固相萃取-气相色谱法检测水中的邻苯二甲酸酯

利用固相萃取技术富集了水中4种邻苯二甲酸酯类（PAEs）化合物：邻苯二甲酸二甲酯（DMP）、邻苯二甲酸二乙酯（DEP）、邻苯二甲酸二丁酯（DBP）、邻苯二甲酸二（2-乙基己基）酯（DEHP）。借助均匀设计法及计算机回归建模优化技术对4种PAEs的固相萃取条件进行了设计与优化，得到的最佳固相萃取条件：洗脱剂配比（正己烷与丙酮的体积比）30：1，洗脱体积2mL，洗脱速率4mL／min，上样速率8mL／min。富集后的试样用带电子捕获器的毛细管气相色谱仪检测，方法的线性范围为1～1000μg／L（DMP，DEP），0．2—100μg／L（DBP，DEHP），线性回归方程的相关系数为0．9970～1．0000，检出限为0．02-0．4μg／L，4种PAEs的回收率为69％～117％，相对标准偏差为2．5％～9．5％。[关键词]     

微波场协同提取金银花黄色素的正交工艺优化研究

目的是研究金银花黄色素的最佳提取工艺条件。采用正交试验法，以提取剂与原料用量比（A）、提取时间（B）、微波功率（C）和提取次数（D）4个因素，每个因素选取3个水平进行实验，提取次数与微波功率对提取有极显著影响。其最佳工艺条件为：提取剂为无水乙醇，提取剂与原料用量比为1：50（g／ml），提取时间为50s，微波功率为700W，提取次数为3次。     

格栅类通透性吊顶对自动喷水灭火系统水量分布影响的实验研究

本文通过实验研究了自动喷水灭火系统在安装格栅类通透性吊顶后的水量分布特性。研究结果表明：格栅会严重改变自动洒水喷头的水量分布，其影响与喷头的安装高度和工作压力有关。当压力增加时，无格栅区域的水量增加明显大于有格栅的区域的水量增加。增大水压时，格栅对水量的分布的影响会减弱，当压力足够大时，能够接近无格栅时的灭火效率，可以保证自动喷水灭火系统在安装格栅吊顶后的灭火有效性。本文研究成果对实际工程应用具有指导意义。     

Evaluation and comparison of alarm reset modes in advanced control room of nuclear power plants

An automation function has been widely applied in main control room of nuclear power plants (NPPs). The alarm system of fourth nuclear power plant (FNPP) in Taiwan is also going to be developed with automatic technology that is expected to support the operators’ performance and reduce the number of alarms. In this study, an experiment with a training simulator as an advanced alarm system was conducted to compare the effects of different alarm reset modes on performance and subjective ratings. The objective was to evaluate the practicability of alarm system with only auto-reset function in FNPP. Results revealed that, using the auto-reset mode, participants had lower task load index (TLX) on effort in the first test trial and was more satisfied under multi-task condition. In contrast, using manual reset mode, participants were more satisfied on alarm handling, monitoring, and decision making. In other words, both reset modes are necessary to assist the operator in different aspects, but with only single reset mode is insufficient. The reset function in advanced alarm system therefore should be very flexible.     

Sustainable oil-in-water analysis using a supercritical fluid carbon dioxide extraction system directly interfaced with infrared spectroscopy

A direct aqueous supercritical fluid extraction (SFE) system using carbon dioxide provides a sustainable means by which a vast range of industries may continue to depend on well established infrared (IR) techniques to determine oil-in-water. The SFE-IR method provides an environmentally friendly substitute for current national standard IR reference methods for measuring oil-in-water that rely on using increasingly restricted ozone depleting solvents whose manufacture is being phased out in accordance with international law. The SFE-IR analysis of a 500 mL water sample can be accomplished in 15 min. A rapid on-line SFE-IR calibration method has been implemented. With this calibration method, SFE-IR accuracy for determining diesel oil in 500 mL spiked water samples using single wave number measurement was 86.0%–98.8% with precision (RSD) ranging from 2.5%–7.0%. Using a general purpose calculation which involves measuring infrared absorbance values at three di erent wave numbers, SFE-IR method accuracy for determining diesel oil in 500 mL spiked water samples was 83.7%–92.2% with RSD 1.0%–9.3%. Data is presented that indicates current long established national standard IR reference methods involving three wave number calculations should be reviewed since, without careful consideration, the inclusion of calculated aromatic hydrocarbon species contributions to final oil-in-water concentration values may provide less accurate results.     

