固相萃取-高效液相色谱法测定水中丙烯酰胺研究

采用固相萃取-高效液相色谱法对水中的丙烯酰胺定性、定量分析。结果显示:丙烯酰胺含量在20μg/L~400μg/L之间呈良好线性关系,回归方程Y=0.476 8X+0.845 4,相关系数R为0.997 72,检出限0.1μg/L,样品回收率在71.85%~92.28%之间,相对标准偏差为3.4%~10.9%。该方法减少了有机溶剂用量,缩短了有机溶剂暴露时间,降低污染,且能满足地表水环境质量标准(GB 3838-2002)限值要求,是水中丙烯酰胺含量准确稳定的检测方法。用该方法测定了呼和浩特市引黄入呼左岸、右岸、中浅和中深4个断面水样,均未检出丙烯酰胺。     

柠檬酸对砷污染土壤的萃取优化条件实验研究

论文以新邱矿矸石山排土场土壤为研究对象,以去离子水做空白试验,选取尿素、十二烷基磺酸钠、碳酸氢钠、醋酸、柠檬酸等12种化学试剂做了萃取剂初选试验;并以柠檬酸为萃取剂进行了三因素三水平L9(33)正交实验。实验结果表明:柠檬酸和氢氧化钠可作为砷污染土壤的萃取剂,具有良好的萃取效果。柠檬酸作为砷污染土壤萃取剂的最优化条件是液土比为10mL/g,萃取时间为12h,萃取剂浓度为0.1mol/L。实验结果可为砷污染土壤的治理提供参考。     

Selective extraction and separation of Fe, Mn oxides and organic materials in river surficial sediments

In order to investigate the adsorption mechanism of trace metals to surficial sediments （SSs）, a selective extraction procedure was improved in the present work. The selective extraction procedure has been proved to selectively remove and separate Fe, Mn oxides and organic materials （OMs） in the non-residual fraction from the SSs collected in Songhua River, China. After screening different kinds of conventional extractants of Fe and Mn oxides and OMs used for separation of heavy metals in the soils and sediments, NH2OH .HCl （0.1 mol/L） ＋ HNO3 （0.1 mol/L）, （NH4）2C2O4 （0.2 mol/L） ＋ H2C2O4 （pH 3.0）, and 30% of H2O2 were respectively applied to selectively extract Mn oxides, Fe/Mn oxides and OMs. After the extraction treatments, the target components were removed with extraction efficiencies between 86.09%--3.36% for the hydroxylamine hydrochloride treatment, 80.63%- 101.09% for the oxalate solution extraction, and 94.76%-102.83% for the hydrogen peroxide digestion, respectively. The results indicate that this selective extraction technology was effective for the extraction and separation ofFe, Mn oxides and OMs in the SSs, and important for further mechanism study of trace metal adsorption onto SSs.     

瓦斯抽采PC-CAS基封孔材料优化及其膨胀作用分析*

为了研制以硅酸盐/铝酸盐水泥、生石灰、生石膏为主的PC-CAS基封孔材料,采用正交试验优化材料配比、开展膨胀力研究,并用扫描电镜观测料-煤胶结形貌。研究结果表明:材料的最优配比为A2B2C4,其具备优良的流动性、强度及致密性,造浆量达2 100 mL/kg;PC-CAS基材料具有显著的膨胀性,其膨胀力随时间先增大而后趋于稳定,并且该膨胀力随着径向约束的提高而增大;相比于FP材料,PC-CAS基材料产生的膨胀力能够显著降低材料-煤岩界面的空隙并在一定程度上压密煤体内部的裂隙;该材料产生的膨胀力可压密封孔段围岩、提高封孔质量,并为后期“二次注浆”提供保压条件。工业试验结果表明,采用PC-CAS基材料进行封孔可显著改善抽采效果,将原有平均浓度10.11%提升至20.08%。     

基于ZIF-L的微固相萃取技术测定地表水中痕量典型多环芳烃

制备类沸石咪唑酯骨架ZIF-L材料,将其用作微固相萃取吸附剂,处理水中萘、苊、苊烯、芴、菲、蒽、荧蒽、芘等8种痕量典型多环芳烃,再用HPLC测定。试验表明,ZIF-L对上述多环芳烃的萃取效率明显高于商品化萃取材料C 18和多壁碳纳米管。方法在0.100μg/L^200μg/L范围内线性良好,方法检出限为0.02μg/L^0.03μg/L,标准溶液5次测定结果的RSD为4.7%~9.5%,实际水样加标回收率为84.5%~115%。将该方法用于北太湖5个点位水样的测定,测定值为未检出~3.40μg/L。     

Metal Fractionation Studies in Surfacial and Core Sediments in the Achankovil River Basin in India

