高效液相色谱法测定水中的六种邻苯二甲酸酯研究

建立了高效液相色谱法测定水中六种邻苯二甲酸酯(邻苯二甲酸二甲酯、邻笨二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二辛酯、邻苯二甲酸丁基苄酯)的检测方法.对水样中邻苯二甲酸酯的萃取条件和高效液相色谱分析条件进行优化,采用正己烷二次萃取,浓缩定容后分析,以乙腈-水为流动相梯度洗脱,紫外检测波长226 nm,16 min可将六种邻苯二甲酸酯分离出.方法的检出限为0.13μg/L ～0.37 μg/L,加标回收率为78.6％～118.5％,相对标准偏差为0.82％～2.17％,是一种理想的测定水中六种邻苯二甲酸酯的方法.     

顶空毛细柱气相色谱法测定水中七种苯系物研究

选用Elite-FFAP色谱柱,利用顶空-毛细柱气相色谱技术对水中的苯、甲苯、乙苯、对二甲苯、间二甲苯、邻二甲苯、苯乙烯七种挥发性苯系物进行同时测定,并对样品的平衡温度、保温时间、程序升温的条件控制、水中含盐量等影响因素进行了探讨,优化了检测条件,使七种挥发性苯系物得到不错的分离。样品平衡温度控制在70℃,样品平衡时间19 min,进样口温度180℃,检测器温度230℃,10 mL水样中加入4 g NaCl的条件下,分离效果最佳。     

热脱附-气相色谱法测定空气中的总挥发性有机化合物研究

建立了热脱附-毛细管气相色谱法测定空气中苯、甲苯、乙酸丁酯、乙苯、对/间二甲苯、邻二甲苯、苯乙烯和十一烷等挥发性有机物的检测方法。九种挥发性有机物在一定浓度范围内标准曲线线性良好,相关系数均在0.997~0.999之间。检出限在0.002~0.005 mg/m3(采样体积1.0 L计)。用该方法检测了企业产生的有机废气及厂区周边环境空气,实验结果表明该方法灵敏度高、操作简单、重现性好、准确可靠,能够满足对实际样品的分析要求。     

顶空气相色谱法测定工业废水中乙醇和异丙醇研究

建立了测定工业废水中乙醇和异丙醇的顶空毛细管气相色谱法.采用顶空进样技术,分析过程不使用有机试剂,避免了对分析人员和环境的危害.乙醇和异丙醇在3.00～ 20.0mg/L浓度范围内呈良好线性关系,水样测定结果重现性较好,相对标准偏差范围均小于2％,乙醇加标回收率为93.6％～104.0％,异丙醇加标回收率为94.0％～ 102.0％.本方法操作简单快速,灵敏度高,能满足工业废水中乙醇和异丙醇的监测.     

离子色谱法测定多种水体中碘化物应用研究

利用AS19阴离子交换分离柱,KOH淋洗液自动发生器,抑制型电导检测器,建立了测定多种水体中碘化物的离子色谱法.讨论了干扰及消除、色谱条件的优化,分析方法的线性与检出限、精密度、准确度等,并应用该方法对多种水体中碘化物进行了测定.结果表明:该方法不受水体中其他阴离子干扰,检出限低,线性范围宽,相关系数R2=0.999 9,精密度高,准确度好,操作简便可行,适用于多种水体中碘化物的测定.     

固相膜萃取-气相色谱法测定地表水中有机氯农药研究

研究了固相膜萃取对地表水中有机氯农药(OCPs)物质的提取效果,并与液液提取法(LLE)进行比较.建立了固相膜萃取/气相色谱法检测地表水中20种有机氯农药的方法.结果表明:当萃取膜为HLB膜,洗脱液溶剂为丙酮和正己烷,萃取效果最理想,20种OCPs的回收率稳定在74.1%~94.3%之间,固相膜萃取法与传统液液提取法相比,既提高了萃取效率同时又减少了有机萃取溶剂的用量.该法检测实际样品时,同时加入2种内标指示剂对方法的性能进行了验证,2种内标示踪剂的回收率分别为71.6%~94.8%和69.9%~109.5%,样品中20种OCPs均未检出.     

