气相色谱-质谱法检测白酒和黄酒中18种邻苯二甲酸酯类增塑剂

建立了白酒和黄酒中增塑剂的液液萃取法提取,气相色谱-质谱法检测技术,内标法定量。考察了基质效应,萃取方法等主要条件,并最终确定正己烷为提取溶剂的液液萃取技术,并且提取过程中加入NaCl和H2O。在优化的条件下,18种增塑剂均具有较好的线性相关性,线性相关系数均大于0.9978,白酒和黄酒的添加回收率、相对标准偏差分别为75.7%~97.5%、2.3%~6.7%和74.8%~96.0%、1.9%~7.1%;检出限均小于0.05 mg/kg。方法可为酒中增塑剂检测的标准方法的建立提供参考。     

激光微织构硬质合金表面润湿性

为了研究硬质合金表面激光微织构对其表面润湿性的影响,利用光纤激光不同功率(3,5,7,9,10W)及不同加工次数(1,2,3,4,5)加工微凹坑,采用VHX1000c超景深三维显微镜、光学显微镜分析微凹坑形貌,利用CAM 200光学接触角仪测量表面微织构(微凹坑直径、深度和织构密度)与润湿性之间的关系。结果表明:随着激光功率的增大,微凹坑深度增加,直径变化不明显;硬质合金表面的亲水性能随着微凹坑深度的增加而减小;随着微凹坑直径的增大,亲水性增强;随着微织构密度的增加,亲水性出现极值。     

超高效液相色谱-串联质谱法分析化妆品中的常见抗生素及甲硝唑

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)测定化妆品中常见的6种抗生素(美满霉素、土霉素、四环素、金霉素、多西环素、氯霉素)及甲硝唑的方法,并用于实际样品的分析。样品经甲醇-0.1 mol/L甲酸溶液(体积比为1∶1)超声提取后,以甲醇(含1%甲酸)-水(含1%甲酸)为流动相,经UPLC梯度洗脱分离后以多反应监测(MRM)模式质谱测定。方法的检出限为3～20 ng/g,回收率为87%～101%,工作曲线的线性相关系数大于0.995,线性范围为2～1000 μg/L (达3个数量级)。对11份市售化妆品进行分析检测,其中2份检出氯霉素,质量分数分别为0.37%和0.19%;1份检出甲硝唑,质量分数为1.02%;美满霉素、土霉素、四环素、金霉素、多西环素未检出。     

Raman scattering studies on the collapsed phase of CaCo_2As_2

In this work,Raman scattering measurements have been performed on the collapsed phase CaCo_2As_2 crystals.At least 8 Raman modes were observed at room temperature though CaCo_2As_2 is structurally similar to other 122 compounds like BaFe_2As_2.Two Raman modes are assigned to the intrinsic A_(1g)and B_(1g)of this material system respectively.The other ones are considered to originate from the local vibrations relevant to cobalt vacancies.Careful polarized measurements allow us to clearly resolve the four-fold symmetry of the B_(1g)mode,which put strong constraints on possible point group symmetries of the system with Co vacancies.The temperature-dependent measurements demonstrate that the anomalies in both frequency and width of the B_(1g)mode occur around Neel temperature T_N.The anomalies are considered to be related to the gap opening near the magnetic transition.The study may shed light on the structural and magnetic changes and their correlations with superconductivity in 122 systems.     

激光诱导2024铝合金表面动态应变检测

采用PVDF贴片传感器对脉冲激光作用下2024铝合金表面的动态应变进行了测量,分析了动态应变曲线的特性。结果表明,PVDF贴片传感器在动态应变测量中动态响应快,灵敏度高,可有效应用于脉冲激光诱导材料表面动态应变的实时测量。脉冲激光作用过程中,2024铝合金冲击光斑周围材料先受挤压,后压应变减小。脉冲激光作用结束后,2024铝合金冲击光斑周围材料表面粒子在卸载稀疏波和表面稀疏波的作用下不断往复运动,冲击光斑周围材料甚至受到了拉应变的作用。最后随着时间的推移,材料表面粒子的动态响应经反复震荡后逐渐衰弱形成最终的稳定状态。     

