北京市大气气溶胶PM2.5中极性有机化合物的测定

提出了用GC-MS分析大气细粒子中极性有机化合物的测定方法,给出了2类衍生化反应的最佳条件.标准物质工作曲线相关系数在0.995～1.000之间,仪器精密度为1%～10%,标准物质的标准偏差为3%～20%,实际样品的标准偏差为3%～17%,仪器定量限为0.1～4.0 ng·μL^-1.实测了北京市夏、秋、冬3季大气细粒子样品,定量极性有机化合物42种,其中一元羧酸30种、二元羧酸5种、无水单糖3种、甾醇类3种和苯甲酸,并对这些化合物的可能来源进行了探讨.     

滨海城市大气中多氯联苯的污染特征

选取滨海城市厦门的城区、郊区、工业区和背景区为研究对象,于2008年10月至2009年9月对厦门市大气进行了为期四个季节的采样工作,用GC-MS对气相和颗粒相中的28种多氯联苯(PCBs)同系物进行测定。研究结果表明,厦门市PCBs具有明显的时空分布特征,PCBs的含量在66.94～689.59 pg/m3之间,平均值...     

亚甲基兰分光光度法测定气态硫化氢方法研究

对气态污染物H2S测定方法亚甲基兰分光光度法进行了深入细致地探索研究,得出该方法最佳实验室测定条件,包括标准溶液和吸收溶液的选择,显色剂和样品的稳定时间,SO2、NOx对测定方法的影响以及样品的吸收效率等。实验结果表明,该方法校准曲线斜率为0.148～0.151吸光度/μgH2S·11mL,标准偏差1.2×10\+-3,环境监测样品回收率为84%～89%。     

兰州市大气OPAHs污染特征及潜在来源分析

对兰州市冬季（2016-12-01~07）和夏季（2017-08-03~10）大气气相和颗粒相（PM_1.0、PM_2.5和PM₁₀）中含氧多环芳烃（OPAHs）进行观测,结果显示：Σ₈OPAHs （气相+颗粒相）的浓度范围为1.83~19.28ng/m³,平均浓度为（6.45±3.43） ng/m³.冬季是夏季的2.06倍.冬季颗粒相OPAHs在2.5~10和<1.0μm粒径段均具有较大占比,而夏季则主要赋存于PM_1.0中.9-芴酮（9-FLU）、9,10-蒽醌（9,10-ANT）和苯并蒽酮（BZA）为OPAHs中最主要的几种单体物质,其占比为51.8%~94.9%.气粒分配机制研究结果表明：OPAHs在气粒两相间的分配以吸收机制为主导.基于浓度权重轨迹分析法（CWT）对兰州市大气中OPAHs的潜在污染源区进行了分析,发现其潜在污染源区在冬季主要位于当地及其西北方向位于新疆和青海境内的部分地区,而夏季则主要位于该研究区域的东南方向（定西市、天水市等）和东北方向（宁夏回族自治区中卫市）.     

西安市大气中多溴联苯醚的季节变化特征及人体暴露评估

利用大流量主动采样器于2008年8月至2009年7月采集了西安城区气态和颗粒态大气样品,研究了大气中多溴联苯醚(PBDEs)的季节变化特征.结果表明,西安大气中总PBDEs(气相+颗粒相)浓度范围为21.38~161.84pg/m3,平均值为66.34pg/m3.大气中PBDEs在冬季污染最严重,颗粒相PBDEs季节变化趋势与总悬浮颗粒(TSP)较为相似,气相PBDEs的季节变化没有颗粒相明显.对PBDEs的总浓度、气相浓度、颗粒相浓度与采样期间气象因素做偏相关分析,发现总浓度和颗粒相浓度均与气压呈显著正相关,与温度呈显著负相关,表明西安大气中PBDEs浓度主要受气压和温度的影响.对西安普通人群的PBDEs吸入暴露量进行计算,并采用BDE-99的吸入量进行人体暴露评估,西安普通儿童和成人对BDE-99总摄入量低于De Winter-Sorkina提出的最大允许摄入量260pg/(kg·d).     

