微波萃取技术在分析土壤中有机污染物的应用

介绍了微波萃取技术及其使用的试剂、设备和条件,对微波萃取在分析土壤中有机污染物的应用予以综述,阐述了微波萃取技术是分析土壤中有机污染物的好方法。     

高氯低COD值水样的无汞快速测定法

以硝酸银和硫酸铬钾代替硫酸汞来消除 COD 测定中的氯离子干扰,同时将重铬酸钾溶液的浓度降低为0.100 mol／L,并用硫磷混酸代替硫酸,该方法经过对标准样品和实际样品的测定,表现出对于测定氯离子含量低于25000 mg／L的高氯低 COD 值水样具有较好的准确度和精密度,同时可以实现银盐的回收再利用。     

A New Approach to Plant Diversity Assessment Combining HPLC Data, Simplex Mixture Design and Discriminant Analysis

The quantitative assessment of plant diversity and its monitoring with time represent a key environmental issue for management and conservation of natural resources. Assessment of plant diversity could be based on chemical analyses of secondary metabolites (e.g. flavonoids, terpenoids), because of the substantial quantitative and qualitative between-individual variability in such compounds. At a geographical scale, the plant populations become widely dispersed, and their monitoring from numerous routine individual analyses could become restricting. To overcome such constraint, this study develops a multivariate calibration model giving the relative frequency of a particular taxon from a simple high-performance liquid chromatography (HPLC) analysis of a plant mixture. The model was built from a complete set of mixtures combining different taxons, according to an experimental design (Scheffé’s matrix). For each mixture, a reference HPLC pattern was simulated by averaging the individual HPLC profiles of the constitutive taxons. The calibration models, based on Bayesian discriminant analysis (BDA), gave statistical relationships between the contributions of each taxon in mixtures and reference HPLC patterns of these mixtures. Finally, these models were validated on new mixtures by using outside plants. This new biodiversity survey approach is illustrated on four chemical taxons (four chemotypes) of Astragalus caprinus (Fabaceae). The more differentiated the taxon, the better predicted its contributions (in mixtures) were by BDA calibration model. This new approach could be very useful for a global routine survey of plant diversity.     

盲样考核浓度预判及稀释方法——以原子荧光法测定水中砷为例

以原子荧光法测定水中砷为例,探讨了实验室盲样考核浓度预判及稀释方法.分析了3个砷盲样考核实例,归纳了“直接稀释法”“系列稀释法”“最大稀释法”3种方法,分别适用于盲样浓度范围窄、适中、宽3种情况,检测人员可根据考核机构给定的浓度范围合理选用.     

挥发性有机物污染土壤样品采样方法比较

以苯系物污染土壤样品的采集为例,比较了4种不同采样方法导致样品检测结果的差异。其中,方法 1将样品装填至广口瓶内并压实密封,方法2采用非扰动采样器采集10 g样品后转移至加有10 mL甲醇保护剂的Vial瓶中密封,方法 3用非扰动采样器采集10 g样品后直接将其密封于采样器内,方法 4用Encore采样器采样后将其密封于采样器内。结果表明,方法 2采集样品的检出率最高,其余3种方法的差异不明显,方法 2采集样品的检出结果 71%以上都大于其余3种方法。而且,对于挥发性较强的苯与甲苯,以方法 2采集的样品91%以上都大于其余3种方法,最大及平均检出浓度高出2~3个数量级。5种不同土质样品检测结果表明,对于有机质含量较低的细砂,方法2的最高及平均检出浓度均高于其余3种方法 1~3个数量级,差异随土壤有机质含量的升高而降低。可见,对于苯系物及挥发性强于苯系物的其他挥发性有机物污染土壤样品的采集,方法 2效果最优,可指定为VOCs污染场地土壤样品的采样方法。     

Biomethanation of plant materials and agricultural residues using dung samples as wild population of microbes and also with isolated methanogens

