TSC大孔螯合树脂对金铂钯的吸附特性及其在岩矿分析中的应用

本文研究了TSC大孔螯合树脂对贵金属Pt(Ⅳ)、Pd(Ⅱ)、Au(Ⅲ)和贱金属Cu(Ⅱ)、Pb(Ⅱ)、Zn(Ⅱ)、Fe(Ⅲ)、Al(Ⅲ)等的吸附特性。测定了树脂在不同酸度下对Au(Ⅲ)、Pt(Ⅳ)、Pd(Ⅱ)的饱和吸附容量。研究结果表明,该树脂可从稀HCl、稀王水溶液中定量吸附Au(Ⅲ)、Pt(Ⅳ)、Pd(Ⅱ),而贱金属离子则不被吸附。吸附在树脂上的Au、Pt、Pd可被5％硫脲溶液洗脱,洗脱液中的Au、Pt、Pd可分别用火焰和无火焰原子吸收法测定。标准加入回收率为97—107％。通过对MGI-Au-07,MCM-02标准样品和其它样品的测定,说明应用本法可获得满意的结果。     

Determination of Fluoride Ions in Iron Ores by UV–VIS Spectrophotometry after Matrix Removal Using Diphonix® Resin

A modification of the spectrophotometric method for the determination of fluoride ions in iron‐rich materials is proposed. In this method the iron matrix was successfully removed using Diphonix^® resin. The studied sample was a ferruginous mineral which contained about 38% of iron. The Euronorm certified reference material (ECRM) 676‐1 (Iron Ore Sinter), as a commercially available material having a similar matrix (39.76% w/w Fe) and fluoride level (0.1% w/w), was used to validate the method. After partial digestion in concentrated hydrochloric acid the samples were diluted and passed through Diphonix^® resin. The concentration of fluoride ions was determined by a spectrophotometric method using a Zr:ER complex (λ = 540 nm). The result obtained for the ECRM was in good agreement with the certificate specification and thus proved the method to be applicable for the determination of fluoride ions in iron‐rich materials. Due to the easy digestion step and simple requirements for equipment, this method can be used in most laboratories.     

柑桔皮中黄酮类物质的提取与纯化研究

采用微波法对蜜桔皮中黄酮类化合物进行提取。将单因素分析与正交试验相结合,得到微波法提取蜜桔皮中黄酮类化舍物的最佳工艺条件：提取剂乙醇体积分数为50％;微波功率为560w;提取时间为4min;料液比（g／mL）为1：30。每克蜜桔皮中提取黄酮类化合物为0．52mg,回收率为93．3％。在最佳参数组合下,桔皮黄酮提取量可这最大,并且研究了AB-8大孔吸附树脂对桔皮黄酮的吸附和解吸附特性和纯化效果,结果表明AB-8大孔树脂可用与桔皮中总黄酮的纯化。     

紫菜中类菌孢素氨基酸纯化工艺的优化及其抗紫外辐射作用研究

为了筛选纯化紫菜类菌孢素氨基酸(mycosporine-like amino acid,MAAs)的离子交换树脂,优化纯化工艺,并研究纯化后MAAs体外抗紫外辐射活性,本研究通过静态动力学吸附及解析实验,筛选纯化树脂;结合动态动力学吸附及解析单因素实验建立响应面法对SA-2型阳离子树脂纯化MAAs的二次多项式模型,对MAAs的纯化工艺进行优化;通过建立大肠杆菌、金黄色葡萄球菌的复合紫外线(UVA+UVB)损伤模型,分析纯化后MAAs样品的体外抗辐射活性。结果表明:静态动力学吸附及解析实验筛选出SA-2型阳离子树脂为纯化MAAs的最佳树脂,吸附率和解析率分别为86.01%和56.63%;吸附的最佳工艺条件为:上样液质量浓度3 g/L、上样流速1 m L/min、上样液pH为6、洗脱液体积分数为3%、洗脱流速为1.5 m L/min、洗脱液pH为6;在此条件下吸附率为79.21%,洗脱率为64.02%;纯化后的MAAs样品能有效抑制紫外辐射而造成的损伤,将菌种失活速度分别降低了39.10%和40.58%,表现出显著的抗紫外辐射活性。     