QuEChERS: a sample preparation for extraction of carbaryl from rat feces

Carbamate compounds are an important group of cholinesterase inhibitors. There is a need for creating awareness regarding the risks of the inadequate carbamate use in the residential areas due to potential adverse human effects. Carbaryl is a commonly used pesticide worldwide. A simple, fast, and high-throughput method was developed employing liquid chromatography with fluorescence detector to determine carbaryl residues in rat feces. The extraction was performed by using a rapid, easy, cheap, effective, reliable, and safe (QuEChERS) method, using acetonitrile as the extracting solvent. The parameters for the performance of the extraction method were optimized, such as ratio of mass of sample per volume of extraction solvent, QuEChERS content, and cleanup columns. Linear response was obtained for all calibration curves (solvent and matrix-matched) over the established concentration range (5–500 μg/L) with a correlation coefficients higher than 0.999. The achieved recovery was 97.9% with relative standard deviation values of 1.1% (n = 4) at 167 μg/kg fortified concentration level and the limits of detection and quantification were 27.7 and 92.3 µg/kg, respectively.     

基于放射性碳分析的多环芳烃源解析:技术进展和准确性评估

化石燃料燃烧和生物质燃烧是污染物多环芳烃(polycyclic aromatic hydrocarbon,PAHs)的两大来源.放射性碳(14C)分析近年用于评估这两类源对环境中PAHs的相对贡献.此方法基于化石燃料和生物质的14C含量差异,即化石燃料不含14C,而生物质的14C浓度有一个较稳定值.14C的自然丰度极低(约10-12),因此检测PAHs这样的痕量污染物的14C含量一度极具挑战.1990年代中期,加速器质谱的技术突破使得对环境样品PAHs的14C分析具有实用价值.要准确测出PAHs的14C含量,须先从化学成分复杂的环境样品中分离出高纯度的PAHs.制备气相色谱因其出色的分离能力而成为目前环境样品PAHs14C分析必备的工具.本文意在简介基于14C分析的PAHs源解析的基本原理、技术进展,以及评估该方法获得的PAHs源解析结果的准确性.     

Experimental investigation of the efficiency of triple rinsing of agricultural containers regarding their characterization as non-hazardous wastes

The efficiency of water rinsing for removing fenthion from non-combustible used pesticide containers was investigated. Four hundred empty containers from four olive oil producing areas in Greece were studied. Following triple rinsing cleaning procedures, the amount of fenthion retained in the container ranged from 0.01% to 0.1% w/w of its initial concentration. Extraction was accomplished with acetone, and the extracts were analyzed with a capillary gas chromatographic system coupled with flame ionization detector. The results obtained showed that triple rinsing is an effective procedure for removing fenthion from used pesticide containers, since the remaining pesticide concentration was below the legislated threshold value. Consequently, the containers can be handled as non-hazardous solid wastes.     

高效液相色谱-电感耦合等离子体质谱联用测定生物样品中的有机汞

建立了酸提取-高效液相色谱-电感耦合等离子体质谱联用技术(HPLC-ICP-MS)测定生物样品中甲基汞、乙基汞、苯基汞等3种有机汞的分析方法。鱼肉和贝类样品经盐酸消解,苯萃取,硫代硫酸钠溶液反萃取后,采用醋酸铵/L-半胱氨酸缓冲盐及甲醇体系组成的流动相按一定比例进行梯度洗脱,经前处理的生物样品在液相色谱中经C18柱分离后,进入电感耦合等离子体质谱检测其甲基汞、乙基汞和苯基汞的浓度。3种有机汞化合物均在0.50~50.0μg/L范围内呈现良好的线性关系,线性相关系数(r)均大于0.9998。方法检出限为0.010~0.038mg/kg;3种有机汞样品加标的RSD均小于12.2%;两个水平的加标回收率在50.8~129%。