液相色谱法测定土壤中苯并(a)芘

用快速溶剂萃取法ASE300对土壤样品进行前处理,以配有荧光检测器的高效液相色谱仪分析土壤样品中苯并(a)芘的含量,该方法以乙腈、水梯度比例混合作为流动相,流速为1.0 ml/min;激发波长和发射波长分别为255 nm和420 nm;保留时间为27.58 min。样品的称样量为25 g时,测定检出限为8.28×10-5mg/kg,相对标准偏差(RSD)为1.0%~12%,回收率为60%~87%,以上指标均能满足环境中土壤样品的检测要求。     

沥青烟中苯并(a)芘的等速采样与监测

新的大气污染综合排放标准对沥青及碳素制品生产和加工制定了沥青烟和苯并(a)芘的排放标准,然而空气和废气监测分析方法没有给出沥青烟气中苯并(a)芘的分析方法.为此,用色谱固定液滤筒及新设计的富集器等速采样,进行沥青烟苯并(a)芘的分析,为执行新的大气污染综合排放标准提供了实用技术.     

燃煤电厂烟气降温过程中多环芳烃分布特征

分别以燃用褐煤与烟煤无烟煤的2个电厂为例,研究2个电厂烟气降温过程中多环芳烃的分布及转化特征。研究表明,萘、菲、苯并[a]蒽和苯并[a]芘4种多环芳烃在烟气降温过程中呈过渡分子状态,在适当的条件下,存在相互转化的可能性;萘、菲、苯并[a]蒽和苯并[a]芘在不同的电厂随飞灰粒径变化所表现出来的吸附特性不同,颗粒的粒度影响多环芳烃的形成与吸附。在烟气降温过程中飞灰表面吸附的萘、菲、苯并[a]蒽和苯并[a]芘含量随着飞灰粒径的变小呈现出逐渐增加的趋势。     

高效液相色谱法测定饮用水中苯并[a]芘

本文采用高效液相色谱-荧光检测器法，用反相C18柱，在乙腈：水（V／V）=90：10作为流动相，检测波长：λEx=265nm，λEm=410nm，流速为1．5mL／min的条件下对饮用水中苯并[a]芘进行了方法学考查，本方法对苯并[a]芘的线性相关系数等于0．9998，RSD为1．46％，平均回收率为93．1％，方法操作简便、准确可靠、灵敏度较高。     

超高效液相色谱测定地表水中超痕量苯并(a)芘及其前处理干扰研究

本研究采用液液萃取-超高效液相色谱仪接荧光检测器测定地表水中超痕量的苯并(a)芘,仪器检出限为0.005ng/m L,水样分析方法检测限为0.05ng/L,可对地表水中超痕量的苯并(a)芘实现定量检测。通过验证试验发现在实验室分析水样时,二氯甲烷等萃取溶剂中含有少量的苯并(a)芘是导致空白干扰的主要因素,溶剂经蒸馏提纯后可排除干扰。     

燃煤锅炉烟道气中苯并(a)芘的研究

本文选择中小型燃煤锅炉为对象,建立适合于这一类锅炉烟道气中苯并(a)芘(B(a)P)的采样分析方法,研究了影响烟气B(a)P浓度的因素,得出了 炉型及燃烧条件与烟气B(a)P含量的关系实验结果说明,目前国内大量使用的中小锅炉排放的B(a)P对大气的污染是严重的,应予以注意。     

隧道路面沥青摊铺过程空气中TSP和多环芳烃污染研究

分析了隧道沥青摊铺过程环境空气中的TSP及多环芳烃质量浓度。TSP用膜法,中流量采样器采样15 min,重量法分析;超声波萃取,高效液相色法分析多环芳烃。结果表明,摊铺机周围空气中TSP超过8 mg/m3,道路空气中TSP超过3 mg/m3;环境空气中苊烯等12种多环芳烃均有检出,苊烯和艹屈质量浓度较高,苯并[a]芘和二苯并[a,h]蒽质量浓度较低。苯并[a]蒽、苯并[a]芘和二苯并[a,h]蒽超标,对人体健康危害较大。建议加强相关行业PAHs的排放水平及其健康风险研究,制定相关限值标准和沥青摊铺过程环境空气的沥青烟监测方法标准。     

