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1.
A field study was undertaken to compare dissolved organic carbon (DOC) concentrations in soil solutions obtained with three different sampling methods over a range of soil types. The sampling devices used were a tension‐free collector, a tension Prenart collector and a tension Rhizon collector. Samples were collected fortnightly for a year at seven sites in northern England, each collection being replicated three times. The soil solution DOC ranged from 1.3 g m?3 in an acid ranker to 34.7 g m?3 in a peat. The DOC concentrations obtained with the three methods correlated reasonably well (r2 = 0.6–0.8) but with an indication of bias, as the best fit line differed from the 1:1 line. The tension‐free collector gave generally higher DOC concentrations except at very low concentrations (in the acid ranker soil). The DOC concentrations measured with the tension‐free collectors were significantly (P < 0.05) higher than those obtained with Prenart and Rhizon collectors at four and six sites, out of seven, respectively. Subsequent laboratory tests on tension‐free collected samples showed no DOC loss on filtration through 0.1 and 0.22‐μm membranes, whereas a significant loss of DOC occurred when tension‐free collected samples were subsequently passed through Prenart and Rhizon collectors, indicating a probable sampling artefact with the tension devices. The difficulties of acquiring representative soil solution samples are discussed, together with the advantages and disadvantages of tension and tension‐free methods.  相似文献   

2.
A sensitive enzyme immunoassay (EIA) based on polyclonal antibodies from sheep was used to screen for atrazine in electro-ultrafiltration (EUF) soil extracts without clean-up. Matrix effects were circumvented by diluting the aqueous EUF extracts. The EUF proved to be a convenient method for the extraction of atrazine residues in soil. The efficiency of EUF appeared to be equivalent to that of organic extraction methods except on weathered residues, which generally resulted in lower yields. Both the combined gas chromatography/automated Soxhlet (GC/Soxtec) and the immunochemical technique EIA/EUF yielded similar data for the 26 soil samples identified as positive (> 0.02 mg/kg) during the first screening of 479 EUF extracts by the EIA.  相似文献   

3.
Acid phosphomonoesterase (APM) (E.C. 3.1.3.2) in soil is either of plant‐root or microbial origin. Each of these sources may be dominant in certain ecosystems. Generally, extracellular APM in soil has been reported. However, the lack of suitable methods limits investigations of APM in soil. Root‐derived APM comes from intact plant roots, root exudates, root apoplastic sap, root extracts, or mycorrhizal fungi. The significance of these sources of APM is discussed in this review being the highest in intact roots or root extracts, and within wall‐ and membrane‐bound fraction of mycorrhizal fungi. Evaluation of the location of APM has been based on extraction of fractions of APM with different types of extractants. The suitability of individual extractants and lack of these procedures as well as the need to search for other suitable solutions to increase extraction efficiency, minimalize extraction of inhibitors and solubilization of organic compounds are discussed. As APM derived from roots and soil microorganisms show different kinetic properties, and differ in their response to environmental factors, determination of the significance of root and microbial APM within ecosystems requires further research aimed at evaluating the response of P transformation to climatic and other environmental changes.  相似文献   

4.
Different procedures to investigate dissolved trace element concentration at the transition from unsaturated to saturated zone in soils were compared by concurrent sampling of soil solution and solid soil material in this zone. The in situ sampled soil solution from the percolated water was used to measure in situ concentrations, while solid soil material was used to measure concentrations at two liquid–solid ratios using batch experiments on 250 sample pairs. The liquid–solid ratios were 2 L kg–1 and 5 L kg–1. At 5 L kg–1, the ionic strength was adjusted with Ca(NO3)2 to a sample‐specific value similar to in situ, while at 2 L kg–1, the ionic strength was not adjusted. The extracted concentrations of most trace elements exhibited a statistically significant but weak correlation (p value < 0.01) to the corresponding in situ concentrations. In the liquid–solid ratio of 2 L kg–1 extracts, Pb and Cr showed very poor comparability with the in situ equivalent. A likely cause was the enhanced dissolved‐organic‐C release in the extract due to the lower ionic strength compared to in situ conditions in combination with effects from drying and moistening soil samples. For the other elements, correlation increased in the order As < Cu, Zn, Sb, Mo, V < Cd, Ni, Co where adjustment of the ionic strength led to slightly better results. In addition to the element‐specific shortcomings, it appeared that low concentration levels of in situ concentrations were generally underestimated by batch extraction methods. The liquid–solid ratio of 2 L kg–1 extracts could only be used as a method to predict exceedance of thresholds if a safety margin of approximately one order of magnitude higher than the thresholds was adopted. The ability of the batch‐extraction methods to estimate in situ concentrations was equally limited.  相似文献   

