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31.
地下水中半挥发性有机污染物痕量分析的5个问题探讨   总被引:1,自引:1,他引:0  
魏峰  陈海英  沈小明  吕爱娟 《岩矿测试》2012,31(6):1043-1049
针对地下水中有机氯农药、多氯联苯和多环芳烃等半挥发性有机污染物的痕量分析,从实验室分析测试人员的角度,探讨了提高定量分析准确度的三个问题:分级绘制标准曲线、注重标准溶液配制细节、避免假阳性与假阴性.从实验室管理人员的角度探讨了提高实验室竞争力的两个问题:提高服务质量和降低分析成本.本文对这几个重要但往往易被忽视的问题进行逐一分析,并探讨了分级绘制标准曲线的方法、配制标准溶液应考虑的要点、避免假阳性与假阴性的措施,以及提高服务质量和降低成本的因素.  相似文献   
32.
狄氏剂与多氯联苯均是海洋环境中毒性大、难降解的有机污染物,建立海水中狄氏剂与多氯联苯快速、灵敏、准确的检测方法,具有重要意义。本文采用聚苯乙烯/二乙烯基苯(Cleanert PS)固相萃取柱对海水样品中的狄氏剂与7种多氯联苯进行分离富集,建立了气相色谱-电子捕获检测器(GC-μECD)的分析方法。实验了萃取流速、洗脱液、水样盐度与pH等实验条件对萃取效率的影响,确定样品以5.0 mL/min的流速经Cleanert PS固相萃取柱富集,真空抽干后用5.0 mL丙酮洗脱,挥干洗脱液,用1.0 mL正己烷定容,在选定的色谱条件下进行分析。方法精密度(RSD)为0.9%~4.4%,与《海洋监测规范》GB 17378.4—2007的RSD指标相比,精密度良好;加标回收率为82.1%~123.9%。狄氏剂的检出限(0.0088 μg/L)低于文献的检出限(0.05 μg/L),7种多氯联苯的检出限(0.0012~0.0067 μg/L)低于文献的检出限(0.147~0.289 μg/L)。该方法适合于海水中痕量狄氏剂与多氯联苯的快速分析,具有一定的实用价值。  相似文献   
33.
试验了加速溶剂萃取土壤中有机氯农药和多氯联苯残留的最佳条件。结果表明,采用正己烷-丙酮混合溶剂(体积比1:1)为提取剂,萃取温度100℃,压力为10.3MPa;采用弗罗里硅土固相萃取柱对样品净化,毛细管柱分离,用配有电子捕获检测器的气相色谱进行检测,平均加标回收率为83.6%~109.0%,相对标准偏差(RSD,n=11)为1.11%~5.88%,检出限为0.69~1.85ng/g。方法简单、快捷、经济,适应于土壤中的有机氯农药和多氯联苯的测定。  相似文献   
34.
Plastic pellets found stranded on beaches are hydrophobic organic materials and thus, they are a favourable medium for persistent organic pollutants to absorb to. In the present study, plastic pellets are used to determine the diffuse pollution of selected Greek beaches. Samples of pellets were taken from these beaches and were analyzed for PCBs, DDTs, HCHs, and PAHs. The observed differences among pellets from various sampling sites are related to the pollution occurring at each site. Plastic pellets collected in Saronikos Gulf beaches demonstrate much higher pollutant loading than the ones collected in a remote island or close to an agricultural area. Based on data collected in this study and the International Pellet Watch program, pollution in Saronikos Gulf, Greece, is comparable to other heavily industrialized places of the world. The present study demonstrates the potential of pellet watch to be utilized as a detailed-scale monitoring tool within a single country.  相似文献   
35.
Information on temporal distribution of polychlorinated biphenyls (PCBs) in the coastal sediments of Mediterranean Sea, Mersin was compiled using data published between 1980 and 2009, and the present study. The first congener specific PCB results from the region yield concentration levels of Σ41PCBs in sediments ranging from 0.61 to 1.04 ng g−1. Sediment profiles show penta-, hexa- and hepta-chlorobiphenyls, specifically, #149 and 153 as the most abundant congeners in all samples. Comparison of total PCB concentrations over time suggests no recent PCB input to the region. Using congener specific PCB data for the region, identity and contribution of PCB sources were also predicted using a chemical mass balance -based (CMB) receptor model. The CMB model identified Aroclor 1260 to be the major PCB source in coastal sediments. The potential sources for the PCBs were briefly discussed in terms of their use in various industrial applications.  相似文献   
36.
