自动索氏提取-气相色谱-质谱法测定电子电气产品材料中多氯联苯

本文建立了采用自动索氏提取-气相色谱-质谱联用检测电子电气产品中多氯联苯的方法。通过以丙酮-正己烷(1+1)为溶剂,自动索氏提取材料中多氯联苯,用硅胶柱净化,气相色谱-质谱联用仪检测,该方法检测限在0.1mg/kg,加标回收率在60%～99%之间,相对标准偏差(RSDs)小于6%,线性范围在0.4mg/L～250mg/L,相关系数(r)大于0.999。实验结果表明,该方法简便、可靠,能满足电子电气产品材料中多氯联苯的检测要求。     

超声波萃取-气相色谱-质谱法同时测定土壤中16种多环芳烃和18种多氯联苯

建立超声波萃取结合气相色谱-质谱法(GC-MS)同时分析土壤中16种多环芳烃(PAHs)和18种多氯联苯(PCBs)的方法,并比较不同萃取方式、超声萃取时间和萃取次数等对加标回收率的影响.得到最佳检测方法为10.0 g样品用20 mL的正己烷和丙酮混合液(体积比1:1)超声波萃取15 min,萃取4次,萃取液经过浓缩、...     

索氏提取-气相色谱三重四极杆串联质谱联用法测定空气中的多环芳烃

建立了索氏抽提前处理,气相色谱-三重四极杆串联质谱法测定空气中15种多环芳烃。该法的液体检出限为0.008~0.071μg/m L,空白基体加标的相对标准偏差范围为1.1%~9.3%,平均回收率为89.4%~113%;将其运用到实际样品分析中,并与GC-MS法结果进行了比对。结果表明,该法选择性高,精密度好,适用于空气中多环芳烃的检测。     

电子制冷浓缩-气相色谱-质谱法测定废气中挥发性有机物

用化学惰性优良的氟聚合物薄膜气袋采集固定污染源废气样品,经电子制冷冷冻浓缩、热解析后,进入气相色谱分离,用质谱检测器进行检测,根据保留时间、质谱图或特征离子定性,外标法定量测定废气中挥发性有机物。方法检出限为0.10nmol/mol,实验相对标准偏差范围在2.01%—7.89%,相对误差范围在0.2%—14.0%,同时具有较高的回收率。     

气相色谱-质谱法测定洋葱中129种农药残留

建立了组合柱固相萃取-气相色谱-质谱法快速测定洋葱中129种农药残留的分析方法。样品用乙腈均质提取,盐析分配,提取液经C18和PSA组合柱固相萃取净化后供气相色谱-质谱仪(GC-MS)分析。采用选择离子扫描方式,外标法定量。该方法简便、快速,通过优化前处理和上机条件,在最优条件下进行测试,方法的定量下限(S/N≥10)为0.01~0.1 mg/kg,在加标水平为0.1 mg/kg时,方法回收率为63.2%~113.1%,相对标准偏差为5.3%~14.4%。     

质谱法分析清洁柴油中的多环芳烃

采用质谱法分析符台欧Ⅲ标准的清洁柴油中的多环芳烃,确定了操作条件。柴油试样预分离后,蒸发溶剂的温度控制在50℃。除去溶剂的液体先用丙酮稀释,然后使用直接进样杆进样．一级真在时间定为3S。     

气相色谱-质谱法测定皮革中对苯二胺含量

采用气相色谱一质谱法测定皮革中的对苯二胺含量。通过对色谱参数、提取方式、提取温度、提取时间、提取次数等条件的优化,建立了皮革中对苯二胺含量的检测方法。对苯二胺标准曲线线性范围为0.1～5.0 mg/L,相关系数为0.9996,检出限为1.22 mg/kg,平均回收率为86.4%～108.2%,相对标准偏差(RSDs,n=6)为3.52%～7.48%。     

气相色谱-质谱法测定土壤中苯胺的方法确认研究

研究了气相色谱-质谱法测定土壤中苯胺的非标方法确认过程.通过三家实验室间的比对得出:苯胺的检出限为0.02mg/kg～0.03mg/kg,测定下限为0.08mg/kg～0.12mg/kg,三家实验室分别对加标浓度为0.25mg/kg、0.50mg/kg和1.0mg/kg的样品进行测定,实验室内相对标准偏差为2.5％～9...     

