高盐样品中锂的电感耦合等离子体发射光谱法(ICP-OES)测定研究

锂是重要的战略金属和新能源材料,其开发利用受到全球的高度关注。在高盐卤水特别是盐湖卤水和地下卤水中富含巨量的锂资源,在对这些资源进行锂的开发利用过程中,需对锂的含量进行准确测定,然而卤水中共存的高浓度Na+, K+, Ca2+和Mg2+会对微量锂的准确测定产生严重的干扰。电感耦合等离子体发射光谱法(ICP-OES)具有线性范围宽和多元素同步分析能力,针对卤水中锂的快速准确测定,详细开展了高盐样品中锂的ICP-OES分析方法研究。结果表明,锂在610.364 nm处具有较高的信噪比,且Na+, K+, Ca2+, Mg2+和Ar不会对锂的测定产生显著的谱线干扰。然而,样品中大量共存的Na+, K+和Mg2+会对锂的测定产生严重的基体正干扰,而Ca2+产生负干扰。尽管内标法在消除基体干扰方面具有广泛的应用,但传统的以钇和钪为内标元素的内标法不能有效解决该问题。此外,针对标准加入法操作繁琐、不适合批量样品分析问题,以及基体匹配法需多离子匹配,且不适合样品基体组成变化的批量样品分析等问题,考察了采用单一组分进行复杂基体匹配的可行性。由于NaCl广泛存在于卤水中,且对锂的测定具有显著的增敏效应,通过系列研究发现,通过同时向样品和标准溶液中加入10 g·L-1的NaCl,成功解决了总量不超过40 g·L-1的NaCl, KCl和MgCl2所产生的干扰。尽管采用该法或沉淀预分离方式均不能消除Ca2+产生的负干扰,但当样品中Ca2+含量不高于1.8 g·L-1时,对测定不产生显著的影响。通过采用该方法对三种不同基体组成的卤水样品进行加标回收测定,其回收率在96.60%~104.20%范围内。此外,通过与电感耦合等离子体质谱法(ICP-MS)测定结果进行对比,充分论证了该法的准确性和可靠性(相对误差±3.66%)。该法仅以单一的NaCl进行复杂基体匹配,不仅简化了操作,还实现了基体组成变化的批量样品分析,因而在卤水中锂的快速准确测定及锂资源开发利用方面具有重要意义。     

Minimization of Interferences in Flow Injection Amperometric Glucose Biosensor Based on Oxidation of Enzymatically‐produced H2O2

One of the major problems in amperometric biosensors based on detection of H₂O₂ produced by enzymatic reaction between oxidase enzymes and substrate is the interference of redox active compounds such as ascorbic acid (AA), dopamine (DA) and uric acid (UA). To minimize these interferences, sodium bismuthate was used for the first time as an insoluble pre‐oxidant in the flow injection (FI) amperometric glucose biosensor at a Glucose oxidase (GOx) immobilized Pt/Pd bimetallic modified pre‐anodized pencil graphite electrode (p.PGE). In this context, these interfering compounds were injected into a flow injection analysis (FIA) system using an injector which was filled with NaBiO₃. Thus, these interferents were converted into their redox inactive oxidized forms before reaching the electrode in the flow cell. While glucose was not influenced by the pre‐oxidant in the injector, the huge oxidation peak currents of the interferents decreased significantly in the biosensor. FI amperometric current time curves showed that the AA, DA and UA were minimized by 96 %, 86 %, and 98 % respectively, in the presence of an equivalent concentration of interferences in a 1.0 mM glucose solution. The proposed FI amperometric glucose biosensor exhibits a wide linear range (0.01–10 mM, R²=0.9994) with a detection limit of 2.4×10^?3 mM. Glucose levels in the artificial serum and two real samples were successfully determined using the fabricated FI amperometric biosensor.     

Contrasting confocal with defocusing microscale spatially offset Raman spectroscopy

The study compares and contrasts conventional confocal Raman microscopy/spectroscopy (CRM) with a recently developed micrometer scale defocusing spatially offset Raman spectroscopy (micro‐SORS), a method providing a new analytical capability for investigating non‐destructively the chemical composition of subsurface, micrometer‐scale‐thick diffusely scattering layers at depths beyond the reach of CRM. Because of close similarities between the two techniques and comparable embodiment of the instrumentations, but radically different interpretations of data, it is crucially important to recognise which type of method is pertinent to a specific measurement. The distinction comes principally from the nature of sample, whether turbid (micro‐SORS measurement) or transparent (CRM measurement) on the spatial scale of the axial (z‐)scan of the measurement. Which type of sample one deals with may not always be easily recognisable with micro‐scale thick layers, and the study therefore also presents a simple method for suggesting whether CRM or micro‐SORS methodology applies. This test relies on an axial (z‐)scan performed through the sample in both the positive and negative directions from the normal, imaged sample surface position using conventional CRM instrument. The absence or presence of symmetry or asymmetry of the intensity profiles of measured Raman signals around the imaged sample surface position as a function of sample axial displacement then suggests which interpretation could apply. The study paves a way for the development of micro‐SORS as a widely applicable analytical tool deployable on conventional Raman microscopes. Copyright © 2015 John Wiley & Sons, Ltd.     

