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1.
The adsorption of herbicides on soil colloids is a major factor determining their mobility, persistence, and activity in soils. Solvent extraction could be a viable option for removing sorbed contaminants in soils. This study evaluated the extractability of three herbicides: 2,4 dichlorophenoxy-acetic acid (2,4-D), 4-chloro-2-methylphenoxypropanoic acid (mecoprop acid or MCPP), and 3,6-dichloro-2-methoxybenzoic acid (dicamba). Three solvents (water, methanol, and iso-propanol) and three methods of extraction (column, batch, and soxhlet) were compared for their efficiencies in removing the herbicides from three soils (loamy sand, silt loam, and silty clay). Both linear and non-linear Freundlich isotherms were used to predict sorption intensity of herbicides on soils subjected to various extraction methods and conditions. High Kdand Kfr, and low N values were obtained for all herbicides in silty clay soil by batch extraction. Methanol was the best solvent removing approximately 97% of all added herbicides from the loamy sand either by column or soxhlet extraction method. Isopropanol ranked second by removing over 90% of all herbicides by soxhelet extraction from all three soils. However, water was ineffective in removing herbicides from any of the soils using any of the three extracting procedures used in this study. In general, the extent of herbicide removal depended on soil type, herbicide concentration, extraction procedure, solvent type and amount, and extraction time. 相似文献
2.
Extraction using ethylenediaminetetraacetic acid (EDTA), and other chelates has been demonstrated to be an effective method of removal of Pb from many contaminated soils. However, column leaching of Pb from alkaline soils with EDTA has been problematic due to extremely low soil permeability. The first purpose of this study was to develop batch extraction procedures and methods of analysis of batch extraction data to provide Pb solubility information which can be used to model the column extraction of Pb from soils. The second purpose was to determine the effect of the addition of KOH and CaCl2 to K2H2EDTA extract solution on both hydraulic conductivity and Pb removal. A Pb-contaminated soil sample was collected from an abandoned battery recycling facility. Both batch shaker extractions and column leaching experiments were completed using 5 different EDTA extract solutions. When only CaCl2 was added to EDTA no change in the amount of Pb removed by batch extraction was observed. As expected, lead solubility was observed to decrease as pH was increased by the addition of KOH. However, Pb solubility was only slightly decreased by the addition of both CaCl2 and KOH. The amount of time required to leach 6.0 L of extraction solution through the soil columns varied from 2 to 33 days. The addition of CaCl2 and/or KOH resulted in increased soil hydraulic conductivity relative to the EDTA-only solution. The hydraulic conductivity was related to residual calcium carbonate content, suggesting that dissolution of CaCO3 and subsequent production of CO2 gas in the soil pores was partially responsible for the observed reductions in soil permeability. However, Pb removal was diminished with the addition of CaCl2 and KOH because of the decreased Pb solubility and also kinetic limitations associated with the shorter residence time of the extract solution in the column. 相似文献
3.
针对国内缺乏土壤中多环芳烃（PAHs）检测的国家标准方法的现状,以提取效率和回收率作为不同溶剂、不同提取方式前处理优劣的表征,研究了目前国内较常用的3种提取技术（索氏提取、超声波提取、水平振荡提取）和2种不同的提取剂（二氯甲烷、二氯甲烷／丙酮=5：1）对提取效率和回收率的影响。结果表明,以二氯甲烷作为提取溶剂,水平恒温振荡提取4h,可以有效地提取土壤中的15种多环芳烃类污染物。此技术提取时间短,节省提取溶剂且提取效率较高,方法回收率在73．3％－117．5％范围内。 相似文献
4.