Recycling of plant materials and agricultural residues for biomethanation was attempted in vials. The methanogenic activities of certain sewage samples have also been tested. Both sterilized and non-sterilized biomasses were used. Biomethanation was carried out with dung samples (cow, goat, buffalo, piggery wastes and poultry wash) as wild populations of microbes and in combination with other microbial isolates (isolated in the laboratory).Biomethanation had been observed to be good in most cases and particularly with the sterilized biomass. Mixed inoculum (dung samples and poultry wash) was found to be best for biomethanation. Of the microbe isolates, isolates from buffalo, pig and paper mill wastes appear to be most effective. Pretreated sawdust and rice straw were found to be good subtrates for biomethanation. Of the different plant biomass used Spirogyra (algae), Ipomea and water hyacinth were most effective whereas Jatropa gossypifolia and Parthenium sp. were the least effective. Biomethanation of Spirogyra was carried out both in anoxic and oxic conditions. Though methane production decreased enormously under oxic conditions, definite methane production continued indicating that the biomethanation process is not exclusively anoxic. Similarly, biomethanation of sewage samples from different sewage treatment plants were carried out with and without isolated methanogens and methane production was found to be moderate.     

Determination of Q1, an unknown organochlorine contaminant, in human milk, Antarctic air, and further environmental samples

Q1, an organochlorine component with the molecular formula C(9)H(3)Cl(7)N(2) and of unknown origin was recently identified in seal blubber samples from the Namibian coast (southwest of Africa) and the Antarctic. In these samples, Q1 was more abundant than PCBs and on the level of DDT residues. Furthermore, Q1 was more abundant in seals from the Antarctic than the Arctic. To prove this assumption, gas chromatography-electron-capture negative ion mass spectrometry (GC/ECNI-MS), which is sensitive and selective for Q1, allowed for screening of traces of Q1 even in samples with particularly high levels of other organochlorine contaminants. Q1 was isolated by high-performance liquid chromatography (HPLC) from a skua liver sample. A 1:1 mixture with trans-nonachlor in electron-capture detectors (ECDs) was used to determine the relative response factor with ECNI-MS. The ECNI-MS response of Q1 turned out to be 4.5 times higher than that of trans-nonachlor in an ECD. With GC/ECNI-MS in the selected ion-monitoring mode, four Antarctic and four Arctic air samples were investigated for the presence of Q1. In the Antarctic air samples, Q1 levels ranged from 0.7 to 0.9 fg/m(3). In Arctic air samples, however, Q1 was below the detection limit (<0.06 fg/m(3) or 60 ag/m(3)). We also report on high Q1 levels in selected human milk samples (12-230 microg/kg lipid) and, therefore, suggested that the unknown Q1 is an environmental compound whose origin and distribution should be investigated in detail. Our data confirm that Q1 is a bioaccumulative natural organochlorine product. Detection of a highly chlorinated natural organochlorine compound in air and human milk is novel.     

Analysis of trace dicyandiamide in stream water using solid phase extraction and liquid chromatography UV spectrometry

An improved method for trace level quantification of dicyandiamide in stream water has been developed. This method includes sample pretreatment using solid phase extraction. The extraction procedure (including loading, washing, and eluting) used a flow rate of 1.0 mL/min, and dicyandiamide was eluted with 20 mL of a methanol/acetonitrile mixture (V/V = 2:3), followed by pre-concentration using nitrogen evaporation and analysis with high performance liquid chromatography–ultraviolet spectroscopy (HPLC–UV). Sample extraction was carried out using a Waters Sep-Pak AC-2 Cartridge (with activated carbon). Separation was achieved on a ZIC^®-Hydrophilic Interaction Liquid Chromatography (ZIC-HILIC) (50 mm × 2.1 mm, 3.5 μm) chromatography column and quantification was accomplished based on UV absorbance. A reliable linear relationship was obtained for the calibration curve using standard solutions (R² > 0.999). Recoveries for dicyandiamide ranged from 84.6% to 96.8%, and the relative standard deviations (RSDs, n = 3) were below 6.1% with a detection limit of 5.0 ng/mL for stream water samples.