多氯联苯的气相色谱/质谱/质谱(GC/MS/MS)法测定

采用气相色谱/质谱/质谱(GC/MS/MS)法测定多氯联苯(PCB),具有良好的灵敏度和选择性,在地表水样品检测时,样品只须进行简单的液液萃取-浓缩,不须任何净化过程即可上机分析,方法检出限低于ng/L级。     

垃圾填埋场渗出液中有害成分的研究

研究垃圾填埋场渗出液中的有害成分。渗出液样品用适当的方法处理后 ,用气相色谱 -质谱联用方法和原子发射光谱法进行定性分析。然后用原子吸收分光光度法和反相高效液相色谱法定量测定样品中微量的 Cu、Zn、Pb、Cr、Cd、Hg、苯酚、对甲苯酚、萘、蒽     

洹河水中痕量有机污染物的研究

采用固相萃取技术 ,对洹河水中痕量有机物进行富集 ,大量的地表水被 C1 8键合相萃取后 ,洗脱液经干燥浓缩用于 GC和 GC/MS分析 ,鉴定出 64种有机物 ,并对苯系物、杂环类等 2 7种主要污染物作了定量测定 ,得出有机物的沿途变化规律。     

吹扫捕集气相色谱质谱法测定土壤中挥发性有机物

建立了吹扫捕集气相色谱质谱法同时测定土壤中卤代烃类、苯系物类、氯代苯类等二十多种挥发性有机物.使用模拟土壤和实际土壤样品优化了吹扫时间、吹扫温度等参数;采用内标法绘制了校正曲线,各目标化合物5个浓度水平的响应因子的相对标准偏差均小于20%,相关系数均大于0.999;测定了方法检出限,采用2g土壤,各目标化合物方法检出限界于0.02～1.00μg/kg;对两种总有机碳含量的实际土壤样品进行了加标回收实验,回收率范围64%～123%.     

Determination of particulate polycyclic aromatic hydrocarbons in ambient air by gas chromatography-mass spectrometry after molecularly imprinted polymer extraction

A solid phase extraction procedure (SPE) is described for the quantitative analysis of polycyclic aromatic hydrocarbons (PAHs) in atmospheric particulate matter (PM), as ubiquitous environmental pollutants routinely measured in air quality monitoring. A SPE cartridge was used based on a molecular imprinted polymer (MIP-SPE) properly tailored for selective retention of PAHs with 4 and more benzene fused rings. The performance of the clean-up procedure was evaluated with the specific concern of selective purification towards saturated hydrocarbons, which are the PM components mostly interfering GC analysis of target PAHs. Under optimized operative conditions, the MIP-SPE provided analyte recovery close to 95% for heavier PAHs, from benzo(α)pyrene to benzo(ghi)perylene, and close to 90% for four benzene rings PAHs, with good reproducibility (RSDs: 2.5%-5.9%). Otherwise, C₁₇-C₃₂ n-alkanes were nearly completely removed. The proposed method was critically compared with Solid Phase Micro Extraction (SPME) using a polyacrylate fiber. Both methods were successfully applied to the analysis of ambient PM_2.5 samples collected at an urban polluted site. Between the two procedures, the MIP-SPE provided the highest recovery (R% ≥ 93%) for PAHs with 5 and more benzene rings, but lower for lighter PAHs. In contrast, SPME showed a mean acceptable R% value (∼ 80%) for all the investigated PAHs, except for the heaviest PAHs in the most polluted samples (R%: 110%-138%), suggesting an incomplete purification from the interfering n-hydrocarbons.     

气提式三重循环生物膜反应器处理制药废水中的甾体雌激素

为验证气提式三重循环生物膜反应器处理甾体雌激素的效能,建立了一套SPE/HPLC/MS/MS分析方法,对反应器进、出水中的甾体雌激素--甾酮(E1),17β-雌二醇(E2),雌三醇(E3)以及17α-乙炔基雌二醇(EE2)进行检测.该方法的加标回收率为88%～103%,精密度为4%～9%.该方法对E1,E2,E3和EE2的进水定量限(LOQ)分别为0.7,0.8,0.9和0.5 ng/L;对出水的定量限分别为2.0,1.0,2.0和 1.0 ng/L.CODCr和氨氮容积负荷最高为7.5和1.6 kg/(m3·d),出水依然能够保持稳定.进水pH稳定在9.0～10.5,而反应器的pH一直稳定在9.0以下,体系对pH变化造成的冲击比较适应.同时,反应器内形成了稳定的NO2--N积累,CODCr和氨氮的去除率分别达到了70%和73%.     

电感耦合等离子体-质谱法研究大气颗粒物中元素浓度

1　IntroductionAirborneparticulatematterisoneoftheimportantmarkersofairqualityandisanimportanthealthconcerninurbanareas,especiallywithrespecttoanumberofchronicrespiratorydiseases.Medicaldatasuggeststhatitisthisfractionofparticulatematterthatbecomesdeeplyi…     

Arsenic tissue concentration of immature mice one hour after oral exposure to gold mine tailings

A potentially high bioavailability of arsenic in gold mine tailings from a site in northern California has been suggested by solubility studies. To help address this issue, an in vivo dosing study was conducted using 12dayold Swiss Webster mouse pups (n=8/group). A sample of sizefractionated mine tailings from the site (<20m particle size, 691g g^–1 arsenic) was prepared as an aqueous suspension and administered by gavage in a volume that provided 4mg As/kg body weight. The control group received the same volume of a commercial soil (1g g^–1 As) of similar particle size (<60m). No mortality or toxic signs were noted in either group. Tissue samples were collected 1h after gavage, freezedried, microwavedigested and analysed for arsenic by ICP/MS (detection limit 2ng As g^–1 dry weight). Arsenic concentrations (ng As g^–1 dry weight) in tissues from the pups who received mine tailings were significantly higher than in control tissues. The mean elevation in arsenic concentration was highest in the liver (3364% of control, p<0.0001), followed by blood (818 of control, p<0.0001), skin (207% of control, p=0.07), and brain (143% of control, p<0.0001). The carcass arsenic concentration (excluding the GI tract, liver, brain and skin) was 138 of control (p=0.02). The data indicate uptake of arsenic from weathered mine tailings by the immature mouse pups after oral exposure.     

微区有机质激光热解GC/MS新技术及其应用

微区有机质激光热解GC/MS是国际上近年来发展起来的新分析技术。它利用激光的高相干性和高平行性准确地聚焦于有机质表面某个微小区域内 ,使之发生热降解而产生能反映有机质化学组成和结构的分子级产物 ,借助GC/MS系统进行分离和鉴定。这一新技术为生油岩和煤中单个显微有机组分的研究开辟了一条途径 ,在生油岩评价、油气源对比和油藏地球化学研究中有广泛的应用前景。     

Advanced analytical determination of volatile organic compounds (VOC) and other major contaminants in water samples using GC-Ion Trap MS

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