咸水冰融化入渗对重盐碱地具有明显的改良作用,而咸水冰融化是融水水质和水量的动态变化过程。为模拟咸水冰融化入渗滨海盐土过程,探讨咸水灌溉改良盐碱地的可行性,本研究设置了不同咸水梯次入渗滨海盐土的土柱试验,试验处理为:咸水梯次入渗(GSI)、咸水单一入渗(DSI)和咸水冰融化入渗(MSI),以淡水入渗(CK)为对照;其中咸水矿化度和水量分别为15g·L~(–1)和314.3mm。根据咸水冰融化过程中融水水质和水量的变化过程,GSI设置了4个矿化度和水量(S1:81 g·L~(–1)和25 mm;S2:19 g·L~(–1)和125.8 mm;S3:3 g·L~(–1)和94.3 mm;S4:0 g·L~(–1)和69.2 mm)的咸水连续入渗。结果表明:相同时间内,咸水处理的入渗深度和速度均大于CK;入渗初期,GSI的入渗深度和速率均高于DSI,且上一梯次咸水的入渗能显著提高下一梯次咸水的入渗率,后期GSI处理随着入渗咸水矿化度的降低,入渗率显著低于DSI。入渗后,0～40 cm土层土壤水盐含量由大到小依次为DSIGSIMSI,GSI和MSI土壤水盐分布一致,脱盐率分别为92.87%和91.38%,显著大于DSI的74.74%。以上结果明确了不同咸水梯次入渗滨海盐土的入渗特征,咸水梯次入渗可获得与咸水冰融化入渗一致的脱盐效果,这为后续模拟咸水冰融水入渗盐碱土过程提供了手段,同时也为咸淡水轮灌技术提供了理论依据。 相似文献
5.
黄米醇溶蛋白脱色工艺研究 总被引：1，自引：0，他引：1
该文采用有机溶剂、颗粒活性炭、凝胶层析、超临界CO2流体萃取等方法,研究了黄米醇溶蛋白的脱色效果及脱色后蛋白的回收率。结果显示甲苯脱色效果好,蛋白质回收率较高,但工艺繁琐,成本高;凝胶层析费时,而且处理量有限,在生产中会受到限制;颗粒活性炭成本低,脱色效果较好,工艺简单,可大量处理样品;超临界CO2流体萃取在脱色效果和蛋白质回收率上都优于其他方法,且不需后处理即可直接得到脱色蛋白成品。因此,颗粒活性炭、超临界CO2流体萃取脱色工艺适合于不同层次的无色黄米蛋白的工业化生产。 相似文献
6.
Summary Low molecular weight fractions (LMW; <5000 daltons) of organic matter were isolated from three soils by a mild extraction procedure and gel-permeation chromatography. The peptides present in the LMW soil extracts were separated on a Whatman Partisphere C18 and a Beckman Ultrapore C8 column by reverse-phase high performance liquid chromatography (HPLC). The peptide fractions were collected, acid hydrolyzed, and analyzed for amino acid composition. The C8 bonded-phase column gave better separation of the LMW soil peptide material than the C18 column. The total quantities of amino acids released from LMW peptides by acid hydrolysis were greater than the quantities released by immobilized protease hydrolysis (Warman and Isnor 1990). Total soil N present in the form of LMW peptides in these three soils ranged from 4 to 15%. The total recovery of peptide amino acid-N showed little difference between the C18 and C8 columns for two of the soils tested. 相似文献
7.
F. Eiland 《Soil biology & biochemistry》1979,11(1):31-35
Different methods for extraction of ATP from soil were examined. The methods were compared with respect to the efficiency of extraction of ATP from soil, and the content of ATP in the extracts was measured by the luciferin-luciferase system. The following extraction procedure was found to be the most efficient:Shaking of the soil with sulphuric acid, followed by filtration, cation exchange of the extract on Na+ resin, and adjustment to pH 9.8 with ethanolamine.The method is simpler, faster and more convenient for processing large numbers of samples, than the earlier-described acid extraction methods. Furthermore, ATP levels of 5ngATPg?1 dry wt soil can be measured and results can be reproduced within ± 5%.The respiration rates of the soils were also measured, and a high degree of correlation was found between carbon dioxide production and ATP levels determined by extraction with sulphuric acid or dimethylsulfoxid. 相似文献
8.
