, Analysis and Utilisation in Organic Agriculture. Elm Farm Research Centre, Practical Handbook Series, EFRC, Hamstead Marshall, UK, pp. 36M3. 

Adams, M.A. and Byrne, L.T. (1989) NMR analysis of phosphorus compounds in extracts of surface soils from selected Karri Eucalyptus diversicolor F. Muell.) forests. Soil Biology and Biochemistry 2), 523-528. 

For the analysis of trace quantities of analytes, or where an exhaustive extraction of the analytes is required, purge and trap, or dynamic headspace extraction methods, are preferred over static headspace extraction methods. Purge and trap has been used for both solid and liquid samples, which include environmental [water (45-47) and soil], biological (47,48), industrial, pharmaceutical, and agricultural samples. Like SHE, purge and trap relies on the volatility of the analytes... 

PANCHOLY S.K. and LYND J.Q. 1972. Quantitative fluorescence analysis of soil lipase activity. Soil Biology and Biochemistry, 4, 257-259. 

TAN K.H. 1978. Fomation of metal-fulvic acid complexes by titration and their characterisation by differential themal analysis and infrared spectroscopy. Soil Biology and Biochemistry, 10, 123-129. 

Determination of benzene in air samples has been achieved by bubbling contaminated air through various solvents, followed by uv or in analysis of the solution (90). Methods for identifying benzene in soil, water, and biological media are further described in references 84 and 85. 

Instiximental neutron activation analysis (INAA) is considered the most informative and highly sensitive. Being applied, it allows detecting and determination of 30-40 elements with the sensitivity of 10 -10 g/g in one sample. The evident advantage of INAA is the ability to analyze samples of different nature (filters, soils, plants, biological tests, etc.) without any complex schemes of preliminai y prepai ation. 

There are numerous examples of successful application of the developed procedures using native and immobilized enzymes in analysis of environmental (waters and soils of different types, air) and biological (blood semm, urine) samples. 

Supercritical fluid extraction (SFE) and Solid Phase Extraction (SPE) are excellent alternatives to traditional extraction methods, with both being used independently for clean-up and/or analyte concentration prior to chromatographic analysis. While SFE has been demonstrated to be an excellent method for extracting organic compounds from solid matrices such as soil and food (36, 37), SPE has been mainly used for diluted liquid samples such as water, biological fluids and samples obtained after-liquid-liquid extraction on solid matrices (38, 39). The coupling of these two techniques (SPE-SFE) turns out to be an interesting method for the quantitative transfer... 

In situ densitometry has been the most preferred method for quantitative analysis of substances. The important applications of densitometry in inorganic PLC include the determination of boron in water and soil samples [38], N03 and FefCNfg in molasses [56], Se in food and biological samples [28,30], rare earths in lanthanum, glass, and monazite sand [22], Mg in aluminum alloys [57], metallic complexes in ground water and electroplating waste water [58], and the bromate ion in bread [59]. TLC in combination with in situ fluorometry has been used for the isolation and determination of zirconium in bauxite and almnimun alloys [34]. The chromatographic system was silica gel as the stationary phase and butanol + methanol + HCl -H water -n HF (30 15 30 10 7) as the mobile phase. 

The classical approach for particle size determination, or more correctly for particle size selection - which is still used for solids like soils, sediments and other technical materials like coal, and also for biological materials - is sieving analysis. The raw material is milled, generally after drying, see Section 2.1, and if the required particle size is obtained, typically ranging from <0.1 to a few mm, it is allowed to pass sieves with different apertures to discard coarse particles and remaining materials. For materials consisting of numerous different particles microscopical inspection is used. 

Reversed-phase HPLC followed by post-column derivatization and subsequent fluorescence detection is the most common technique for quantitative determination of oxime carbamate insecticides in biological and environmental samples. However, for fast, sensitive, and specific analysis of biological and environmental samples, detection by MS and MS/MS is preferred over fluorescence detection. Thus, descriptions and recommendations for establishing and optimizing HPLC fluorescence, HPLC/ MS, and HPLC/MS/MS analyses are discussed first. This is followed by specific rationales for methods and descriptions of the recommended residue methods that are applicable to most oxime carbamates in plant, animal tissue, soil, and water matrices. 

Biological and Analytical Applications. - Phosphorus-31 n.m.r. continues to expand its application in the medical and biological fields20 and is now being applied to soil analysis.21 The problems involved in the use of FT 31P n.m.r. for quantitative determinations have been discussed.22 Samples of phosphinic carboxylic acids were cooled to -40°Cfor quantitative estimations.23... 

Methods for determining acrylonitrile in environmental samples are quite good. It may be assumed that the normal incentives for both research and the development of commercial methods of analysis will result in new analytical methods for acrylonitrile that have improved sensitivity and selectivity. Degradation products of acrylonitrile in environmental media are difficult to determine. This difficulty is not as much an analytical problem as it is a problem of knowing the fundamental environmental chemistry of these compounds in water, soil, air and biological systems. 

The potential for the employment of plasma emission spectrometry is enormous and it is finding use in almost every field where trace element analysis is carried out. Some seventy elements, including most metals and some non-metals, such as phosphorus and carbon, may be determined individually or in parallel. As many as thirty or more elements may be determined on the same sample. Table 8.4 is illustrative of elements which may be analysed and compares detection limits for plasma emission with those for ICP-MS and atomic absorption. Rocks, soils, waters and biological tissue are typical of samples to which the method may be applied. In geochemistry, and in quality control of potable waters and pollution studies in general, the multi-element capability and wide (105) dynamic range of the method are of great value. Plasma emission spectrometry is well established as a routine method of analysis in these areas. 

Flame emission spectrometry is used extensively for the determination of trace metals in solution and in particular the alkali and alkaline earth metals. The most notable applications are the determinations of Na, K, Ca and Mg in body fluids and other biological samples for clinical diagnosis. Simple filter instruments generally provide adequate resolution for this type of analysis. The same elements, together with B, Fe, Cu and Mn, are important constituents of soils and fertilizers and the technique is therefore also useful for the analysis of agricultural materials. Although many other trace metals can be determined in a variety of matrices, there has been a preference for the use of atomic absorption spectrometry because variations in flame temperature are much less critical and spectral interference is negligible. Detection limits for flame emission techniques are comparable to those for atomic absorption, i.e. from < 0.01 to 10 ppm (Table 8.6). Flame emission spectrometry complements atomic absorption spectrometry because it operates most effectively for elements which are easily ionized, whilst atomic absorption methods demand a minimum of ionization (Table 8.7). 

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