Headspace solid-phase microextraction with novel sol-gel permethylated-beta-cyclodextrin/hydroxyl-termination silicone oil fiber for determination of polybrominated diphenyl ethers by gas chromatography-mass spectrometry in soil

A simple, sensitive, and accurate method for determination of polybrominated diphenyl ethers (PBDEs) in soil has been developed based on headspace solid-phase microextraction (HS-SPME) followed by gas chromatography-mass spectrometry (GC-MS). Permethylated-beta-cyclodextrin/hydroxyl-termination silicone oil (PM-beta-CD/OH-TSO) fiber was first prepared by sol-gel technology and employed in SPME procedure. By exploiting the superiorities of sot-gel coating technique and the advantages of the high hydrophobic doughnut-shaped cavity of PM-beta-CD, the novel fiber showed desirable operational stability and extraction ability. After optimization on extraction conditions like water addition, extraction temperature, extraction time, salts effect, and solvents addition, the method was validated in soil samples, achieving good linearity (r>0.999), precision (R.S.D. < 10%), accuracy (recovery>78%), and detection limits (S/N =3) raging from 13.0 to 78.3 pg/g. (c) 2007 Published by Elsevier B.V.

Relationship between organic carbon concentration and potential pond bottom soil respiration

There was a positive correlation between the concentration of organic carbon and potential respiration as measured by carbon dioxide evolution (R-2 = 0.923) and oxygen consumption (R-2 = 0.986) in soil samples collected from the bottoms of drained ponds. This finding supports the frequent use of organic carbon analysis as an indicator of sediment respiration rate under optimal conditions in commercial aquaculture facilities. (c) 2005 Elsevier B.V. All rights reserved.

A solid-phase microextraction fiber coated with diglycidyloxycalix[4]arene yields very high extraction selectivity and sensitivity during the analysis of chlorobenzenes in soil

A novel fiber coated with novel sol-gel (5,11,17,23-tetra-tert-butyl-25,27-dihydroxy-26,28-diglycidyloxycalix[4]arene/hydroxy-terminated silicone oil; diglycidyloxy-C[4]/OH-TSO) was prepared for use with headspace solid-phase microextraction (HS-SPME) combined with gas chromatography (GC) and electron capture detection (ECD), which was applied in order to determine nine chlorobenzenes in soil matrices. Due to the improved fiber preparation, which increases the percentage of calixarene in the coating, the new calixarene fiber exhibits very high extraction selectivity and sensitivity to chlorine-substituted compounds. Various parameters affecting the extraction efficiency were optimized in order to maximize the sensitivity during the chlorobenzene analysis. Interferences from different soil matrices with different characteristics were investigated, and the amount extracted was strongly influenced by the matrix. Therefore, a standard addition protocol was performed on the real soil samples. The linear ranges of detection for the chlorobenzenes tested covered three orders of magnitude, and correlation coefficients > 0.9976 and relative standard deviations (RSD) < 8% were observed. The detection limits were found at sub-ng/g of soil levels, which were about an order of magnitude lower than those given by the commercial poly(dimethylsiloxane) (PDMS) coating for most of the compounds. The recoveries ranged from 64 to 109.6% for each analyte in the real kaleyard soil matrix when different concentration levels were determined over the linear range, which confirmed the reliability and feasibility of the HS-SPME/GC-ECD approach using the fiber coated with diglycidyloxy-C[4]/OH-TSO for the ultratrace analysis of chlorobenzenes in complex matrices.

