基于Android平台的便携式痕量重金属离子检测仪的研制

基于Android平台,设计了一种用于痕量重金属离子检测的便携式电化学分析检测仪。仪器输出电压范围为-3~3 V,精度为0.1%,分辨率<1 mV;电流检测范围为-10~10 mA,精度为0.1%,最小分辨率为10 pA,已达到普通电化学分析的要求。借助Android智能设备在人机交互方面的优势,仪器设有专业检测模式与快速检测模式,简化了复杂的电化学检测分析过程,可同时满足专业用户与普通用户的操作需求。使用本仪器,并结合商品化的电极对Cu, Cd, Pb及Hg等常见的重金属离子进行了初步检测,线性范围、重复性及结果准确度方面都获得了满意的结果。     

基于X射线荧光光谱仪的儿童沙坑重金属污染特征调查研究

儿童沙坑是学龄前儿童重要的户外游乐场所,同时具有较好的雨水下渗性能,导致伴随周边地表径流而来的污染物容易在其中富集。因此儿童在沙坑内玩耍时,面临重金属类污染物进入体内的健康风险。研究利用X射线荧光光谱法（XRF）快速、无损的检测特点,对北京市儿童沙坑重金属污染特征进行调查。结果表明：（1）XRF对自制标准试样中Pb,Cu,As和Cd的测量值与理论值的准确度为-1.3%～7.5%,精确度在1.1%～5.3%范围内,均符合相关环境质量检测技术规范中规定的仪器检测准确度和精密度要求（均小于10%）;（2）4种重金属测量值与理论值之间均呈现极显著正相关关系（p<0.001）,其决定系数（R2）分别为0.999,0.999,0.996和0.998,基于结果建立了测量值和理论值的拟合方程;（3）应用XRF对北京市17家公园和13个居民小区内儿童沙坑重金属含量进行测定,两组样点中Pb和As含量差异显著,而Cu和Cd含量无显著差异。4种重金属标准差的变异系数范围在0.24～0.43,其中除Cd的变异系数小于0.3外,其余重金属均大于0.3,表明空间变异明显;（4）与北京市土壤元素背景值相比,样点儿童沙坑4种重金属平均含量除As外,Pb,Cu和Cd明显高于背景值,分别是背景值的1.87和1.53,1.79和2.23,12.02和11.68倍。由此可见,采样点儿童沙坑内Pb,Cu和Cd都有不同程度的富集,其健康风险不容忽视。XRF可以为儿童活动场所管理和维护提供准确、快速的数据支撑。     

基于基体效应校正和对应分析的便携式X荧光光谱法对土壤重金属的研究

随着工业化和城市化的加深,城市土壤重金属污染状况愈发严重,而传统的实验室化学分析方法例如电感耦合等离子体质谱法分析周期较长,易产生废弃实验试剂二次污染环境。便携式X荧光光谱法是一种可以在野外现场直接进行快速、无损分析的测试手段,而基体效应是影响该方法测试准确度和精密度的最主要因素。当今较为常用的校正方法为传统线性回归法,该方法受离群值影响较大,处理后数据依然存在较大的偏差。本研究通过将常量元素的测试数据加入到待测元素的校正方程中,来减弱测试过程中基体效应的影响。利用便携式X荧光光谱仪对吉林大学各校区土壤样品的Cr,Ni,Cu,Zn和Pb重金属含量在原位条件下进行了快速测试,探究了对各重金属元素基体效应影响最大的常量元素,并结合偏最小二乘法及多元线性回归对原始谢尔曼方程进行调整,利用电感耦合等离子体质谱法作为参照,通过新方程对各重金属元素进行了基体效应校正,通过统计学参数对比该方法处理后的数据和经传统线性回归法处理后的数据的区别,并通过对应分析综合分析元素及样品间的相关性。结果表明常量元素是基体效应影响的重要元素,基于不同常量元素的基体效应校正方程效果较好,适用性Cr>Pb>Zn>Ni>Cu,校正后数据质量得到了明显提高,决定系数增大,回归图像更加集中,平均绝对误差、均方根误差等参数均进一步减小,校正效果优于传统的线性回归法。基体效应校正法主要是通过减小离群值的偏离程度来减小数据总体的平均误差和离散程度。处理后数据满足定量分析要求,可以推广至便携式X荧光光谱法对于土壤重金属快速的大面积扫面测试,检测环境质量。同时对应分析是一种多维数据维度与多维数据维度之间的分析方法,用于多种变量间的分类与相关性分析具有非常优秀的效果。     

Determination of ultratrace nitrogen in pure argon gas by dielectric barrier discharge-molecular emission spectrometry

A dielectric barrier discharge (DBD) was used as a new atmospheric optical emission detector for the determination of trace nitrogen in pure argon gas in this work. The whole system was composed of an ac ozone generation device for power supply, a six-way valve, a laboratory-built DBD device and a USB2000 charge coupled device (CCD). Trace nitrogen in argon was detected at nitrogen molecular emission line of 337 nm. This method features with several advantages: atmospheric working condition, low power consumption (≤ 12 W), simple and cheap instrumentation, fast response and high sensitivity and accuracy. Under the optimized conditions, the limits of detection can be down to 34 ppb.     

