Gas Chromatography for Determination of Pesticides in Aquatic Systems — Analytical Basis Gaschromatographie zur Bestimmung von Pestiziden in aquatischen Systemen — Analytische Grundlagen

High resolution gas chromatography (HRGC) with ECD, NFID and MSD is a very efficient determination method for pesticides in water. Because of their relatively low concentrations in aquatic systems enrichment and preconcentration procedures are essential. Some examples for pesticide determination by GC methods are given. Potentials and limitations of HRGC for pesticide analysis are also discussed. An extensive pesticide analysis in water has to include different methods like HRGC, HPLC and GC/MS.     

Natural Gas Hazard (CO2, 222 Rn) within a Quiescent Volcanic Region and Its Relations with Tectonics: The Case of the Ciampino-Marino Area, Alban Hills Volcano, Italy

Groundwater surveys were performed by detailed(around 300 sites) grid-analysis of water temperature, pH, redox potential, electrical conductivity, ²²²Rn, alkalinity and by calculating the pCO₂, throughout the Ciampino and Marino towns in the Alban Hills quiescent volcano (Central Italy). Following several episodes of dangerous CO₂ exhalation from soils during the last 20 years and earlier ashistorically recorded, the work aimed at assessing the Natural Gas Hazard (NGH) including the indoor-Rn hazard. The NGH was defined as the probability of an area to become a site of poisonous peri-volcanic gas exhalations from soils to the lower atmosphere (comprising buildings). CO₂ was found to be a ``carrier' for the other poisonous minor and in trace components (H<sub>s</sub>S, CH<sub>4</sub>, <sup>222</sup>Rn, etc.). This assessment was performed by extrapolating in the aquifer CO<sub>2</sub> and <sup>222</sup>Rn conditions, and discriminating sectors where future CO<sub>2</sub> flux in soils as well as indoor-Rn measurements have to be noted. A preliminary indoor-Rn survey was performed at about 200 sites. The highest values were found in the highest pCO<sub>2</sub> and high <sup>222</sup>Rn values in groundwater. This indicates convection and enhanced permeability in certain sectors of the main aquifer, i.e., along the bordering faults and inside the gas-trap of the Ciampino Horst., where ``continuous gas-phase micro-macro seepage mechanism' is invoked to explain the high peri-volcanic gases flux.     

抑制型离子色谱法同时测定水中锂和锶

对离子色谱法测定水中的锂、锶含量及其影响因素进行了研究。以甲烷磺酸为流动相，用IonPacCS12A阳离子色谱柱分离后，电导检测器同时测定矿泉水中锂和锶，其检出限分别为0．003mg／L和0．006mg／L。对Li^＋和Sr^2＋的离子色谱条件进行了优化，并对流动相的选择及干扰离子的影响进行了讨论。     

离子色谱法测定五氧化二铌和五氧化二钽中痕量氟氯和硫酸根离子的前处理方法

采用马弗炉将样品与NaOH混合进行熔融煅烧，热去离子水提取、离心、稀释后过OnGuard Ⅱ H柱和过滤膜进行前处理，抑制型电导离子色谱法检测，测定了Ta2O5和Nb2O5的氟离子、氯离子和硫酸根离子。该方法对三种被测阴离子的检测限（s／N=3）在0．15～0．70μg／g（以固体样品实际浓度计）或0．136～0．623μg／L（以溶液浓度计），标准曲线线性范围均在两个数量级以上，方法的精密度（RSD，n=7）小于5．46％，回收率为88％～106％，具有灵敏度高、选择性好、重现性佳、对环境友好等特点，用于实际样品的检测，结果令人满意。     

南海含天然气水合物地层地震反射特征及可能分布研究

天然气水合物是当前能源与环境领域的研究热点之一,南中国海是天然气水合物赋存的有利区域。天然气水合物的存在改变了沉积地层的声学特征,这一性质使多道地震勘探成为发现海洋天然气水合物的主要手段。本文首先根据地震成像结果定性分析南海可能含天然气水合物沉积地层的地震反射特征,初步确定天然气水合物存在的可能性并指出地震成像关键技术。在无井条件下,构建虚拟井进行波阻抗反演得到定量的地层速度参数进一步证实这一可能性,最后将反演获得的速度场与ODP184 航次在此区域获得的地球物理、地球化学信息综合分析,可以确定此区域天然气水合物的存在及其空间展布。     

