基于1⁃(3,5⁃二羧基苄基)⁃3,5⁃吡唑二羧酸的镍(Ⅱ)配位聚合物的合成、结构、磁性和光催化性质

用水热法合成了一个新的镍配位聚合物{[Ni2(L)(bib)1.5(H2O)4]·3H2O}n (1)(H4L=1-(3,5-二羧基苄基)-3,5-吡唑二羧酸,bib=1,4-双(1-咪唑基)苯),通过单晶X射线衍射、元素分析和热重分析等方法对其结构进行表征。结构分析表明配合物1具有三维网状结构。通过变温磁化率测量发现,配合物1中的Ni(Ⅱ)离子之间存在反铁磁相互作用。另外,光催化实验表明,配合物1对亚甲基蓝污染物的光催化降解效率达到了82.7%。     

基于四核金属单元的锌/镉配合物的合成、晶体结构及荧光性质

在水热条件下合成了2个金属配合物Zn4(Hhpa)4(phen)4(1)和{[Cd8(cnam)2(bpy)4(C2O4)6(H2O)8]·2H2O}n(2)(H2hpa=2-羟基间苯二甲酸,phen=菲咯啉,H2cnam=4-氧代-4H-吡喃-2,6-二甲酸,bpy=2,2′-联吡啶),通过元素分析、红外光谱、X-射线单晶衍射、荧光、热重分析和X-射线粉末衍射对其进行表征。配合物1为环状四核锌结构,相邻的四核锌单元通过π…π堆积作用扩展为三维超分子结构;配合物2是基于四核镉单元通过C2O42-离子和cnam2-配体连接而成的三维网状结构。在配合物1和2中Hhpa2-,cnam2-和C2O42-离子表现了丰富的配位模式。此外还研究了配合物1和2的荧光性质和热稳定性。     

具有三重螺旋链的二氯苯氧乙酸铽(Ⅲ)配位聚合物的晶体结构与荧光性质

采用水热法制备了一种新型金属配位聚合物[Tb2(2,4-D)6(2,2'-bipy)2]n(1)(2,4-D=2,4-二氯苯氧乙酸;2,2'-bipy=2,2'-联吡啶),用X-衍射单晶结构分析、红外光谱分析、荧光光谱法对产物进行了结构表征。结构分析表明,标题配合物属于单斜晶系,P2(1)/n空间群,晶胞参数a=2.792(1)nm,b=0.851(3)nm,c=3.335(1)nm,β=113.6470(1)°,V=7.2575(5)nm3,Z=4。金属离子Tb3+处于扭变的四方反棱柱构型中,金属离子之间通过配体2,4-D的羧基的桥联作用,链接成为一维三重螺旋链状配位聚合物。配合物的荧光光谱表明,配合物有望成为潜在的绿光材料。     

催化甲基紫褪色光度法测定茶叶中的微量铁

在稀硫酸介质中,微量铁对过氧化氢氧化甲基紫褪色反应具有强烈的催化作用,据此建立了催化褪色光度法测定微量铁的新方法.该方法线性范围为0.1-1.5μg/25mL,检出限为4.36×10-4μg/mL.可用于茶水中微量铁的测定,回收率在95.0％-101.6％之间,结果满意.     

A 3D Nickel(II) Coordination Polymer with cds Nets Constructed from 3‐Pyridin‐4‐yl‐benzoic Acid

A new coordination polymer, [Ni(3,4‐pybz)₂(H₂O)]_n ( 1 ), was hydrothermally synthesized from Ni(NO₃)₂ · 6H₂O and an unsymmetrical 3‐pyridin‐4‐yl‐benzoic acid (3,4‐Hpybz). It was characterized by IR spectroscopy, elemental analysis, thermogravimetric analysis, and single‐crystal X‐ray diffraction. In complex 1 , the 3,4‐pybz ligands act as linear linkers to join 4‐connected nickel(II) ion nodes, to build a 3D 4‐connected twofold interpenetrated 6⁵8‐cds coordination framework. In addition, the magnetic and thermal properties of complex 1 were also investigated.     