气相色谱-三重串联四极杆质谱法测定海洋沉积物中35种多环芳烃

研究建立了气相色谱-三重串联四极杆质谱测定海洋沉积物中多环芳烃的方法,采用同位素稀释法对海洋沉积物中35种多环芳烃进行了测定,并与气相色谱质谱方法的检测参数进行比较。结果表明,该方法的仪器检出限和定量限均优于气相色谱质谱法,并具有更好的灵敏度和选择性;35种多环芳烃的加标回收率范围为71%~105%,16种同位素替代内标平均回收率范围为55%~101%;实验选取辽东湾表层海洋沉积物的实际样品进行测定,沉积物平行样品相对标准偏差为2.2%~4.5%,样品中多环芳烃单体组分含量在0.25×10-9（干重）~30.1×10-9（干重）之间。     

Kinetic and thermodynamic behaviour of volatile ammonium compounds in industrial and marine atmospheres

Measurements of volatile ammonium aerosol compounds and respective acidic and basic gaseous precursors were taken at an industrial site emitting HCl, HNO₃ and NH₃ and at a marine suburban location.Because of fresh industrial emissions the gaseous acid and base concentration products show values orders of magnitude higher than thermodynamic equilibrium previsions, at the industrial site. To our knowledge these are the first published field measurements that strongly confirm that gas-particle equilibrium conditions are not attained instantaneously in the atmosphere and that kinetic constraints play an important role on gas-particle conversion for ammonium chloride and ammonium nitrate compounds. The results permit to conclude that, for temperature conditions lower than 15°C, transformation rates are not high, several minutes being necessary, at least, for the equilibrium between gaseous precursors and ammonium particulate products to be reached.At the marine suburban location a diurnal variation was observed for gaseous and particulate compounds in agreement with known emission and transformation mechanisms. The behaviour of nitric and hydrochloric acids in the marine atmosphere can be better explained if kinetic limitations are considered for the reaction of HNO₃ with NaCl aerosol particles and for the transference of acids and ammonia to the particulate phase.     

煤化工废水中硝基苯胺类污染物的HPLC测定

通过试验建立了工业废水中苯胺类污染物的液相色谱测定方法,优化了试验条件.该方法吸收值与基质质量浓度之间的线性关系非常显著,苯胺和6种硝基苯胺类成分的检出限在0.000 1～0.000 3 mg/L之间,空白加标试验的相对标准偏差(RSD)在1.8％～4.8％之间,基质加标回收率在58.6％～93.8％之间.对煤化工园排...     

北京市石景山区夏季雨水和大气中PCBs的特征解析

利用气相色谱-质谱联用技术(GC-MS)对北京市石景山城区夏季雨水和大气中多氯联苯(PCBs)的分布特征进行了解析.结果表明,雨水中主要为溶解态PCBs,比例高达65.23%.大气中的PCBs以气态为主,占67.70%.研究表明,雨水对大气中颗粒态和气态PCBs的清除系数相当,分别为6.00×104和5.37×104.8种类二 PCBs同类物的毒性当量总和在大气气相、颗粒相和雨水中分别为0.36pg/m3、0.02pg/m3和0.29ng/L.北京石景山地区8种类二 PCBs同类物对成人呼吸暴露值为0.08pg/(kg·d),说明北京石景山地区人群呼吸暴露风险比较低.     

Pollution level and distribution of PCDD/PCDF congeners between vapor phase and particulate phase in winter air of Dalian,China

In December 2009, ambient air was sampled with active high-volume air samplers at two sites: on the roof of the No. l building of Dalian Jiaotong University and on the roof of the building of Dalian Meteorological Observatory. The concentrations and the congeners between vapor phase and particulate phase of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) in the air were measured. Sample analysis results showed that the concentrations of PCDD/Fs in particulate phase was higher than that in gaseous phase. The ratio of PCDD to PCDF in gaseous phase and particulate phase was lower than 0.4 in all samples. The total I-TEQ value in gaseous phase and particulate phase was 5.5 and 453.8 fg/m³ at Dalian Jiaotong University, 16.6 and 462.1 fg/m³ at Dalian Meteorological Observatory, respectively. The I-TEQ value of Dalian atmosphere was 5.5-462.1 fg/m³ which was lower than international standard, the atmospheric quality in Dalian is better.     

戊唑醇残留分析方法实验室内质量控制研究

文章确立了小麦、香蕉中戊唑醇残留检测方法,小麦样品加水10 mL用丙酮为萃取溶剂,石油醚液液分配,中性氧化铝柱层析净化,用气相色谱(GC-NPD)检测。香蕉样品加水5 mL用丙酮为萃取溶剂,石油醚液液分配,浓缩后用气相色谱(GC-NPD)检测。分别设置不同时间批次,同一批次间的平行样及实验室内人员分析,分别从方法灵敏度、方法准确度、方法精密度及其质量控制图、标准工作液的稳定性来探讨该方法的可靠性,结果表明该方法可以作为香蕉和小麦种戊唑醇残留检测的标准分析方法。     

