HZMMA对离子聚合物/聚氨酯(脲)弹性体合金增强机制的研究

采用热失重分析(TG)和原位红外研究了含有不饱和双键和羟基的单甲基丙烯酸锌(HZMMA)的化学反应行为;采用X射线衍射(XRD)、扫描电子显微镜(SEM)研究了HZMMA由于其官能团的反应而发生的结构与形态变化。结果表明,针状的HZMMA晶体在引发剂的作用下能自聚形成大小不等的粒子,证实了HZMMA作为反应型增强剂用于制备离子聚合物/聚氨酯(脲)弹性体合金的可能性。以HZMMA作为增强剂,采用预聚体法,以PTMG-1000/甲基二异氰酸酯(TDI)为原料制备预聚物,与自制的混合扩链剂制备出了含有不同量的离子聚合物聚氨酯(脲)弹性体合金,研究了HZMMA的用量对离子聚合物/聚醚型聚氨酯(脲)合金力学性能的影响。当HZMMA的质量分数为0.2%、过氧化二异丙苯(DCP)质量分数为0.2%时,离子聚合物/聚醚型聚氨酯(脲)合金表现出最优的力学性能。     

Analysis of Ochratoxin A in Wine by High-Resolution UHPLC-MS

A method for determination of ochratoxin A (OTA) in wines using a new-solid phase extraction clean-up procedure followed with ultra performance liquid chromatography (UHPLC)-Orbitrap MS based on two scan events (full-scan Fourier transform mass spectrometer [FTMS] and higher energy-induced collision dissociation[HCD] data-dependent MS/MS) in positive ionization mode has been developed. The limit of detection (LOD) was estimated at 0.46 μg l^?1 for white wine, 0.53 and 0.54 μg l^?1 for rosé and red wines, respectively. The limit of quantification (LOQ) was estimated at 1.57 μg l^?1 in white wine, 1.77 and 1.81 μg l^?1 in rosé and red wines. Recovery experiments were carried out with spiked samples at three concentration levels (2, 5 and 10 μg l^?1). The OTA recoveries in spiked white wine samples varied from 69.6 % to 99.8 %, while the recoveries for rosé and red wine samples were in the range of 63.0–110.2 % and 63.6–103.2 %, respectively. Finally, based on the results, it is concluded that the combination of C18 cartridge with conventional particle packed columns and UHPLC LTQ-Orbitrap XL is an appropriate procedure for OTA analysis in wines.     

金属锌表面超疏水薄膜的耐蚀及摩擦学性能的表征

目的改善金属锌在海洋环境中的耐蚀及摩擦学性能。方法通过简单的化学刻蚀及自组装技术在金属锌表面制备超疏水薄膜,对薄膜的结构和润湿性进行了表征,研究了超疏水薄膜在模拟海水(3.5%Na Cl溶液)中的耐蚀性能和摩擦学性能。结果经N,N-二甲基甲酰胺水溶液刻蚀后,金属锌表面呈多尺度微纳的Zn O结构,Zn O结构经硬脂酸修饰后,表面呈现出超疏水特性,表面静态接触角达150°,滑动角小于5°。同时发现,在3.5%Na Cl水溶液中,金属锌表面超疏水薄膜具有优异的耐蚀性能,并能够显著降低摩擦和磨损。结论经简单的化学刻蚀及自组装技术可在锌表面构筑超疏水薄膜,薄膜在海洋环境下具有良好的耐蚀、减摩及耐磨性能。     