Yoder RN Huskin MA Kennard LM Zabik JM 《Journal of agricultural and food chemistry》2000,48(9):4335-4340
Degradation of the sulfonanilide herbicide diclosulam was studied on nine soils from three countries to determine the rates and products of aerobic metabolism. Diclosulam was applied to four agricultural soils from the United States, three from Argentina, and two from Brazil at a rate of 0.1 ppm, equivalent to approximately twice the maximum field application rate of 52 g of active ingredient/ha. U.S. and Brazilian soils were incubated in the dark at 25 degrees C at 75% 0.3 bar moisture; Argentinean soils were incubated in the dark at 20 degrees C and 45% moisture holding capacity. Samples were analyzed up to one year after treatment. Two-compartment DT(50) and DT(90) values averaged 28 +/- 12 and 190 +/- 91 days, respectively. Three soil metabolites reached levels of >10% of applied in at least one soil and were identified as the 5-hydroxy analogue of diclosulam (5-OH-diclosulam), aminosulfonyl triazolopyrimidine (ASTP), and the 8-chloro-5-hydroxy analogue of diclosulam (8-Cl-diclosulam). The terminal products of diclosulam soil metabolism were mineralization to CO(2) and bound soil residues. Apparent sorption coefficients (K(d)) were determined on a subset of samples by extraction with a 0. 01 M CaCl(2) solution followed by an acidified acetone extraction. Initial sorption coefficients were similar to those obtained in a batch equilibrium study and averaged 1.1 L/kg for the six soils tested. K(d) coefficients for the metabolites, when available, tended to be slightly lower than that for diclosulam. Sorptivity of diclosulam and degradates increased with time. 相似文献
9.
The use of solid-state fermentation (SFF) of low cost substrates by fungal species to generate organic acid solutions for washing of lead from a contaminated soil was evaluated in this study. SFF filtrates were generated by fermentation of four substrates (corn cobs, apple pomace, rice and hay) with three fungal species (Aspergillus niger NRRL 2001 (A. niger 1), Aspergillus niger ATCC 64065 (A. niger 2), Aspergillus foetidus NRRL 337) at three fermentation times. The concentration and speciation of organic acids of the filtrates was found to be a function of the substrate type, the fungal species and the fermentation time. Fermentation of rice resulted in the highest concentrations of citric acid while fermentation of corn cobs, apple pomace and hay tended to generate oxalic acid with an increasing fraction of this acid as the fermentation progressed. Batch extraction tests that employed the SSF filtrates revealed that soluble lead concentrations as high as 35 mg/l could be achieved. Filtrates containing elevated concentrations of citric acid resulted in the greatest lead extraction while oxalic acid inhibited solubilization. Due to the buffering of pH that was provided by the soil in the batch tests this factor did not appear to influence lead extraction. Lead extraction was observed over an extended period of time in a column test. Lead extraction was strongly influenced by the pH of the soil column and less strongly influenced by the organic acid content of the SSF filtrate. The speciation of organic acids was substantially modified from primarily citric acid in the SSF filtrate to gluconic acid in the soil column discharge. 相似文献
10.
11.
用连续流动分析仪测定土壤微生物态氮的方法研究 总被引：9，自引：1，他引：8
本文在用连续流动分析仪 TRAACS2000测定土壤中常见十几种有机态氮化合物的基础上,对连续流动分析仪法和凯氏法测定土壤浸提液全氮和土壤微生物态氮的方法进行了比较研究。结果表明,连续流动分析仪所测标准有机态氮化合物的回收率平均为94%;连续流动分析仪测得浸提液中全氮量与凯氏定氮法所测浸提液中全氮量之间呈显著线性正相关;连续流动分析仪法测得的土壤微生物态氮与凯氏法测得的土壤微生物态氮的之间亦呈显著线性正相关,表明两种方法测得的氮来自土壤氮的同一组分,其转换系数分别为 Kn=0.48(CaCl2浸提) 或Kn=0.53(K2SO4浸提)。 相似文献
12.
