超高效合相色谱法快速检测塑料食品接触材料中13种紫外吸收剂

建立了一种同时检测塑料食品接触材料中13种紫外吸收剂的超高效合相色谱法。以甲醇为溶剂对塑料食品接触材料样品进行超声提取，经C18固相萃取柱净化，过0.22 μm有机滤膜，采用超高效合相色谱仪分析。选择ACQUTY UPC² HSS C18 SB色谱柱（150 mm×3.0 mm，1.8 μm），以超临界二氧化碳为流动相，异丙醇为改性剂进行梯度洗脱，在最优色谱条件下，13种紫外吸收剂能够在4 min内实现有效分离。结果表明，在各自线性范围内，13种紫外吸收剂的线性关系良好，标准曲线相关系数不低于0.9985，检出限（S/N=3）为0.05~0.15 mg/kg，加标回收率为86.8%~115.7%，相对标准偏差为0.73%~5.61%。该方法快速简便，准确可靠，同时大大减少了有机溶剂的消耗，可用于塑料食品接触材料中13种紫外吸收剂的快速检测。     

铁氧簇合物[Fe11O6(OH)6(O2CCH3)15](C5H5N)6的结构和磁性质

通过三核铁盐[Fe₃O(O₂CCH₃)₆(H₂O)₃]C1在吡啶溶液中水解聚合得到铁氧簇合物[Fe₁₁O₆(OH)₆(O₂CCH₃)₁₅](C₅H₅N)₆。晶体结构表明11个铁离子(Ⅲ)中6个位于扭曲的三棱柱的顶点上，其余5个分别位于三棱柱的每个面之外。铁离子(Ⅲ)之间以氧桥或者羟基氧桥相连。变温磁化率证实铁离子(Ⅲ)之间是反铁磁耦合的。     

Synthesis and Characterization of the Chiral Skeleton Cluster [NiRuMo(CO)_5(μ_3-S)(η~5-C_5H_5)(η~5-C_5H_4COCH_3)]

1 INTRODUCTION The chemistry of transition metal cluster has enjoyed an exceptional growth since the mid 1970s[1, 2], especially in recent years the structural and bonding aspects of mixed-metal tetrahedral skeleton clusters have been extensively studied[3]. One important reason is that such chiral cluster can induce an asymmetric catalysis potentially. In our research group, considerable efforts have been directed to the synthesis of chiral tetrahedral clusters containing four different…     

化学键合吸附剂的合成及吸附行为

在无定型硅胶上化学键合十八烷基三氯硅烷，键合率17%-20％，粒度5μm-10μm，以此键合的吸附剂可有效地吸附香烟烟气中的焦油、亚硝胺，吸附率分别为15%-18％和37%-43％，研究了化学键合吸附剂的粒度和加入量对吸附性能的影响。     

水性丙烯酸酯共聚物交联体系的流变性

用旋转粘度计研究了甲基丙烯酸甲酯／丙烯酸丁酯／丙烯酸三元共聚物水性交联体系的流变性，考察了树脂含量、金属鳌合物含量和氨水水化对其流变性的影响。结果表明：三元共聚物水性交联体系呈非牛顿流体流变行为，具有剪切变稀特性；随树脂含量或鳌合物含量增加，体系的增稠能力得以增强；水化不仅可改善体系的增稠性能，而且可增强体系的非牛顿流变性。     

双2-乙酰基二茂铁合汞的合成及其晶体结构

标题化合物(C24H22Fe2HgO2)3是由2 氯汞基 1 乙酰基二茂铁与乙二胺反应得到的,其结构通过单晶X 射线衍射法确定。其晶体属三斜晶系,P 1空间群,Mr=1964 12,a=10 193(2),b=11 504(2),c=14 413(3) ,α=92 21(3),β=104 12(3),γ=102 67(3)°,V=1591 55(5) 3,Z=1,Dc=2 049mg/cm3,μ=8 583mm-1,F(000)=942,最终偏离因子为R=0 0859,wR=0 2617。该晶体中同时含有meso型及dl型分子,各分子中Hg原子的配位情况不一样。meso分子中的两个二茂铁是相互平行的,而另两分子dl型的二茂铁是相互垂直的。Hg原子以桥联形式连接两个二茂铁部分。meso型与dl型分子通过Hg O弱配位作用相连。     