The Fractionation of Fe, Zn, Cu, Pb, Mn and Cd in the sediments of the Achankovil River, Western Ghats, India using a sequential extraction method was carried out to understand the metal availability in the basin for biotic and abiotic activities. Spatial distribution of heavy metals has been studied. Sediment grain size has significant control over the heavy metal distribution. The fluctuations in their concentration partly depend upon the lithology of the river basin and partly the anthropogenic activities. The sediments are dominated by sand and are moderately to strongly positively skewed and are very leptokurtotic in nature. The quartzite and feldspars are abundant minerals along with significant amount of mica with low clay content. The core sediments show increasing trend of heavy metal concentration with depth due to the recent addition of anthropogenic sources and post-diagenic activities. Significant amount of Cd (18%) was found in carbonate fraction, which may pose environmental problems due to its toxic nature. Small concentrations of metals, except Cd and Cu, are in exchangeable fraction, which indicate low bio-availability. Enrichment Factor (EF) for individual metals shows the contribution from terrregious and in part from anthropogenic sources. Selective Sequential Extraction (SSE) study shows the variation in specific metal distribution pattern, their distribution in different phases and their bio-availability. Maximum amount of the metals were bound to the non-residual fractions (mainly Fe-oxides). Overall, bio-availability of these micronutrients from sediments seems to be very less. Non-residual phase is the most important phase for majority of heavy metals studied. Among the non-residual fraction, maximum amount of the heavy metals bound to Fe-oxides. The study high lights the need for in-depth study of heavy metals distribution and fractionation in the smaller river basins to get precise information on the behavior and transport of heavy metals in the fluvial environment and their contribution to the world ocean.     

Fractionation and Sequential Extraction of Heavy Metals in the Soil of Scrapyard of Discarded Vehicles

Chemical and physical size fractionation of heavy metals were carried out on 20 soil samples from the scrap yard area. Tessier method was used in sequential extraction. Cadmium showed the highest levels among the other elements studied in the exchangeable fraction (about 33%), while other elements showed low levels in this fraction (≥1%). Lead and manganese were mostly found in the Fe–Mn oxide fraction, zinc and iron were mostly in residual fraction, while copper was mostly found in the organic fraction of the soil. Soil samples were size-fractionated into four sizes: 1000–500, 500–125, 125–53, and less than 53 μm. The highest levels of Fe, Cu, Pb, Mn, and Cd were found in the medium fraction (500–125 μm), while zinc showed its highest levels in the fine fraction (125–53 μm). The order of heavy metal load in the size fractions was found to be medium > fine > coarse > silt for Fe, Mn, Cu, Pb, and Cd, where it was found as fine > medium > coarse > silt for zinc.     

Temperature Effect on Migration of Zn and Cd Through Natural Clay

To investigate the effect of temperature on effective diffusion coefficients and retardation factors for Zn and Cd, combined diffusion and sequential extraction analyses were conducted at 15 ^˚C and 55 ^˚C. The effective diffusion coefficients of the metals increased up to ten times according to the increased temperature. On the other hand, the effect of temperature on the retardation factor depended on the retention mechanisms of the metals. The distribution coefficient for Zn, which was mainly partitioned in the carbonate phase, increased up to two times with the increase in temperature. On the other hand, the distribution coefficient for Cd, which was mainly partitioned in the exchangeable phase, was hardly affected by the temperature change. Results of combined diffusion and sequential extraction analysis showed that the effect of temperature on the heavy metals’ (Zn and Cd) migration through the compacted natural clay was influenced by the combined effects of the diffusion coefficient and the retardation factor. Additionally, we could also observe the change in retention mechanism for the metals with the change in pore water concentration.     

分子印迹技术在环境科学领域中的应用

分子印迹技术（MIT）是一门新兴的边缘科学技术,它的产生与发展为环境科学打开了又一视角。介绍了MIT的产生与发展及基本原理,综述了MIT在环境科学领域中的应用,主要包括MIT在固相萃取、膜分离、色谱分析、传感器及分子印迹聚合物作为催化剂在环境修复中的应用。     

聚丙烯中空纤维膜萃取水溶液中铜离子的研究

研究了聚丙烯中空纤维膜萃取二(2-乙基己基)膦酸(D2EHPA)水溶液中铜离子的工艺条件.结果表明,两相流速、膜面积对萃取率基本无影响;而水溶液的pH值和有机相初始铜离子浓度的改变使萃取率在40%-99%之间变化.整个萃取过程的传质阻力主要来源于D2EHPA和 Cu2 的界面配位络合反应阻力,铜浓度比较高时,传质阻力与铜浓度无关;而当铜浓度降低时,传质阻力随着铜浓度的降低而增大.