Subcritical water extraction to evaluate desorption behavior of organic pesticides in soil 总被引：2，自引：0，他引：2
We evaluated the feasibility of extracting organic pesticides in soil using a hot-water percolation apparatus at 105 degrees C and 120 kPa pressure. Efficiency of the method was assessed by extracting six selected pesticides (acetochlor, atrazine, diazinon, carbendazim, imidacloprid, and isoproturon) from previously equilibrated soil at 13.6-65.8 mg/kg concentration range. Studies were performed on brown forest soil with clay alluviation (Luvisol). The method developed was compared to the traditional batch equilibrium method in terms of desorbed amount of pesticides from soil and extraction time. Pesticides in the liquid phase from the batch sorption experiment and in the effluent from the hot-water percolation were quantified by high-performance liquid chromatography with UV detection. The results of the percolation experiment are in close correlation with those of the conventional soil testing method. Desorbed quantities by hot-water percolation were 85% acetochlor, 62% atrazine, 65% carbendazim, 44% diazinon, 95% imidacloprid, and 84% isoproturon, whereas using batch equilibrium method 101, 66, 64, 37, 81, and 90% were desorbed, expressed as the percentage of the adsorbed amount of pesticide on soil following equilibration. The average time for hot-water extraction was 3.45 min, in contrast to the 16 h time consumption of the traditional batch method. The effect of temperature on stability of selected compounds was also evaluated using pesticide-spiked sand without soil. Recoveries of analytes ranged between 84.6 and 91.1% with reproducibility of 7.9-10.2%, except for diazinon, for which recovery was 59.4% with 14.4% relative standard deviation since decomposition occurred at elevated temperature. The percolation process has been described by a first-order kinetic equation. The parameters calculated from the equation provide an opportunity to estimate the amount of compound available for desorption, the rate of desorption processes in the studied soil-pesticide-water system, and modeling the leaching process to obtain additional information on the environmental behavior of the examined pesticide. 相似文献
13.
砂质土壤磷素主要以可提取态形式积累,有很高的释放潜力。该类土壤磷素的释放受土壤pH、土水作用时间和土壤溶液化学组成等的影响。土壤酸化、土壤溶液中Na+浓度的提高及土壤与水的作用时间增加可促进土壤磷素的释放。用淋洗方法和平衡提取等2种方法对土壤磷素的释放评价表明,淋洗方法测得的P量较小,可代表土壤短期内P释放强度;而平衡提取法提取的P数量较大,可代表土壤P长期释放的容量。 相似文献
14.
A method for the extraction of bentazone, dichlorprop, and MCPA in three selected Norwegian soils of different textures is described. Initially three different extraction methods were tested on one soil type. All methods gave recoveries >80% for the pesticide mixture, but extraction with sodium hydroxide in combination with solid-phase preconcentration was used for further recovery tests with soils of different properties spiked at four herbicide concentration levels (0.001-10 microg/g of wet soil). The method was rapid and easy and required a minimum of organic solvents. The recoveries were in the range of 82-109, 80-123, and 45-91% for the soils containing 1.4 (Hole), 2.5 (Kroer), and 37.8% (Froland) organic carbon, respectively. Limits of quantification using GC-MS were 0.0003 microg/g of wet soil for bentazone and 0.0001 microg/g of wet soil for both dichlorprop and MCPA. 相似文献
15.
《Communications in Soil Science and Plant Analysis》2012,43(13-14):2295-2308
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
16.
Effectiveness of a Full-Scale Constructed Wetland for the Removal of Metals from Domestic Wastewater
The mobility of fluorescein and bromide used as tracers in packed soil columns was investigated. Five different soils were used in two application methods: soil surface application and soil incorporation, both of which simulate accepted methods of soil application of termiticides to prevent structural infestation. The breakthrough of bromide and fluorescein in column eluates were measured. The absorbance of fluorescein at 492 nm was pH dependent, and proper adjustments were made after measuring the eluate pH. Although high recoveries of bromide from the soil columns were observed, the breakthrough was different among the soil types, indicating that bromide behaves differently in different soils. Recovery of fluorescein, a weak acid, varied depending upon the pH of the soil used, and was only observed in the eluates of two of the five soils tested. Soil treated with bromide and fluorescein followed by soaking extraction showed high recovery of bromide but low recovery of fluorescein, except for in the most alkaline of the soils tested. If fluorescein is used as a conservative tracer in pesticide soil mobility studies, mobility can be underestimated in acidic soils because the active ingredient might travel more quickly than does the fluorescein. 相似文献
17.
