静态液相微萃取-气质联用测定烷基酚方法优化

采用静态液相微萃取前处理方法与气相色谱—质谱联用技术相结合对水样中烷基酚测定方法进行优化。     

Effects of soil composition on solid phase microextraction determination of triazine and organophosphorus pesticides

The influence of organic matter and clay contents on headspace solid phase microextraction (HS-SPME) determination of triazine and organophosphorus pesticides in different soils was studied. The results of the study showed that content of soil organic matter dominantly participated in sorption of triazines (simazine, atrazine and prometryn) to soil, while sorption of organophosphorus pesticides (phorate and tebupirimfos) could not be explained only by contents of dominant soil sorption components (soil organic matter and clay). Sorption of all pesticides studied to different soil types was similar at their lower concentrations while the influence of soil composition was expressed at higher concentration levels. Except for phorate, the obtained sorption trends were different from those obtained by direct SPME mode (DM-SPME) and exhaustive liquid-solid extraction (LSE) method. These results indicated that most likely co-extractants from the analyzed medium complicated evaporation and diffusion of the pesticides to the PDMS fiber during HS-SPME sampling.     

Concentration and fate of persistent organochlorine pesticides in estuarine sediments using headspace solid-phase microextraction

The concentration and fate of persistent organochlorine pesticides (OCPs) in estuarine surface sediments in Erh-jen and Lan-yang rivers, Taiwan were investigated using headspace solid-phase microextraction (HSSPME) method to evaluate the possible pollution potential and guideline for OCP concentrations in Taiwan. The HSSPME method exhibits a good analytical performance with low detection limits for OCP determination in sediment. In addition, results obtained using the developed HSSPME method were in good agreement with those obtained using Soxhlet extraction in a certified sample. The developed analytical method was further applied to the determination of concentrations of OCP residues in surface sediments from the estuaries of the selected rivers in Taiwan. A total of 20 surface sediments from each river was collected from 10 sampling stations. The total OCP concentrations in sediments from Erh-jen River ranged from 0.17 to 5.04 ng/g-dw with the mean values of 0.25–1.24 ng/g-dw for HCHs, 0.10–0.89 ng/g-dw for cyclodienes and 0.16–0.64 ng/g-dw for DDTs. The concentrations of OCPs in sediments from Lan-yang River were in the range 0.37–0.9 ng/g-dw with an average of lower than 0.5 ng/g-dw. HCHs and DDTs were abundant in the estuarine sediments from the selected rivers. Results obtained in this study show that the origin of OCPs in the surface sediments from Erh-jen River is a combination of erosion of the weathered soils and long-range atmospheric transport, while the OCP concentrations found in Lan-yang River could be regarded as the background levels of OCPs in Taiwan.     

静态顶空气相色谱法对土壤中乙醛等物质分析及研究

研究用静态顶空技术处理土壤,从而建立了静态顶空-气相色谱(GC-FID)测定土壤中的乙醛、丙烯醛、丙烯腈和吡啶的检测分析方法。在一定的静态顶空和气相色谱条件下,进行了顶空的时间和温度优化,确定了静态顶空气相色谱法测定土壤中乙醛、丙烯醛、丙烯腈和吡啶方法的检出限,并取得了满意的分离效果、线性回归方程、精密度和准确度。结果表明:用顶空气相色谱法处理土壤样品,可以减少土壤中待测有机物的损失,提高实验分析的灵敏度和准确度。     

顶空气相色谱/质谱法测定水中四乙基铅的关键因素研究

采用顶空气相色谱/质谱法联用技术测定水中的四乙基铅,对涉及的关键操作环节及重点技术问题进行了研究。结果表明,在避光条件下于4℃低温冷藏并密封保存,添加甲醇作为保护剂,保存时间不应超过3 d。实验选择进样口温度为220℃,顶空瓶压力为96.52 kPa,调节载气流量设置实际分流比为51,可以有效改善顶空进样测定样品时存在的不出峰、不稳定或灵敏度降低的问题。对地表水、自来水及生活污水实际样品进行四乙基铅测定和加标回收分析,加标回收率为81.0%~110%,相对标准偏差(RSD)为2.5%~7.4%,能够满足《水质四乙基铅的测定顶空/气相色谱质谱法》(HJ 959—2018)的测定要求。将顶空进样法与吹扫捕集法进行比较,结果表明顶空进样法稳定性更好,适合大批量四乙基铅样品的连续测定。     

环境空气中异丙醇的测定

建立了顶空气相色谱法测定环境空气中异丙醇的方法。空气中异丙醇经蒸馏水吸附,顶空进样氢火焰离子化检测器检测,时间定性,峰面积定量。本方法前处理简便,分析灵敏度高,不使用有机试剂,满足环境分析要求。     

顶空毛细管气相色谱法同时测定水中丙酮甲醇乙腈

采用顶空毛细管气相色谱法同时测定水中丙酮、甲醇和乙腈,确定顶空平衡温度为95 ℃,平衡时间为30 min,氯化钠质量浓度为200 g/L。丙酮、甲醇和乙腈在0.500 mg/L～5.00 mg/L范围内线性良好,检出限分别为0.02 mg/L、0.10 mg/L和0.04 mg/L,标准溶液平行测定的RSD≤3.0%,两个质量浓度水平的空白加标回收率范围为90%～108%。苯系物对测定不产生影响,吡啶会影响甲醇的测定。     

顶空气相色谱法测定土壤或底泥中挥发性苯系物

采用顶空气相色谱法测定了土壤或底泥中的挥发性苯系物,测定了苯系物在10%NaCl水溶液60℃时的分配常数,给出了加入土壤导致液相体积改变的校正方法。用10% NaCl水溶液作为提取剂在 60℃加热平衡60min, 对5个苯系物的平均回收率达到73.6%, 检出限为4.2~5.5ng/g。     

顶空-毛细管气相色谱法同步测定水中吡啶丙酮乙腈

建立了顶空-毛细管气相色谱测定水中吡啶丙酮乙腈的方法,不用有机溶剂萃取和浓缩,减少了损失和对环境的污染,具有灵敏度高、检出限低、定量准确、操作简便等特点。当取样量为5ml时,检出限可达到0.006~0.03mg/L级,相对标准偏差为1.0%~2.3%,加标回收率在78.0%~100.2%之间,完全适合水中吡啶丙酮乙腈的测定。