真空离心浓缩/气相色谱-质谱联用法测定白酒中6种邻苯二甲酸酯类增塑剂

建立了测定白酒中6种邻苯二甲酸酯类增塑剂的真空离心浓缩/气相色谱-质谱联用(GC-MS)分析方法。样品经真空离心浓缩,正己烷提取,取上层正己烷,4000r/min离心5min,采用GC-MS测定,外标法定量。在0.10～5.00μg/mL范围内,相关系数r20.992,样品在0.10～2.00 mg/kg范围内加标,平均回收率在88.83%～111.67%之间,相对标准偏差(RSD)为4.85%～11.35%,检出限(LOD)在0.02～0.05 mg/kg之间。采用该方法对16个白酒样品进行测定,结果表明该法简便、快速、结果准确可靠、灵敏度高,能够满足白酒中6种邻苯二甲酸酯增塑剂检测需求。     

气相色谱-串联质谱法测定白酒中16种增塑剂

采用气相色谱-串联质谱法测定白酒中16种增塑剂的含量。样品经30℃水浴真空旋转蒸发10min去除乙醇后,用正己烷萃取,漩涡振荡1min,取上层有机相用TR-5MS色谱柱分离,选择反应监测扫描(SRM)模式测定。16种增塑剂的质量浓度在5~1 000μg·L-1范围内与其峰面积呈线性关系,检出限(3S/N)在5~15μg·kg-1之间。在50,100,500μg·kg-1等3个浓度水平进行加标回收试验,回收率在70.5%~120%之间,相对标准偏差(n=6)小于15%。     

基于愈创木酚荧光减量准确测定过氧化物酶活性的新方法

利用H2O2/过氧化物酶(POD)/愈创木酚(GA)反应体系的产物(470 nm)吸光度去定量POD活性是目前常用方法之一,但产物不稳定且对比色皿有吸附现象是该反应的主要缺点之一。为了解决此问题,本研究利用GA的荧光特性建立了一种能准确测定POD活性的方法。用辣根过氧化物酶( HRP)作为测试样品得到了以下优化条件：0.5 mmol/L GA,0.5 mmol/L H2O2,0.05 mol/L PBS缓冲液(pH 6.0),反应温度20℃,样品耗量20μL;本方法的线性范围为500~60000 U/L(r=0.9993),RSD≤2.4%(n=11),检出限为385 U/L。在优化条件下,用白萝卜提取液作为测试样品,用本方法((9714依132) U/L)与比色法((9926依352) U/L)和循环催化流动分析法((9608依456) U/L)进行了对比,结果表明,3种方法相互一致性很好。     

Recent progress in the development of polymers for white light-emitting polymer devices

Much effort has been devoted to the design and synthesis of polymers for use in flat panel display, solid state lighting, transistors, and photovoltaic devices. Especially, development of white light emitting polymeric materials has recently attracted much interest owing to their possible use in lighting application and backlights for flat panel displays. White emission has been obtained from polymeric molecules, small organic molecules, organometallic molecules, and phosphor-based or quantum dot-based inorganic molecules. Among materials used in white light emitting diodes, we summarize the white light emitting polymeric materials synthesized and published till December 2007. Correspondence: In Tae Kim, Department of Chemistry, Kwangwoon University, 447-1 Wolgye-Dong, Nowon-Ku, Seoul 139-701, Korea, So Ha Lee, Life Sciences Research Division, Korea Institute of Science and Technology, P.O. Box 131, Cheongryang, Seoul 130-650, Korea.     

Sr2SiO4∶Dy3+材料制备及发光特性

采用高温固相法制备了Sr2SiO4∶Dy3+发光材料. 在365 nm紫外光激发下, 测得Sr2SiO4∶Dy3+材料的发射光谱为一个多峰宽谱, 主峰分别为486, 575和665 nm; 监测575 nm的发射峰, 所得材料的激发光谱为一个多峰宽谱, 主峰分别为331, 361, 371, 397, 435, 461和478 nm. 研究了Dy3+掺杂浓度对Sr2SiO4∶Dy3+材料发射光谱强度的影响. 研究结果显示, 随着Dy3+浓度的增大, 黄、蓝发射峰比值(Y/B)也逐渐增大; 随着Dy3+浓度的增大, 575 nm发射峰强度先增大后减小. 加入电荷补偿剂Li+, Na+和K+均提高了Sr2SiO4∶Dy3+材料的发射光谱强度, 其中以Li+的情况最为明显.     