一端弹性支撑的串列双柱和并列双柱在气流中自由端的振幅响应

本文研究了一端弹性支撑的并列双柱和串列双圆柱在气流中自由端的振幅响应，与单圆柱相比，在小间距时，串列双圆柱中前柱的横向振幅受到较强的激励。而在大间距时，振幅受到抑制，特别当Ｌ／Ｄ＝３．５和４．０时，其振幅响应仅为单柱的１／３左右，而对于后柱，则在大间距时，纵向振幅响应有所增大，而且后柱的振幅响应要比前柱的大得多，而并列双圆柱的自由端振幅基本上受到抑制，在Ｔ／Ｄ＞３．０之后，干扰很快减小到接近单个圆     

Interference effects of two and three super-tall buildings under wind action

Most previous investigations on interference effects of tall buildings under wind actions focused on the wind induced interference effects between two buildings,and the interference effects of three or more buildings have seldom been studied so far due to the huge workload involved in experiments and data processing.In this paper,mean and dynamic force/response interference effects and peak wind pressure interference effects of two and three tall buildings,especially the three-building configuration,are investigated through a series of wind tunnel tests on typical tall building models using high frequency force balance technique and wind pressure measurements.Furthermore,the present paper focuses on the effects of parameters,including breadth ratio and height ratio of the buildings and terrain category,on the interference factors and derives relevant regression results for the interference factors.     

QoS enhancement in OFDM based systems under transceiver impairments

Broadband wireless systems generally use orthogonal frequency division multiplexing (OFDM) with link adaptation (LA) to achieve high throughput while meeting bit error rate (BER) constraint. OFDM systems are known to be affected by non-linearity of high power amplifier (HPA) at transmitter, carrier frequency offset (CFO), symbol timing offset (STO) and channel estimation error at the receiver. The delay in feedback of channel state information (CSI) further affects the performance of LA procedures. The focus of this work is on performance analysis in presence of simultaneous affect of all these impairments on LA based OFDM systems. The results are found to be useful for threshold readjustment which is essential for successful implementation of LA scheme to counter the effects of change in operating conditions from ideal to as listed above.     

连动型抗干扰干涉具井下瓦斯浓度监测系统（英文）

针对井下甲烷浓度监控干扰大的问题,结合实时监测甲烷浓度的系统要求,设计角镜连动的自消震光学结构,构建了基于无线网络的实时数据通信系统.在干涉系统中,固定两个角镜位置,将两片半透半反镜用连杆结构同步旋转,由此产生光程差.由于采用了连杆结构,任意时刻引入的震动在两个分束镜上等量存在,其结果是差分值,可实现完全相消.由分析分束器的最大旋转范围计算得到系统的光程差变化范围.结合比尔朗伯定律,给出系统在井下工作的甲烷气体浓度最低检出限.分别在实验室及矿井主巷道中完成实验过程,通过化学反应法求得被测甲烷气体的标准浓度,与WQF530型光谱分析仪的测试结果作比较,结果表明:在实验室无干扰条件下,两种检测方法的相对误差均小于1.0%;在井下实验中,传统光学检测方法受环境影响明显,相对误差大幅增加,而本系统测试结果基本稳定,具有较强的抗干扰能力及较高的稳定性.     

基于非同步替代光谱定标的地表下垫面影响分析

对760nm附近的氧气吸收带,选用植被、枯萎植被、人工地物、沙地和雪地五种典型地表类型,基于模拟数据进行非同步替代光谱定标方法的误差分析,比较不同地表类型得到的光谱定标准确度,为高光谱成像仪的非同步替代光谱定标提供定标图像选择策略.结果表明:运用两种光谱匹配方法——光谱角度匹配和欧氏距离法得到的定标误差基本一致;730~800nm的地表反射率曲线标准差在0.05nm以内时,定标误差集中在±0.5nm范围内;人工地物类型中个别地物如橄榄绿光泽涂料和植被大面积覆盖的图像数据不适合用于非同步替代光谱定标.     

基于U型弯曲光纤模间干涉的折射率传感

研究了去包层U型弯曲光纤的折射率传感特性.首先根据模间干涉理论,分析了U型光纤传感器的传感原理,指出干涉谱损耗峰波长与环境折射率和弯曲半径有关.利用单模光纤(SM-28)实验制作不同曲率半径的U型光纤传感器,把传感器的U型部分浸入不同折射率的液体中,研究其折射率传感特性.当U型光纤曲率半径为2.5~5.0mm时,传输光谱中均能观察到明显的模间干涉现象;当液体折射率从1.30RIU变到1.43RIU时,光谱损耗峰波长发生红移,且弯曲半径越大,折射率传感灵敏度越高;在曲率半径为5mm时灵敏度为207nm/RIU(折射率1.30~1.40RIU)和1 220nm/RIU(折射率1.40~1.42RIU).干涉峰的波形参量(半高宽、对比度)决定于包层模和纤芯导模之间的比例,当曲率半径为4mm时,损耗峰半高宽最小达3.2nm.综合半高宽和灵敏度两个参量,得出曲率半径4.5mm的U型光纤传感器品质因素最高,分别为43.1RIU-1(折射率1.30~1.40RIU)和191.2RIU-1(折射率1.40~1.42RIU),可直接由SM-28单模光纤制成,且制作工艺简单、成本低、机械强度高不需要任何特殊处理,具有很好的应用前景.