丹江口水库表层沉积物不同形态氮的赋存特征及其生物有效性

为了揭示丹江口水库沉积物氮空间分布特征及其生物有效性,采用连续分级提取法研究了表层沉积物中可交换态氮(Exchangeable nitrogen,EN)、酸解态氮(Acid hydrolysable nitrogen,HN)及残渣态氮(Residue nitrogen,RN)的赋存特征,同时结合生物可利用态氮的含量,探讨了各形态氮对生物可利用态氮的贡献。结果表明,丹江口水库沉积物中总氮(Total nitrogen,TN)在425~5796 mg/kg之间,平均为1 319.32 mg/kg,其中EN、HN和RN的平均值相对比例为2.15∶1.95∶1,且各形态氮含量的空间分布呈入库河流大于库区开阔区域的特征,尤其在丹江、老灌河以及犟河-堵河入库口的含量较大。潜在矿化氮(Potential mineralized nitrogen,PMN)含量在40.20~1 468.95 mg/kg之间,平均为275.06 mg/kg,其中EN对丹江口水库沉积物PMN的贡献较大,比例在19.85%~90.80%之间,平均为63.47%。各形态氮在不同的水环境条件下发生迁移转化,保持着水-沉积物界面氮的动态平衡。     

Determination of 4-tert-octylphenol in surface water samples of Jinan in China by solid phase extraction coupled with GC-MS

Octylphenols, considered as xenoestrogens, mainly exist as 4-tert-octylphenol (OP) in aquatic environments. The high stability and accumulation of OP in aquatic systems have caused endocrine disruption. The OP in surface water in Jinan, China was analyzed by gas chromatography-mass spectrometry (GC-MS) coupled with solid phase extraction (SPE). Water samples were extracted by SPE on a cartridge system containing C-18 as sorbent. To increase sensitivity and selectivity, OP was derivatized to 4-tert-octyl-phenoxy silane. With the use of phenanthrene-d10 as internal standard, the detection limit based on signal-to-noise ratio (S/N = 3) was 0.06 ng/mL. The average recovery was from 84.67% to 109.7%. The precision of the method given as the relative standard deviations (RSD) was within the range 6.24%-12.96%. In the target water samples, the concentrations of OP were as follows: 15.88-71.24 ng/L for Jinxiuchuan Reservoir, 3.850-26.68 ng/L for the city moat, 6.930-41.56 ng/L for Daming Lake, 66.03-474.2 ng/L for Xiaoqing River, 14.66-17.72 ng/L for the Yellow River, and 10.60-26.43 ng/L for Queshan Reservoir. The Xiaoqing River was seriously polluted due to the discharge of wastewater from Jinan. Jinxiuchuan Reservoir had a higher concentration of OP compared with the Yellow River and Queshan Reservoir, which is ascribed to the surrounding human activities. These data are reported for the first time, providing strong support for the control of OP pollution in Jinan.     

预富集技术在原子吸收光谱环境分析中的应用

原子吸收光谱法是分析环境水样中金属离子含量的有效方法之一。在测定时往往需要对样品进行前处理,然后再进行测定。文章介绍了近些年较新的一些分离富集技术在原子吸收光谱分析环境中金属离子时的应用,分析了离子交换树脂在样品中金属离子富集分离过程中的研究近况,评述了固相萃取、析相微萃取、单滴液滴微萃取、分散液液微萃取、离子液体萃取、浊点萃取等多种萃取方式在样品预富集中的应用进展,综述了活性炭、纳米粒子、淀粉、分子筛等吸附剂在富集环境水样中金属元素的应用现状,同时还对在线富集技术与流动注射分析技术联用在金属元素分析中的应用进展进行了评述。     

Evaluation of soil washing process with carboxymethyl-β-cyclodextrin and carboxymethyl chitosan for recovery of PAHs/heavy metals/fluorine from metallurgic plant site

