冲积平原区土壤中重金属元素的存在形态分析

采用0.1mol／L氢氧化钠浸提腐殖酸的方法,将土壤中的腐殖酸及与腐殖酸结合的重金属元素分离出来;分别用分光光度法、原子荧光光谱法、等离子质谱法测定样品中腐殖酸及重金属元素的含量;初步测定结果显示：与腐殖酸结合的重金属元素是冲积平原区表层土壤中重金属元素的1种重要存在形态,而且可能是土壤中重金属污染元素主要的存在形式。     

Production and properties of a biosurfactant applied to polycyclic aromatic hydrocarbon solubilization

Microorganisms isolated from a soil sample collected from a gasoline filling station (located in Guwahati) were tested for their pyrene- and anthracene-degrading potential. Preliminary studies showed the ability of the organism to grow on carbon-free mineral medium (CFMM) supplemented with pyrene as the sole source of carbon. The organisms were found to produce a bioemulsifier when grown on CFMM with glucose or glycerol and/or pyrene as the carbon source. The organisms could also utilize anthracene when grown on mineral salt medium along with 2% glycerol. Within 2 d, anthracene concentration dropped less than 30% of the original concentration. Approximately 100 mg of the emulsifier was isolated from 25 mL of the 5-d-grown culture. The emulsifier was tested to produce emulsion with both an aliphatic and an aromatic group of hydrocarbons and resulting emulsions were found to be stable for a long period of time when keptat 10–15°C. The emulsifier was also quite stable in a pH range of 3.0–11.0. In a concentration range of 0.5–10 mg/mL, it resulted in a linear increment of apparent pyrene and anthracene solubility in water.     

微分电位溶出法测定土壤中的微量砷

用金膜电极－微分电位溶出法测定了土壤中的微量砷，讨论了最佳测定条件。     

Secondary succession and its effects on soil moisture and nutrition in abandoned old-fields of hilly region of Loess Plateau, China

Floristic composition, community structure and soil moisture and nutrient contents in abandoned fields of different ages were analyzed to clarify the regenerative aspects of succession as a tool for vegetation restoration. The results indicated that secondary succession in this region can be interpreted as an auto-succession: there are main changes in species-relative abundance and species turnover. Annual or biennial species (e.g. Artemisia scoparia), acted as pioneers and strongly dominated the early stages. Then, they underwent a progressive decline, while forbs (e.g. Artemisia sacrorum) and grasses (e.g. Xanthium sibiricum) had their peak abundance at intermediate stages. Dwarf shrubs (e.g. Lespedeza dahurica) and short rhizome grass (e.g. Bothriochloa ischaemum) appeared at mid-succession stage and gradually increased in abundance during succession, becoming dominant at late stages. The first axis of detrended correspondence canonical analysis arranged the sites according to their fallow time, indicating a successional sere. The second axis, associated with diverging pathways of regeneration, correlated with topographic factors and soil moisture and nutrition. Structural divergence between plots increased as succession went on, attained the highest at the mid-succession stage, decreased at the late stage.

Soil moisture and available phosphorus content decreased steadily with field age after their abandonment, whereas pools of organic matter, total and available nitrogen, potassium and total phosphorus increased with field age. The pace and direction of recovery of native vegetation and natural soil properties in these abandoned fields resembled classic old-field succession, which is a form of secondary succession that often serves as a template for guiding restoration efforts. Interface between the abandoned field soil and plant system was crucial to the above process. Our current study supported the generally accepted hypothesis in the succession literature.     

高效毛细管电泳-二极管阵列检测法测定土壤中的苯酚

建立了高效毛细管电泳-二极管阵列检测器测定土壤样品中苯酚的方法,研究了检测波长、缓冲体系、缓冲体系的pH值及浓度、分离电压、进样时间及压力等因素。结果表明,在温度25℃、pH=10的30mmol/L K2HPO4+0.5mmol/L十四烷基三甲基溴化铵(TTAB)运行缓冲溶液、检测波长206nm、20kV运行电压、负电压模式、0.5psi进样10s条件下,苯酚在4.2到4.4min内出峰,迁移时间和峰面积的相对标准偏差(RSD)分别为0.11%、0.28%,检出限(3Sb/Sx)为0.01mg/L。该方法成功地应用于土壤中苯酚的测定,其回收率为98.4%。     

Enantioselective separation of the carfentrazone‐ethyl enantiomers in soil,water and wheat by HPLC