Effects of afforestation on soil carbon turnover in China's subtropical region

Afforestation in China's subtropics plays an important role in sequestering CO2 from the atmosphere and in storage of soil carbon (C). Compared with natural forests, plantation forests have lower soil organic carbon (SOC) content and great potential to store more C. To better evaluate the effects of afforestation on soil C turnover, we investigated SOC and its stable C isotope (delta C-13) composition in three planted forests at Qianyanzhou Ecological Experimental Station in southern China. Litter and soil samples were collected and analyzed for total organic C, delta C-13 and total nitrogen. Similarly to the vertical distribution of SOC in natural forests, SOC concentrations decrease exponentially with depth. The land cover type (grassland) before plantation had a significant influence on the vertical distribution of SOC. The SOC delta C-13 composition of the upper soil layer of two plantation forests has been mainly affected by the grass biomass C-13 composition. Soil profiles with a change in photosynthetic pathway had a more complex C-13 isotope composition distribution. During the 20 years after plantation establishment, the soil organic matter sources influenced both the delta C-13 distribution with depth, and C replacement. The upper soil layer SOC turnover in masson pine (a mean 34% of replacement in the 10 cm after 20 years) was more than twice as fast as that of slash pine (16% of replacement) under subtropical conditions. The results demonstrate that masson pine and slash pine plantations cannot rapidly sequester SOC into long-term storage pools in subtropical China.

Distribution characteristics of (CS)-C-137 in wind-eroded soil profile and its use in estimating wind erosion modulus

Due to its inert reaction in soil system and distinctive vertical distribution in soil profile, caesium-137 (Cs-137) has been used as a tracer to assess wind erosion. In this study, 62 soil samples were collected from 4 sampling sites in Taipusi County, Inner Mongolia; Caesium-137 activities for those soil samples were measured using a gamma-ray spectrometry in Sichuan University, Chengdu. Distribution pattern of Cs-137 in vertical soil profile was different for different land use and land cover types. Caesium-137 was distributed homogeneously in plow layer of cropland, and negatively exponential in low to medium cover grassland. Distribution pattern in high covered grassland was represented by a peak at 2-4 cm soil depth followed by a negative exponential curve. Based on those findings, simplified mass balance model was chosen to estimate the rate of wind erosion for cropland, while profile distribution model was used for grassland. Estimated wind erosion rates were 7990, 4270 and 1808 Mg(.)km(-2.)a(-1) for cropland, low cover grassland and medium cover grassland, respectively. Wind erosion intensity correlated negatively with plant cover.

Adsorption Behavior of Exogenous Thorium on Soil Contaminated by Rare Earth Industries

The adsorption behavior of exogenous thorium on soil was studied to evaluate the contaminated risk on soil. The adsorption capacity, equilibrium time, distribution coefficient and desorption ability were investigated by the experiments of static adsorption. The strong adsorption ability of exogenous thorium on soil samples was observed by high adsorption ratio (> 92%) and low desorption ratio (< 5%) in equilibrium, and the biggest distribution coefficient was over 10(4). The adsorption capacity and equilibrium time were related to soil properties. According to the results of adsorption, Freundlich equation (r >= 0.916 7) and Elovich equation (R-2 >= 0. 898 0) were primely fit for describing the thermodynamics and kinetics of the adsorption of exogenous thorium on soil samples, respectively, which indicated that the adsorption was belonged to the nonlinear adsorption, and was affected by the diffusion of thorium on soil surface and in mineral interbed. Sequential extraction procedure was employed to evaluate the bound fractions of exogenous thorium adsorbed on soil samples.

Determination of free fatty acids in bryophyte plants and soil by HPLC with fluorescence detection and identification by online MS

A method for the determination of long and short chain free fatty acids (FFAs), using 1-[2-(ptoluenesulfonate)-ethyll-2-phenylimidazole-[4,5-f-9,10-phenanthrene (TSPP) as labeling reagent, has been developed. Identification of FFA derivatives was carried out by HPLC-MS with atmospheric pressure chemical ionization (APCI) in positive ion mode. Gradient elution on an Agilent Eclipse XDB-C-8 column gave good separation of the derivatives. Excellent linear responses were observed and good compositional data could be obtained from as little as 200 mg of bryophyte plants and soil samples. Facile TSPP derivatization coupled with HPLC-APCI-MS analysis allowed the development of a highly sensitive method for the quantitative analysis of trace level of FFAs from biological and natural environmental samples.