某大型化工企业周边居民区积尘中多环芳烃调查及健康风险评价

以江苏省某大型化工企业周边居民区为研究区域,调查企业主导风的下风向2 km范围内的居民区以及对照区积尘中多环芳烃(PAHs)含量,对16种PAHs污染分布和特征进行研究,并评估积尘PAHs通过暴露途径对人群健康风险。结果表明:居民区积尘中16种PAHs全部检出,污染区∑PAHs均值为2 294μg/kg,明显高于对照区145μg/kg;污染区7个测点中有6个测点苯并(a)芘出现超标,超标倍数为0. 17～2. 5倍;所测的16种PAHs化合物中蒽、荧蒽、芘、、苯并(b)荧蒽、苯并(k)荧蒽、苯并(a)芘浓度相对较高;通过PAHs主成分分析和特征比值判断,不完全燃烧源对积尘中PAHs贡献率达77. 4%,污染区PAHs来源呈现石油燃烧、煤燃烧以及石油源的复合污染特征,对照区PAHs主要来源为煤的不完全燃烧;以苯并(a)芘毒性等效浓度进行风险评估,污染区致癌风险值明显高于对照区,儿童摄入PAHs风险总体高于成人;对照区儿童和成人致癌风险均小于1×10~(-6),不存在致癌风险;污染区儿童和成人平均致癌风险值分别为3. 95×10~(-6)、2. 65×10~(-6),在可接受范围内,但存在潜在致癌风险。     

马鞍山市大气环境中苯并(a)芘分布与变化规律研究

研究了马鞍山市大气环境中苯并（a）芘的分布与变化规律，监测了马鞍山市各功能区，新老市区的居民区及交通要道大气环境中苯并（a）芘的含量，该市功能区内的工业区大气中苯并（a）芘污染严重，最高质量浓度达50．31ng/m^3，居民区内老市大气中的苯并（a）芘污染明显高于新市区，究其原因，老市区是马鞍山，市工业发源地，属居民，商业及工业混合区，研究中发现，大气中苯并（a）芘含量高低有季节性的昼夜变化现象，时空分布和迁移变化规律明显，并且大气中总悬浮颗粒物与苯并（a)芘的相关性显著。     

不同粒径空气颗粒物中11种多环芳烃的分析测定

将五段多孔冲击分级器 (粒径分级 :≤ 1 .1 ,1 .1～ 2 .0 ,2 .0～ 3 .3 ,3 .3～ 7.0 ,≥ 7.0μm)与大流量采样器连接 ,采集呼和浩特市冬夏两季空气颗粒物样品 ,用高压液相色谱仪 (HPLC)测定样品中的蒽 (An)、菲 (Ph)、萤蒽 (Fl)、芘 (Py)、(Ch)、苯并 [a]蒽 (Ba A)、苯并 [a]芘 (Ba P)、二甲基苯并 [a]蒽 (DMBa A)、二苯并 [ah]蒽 (DBah A)、苯并 [ghi] (Bghi P)和晕苯 (Cor)等 1 1种多环芳烃化合物 (PAHs)。数据表明 :呼和浩特市空气颗粒物中 PAHs的浓度较高 ;有约 97%的 PAHs富集于可吸入颗粒中。     

Apportionment of the airborne PM10 in Spain. Episodes of potential negative impact for human health

The particulate matter with an aerodynamic diameter less than or equal to 10 and 2.5 microns respectively (PM10 and PM2.5) constitutes one of the main air pollutants, which is currently regulated in Europe through Directive 2008/50/EC due to its proven harmful effects on human health. In this paper, the airborne PM10 samples collected in Zaragoza city during 2001-2009 were apportioned by statistical tools based on principal component analysis with absolute principal component scores (PCA-APCS). PM10 samples were characterized regarding their concentrations of polycyclic aromatic hydrocarbons (PAH) and water-soluble ions. PAH were analyzed by gas chromatography-mass spectrometry-mass spectrometry detection (GC-MS-MS) and ions were analyzed by ion chromatography. A total of five factors were identified by PCA-APCS corresponding to different anthropogenic and natural sources. This work was focused on analyzing in more detail those samples involving higher negative impact on human health, in particular, PM10 samples exceeding the daily PM10 limit value of 50 μg m(-3) according to Directive 2008/50/EC and samples with concentrations of benzo[a]pyrene (BaP) higher than the upper assessment threshold (BaP > 0.6 ng m(-3)) established by the Directive 2004/107/EC. Most of the exceedances of the daily PM10 limit value were associated with direct and indirect North-African long-range transport. During these exceedances, it was observed that anthropogenic pollution sources slightly decreased with regard to the natural sources. This indicated that episodes of high PM10 could have a natural origin associated with long-range transport from the African continent. On the contrary, those exceedances with regional contribution and samples with BaP concentrations higher than 0.6 ng m(-3) showed an important contribution of anthropogenic pollution sources increasing their negative impact on human health.     