西安市大气棕碳污染特性及发色团种类

为探究西安市大气棕碳（BrC）的光学特性及化学组成,利用大气颗粒物采样器和吸附剂同时采集了颗粒相和气相大气样品,并运用紫外-可见分光光度计和三维荧光光度计测定了样品中BrC的吸光和荧光特性,基于平行因子分析（PARAFAC）法解析三维荧光光谱得到BrC的种类和组成信息.结果表明,在波长为365 nm时,颗粒相和气相BrC的吸光度分别为（13.8±7.9）Mm^-1和（8.0±3.1）Mm^-1,两者占比分别为63%和37%.本研究并未发现气相和颗粒相BrC吸光度之间有显著的相关性.PARAFAC结果表明,西安市大气BrC含有类腐殖质发色团、类酚类发色团和类蛋白发色团,而它们分别在气相和颗粒相BrC中的占比是不同的,类腐殖质发色团和类蛋白发色团在颗粒相中分布较多,分别为41%和36%,而气相中主要包含酚类发色团,其占比为78%.本研究结果揭示了气相BrC也可能是贡献大气正辐射强迫的重要因子,以及参与大气光化学反应的重要大气组分,将来的研究需要给予足够重视和关注.     

Emission factors of polycyclic aromatic hydrocarbons from domestic coal combustion in China

Domestic coal stove is widely used in China, especially for countryside during heating period of winter, and polycyclic aromatic hydrocarbons （PAHs） are important in flue gas of the stove. By using dilution tunnel system, samples of both gaseous and particulate phases from domestic coal combustion were collected and 18 PAH species were analyzed by GC-MS. The average emission factors of total 18 PAH species was 171.73 mg/kg, ranging from 140.75 to 229.11 mg/kg for bituminous coals, while was 93.98 mg/kg, ranging from 58.48 to 129.47 mg/kg for anthracite coals. PAHs in gaseous phases occupied 95% of the total of PAHs emission of coal combustion. In particulate phase, 3-ring and 4- ring PAHs were the main components, accounting for 80% of the total particulate PAHs. The total toxicity potency evaluated by benzo[a]pyrene-equivalent carcinogenic power, sum of 7 carcinogenic PAH components and 2,3,7,8-tetrachlorodibenzodioxin had a similar tendency. And as a result, the toxic potential of bituminous coal was higher than that of anthracite coal. Efficient emission control should be conducted to reduce PAH emissions in order to protect ecosystem and human health.     

2019—2020年天津市津南区多环芳烃和有机磷阻燃剂气固分配特征及健康风险评价

多环芳烃(PAHs)及有机磷阻燃剂(OPEs)种类繁多且具有易挥发性,通过气固分配行为完成气态和颗粒态的转化. 为准确评估天津市津南区PAHs、OPEs和各组分气固分配行为及风险评价,选择16种PAHs及7种OPEs作为研究对象,利用色谱质谱联用技术测定2019—2020年天津市津南区大气环境中的PAHs和OPEs浓度水平,利用气固分配实测及预测模型研究PAHs及OPEs分配行为,并通过健康风险评价模型对其健康风险进行评估. 结果表明:①天津市津南区2019—2020年∑G-PAHs (气态PAHs总和)年均浓度为36.7 ng/m3,PM_2.5中∑P-PAHs (颗粒态PAHs总和)年均浓度为7.3 ng/m3;∑G-OPEs (气态OPEs总和)年均浓度为5 142.0 pg/m3,PM_2.5中∑P-OPEs (颗粒态OPEs总和)年均浓度为2 752.0 pg/m3. ②研究期间,PAHs气固分配机制受吸收和吸附机制共同影响,低分子量、高分子量PAHs分别受吸附机制、吸收机制影响,而OPEs则主要受有机物吸收机制影响. ③颗粒态的2~3环PAHs、4环PAHs和5~6环PAHs的非致癌风险值占比分别为0.01%~8%、1%~31%和62%~98%,颗粒态的2~3环PAHs、4环PAHs和5~6环PAHs的致癌风险值占比分别为0.2%~1.5%、3%~71%和70%~99%,颗粒态的TNBP (磷酸三丁酯)、TCEP〔三-(β-氯乙基)磷酸酯〕、TCPP〔三(异氯丙基)磷酸盐〕、TPHP (磷酸三苯酯)和TDCPP〔三(1,3 -二氯异丙基)磷酸盐〕的非致癌风险值占比分别为36% (范围为10%~58%)、40% (范围为11%~72%)、45% (范围为13%~67%)、51% (范围为38%~75%)和49% (范围为37%~60%). 研究显示,OPEs的健康风险远低于PAHs,气态OPEs和颗粒态PAHs对人体健康的影响较显著.      

