基于质谱技术的在线大气颗粒物来源与污染过程解析研究——以江苏省淮安市为例

通过大气细颗粒物实时在线源解析技术(质谱直接测量法)采集录入淮安市市区部分特征污染源排放成分谱,对淮安市大气细颗粒物进行在线源解析,获取高时间分辨的颗粒物源解析结果,分析颗粒物来源、季度变化和重污染天气的污染过程,评估形成重污染过程的污染影响因子和影响程度,为区域大气污染综合整治提供重要目标指向,同时也为淮安环境空气PM2.5重度污染实时预警与监控、大气污染源减排方案评估、污染事件监控等提供有效的在线监测技术平台.     

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.     

热脱附-气相色谱-质谱法测定环境空气中5种挥发性卤代烃

建立热脱附-气相色谱-质谱联用测定环境空气中三氯甲烷、四氯化碳、三氯乙烯、四氯乙烯、溴仿等5种挥发性卤代烃的分析方法。该方法在一定浓度范围内工作曲线线性良好,相关系数均在0．9990～0．9998之间,加标回收率在94．0％～106．6％之间,RSD为2．18％-7．62％,检出限为0．22μg／m3～0．30μg／m3。该方法具有操作简单、分析快速、准确度高、灵敏高的特点,用热脱附-气相色谱-质谱联用测定环境空气中5种挥发性卤代烃,结果令人满意。     

火焰原子吸收光谱法测定电镀废水中高浓度的锡

采用盐酸消解样品,用火焰原子吸收光谱法测定电镀废水中高浓度的锡的质量浓度,方法简单可靠。通过实验样品的分析,验证了方法的准确度和精密度。该方法干扰少,数据准确,适合废水分析。     

2-丁烯醛生产废水中溶解性有机物的分级解析

采用超滤膜法将2-丁烯醛生产废水中的有机物分为相对分子质量不同的7个级分,并应用溶解性有机碳(dissolved organic carbon,DOC)、紫外吸收光谱(ultraviolet spectrum,UV)、傅里叶变换红外光谱(fourier transform infrared spectrometer,FT-IR)和气相色谱/质谱联用仪(gas chromatography with mass spectrometry,GC-MS)技术对不同相对分子质量区间的有机物所占比例及物质结构进行了研究.结果表明,废水中相对分子质量1×103的有机物所占比例最高,达到88.57%;采用GCMS对废水中相对分子质量1×103的级分进行分析,定性出27种化合物,包含醛、酮、酯、醇、酚、酸、烷烃类及其他苯系物等,其峰面积占有机物峰面积总和的比例分别为6.9%、5.3%、35.4%、13.2%、4.6%、0.4%、1.7%、16.8%,总和为84%.UV和FT-IR分析结果均显示不同相对分子质量区间的光谱吸收特征没有明显差别,级分中存在含有不饱和双键、羟基、羰基化合物及芳香族化合物,与GC-MS检测结果相吻合.研究结果为废水处理工艺的开发与优化提供了重要的指导作用.     

电感耦合等离子体质谱法测定地表水中铊的研究

本研究建立了电感耦合等离子体质谱法(ICP-MS)测定地表水中铊的方法。对仪器工作条件进行了优化,用在线内标校正基体效应的干扰,重点考察了样品测定介质、酸度、共存元素干扰等因素对测定结果的影响。在最佳实验条件下,该方法的检出限可达0.003μg/L,线性相关系数不小于0.999 9,加标回收率为93%~110%。与传统的原子吸收法相比,该方法不需要富集等繁琐的前处理过程,具有检出限低、快速、精密度和准确度高等优点。     