Measurements of polycyclic aromatic hydrocarbons at an industrial site in India

Polycyclic Aromatic Hydrocarbon (PAH) concentrations were measured in Total Suspended Particulate Matter (TSPM) from December 2005 to August 2006 at Nunhai, an industrial site in Agra (India). Particulate matter samples were collected on glass fibre filters using High Volume Sampler (HVS-430) and were extracted using dichloromethane with ultrasonication and analyzed by GC. Total PAH concentration varies between 0.04 to 2.5 microg m(-3) accounting only 1.6 x 10(-3)% of TSPM. The mass distribution in air was dominated by high molecular weight DbA, BghiP, BaP, BkF and IP. Combustion PAH (CPAH) except BeP represents 58% of the total PAH mass and IARC classified total carcinogenic PAH accounting 63% of TPAH concentration. Correlation studies between PAH revealed the contribution of low molecular weight PAH was mainly due to primary emission from diesel exhaust while high molecular weight PAH were formed during combustion. The presence of specific tracers and calculation of characteristic molecular diagnostic ratios Fla/(Fla + Pyr), BaP/(BaP + Chy), BaA/(BaA + Chy), IP/(IP + BghiP), BaP/BghiP and IP/BghiP) were used to identify the sources of the emissions of PAHs in the atmospheric samples. Seasonal variation in atmospheric PAH showed four fold increase in winter concentration than summer. The BaP and relative BaP amount calculated from the measurements suggested that photo-oxidation may also be responsible for the variation in PAH concentrations during winter and summer. Seasonal trends in atmospheric PAH concentration in the study area were influenced by fossil fuel usage for domestic heating, boundary height and temperature.     

Diffusive sampling of methyl isocyanate using 4-nitro-7-piperazinobenzo-2-oxa-1,3-diazole (NBDPZ) as derivatizing agent

A diffusive sampling method for the determination of methyl isocyanate (MIC) in air is introduced. MIC is collected using a glass fiber filter impregnated with 4-nitro-7-piperazinobenzo-2-oxa-1,3-diazole (NBDPZ). The urea derivative formed is desorbed from the filter with acetonitrile and analyzed by means of high-performance liquid chromatography (HPLC) using fluorescence detection (FLD) with lambdaex = 471 nm and lambdaex = 540 nm. Additionally, a method was developed using tandem mass spectrometric (MS-MS) detection, which was performed as selected reaction monitoring (SRM) on the transition [MIC-NBDPZ + H]+ (m/z 307) to [NBDPZ + H]+ (m/z 250). The diffusive sampler was tested with MIC concentrations between 1 and 35 microg m(-3). The sampling periods varied from 15 min to 8 h, and the relative humidity (RH) was set from 20% up to 80%. The sampling rate for all 15 min experiments was determined to be 15.0 mL min(-1) (using HPLC-FLD) with a relative standard deviation of 9.9% for 56 experiments. At 80% RH, only 15 min sampling gave acceptable results. Further experiments revealed that humidity did not affect the MIC derivative but the reagent on the filter prior to and during sampling. The sampling rate for all experiments (including long term sampling) performed at 20% RH was found to be 15.0 mL min(-1) with a relative standard deviation of 6.3% (N = 42). The limit of quantification was 3 microg m(-3) (LC-MS-MS: 1.3 microg m(-3)) for 15 min sampling periods and 0.2 microg m(-3) (LC-MS-MS: 0.15 microg m(-3)) for 8 h sampling runs applying fluorescence detection.     

鞍山市城区采暖期大气PM_(2.5)中PAHs的污染特征研究

通过对鞍山市(1个工业区、2个工业区周边、3个居住区、1个对照点)2015年1月采暖期大气PM_(2.5)中多环芳烃(PAHs)的监测,采用BaP当量致毒系数TEF,分析了鞍山市大气PM_(2.5)中典型PAHs毒性当量分布特征。研究表明,鞍山市大气PM2.5中工业区及工业区周边Ba P毒性当量浓度要远高于居住区和对照点,污染物主要由4~6环的PAHs组成,很强致癌BaP当量浓度为9.351~38.59 ng/m3。     

A diffusive sampling device for the determination of formaldehyde in air using N-methyl-4-hydrazino-7-nitrobenzofurazan (MNBDH) as reagent