为有效测定土壤中土霉素残留量,建立了固相萃取－高效液相色谱法提取以及测定潮土、红壤、紫色土中土霉素残留量的方法。土壤中土霉素残留经提取缓冲溶液进行有效提取,经过DVB固相萃取小柱纯化、无水甲醇洗脱和氮气流浓缩后,经HPLC测定。对提取缓冲液、流动相以及流动相pH值、有机相与无机相的比例以及流速等测定条件进行优化研究。结果表明：提取液为Na2EDTA-Mcllvaine,流动相为乙腈∶0.01mol/L磷酸二氢钠（pH值2.5,V∶V=10∶90）,温度25℃,流速1.2ml/min,检测波长350nm对3种不同性质的土壤中土霉素残留量的测定最为合适。应用本方法进行土壤中土霉素残留量的测定,土霉素含量与峰面积具有良好的线性关系,相关系数（n=9）分别为红壤0.997,紫色土0.995,潮土0.987;检出限分别为红壤0.11mg/kg,紫色土0.17mg/kg,潮土0.09mg/kg;回收率(n=18)分别为红壤80.7%~128.8%,紫色土70.5%~100.0%,潮土61.5%~103.9%;相对标准偏差(RSD, n=18)分别为红壤7.1%~28.2%,紫色土11.9%~38.1%,潮土4.1%~17.0％。本方法简便、准确,适合于测定不同土壤中土霉素残留量,结果可靠。 相似文献
18.
常规方法准确测定土壤有效钾素变化可能性的探讨 总被引：1，自引：0，他引：1
土壤中的有效钾状况通常用1 mol L-1中性醋酸铵提取的速效钾或1 mol L-1硝酸煮沸法提取的缓效钾量来表征。我国农田土壤中近些年来1 mol L-1中性醋酸铵提取的速效钾量呈普遍下降趋势。但土壤中的有效钾素的实际下降值,到目前为止还没有办法通过测土的方法进行准确评估。本文通过室内培养实验,人为改变土壤有效钾量,对常规土壤有效钾测定方法反应土壤有效钾素变化的效果进行了比较和评价。并对硝酸连续提取法准确测定土壤钾素变化的可能性进行了探讨。结果表明,几种提取方式中,以2 mol L-1冷硝酸超声波连续提取10次获得的外源钾变化的回收率最高,达75%~80%。其次是1 mol L-1硝酸100℃水浴法连续提取6次,测钾变化的累计回收率可达75%。如进一步增加提取次数,可能会有限地提高测钾变化的回收率,但随提取次数的增加,提取过程的可操作性和结果的稳定性将显著下降。因而用硝酸作为提取剂,即使是在高温、超声波等方式下,也很难准确测定强固钾能力土壤中有效钾的变化。能够准确测定土壤有效钾素变化的方法必须能将土壤中易发生变化的有效态钾全部提出,并尽量不提取土壤的原生矿物态钾,寻找这一方法将是未来土壤钾素测定工作中值得关注的问题。 相似文献
19.
