加速溶剂萃取-凝胶净化色谱-气相色谱质谱法测定农用地土壤中有机氯农药方法研究

通过对加速溶剂萃取、平行蒸发及净化方法等环节的优化实验,建立了加速溶剂萃取-凝胶净化色谱-气相色谱质谱法测定农用地土壤中23种有机氯农药的检测方法。结果表明,方法检出限为0.0034~0.0052 mg/kg;对化合物质量分数为0.25 mg/kg的土壤加标样品进行平行实验,回收率为82.0%~93.7%;测定结果的相对标准偏差（RSD）≤8.7%。对土壤有证标准质控样品进行分析,测定结果均在验收范围之内。该方法准确可靠,灵敏度较高,样品净化效果较好,能够满足农用地土壤中有机氯农药残留痕量分析的要求。     

Decoupling the adsorption mechanisms of arsenate at molecular level on modified cube-shaped sponge loaded superparamagnetic iron oxide nanoparticles

In this study, a commercial cube-shaped open-celled cellulose sponge adsorbent was modified by in-situ co-precipitation of superparamagnetic iron oxide nanoparticles (SPION) and used to remove As(V) from aqueous solutions. Fe K-edge X-ray absorption spectroscopy (XAS) and TEM identified maghemite as the main iron phase of the SPION nanoparticles with an average size 13 nm. Batch adsorption experiments at 800 mg/L showed a 63% increase of adsorption capacity when loading 2.6 wt.% mass fraction of SPION in the cube-sponge. Experimental determination of the adsorption thermodynamic parameters indicated that the As(V) adsorption on the composite material is a spontaneous and exothermic process. As K-edge XAS results confirmed that the adsorption enhancement on the composite can be attributed to the nanoparticles loaded. In addition, adsorbed As(V) did not get reduced to more toxic As(III) and formed a binuclear corner-sharing complex with SPION. The advantageous cube-shape of the sponge-loaded SPION composite together with its high affinity and good adsorption capacity for As(V), good regeneration capability and the enhanced-diffusion attributed to its open-celled structure make this adsorbent a good candidate for industrial applications.     

NaOH改性鱼骨粉材料对Cd(II)的吸附

以鱼骨粉（FBM）为原料,利用NaOH处理制备高性能改性鱼骨粉材料（FBM_T）,通过比表面积仪（BET）、X射线衍射仪（XRD）、傅里叶红外光谱（FTIR）、扫描电镜-光电子能谱（SEM-EDS）、透射电镜（TEM）等手段对吸附前后材料形貌、孔结构、功能基团进行表征分析.结果表明,与FBM相比,FBM_T出现一定数目中孔和大孔,具备了高孔容和平均孔径,分别增加68.57%和24.69%.FBM_T材料表面-OH、C=O和PO₄^3-等官能团含量增加,显示出一定的缓冲性能.FBM和FBM_T对Cd（Ⅱ）的吸附经历快速的分配和慢速的吸附两个阶段,符合准二级动力学模型,相关系数R²分别达到0.8635及0.9480.Langmuir模型较好地拟合FBM和FBM_T对Cd（Ⅱ）的等温吸附过程,对Cd（Ⅱ）饱和吸附量由改性前的9.28mg/g增至改性后的22.47mg/g,对应的吸附强度K_F值也随之增加.分离因子0 < R_L < 1表明Cd（Ⅱ）的去除过程为有利吸附.功能材料与Cd（Ⅱ）的作用机理主要包括阳离子专性吸附、静电吸附、离子交换、表面络合及沉淀作用.以上研究为鱼骨粉修复Cd污染提供一种经济有效的方法.     

Degradation of duloxetine: Identification of transformation products by UHPLC-ESI(+)-HRMS/MS, in silico toxicity and wastewater analysis

Duloxetine (DUL), an antidepressant drug, has been detected in surface water and wastewater effluents, however, there is little information on the formation of its transformation products (TPs). In this work, hydrolysis, photodegradation (UV irradiation) and chlorination experiments were performed on spiked distillated water, under controlled experimental conditions to simulate abiotic processes that can occur in the environment and wastewater treatment plants (WWTPs). Eleven TPs, nine from reaction with UV light and two from chlorine contact, were formed and detected by ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry, and nine of them had their chemical structures elucidated upon analyses of their fragmentation patterns in MS/MS spectra. The formation and degradation of the TPs were observed. The parent compound was completely degraded after 30?min in photodegradation and after 24?hr in chlorination. Almost all TPs were completely degraded in the experiments. The ecotoxicity and mutagenicity of the TPs were predicted based on several in silico models and it was found that a few of these products presented more ecotoxicity than DUL itself and six TPs showed positive mutagenicity. Finally, wastewater samples were analyzed and DUL and one TP, possibly formed by chlorination process, were detected in the effluent, which showed that WWTP not only did not remove DUL, but also formed a TP.     

