GC-MS与HPLC/DAD联用对纺织品中4-氨基偶氮苯的测定

从化学反应条件的控制及气相色谱-质谱(GC-MS)和高效液相色谱/二极管阵列检测器(HPLC/DAD)联用方面,探讨了4-氨基偶氮苯的检测方法。实验表明,在样品中加入氢氧化钠,样品中的4-氨基偶氮苯和新鲜配制的连二亚硫酸钠发生反应,使4-氨基偶氮苯的碳碳双键断裂。释放的4-氨基偶氮苯在氯化钠存在的混合物中与叔丁基甲醚进行液液萃取。取叔丁基甲醚层进行分析,通过GC-MS的保留时间及特征离子碎片并结合HPLC/DAD紫外法对4-氨基偶氮苯进行定性和定量分析。4-氨基偶氮苯在2.5~30 mg/kg范围内呈良好的线性关系,其线性方程为:y=91.23x+5.272,相关系数r=1.000,检出限为3.20 mg/kg,平均回收率不低于90%。     

柳珊瑚中西松烷型二萜化合物的结构分析

首次从柳珊瑚Verrucella sp.中分离纯化得到无色结晶化合物,根据NMR和MS谱推知其为具有西松烷型骨架的萜类,为含有4个乙酰氧基,2个末端双键,1个六元环醚,1个γ-内酯的二萜--Junceellin,普通命名法命名为(1R,2R,3S,4R,6S,7R,8R,9S,10S,14S)-四乙酰氧基-6-氯代-4,8-环氧-5(16),11(20)-二烯-18,7-内酯.通过晶体X-射线衍射技术研究了其立体结构.     

少精、弱精不育症患者精液中微量元素含量的测定分析

用ICPOES法检测了54例男性少精、弱精不育者精液中Ca、Cd、Cu、Fe、Mg、Mn、Ni、Zn元素的含量,并对相关含量进行数据分析。结果表明,精液中微量元素含量的改变是影响精液质量的重要原因之一。     

Co(Ⅱ)-SCN~--中性红-聚乙烯醇体系共振瑞利散射法测定钴

研究了在聚乙烯醇(PVA-124)存在的条件下Co(Ⅱ)与硫氰酸根、中性红(NR)体系的共振瑞利散射光谱(RRS)。考察了该体系的光谱特性,影响因素及适宜的反应条件,确定了共振瑞利散射光谱强度与Co(Ⅱ)浓度之间的关系。在酸性和PVA-124存在的条件下,配阴离子[Co(SCN)4]2-与NR形成离子缔合物,其RRS显著增强,最大散射峰位于592 nm处,据此建立了一种测定微量钴的方法。Co(Ⅱ)的浓度在0~0.48μg/mL范围内与△IRRS具有良好的线性关系(r=0.9989),方法检出限为4.4×10-5μg/mL。该法应用于维生素B12注射液中钴的测定,结果令人满意。     

无溶剂条件下α-羟基磷酸酯的合成

在无溶剂条件下,以碳酸钾做催化剂,芳香醛与亚磷酸酯在室温下通过研磨,合成了一系列磷酸酯类化合物.该反应条件温和,操作简单,时间短,对环境友好,是一种绿色的合成方法.产物结构经IR,MS,1HNMR等方法表征.     

Understanding the effect of cobalt particle size on Fischer-Tropsch synthesis: surface species and mechanistic studies by SSITKA and kinetic isotope effect

