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.     

超临界流体中MoO3与WO3溶解度实验探讨

超临界地质流体以其独特的性质对金属成矿元素具有超强的萃取、层析和搬运能力,在热液矿床成矿机制研究中对揭示成矿物质的源、流和汇起着特殊和重要作用。本文利用分析纯H2MoO4在高温下脱水制备了MoO3(白色斜方晶系),在冷封式高压釜中实验测定了417℃超临界条件下,MoO3在纯水中的溶解度分别为7.3(29MPa)、14.2(45MPa)、21.6(55MPa)、27.7(78MPa)、32.5(100MPa)、和34.2(150MPa)mmol/l,热液中钼的存在形式为H2MoO4。依据前人的实验方案,补充测定了WO3在4.0%NaCl水溶液中于450%条件下的溶解度,其值分别为27.51(50MPa)和30.52(100MPa)mmol/l。结合前人研究结果发现,MoO3、WO3的溶解度在临界区域内具有超临界现象,在超临界条件下其溶解度与石英的超临界溶解度行为基本相似,表现为溶解度随体系温度和压力的升高而增大,这对揭示岩浆热液型和石英脉型钨、钼矿床的形成机制具有重要指导作用。     

流体的热力学前缘研究

总结了当前国内外关于流体的热力学前缘研究领域如下：（１）流体体系的ｐ－Ｖ－Ｔ－ｘ相关系研究，主要对象是Ｈ２Ｏ－ＣＯ２－盐类多组分体系高温高压下相图的实验和理论研究。（２）矿物在流体中的溶解度及溶解后在流体中溶解类型的形式和热力学性质——平衡常数（或Ｇｉｂｂｓ自由能）及各种偏摩尔性质的研究。（３）流体热力学模型化研究，已研制出大量的计算机软件，包括多种矿物、溶解类型的热力学数据库和模拟热液平衡、矿物溶解性质、反应路径和水—岩相互作用的实用程序。（４）超临界流体的相关系和化学反应等有许多特殊的性质，对认识地球内部的演化将有重要意义。（５）新技术新方法的发展，使分析单个矿物包裹体成分变成了现实。