Sun H F, Hase T, Hata N, Kasahara I, Taguchi S
Faculty of Science, Toyama University, Gofuku 3190, Toyama 930-8555, Japan.
Anal Sci. 2001 Nov;17(11):1291-4. doi: 10.2116/analsci.17.1291.
The quantitative extraction of cationic surfactant (CS+) in river sediments was studied. Further, the developed method was applied to the spectrophotometric determination of CS+ in urban river sediment samples by solid-phase extraction with membranes. A mixture of methanol and hydrochloric acid was proposed as an eluent. Dried sediment was digested in the eluent under ultrasonic irradiation. After elution, the eluent was evaporated to almost dryness. The residue was dissolved in a small volume of methanol and diluted to a certain volume with water. The pH of the solution was adjusted to 4-5 to separate iron and some other metals as precipitates of hydroxides. The solution was passed through two-piled membranes: first glass-fiber and then polytetrafluoroethylene (PTFE) membranes. A small volume of methanol was passed through the membranes to elute any CS+ retaining on the membranes. After passing the methanol solution through a cationic exchange resin column, the retained CS+ was eluted with methanol containing a high concentration of sodium chloride. Water, Bromophenol Blue (BPB) and hydrochloric acid were added to the solution. The solution was passed through a mixed cellulose ester membrane filter to retain an ion associate of CS+.BPB-. The retained ion associate was dissolved in a small volume of N,N-dimethylformamide together with the membrane filter, followed by the addition of triethanolamine to make the solution alkaline. The absorbance due to BPB2- was measured at 603 nm against a reagent blank. This method was applied to the determination of CS+ in river water and sediment. A cationic surfactant in sediments at 10(-5) mol kg-1 levels was detected with satisfactory precision. It was found that CS+ was about 500-fold enriched in the sediment from water at the place where domestic wastewater was discharged.
研究了河流沉积物中阳离子表面活性剂(CS+)的定量提取方法。此外,将所建立的方法应用于城市河流沉积物样品中CS+的分光光度法测定,采用膜固相萃取法。提出用甲醇和盐酸的混合液作为洗脱剂。将干燥的沉积物在超声辐射下用洗脱剂消化。洗脱后,将洗脱剂蒸发至近干。残渣用少量甲醇溶解,再用水稀释至一定体积。将溶液的pH值调至4 - 5,以分离出铁和其他一些金属的氢氧化物沉淀。溶液依次通过两层叠放的膜:首先是玻璃纤维膜,然后是聚四氟乙烯(PTFE)膜。少量甲醇通过膜以洗脱保留在膜上的任何CS+。将甲醇溶液通过阳离子交换树脂柱后,用含高浓度氯化钠的甲醇洗脱保留的CS+。向溶液中加入水、溴酚蓝(BPB)和盐酸。溶液通过混合纤维素酯膜过滤器以保留CS+·BPB-离子缔合物。将保留的离子缔合物与膜过滤器一起溶解在少量N,N - 二甲基甲酰胺中,然后加入三乙醇胺使溶液呈碱性。以试剂空白为参比,在603 nm处测定BPB2-产生的吸光度。该方法应用于河水和沉积物中CS+的测定。检测到沉积物中10(-5) mol kg-1水平的阳离子表面活性剂,精密度令人满意。发现在生活污水排放处,沉积物中CS+的含量比水中约富集500倍。