Co/γ-Al(2)O(3) catalysts with particle sizes in the range of 4-15 nm were investigated by isothermal hydrogenation (IH), temperature programmed hydrogenation (TPH), and steady-state isotopic transient kinetic analysis (SSITKA). Kinetic isotope effect experiments were used to probe possible mechanisms on Co/γ-Al(2)O(3) with different particle size. It was found that CO dissociated on Co/γ-Al(2)O(3) catalysts at 210 °C. The total amount of CO(2) formed following the dissociation depends on the cobalt crystal size. O-Co binding energy was found to be highly dependent on the Co metal particle size, whereas similar C-Co binding energy was found on catalysts with different Co particle size. Very strongly bonded carbon and oxygen surface species increased with decreasing particle size and acted as site blocking species in the methanation reaction. SSITKA experiments showed that the intrinsic activity (1/τ(CH(x))) remained constant as the particle size increased from 4 to 15 nm. The number of surface intermediates (N(CH(x))) increased with increasing particle size. The apparent activation energies were found similar for these catalysts, about 85 kJ/mol. D(2)-H(2) switches further confirmed that the particle size did not change the kinetically relevant steps in the reaction. The reactivity of the active sites on the 4 nm particles was the same as those on the 8, 11, and 15 nm particles, and only the number of total available surface active sites was less on the 4 nm particles than on the others.     

Viscosity effect on the CIDEP of laser photolysis of duroquinone in hydrogen-donor solvents

Chemically induced dynamic electron polarization (CIDEP) is one of the important research fields of dynamic spin chemistry. In the present work, with ethylene glycol, 1,2-propanol and their mixtures with different ratios in volume as solvents and duroquinone as photosensitive molecule, the influence of solvent viscosity on the CIDEP of photolyzed duroquinone radicals has been studied experimentally. In each solvent, duroquinone neutral radicals are observed. Duroquinone neutral radicals are generated through hydrogen transfer reaction from hydrogen-donor solvent molecules to excited duroquinone triplet. The CIDEP mechanism is mainly triplet mechanism. The CIDEP intensity of duroquinone neutral radicals decreases with the increase in the solvent viscosity, and the variation was rapid in low-viscosity range and slow in high-viscosity range.     

Electrophoretic sol–gel synthesis of SrBi<Subscript>2</Subscript>Ta<Subscript>2</Subscript>O<Subscript>9</Subscript> nanowires

We report the independent invention of perovskite ferroelectric nanowires strontium bismuth tantalate (SrBi₂Ta₂O₉, SBT). Electrophoretic sol–gel techniques have been used successfully. The morphology and structures are analyzed via SEM, TEM and XRD. SBT nanowires and nanoparticles filled template revealed 30 and 40 μm long, respectively. SBT are proved to be a single phase of orthorhombic perovskite structure. As it indicated, SBT nanowires has been crystallized at 700 °C. To minimize surface polarity, SBT nanowires oriented preferentially along the growing axis (c axis) by translation and rotation of atomic clusters of SBT.     

Facile and ultra large scale synthesis of nearly monodispersed CoFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles by a low temperature sol–gel route

Nearly monodispersed cobalt ferrite nanoparticles were synthesized by a low temperature sol–gel route using propylene oxide as a gelation agent. The nanoparticles were obtained by the reaction of FeCl₂ and CoCl₂ in ethanol solution with propylene oxide to form the sol, followed by the boiling of the sol solution. The unique chemistry of this procedure allows the formation of highly homogeneous gel intermediate, resulting in the great reducing of crystallization temperature of ferrites to less than 100 °C without postannealing step. This guarantees the preparation of well defined and non-aggregated ferrite nanoparticles on an ultra-large scale of about 75 g in a single reaction. This large scale synthesis strategy offers important advantages over other conventional routes for the preparation of CoFe₂O₄ nanoparticles, showing the promising application of this route in the industrial production.     

Organocatalytic Tandem Reaction to Construct Six‐Membered Spirocyclic Oxindoles with Multiple Chiral Centres through a Formal [2+2+2] Annulation

An efficient tandem reaction for the asymmetric synthesis of six‐membered spirocyclic oxindoles has been successfully developed through a formal [2+2+2] annulation strategy. The amine‐catalysed stereoselective Michael addition of aliphatic aldehydes to electron‐deficient olefinic oxindole motifs gave chiral C3 components, which were further combined with diverse electrophiles (activated olefins or imines) to afford spirocyclic oxindoles with versatile molecular complexity (up to six contiguous stereogenic centres, high diastereo‐ and enantioselectivities).