Analysis of heavy metal distribution in superficial estuarine sediments (estuary of Bilbao, Basque Country) by open-focused microwave-assisted extraction and ICP-OES

Open-focused microwave-assisted extraction and ICP-OES determination of As, Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn from surface sediments of the estuary of Bilbao (Basque Country, North of Spain) was carried out. All the samples were collected at three different tributaries of the estuary (Asua, Galindo and Nerbioi-Ibaizabal) every two months during 1999. The digestion procedure was proposed from the conclusions of a fractionated factorial design, and the precision and accuracy of the method was verified using a certified reference sediment (RTC008-050). The results of the analysis were statistically treated by means of principal component analysis and correlation analysis. The principal component analysis of sediment data (32 samples × 9 metals) indicated different patterns of contamination regarding the tributary and sampling station. The two main patterns observed were a steady increment of the metal concentration along all the campaigns in the samples collected in the Galindo River and a seasonal variation in the Nerbioi-Ibaizabal River, with higher metallic content during summertime and lower content during wintertime.     

微波辅助萃取法提取滇池沉积物中的多氯联苯

研究运用微波辅助萃取-固相萃取-气相色谱/质谱检测滇池沉积物中6种指示性多氯联苯（PCB28、PCB52、PCB101、PCB138、PCB153和PCB180）.重点优化了微波辅助萃取技术,在萃取温度为100℃和萃取时间为30 min（升温和恒温各15 min）条件下,以30 mL正己烷∶二氯甲烷（1∶1,V∶V）的...     

Simultaneous determination of organophosphorus and organonitrogen pesticides residues in Angelica sinensis

Gas chromatography with nitrogen phosphorus detector (GC-NPD) was applied to the simultaneous determination of 15 organophosphorus and 6 organonitrogen pesticides residues in Angelica sinensis. The pesticides were extracted by microwave-assisted extraction (MAE) and ultrasound-assisted extraction (UAE) techniques, respectively. The experimental variables were optimized through orthogonal array experimental design. Cleanup of extracts was performed with column chromatography using florisil and neutral aluminum as the sorbents. The determination of pesticides in the final extracts was carried out by GC-NPD. Under optimized conditions, the average recoveries obtained from MAE and UAE are in the range of 75.1–129% and 70.6–129%, respectively, and the relative standard deviations of MAE and UAE were 3.1–10.6% and 1.0–17.8%, respectively.     

微波消解-ICP—MS测定土壤和水系沉积物中的重金属

建立了一种采用逆王水和氢氟酸的混合体系微波酸消解土壤与水系沉积物,电感耦合等离子体质谱法快速测定六种金属元素（As、Cd、Pb、Cu、Cr和Ni）含量的方法。本文研究了消解温度和消解时间对消解效果的影响。结果表明,在190℃下运行25分钟对土壤与水系沉积物中的六种金属元素均具有很好的消解能力,备元素的测定值与标准值相符。在对实际土壤与水系沉积物样品进行分析后得出采样区域的土壤与沉积物中这六种金属含量水平正常。     

ICP-AES测定南宁市大气颗粒物中重金属含量

采用石英滤纸和隔膜真空泵自制采样装置,对南宁市区的居民区、校园区、商业区和工业区进行连续10d的大气采样,所得样品经微波消解后,用电感耦合等离子体发射光谱法(ICP-AES)同时测定铬、铁、铜、锌、砷、镉和铅七种重金属元素含量以检测南宁市空气质量,同时考察了仪器工作参数对测定结果的影响。实验表明:在选定的实验条件下,各元素的检出限低,准确性和精密度良好。样品测定结果表明,大气环境中重金属污染物以Fe、Zn和Pb为主;工业区,商业区,居民区重金属含量高于校园区。重金属平均浓度最大值为:Cr(0.06027μg/m)3、Fe(1.8541μg/m)3、Cu(0.02214μg/m)3、Zn(0.3666μg/m)3、As(0.02272μg/m)3、Cd(0.004733μg/m)3、Pb(0.1843μg/m)3,低于我国(TJ36-96)《居住区大气中的有害物质最高容许量》中规定值,说明南宁市空气质量良好。     