A new method utilizing the diffusive sampling of formaldehyde in air has been developed. Formaldehyde is sampled with the use of a glass fiber filter impregnated with N-methyl-4-hydrazino-7-nitrobenzofurazan (MNBDH) and phosphoric acid. The formaldehyde hydrazone formed is desorbed from the filter with acetonitrile and determined by high-performance liquid chromatography (HPLC) with UV/visible detection at 474 nm. The sampling rate was determined to be 24.7 mL min-1 with a relative standard deviation of 7% for 48 experiments. The measured sampling rates were not dependent on the formaldehyde concentration (0.1-1.0 mg m-3), sampling time (15-482 min) or relative humidity (20-85%). The detection limit was 70 micrograms m-3 for a 15 min sampling period and 2 micrograms m-3 for an 8 h sampling period.     

Polycyclic Aromatic Hydrocarbons: Need for Assessment of Health Risks in India? Study of An Urban-Industrial Location in India

This paper reports the PAHs levels in the atmosphere of an urbanised industrial site of India. A high-resolution capillary gas chromatograph with a mass spectrometric detector (HRCGC-MS) and a high performance liquid chromatograph (HPLC) equipped with a fluorescence detector were used for the identification and quantitation of PAHs. The atmospheric levels of PAHs were higher (4.66 ng/m³ yearly average) than most of the concentrations previously reported in the literature. Indian sites were found more contaminated with potently carcinogenic: four and above ringed PAHs. Based on a good correlation between the levels of lead, vanadium, BaP and BghiP, the vehicular emission appears to be a major source of the PAHs. Further, the higher levels of observed PAHs could be attributed to the vertical distribution of the aerosols, the preference of the PAHs for the particulate phase and the greater availability of the substrate in the atmosphere for their sorption. This paper also discusses the need for development of a PAHs monitoring protocol and related health effect studies in developing countries such as India.     

Benzo(a)pyrene induced structural and functional modifications in lung cystatin

Cystatins are thiol proteinase inhibitors ubiquitously present in the mammalian body. They serve a protective function to regulate the activities of endogenous proteinases, which may cause uncontrolled proteolysis and damage. In the present study, the effect of benzo(a)pyrene [BaP] on lung cystatin was studied to explore the hazardous effects of environmental pollutant on structural and functional integrity of the protein. The basic binding interaction was studied by UV-absorption, FT-IR, and fluorescence spectroscopy. The enhancement of total protein fluorescence with a red shift of 5 nm suggests structural scratch of lung cystatin by benzo(a)pyrene. Further, ANS binding studies reaffirm the unfolding of the thiol protease inhibitor (GLC-I) after treating with benzo(a)pyrene. The results of FT-IR spectroscopy reflect perturbation of the secondary conformation (alpha-helix to β-sheet) in goat lung cystatin on interaction with BaP. Finally, functional inactivation of cystatin on association with BaP was checked by its papain inhibitory activity. Benzo(a)pyrene (10 μM) caused complete inactivation of goat lung cystatin. Benzo(a)pyrene-induced loss of structure and function in the thiol protease inhibitor could provide a caution for lung injury caused by the pollutants and smokers.     

超高效液相色谱法测定土壤中微量阿特拉津

采用超高效液相色谱仪,建立了土壤中微量阿特拉津的快速检测方法。研究结果表明:采用反相C18色谱柱,以甲醇/水(70∶30,v/v)为流动相,流速为0.2 ml/min,柱温为30℃,检测波长为220 nm条件下,在12.5~1000μg/L质量浓度范围内线性关系良好(r=0.9999),检出限0.18×10^-3 mg/kg,加标回收率为69.0%~94.8%,相对标准偏差为2.5%~8.0%,该方法具有灵敏度高、重复性好、简便、快速、干扰小、精密度高的特点,可用于土壤中阿特拉津的快速检测。     

化学吸收法采集固定污染源氨气的影响因素探究

固定污染源氨气的手工监测，干扰因素较多，其中采样环节尤为关键。实验通过催化氧化-化学发光法考察不同采样管线材质对氨气的吸附效果，离子色谱法考察化学吸收法采集氨气的吸收瓶类型、采样流量、吸收液种类、吸收液浓度及体积等采样条件对氨气吸收效率的影响。实验表明，316 L不锈钢与聚四氟乙烯对氨气的吸附较小，氨气的采样流量不宜超过1.0 L/min,棕色气泡式吸收瓶更适用于氨气样品的采集，磷酸溶液作吸收液对氨气的吸收效率较好，对于低浓度的氨气样品，应采用低流量长时间采集。