5.
Abstract

We measured the concentration and composition (sensu Leenheer, 1981) of dissolved organic carbon (DOC) in lysimeter solutions from the forest floor of a spruce stand in Maine and in laboratory extracts of organic (Oa horizon) and mineral soils collected from various forests in Maine, New Hampshire, and Vermont. All soils were acid Spodosols developed from glacial till. The effects of different storage, extraction and filtration methods were compared. Extracts from Oa horizons stored fresh at 3°C contained a larger fraction of hydrophobic neutrals than lysimeter forest floor solutions (31 and 4% of DOC in stored and lysimeter solutions, respectively), whereas extracts from Oa horizons which had been extracted, incubated at 10–15°C, and extracted again had DOC compositions similar to that in lysimeter solutions. Mechanical vacuum and batch extractions of Oa horizons yielded DOC similar in concentration and composition if the extracts were filtered through glass fiber filters. Nylon membrane filters, however, removed more hydrophobic acids from batch extracts. Dissolved organic carbon extracted from frozen, air‐dry, and oven‐dry Oa and Bh horizons was relatively rich in hydrophilic bases and neutrals and was similar to that released after chloroform fumigation, indicating that common soil‐storage methods disrupt microbial biomass.  相似文献   

6.
Abstract

Two digestion procedures, employing aqua regia‐HF (ARHF) and HNO3‐HCIO4‐HF (HHH), were used to analyze residual metals (following a chemical fractionation scheme) and total metal content of two soils, one moderately polluted by municipal sludge applications and the other a grossly‐contaminated sample (20.8% Pb) from a battery recycling site. Although commonly used in sequential extraction analyses, the ARHF method solubilized only 53% (significant at p = 0.05) of the HHH‐determined residual Pb in the battery soil. For the sludge‐amended soil, residual Cd, Pb, and Zn were not statistically different by the two methods. For the battery soil, a single ARHF extraction also underestimated total Pb and Cu relative to HHH, but both methods gave statistically‐similar total Cd, Cu, Pb, and Zn for the sludge‐amended soil. As the sample metal concentration increased, the ability of ARHF to solubilize HHH‐equivalent metal quantities generally decreased. Since the degree of contamination is often unknown for environmental samples, the HHH method is more reliable for assessing residual and total metals in polluted soils  相似文献   

7.
There is growing concern about the fate and toxicity of herbicides to non‐target receptors and an increasing need to measure these analytes sensitively. The responses of cellular and immunological biosensors to four commonly used herbicides (atrazine, diuron, mecoprop and paraquat) were investigated. In combination, these sensors assess toxicity and quantify concentrations of herbicides present in extracts from soil. The bioluminescence response of the lux‐marked bacterial biosensor Escherichia coli HB101 was determined in aqueous extracts from soil to indicate toxicity. Smaller concentrations caused a toxic response for all four herbicides recovered from the Insch series than for those recovered from spiked water samples, but this was not a result of biodegradation of herbicides in the soil. This suggests that intrinsic soil factors may be altering the bioavailable fraction of herbicides, making them more toxic than equivalent concentrations in water. Herbicide concentrations were determined using immunological biosensors consisting of stabilized recombinant single chain antibodies (stAbs) specific for the four different groups of herbicides. These stAb fragments retain functionality in organic solvents such as methanol commonly used in soil extraction. Anti‐atrazine, mecoprop, diuron and paraquat stAbs were successfully used to identify and quantify herbicides present in aqueous and methanol extracts from soil. The amounts recovered from immunoassay analysis were compared with chemical analysis using high performance liquid chromatography, and the two methods correlated. These stAb fragments might provide a more rapid and sensitive means of quantifying trace amounts of herbicides and their metabolites in aqueous and methanol extracts from soil.  相似文献   