华北平原冬麦田土壤CH4的吸收特征研究

利用静态箱/气相色谱(GC)法,对华北平原冬小麦拔节-成熟期间麦田土壤CH₄气体通量进行了测定,得出华北平原典型冬麦田土壤是大气CH₄的弱吸收汇。试验期间土壤CH₄通量存在明显的季节变化和日变化,麦田拔节-成熟期间土壤CH₄通量日平均值为-18.3μg·m^-2·h^-1,波动范围为-4.3-24.4μg·m^-2·h^-1;在土壤CH₄通量的日变化中,观测到麦田土壤在午间和夜间都有一个吸收峰,峰值出现的时间因生育期不同而有所不同。试验期间CH₄通量日平均值与土壤温度关系不明显,而与土壤水分呈负相关(α=0.01);日变化中土壤CH₄通量与地表温度的相关性较差,而与5cm地温相关密切。麦田拔节-成熟期间土壤CH₄通量日平均值随NH4+-N施用量的增加呈递减规律,农田秸秆还田后不利于土壤对CH₄的吸收。     

Scalar Similarity for Relaxed Eddy Accumulation Methods

The relaxed eddy accumulation (REA) method allows the measurement of trace gas fluxes when no fast sensors are available for eddy covariance measurements. The flux parameterisation used in REA is based on the assumption of scalar similarity, i.e., similarity of the turbulent exchange of two scalar quantities. In this study changes in scalar similarity between carbon dioxide, sonic temperature and water vapour were assessed using scalar correlation coefficients and spectral analysis. The influence on REA measurements was assessed by simulation. The evaluation is based on observations over grassland, irrigated cotton plantation and spruce forest.Scalar similarity between carbon dioxide, sonic temperature and water vapour showed a distinct diurnal pattern and change within the day. Poor scalar similarity was found to be linked to dissimilarities in the energy contained in the low frequency part of the turbulent spectra ( < 0.01 Hz).The simulations of REA showed significant change in b-factors throughout the diurnal course. The b-factor is part of the REA parameterisation scheme and describes a relation between the concentration difference and the vertical flux of a trace gas. The diurnal course of b-factors for carbon dioxide, sonic temperature and water vapour matched well. Relative flux errors induced in REA by varying scalar similarity were generally below ± 10%. Systematic underestimation of the flux of up to − 40% was found for the use of REA applying a hyperbolic deadband (HREA). This underestimation was related to poor scalar similarity between the scalar of interest and the scalar used as proxy for the deadband definition.     

GDX-502树脂富集高效液相色谱法测定地表水中酚类化合物

采用自制GDX-502固相萃取小柱萃取水中苯酚、对硝基酚、间甲酚、2，4-二氯酚、2，4，6-三氯酚、五氯酚等6种酚类化合物，以乙腈作为洗脱剂，选择280nm和290nm双波长紫外高效液相色谱进行检测。结果表明，方法检出限为0．01-0．05mg／L，IL水的平均加标回收率为82．5％-95．0％，精密度（RSD，n=7）为3．6％-9．2％。方法用于实际地表水中痕量酚类化合物的检测，操作简单，有机溶剂用量少，分析效率高；萃取小柱可多次重复使用，分析成本低。     

离子色谱法测定水果和蔬菜中硝酸盐

利用DIONEX-2020i离子色谱仪、IonPac AS3分离柱对蔬菜和水果中硝酸盐进行测定。通过．等冀合适的前处理方法，获得纯清溶液。提出只使用分离柱，以提高灵敏度、缩短出峰时间和改善峰形。方法精密度好、检出限低、操作简便快速，用于实际样品的检测，10次测定的相对标准偏差小于2％，加标回收率为97％～98％。