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固相萃取与气相色谱-质谱联用测定水中痕量多环芳烃 总被引:3,自引:0,他引:3
采用固相萃取与气相色谱-质谱联用测定水中痕量多环芳烃(PAHs)。通过正交试验,得到最佳固相萃取条件为:上样流速为5mL/min、采用二氯甲烷洗脱、洗脱剂用量为3mL、洗脱流速为2mL/min。测定结果显示,固相萃取与气相色谱—质谱联用技术对萘、菲、荧蒽3种PAHs的检出限为0.03~0.07μg/L,加标回收率为70%~100%,相对标准偏差为3.90%~9.58%。该方法精密度高、准确度好,能满足实际水样中痕量PAHs的测定要求。 相似文献
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先利用C-18固相萃取小柱富集大港油田港东联合处理站污水处理站的采油废水中16种多环芳烃(PAHs,即萘、苊烯、苊、芴、菲、蒽、荧蒽、芘、、苯并[a]蒽、苯并[b]荧蒽、苯并[k]荧蒽、苯并[a]芘、茚并[1,2,3-cd]芘、二苯并[a,h]蒽和苯并[g,h,i]苝),再用气相色谱/质谱(GC/MS)分析测定其浓度,以评价PAHs的去除率和生态风险。结果表明:(1)采油废水经处理后,COD、石油类去除率分别达到82.27%、91.06%;外排水COD、石油类达到《污水综合排放标准》(GB 8978—1996)一级标准要求,优于中国采油废水处理的一般水平。(2)采油废水主要以2、3环的PAHs为主,约占总量的93%以上。(3)苯并[a]芘超过《地表水环境质量标准》(GB 3838—2002)中限值。(4)处理前的采油废水中蒽、菲和苯并[a]芘具有一定的生态风险;处理后的外排水中萘、蒽、菲、荧蒽、苯并[a]芘的暴露浓度(PEC)/预测无效应浓度(PNEC)均小于1,目前尚未对环境造成威胁。但是8种PAHs(苊烯和苯并类PAHs除外)总和表现出较大的毒性,需要引起重视。 相似文献
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针对亟待解决的石油开采废水中的多环芳烃(polycyclic aromatic hydrocarbons, PAHs)污染物的生物毒害性问题,利用紫外光辐照g-C3N4/TiO2复合薄膜光催化剂,对取自内蒙某采油现场的采出水水样进行降解处理,研究多组分PAHs污染物共存条件下的不同环数PAHs发生光催化氧化反应的降解规律及降解动力学。采用扫描电子显微镜(scanning electron microscope, SEM)表征光催化剂表面微观形貌,采用固相微萃取法富集和萃取水样中的PAHs,采用气相色谱-质谱联用法(gas chromatography-mass spectrometry, GC-MS)检测分析PAHs含量。经UV/g-C3N4/TiO2光催化反应处理,采出水中不溶的颗粒态萘优先于溶解态萘被降解去除,经60 min后对萘的总去除率可达61.13%。大于4环不溶性高环PAHs,可被优先光催化降解,从而高毒性的PAHs污染物被逐级转化为相对较低生物毒性的苊烯、蒽、菲、萘等,其中苊烯的含量增长最显著。结论石油采出水的外排处理工艺中增加PAHs光催化脱毒工艺具有一定可行性,对于保障原有水厂中的生化工艺段高效率、稳定运行将极具价值。 相似文献
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污水处理厂各工艺阶段多环芳烃变化规律研究 总被引:5,自引:0,他引:5
采用固相萃取-气相色谱/氢火焰离子化检测器联用技术(SPE-GC/FID),对西安市某污水处理厂不同工艺段水体中的16种多环芳烃(PAHs)含量进行了长期监测。结果表明,原水中有13种PAHs检出,按浓度从大到小排序分别为:萘、菲、芴、芘、艹屈、二氢苊、苊、蒽、苯并(a)蒽、荧蒽、苯并(b)荧蒽、苯并(k)荧蒽、苯并(a)芘;原水中PAHs的总量在477.1~3 067.7 ng/L之间,平均值为1 833.1 ng/L,同国内外报道的结果相比,可认为西安市生活污水中PAHs的含量处于中等水平;二级处理工艺对PAHs有较好的去除效果,平均去除率为79%,其中,生物处理单元的贡献最大,去除率达到68%。 相似文献
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利用PUF被动采样器于2008年8月—2009年7月采集了西安大气样品,研究了大气气相中多环芳烃(PAHs)的含量和季节分布特征。结果表明,西安大气气相中16种美国EPA优控的PAHs(Σ16PAHs)质量浓度为10.9-489.6 ng/m3(平均为143.4 ng/m3),四季具有明显的季节差异,依次为夏季(62.5 ng/m3)〈春季(80.1 ng/m3)〈秋季(175.8 ng/m3)〈冬季(255.2 ng/m3)。气相中PAHs主要以3-4环为主,占总量的86.5%-94.1%。利用主成分分析法判断四季气相中PAHs的污染来源类型,主要为燃煤和机动车尾气及生物质燃烧的复合源。 相似文献
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Broad range analysis of endocrine disruptors and pharmaceuticals using gas chromatography and liquid chromatography tandem mass spectrometry 总被引:3,自引:0,他引:3
Endocrine disrupting compounds (EDCs) and pharmaceuticals and personal care products (PPCPs) have been globally detected in impacted natural waters. The detection of trace quantities of EDCs and PPCPs in the environment is of great concern since some of these compounds have known physiological responses at low concentrations. EDCs can have a wide range of polarities, acidic and basic moieties, and exist in trace quantities, which often requires numerous complex extractions, large sample collection volumes, and multiple instrumental analyses. A comprehensive method has been developed allowing for the analysis of 58 potential EDCs in various water matrices using a single solid-phase extraction (SPE) of a 1 L sample with subsequent analyses using both gas chromatography and liquid chromatography, each coupled with tandem mass spectrometry (GC–MS/MS and LC–MS/MS). Instrument detection limits ranged between 0.12–7.5 pg with corresponding method reporting limits of 1–10 ng l−1 in water. Recoveries for most compounds were between 50% and 112% with good reproducibility (RSD 6–22%). 相似文献
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Honoria Kwok Jeffrey Yan Pamela Brunswick Mark McMaster Marlene Evans Marcus Kim 《Environmental Forensics》2020,21(1):87-98