8.
Soil water repellency is usually unstable, as exemplified by the common method of quantifying repellency degree – the water drop penetration time (WDPT) test. Dynamic penetration and infiltration of water into repellent soils is generally attributed to either reduction of the solid‐liquid interfacial energy (γSL) or reduction of the liquid‐vapour interfacial energy (γLV), or both. The reduction of γSL can result from conformation changes, hydration, or rearrangement of organic molecules coating soil particle surfaces as a result of contact with water, while the reduction of γLV can result from dissolution of soil‐borne surface active organic compounds into the water drop. The purpose of this study was to explicitly test the role of the second mechanism in dynamic wetting processes in unstably repellent soils, by examining the drop penetration time (DPT) of water extracts from repellent soils obtained after varying extraction times and at different soil : water ratios. It was indeed found that soil extracts had lower surface tensions (γLV approx. 51–54 mN m−1) than distilled water. However, DPT of the soil extracts in water repellent soils was generally the same or greater than that of water. Salt solutions with the same electrical conductivity and monovalent/divalent cation ratio as the soil extracts, but lacking surface active organic substances, had the same DPT as did the extracts. In contrast, DPT of ethanol solutions prepared with the same γLV, electrical conductivity, and monovalent/divalent cation ratio as the soil extracts, was much faster. Ethanol solutions are usually used as an agent to reduce γLV and as such, to reduce DPT. It is concluded that the surface‐active, soil‐derived organic substances in aqueous soil extracts do not contribute to wetting dynamics, and as such, this mechanism for explaining kinetics of water penetration into water repellent soils is rejected. It is also concluded that the rapid penetration of ethanol solutions must be due not only to changes in γLV, but to also to changes in either or both γSL and the solid‐vapour interfacial energy (γSV). These results stand in sharp contrast to well‐accepted logical paradigms.  相似文献   

9.
Compositions of soil solution obtained by the following methods were compared with those obtained by lysimetry: centrifugation; 2:1 extracts of air dried (2:1dried) and field moist (2:1moist) samples; saturation extracts; the ‘equilibrium soil pore solution’︁ method using columns with undisturbed (ESPS) and composited soil (ESPScomp); and a method using pressure. Two soil depths of a Spodic Dystric Cambisol at Solling, Germany, were sampled with 10 to 12 replications. A coupled equilibrium model was used to describe the effect of soil to solution ratio on the solution composition. The model included multiple cation exchange and inorganic complexation, and for the subsoil solubility products of AlOHSO4 and Al(OH)3. Saturation extracts gave similar results as lysimetry and thus may be useful for calculating output fluxes. However, biological transformations (N mineralisation, solubilisation of organic matter) occurred during the preparation of saturation extracts. Composition of soil solutions obtained by either 2:1dried extracts or centrifugation differed greatly from the results of other methods, indicating that these two methods may not be the best means to investigate equilibrium soil solutions. The values of molar ion ratios depended largely on the method used to obtain soil solutions: Ca2+/Al3+ ratios for each depth ranged from less than 0.3 (which suggests that liming is required urgently) to greater than 1 (liming not necessary). Modelling described the effect of soil to solution ratio on element concentrations for the methods pressure, saturation extracts, ESPScomp and 2:1moist extracts qualitatively with a few exceptions. The model suggested that differences in element concentrations using these methods may be mainly due to dilution, cation exchange and solubilisation of sparingly soluble salts, depending on the soil to solution ratio used.  相似文献   

10.
A high‐performance size‐exclusion chromatography system (HPSEC) was set up with detection based on the specific binding of Calcofluor to β‐glucan for determination of amount and molecular weight of β‐glucan in different cereal extracts. To calibrate the HPSEC system, a purified β‐glucan was fractionated into narrow molecular weight ranges and the average molecular weight was determined before analysis on the HPSEC system. The detector response was similar for β‐glucans from oats and barley and appeared to be independent of molecular weight. Four different methods for extraction of β‐glucan from different cereal products were tested: two alkaline, one with hot water and added α‐amylase, and one with water and added xylanase. Inactivation of endogenous β‐glucanase was crucial for the stability of the extracts, even when extracting at high temperature or pH. Yields varied widely between the different extraction methods but average molecular weight and molecular weight distribution were similar. Extraction with sodium hydroxide generally gave a higher yield and molecular weight of β‐glucan in the extracts.  相似文献   