The Effects of Grain Size Distribution and Structure on Mechanical Behavior of Silt

Abstract: In order to investigate the effects of the grain size distribution and the micro-structure of soils on the mechani- cal characteristics, some static triaxial compression tests were carried out, and then the relationship of stress-strain and the strength behavior of silty sand were compared among undisturbed samples with different grain size distribution, undis- turbed and remolded samples with the same grain size distribution, and reconstituted samples (or called mixed samples) with different grain size distribution. The effects of grain size distribution and structure on the mechanic behavior of silty sands were mainly analyzed. It is shown that the obvious differences of the mechanical characteristics between undis- turbed soils and remolded soils are caused by the differences of soil structures. Although the grain size distribution are different between two soil samples, their mechanical characteristics may be close to each other, or may have obvious differences because of the effects of micro-structure.

黄土沟壑区小流域不同地形下土壤微量元素分布特征

研究了黄土沟壑区小流域塬面、坡地、梯田和沟道土壤微量元素的剖面分布特征,以揭示不同地形条件下微量元素的有效性及地球化学特性.结果表明,不同土层土壤全量微量元素的变异系数均小于15%,为小变异土壤性质,有效态和吸附态铁和锰的变异系数均高于36%,为高度变异土壤性质;有效态和吸附态锌和铜属于中到高度变异.全量铁、锰和铜以沟道土壤较高,全锌、有效态和吸附态微量元素含量以塬面土壤较高.不同形态微量元素的剖面分布趋势取决于地形条件.不同地形下成土过程及不同地形条件所对应的土地利用方式造成了全量微量元素的差异,而土壤有机质含量的差异是不同地形条件下有效态和吸附态微量元素剖面分布特征不同的主要原因.

黄土丘陵区土壤基础呼吸对草地植被恢复的响应及其影响因素

为探讨黄土丘陵区草地植被自然恢复过程中土壤微生物活性的变化特征及其影响因素,采用"时空互代"法采集宁夏云雾山自然保护区8个不同植被恢复年限的春、夏两季0～20cm和20～40cm的土样,用室内密闭静态培养—碱液吸收法测定了新鲜和风干土样的基础呼吸。结果表明:土壤基础呼吸随植被恢复年限增加呈增加趋势,土壤呼吸强度和累积呼吸量都表现为植被恢复73年和78年较高,而耕地和植被恢复3年最低。采样季节对呼吸强度测定有较大影响,春季土样能更好地反映土壤微生物活性的变化。风干土样可以通过预培养后测定土壤的呼吸作用,且能更加稳定地反映不同土壤之间的差异。在测定土壤基础呼吸时,利用1d或3d的培养平均值能更稳定地表现不同土壤的特性。累积呼吸量可较呼吸强度更直观地反映不同土壤的微生物活性。土壤有机质和全氮含量与土壤呼吸强度密切相关。

黄土丘陵区草地土壤微生物C、N及呼吸熵对植被恢复的响应

以野外样地调查和室内分析法研究了黄土丘陵区不同植被恢复年限下草地土壤微生物C、N及土壤呼吸熵的变化。结果表明,土壤微生物量碳明显地随着植被恢复年限的增加而增加。在恢复前23a,土壤微生物量碳在0～20cm土层年增加率为24.1%;20～40cm为104.4%。植被恢复23a后,0～20cm土层增长率为0.83%,20～40cm为0.19%。土壤微生物量N表现为在植被恢复的初期略有下降,3a后,开始出现明显增加。0～20cm土层年增长率为20.14%,20～40cm为15.11%。在植被恢复23a后,0～20cm土层的年增长率为0.14%,20～40cm变化不大。土壤微生物呼吸强度随着恢复年限的增加逐渐加强;土壤呼吸熵随植被封育时间的增加而呈对数降低趋势。土壤呼吸熵(qCO2)在反映土壤的生物质量变化时,显得更加稳定,受植物生长状况影响较小。相关分析表明,土壤微生物量和土壤微生物活性与土壤有机质、碱解氮和粘粒含量显著正相关;与土壤粉粒含量明显负相关;表层土壤pH值对其也有明显影响。草地植被自然恢复过程可增加土壤微生物活性,有利于土壤质量的提高。