利用SPAMS研究华北乡村站点(曲周)夏季大气单颗粒物老化与混合状态

利用单颗粒气溶胶飞行时间质谱(SPAMS)于2013年6月30日~7月8日对华北地区乡村站点曲周大气单颗粒粒径及其化学组成进行了在线测量,共采集到同时含有正负离子谱图的颗粒230 152个,其粒径主要集中在0.2~2.0μm.结果表明,该地区的大气颗粒物主要分为8类:元素碳(EC,55.5%)、有机碳(OC,10.7%)、钠,钾等碱金属颗粒(alkalis,17.4%)、其他金属颗粒(other metals,1.7%)、富铁颗粒(Fe-rich,6.3%)、富铅颗粒物(Pb-rich,3.1%)、沙尘颗粒(dust,4.8%),other颗粒(0.8%),观测得到的8类气溶胶颗粒中绝大部分包含46NO-2、62NO-3、80SO-3、96SO-4、97HSO-4等二次组分离子,说明这些颗粒都经历了不同的老化过程或与二次组分进行了不同程度的混合.从气溶胶类型的谱分布看,各类型颗粒数浓度峰值基本出现在700~800 nm之间,dust、Fe颗粒主要集中在粗粒径段,EC颗粒子类研究表明随着表面不断吸附NH+4、NO-3、SO2-4等二次组分,EC颗粒逐步演化成老化程度较低的NO-3吸附型EC(ECN)和严重老化的SO2-4吸附型EC(ECS)混合态,两者日变化呈现明显的负相关性,也可能随着二次有机物在EC表面吸附,形成OC/EC混合态.     

固相萃取-超高效液相色谱-串联质谱测定水中痕量苯甲地那铵

苯甲地那铵是一种广泛使用的苦味剂,近年来被发现在欧洲水体中普遍存在。建立灵敏可靠的环境样品前处理分析方法对评价其环境行为具有重要意义。通过优化关键前处理过程参数,建立了水中苯甲地那铵的固相萃取-超高效液相色谱串联质谱分析方法,系统考察了该方法的准确度、精密度、基质效应、检出限以及线性范围。研究表明：当调节水样pH至8以上,采用混合型阳离子交换小柱(200 mg, 3 mL)富集水样,采用含体积分数2%甲酸的甲醇溶液洗脱时,该方法可获得最佳回收率;纯水和环境水样中加标回收率分别为97%～105%和89%～119%,相对标准偏差小于7%;基质效应均在24%以内;方法检出限为0.07 ng/L,线性范围为0.01～50μg/L。该方法可用于环境水体中苯甲地那铵的痕量检测。     

Investigation of heavy metal contaminations in the lower Sakarya river water and sediments

In this work, water and sediment samples were collected from three different stations located along the Sakarya river between May and September 2003. Lead, copper, chromium, zinc, nickel and cadmium concentrations were determined by using solvent extraction and flame atomic absorption spectrometric method. The results show that differences based upon sampling times, regions, sediment and water samples were observed. The mean levels of copper, nickel, chromium, lead, cadmium, zinc for sediment samples are; 4.630 μg g⁻¹, 13.520 μg g⁻¹, 8.780 μg g⁻¹, 2.550 μg g⁻¹, 9.990 μg g⁻¹ and for water samples are; 0.851 μg g⁻¹, 1.050 μg g⁻¹, 0.027 μg g⁻¹, 1.786 μg g⁻¹, 0.236 μg g⁻¹, 0.173 μg g⁻¹, respectively.     

226Ra, 232Th and 40K analysis in soil samples from some areas of Malwa region, Punjab, India using gamma ray spectrometry

The activity concentrations of soil samples collected from thirty different locations of Malwa region of Punjab were determined by using HPGe detector based on high-resolution gamma spectrometry system. The range of activity concentrations of ²²⁶Ra, ²³²Th and ⁴⁰K in the soil from the studied areas varies from 18.37 Bq kg⁻¹ (Sangrur) to 53.11 Bq kg⁻¹ (Sitoguno), 57.28 Bq kg⁻¹ (Dhanola) to 148.28 Bq kg⁻¹ (Sitoguno) and 211.13 Bq kg⁻¹ (Sunam) to 413.27 Bq kg⁻¹ (Virk Khera) with overall mean values of 35 Bq kg⁻¹, 80 Bq kg⁻¹and 317 Bq kg⁻¹ respectively. The absorbed dose rate calculated from activity concentration of ²²⁶Ra, ²³²Th and ⁴⁰K ranges between 8.47 and 24.48, 35.68 and 92.38, and 8.74 and 17.11 nGy h⁻¹, respectively. The total absorbed dose in the study area ranges from 58.08 nGy h⁻¹ to 130.85 nGy h⁻¹ with an average value of 79.11 nGy h⁻¹. The calculated values of external hazard index (H_ex) for the soil samples of the study area range from 0.35 to 0.79. Since these values are lower than unity, therefore, according to the Radiation Protection 112 (European Commission. Radiation Protection 112 1999) report, soil from these regions is safe and can be used as a construction material without posing any significant radiological threat to population.