气质联用法测固定污染源中三氟甲烷、四氟甲烷、六氟乙烷和六氟化硫

建立了固定污染源排气中三氟甲烷、四氟甲烷、六氟乙烷和六氟化硫的采样和气质联用分析方法,检出限分别为0.06、0.15、0.21、0.71 mg/m3,精密度在3.2%以下,相关系数大于0.999 6,并对浙江省内2家典型企业排放的温室气体进行了监测,实际样品监测结果表明,该方法能够满足废气中4种温室气体的监测要求。     

三峡库区重庆段江水中持久性有机污染物污染状况分析

对三峡库区重庆段水域中持久性有机污染物的污染状况进行了分析,两期水样检出百多种有机物,冬季枯水期检出178种;夏季丰水期检出144种。其中属于美国国家环保局优先控制污染物黑名单的有18种,属于我国优先控制污染物黑名单的有7种。分析结果表明,重庆段水域多环芳烃类和邻苯二甲酸酯类检出率比较高,需要予以密切关注。     

毛细管柱气相色谱质谱法分析优先监测物的质量控制研究——Ⅰ.半挥发性有机物

报道了毛细管柱气相色谱质谱联用(GC-MS)方法分析半挥发性有机物的质量控制研究结果.对分析的全过程提出了质量控制标准.应用同位素标记内标物(IS),替代掺样物(SS)和基质掺样/重复基质掺样(MS/MSD)的回收率来判断样品处理与分析结果的可靠性.根据77种目标化合物,特别是标定检验化合物(CCC)和系统检验化合物(SPCC)的响应系数范围,确定GC-MS系统的工作状态和最终结果的正确性.给出了满足质量控制标准的12个土壤样品的结果.     

气相色谱—串联质谱法检测水中苯霜灵、甲霜灵、噁霜灵残留量

建立水中甲霜灵、苯霜灵、噁霜灵农药残留量的气相色谱—串联质谱(GC-MS/MS)的检测分析方法。样品采用乙腈提取、固相萃取(SPE)柱净化。采用GC-MS/MS分析时,三种农药在15 mim内完全分离并流出。添加浓度加标回收率为80.6%~88.4%,相对标准偏差(RSD)小于5.0%。在0.01~0.20 mg/L质量浓度范围之间线性关系良好(r~20.999 0)。该方法的灵敏度、精密度和准确度均满足农药残留分析要求,适用于水中的农药残留的快速筛查与定性、定量分析。     

Plant steroid hormones produced under Ni stress are involved in the regulation of metal uptake and oxidative stress in Brassica juncea L

Brassinosteroids (BRs) are involved in the amelioration of various biotic and abiotic stresses. With an aim to explore the role of BRs under heavy metal stress, plants of Brassica juncea L. were grown in pots. The plants were subjected to various concentrations of Nickel metal (0.0, 0.2, 0.4 and 0.6 mM) and harvested on 60th day in order to observe the expression of these hormones. The isolated BRs from the leaves of Brassica plants characterized by GC-MS include 24-Epibrassinolide (24-EBL), Castasterone, Dolicholide and Typhasterole. The effect of isolated 24-EBL was studied on Ni metal uptake and antioxidative defense system in 60 d old plants of Brassica. It was observed that 24-EBL significantly increased the activities of stress ameliorating enzymes and lowered the metal uptake in plants. This is the first report in B. juncea L. plants showing the expression of BRs under metal treatments and effect of the isolated 24-EBL on metal uptake and in oxidative stress management.     

Decay profile and metabolic pathways of quinalphos in water, soil and plants

The widespread occurrence of pesticide residues in different agricultural and food commodities has raised concern among the environmentalists and food chemists. In order to keep a proper track of these materials, studies on their decay profiles in the various segments of ecosystem under varying environmental conditions are needed. In view of this, the metabolites of quinalphos in water and soil under controlled conditions and in plants, namely tomato and radish in field conditions have been analysed and possible pathways suggested. In order to follow the decay of the pesticide, an HPLC procedure has been developed. Studies conducted in water at different temperatures, pH and organic content reveal that the persistence of the pesticide decreases with the increase in all the three variables. In the three different types of soils studied, the effect of pH is more or less apparent on a similar line. On an average a faster decay is observed in the case of plants than in water and soil. The decay profiles in all these cases follow first order kinetics. The metabolites were identified by GC-MS. The investigations reflect that degradation occurs through hydrolysis, S-oxidation, dealkylation and thiono-thiol rearrangement. The pathways seem to be complex and different metabolites were observed with the change in the matrix. Quinalphos oxon, O-ethyl-O-quinoxalin-2-yl phosphoric acid, 2-hydroxy quinoxaline and quinoxaline-2-thiol were observed in all the matrices. Results further indicate that the metabolites, 2-hydroxy quinoxaline and oxon, which are more toxic than parent compound, persist for a longer time.     