A simple enantioselective HPLC method was developed for measuring carfentrazone‐ethyl enantiomers. The separation and determination was accomplished on an amylose tris[(S)‐α‐methylbenzylcarbamate] (Chiralpak AS) column using n‐hexane/ethanol (98:2, v/v) as mobile phase at a flow rate of 1.0 mL/min with UV detection at 248 nm. The effects of mobile‐phase composition and column temperature on the enantioseparation were discussed. The accuracy, precision, linearity, LODs, and LOQ of the method were also investigated. LOD was 0.001 mg/kg in water, 0.015 mg/kg in soil and wheat, with an LOQ of 0.0025 mg/kg in water and 0.05 mg/kg in soil and wheat for each enantiomer of carfentrazone‐ethyl. SPE was used for the enrichment and cleanup of soil, water, and wheat samples. Recoveries for two enantiomers were 88.4–106.7% with RSD_r of 4.2–9.8% at 0.1, 0.5, and 1 mg/kg levels from soil, 85.8–99.5% with the RSD_r of 4.4?9.6% at 0.005, 0.025, and 0.05 mg/kg levels from water, and from wheat the recoveries were 86.3?91.3% with RSD_r below 5.0% at 0.2, 0.5, and 1 mg/kg levels. This method could be used to identify and quantify the carfentrazone‐ethyl enantiomers in food and environment.     

气相色谱-火焰光度法测定土壤中有机磷农药残留

建立了气相色谱-火焰光度(GC-FPD)分析土壤中敌敌畏、氧化乐果、二嗪农、乐果、甲基对硫磷、马拉硫磷、对硫磷、水胺硫磷、喹硫磷等9种有机磷农药残留量的方法。样品用丙酮-二氯甲烷(1:3)提取,浓缩、定容后用Hp-5MS(30m×0.25 mm×0.25μm)毛细管柱分离,FPD检测器检测。方法回收率在68.71%～110.39%之间;RSD在5.5%～11%之间;检出限在0.397～1.60μg/mL之间,方法可用于环境土壤样品中有机磷农药残留的测定。     

Determination of maize and grain herbicides and their transformation products in soil by use of soil column extraction then liquid chromatography with tandem mass spectrometry

Summary A multiresidue method has been developed for identification and quantitation of the herbicides most commonly used in cultivation of maize and grain, and of their transformation products, in soil samples. The analytes were isolated by soil column extraction (SCE) and the extracts were purified by use of a Carbograph-1 cartridge. Analysis was performed by liquid chromatography coupled with tandem mass spectrometric detection (LC-TISP-MS-MS) in negative-ion mode. To optimize the extraction conditions affecting the performance of SCE, e.g. the extracting solvent used, temperature, extracting volume, and solvent flow rate, were studied. To evaluate the matrix effect in SCE, recovery experiments were performed on soil samples, with different physical and chemical characteristics, fortified with the 100 ng g⁻¹ of the target compounds. Recovery data were satisfactory and the method detection limits were between 3 and 100 ng g⁻¹, depending on the compound.     

土壤中挥发性有机化合物的GC-MS测定

利用气相色谱－质谱联用技术，对某废弃化工厂原厂区及附近农田的土壤中可能存在的60种挥发性有机化合物进行了定性和定量分析；采用质量保证和质量控制步骤对分析结果进行监测，结果令人满意。     

重量法测定土壤水溶性盐总量的优化

土壤水溶性盐是表征土壤盐碱化程度的重要指标,也是评价耕地地力的重要参数,被纳入第三次全国土壤普查（“三普”）监测指标体系中。重量法是测定土壤水溶性盐总量的最常用方法,其测定过程易受多种因素影响,导致其测定结果不准。鉴于此,本文设计试验分别验证了水溶性盐浸提和浸提液固液分离这两个过程对测定结果的影响,结果表明浸提液固液分离是影响土壤水溶性盐总量测定准确度和精密度的主要因素。基于此进一步探究4种不同固液分离方式（布氏漏斗过滤、滤膜真空抽滤、离心、滤纸组合过滤）对测定结果的影响,结果表明相较于其它方式,滤纸组合过滤测定结果准确度高,适用于土壤水溶性盐总量的测定。对改进后的重量法测定土壤水溶性盐总量进行方法学确认,结果表明其检出限为0.01 g/kg,测定下限为0.04 g/kg;方法的准确度和精密度、适用范围等均符合相关要求。本文推荐的土壤水溶性盐总量测定方法为：土壤样品采用1:5土水比浸提,180 r/min振荡3 min,浸提液采用滤纸组合自然过滤;其测定结果的准确度和精密度符合相关要求。本文旨在为“三普”内业检测提供参考和借鉴,为全面摸清不同区域土壤水溶性盐含量水平及土壤盐渍化程度提供技术支撑。