Goal, Scope and Background
The suitability of leaching tests for the assessment of soil water concentrations is a controversial issue. The aim of this paper is to review and critically discuss the applicability and comparability of leaching tests in the scope of groundwater risk assessment of inorganic contamination and to discuss soil water sampling methods as alternative.Main Features
First, the theoretical background of leaching tests and the main leaching controlling parameters (pH, redox, ionic strength, reaction kinetics, surface, and speciation) are discussed. Experience with common batch leaching tests (the German DEV S4 test (S4), saturation soil extraction (SSE), ammonia nitrate extraction (ANE), and pHstatic tests) are compiled and an emphasis is set on the comparability of the results of batch leaching tests. Additionally, the comparability between batch tests and column tests is discussed and comparison studies are reviewed. As a feasible alternative, soil water sampling strategies (the suction cup method and centrifugation) are outlined.Results and Conclusions
For an expedient application of leaching tests, it is crucial to identify the main release controlling parameters, which can be both site and contaminant specific. Possible controlling parameters are, for example, pH, redox conditions, specific surface area of the investigated material, liquid to solid-ratio, ionic strength, cation exchange capacity, DOC, speciation, temperature and contact time. It depends on the release process of the contaminant in the investigated material, which parameters are influencing the release predominantly. The following questions have to be answered: Is the release process availability controlled or solubility controlled and are there kinetic limitations? Suction cups are particularly useful for long-term monitoring. In contrast, centrifugation is a fast and simple method to sample soil water also at larger and heterogeneous sites. SSE or similar batch tests for coarse material are suitable if the soil water cannot be investigated directly. Contaminant concentrations of the SSE fit best to contaminant concentrations in soil water compared to other leaching tests. Concentrations measured with S4 tests are usually significantly lower than in real soil water due to the unrealistically high liquid to solid-ratio. The ANE is used for the evaluation of plant uptake. It does not represent realistic soil water concentrations. Cationic contaminants are usually significantly higher concentrated in ANE eluates. pHstatic tests provide an evaluation of the pH dependency of contaminant release and buffer capacity of the investigated material. It provides indications to release processes and often explains deviations in the results of different leaching tests. Previous practical experience and fundamental research studies show that a conversion of leaching test results, as is proposed by the (already withdrawn) DIN V 19735, is impossible. Correlations of results from different methods, regarding different kinds of materials and different sites, are not significant. This is due to different leaching processes.Recommendation
. For short-term risk assessment, soil water should be sampled and investigated directly by suction cups (for monitoring purposes) or centrifugation (for inventory purposes). If this is not possible, the SSE or analogous batch tests for coarse material with a narrow L/S ratio should be applied. A suggestion could be a modified saturation soil extraction where a soil column is saturated and the eluate is removed by suction at the bottom of the column. With this method, an unsaturated column test could follow in the same vessel. In order to assess the long-term leaching behavior, total contents of the investigated material have to be taken into account additionally. Furthermore, it is essential to understand the dominant physical and chemical release processes and to figure out the main leaching controlling parameters. Therefore, the following methods are recommended: pHstatic tests at different pH values provide an insight to leaching processes and possible future leaching scenarios. Batch tests similar to the S4 procedure with different L/S ratios are useful to find out whether the release process is solubility or availability controlled. Additionally, this method allows the determination of maximum solubility and maximum availability, respectively. Furthermore, unsaturated column tests provide an insight into leaching processes and releasable amounts even though they require great experimental effort. Other leaching tests like S4 or ANE are not suitable for the estimation of soil water concentrations. 相似文献20.
Jirina Machackova Zdena Wittlingerova Kvetoslav Vlk Jaroslav Zima Ales Linka 《Water, air, and soil pollution》2008,187(1-4):181-194
In 1997, total petroleum hydrocarbon (TPH) remediation started at a former Air Force Base, which operated from 1940 to 1991. TPH had been released to soil and groundwater at the site by military activities. The TPH was 70% jet fuel and the affected area covered 28 ha. Remediation involved a combination of technologies, including removal of volatile organic compounds using soil vapor extraction and air sparging, free product vacuum recovery and aerobic biodegradation of organics with oxygen supplied by the air sparging system, along with nutrient addition. The primary remedial method was found to be biodegradation, which has removed 93% of the contaminants from the site to date. A significant aspect of the remedial action was performance monitoring, including documentation of remediation efficiency. The goal of the research was to assess the relative accuracy of methods commonly used for monitoring in situ TPH remediation. Two such methods were selected for the research: monitoring change in soil TPH concentration (specified as non-polar extractable substances) and monitoring respiration activity in soil with a subsequent stoichiometric mass balance to estimate the mass of TPH destroyed. The study demonstrated that both of the methods provided comparable results regarding the effectiveness of in situ TPH remediation, despite the fact that their methodologies are very different. 相似文献