CdS纳米材料共振瑞利散射测定氧氟沙星的研究

在表面活性剂十二烷基磺酸钠SDS存在下,硫化镉能与氧氟沙星借静电引力及疏水作用力结合,形成粒径较大的聚集体.这种聚集体的形成导致硫化镉共振散射RRS强度显著增强,最大散射峰位于365nm.在适当条件下,散射强度△Ⅰ与氧氟沙星浓度成正比,据此提出了硫化镉-氧氟沙星-SDS体系测定氧氟沙星的新方法.方法的线性范围为4.0×...     

CdTe/CdS荧光探针测定痕量铜(Ⅱ)

以巯基乙酸为稳定剂,在水溶液中合成CdTe/CdS量子点,基于量子点与Cu2+混合后发生荧光猝灭作用,建立CdTe/CdS量子点作为荧光探针检测微量铜的新方法。在pH 4.60的HAc-NaAc缓冲溶液中,反应时间为10 min时,Cu2+质量浓度在0.01～1.00μg/mL范围与CdTe/CdS量子点的荧光猝灭程度呈良好的线性关系,相关系数为0.9978,检出限为9.90×10-3μg/mL。方法可以用于雨水、自来水和延河水中Cu2+的分析。     

卡维地洛的电化学测定及与牛血清白蛋白相互作用的研究

建立了测定卡维地洛(CAR)新的电化学方法.结合紫外、红外光谱分析,研究了CAR与牛血清白蛋白(BSA)的相互作用.实验发现,在pH4.0Britton-Robinson(B-R)缓冲溶液中,CAR在碳糊电极上产生3个不可逆的氧化峰.以0.92V处的氧化峰为研究对象,结果发现峰电流Ipa,1与CAR浓度在2.45×10-5～1.19×10-3mol/L范围呈良好的线性关系,CAR的检出限为5.6×10-6mol/L.当BSA加入CAR溶液后,CAR峰电流降低,氧化峰电流的降低值△Ipa,1与BSA的浓度在2.92×10-7～1.09×10-5mol/L范围内呈良好线性关系,BSA的检出限为4.1×10-8mol/L.电化学结果表明,CAR与BSA之间形成1∶1的结合物,结合常数为3.14×106L/mol.紫外光谱表明CAR的加入使BSA的吸收峰发生红移且有增色效应.红外光谱表明CAR与BSA分子中氨基酸残基的硫及氮原子形成键合作用.     

溴酸钾氧化孔雀石绿和甲基橙褪色光度法测定水中亚硝酸根

在H3PO4介质中,利用痕量NO2-催化KBrO3氧化孔雀石绿和甲基橙褪色的反应,建立了双波长双指示剂催化动力学光度法测定痕量NO2-的新方法。该反应在最大吸收峰505nm和615nm处,催化和非催化体系吸光度的变化与NO2-浓度呈线性关系,线性范围为0.01～0.80μg/mL,检出限为1.3×10-3μg/mL,该方法用于环境水样(自来水、雨水、延安卷烟厂废水)中痕量NO2-的测定,加标回收率为97%～110.2%.     

Production of activated carbon from sludge of food processing industry under controlled pyrolysis and its application for methylene blue removal

The present work aims to conduct a process optimization for the production of activated carbon from sludge of food processing industry. The significant feature of this sludge based activated carbon that makes it unique and economic is that it can be produced from waste material. The carbonaceous nature of this sludge does not allow its direct disposal to land because of excess organic and nutrient load contents, however, can be converted to a value added product. This process not only eliminates the need for further treatment of sludge but also reduce the cost of its handling, land filling, and transportation as well as the utilization in the same industry in the purification system.In the present work, activated carbon produced from pyrolysis of sludge was chemically activated by various activating agents. Optimization of impregnation ratio, impregnation time, activation temperature, and activation time was studied. The product was characterized through its iodine value and yield percentage. It was observed that the product had maximum iodine value of 624 mg g⁻¹ with ZnCl₂ as an activating agent. The FT-IR analysis depicts the presence of a variety of functional groups attached on the surface of activated carbon which are used in the interaction with the adsorbate during the process of adsorption. The XRD analysis reveals that the produced activated carbon has low content of inorganic constituents compared with the precursor. The product formed was applied for methylene blue adsorption. The adsorption equilibrium of methylene blue dye was examined at room temperature. Adsorption isotherm was drawn by applying Langmuir and Freundlich models fitting the data indict, with an adsorption capacity of 23.6 mg g⁻¹ and 14.2 mg g⁻¹, respectively. The data show that methylene blue adsorption is best suited to Langmuir equation.