ICP-AES法测定大气颗粒物中的金属

采用微孔滤膜采集大气颗粒物中的铬、铜、铅、锰、锌、镍、铁 ,消解后使用电感耦合等离子体发射光谱法测定。在选定的最佳条件下测铬、铜、铅、锰、锌、镍、铁的检出限分别为 5 .3、7.3、3.4、2 .9、4.2、13.9、7.8ng· m L - 1 ,回收率为 98.4%～ 10 5 .7% ,RSD为 0 .48%～ 2 .2 7%。该法准确、快速、简便 ,应用于大气颗粒物的测定 ,结果满意。     

PM2.5中类腐殖质表面活性测定方法与实例分析

建立了大气细粒子中类腐殖质（HULIS）表面活性的动态表征方法,并以华北平原乡村站点冬季大气PM_2.5样品为例,对PM_2.5中HULIS的表面活性进行表征.HULIS碳质组分（HULIS-C）浓度为2.0~4.6μg C/m³,占水溶性有机碳和总有机碳的比例分别为31%~40%和20%~26%.浓度为88~200mg C/L的HULIS水溶液,其表面张力相对于纯水降低了18%~22%.HULIS-C浓度在低于70mg C/L时表面张力降低显著,在88~320mg C/L之间降低相对缓慢.动态表面张力随着时间变化逐渐降低,在液滴形成后200s以内表面张力下降迅速,之后趋于平缓,说明表面活性分子在液滴中扩散趋于稳定需要一定的时间,该特征时间可能影响表面活性物质在云凝结核活化时的作用.证实了在污染地区的大气PM_2.5中含有一定量的表面活性物质,这些物质可能对颗粒物活化为云滴、雾滴过程产生显著影响;表面活性物质的存在可能在外界湿度变化过程中导致颗粒物发生液-液相分离现象,在颗粒物表面形成有机膜,影响活性分子摄取以及半挥发性物质的气-粒分配过程,从而影响大气非均相反应过程.     

Simultaneous preconcentration of cadmium and lead in water samples with silica gel and determination by flame atomic absorption spectrometry

A new method that utilizes pretreated silica gel as an adsorbent has been developed for simultaneous preconcentration of trace Cd(II) and Pb(II) prior to the measurement by flame atomic absorption spectrometry. The effects of pH, the shaking time, the elution condition and the coexisting ions on the separation/preconcentration conditions of analytes were investigated. Under optimized conditions, the static adsorption capacity of Cd(II) and Pb(II) were 45.5 and 27.1mg/g, the relative standard deviations were 3.2% and 1.7% (for n = 11), and the limits of detection obtained were 4.25 and 0.60 ng/mL, respectively. The method was validated by analyzing the certified reference materials GBW 07304a (stream sediment) and successfully applied to the analysis of various treated wastewater samples with satisfactory results.     

Determination of arsenic in air particulates and diesel exhaust particulates by spectrophotometry

A method was developed for the determination of trace arsenic by spectrophotometry. The proposed method is rapid, simple,and inexpensive. This method can be used for sensitive determination of trace arsenic in environmental samples and especially in air particulates. The results obtained by this method as a proposed method were compared with those obtained by hydride generation atomic absorption spectrometry as a popular reported method for the determination of arsenic and an excellent agreement was found between them. The method was also used for determination of arsenic associated with airborne particulate matter and diesel exhaust particulates.The results showed that considerable amount of arsenic are associated with diesel engine particulates. The variation in concentration of arsenic was also investigated. The atmospheric concentration of arsenic was different in different sampling stations was dependent to the traffic density.     

Polychlorinated biphenyls in the atmosphere of Taizhou, a major e-waste dismantling area in China

PM2.5,total suspended particles(TSP) and gas phase samples were collected at two sites of Taizhou,a major e-waste dismantling area in China.Concentrations,seasonal variations,congener profiles,gas-particle partitioning and size distribution of the atmospheric polychlorinated biphenyls(PCBs) were studied to assess the current state of atmospheric PCBs after the phase out of massive historical dismantling of PCBs containing e-wastes.The average 38PCBs concentration in the ambient air(TSP plus gas phase) near the e-waste dismantling area was(12,407 ± 9592) pg/m3 in winter,which was substantially lower than that found one decade ago.However,the atmospheric PCBs level near the e-waste dismantling area was 54 times of the reference urban site,indicating that the impact of the historical dismantling of PCBs containing e-wastes was still significant.Tri-Penta-CBs were dominant homologues,consisting with their dominant global production.Size distribution of particle-bound PCBs showed that higher chlorinated CBs tended to partition more to the fine particles,facilitating its long range air transportation.     

液液萃取-气相色谱法测定地表水中17种有机氯农药研究

建立了二氯甲烷液液萃取-气相色谱法同时测定地表水中17种有机氯农药的方法。标准曲线线性良好,17种化合物的相关系数R2均大于0.999。当取样量为200 mL时,方法检出限在0.015μg/L~0.062μg/L之间。以超纯水样品进行基质加标实验,重复测定6次的相对标准偏差为1.2%~6.2%,平均加标回收率为72.8%~93.5%。方法简单快捷,精密度良好,准确性高,适用于地表水中痕量有机氯农药的测定。