11.
The characteristics of dissolved organic matter (DOM) in soils are often determined through laboratory experiments. Many different protocols can be used to extract organic matter from soil. In this study, we used five air‐dried soils to compare three extraction methods for water‐extractable organic matter (WEOM) as follows: (i) pressurised hot‐water‐extractable organic carbon (PH‐WEOC), a percolation at high pressure and temperature; (ii) water‐extractable organic carbon (WEOC), a 1‐hour end‐over shaking; and (iii) leaching‐extractable organic carbon (LEOC), a leaching of soil columns at ambient conditions. We quantified the extraction yield of organic carbon; the quality of WEOM was characterized by UV absorbance, potential biodegradability (48‐day incubation) and parallel factor analysis (PARAFAC) modelling of fluorescence excitation emission matrices (FEEMs). Biodegradation of dissolved organic carbon (DOC) was described by two pools of organic C. The proportions of labile and stable DOC pools differed only slightly between the WEOC and LEOC methods, while PH‐WEOC contains more stable DOC. The mineralization rate constants of both labile and stable DOC pools were similar for the three methods. The FEEMs were decomposed into three components: two humic‐like fluorophores and a tryptophan‐like fluorophore. The effect of extraction method was poorly discriminant and the most similar procedures were PH‐WEOC and LEOC while WEOC extracts were depleted in humic‐like fluorophores. This study demonstrates that WEOM quality is primarily determined by soil characteristics and that the extraction method has a smaller, but still significant, impact on WEOM quality. Furthermore, we observed considerable interaction between extraction procedure and soil type, showing that method‐induced differences in WEOM quality vary with soil characteristics.  相似文献   

12.
Abstract

The applicability of 0.01 M CaCl2 solution as a single extraction agent for soils as a basis for fertilizer recommendation was tested on a variety of soils both from the Netherlands and from some tropical countries. Air‐dry soil samples were subjected to extraction with 0.01 M CaCl2 and to several conventional extraction procedures, and the results were compared. In the soil suspensions pH was measured, whereas in the extracts Na, K, Mg, P, different extractable N‐forms and Zn were measured. The values found in CaCl2 extracts are discussed in relation to results of other extraction procedures and as to their potential value in soil quality assessment. It is concluded that a single extraction procedure with 0.01 M CaCl2 can be applied for fertilizer recommendation purposes. The possibility of determining different extractable N‐forms (NH4, NO3, soluble organic N) significantly enhances the value of the method in predicting the N‐fertilizer needs. Furthermore it was found that the concentration of Zn in 0.01 M CaCl2 extracts was a good indicator of phytotoxicity in a polluted area. Additional advantages of this extraction are low costs, simplicity and repro‐ducibility.  相似文献   

13.
Abstract

Measurement of total soil cadmium (Cd) is difficult due to calcium (Ca) and other chemicals which cause high background absorbance when trace levels of Cd are to be determined. When soil Cd is low, even use of deuterium background correction with flame atomic absorption spectroscopy (AAS) cannot provide accurate Cd results. Use of furnace atomic absorption with method of standard additions can circumvent these interferences, but the cost and time required are substantial. We desired a more rapid, convenient, and reliable alternative to extraction using dithizone and back‐extraction into acid, or to ammonium pyrollidinedithiocarbamate (APDC) which does not require close pH adjustment nor have many sources of potantial contamination. We evaluated analysis of these complex soil extracts with the method of Viets (1978) which extracts metals from 1N acid solutions using Aliquat‐336 in methylisobutyl‐ketone (MIBK). We tested the use of the less toxic and less water soluble 3‐heptanone as an organic solvent alternative to MIBK which can be directly analyzed by flame atomic absorption. A series of extraction experiments were conducted to determine if Cd was extracted from standard solutions and from total metal digests of calcareous soils into an Aliquat‐336/3‐heptanone solution, and under what conditions extraction was optimum. In the optimum method, Cd was extracted from aqua regia soil digests by 10% Aliquat‐336 in 3‐heptanone without addition of ascorbic acid or potassium iodide (KI) used by Viets. Excellent recovery of Cd was obtained for both standard reference soils and low Cd highly calcareous soils from North Dakota and Minnesota. Addition of ascorbic acid and KI did not increase the efficiency of extraction indicating that the extraction system used was free of ferric‐iron [Fe(III)] interference. The ion‐association complex of Cd remained stable for at least 24 hr after extraction, providing a very convenient method to analyze low levels of total Cd in soils and other geologic materials.  相似文献   

