环境土壤样品微波消解及钚的ICP-MS测量

钚是环境放射性污染调查和核事故应急监测重点关注的污染核素，土壤样品中钚的定量分析包括样品消解、化学分离和仪器测量等3个步骤。为缩短样品消解时间、提高化学分离效率，对土壤样品微波消解和钚的阴离子交换分离进行了研究，建立了微波消解-阴离子交换分离-电感耦合等离子体质谱（ICP-MS）测量 同位素稀释法定量分析污染土壤样品中²³⁹Pu的流程。以6 mol/L盐酸为浸取试剂，在浸取液体积与土壤质量之比为4∶1~5∶1 mL/g时，5 g土壤样品中²³⁹Pu的加标回收率大于99%。以氢氟酸、硝酸和盐酸的混酸为消解试剂，在氢氟酸浓度为13.2 mol/L时，1 g土壤样品中²³⁹Pu的加标回收率大于94%。用所建流程测得的IAEA-375土壤标准样品中²³⁹Pu的含量与参考值无显著差异，该流程对1 g土壤样品中²³⁹Pu的检出限为84 mBq/kg。     

应用膨胀算法提取目标的直接定位算法

为了解决被动雷达系统中的多发射源定位问题，提出了一种基于多重信号分类(MUSIC)算法和图像膨胀(IE)算法的直接定位方法。该方法结合了谱分析中的MUSIC思想，通过对接收量测协方差矩阵进行特征分析求解目标的位置。首先，在目标个数未知的前提下，利用Akaike信息准则(AIC)来确定模型阶数；然后，推导了基于MUSIC的定位代价函数；之后，利用图像膨胀算法处理得到的代价函数平面；最后，膨胀处理后的输出为目标个数及目标位置的估计值。提出的算法有效地解决了目标检测及提取的问题，能够确定多个目标的位置坐标，为后续的定位性能分析提供可能性，也保证了算法的完整性。进一步地分析了多个临近目标情况下影响目标提取性能的主要因素。     

H2-selective mixed matrix membranes modeling using ANFIS,PSO-ANFIS,GA-ANFIS

The novel contribution of the current study is to employ adaptive neuro-fuzzy inference system (ANFIS) for evaluation of H₂-selective mixed matrix membranes (MMMs) performance in various operational conditions. Initially, MMMs were prepared by incorporating zeolite 4A nanoparticles into polydimethylsiloxane (PDMS) and applied in gas permeation measurement. The gas permeability of CH₄, CO₂, C₃H₈ and H₂ was used for ANFIS modeling. In this manner, the H₂/gas selectivity as the output of the model was modeled to the variations of feed pressure, nanofiller contents and the kind of gas, which were defined as input (design) variables. The proposed method is based on the improvement of ANFIS with genetic algorithm (GA) and particle swarm optimization (PSO). The PSO and GA were applied to improve the ANFIS performance. To determine the efficiency of PSO-ANFIS, GA-ANFIS and ANFIS models, a statistical analysis was performed. The results revealed that the PSO-ANFIS model yields better prediction in comparison to two other methods so that root mean square error (RMSE) and coefficient of determination (R²) were obtained as 0.0135 and 0.9938, respectively. The RMSE and R² values for GA-ANFIS were 0.0320 and 0.9653, respectively, and for ANFIS model were 0.0256 and 0.9787, respectively.     