喷涂废水中邻苯二甲酸酯测定的优化研究

选取固相萃取GC-MS法定量检测喷涂废水中四种邻苯二甲酸酯类(PAEs),运用正交设计法,研究了pH、洗脱剂、洗脱体积、洗脱速率和水样流速对废水中PAEs回收率的影响。结果表明,pH为2.5时回收率最佳(均100%);在该pH下,洗脱剂对4种PAEs的回收率影响最大,水样流速次之,洗脱速率与洗脱体积对4种PAEs的回收率影响相对较小。样品前处理最优参数为:水样流速8mL/min、洗脱剂为乙酸乙酯、洗脱体积4mL、洗脱速率2mL/min;该条件下4种PAEs的线性范围为0.2～8.0μg/mL,相关系数均0.99,喷漆废水中平均加标回收率为61.1%～103%,相对标准偏差为3.1%～14.6%,均可满足试验要求。     

武汉市地下水中酞酸酯污染物检测及来源分析

在武汉市区长江与汉江交界地带采集了具有代表性的地下水水样。采用固相萃取-气相色谱联用法对样品中的痕量邻苯二甲酸酯污染物进行定性定量分析,方法线性范围1ng/L～1000ng/L,检出限22ng/L～341ng/L。武汉市地下水中邻苯二甲酸酯的检出种类主要包括DBP、DEHP与DIBP等3大类。DBP污染最严重的地点在S1(东西湖区),浓度达1023.8ng/L;DEHP污染最严重的地点在S4(常青花园),浓度达481.0ng/L;DIBP污染最严重的地点在S9(唐家墩),浓度达237.8ng/L。将检测结果与武汉市湖泊水,长江、汉江武汉段,武汉市垃圾填埋场垃圾渗滤液中的PAEs污染物种类及浓度进行对照,并结合采样点周边环境与水文地质条件进行分析。确定了PAEs污染物的土壤淋滤作用,汉江、长江水体对地下水的补给以及垃圾填埋场垃圾渗滤液的渗滤作用是武汉市地下水PAEs污染物的主要来源。     

润滑油废白土的应用探索

针对炼油企业废白土排放污染环境问题,在实验室中利用溶剂进行脱油处理,其脱油率及脱油废渣活性度都较高,但再生后的脱油废渣仍难以重复利用。而利用废白土作型砂添加剂的试验研究,其工业试验结果较为理想,且能彻底解决废渣的污染问题,实现其环保利用。     

加速溶剂萃取-固相萃取及铜粉净化技术在土壤有机氯农药分析中的应用

对比了索氏提取、超声提取和加速溶剂萃取样品前处理方法在土壤中有机氯农药的萃取效果,首次采用两级温度相结合的加速溶剂萃取方式,兼顾不同挥发性萃取物的萃取效果,建立了土壤中有机氯农药的加速溶剂萃取样品前处理方法.萃取液经无水硫酸钠脱水、Florisil柱脱色和铜粉除硫后,进色谱分析,目标组分能有效避免杂质干扰,实现基线分离.实验结果表明,在优化条件下,8种有机氯农药检出限在0.05～0.20μg·kg-1之间,空白加标回收率为74.9%～124.8%,RSD为3.1%～8.8%;标准样品实验中,α-HCH及DDTs均在标准值范围内,加标回收率在78.5%～117.9%之间.     

活性污泥胞外聚合物提取方法的研究

对两种不同来源的活性污泥中EPS的提取效率进行了研究,采用的提取方法有NaOH法,阳离子交换树脂法（CER法）,加热法和离心法。结果表明,CER法是两种污泥EPS提取中最有效的方法。经过16h的提取,EPS中DNA的含量分别为0．73％和1．61％,这表明EPS的提取没有受到胞内物质的污染。两种污泥EPS的提取量分别为74mg／gVSS和80mg／gVSS,其中多糖和蛋白质是EPS的主要成分。在研究中,CER法最佳提取时间为8h,高搅拌强度和CER投加量都有利于EPS提取量的增加。