Cleanup by solid‐phase extraction and HPLC of organochlorine insecticides and PCBS in various nonfatty and fatty samples

An accurate, simple and cheap extraction and cleanup procedure for capillary GC analysis of organo‐chlorine insecticides (OCs) in vegetables (cabbage and carrots) at the ng/g level, and for soil at the μg/g level is presented. The cleanup is carried out on solid‐phase extraction (SPE) cartridges, filled with 500 mg silica, 1 g of deactivated Florisil (10% w/w water), and 100 mg of anhydrous sodium sulphate. Recoveries >90% are obtained. The cleanup of OCs in fatty samples on an HPLC LiChrosorb Si 100 column is evaluated for subsequent capillary GC analysis. Fractionation of OCs and Aroclor 1254 and 1260 on an HPLC Nucleosil 100 column appears to be satisfactory.     

Evaluation of linear alkylbenzenesulfonate (LAS) biodegradability in sediment by solid‐phase extraction and HPLC analysis

The linear alkylbenzenesulfonate (LAS) sorption on environmental sediments has been known long ago. Their high concentrations reflect the massive input of these chemicals from household and industrial uses. However few attempts were made to identify biodegradation metabolites of LAS in sediment. In this report, a method for the determination of these compounds in sediment samples by high‐performance liquid chromatography (HPLC) is described. The first step of our work was performed by solid‐phase extraction with octadecyl‐bonded silica (C18) mini‐columns and provided a suitable recovery of LAS (90 ± 5%) and most metabolites. Furthermore, laboratory investigations led to study the behaviour of LAS in sediment. The environmental samples used for this purpose were collected from a pond (named étang de Bolmon) located in the French Mediterranean coast. Our results were in agreement with an aerobic biodegradation process of LAS that occurred only with high values of sediment redox potential and needed the samples to be vigorously shaken to ensure adequate mixing and suspension of particulate material. In a stagnant sediment or under anaerobic conditions, LAS is not degraded. p‐Sulfophenylacetic acid and p‐sulfocinnamic acid were evidenced as predominant metabolites and were found not to be persistent.     

煤矿瓦斯涌出时序预测的自组织数据挖掘方法

为分析煤矿瓦斯涌出复杂系统时间序列预测方法,提出自组织数据挖掘(SODM)与相空间重构(PSR)相结合的预测建模方法。首先应用C-C方法计算时间序列的最佳嵌入维数和延迟时间后进行PSR;然后以二元二次方程为传递函数,以嵌入维数变量为自变量,以延迟时间后的时间序列为因变量,通过内准则确定传递函数系数和外准则选择最优传递函数,并以最优传递函数的输出为下层迭代传递函数的输入,最后获得最优复杂度预测模型。算例结果表明:该方法对煤矿瓦斯涌出量预测的相对误差为-5.751 7% ~6.049 3%,平均相对误差2.145 7%,预测结果能满足煤矿安全生产实际工程应用要求。     

猪粪中典型类固醇雌激素的固相萃取/GC-MS检测

以猪粪中常见且具有较大潜在危害的E1(雌酮),17α-E2(17α-雌二醇),17β-E2(17β-雌二醇)和E3(雌三醇)为研究对象,建立了猪粪中这4种典型类固醇雌激素的GC-MS(气相色谱-质谱)分析检测方法.着重优化了样品的前处理方法,包括对超声提取剂、超声提取时间、固相萃取淋洗剂、衍生化温度和时间的优化选择.结果表明:在优化的试验条件下,猪粪中的典型雌激素E1,17α-E2,17β-E2和E3检出限分别为8.0,2.5,5.1和3.3 μg/kg,平均加标回收率在92.3%～137.4%之间.      