气相色谱质谱法测定电子电器产品中十溴二苯醚含量的不确定度评估

气相色谱质谱法（GC-MS）测定电子电器产品中多溴二苯醚含量是目前最常用的方法,但对于检测过程的不确定度分析还不多见,本文以十溴二苯醚（DecaBDE）为例,根据《化学分析中不确定度的评估指南》和《测量不确定度评定与表示》对气相色谱质谱法测定电子电器产品的多溴二苯醚的检测结果进行了不确定度分析。     

高效液相色谱荧光法测定土壤中16种多环芳烃

本文介绍了采用高效液相色谱、荧光检测器测定土壤中16种多环芳烃。通过对液相色谱柱的选择、色谱条件、荧光激发和发射波长等条件的优化,实现16种多环芳烃完全分离。特别是对16种多环芳烃的激发和发射波长进行选择,进一步提高检测灵敏度、选择性,降低了干扰。在优化的实验条件下,荧光检测器的检出限为0.09～1.57ng/mL,样品加标回收率为86%-108%。     

色谱-质谱联机测定厦门港和员当湖表层沉积物中的石油烃和多环芳香烃的含量

2002年4月厦门港沿岸设九个站,员当湖设两个站采集表层积物,用有机溶剂萃取,硅胶柱色层分离,气相色谱-质谱联机带SIM数据采集系统对样品的石油烃类(M/Z=55),多环芳香烃类(15个典型的多环芳香烃,9个甲基化多环芳香烃作外标)进行分析,结果显示员当湖石油烃和多环芳香浓度分别高达1397微克/克(干)和1376.5纳克/克(干)。厦门港沉积物石油烃和多环芳香浓度范围为:石油烃133.3～943.3微克/克(干)多环芳香烃97.6～308.5纳克/克(干)。厦门港船只活动,厦门港四周工业废水、车辆燃油滴漏是石油烃污染的主要来源。厦门工业用煤、用油、生活用煤及船只、车辆燃料泄漏是沉积物多环芳香烃的主要来源,其工业排废、生活废水排放,市区雨水冲刷和大气灰尘沉降是多环芳香烃进入海湾的主要途径。     

Pollution patterns of polycyclic aromatic hydrocarbons in tobacco smoke

Concentrations of polycyclic aromatic hydrocarbons (PAHs) in tobacco smoke of 12 commercial brand cigarettes were determined in a simulated chamber of 20.25 m3 in size. The total concentrations of 17 PAHs (summation operatorPAHs) in the chamber were 3500 and 1152 ng/m3 in vapor phase and particulate phase, respectively. In vapor phase, the yield of naphthalene (NA) appeared to be the most abundant (2462 ng/cig) followed by fluorene (FLUOR) and acenaphthylene (ACY), while the yield of benzo[ghi]perylene (BP) was the most abundant (259.7 ng/cig) in particulate phase followed by phenanthrene (PHEN) and FLUOR. The proportion of PAHs in particulate phase increased with increasing molecular weight. PAHs with two to six rings accounted for 40.2%, 35.3%, 11.7%, 7.6%, 5.2% of summation operatorPAHs, respectively. There was no obvious correlation between PAHs, benzo[a]pyrene (BaP) concentrations in tobacco smoke and smoking tar contents, nicotine contents. With the source fingerprint of PAHs in tobacco smoke, NA could be regarded as the marker of tobacco smoke source because of its largest contribution to summation operatorPAHs (40.2%), followed by FLUOR (12.7%) and ACY (9.8%). Further study indicated that more than 80% of BaP in indoor air of resident homes in Hangzhou was from tobacco smoke.     