Membrane-introduction mass spectrometry (MIMS)

Membrane-introduction mass spectrometry (MIMS) for chemical analysis involves directly sampling analytes in gaseous, liquid and solid samples through a semi-permeable membrane coupled to a mass spectrometer, yielding selective and sensitive quantitation. Because MIMS is an on-line technique, in which samples can be continuously flowed over a membrane interface, it can yield analytical results in real time without the need for sample clean-up and chromatographic separation. This review highlights trends and developments in MIMS over the past decade and describes recent studies that pertain to its use for on-site, in-situ and in-vivo chemical analysis. We report on advancements in instrumentation, including membrane materials, interface configurations and ionization techniques that have extended the range of analytes amenable to MIMS.We summarize the progress made in the miniaturization of mass spectrometers that have resulted in field-portable systems and review recent applications of continuous mobile monitoring and on-site environmental monitoring to yield both temporally and spatially resolved quantitative and semi-quantitative data. Finally, we describe recent work involving the use of MIMS for in-vivo chemical analysis.     

On‐site sampling and sample‐preparation approach with a portable sampler based on hollow‐fiber/graphene bars for the microextraction of nitrobenzene compounds in lake water

A novel on‐site sampling and sample‐preparation approach was developed and evaluated in the present work. In this procedure, hollow‐fiber/graphene bars (HF/GBs) were used for sampling and sample preparation. A handheld battery‐operated electric egg beater was utilized to support the HF/GBs and stir the sample solution to facilitate extraction at the sampling site. Four nitrobenzene compounds (nitrobenzene, o‐nitrophenol, m‐nitrophenol, and p‐nitrophenol) were used as model compounds. Several factors affecting performance, including types and amount of graphene used and extraction and desorption times, were investigated and optimized in the laboratory. Under optimized conditions, the enrichment factors of the four nitrobenzene compounds ranged from 46 to 69. Good linearities of 0.01–10 μg/mL with regression coefficients between 0.9917 and 0.9973 were obtained for all analytes. The LOD of the method was 0.3 ng/mL. Satisfactory recoveries (98–102%) and precision (1.0–5.8%) were also achieved. The ultrastructures and extraction mechanism of the HF/GBs were characterized and analyzed. The proposed approach coupled with high‐performance liquid chromatography was successfully applied in the extraction and determination of trace nitrobenzene compounds in lake water. Experimental results showed that the approach is simple, convenient, rapid, and practical for routine environmental monitoring.     

基于FPGA的便携式轴承状态监测仪设计

本文提出了一种基于FPGA的便携式轴承状态监测巡检仪的设计方案。介绍了模拟信号放大电路、滤波电路、包络检波电路和电源管理电路等硬件电路设计以及FPGA功能模块设计和软件工作流程。本仪器通过提取分析加速度高频包络信号实现了轴承状态监测功能,利用了FPGA的并行处理优势实现低功耗高性能的优点。     

一种便携式多生理参数采集系统的设计

本文设计了一种便携式多生理参数采集系统。该系统可以实现对人体呼吸、指脉、动作、皮电、血压、心电等六个体征参数的采集;该系统利用串口转USB传输可以实现采集到的人体生理参数与PC间的相互传输,测量结果和分析报告可以在PC 机进行实时显示和存储或者可以通过Internet向远程医疗服务中心进行数据的上传、备份、分析与反馈。所以,利用该系统可以实现对人体体征参数实时、连续的采集与监测。     

便携式自调心小型圆度仪控制系统设计

设计一种简单易行的便携式小型圆度仪的自动调心控制系统方案,使圆度仪的调心功能能够自动实现,不需要繁琐的人工找心定心步骤,提高圆度仪的测量效率,节省测量时间。此设计适合测量小型工件。传感器采用差动电感传感器(LVDT);使用集成电感传感器处理芯片;采用MC9S12DG128型单片机为主控芯片,偏心量采用DFT算法计算,转台的回转及调心都使用微步进电机实现。     

On-site environmental analysis by membrane extraction with a sorbent interface combined with a portable gas chromatograph system

A novel device, membrane extraction with a sorbent interface (MESI) coupled with a portable gas chromatograph (GC) system, has been developed. The main components of this system include a membrane module, a microtrap, and a control unit for the heater and cooler. The membrane module, as an on-line sample-introduction device for this system, can be manipulated in different configurations, allowing for the selective permeation of analytes across the membrane into the carrier/stripping gas. The analytes are trapped and concentrated onto a microtrap, which serves as an injector for gas chromatography separation. A concentration pulse of the trapped analytes is generated through direct electrical heating of the microtrap. The characteristics of this system have been explored, and its applicability and effectiveness have been demonstrated in field monitoring applications including the analysis of toluene in wastewater, Volatile organic compounds (VOCs) in laboratory air, and chloroform in swimming-pool water. This system is very promising, as it is a simple, fast, and portable tool for on-site process environmental monitoring.