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.     

平煤十矿底板巷穿层钻孔瓦斯抽采模拟研究

为了降低平煤十矿己15-16-24130工作面运输巷掘进中的突出危险性,基于实际工程背景,考虑瓦斯抽采中的瓦斯运移及煤岩变形等因素,建立了瓦斯抽采气固耦合模型,并利用COMSOL Multiphysics软件对平煤十矿己15-16煤层的底板巷穿层钻孔瓦斯抽采方案进行数值模拟,研究了瓦斯抽采对于降低掘进过程中突出危险性的影响。研究结果表明:在己18煤层开挖底板巷对己15-16煤层进行穿层钻孔瓦斯抽采,瓦斯抽采180 d后,己15-16-24130工作面运输巷附近煤层残余瓦斯压力及瓦斯含量分别降至0.315 MPa和3.84 m3/t;将底板巷穿层钻孔瓦斯抽采方案进行工程应用,实测抽采后的残余瓦斯压力及瓦斯含量在0.32 MPa和3.17 m3/t,均小于平煤十矿煤与瓦斯突出防治规定的“双6”指标（残余瓦斯压力小于0.6 MPa,残余瓦斯含量小于6 m3/t）,可有效降低运输巷掘进过程中的突出危险性。     

煤与瓦斯共采在错层位巷道布置中的机理研究及应用构想

为了完善现有煤与瓦斯共采技术,创新煤与瓦斯共采方法,对错层位巷道布置下的煤与瓦斯共采系统展开研究,利用相似模拟试验,分析错层位巷道布置覆岩运动情况,预测其开采围岩裂隙发育和瓦斯运移形式,提出了创新煤与瓦斯共采技术构想。研究结果表明:采空区覆岩三带高度随接续工作面的增加而增大,相邻采空区垮落矸石压实区呈现“O-L-O”形变化,多个相邻采空区覆岩出现大“O”形圈裂隙带;相邻采空区内瓦斯可实现相互运移,大“O”形圈裂隙带内赋存大量瓦斯气体;研究提出了地面钻井抽采瓦斯、走向高位瓦斯抽采巷和外错尾巷穿层钻孔3种煤与瓦斯共采技术,比传统巷道布置情况下的煤与瓦斯共采技术在安全、经济等方面更具优势。     

气相色谱-串联质谱法测定沉积物中多环芳烃

采用ASE法提取沉积物中16种多环芳烃,以固相萃取法净化提取液,用气相色谱-串联质谱法测定。通过优化测定条件,使方法在5.00μg/L~1 600μg/L范围内线性良好,方法检出限为0.15μg/kg~0.66μg/kg。空白石英砂的加标回收率为61.9%~121%,7次测定结果的RSD为2.6%~11.1%。     

液液萃取-气相色谱法测定水质可萃取性石油烃C10~C40

建立了以环己烷为萃取剂、气相色谱法(氢火焰离子化检测器,FID)测定水质样品中可萃取性石油烃(C_(10)～C_(40))的分析方法。以正构烷烃混合标准溶液为定性和定量校准标准,以色谱峰面积总和与混合标准溶液总浓度建立校准曲线进行外标法定量。方法检出限为0.01 mg/L,经验证方法精密度和准确度良好。同时,分别以气相色谱法和红外光度法测定了地表水、污水处理厂出水、海水和化工废水等实际样品,对比实验结果表明,在可萃取性石油烃C_(10)～C_(40)的碳数范围内,气相色谱法的测试结果与红外光度法无明显差异,有较好的可比性。