环境样品中有机物分析的前处理技术

综述了顶空法、吹脱－捕集法、固相萃取、微波萃取、超临界流体萃取技术在环境样品前处理中的应用现状并比较了这种几样品处理方法的优缺点。     

浮游植物叶绿素a测定的“热乙醇法”及其测定误差的探讨

详细介绍了一种国际上通用的浮游植物叶绿素a测定方法-热乙醇萃取法,并根据文献记载和作者多年的实践经验．对这种测定方法可能产生的误差进行全面的探讨,为国内水环境研究人员尽快掌握这种方法提供了科学的参考．     

加速溶剂提取-气相色谱法同时测定土壤中的22种有机氯和有机磷农药

我国环境污染调查评价测试项目中开展了大量有关土壤中有机氯及有机磷农药残留的测定工作,多种有机污染物同时分析测试的方法是研究的新热点.本文以正己烷-丙酮(体积比1∶1)为提取剂,采用加速溶剂提取,毛细管柱气相色谱法测定土壤中六氯苯等9种有机氯及敌敌畏等13种有机磷农药残留.方法回收率为79.1％ ～ 107.7％,相对标准偏差为3.62％ ～9.94％ (n =7),检出限为0.02 ～ 0.45 μg/kg.本方法将两类农药同时提取且实现了各组分的完全分离,拓展了方法的适用范围,与传统的超声提取和索氏提取法相比,提取时间缩短至20 min,提取溶剂体积降至50 mL,缩短了分析时间,降低了成本,精密度和回收率能够满足全国环境污染调查评价的需要.     

Orthogonal design for optimization of pigment extraction from surface sediments of the Changjiang River Estuary

Using a suitable solvent for extracting pigments from sediment for high performance liquid chro-matography (HPLC) analysis is critical for obtaining qualitative and quantitative estimates of phytoplanktonic and benthic algal biomass, as well as community composition. Five methodolog-ical factors (sample dehydration, extraction solvent, extraction duration, number of extractions, and ratio of solvent volume: sample weight) were studied using an L₉ (3⁴) orthogonal design in a sedimentary pigment extraction experiment on samples collected from the Changjiang large-river delta-front estuary (LDE), using HPLC analysis. The results show that the optimal extraction method for sedimentary pigments should include freeze-drying samples prior to extraction. The effects of different factors on sedimentary pigment extraction were separated by the L₉ (3⁴) or-thogonal design experiments and showed that the extraction solvent was the most important, with extraction duration the second most important, and numbers of extraction and ratio of solvent vol-ume: sample weight was the least important. The mixed solvent treatment comprised of acetone, methanol and water (80:15:5, by volume) was best for polar pigment extraction, with 100% acetone better for apolar pigments. For most pigments employed in this study (i.e., peridinin, fucoxanthin, alloxanthin, diatoxanthin, zeaxanthin, pheophytin-a and β-carotene), 3 h was found to be enough time for extraction from these deltaic sediments. However, for chlorophyll-a, the most important pigment used for estimating algal biomass, 12 h was needed. A small amount of solvent (3 ml) with duplicate extractions obtained the greatest amount and diversity of pigments. Unfortunately, no extraction method was found to be suitable for all pigments in sediments. The choice of extraction procedure should be made in accordance with the objective of each study, taking into consideration the properties of sediments and pigments in question.     

油气化探样品前处理条件对稠环芳烃测定结果的影响

在油气化探工作中,稠环芳烃含量对区域油气异常有着重要的指示作用。对于稠环芳烃的测定,诸多前处理条件对稠环芳烃的提取效率有显著的影响。本文研究了油气化探样品振荡提取法的多种前处理条件(提取溶剂、样品粒径、振荡时间和静置时间、提取温度)对荧光强度测定结果的影响。实验结果表明,提取溶剂不同,测定结果存在较大差异,各提取溶剂的提取效率大小依次为:二氯甲烷正己烷乙酸乙酯石油醚。综合考虑溶剂背景值对测定结果的影响,选择以正己烷为提取溶剂进行条件实验。在研究的粒径范围内,荧光强度随样品粒径的减小而增大,但粒径过小荧光强度反而降低,粒径在0.125~0.090 mm之间的样品荧光强度最高;荧光强度随着振荡时间和静置时间的增加而增强,其中静置时间的影响较大,静置9 h后荧光强度提高不显著;振荡时间的影响相对较小,振荡20 min后提取效率提高不显著;提取温度对荧光强度的影响最为显著,在相同条件下,提取温度越高荧光强度越大,且提取温度是影响稠环芳烃测定结果重现性的关键因素。油气化探样品前处理的最优化条件为:采用粒径在0.090~0.177 mm之间的样品,以色谱纯正己烷为溶剂,提取温度25℃,振荡时间20 min,静置时间12 h。     

湿巾多含“低毒”宜慎用

在各类湿巾的成分标注中,多数都标明含有“丙二醇”等化学物质,但并未标明含量。丙二醇是种低毒的化学溶剂,具有一些保湿、抗菌作用,因此常用于湿巾、卸妆油、洗面奶等制品。一般洗面奶等制品中,丙二醇的添加量不会超过5％,而且涂料里面也常添加这类物质,由于易挥发,影响并不大,但丙二醇对皮肤渗透力强,溶解力大,长期且过量使用会伤害皮肤,尤其是敏感性皮肤。     

小杂鱼脱脂技术的研究

以小杂鱼或低值鱼为原料，采用常温溶剂萃取法进行脱脂，研究了不同溶剂、溶剂混合比、流速和萃取时间对鱼类脱脂的影响。结果表明，在常温下用等体积的异丙醇和乙酸乙酯混合溶剂，以流速4-8mL／min连续萃取4—6h，脱脂鱼肉的脂肪平均含量ω为0．19％，脱脂率高达96．26％。该方法的溶剂损耗量为加热溶剂萃取法的1／3倍。     

地质流体中络合物同位素平衡分馏系数的第一性原理计算

地质流体中不同络合物之间的稳定同位素平衡分馏系数是利用稳定同位素示踪地质流体演化过程的必要前提.但由于受实验条件的限制,流体中部分元素不同络合物之间的同位素分馏系数难以通过实验精确测定.基于第一性原理的理论计算是获得溶液中不同络合物之间稳定同位素平衡分馏系数的一种重要手段,能够获取各种极端条件下同位素分馏系数.在应用第...     

进样溶剂极性对地下水中有机氯农药色谱行为的影响

地下水中有机氯农药分析时采用正己烷为进样溶剂,而考核样品的溶剂通常为甲醇。正己烷和甲醇分别是典型的非极性溶剂和极性溶剂。文章研究了正己烷和甲醇两种溶剂对地下水中9种必测有机氯农药(六氯苯、α-六六六、β-六六六、γ-六六六、δ-六六六、p,p′-DDE、p,p′-DDD、o,p′-DDT、p,p′-DDT)色谱行为的影响。结果表明,溶剂的极性对有机氯农药的响应值有显著的影响:甲醇为进样溶剂时,由于极性强,造成汽化室内活性位点的暴露,导致某些待测组分被活性位点吸附,甲醇相的待测物响应值明显低于正己烷相待测物响应值。     

铅物相分析选择性溶剂、浓度及浸取时间探讨

个旧铅矿石以铅钒、白铅矿、砷铅矿、方铅矿、铅铁钒为主要赋存状态。试验探讨浸取时间、选择性溶剂、及其浓度对各赋存状态下铅的溶解情况,制定适合个旧地区铅矿石的物相分析方法,取得满意效果。