14.
Abstract

Turbidimetric methods, using Ba ions to precipitate SO4, are frequently used to determine soil sulfates extracted with phosphate solutions. These methods, as routinely performed, seriously underestimate SO4 in some soils of the tropics because phosphate is removed from the extractant by soil adsorption and because many extracts fail to yield satisfactory precipitate even if the extracting procedure is adequate. Decolorizing the extracts with carbon black, treating extracts with strong oxidizing agents, adding SO4 spikes, and seeding the extracts with BaCl2 seed‐crystals improve precision, but some extracts, especially those from soils derived from volcanic ash, do not yield reliable precipitates even though these procedures are employed. This paper presents a method that consistanlty yielded more SO4 than other turbidimetric procedures with which it was compared. The proposed method was further validated against an ion‐chromatographic method for SO4 determination. The two methods yielded virtually identical results.

The proposed method consists of extracting SO4 with 0.04 M Ca(H2PO4)2 pH 4, at a soil‐to‐solution ratio of 1: 10. Repeated extraction is necessary for phosphate‐retentive soils. (A. single extraction was approximately 40% effective for removing indigenous SO4 from a Hydric Dystrandept subsoil, approximately 78% effective for an Eutrustox.) Organic materials are removed from the extracts by adsorption on charcoal; SO4 is concentrated in the extract by volume reduction; a SO4 spike is added; BaCl2‐seed crystal is added, after which volume is increased by adding BaCl2 solution. Optical density is read at 600 nm.  相似文献   

15.
Abstract

A method is presented for estimating the sodium adsorption ratio (SAR) of the saturated soil‐paste extract from three electrode measurements made directly in the saturated soil‐paste. An analogous method is presented for the determination of the SAR of extracts and solutions solely from electrode measurements made in the extract or solution. Both methods are carried out without the use of pH and ionic strength buffers. The methods were tested on a widespread range of salt‐affected soils and their extracts; they are deemed suitable for field applications in the diagnosis, screening, and classification of sodic soils and waters.  相似文献   

16.
Abstract

In order to better understand some of the factors likely to affect measurements of KC1 extractable acidity, experiments were conducted using synthetic solutions and extracts from a wide range of contrasting soils. The reagents used for measuring exchangeable acidity (i.e., KC1 and KF) were also examined to evaluate the effects of chemical impurities on acidity measurements. Two commonly used titrimetric methods were adapted and tested to determine the accuracy and precision of acidity measurements. The exchangeable acidity of soil extracts was investigated by extraction methods, extractant concentration, and extractant volume. Results from the soil extract experiments indicated that continuous shaking has no significant effect on acidity measurements. Filtration, however, is critical, especially for acidic organic‐rich soils, since aluminum (Al) ions can be lost during centrifugation. Extractant concentration and volume had variable effects on the acidity measurements for individual soils. In general, the modified Yuan's method is preferable to the modified Thomas’ method for estimating exchangeable Al. To ensure successful determination of exchangeable acidity, we recommend using a wider KCl:soil ratio (>15:1, v/w) for organic soils with low base saturation and allophanic Andisols. In sum, potassium chloride and potassium fluoride extraction for estimating exchangeable acidity is applicable for most soils.  相似文献   

17.
Abstract

Rapid, methanol‐extraction techniques for fluometuron (N, N‐dimethyl‐N'‐[3‐(trifluoromethyl) phenyl] urea) and norflurazon (4‐chloro‐5‐(methylamino)‐2‐(3‐(trifluoromethyl)phenyl)‐3(2(H)‐pyridazinone) from fortified soils have been reported to attain >90% recoveries. Analytical methods involving chromatographic separation coupled with fluorescence detection have also been described. The objectives of this study were to describe an analytical method for the simultaneous detection of fluometuron and norflurazon using ultraviolet spectro‐scopy in soil leachates and extracts and to examine the influence of residence time on herbicide recovery from fortified soil. The analytical method requires a gradient HPLC system, a reverse‐phase C‐18 column, and ultraviolet spectroscopy at a wavelength of 240 nm. The method is characterized by high reproducibility (spike recovery and diluted sample results are generally within 10% of the expected herbicide concentrations), low limits of detection (less than 1 (μg/L in soil leachates and 20 μg/L in soil extracts, depending on organic carbon content), and an applicable concentration range of more than two orders of magnitude. The recovery of fluometuron and norflurazon from fortified soils was significantly influenced by equilibration time, loading rate, and soil type (assuming zero chemical degradation). Most significantly, as herbicide contact time with the soil increased, recovery decreased. Thus, herbicide recoveries determined in the laboratory may not provide a true measure of herbicide recoveries from field soils.  相似文献   