Fenton法处理竹制品废水生化出水的研究

采用Fenton法对竹制品废水生化出水的脱色和有机物去除进行了研究.在综合考虑经济性和去除效果的基础上,起始COD质量浓度为430 mg·L-1、色度为1 500倍的废水,在反应条件:t=30℃,pH为3.5,ρ(H2O2)=1 665 mg·L-1,c(Fe2+)/c(H2O2)=0.072,反应时间3 h的情况下,Fenton氧化处理后,COD和色度的去除率分别高达87.5%和94.4%.研究发现,色度的去除率要优于有机物(以COD计)的去除率,且受外界因素影响小.GC-MS分析结果表明:经过Fenton处理后,废水中的发色团和助色团基本上完全被去除.中间产物主要是脂类衍生物,副产品有1-碘十三烷和正辛基醚等.     

Determination of 4-tert-octylphenol in surface water samples of Jinan in China by solid phase extraction coupled with GC-MS

Octylphenols, considered as xenoestrogens, mainly exist as 4-tert-octylphenol (OP) in aquatic environments. The high stability and accumulation of OP in aquatic systems have caused endocrine disruption. The OP in surface water in Jinan, China was analyzed by gas chromatography-mass spectrometry (GC-MS) coupled with solid phase extraction (SPE). Water samples were extracted by SPE on a cartridge system containing C-18 as sorbent. To increase sensitivity and selectivity, OP was derivatized to 4-tert-octyl-phenoxy silane. With the use of phenanthrene-d10 as internal standard, the detection limit based on signal-to-noise ratio (S/N = 3) was 0.06 ng/mL. The average recovery was from 84.67% to 109.7%. The precision of the method given as the relative standard deviations (RSD) was within the range 6.24%-12.96%. In the target water samples, the concentrations of OP were as follows: 15.88-71.24 ng/L for Jinxiuchuan Reservoir, 3.850-26.68 ng/L for the city moat, 6.930-41.56 ng/L for Daming Lake, 66.03-474.2 ng/L for Xiaoqing River, 14.66-17.72 ng/L for the Yellow River, and 10.60-26.43 ng/L for Queshan Reservoir. The Xiaoqing River was seriously polluted due to the discharge of wastewater from Jinan. Jinxiuchuan Reservoir had a higher concentration of OP compared with the Yellow River and Queshan Reservoir, which is ascribed to the surrounding human activities. These data are reported for the first time, providing strong support for the control of OP pollution in Jinan.     

2-丁烯醛生产废水中溶解性有机物的分级解析

采用超滤膜法将2-丁烯醛生产废水中的有机物分为相对分子质量不同的7个级分,并应用溶解性有机碳(dissolved organic carbon,DOC)、紫外吸收光谱(ultraviolet spectrum,UV)、傅里叶变换红外光谱(fourier transform infrared spectrometer,FT-IR)和气相色谱/质谱联用仪(gas chromatography with mass spectrometry,GC-MS)技术对不同相对分子质量区间的有机物所占比例及物质结构进行了研究.结果表明,废水中相对分子质量1×103的有机物所占比例最高,达到88.57%;采用GCMS对废水中相对分子质量1×103的级分进行分析,定性出27种化合物,包含醛、酮、酯、醇、酚、酸、烷烃类及其他苯系物等,其峰面积占有机物峰面积总和的比例分别为6.9%、5.3%、35.4%、13.2%、4.6%、0.4%、1.7%、16.8%,总和为84%.UV和FT-IR分析结果均显示不同相对分子质量区间的光谱吸收特征没有明显差别,级分中存在含有不饱和双键、羟基、羰基化合物及芳香族化合物,与GC-MS检测结果相吻合.研究结果为废水处理工艺的开发与优化提供了重要的指导作用.