Source identification and health risk of polycyclic aromatic hydrocarbons associated with electronic dismantling in Guiyu town, South China

In this study the concentrations and distribution of sixteen polycyclic aromatic hydrocarbons (PAHs) were investigated in gas and total suspended particle (TSP) samples collected during daytime and night time. The sampling locations included an electronic waste dismantling workshop (EW), a plastic recycling workshop (PW) and a waste incineration field (WF) in Guiyu, China. A large residential area (RA) in this region was used as a control site. In the daytime, the highest concentration was found at WF (1041 ng m⁻³); while in the night time the highest concentration was found outside of EW (744 ng m⁻³). Comparison between work hours (daytime) and rest hours (night time) displayed that the total PAHs (gas + particulate phase) concentrations and the percentages of PAHs associated with TSP were higher at night than those in the daytime in all sampling workshops except WF. Source diagnostic-ratio analysis revealed that unwanted materials and smoldering honeycomb coals were the main sources of PAHs in EW, WF and PW. Benzo[a]pyrene equivalent [BaPeq] concentrations calculated by using the toxic equivalent factors [TEFs] suggested that the occupational exposure levels were not significantly high when compared with other occupational exposure. Additionally, our study suggested that the smoldering of unwanted materials could produce much more toxic PAHs compounds.     

静态顶空GC-MS法测定三种不同性状化妆品中的甲醛

建立了三种不同性状化妆品中甲醛的快速、准确的检测方法。采用静态顶空结合GC-MS法,水剂、乳液、膏状物化妆品平衡温度分别为50、60、70℃,平衡时间为15 min。结果表明,甲醛浓度在10~200 mg/kg范围内,线性相关性良好(r=0.9996)。三个浓度系列测定结果的相对标准偏差为1.02%~1.42%,回收率为85.5%~104.2%,方法最低检出浓度为1.25 mg/kg。     

The influence of baking fuel on residues of polycyclic aromatic hydrocarbons and heavy metals in bread

The influence of fuel type used to bake bread on the spectrum and concentrations of some polycyclic aromatic hydrocarbons and heavy metals in baked bread was assessed. Bread samples were collected from different bakeries operated by either electricity, solar, mazot or solid waste and their residue content of PAHs and heavy metals was assessed. The total concentration of PAHs detected in mazot, solar, solid waste and electricity operated bakeries had an average of 320.6, 158.4, 317.3 and 25.5 μg kg⁻¹, respectively. Samples collected from mazot, solar and solid waste operated bakeries have had a wide spectrum of PAHs, in comparison to that detected in bread samples collected from electricity operated bakeries. Lead had the highest concentrations in the four group of bread samples, followed by nickel, while the concentrations of zinc and cadmium were the least. The concentration of lead detected in bread samples produced from mazot, solar, solid waste and electricity fueled bakeries were 1375.5, 1114, 1234, and 257.3 μg kg⁻¹, respectively. Estimated daily intake of PAHs based on bread consumption were 48.2, 28.5, 80.1, and 4.8 μg per person per day for bread produced in bakeries using mazot, solar, solid waste and electricity, respectively. Meanwhile, the estimated daily intake of benzo (a) pyrene were 3.69, 2.65, 8.1, and 0.81 μg per person per day for bread sample baked with mazot, solar, solid waste and electricity, respectively. The daily intake of lead, based on bread consumption was 291, 200.5, 222, and 46.31 μg per person per day for bread sample baked with mazot, solar, solid waste and electricity, respectively. The present work has indicated the comparatively high level of daily intake of benzo (a) pyrene and lead in comparison to levels reported from many other countries and those recommended by international regulatory bodies. It is probable that residues detected in bread samples are partially cereal-borne but there is strong evidence that the process of baking and the gases emitted are responsible for most of the contamination load.     