18.
Abstract

The determination and speciation of aluminium in soil solutions and extracts by ion chromatography with post‐column reaction and fluorescence detection is described. The fluorogenic post‐column reagent consists of 4 x 10‐3 M 8‐hydroxyquinoline‐5‐sulfonic acid and 2 x 10‐3 M cetyltrimethylammonium bromide in a 1 M acetate buffer at pH 4.4. The method is applicable to soil solutions and extracts and is more sensitive than existing colorimetric methods. Aluminium species could be detected at concentrations of 35 nM. Nine metals were checked for interference; only Zn2+ and Cd2+ were found to give responses, which were however well separated from the Al3+ peak.  相似文献   

19.
The aim of this paper was to compare the concentration of P in soil extracts prepared with water and a ‘soil solution proxy’ (‘SSP’, that is, a salt solution similar in ionic composition and strength to the actual soil solution) with that in 0.01 m CaCl2 extracts, which is usually taken as a measure of soil P intensity. Seventy widely ranging agricultural soils from the Mediterranean part of Spain were used. Soil/solution ratio was 1:10 and extraction time 3 days. For 0.01 m CaCl2, a short extraction time of 30 min was also used as the reference method. CaCl2‐P(3 days) and CaCl2‐P(30 min) were not significantly different for the 40 noncalcareous soils group, but CaCl2‐P(3 days) was significantly larger than CaCl2‐P(30 min) for the 30 calcareous soils group. The Water‐P/CaCl2‐P(30 min) ratio was not significantly related to any soil property, its mean being 6.3 for the noncalcareous and 5.8 for the calcareous soils group. The mean SSP‐P/CaCl2‐P(30 min) ratio was 2.6 for the noncalcareous and 3.1 for the calcareous soils group, and decreased slightly with increasing ionic strength of the soil solution in the noncalcareous soils group. These results are consistent with the promoting influence of the Ca ion and ionic strength on P adsorption by permanent‐charge soils. The fact that extraction with 0.01 m CaCl2 generally results in underestimation of the actual concentration of P in the soil solution should be considered when CaCl2‐P is used as a soil P test.  相似文献   

20.
The electrical conductivity at 25°C (EC25) of soil solutions or irrigation waters is the standard property for assessing salinity. Many models for soil salinity prediction calculate the major ion composition of the soil solution. The electrical conductivity of a solution can be determined from its composition through several different empirical equations. An assessment of these equations is necessary to incorporate the most accurate and precise equations in such models. Twelve different equations for the EC25 calculation were calibrated by means of regression analyses with data from 133 saturation extracts and another 135 1:5 soil‐to‐water extracts from a salt‐affected agricultural irrigated area. The equations with better calibration parameters were tested with another data set of 153 soil solutions covering a wide range of salt concentrations and compositions. The testing was conducted using the standardized difference t‐test, which is a rigorous validation test used in this study for the first time. The equations based on the ionic conductivity decrement given by Kohlrausch's law presented the poorest calibration parameters. The equations founded on the hypothesis that EC25 is proportional to analytical concentrations had worse calibration and validation parameters than their counterparts based on free‐ion concentrations and ionic activities. The equations founded on simpler mathematical relationships generally gave improved validation parameters. The three equations based on the specific electrical conductivity definition presented a mean standardized difference between observations and predictions indistinguishable from zero at the 95% confidence level. The inclusion of the charged ion‐pair concentrations in the equation based on free‐ion concentrations improved its predictions, particularly at large electrical conductivities. This equation can be reliably used in conjunction with chemical speciation software to assess EC25 from the ion composition of soil solutions.  相似文献   

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