苯甲醛缩三乙烯四胺Schiff碱Co(Ⅱ)配合物固相合成及氧合性能研究

Three new cobalt complexes were synthesized by solid-state reaction at room temperature. It was found that one mole of complex reacted with two moles of oxygen at room temperature. And the oxygenated complexes [Co·(L₁)₂·2O₂](NO₃)₂·2H₂O (L₁=N,N′-bis(4-hydroxyl-3-methoxy-benzyl)-triethylenetetramine), [Co·(L₂)₂·2O₂](NO₃)₂ ·2H₂O (L₂=N,N′-bis(4-hydroxyl-benzyl)-triethylenetetramine) and [Co·L₃·2O₂](NO₃)₂·2H₂O (L₃=N,N′-bis(2-hydroxyl-benzyl)-triethylenetetramine) were obtained and characterized by elemental analysis, IR spectra, ¹H NMR, TG/DTA, UV-Vis and molar conductance. The coordinated oxygen contents in the oxygenated complex were also determined by weight method. It was found that one O₂ molecule coordinated to the Co ion and formed superoxo type oxygenated complex.     

四核钴羰基簇合物Co4(CO)8(μ-CO)2(μ4-PSR)2的合成和晶体结构

The title compounds Co4(CO)8(μ-CO)2 (μ4-PSR) [R=-CH3, -C2H5, -C(CH3)3,-(CHa)4CH3] were synthesized by the reaction of Co2(CO)8 with RSPCl2. They were characterized by IR, 1HNMR, elemental analysis. The crystal and molecular structure of Co4(Co)8(μ-CO)2 (μ4-PSC2H5) has been determined by single crystal diffraction method. Crystal data: monoclinic, space group P21 /c, with a=8-445(3), 6=8.562(3), c= 17.125(6)Å, β=104.26 (3)' 9 V=1200.1Å3, Z=2, Dc=1.937gcm-3. Its molecular structure contains an octahedral Co4P2 skeleton which consists of a rectangular four cobalt atoms core and the Co4 core is capped above and below by two quadruply bridging PSR ligands.     

鲁米诺—六氰合铁（Ⅱ）酸钾—铁（Ⅲ）化学发光反应体系的研究与应用

微量铁的测定方法已有许多报道,其中较为理想的分析方法是邻二氮菲比色法和磺基水杨酸比色法。近年来,随着测试技术的提高和新试剂的应用,测铁的灵敏度在不断提高。如荧光熄灭法和催化吸光光度法。其检出限可达2×10~(-8)g·ml~(-1)。但这些方法条件苛刻且测定的线性范围窄。Seitz等利用Fe(Ⅲ)催化鲁米诺-过氧化氢的化学发光反应,测铁的灵敏度已达2×10~(-10)g·ml~(-1)。但该方法中,除Fe(Ⅲ)外,其它金属离子共存时同样有催化作用,干扰大。因而事先大多需要分离。本文对鲁米诺-六氰合铁(Ⅱ)酸钾-铁(Ⅱ)化学发光反应体系的研究,发现在碱性介质中痕量Fe(Ⅲ)对鲁米诺-六氰合铁(Ⅱ)酸钾的化学发光反应有很强的催化作用,且发光强度与Fe(Ⅲ)浓度在较宽范围内呈良好的线性关系。由此建立了一个灵敏度高、选择性好、操作简便、快速,对共存金属离子无需分离的测铁新方法。此法应用于大米、乳粉及水样中铁量测定,结果与邻二氮菲比色法测定结果一致。