AbstractA saponification extraction method with gas chromatography pseudo-MRM (pMRM) mass spectrometry detection was developed for the determination of 50 total polycyclic aromatic hydrocarbons (TPAH50, a combination of parent and alkylated homologues) in biota. The method was aimed at monitoring and identification of potential TPAH contaminants in bitumen impacted environments. Alkylated PAHs were determined by multi-level, quantitative calibration using parent PAHs. The developed and thoroughly validated method required only one injection for TPAH50 analysis which represents significant saving of time and expensive authentic alkylated standards. The current method was tested with certified reference mussel tissue NIST 1974c and performed well. In a comparison study, the method reached a limit of quantitation (LOQ) for the TPAH50 between 0.1 and 0.2?ng g?1, while the QuEChERs enhanced matrix removal – lipid (EMR) kit produced by Agilent showed an LOQ of 5–10?ng g?1. The current method relied on response factors (RF) for the quantitation of alkylated PAHs determined against parent PAHs. These RFs were shown to be stable and consistent over the course of 1 year, during which over 200 routine environmental biota monitoring samples were analyzed. The environmental biota monitoring samples analyzed include muscle, carcass and liver, with an average total PAH50 concentration of 13, 90 and 135?ng g?1, respectively. Results show significant differences in the distributions of 1 ringed, 2 ringed, 3 ringed, 4 ringed, and 5+ ringed TPAHs between the types of biota samples. 相似文献
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Distribution of polycyclic aromatic hydrocarbons in agricultural soils in South Korea 总被引:32,自引:0,他引:32
The content and type of polycyclic aromatic hydrocarbons (PAH) in soils from paddy fields and upland areas in South Korea were determined using gas chromatography linked to mass spectrometry (GC–MS). The distribution map of total PAH content was obtained as a contour plot using a geographical information system. The overall distribution of PAH was found to be closely related to the pollution sources, the size of city and the type of industry. The average content of total PAH in all samples was 236 μg kg−1, and the range was from 23.3 to 2834 μg kg−1. The highest concentrations were found in soils sampled near iron processing plants. The concentration of PAH decreased in the order fluoroanthene>benzo(b)fluoroanthene>pyrene. Special PAH compound ratios, such as phenanthrene/anthracene and fluoroanthene/pyrene, were calculated to evaluate the origin. The collected data suggested that the pyrogenic origins such as motor vehicle exhaust and heavy industry emission were the dominant source of PAH in Korean soils. 相似文献
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Artur Ciemniak Agata Witczak Kamila Mocek 《Journal of environmental science and health. Part. B》2013,48(11):993-998
The aim of this study was to assess honey contamination by polycyclic aromatic hydrocarbons. Six species of honey were examined, as well as rape blossom and soil from villages P?czerzyno and Przybys?aw in West Pomerania, Poland. The instrumental analysis was performed using a HP 6890 gas chromatograph coupled to a HP 5973 mass spectrometer with selected ion monitoring (SIM). Quantification was done by gas chromatography-mass spectrometry (GC-MS) using perdeuterated internal standards. Both soil samples showed high levels of all 23 PAHs, whereas honey contained mostly non-carcinogenic PAHs of low molecular weight. The most contaminated honey from P?czerzyno contained 0.24 μg kg-1 benzo[a]pyrene. Moreover, despite low contamination of honey, a positive correlation was found between PAH content in honey, blossom and soil. 相似文献
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建立了活性污泥中多溴联苯醚(PBDEs)的分析方法。活性污泥经超声波辅助萃取,用酸性硅胶、铜粉及复合硅胶柱纯化后,采用气质联用色谱(GC/MS)对7种PBDEs单体进行测定,内标法定量。结果表明,该方法具有很好的精密性和准确性,方法检测限为17~121 pg/g,加标回收率为84.5%~109.0%,相对标准偏差(RSD)为0.5%~2.8%,回收率指示物3,3’,4,4’-四溴联苯醚(BDE-77)的回收率平均值为89.2%,RSD为0.8%,能够满足活性污泥中PBDEs的测定要求。采用所建立的方法对杭州和台州的活性污泥样品进行了测定,结果显示,台州样品中PBDEs含量高于杭州样品,但两者都低于相关文献所报道的北美及欧洲国家活性污泥中PBDEs的含量。 相似文献