Polycyclic aromatic hydrocarbons(PAHs)/heavy metals/fluorine(F) mixed-contaminated sites caused by abandoned metallurgic plants are receiving wide attention. To address the associated environmental problems,this study was initiated to investigate the feasibility of using carboxymethyl-β-cyclodextrin(CMCD) and carboxymethyl chitosan(CMC) solution to enhance ex situ soil washing for extracting mixed contaminants. Further,Tenax extraction method was combined with a first-three-compartment model to evaluate the environmental risk of residual PAHs in washed soil. In addition,the redistribution of heavy metals/F after decontamination was also estimated using a sequential extraction procedure. Three successive washing cycles using50 g/L CMCD and 5 g/L CMC solution were effective to remove 94.3% of total PAHs,93.2% of Pb,85.8% of Cd,93.4% of Cr,83.2% of Ni and 97.3% of F simultaneously. After the 3rd washing,the residual PAHs mainly existed as very slowly desorbing fractions,which were in the form of well-aged,well-sequestered compounds; while the remaining Pb,Cd,Cr,Ni and F mainly existed as Fe–Mn oxide and residual fractions,which were always present in stable mineral forms or bound to non-labile soil fractions. Therefore,this combined cleanup strategy proved to be effective and environmentally friendly.     

Antimony smelting process generating solid wastes and dust：Characterization and leaching behaviors

A large amount of solid waste has been produced by the antimony smelting process in the＂World Capital of Antimony＂, Xikuangshan area in China. This study comprehensively investigated the physical and chemical characteristics of the various solid wastes, as well as the leaching behavior of the solid wastes, which included water-quenched slag,arsenic-alkali residue, desulfurized slag and blast furnace dust. These four types of waste were enriched in a variety of heavy metals and metalloids and more specifically with As and Sb levels up to 8.6 × 104 and 3.16 × 105mg/kg, respectively, in arsenic-alkali residue. For desulfurized slag and water-quenched slag, the leaching concentration of Sb significantly exceeded the acceptable limits during the leaching tests using the toxicity characteristic leaching procedure and the synthetic precipitation leaching procedure. In addition, As leaching in arsenic-alkali residue was extraordinarily hazardous, being three orders of magnitude higher than the regulatory level of As. According to the results of the extraction tests, all the tested wastes were classified as hazardous waste.     

2-萘酚生产废水综合治理与资源化利用工程实例

针对2-萘酚生产废水p H值低、色泽深,亚硫酸盐和萘磺酸盐高、COD浓度高的特点,采用酸化脱硫-两级络合萃取-氧化絮凝工艺处理,介绍了专利工艺的流程设计,给出了主要工艺设计参数及投资运行成本。工程运行结果表明,该工艺设计合理、技术成熟、处理效果稳定,2-萘酚生产废水经处理后达到GB 8978—1996《污水综合排放标准》一级排放标准要求;回收的萘磺酸钠固体可返回2-萘酚生产系统套用;反萃取黑液经蒸发浓缩,合成的减水剂产品各项指标达到或超过GB 8076—2008《混凝土外加剂》高效减水剂指标要求。     

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。     

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。     

一种简便高效的土壤石油烃提取方法的建立

通过开展单因子实验与正交实验,考察不同参数下超声萃取法对土壤中总石油烃(TPH)的提取效率,并对比了超声萃取法、超声-索氏萃取法及传统索氏萃取法对不同原油污染土壤的提取效果。结果表明:超声萃取法的最优工作参数为20 m L二氯甲烷,超声10 min,4000 r/min离心10 min,萃取4次。3种提取方法中,超声萃取法对石油烃平均回收率最高,为100.95%,而传统的索氏萃取法最低,仅为94.54%。可见,超声萃取法操作简单,效率高,可广泛用于土壤中总石油烃含量的提取测定。     

反渗透膜面细菌胞外多聚物提取方法研究

城市污水脱盐系统的反渗透(RO)膜面生物污堵问题严重影响了该技术的稳定运行,解析生物污堵机理的关键因素是微生物胞外多聚物(EPS)特征分析,然而目前细菌EPS提取方法多样,无统一标准,制约了EPS分析的可靠性和可对比性.基于此,本文以再生水厂RO膜面污堵物中分离的细菌为对象,采用水浴、超声、离子树脂、碱液4种方法提取EPS,以DOC和DNA含量表征提取的EPS总量和提取过程细胞破裂程度.结果表明,45℃水浴法不造成细胞破裂,提取总量多,是一种有效的提取方法.进一步对比不同提取时间条件下EPS溶液中多糖和蛋白含量变化,以及分子量、荧光特征等,综合认为提取1 h时,提取的EPS中多糖与蛋白相对含量稳定,不同分子量化合物均溶于水中,能客观地反映EPS特征.研究表明,45℃水浴1 h可以作为细菌EPS提取的适用方法应用.