纺织助剂中的甲醛测定

基于更为严厉的甲醛重新分类的背景,TEGEWA协会整理工作组已开发出一种可确定纺织助剂中游离甲醛含量的新方法。目前此法鉴于其统一的程序,可使因不同的内部测试方法而得出不同观点的测试成为过去。     

化学计量学-荧光分析法同时测定甲酚的3种同分异构体

利用化学计量学中的主成分回归法(PCR)和荧光分析法相结合,并用遗传算法(GA)对其进行优化,建立了同时测定甲酚混合物中3种同分异构体的新方法。在p H 4.92的磷酸氢二钠-磷酸二氢钾缓冲介质中,邻、间、对甲酚浓度在3.00~12.0μg/m L范围内,以λ=274 nm为定激发波长,测定300~335 nm波长范围内的荧光光谱,分别使用PCR和GA-PCR两种校正模型对光谱数据进行解析,并同时对3种异构体进行定量分析。研究结果表明,两种方法对邻、间、对甲酚进行预测的平均回收率分别为89.0%、107.5%、100.4%和100.6%、99.1%、98.0%,均方根预测误差分别为0.71、0.49、0.15μg/m L和0.17、0.16、0.21μg/m L,精密度试验的相对标准偏差均小于1.0%,且经GA优化后的PCR方法的加标回收率得到了明显改善,均方根预测误差减小50%,具有更好的准确度。     

卡系费休法测定氯乙烯单体中水含量的影响因素

介绍了卡尔费休法的测定原理,具体分析了采用卡尔费休法测定氯乙烯单体中水含量的影响因素,指出采用闪蒸仪进样器,能有效提高分析结果的准确性和工作效率。     

Simple validated method for simultaneous determination of deoxynivalenol,nivalenol, and their 3-β-D-glucosides in baby formula and Korean rice wine via HPLC-UV with immunoaffinity cleanup

A simple and reliable method for the simultaneous determination of major type B trichothecene mycotoxins, deoxynivalenol (DON) and nivalenol (NIV), along with their 3-β-d-glucosides (DON-3-glucoside (DON3G) and NIV-3-glucoside (NIV3G)) in baby formula and Korean rice wine was validated in the present study. The method was based on immunoaffinity cleanup followed by analysis using an HPLC-UV technique. The method was validated in-house for two matrices as follows: linearity (R² > 0.99) was established in the range of 20–1000 μg kg^–1; accuracy (expressed as recovery) ranged from 78.7 to 106.5% for all the analytes; good intermediate precision (relative standard deviation < 12%), and adequate detection and quantitation limits (< 4.4 and < 13.3 μg kg^–1, respectively) were achieved. Furthermore, the estimated measurement expanded uncertainty was determined to be 4–24%. The validated method was successfully applied to the analysis of 31 baby formulas and Korean rice wines marketed in Korea.     

Deposition of UF5 on the surface of steel material having oxide coating in contact with gaseous UF6

When UF6 is handled in leak tight system, the amount of uranium compound formed on the surface of containers, valves, and others in UF6 handling facilities is not so significant for a short term that special attention has not been given to this problem. The present work was done to throw some more light on this problem based on the recent experiment. We discuss the possibility that the intermolecular transfer of a fluorine atom from UF6 to UF5 may participate in the formation of uranium compound. The discussion includes also the unique features contained in the experimental result, the reaction processes assumed in this problem, and the derivation of a rate equation for expressing the deposition of uranium compound. Furthermore, we propose a new method for determining nonlinear parameters included in a governing differential equation having two variables for expressing the deposition of uranium compound from experimental raw data.     

车用汽柴油中硫成分分析标准物质的研究进展

随着世界各国对环境问题的普遍重视,以及汽柴油标准的不断升级和油品质量检测技术的逐步完善,我国对低硫含量汽柴油标准物质的需求日趋迫切。油品中硫含量过高,大大降低了催化转换器中催化剂效率,增加了车辆污染物的排放量。含硫汽柴油标准物质的研制,是制定汽柴油国家强制标准的急需,是有效控制大气污染的急需,是保障交通安全的急需,对元素分析仪器的校准、汽柴油硫含量检测和定值等方面起到极其重要的作用。旨在通过对国内外车用汽柴油质量标准硫含量现状和发展趋势的分析,拟为汽柴油中硫元素标准物质的研制及快速准确地对汽柴油中硫含量的检测,提供必要依据和借鉴。