白光电致发光二极管用发光材料研究进展

白光电致发光二极管(LED)是固体照明的重要光源.荧光体转换是获取白光LED的主要途径之一.当前,转换用荧光体的研究在发光材料领域中最活跃.本文对近年来白光LED用发光材料新体系的研究进展作了评述.     

Luminescence enhancement of Eu, Ce co-doped Ba3Si5O13−δNδ phosphors

Host lattice Ba₃Si₅O_13−δN_δ oxonitridosilicates have been synthesized by the traditional solid state reaction method. The lattice structure is based on layers of vertex-linked SiO₄ tetrahedrons and Ba²⁺ ions, where each Ba²⁺ ion is coordinated by eight oxygen atoms forming distorted square antiprisms. Under an excitation wavelength of 365 nm, Ba₃Si₅O_13−δN_δ:Eu²⁺ and Ba₃Si₅O_13−δN_δ:Eu²⁺,Ce³⁺ show broad emission bands from about 400-620 nm, with maxima at about 480 nm and half-peak width of around 130 nm. The emission intensity is strongly enhanced by co-doping Ce³⁺ ions into the Ba₃Si₅O_13−δN_δ:Eu²⁺ phosphor, which could be explained by energy transfer. The excitation band from the near UV to the blue light region confirms the possibility that Ba₃Si₅O_13−δN_δ:Eu²⁺, Ce³⁺ could be used as a phosphor for white LEDs.     

白色荧光粉NaGd（MoO4）2:Dy3+,Eu3+的水热合成及发光性能

采用谷氨酸辅助水热法合成了八面体形NaGd(MoO4)2:Dy3+,Eu3+白色荧光粉.X射线衍射结果表明,合成的样品为四方晶系的NaGd(MoO4)2纯相.扫描电子显微镜照片显示所制备的粒子为八面体形,各边长约为2μm.荧光光谱结果表明,在NaGd(MoO4)2:4%Dy3+,yEu3+(y=0,0.5%,0.6%,0.7%,0.8%,0.9%,1.0%)样品中,随着Eu3+掺入量的增加,Dy3+的发射峰逐渐减弱,而Eu3+的发射峰逐渐增强,说明Dy3+-Eu3+之间存在能量传递.通过色坐标图可知,当Eu3+掺杂量y=0.9%时,荧光粉的色坐标(0.338,0.281)与标准的白光色坐标(0.33,0.33)接近,表明NaGd(MoO4)2:4%Dy3+,0.9%Eu3+是很好的近紫外光激发下的白色荧光粉.     

Efficient bright white organic light-emitting diode based on non-doped ultrathin 5,6,11,12-tetraphenylnaphthacene layer

High-performance undoped white organic light-emitting diode (OLED) has been fabricated using an ultrathin yellow-emitting layer of 5,6,11,12-tetraphenylnaphthacene (rubrene) inserted at two sides of interface between two N,N′-bis-(1-naphthyl)-N,N′- biphenyl-1,1′-biphenyl-4,4′- diamine (NPB) layers as a hole transporting and blue emissive layer, respectively. The results showed that a maximum luminance of the device reached to as high as 21,500 cd/m² at 15 V. The power efficiencies of 2.5 and 1.6 lm/W at a luminance of 1000 and 10000 cd/m², respectively, were obtained. The peaks of electroluminescent (EL) spectra locate at 429 and 560 nm corresponding to the Commissions Internationale De L’Eclairage (CIE) coordinates of (0.32, 0.33), which is independent of bias voltage. The performance enhancement of the device may result from direct charge carrier trapping in rubrene. Energy transfer mechanism was also found in the EL process.     

High efficiency white luminescence of alumina doped ZnO

The application of alumina-doped ZnO (AZO) films as luminescent material for large area lighting sources has been evaluated. Thin films were grown on quartz using magnetron sputtering and subsequently annealed under argon atmosphere in a rapid thermal annealing experiment. Below 550 °C, red-shift of the optical band gap and increase of the visible emission are observed in agreement with Al diffusion and formation of interstitial oxygen atoms. At temperatures higher than 800 °C, diffusion is activated and Ostwald ripening leads to the formation of larger grains and an increase of the crystalline phase. The photoluminescence (PL) intensity is enhanced, specifically in the UV range. As a result the emission spectrum of AZO thin films can be adjusted by the annealing conditions, with equal contributions from the UV and orange parts of the PL spectrum resulting in an efficient white emission as quantified using the color space map of the Commission Internationale de l'Éclairage.