激光衍射法与吸管法对东北黑土区土壤粒径分布测定的差异性研究

目前激光衍射法(laser diffraction method,LD)逐步被用于土壤颗粒粒径分布(particle size distribution, PSD)的分析,为了对比LD法和吸管法测定东北黑土区土壤PSD的差异性,采用LD法和吸管法分别对东北黑土区宾州河流域36个土壤剖面不同层次178个土壤样品的PSD值进行了测定与分析。结果表明,同吸管法相比,LD法低估了土壤的黏粒含量,平均低估幅度19.69%,而高估了土壤的粉粒和砂粒含量,平均高估幅度分别为14.66%和5.13%。LD法所得PSD结果依据美国土壤质地分类制判定的土壤质地,相对于吸管法总体由粉黏质偏向粉砂质方向。建立了LD法与吸管法测定PSD结果的转换模型,将LD法测定的PSD结果利用转换模型校正后,其测定的各土壤粒级同吸管法相比,准确度达96.97%～98.71%,判定土壤质地的准确率也达83.15%。

半干旱典型草原区封育草地土壤结构特征研究

以宁夏固原云雾山自然保护区典型草原为研究对象,采用空间序列代替时间序列的方法,以坡耕地为对照,对封育演替草地百里香(Thymus mongolicus Ronn.)、铁杆蒿(Artemisia sacrorum Ledeb.)、大针茅(Stipa grandis P.Smirn.)和本氏针茅(Stipa bungeana Trin.)群落0~10 cm表层土壤水稳性团聚体分布、孔隙度及土壤结构评价指标进行了研究和分析。结果表明:草地实施封育措施能明显改善土壤结构特征,随着草地植被自然演替,土壤的结构稳定性和孔隙状况逐步得到提高;在演替过程中,封育草地土壤的>0.25 mm水稳性团聚体含量(WSAC)、平均重量直径(MWD)、几何平均直径(GMD)和孔隙分形维数(Dp)逐渐增加,团聚体分形维数(Da)逐渐减少,说明植被演替能促进形成良好的土壤结构;同时,土壤结构影响因素随着草地植被演替过程表现出有机碳含量显著增加,容重显著降低,毛管孔隙度逐渐增大,非毛管孔隙度逐渐降低。本研究还比较了多项土壤结构评价指标,表明与MWD和GMD相比,指标WSAC(>0.25 mm)、Da及Dp能更好地反映出各封育草地群落之间土壤结...

原状土通气培养法测定黄土高原土壤供氮能力的研究

评价原状土通气培养法在反映黄土高原土壤供氮能力方面的效果。【方法】以采自于黄土高原差异较大的11个农田耕层土壤为供试土样,以包括和不包括土壤起始NO3--N原状土盆栽黑麦草累积吸氮量为参比,进行室内原状土通气培养法测定土壤供氮能力的研究。【结果】以包括土壤起始NO3--N盆栽试验植物吸氮量为参比,通气培养前CaCl2所淋洗起始NO3--N和起始矿质氮与5期黑麦草地上部氮素累积量密切相关,相关系数分别为0.856和0.862,达1%显著水平;与此相反,通气培养30周所矿化氮素、土壤起始矿质氮+通气培养30周矿化氮素、氮素矿化势(N0)及N0+起始矿质氮与5期黑麦草地上部氮素累积量间无显著相关关系,相关系数分别仅为0.410、0.553、0.492和0.419。以不包括土壤起始NO3--N盆栽试验植物吸氮量为参比,通气培养前CaCl2淋洗起始NO3--N和起始矿质氮与五期黑麦草地上部氮素累积量间的相关性尽管有所降低,但相关性仍达5%显著水平,相关系数分别为0.613和0.607;而通气培养30周矿化氮素、土壤起始矿质氮+通气培养30周矿化氮素、N0及N0+起始矿质氮与五期黑麦草地上部吸氮量的相关系数却明显...