同位素稀释高压液相色谱-串联质谱法测定 鱼虾中丙酸睾酮残留量

目的 采用高压液相色谱-串联质谱(high pressure liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)快速检测鱼虾等水产品中丙酸睾酮残留。方法 向捣碎匀浆后的样品中加入内标诺龙-D3混匀后, 叔丁基甲醚超声提取, 80 ℃冷冻30 min后12000 r/min离心净化。以Eclipse Plus C18为色谱分离柱, 以乙腈0.1%甲酸水溶液为流动相, 流速为0.3 mL/min, 采用三重四极杆质谱在正离子模式下进行选择反应离子监测。结果 丙酸睾酮在0.5~100 ng/mL范围内呈线性关系, 相关系数为0.9989; 方法定量限为0.5 μg/kg。当添加水平为0.5~10.0 μg/kg时, 平均回收率为71.2%~104.5%, 相对标准偏差为2.26%~5.65%。结论 该方法操作简单、快速、灵敏度高, 适用于快速检测水产品中丙酸睾酮的残留量。     

内核密度分布与自举法对纺织品镉含量代表值估计

测定了国产织物样品中的镉含量,对镉含量基础统计学特征进行了描述,采用内核密度分布估计对镉含量数据的多态性进行分析,根据非正态分布的特点,使用Bootstrap法对样本值模拟重复取样,以多次Bootstrap模拟取样的均值与标准偏差作为被考察样品有限单次样本代表值及标准偏差的稳健估计。实践证明:该方法得到的均值与标准偏差作为有限单次样本代表值是合理、有效的,该研究为纺织品禁限用物质的风险评估中禁限用物质含量的表述提供了一种新方法。     

Application of nitriding to electroless nickel–boron coatings: Chemical and structural effects; mechanical characterization; corrosion resistance

Electroless nickel–boron coatings, synthesized on mild steel, were submitted to nitridation treatments in varying conditions of pressure, temperature and atmosphere composition. One treatment was carried out under a reduced pressure of a nitrogen-based gas, the other under ambient pressure in a ammonia-based atmosphere.The modifications of the samples’ chemistry after those treatments were investigated by ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectroscopy), GD-OES (Glow Discharge-Optical Emission Spectroscopy) and ToF-SIMS (Time of flight-Secondary Ions Mass Spectroscopy) analysis. Their structures and morphology were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM) and optical microscopy. The mechanical properties of the samples were investigated by micro- and nanohardness measurements successively on the free surface of the sample and on polished cross-sections; their roughness and resistance to scratch test were measured. Electrochemical corrosion tests were also carried out.The effects of both treatments were then compared: after the treatment carried out under lowered pressure, the coatings are dense, present signs of solution hardening and are characterized by a high hardness (close to 1600 hv₁₀₀). A combination layer is observable on the samples treated under an ammonia-based atmosphere. This outer layer possesses poorer mechanical properties but the inner layer of the coating presents properties similar to those of vacuum nitrided coatings. The corrosion resistance of the coatings is as good as that of heat treated coatings.     

烯酰吗啉在大葱中的残留消解动态

采用气相色谱质谱法测定了烯酰吗啉在春季大葱中的残留消解动态和最终残留量.样品经乙腈提取,SAX/PSA固相萃取柱净化,气相色谱质谱选择离子(GC/MS/SIM)检测.结果表明:方法在0.01～0.1 mg/kg水平的平均添加回收率为96.2%～105.7%,相对标准偏差为3.5%～5.7%,烯酰吗啉最小检出量为0.02 ng,最低检测质量分数为0.002 mg/kg.烯酰吗啉在大葱中消解较快,半衰期为3.5 d,药后14 d消解95%以上.50%烯酰吗啉可湿性粉剂按推荐剂量(300 g a.i./hm2)和加倍剂量(600 g a.i./hm2)对水喷雾2～3次,末次施药后7、14、21 d烯酰吗啉在大葱中残留量为0.0094～0.681 mg/kg,低于日本规定的最大允许残留量(MRL).     

HACCP体系在出口冷冻蒜泥微生物控制中的应用

针对目前我国出口冷冻蒜泥微生物控制方面的实际困难,探讨出口冷冻蒜泥HACCP体系建立过程中微生物关键控制点设置的有关问题。对关键控制点及关键限值的确定提出建议,并针对整个食品链中需加强微生物控制的环节提出可行措施,以有效应对进口国针对我国出口冷冻蒜泥的微生物技术壁垒。