流动注射在线液—液萃取原子吸收光谱法测定天然水中铬（Ⅲ）和铬（Ⅵ）

利用新设计的流动注射液－液萃取分相器，研究了液－液在线萃取原子吸收光谱法测定Ｃｒ和Ｃｒ的实验条件、流路参数和操作程序。拟定的新方法用于武汉东湖不同区域水样中铬的测定，检出限为２．２ｎｇ／ｍｌ。     

圆盘固相萃取富集-气相色谱法测定地表水中有机氯和有机磷农药

采用环境友好的圆盘固相萃取新技术富集水体中有机氯农药和有机磷农药,分别用微池电子捕获检测器(μECD)和火焰光度检测器(FPD)气相色谱法检测,实现了水中有机氯和有机磷农药残留物的测定。结果表明,16种有机氯农药的平均回收率为64.7%~102%,精密度(RSD,n=6)为2.9%~15%;13种有机磷农药的平均回收率为65.9%~104%,精密度(RSD,n=6)为1.7%~17%。方法快速、灵敏、低污染,可用于水体中多种有机氯农药和有机磷农药的残留分析。     

针式微萃取结合GC-IRMS测定水溶液中甲酸、乙酸的稳定碳同位素组成

甲酸和乙酸稳定碳同位素组成（δ^13C）的分析对环境、食品、制药和自然产品等的研究具有重要的应用价值。但目前尚缺乏有效的测定方法。本研究利用最近出现的针式固相微萃取技术（NeedlEX）,以吹扫．捕集方式对水溶液中的有机酸进行了萃取,然后利用气相色谱．同位素比值质谱联用仪（GC—IRMS）对所萃取的有机酸分子进行了占δ^13C的测定。结果显示,质谱计的信号强度与水溶液中有机酸的浓度存在显著的线性相关关系（R^2〉0．99,P〈0．05）,表明Needl EX对水溶液中有机酸具有稳定的萃取能力。在甲酸与乙酸含量分别不低于300μg／mL与200μg／mL的水溶液中,1000mL的吹扫体积可以使两者δ^13C多次分析结果的相对误差分别保持在3％和1％左右,且整个实验流程没有造成可检测的碳同位素分馏作用。低于这两个浓度界线,则分析误差随浓度的降低迅速增加。本研究虽然是针对水溶液中有机酸δ^13C的测定,其萃取方法对其他水溶性挥发和半挥发有机物δ^13C的分析也同样具有应用价值。     

海水中234Th的超低水平液闪谱仪测定

本文提出了利用超低水平液闪谱仪测定海水中234Th的方法.海水经氢氧化铁吸附共沉淀富集后,接着用阴离子交换和TBP/煤油萃取进行Th同位素的分离与纯化.对一系列测定条件进行了详细的研究,提出了测定海水中234Th的适宜程序,即在含有234Th和产额示踪剂230Th的纯化后的5mol/dm3HNO3溶液中加入TBP/煤油进行萃取,然后用0.1mol/dm3HNO3反萃取,后者是先用契伦柯夫计数法测量234Th(通过234mPa),后加入闪烁液Hisafe 3用α/β模式测量α放射体230Th.对于α和β放射体液闪谱仪的计数效率分别为100%和55.7%±2.7%.234Th的化学回收率和总探测效率分别为70%～80%和30%～45%.该法测定海水中的234Th快速、简便和高效.     

浮游植物叶绿素a含量简易测定方法的比较

用乙醇、DMF(N,N-二甲基甲酰胺)、丙酮3种不同有机溶剂分别萃取苏州环城河水样中的浮游植物细胞叶绿素a,在分光光度计上测定其叶绿素a含量,试验数据经方差分析、Q检验,结果显示,乙醇法、DMF法的叶绿素a萃取率极显著高于丙酮(F=54.20＞F0.01(2,18)(6.01)).另用这3种萃取方法分别测定无常蓝纤维藻(Dactylococcopsis irregularis )纯培养液叶绿素a含量,通过直线回归,同样证明乙醇法、DMF法重复率较高,稳定性好,萃取率高.从安全、简便、重复性高等方面综合考虑,认为用乙醇萃取法是目前水域环境中浮游植物叶绿素a简易测定的最佳方法.     

Microwave-assisted extraction of organochlorine pesticides from sediments and determination by gas chromatograph with electron capture detection

A simple and rapid procedure to extract organochlorine pesticides （OCPs） from sediments by means of microwave energy is proposed. Sediment samples were irradiated with microwaves in a closed vessel system while immersed in hexane-acetone （1 ： 1, v/v）. The sample extracts were cleaned up using solid phase extraction with Florisil as adsorbent. Pesticides were eluted with hexane-ethyl acetate （80 ： 20, v/v） and determined by gas chromatographic separation with electron capture detection. Three oven programs were assayed with two different solvent mixtures in order to achieve adequate experimental conditions for the complete extraction of organochlorine pesticides from the matrix. Different variables such as the composition of extraction solvent,     

Speciation analysis and significance of ecological geochemistry

Different species of one element have different activities, so it has different effects on environment and human health. To analyze qualitatively and quantitatively the speciation of a special element in sample, which is the important basis for appraising the toxicity and studying the rule of transfer and translation of elements. Since the 1970＇s, the scheme of sequential extraction has already been used at many laboratories both at home and abroard, to get the information about heavy metals＇ activity in polluted soils. Because this method has the experimental nature, many schemes of problem has taken place, the absence of consistency of these sequential extraction have been formed. Thus the complexity of the schemes, the lack of selectivity of reagent, the lack of quality control, the result mainly related to the extraction scheme used, and so on. In the face of these problems, the study of experimental methods of sequential extraction on three different soils, sediment in Dongting Lake, soil in Jiangsu Province and loess in Shanxi Province was made. Reference materials of heavy metal speciation following sequential extraction in soil and sediment had been developed. Nowadays two kinds of sequential extraction methods which are widely used are BCR （three steps） and improved Tessier methods （seven steps）. Based on three steps of BCR, water-soluble speciation and the residual speciation were increased in our research. BCR701 was determined eight times at different laboratories using BCR three steps. The results showed that determined data obtained eight times were identical to the standard value, and it is indicated that this method has good reproducibility. The stability and homogeneity experiments indicated that the preparation of three types of candidates accorded with our requirements. Eight laboratories had afforded the determined values of 12 heavy metal elements （Cu, Pb, Zn, Mn, Co, Ni, Cd, Cr, Mo, As, Sb, Hg, Se et al.） using BCR three steps. Also, these three candidates afforded the determined values by seven steps, and 12 laboratories had participated.     

卤水提锂的萃取体系概述

介绍了国内外萃取法在含锂溶液,尤其在卤水中提取锂的部分研究进展情况,重点对各种萃取体系的机理和特点进行了说明,并对今后我国盐湖卤水萃取法提锂研究的方向进行了总结。