Direct photolysis of polycyclic aromatic hydrocarbons in drinking water sources

The widely used low pressure lamps were tested in terms of their efficiency to degrade polycyclic aromatic hydrocarbons listed as priority pollutants by the European Water Framework Directive and the U.S. Environmental Protection Agency, in water matrices with very different compositions (laboratory grade water, groundwater, and surface water). Using a UV fluence of 1500 mJ/cm², anthracene and benzo(a)pyrene were efficiently degraded, with much higher percent removals obtained when present in groundwater (83-93%) compared to surface water (36-48%). The removal percentages obtained for fluoranthene were lower and ranged from 13 to 54% in the different water matrices tested. Several parameters that influence the direct photolysis of polycyclic aromatic hydrocarbons were determined and their photolysis by-products were identified by mass spectrometry. The formation of photolysis by-products was found to be highly dependent on the source waters tested.     

Degradation of polycyclic aromatic hydrocarbons by the Chilean white-rot fungus Anthracophyllum discolor

The degradation of three- and four-ring polycyclic aromatic hydrocarbons (PAHs) in Kirk medium by Anthracophyllum discolor, a white-rot fungus isolated from the forest of southern Chile, was evaluated. In addition, the removal efficiency of three-, four- and five-ring PAHs in contaminated soil bioaugmented with A. discolor in the absence and presence of indigenous soil microorganisms was investigated. Production of lignin-degrading enzymes and PAH mineralization in the soil were also determined. A. discolor was able to degrade PAHs in Kirk medium with the highest removal occurring in a PAH mixture, suggesting synergistic effects between PAHs or possible cometabolism. A high removal capability for phenanthrene (62%), anthracene (73%), fluoranthene (54%), pyrene (60%) and benzo(a)pyrene (75%) was observed in autoclaved soil inoculated with A. discolor in the absence of indigenous microorganisms, associated with the production of manganese peroxidase (MnP). The metabolites found in the PAH degradation were anthraquinone, phthalic acid, 4-hydroxy-9-fluorenone, 9-fluorenone and 4,5-dihydropyrene. A. discolor was able to mineralize 9% of the phenanthrene. In non-autoclaved soil, the inoculation with A. discolor did not improve the removal efficiency of PAHs. Suitable conditions must be found to promote a successful fungal bioaugmentation in non-autoclaved soils.     

Accumulation of polycyclic aromatic hydrocarbons and heavy metals in lettuce grown in the soils contaminated with long-term wastewater irrigation

Accumulation of polycyclic aromatic hydrocarbons (PAHs) and heavy metals (HMs) by crop plants from contaminated soils may pose health risks. A greenhouse pot experiment using lettuce (Lactuca satuva L.) as a representative vegetable was conducted to assess the concentrations of PAHs and HMs in vegetables grown in wastewater-contaminated soils. The concentrations of total PAHs were ranged from 1.5 to 3.4 mg kg(-1) in the contaminated soils, while 1.2 mg kg(-1) in the reference soil. Linear regression analyses showed that the relationships between soil and shoot PAH concentrations were stronger for LMW-PAHs (R(2) between 0.51 and 0.92) than for HMW-PAHs (R(2) 0.02 and 0.60), suggesting that translocation for LMW-PAHs is faster than HMW-PAHs. Furthermore, the data imply that root uptake was the main pathway for HMW-PAHs accumulation. The plant shoots were also highly contaminated with HMs, particularly Cd (0.4-0.9 mg kg(-1)), Cr (3.4-4.1 mg kg(-1)), Ni (11.7-15.1 mg kg(-1)) and Pb (2.3-5.3 mg kg(-1)), and exceed the guidance limits set by State Environmental Protection Administration (SEPA), China and the World Health Organization (WHO). This study highlights the potential health risks associated with cultivation and consumption of leafy vegetables on wastewater-contaminated soils.