Extraction Procedures - Soils

Operationally, it is common to define HS in terms of the methods used to extract or isolate them from soils, sediments, and natural waters. The classic soil extraction procedure yields three main fractions humic acid [also defined as high-molecular-weight (HMW) or high-molecular-size (HMS) fraction], fulvic acid (FA) [also defined as low-molecular-weight (LMW) or low-molecular-size (LMS) fraction], and humin. These fractions are defined in terms of their solubility in aqueous media as a function of pH or in terms of their extractability from soils or sediments as a function of the pH of the extracting medium. Humic acid is the fraction of HS that is not soluble in water under acidic conditions, but becomes soluble (or extractable) at higher pH values. Fulvic acid is the fraction that is soluble in aqueous media at all pH values. Humin represents the fraction that is not soluble in an aqueous medium (or is not extractable with an aqueous medium) at any pH value. Actually, humin consists of an aggregate of humic and nonhumic materials (Rice and Mac-... 

Sunahara GI et al., Ecotoxicological characterization of energetic substances using a soil extraction procedure, Ecotoxicol. Environ. Saf, 43, 138, 1999. 

Cade-Menun, B.J. and Preston, C.M. (1995) A comparison of soil extraction procedures for P NMR spectroscopy. Soil Science 1 51, 770-785. 

Various soil extraction procedures utilizing a range of inorganic and organic solvents, extraction times, and soil sterilization procedures have been used to extract phenolic acids from soils (Guenzi and McCalla 1966 Turner and Rice 1975 Chou... 

The behavior of elements (toxicity, bioavailability, and distribution) in the environment depends strongly on their chemical forms and type of binding and cannot be reliably predicted on the basis of the total concentration. In order to assess the mobility and reactivity of heavy metal (HM) species in solid samples (soils and sediments), batch sequential extraction procedures are used. HM are fractionated into operationally defined forms under the action of selective leaching reagents. 

Using established extraction and cleanup methods, followed by GC/FPD and GC/thermionic detection, Carey et al. (1979) obtained detection limits in the ppb range and recoveries of 80-110% in soil and 70-100% in plant tissue. Good sensitivity and recovery were maintained in a simplified extraction procedure of sediments followed by GC/FPD analysis (Belisle and Swineford 1988). Bound methyl parathion residues that were not extracted with the usual methods were extracted using supercritical methanol by Capriel et al. (1986). They were able to remove 38% of the methyl parathion residues bound to soil, but 34% remained unextractable, and 28% could not be accounted for. 

Quevauviller Ph, Herzig R. and Muntau H (1996b) Certified reference material of lichen (CRM 482) for the quality control of trace element biomonitoring. Sci Total Environ 187 143-152 Quevauviller Ph, Lachica M., Barahona E, Rauret G, Ure A, Gomez A, and Muntau H (1997) The certification of the EDTA-extractable contents (mass fractions) of Cd, Cr, Ni, Pb, and Zn and of the DTPA-extractable contents (mass fractions) of Cd and Ni in calcareous soil by the extraction procedures given CRM 600. EUR Report 17555 Quevauviller Ph. Maier EA, and Griepink B, eds. (1995) Quality Assurance for Environmental Analysis. Elsevier. Amsterdam. 

Erp P van, Houba V and Beusichem M van (1998) One Hrmdredth Molar Caldum Chloride Extraction Procedure Part i. Commun Soil Sci Plant Anal 29 1603-1623. 

Specifically for triazines in water, multi-residue methods incorporating SPE and LC/MS/MS will soon be available that are capable of measuring numerous parent compounds and all their relevant degradates (including the hydroxytriazines) in one analysis. Continued increases in liquid chromatography/atmospheric pressure ionization tandem mass spectrometry (LC/API-MS/MS) sensitivity will lead to methods requiring no aqueous sample preparation at all, and portions of water samples will be injected directly into the LC column. The use of SPE and GC or LC coupled with MS and MS/MS systems will also be applied routinely to the analysis of more complex sample matrices such as soil and crop and animal tissues. However, the analyte(s) must first be removed from the sample matrix, and additional research is needed to develop more efficient extraction procedures. Increased selectivity during extraction also simplifies the sample purification requirements prior to injection. Certainly, miniaturization of all aspects of the analysis (sample extraction, purification, and instrumentation) will continue, and some of this may involve SEE, subcritical and microwave extraction, sonication, others or even combinations of these techniques for the initial isolation of the analyte(s) from the bulk of the sample matrix. 