3-氨基吲唑、炔醛和NIS串联环化反应合成碘化嘧啶并[1,2-b]-吲唑

本文开发了一种在无需外加添加剂的条件下合成碘代嘧啶并[1,2-b]-吲唑类化合物的方法。经研究发现,3-氨基吲唑、炔醛和碘代丁二酰亚胺在二氯甲烷中室温条件下发生直接串联环化反应,以中等至良好的产率得到碘代嘧啶并[1,2-b]-吲唑类化合物。该反应有较好的底物适应性,并具有绿色环境友好和操作简便等优点。     

反向能量传递增强Er^(3+)上转换发光EI北大核心CSCD

提高上转换发光效率是促进上转换发光材料实际应用的关键。在NaErF_(4)@NaYF_(4)体系中,惰性NaYF_(4)壳层可以抑制高组分Er^(3+)掺杂下的发光浓度猝灭,其上转换发光主要来源于Er^(3+)-Er^(3+)的能量传递上转换。本文利用共沉淀法制备了Er^(3+)和Yb^(3+)分区掺杂的NaErF_(4)@NaYbF_(4)@NaYF_(4)核壳结构的纳米颗粒,通过包覆惰性壳层研究Er^(3+)-Yb^(3+)-Er^(3+)之间的能量传递和反向能量传递过程。由于808 nm波长只能激发Er^(3+)而不能激发Yb^(3+),因此在808 nm波长激发下,Er^(3+)在惰性壳层的保护作用下将激发态能量传递给Yb^(3+),随后通过反向能量传递回Er^(3+),使得Er^(3+)的上转换发光增强。实验结果发现,当中间层Yb^(3+)掺杂浓度为100%时,绿色和红色上转换发光最大增强倍数为24.9和9.79。     

Optical study of charge dynamics in CaCo_2As_2

We present an infrared spectroscopy study of charge dynamics in CaCo_2As_2 single crystal. In this material, the optical conductivity can be described by two Drude components with different scattering rates(1/τ): a broad incoherent background and a narrow Drude component. By monitoring the temperature dependence, we find that only the narrow Drude component is temperature-dependent and determines the transport properties. Especially a Fermi liquid behavior of carriers is revealed by the T~2 behavior in the dc resistivity ρ_n and scattering rate 1/τ_n, indicating a coherent nature of quasiparticles in the narrow Drude subsystem.     

Magnetoresistivity and filamentary superconductivity in nickel-doped BaFe_2As_2

We present magnetotransport studies on a series of BaFe_(2-x)Ni_xAs_2(0.03 ≤ x ≤ 0.10) single crystals. In the underdoped(x = 0.03) non-superconducting sample, the temperature-dependent resistivity exhibits a peak at 22 K, which is associated with the onset of filamentary superconductivity(FLSC). FLSC is suppressed by an external magnetic field in a manner similar to the suppression of bulk superconductivity in an optimally-doped(x = 0.10) compound, suggesting the same possible origin as the bulk superconductivity. Our magnetoresistivity measurements reveal that FLSC persists up to the optimal doping and disappears in the overdoped regime where the long-range antiferromagnetic order is completely suppressed, pointing to a close relation between FLSC and the magnetic order.     

激光冲击诱导弹簧钢丝残余应力状态分析

利用高功率Nd:YAG激光对不同工艺处理的SWOSC-V弹簧钢丝进行单点冲击处理,用X射线应力分析仪测量弹簧内外侧、侧表面的残余应力并计算出残余主应力,建立了激光冲击SWOSC-V弹簧钢丝表面残余应力的产生模型,并利用该模型分析了弹簧钢丝表面残余应力产生的原因。结果表明:弹簧钢丝在经激光冲击处理的表面强化区产生残余压应力,钢丝退火后直接激光冲击处理与经喷丸强化的钢丝激光冲击处理的表面残余应力变化不同,喷丸强化所引起的材料硬化是激光冲击处理弹簧钢丝残余应力变化不同的原因。