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。     

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.     

磺化法净化中丙酮对β、δ六六六的影响与消除

磺化法净化六六六提取液时，残留在石油醚相中的丙酮引起β、δ六六六两组分部分损失。本文研究了丙酮残留量与β、δ六六六两组分磺化损失间的关系，实测了常规条件下丙酮的残留量，找出用2％NaSO4溶液两次洗涤提取液，有效降低丙酮残留量，减少β、δ六六六组分磺化的简便方法，用于土壤样品测定获得满意结果。