Efficient microwave-assisted photocatalytic degradation of endocrine disruptor dimethyl phthalate over composite catalyst ZrOx/ZnO

A highly active ZrOx/ZnO catalyst for microwave-assisted photocatalytic (MW/PC) degradation of endocrine disruptor dimethyl phthalate (DMP) has been prepared via cetyltrimethylammonium assisted hydrothermal method. The ZrOx/ZnO was characterized by XPS, XRD, UV-Vis, BET and SEM techniques. The XPS result showed that Zr oxides with different valences (+2, +3, +4) co-existed in ZrOx/ZnO. By using the ZrOx/ZnO (0.1 g), the TOC removal efficiency of DMP (100 mL of 50 mg/L) was 88% after 30 min reaction, which was about 15% higher than P25 TiO2. It was found that the removal process of DMP by MW/PC followed pseudo first-order kinetics in all cases, and ZrOx/ZnO significantly accelerated the degradation of DMP. The degradation half-life time of DMP was shortened 45% compared with P25 TiO2. A possible catalytic mechanism was proposed based on microwave response and interfacial charge transfer. ZrOx/ZnO could be reused for six times without obvious decrease in catalytic activity. The study offers new insights into designing highly efficient catalysts for MW/PC process and is applicable for MW/PC environmental remediation.     

微波加热PEI改性纤维素纤维的制备及其对水中Cu~(2+)的吸附性能研究

采用微波辅助加热的方法快速制备了聚乙烯亚胺(PEI)改性的纤维素纤维材料,并与常规加热法制备的改性纤维进行对比。利用元素分析(EA)、热重分析(TGA)对改性纤维进行了表征。同时,还讨论了溶液p H、吸附时间、温度、溶液浓度对改性纤维吸附性能的影响。结果表明:与常规加热制备相比,采用微波加热改性的纤维素纤维接枝率更高且反应时间更短。在p H为6时,改性纤维对Cu2+的吸附性能达到最大,最大吸附量为134.4 mg/g,吸附过程符合Langmuir等温模型和准二级动力学方程。100 W微波加热条件下,经5次吸附/解吸后,吸附量无显著变化。     

微波消解法在生物样品分析中的应用

本文利用国产的ＷＭＸ－１型微波炉对牡蛎、牛肝、大米粉和西红柿叶等生物标准样品的微波消解条件进行了研究,并用火焰原子吸收光度法对其中的Ｃｕ、Ｚｎ、Ｆｅ、Ｍｎ等元素进行了分析。     

Development and validation of a spectrophotometric method for soil adsorption study of malathion on three Indian soils

In view of the widespread use of pesticides in agriculture and its associated toxic effects on environment and human beings, the fate of these chemicals in soil is of major concern. The pesticide adsorption process is one of the major factors affecting its persistence and movement in the soil. With a view of studying the fate of malathion in soil, the adsorption of this insecticide was studied on three Indian soils by using batch equilibrium method. To carry out the adsorption study, a new simple, sensitive, and rapid method was developed, based on microwave-assisted alkaline hydrolysis of insecticide to the dimethyl dithiophosphate and its subsequent reaction with copper(I) perchlorate in acetonitrile. On mixing the reagents, a yellow color developed, which was stable for 120?min and was measured at 419?nm. The adsorption of malathion was studied by using Freundlich's adsorption equation and n _f values were observed less than 1 in all the soils. The leaching behavior of the insecticide was studied in terms of ground ubiquity score, which was below 1.8, classifying malathion as non-leacher pesticide, and hence it is not hazardous.     

氢化物发生原子荧光光度法分析空气中铅

为提高空气中铅分析的灵敏度,采用氢化物发生原子荧光分析方法进行空气中铅的测量.分别采用微波加热方法和湿式消解法对样 品进行了预处理,对两种消解方法进行了比较,并探讨了样品前处理过程对分析的影响;对影响氢化物发生效率的各种实验条件,包括增敏剂、酸介质及氢化物发生体系中各物质浓度等,以及原子荧光分析仪器的条件参数进行了优化...