Studies And Applications Of The Separation And Enrichment Of Rare Metals In Chinese Herbal Medicine By The Extraction-elution Resin And Determination With Spectrometry

The amount of rare metals in Chinese herbal medicine is very rare, and most of them are accompany with other metal elements, and their direct deteremination will be easily disturbed by other coexistence ions and effect the accurance of analytic datas. So the separation and enrichment of rare metals is necessary for drawing out more accurate result. The separation and enrichment by extraction elution resin is a new separation technology developed from solvent-extraction and ion-exchange process of the latest years, and the technology has been absorbing the novel achievement from the fields of solvent-extraction and ion-exchange process, which conquered the traits of the lapse of solvent in solvent-extraction and the bad opt in ion-exchange process, and it split a new department for the separation and enrichement of rare metals.The experiment part consists of four chapters:In chapter one, numerous domestic and foreign references denoted that in the medicine field Chinese herbal medicine is famous all around the world. Its research content from the traditional medicineformula, case of illness using the medicine, penetrated to structure ingredient, pharmacology activeness and Chinese medicine preparation develops. It outlined the medical service and health care functionin of Ge, Ga and Mo in the Chinese herbal medicine, and compared concentrating micro rare metals commonlyused several methods, simultaneously has carried on the synthesis comparison to the different analysis examination methods, proposed the spectrographic methods held the superiority status in these analysis methods.In chapter two, the separation and enrichment of germanium with tributyl phosphate levextrel(CL-TBP) resin as the stationary phase was described. The resin was packed in the microchromatographic column, then the suitable liquids for the absorption and separation of germanium (Ge) were adopted respectively, and the disturb elements was eluted by the different eluting-liquids. The eluting-liquid of germanium was detected by PF-CTMAB spectrometry. The dynamic and static saturated absorption capacity of Ge on the resin reached to 34.8mg/g and 38.5mg/g respectively. The recovery was 92.7%~97.8%,and the RSD was less than 4.37%.In chapter three, under the decompressed microchromatographic column,with CL-TBP as the stationary phase and packed under negative pressure,germanium and molybdenum(Mo) could be separated using reversed-phase extraction chromatography by the eluting-technology of zero dead volume.Ge and Mo were eluted continually with only about 1ml eluting-liquids, respectively . The eluted samples were determined with PF-CTMAB spectrophotometry.The saturated adsorption capacity of Ge and Mo on the resin reached to 34.8mg/g and 67.4mg/g respectively.The recovery was 91.4%~98.6% and 96.6%~101.3% , and the RSD was 2.53%~5.74% and 1.91%~4.12% respectively . The method has been successfully applied to the determination of traces of Ge and Mo in Chinese herbal medicine.In chapter four, a novel synergistic extraction elution resin containing di(2-ethylhexyl)phosphoric acid and laurylether monophosphate(P204-H2MPA) was manufactured. In the sulfuric acid solution with pH from 0.1 to 3.0, the adsorption quality of gallium with extraction elution resin was proportional to pH, and the saturation adsorption capacity was 84.0mg/g. After stripped by 1mol/L HCl-0.5mol/L tartaric acid, then FAAS determine Ga, this manner was found with good elution effect and sensitive as well as. A novel determination manner of Ga by extraction elution resin-FAAS was established.In a word, by numerous systematic and scrupulous experimental works, some work of optimal and innovated experiences have been done as following: Firstly, improved the technique of chromatographic column by using packed with micro- choromatographic column and under the zero dead volume situations to separating rare metals, which economized the reagent and improved the analytic rate. Secondly, preparated the co-extraction elution resin with super capability used for sorbent of rare metals. Thirdly, predominanted many terms on enrichment & separation and instrumental detection, which radicated the novel analytic manners, improved enrichment capacity and analytic efficiency, magnified the applied scope for Ge, Mo and Ga separately, and then, the novel approach for analysis of rare metals was inaugurated.