水中有机磷农药分析前处理方法探讨

分别采用液-液萃取、固相萃取前处理方法,提取水中10种常见的有机磷农药,对比了这两种提取方法的测定结果、经济成本、花费时间及对环境的影响,建议逐步用固相萃取法取代液？液萃取法提取水中有机磷农药。     

顶空气相色谱法测定土壤中频哪酮

确定了顶空气相色谱法测定土壤中频哪酮。该法利用气固平衡原理,在密闭容器中,将土壤中频哪酮挥发到气相中,然后用气相色谱测定气相中频哪酮浓度。研究表明,该方法具有分离效果较好,前处理简单、快速、准确、灵敏度高、重复性好等特点,因此适用于土壤中频哪酮的测定。     

超声提取-气相色谱质谱法测定大气PM2.5中正构烷烃

建立了超声提取-气相色谱质谱法测定大气PM2.5中32种正构烷烃方法,经离子温度优化、前处理比较、空白滤膜考察等获得了最佳的实验条件。研究发现,高、中、低3种浓度标准曲线的相关系数均在0.995以上,3种浓度的空白样品加标回收率分别为72.2%~117.8%、73.5%~104.4%、73.8%~109.5%,精密度均小于10%,实际样品加标回收率为75.7%~108.9%。当采样体积为24 m3时,各目标化合物的方法检出限为0.046~2.6 ng/m~3;经正构烷烃浓度范围为0.17~64.3 ng/m~3的1月及浓度范围为0.53~7.67 ng/m~3的6月的实际样品验证,该方法的检出限和测量范围也可较好的满足实际样品的测定。     

甲胺、二甲胺及三甲胺的气相色谱测定

采用气相色谱法、大口径毛细管柱分离了甲胺、二甲胺、三甲胺.用氮磷检测器(NPD)检测,得到了良好的分离效果和很高的灵敏度,检测限可达0.025mg/L.同时,对甲胺类在NPD和氢火焰离子化检测器(FID)上的灵敏度作了比较,发现甲胺类物质在NPD上的灵敏度大大高于FID,因此,前者特别适用于检测环境试样中低含量甲胺类有机物的监测.     

气相色谱法测定环境空气中吡啶

建立了用气相色谱法测定环境空气中吡啶的方法。环境空气中吡啶活性炭吸附,二硫化碳解吸,DB-200毛细管柱分离,直接进样分析,氢火焰离子化检测器检测,时间定性,峰面积定量,吡啶回收率为91．5％～103．1％,当采样体积为20L,吡啶最低检出质量浓度分别为0．006mg/m 3。本方法前处理简便,分离度好,分析灵敏度高,满足环境分析要求。     

Polychlorinated biphenyls in two mollusc species from the coast of Tenerife (Canary Islands, Spain)

Levels of PCBs were determined in two marine organisms, limpets (Patella ullisiponensis aspera) and winkles (Ossilinus atratus), sampled in three stations in the south east coast of Tenerife during 1993. Winkles and limpets exhibited different PCB patterns. Principal Component Analysis (PCA) was used to study the patterns and the relationships among PCBs.     

高效液相色谱法测定矿区塌陷区水体中多环芳烃

高效液相色谱法是目前多环芳烃(PAHs)测定最常用技术之一。针对EPA规定的16种优先控制PAHs污染物,采用高效液相色谱法进行矿区塌陷区水体样品的测试。通过紫外-荧光串联使用,紫外检测器变波扫描,荧光检测器波长切换,合理设定流动相梯度洗脱程序等手段优化分析条件,使16个组分在40min内获得良好的分离效果。并分别选取在紫外和荧光检测条件下各组分的最大响应进行定量,使各组分均具有更低的检出限。本方法精密度为0.98%～10.4%,加标回收率达72.4%～112%,可作为各种环境样品中PAHs分析检测的参考。     

原油降解中微生物群落的16S rDNA-PCR-DGGE分析

为对原油降解过程中微生物群落结构的变化,本文采用直接向原油中加入营养物刺激的方法,获得原油降解菌体系。提取不同培养时间条件下降解菌体系的总DNA,并以之为模板采用PCR-DGGE技术研究了在原油降解过程中微生物群落的组成,结果表明,随着培养时间的不同,微生物的群落结构表现出差异,随着时间的变化其微生物群落也会发生改变。回收了DGGE图谱中的18个条带,测序结果经过Blast比对表明其中10个条带代表的细菌是不可培养的,显示了DGGE技术的优越性。同时采用气相色谱技术对降解过程中的原油烃的变化进行了分析,结果显示原油烃类组分会随着降解菌多样性的变化而发生变化,降解菌体系表现出了其对烷烃类物质的降解能力。     

The conversion of chicken manure to biooil by fast pyrolysis II. Analysis of chicken manure,biooils, and char by curie-point pyrolysis-gas chromatography/mass spectrometry (Cp Py-GC/MS)

The initial chicken manure and the three fractions derived from it by fast pyrolysis, that is, the two biooils Fractions I and II as well as the residual char were analyzed by Curie-point pyrolysis-gas chromatography/mass spectrometry (Cp Py-GC/MS). The individual compounds identified were grouped into the following six compound classes: (a) N-heterocyclics; (b) substituted furans; (c) phenol and substituted phenols; (d) benzene and substituted benzenes; (e) carbocyclics; and (f) aliphatics. Of special interest were the relatively high concentrations of N-heterocyclics in biooil Fraction II which was obtained in the highest yield and had the highest calorific value. Prominent N-heterocyclics in biooil Fraction II were methyl-and ethyl-substituted pyrroles, pyridines, pyrimidine, pyrazines, and pteridine. Also noteworthy was the high abundance of aliphatics in biooil Fraction I and the char. The alkanes and alkenes in biooil Fraction I ranged from n-C₇ to n-C₁₈ and C_7:1 to C_18:1, respectively, and those in the char from n-C₇ to n-C₁₉ and C_7:1 to C_19:1, respectively. The N-heterocyclics in the two biooil Fractions came from the chicken manure, from proteinaceous materials during fast pyrolysis or were formed during the fast pyrolysis manure conversion by the Maillard reaction which involved the formation of N-heterocyclics by amino acids interacting with sugars.     

Behavior of fenhexamid in soil and water

A study was conducted to investigate fenhexamid (FEX) behavior in soil and in water. FEX proved to be rather stable at acid pH but showed slight degradation at neutral and alkaline pH. After 101 days of FEX spiking of a soil sample, 94% at pH 4, 12% at pH 7 and 23% at pH 9 of the active ingredient was still present. In natural water the rate of FEX disappearance appeared to be slow which may be due to abiotic rather than biotic processes. The soil degradation tests showed low persistence of the active ingredient if a good microflora activity is guaranteed (DT₅₀ about 1 day). Moreover, in absence of microorganisms, FEX proved to be stable. Humidities of 25 and 50% of Water Holding Capacity (WHC) influenced in equal measure the rate of degradation. From the same soil, a bacterium was isolated and identified as Bacillus megaterium, which was able to metabolize FEX with the hydroxylation of the cyclohexane ring. Moreover, FEX showed an elevated affinity for humic acid (73%), smectite (31%), and ferrihydrite(20%) and low affinity for vermiculite (11%) and kaolinite (7%).