In this study, the distribution and partition of polybrominateddiphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs) in water from the Pearl River Estuary were investigated. A seasonal dependence for dissolved and particle phase PCB and PBDE levels was observed. A high dissolved phase level occurred in the dry season. The positive correlation between POC content in the particles and phase distribution coefficients (Kp) suggested that POC may play an important role in determining the partition of PBDEs and PCBs. A linear correlation between the observed log KOC and log KOW for PBDEs and PCBs was found with slopes less than one. The observed log KOC values were lower than the predicted log KOC values for PBDEs (except for BDE28). The log KOC values were higher than the predicted values for PCBs. A combination of sorption to colloids (10-98% for PBDEs and less than 25% for PCBs) and adsorption to BC was responsible for this observation.  相似文献   
37.
The influence of the sediment’s physico-chemical properties and black carbon content, on the distribution of polycyclic aromatic hydrocarbons and polychlorinated biphenyls in benthic sediments of the Gulf of Gdansk (Baltic Sea) was determined. Sediments from port, marine dump site of dredged spoils, the Vistula river mouth, Gdansk Deep were selected.The concentrations of ∑PAHs (fluoranthene, pyrene, benzo(a)anthracene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(ah)anthracene, benzo(ghi)perylene) were 294-2200 ng/g d.w. and for ∑PCBs (28, 52, 101, 118, 138, 153, 180) were 2.4-11.3 ng/g d.w.The sediments content of loss on ignition was 1.13-16.15%, total organic carbon was 0.89-7.15%, black carbon was 0.20-1.15%. The highest correlation coefficient values (r = 0.76-0.92, p < 0.05) for a relationship between the concentrations of organic pollutants, and organic matter, organic and black carbon contents were obtained in harbor sediments with low content of organic matter (<5%) and high share of black carbon in total carbon (up to 40%).  相似文献   
38.
研究了海洋沉积物提取液中28种多氯联苯(PCBs)、16种多环芳烃(PAHs)和21种有机氯农药(OCPs)在硅胶-氧化铝复合净化柱上的同时净化与分离效果,结果表明:在充填4 cm3%去活化氧化铝-6 cm 3%去活化硅胶的8 mm i.d×15 cm固相萃取净化柱上,使用10 mL正己烷作为淋洗PCBs的分割点,可实现PCBs、PAHs和OCPs的满意分离,更有利于PCBs与高环数PAHs、极性较强OCPs的分离。继续用20 mL正己烷-二氯甲烷混合液(体积比1∶1)洗脱,28 PCBs、16种PAHs和21种OCPs均可获得有效回收,回收率分别为75%~110%、76%~115%、75%~130%。经海洋沉积物标准参考物质验证,该方法实用、可靠,流程简单,试剂消耗少,成本低,适用于海洋环境地质调查中基质复杂沉积物样品的定量分析。  相似文献   
39.
建立了沉积物样品中17种有机氯农药和8种多氯联苯持久性有机污染物的气相色谱分析方法。针对沉积物样品基质复杂、含有大量硫干扰的特点,重点研究了前处理技术。采用加速溶剂提取(ASE)技术提取样品中的有机污染物,比较了加入铜粉后ASE在线除硫和超声波提取除硫的效果。结果表明,加入铜粉ASE提取不能完全去除硫的干扰,需进一步采用超声波提取10 min除硫才能大大减少杂质对目标化合物的干扰。沉积物样品中的色素类及小分子干扰物质采用凝胶渗透色谱结合固相萃取技术进行净化,满足了气相色谱-电子捕获检测器分析的要求。25种化合物的平均添加回收率为68%~131%,方法精密度(RSD,n=6)小于22.3%,检出限为0.10~0.51μg/kg。建立的样品前处理技术净化彻底,适合用于不同地区、不同类型的沉积物样品气相色谱分析。  相似文献   
40.
对食品中有机氯农药和多氯联苯的气相色谱-质谱联用(GC-MS)分析方法中三种离子化方式,电子轰击电离(EI)、正化学电离(PCI)和负化学电离(NCI)进行了总结和比较。PCI-MS/MS方法和EI-MS/MS方法都有很高的选择性和较高的灵敏度;PCI方法在分析含硝基、羰基等基团的化合物时有明显优势,EI则在分析狄氏剂、异狄氏剂、硫丹及其代谢物时比PCI表现稍好,而NCI-MS的灵敏度最高,但抗干扰能力稍弱,且不适合分析滴滴涕类和多氯联苯类化合物。在食品安全分析中,三种质谱方法的准确性好,精密度高,检测限较低,都能够满足食品中农残检测的要求,在日常检测工作中可互为补充和替代。同时指出,GC在有机氯化合物分析中仍表现出明显的优越性;常规的GC-MS尤其在EI电离模式下,易受到基质干扰而使谱图变得复杂;新型离子化方式包括高选择性化学电离技术的应用,将是食品安全中GC-MS联用分析的发展方向之一。  相似文献   
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