枪头式分散固相微萃取柱方法结合气相色谱-串联质谱测定果蔬中9种农药多残留

目的建立枪头式分散固相微萃取柱(disposable pipette extraction, DPX)结合气相色谱-串联质谱法同时测定番茄、苹果、小青菜3种水果蔬菜中的9种农药残留的方法。方法水果蔬菜样品经均质,乙腈抽提,采用DPX-RP枪头式分散固相微萃取柱进行净化。采用气相色谱-串联质谱法-多反应模式监测(multiple reaction monitoring, MRM)测定,内标法定量。结果9种农药化合物在10～800μg/kg浓度范围内呈现良好的线性关系,相关系数均大于0.995,方法的检出限为0.3～4.7μg/kg,定量限为1.2～13.5μg/kg。分别在番茄、苹果、小青菜中添加水平为50、250、500μg/kg的混标,平均回收率为72.8%～115.9%,方法的相对标准偏差(relative standard deviation, RSD)为0.29%～9.9%,通过与DPX多通道半自动前处理仪结合使用可在10 min内净化处理1～48个样品,有效缩短了样品前处理的时间。结论本方法简便、省时,并且高通量,适用于水果蔬菜中农药残留的测定。     

移液器容量自动校准系统研究

针对移液器人工校准中存在的按压不稳、温度偏差、数据无法批量处理等缺陷,提出了一种基于模拟人工按压的移液器容量自动校准方法。通过测量移液器按钮2个停止点的压力值,获取近似按压的距离;分析数据并与人工操作进行比对,得出模拟手动按压的最佳按压距离。开发了一套同时校准4支移液器容量的自动化装置,采用机械手和LabVIEW软件智能控制取液、排液、称量、数据处理等工作,实现了自动校准。研究结果表明,与人工操作相比,重复性减小了0.0%~0.9%,相对误差减小了0.1%~0.7%。     

单标线吸量管容量测量值的不确定度评定

以10mL单标线吸量管容量测量值为例,说明常用玻璃量器不确定来源、评定方法及步骤。     

Comparison of Subsieving Techniques Based on the Relation of Particle Size and Specific Surface Area in Mineral Processing

This investigation is concerned with the comparison of the advantages and disadvantages of subsieving techniques widely used in mineral processing throughout the world. With this purpose, the subsieving techniques of Andreasen pipette, Coulter counter, and laser diffraction methods were compared each other by determining the relationship between specific surface area and particle size distribution. In the tests, the two different standard quartz sand samples (A and B) from the Official Material Testing Institute for Nonmetallic Minerals, Clausthal-Zellerfeld with a particle density of ρ = 2.65 g/cm³ were used. As a result, the Coulter counter method had the most favorable results in terms of calculated specific surface areas of 3848 cm²/g for sample A and 2852 cm²/g for sample B, with standard deviations 41.29 and 32.48, respectively.     

Convective assembly of linear gold nanoparticle arrays at the micron scale for surface enhanced Raman scattering

A convective assembly technique at the micron scale analogous to the writing action of a “pipette pen” has been developed for the linear assembly of gold nanoparticle strips with micron scale width and millimeter scale length for surface enhanced Raman scattering (SERS). The arrays with interparticle gaps smaller than 3 nm are hexagonally stacked in the vicinity of the pipette tip. Variable numbers of stacked layers and clean surfaces of the assembled nanoparticles are obtained by optimizing the velocity of the pipette tip. The SERS properties of the assembled nanoparticle arrays rely on their stacking number and surface cleanliness.      

膨胀土粒径分布测量方法的试验研究及曲线拟合

土体的粒度成分在土体的定名、鉴别、描述及预测土体工程性质上具有重要应用。为了研究非饱和土体粒度成分的测量方法及测量结果,本文分别采用密度计法、移液管法和激光粒度仪法对合肥地区9种非饱和膨胀土进行了粒度测量,得到了相应的粒径分布,并采用 Fredlund模型进行了曲线拟合,得到了试验土体的粒径分布曲线（PSD ）,求得了相应的曲线拟合参数的均值、均方差及变异系数。在此基础上,对3种测量方法的PSD曲线拟合参数进行了回归分析,求得了激光法的PSD拟合参数与传统的密度计法及移液管法的PSD拟合参数间的相关关系。     

一种基于加样针结构的电容法液位检测系统

为实现全自动凝血分析仪加样过程高灵敏度和高精度的液位检测,采用了电容传感器原理和步进电机运动控制相结合的方法。介绍了探针式电容传感器的结构与工作原理;分析了电容/周期转换法的检测原理;组建了实验系统对灵敏度和测量精度进行检测。实验结果表明：加样针接触液面的瞬间,脉冲周期发生40%左右的显著变化,液位测量的标准差为4.1μm。