The recovery is low on extracting n from soil by refluxing with water containing methanol. Metabolite n in soil can be extracted by sonication with alkaline methanol. Using this alkaline extraction procedure, another metabolite, 2-chlorobenzylsulfonic acid, is also extracted simultaneously. ... 

An efficient and reproducible extraction procedure is mandatory when analyzing agrochemicals in soil. An overview of common soil extraction techniques is given below. 

Some agrochemicals bind strongly to the soil component as bound residues, which cannot be extracted without vigorous extraction procedures. In this case, an acidic (e.g., hydrochloric acid, sulfuric acid) or alkaline solution (e.g., sodium hydroxide, potassium hydroxide) can be used as an extraction solvent, and also heating may be effective in improving the extraction of the residues. Analytical procedures after the extraction are the same as above, but a filtration procedure may be troublesome in some of these situations. However, these procedures are rare exceptions or are needed for specific chemicals that are stable under such harsh extraction conditions. 

The risk assessment has also concluded that a level of 200 mg/kg for lead in the soil will be a protective level for expected site exposures along with an excess cancer risk level for TCE-contaminated soil (56 pg/L). Based on investigations of activities at the site, the TCE-contaminated soil has not been determined to be a listed RCRA hazardous waste, as the cleaning solution records indicate the solution contained less than 10% TCE. However, the lead-contaminated soil is an RCRA hazardous waste by characteristic in this instance due to extraction procedure (EP) toxicity. None of the waste is believed to have been disposed at the site after November 19, 1980 (the effective date for most of the RCRA treatment, storage, and disposal requirements). 

Ahnstrom and Parker (2001) studied Cd reactivity in metal-contaminated soils using a coupled stable isotope dilution-sequential extraction procedure. They found that in uncontaminated arid soil and in... 

Woolson et al. (1971) used a modified soil P procedure to study distribution of As in U.S. soils. The mass of the residual As in both uncontaminated and soils contaminated with arsenic pesticides from Washington and Oregon is found as the Fe oxide bound As (0.1 N NaOH extractable), followed by the Al oxide and the Ca bound As (extracted by NH4F and H2S04, respectively). 

Ahnstrom Z.A.S., Parker D.R. Cadmium Reactivity in Metal-Contaminated Soils Using a Coupled Stable Isotope Dilution-Sequential Extraction Procedure. Environ Sci... 

Ho M.D., Evans G.J. Operational speciation of cadmium, copper, lead and zinc in the NIST standard reference materials 2710 and 2711 (Montana soil) by the BCR sequential extraction procedure and flame atomic absorption spectrometry. Anal Commun 1997 34 353-364. 

Wenzel W.W., Kirchbaumer N., Prohaska T., Stingeder G., Lombi E., Adriano D.C. Arsenic fractionation in soils using an improved sequential extraction procedure. Anal Chimica Acta 2001 436 309-323. 

In this study, 30 soil samples from rice farmland in Zhejiang province, in eastern China. We sampled the cultivation layer soils during rice harvest season. The soils are acidified and the average value of pH is 5.82. A sequential extraction procedure... 

Salts, in addition to causing the soil to be basic, can have deleterious effects on analytical procedures. For example, significant error can occur if a potassium-selective electrode is used to determine potassium in a high-sodium soil (see Chapter 9). As discussed in Chapter 14, other salts could cause inaccurate results when atomic absorption analysis of a soil extract is carried out. 

Because different components are held to soil by different types of bonding and attractions, the interaction can be relatively strong or weak. Thus, extraction procedures must be capable of extracting the desired component when it is held by different forms of bonding to different soils. 

Many researchers have attempted to unravel the mystery of the structure of humus. One approach has been to isolate fractions by extracting humus using various extraction procedures. These procedures result in the isolation of three or more fractions humic acid, fulvic acid, and humin. Humic material is isolated from soil by treating it with alkali. The insoluble material remaining after this treatment is called humin. The alkali solution is acidified to a pH of 1.0 and the precipitate is called humic acid, while the soluble... 

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