夏季高原河流CDOM光学特性、组成及来源研究

对高原河流有色溶解有机物(CDOM)光学特性、组成及来源进行研究,有利于更好的了解高原河流水体生态环境,为高原河流生态系统中溶解有机物(DOM)循环过程的研究提供数据参考.利用2017年夏季无定河和湟水流域河流的实测数据对CDOM的吸收特性、荧光特性、水质参数以及它们之间关系进行分析,进而对高原干旱地区河流CDOM光学特性及其组成与来源进行研究.研究结果表明:两流域河流中CDOM吸收系数随波长的增加呈衰减趋势,但吸收光谱曲线差别较大;两流域CDOM在440 nm处的吸收系数[a(440)]与溶解有机碳(DOC)具有显著相关性(p0.01),而与叶绿素a浓度(Chla)不存在相关性.无定河a(440)与Chla浓度的相关性说明其河流现场产生(生物活动)作用较小.通过对比分析S_(275-295)、SUVA_(254)发现,无定河分子量和芳香性程度均大于湟水,且湟水与无定河CDOM的分子量变化要高于其它河流的研究.根据CDOM三维荧光光谱分析发现,类腐殖质荧光峰是两流域河流CDOM荧光的主要贡献者;通过荧光指数FI、腐殖化指数HIX、生物源指数BIX的研究发现,湟水以陆源输入为主,腐殖化程度高,无定河以陆源输入为主的同时存在一定的自生成分,人为生产活动干扰是其陆源输入的主要影响因素.通过冗余分析发现,湟水DOC、Chla、pH对类腐殖质荧光峰及荧光强度影响较大(p0.01);无定河DOC、电导率(EC)、浊度(Tur)与类腐殖质荧光峰及荧光强度显著正相关(p0.01).     

陶瓷膜接触器在润湿模式下吸收SO2的传质强化

将平均孔径为100 nm的Al_2O_3陶瓷膜组装成膜接触器,以单乙醇胺(MEA)为吸收剂,在考察吸收剂浓度对膜吸收过程影响的基础上,深入比较了陶瓷膜在润湿和非润湿模式下脱除SO_2的传质性能.实验结果表明,当MEA浓度大于0.26 mol·L~(-1)时,润湿模式下SO_2的脱除率和传质系数均高于非润湿模式.根据膜理论和阻力串联模型建立了陶瓷膜吸收SO_2的传质方程,理论计算表明,润湿模式下膜相传质阻力因瞬间化学反应的存在大幅降低,润湿模式更适用于脱除烟气中低浓度的SO_2.本研究结果可为陶瓷膜接触器在膜吸收领域的工业化应用和进一步传质优化提供参考.     

电感耦合等离子体质谱同时测定沉积物中12种重金属元素

比较了王水回流、密闭容器消解及微波消解3种不同方法对海洋沉积物的消解效果,结果表明微波消解效果较好;优化了消解体系和程序,HNO3-HF-H2O2消解体系对重金属的溶出效果较好;并建立了电感耦合等离子体质谱测定沉积物中Cr、Co、Ni、Cu、Zn、Mo、Cd、Sn、Hg、Tl、Pb、U等12种重金属元素的分析方法,各元...     

南京近郊主要森林类型对土壤重金属的吸收与累积规律

研究了南京近郊针、阔叶树种杉木(Cunninghamia lanceolata)、麻栎(Quercus acutissima)对重金属元素铬、铜、镍、铅、锌的吸收和累积规律.研究结果表明,5种重金属元素在2种林分的枯落物层含量均高于灌草层和乔木层各部位,但由于乔木层生物量较大,重金属元索在2种森林生态系统中主要储存在乔...     

氢化物发生原子荧光光谱法测定饮用水中的铅

通过改变仪器条件及试剂配比进行优选实验,利用原子荧光光谱法测定饮用水中的铅可知:铅的检出限是0.020μg/L,能够满足GB 5749-2006《生活饮用水卫生标准》的要求;同时原子荧光光谱仪分析样品灵敏度高、重现性好、干扰少、操作简便、分析快捷,测定样品的准确度和精密度均能达到质量控制要求。     

高效液相色谱-原子荧光光谱联用测定水中形态砷

采用高效液相色谱-氢化物发生-原子荧光光谱联用技术测定水中亚砷酸盐[As(Ⅲ)]、二甲基砷(DMA)、一甲基砷(MMA)和砷酸盐[As(V)]等4种形态砷,以磷酸盐缓冲溶液为流动相,硼氢化钾为还原剂,优化了仪器主要技术参数.As(Ⅲ)、DMA、MMA和As(V)在7 min内实现了良好的基线分离,在5.00 μg/L～...