南宁城市内河水体和表层沉积物中有机氯农药分布特征

采用改进的固相萃取、加速溶剂萃取和气相色谱-电子捕获检测器,对广西壮族自治区南宁5条城市内河的水体和表层沉积物样品中7种痕量有机氯农药(OCPs)的残留状况进行了分析测定. 结果表明,南宁城市内河水体有机氯农药以HCHs为主,ρ(OCPs)为nd～0.141 μg/L. 5个点位沉积物中w(总OCPs)为2.13～2.80 μg/kg,均检出4,4′-DDE和4,4′-DDD,w(DDD)/w(DDE)<1,且DDTs在沉积物中的含量普遍高于HCHs. 各点位沉积物中有机氯农药各组分含量均低于美国环境保护署采用的无毒害风险浓度.      

EMC用V型人工电源网络的解析

本文分别对理想和实用的V型人工电源网络的阻抗(模和相位角)、隔离度进行计算和分析,并将其与某公司生产的ENV216型人工电源网络的测试参数进行比较,验证了ENV216型人工电源网络是完全符合标准要求的,加深了对电源端传导发射测试的理解。     

Do Polynomials Adequately Describe the Hypsometry of Monadnock Phase Watersheds?

Hypsometry has been shown to be a useful tool in geomorphic analysis of watersheds with the use of third‐degree polynomial equations to express the hypsometric curve. Despite its usefulness with watersheds in the equilibrium stage, the third‐degree polynomial has been found to be inadequate to describe the hypsometry of Monadnock phase watersheds. Three other equations — a modified third‐degree polynomial with a rational term, a sigmoidal model, and a double exponential — were used to determine hypsometric attributes of 32 Monadnock phase watersheds and compared to the third‐degree polynomial form. The three other equations were found to be better fits for Monadnock phase watersheds than the third‐degree polynomial equation, regardless of which ratio — area or elevation — was plotted as the independent variable. Due to the occasional failure of each functional form to give logical values for hypsometric attributes, the importance of using more than one form equation is discussed. After determining the best‐fit equation for each watershed, the usefulness of hypsometric attributes is discussed in relation to erosion processes within Monadnock phase watersheds.     

Highly active mixed-phase TiO2 photocatalysts fabricated at low temperature and the correlation between phase composition and photocatalytic activity

The idea of varying volume ratio of water to ethanol in solvent was firstly employed to yield phase composition controllable mixedphase titanium dioxide (TiO2) photocatalysts via a low temperature solvothermal route at 353 K. It was found that anatase contents increase from 0 to 100% with increase of ethanol contents in solvent. The mixed-phase TiO2 with 60% anatase content exhibited the best photocatalytic activity in photodecomposing formaldehyde (FAD) under UV light irradiation, which increases by about ...     

徐闻珊瑚礁保护区海水中多环芳烃的初探

2006年8月,对徐闻珊瑚礁自然保护区中多环芳烃的污染现状进行调查和研究,采用固相萃取,GC-MS检测,分析其中16种多环芳烃（PAHs）单体的含量,结果表明该海域海水中16种PAHs的总平均含量为87.06±90.62 ng·L^-1,变化范围为43.31～435.64 ng·L^-1,与世界其它一些近岸海区海水中的PAHs含量相比污染较为严重。A1站位的PAHs含量偏高,主要来源于陆地的工业废水和生活污水以及渔船油污。PAHs含量的增多对珊瑚礁生态系统具有一定影响,最终将影响到人类的自身健康。     

养殖废水中9种大环内酯及林可酰胺类抗生素的同时测定及分析方法研究

采用固相萃取-超高效液相色谱三重四极杆质谱联用法,建立了同时测定养殖废水中9种大环内酯及林可酰胺类抗生素的方法,并对样品pH值、保存时间、洗脱溶剂、上样流速及过滤材质等进行了优化。测定结果表明,pH值为6,过滤材质为聚丙烯（GHP）,上样速度为5 mL/min时,9种抗生素的加标回收率最优,为71.4%～126%,相对标准偏差最小,为2.4%～7.1%,标准曲线的线性最好,相关系数为0.998 5～0.999 5,检出限为0.78～1.22 ng/L。该方法灵敏度高、检出限低、测定结果准确,能够广泛应用于养殖废水中大环内酯及林可酰胺类抗生素残留量的监测分析。