油页岩灰渣制备人造大理石及其性能

利用油页岩灰渣、不饱和聚酯树脂为主要原料,辅助加入固化剂和促进剂,室温固化合成一种新型人造大理石装饰材料。运用实验系统研究原料配比、固化剂和促进剂用量、固化时间、树脂类型与填料粒度等因素对材料性能的影响,并确定了大理石制备的最佳配方。基层最佳配方（质量分数）：不饱和树脂1号为20%～27%、引发剂0.5%～2.25%、促进剂0.5%～1.5%、油页岩灰渣50%～70%、碳酸钙粉5%～20%;表层最佳配方（质量分数）：不饱和树脂1号为25%～30%、引发剂0.5%～2.0%、促进剂0.5%～2.0%、氢氧化铝40%～50%、碳酸钙粉20%～30%。采用该方法制备的人造大理石外形平整美观,压缩强度为79 MPa,弯曲强度为7.4 MPa,放射性比活度I_Ra和I_r分别为0.67、0.45,质量符合国家标准。     

Novel Polymeric Resin for Solid Phase Extraction and Determination of Lead in Waters

Interest in preconcentration techniques for the determination of metals at ultratrace levels still continues increasingly because of some disadvantages of flameless atomic absorption spectrometry and the high costs of other sensitive methods in compared to flame atomic absorption spectrometry (FAAS). Among preconcentration techniques, solid‐phase extraction is the most popular because of a number of advantages. In this work, thiol‐containing sulfonamide resin was synthesized, characterized, and applied as a new sorption material for solid phase extraction and determination of lead in natural water samples. The optimization of experimental conditions was performed using the parameters including pH, contact time, and volumes of initial and elution solutions. After preconcentration procedure, FAAS was used for determinations. The synthesized resin exhibits the superiority in compared to the other adsorption reagents because of the fact that there is no necessity of any complexing reagent as well as high sorption capacity. Consequently, 280‐fold improvement in the sensitivity of analytical scheme was achieved by combining the slotted tube atom trap‐atomic absorption spectrometry (STAT‐FAAS) and the developed preconcentration method. The limit of detection was found to be 0.15 ng mL^?1. The Pb²⁺ concentrations in the studied water samples were found to be in the range of 0.9–6.7 ng mL^?1.     

苯乙烯型大孔树脂对海水中微量有机磷农药的吸附性能研究

为获得不含农药的当地海水在利用酶传感器监测海水有机磷农药时作为对照溶液使用,选用苯乙烯型大孔吸附树脂ASD5作为吸附剂,对含马拉硫磷和甲基对硫磷的海水样品进行动态吸附研究。发现该树脂较适合去除海水中的微量马拉硫磷,在温度10℃,流速0.5mL.min-1的条件下,10g树脂制成的吸附柱处理含500μg.L-1马拉硫磷的海水样品(乙酰胆碱酯酶活性抑制率为30.0%),出水的乙酰胆碱酯酶(AChE)活性抑制率仅为0.4%,而对海水自身的性质没有显著影响。结果表明:苯乙烯型大孔吸附树脂ASD5适合去除海水中的微量马拉硫磷,在海水有机磷农药的酶传感器监测中有很好的应用前景。     

Separation of Clay Minerals from Host Sediments Using Cation Exchange Resins

Classic physical and chemical treatments applied to separating clay minerals from the host sediments are often difficult or aggressive for clay minerals. A technique using cation exchange resins (amberlite IRC-50H and amberlite IR-120) is used to separate clay minerals from the host sediments. The technique is based on the exchange of cations in the minerals that may be associated clay minerals in sediments, such as Ca and Mg from dolomite; Ca from calcite, gypsum and francolite with cations carried by resin radicals. The associated minerals such as gypsum, calcite, dolomite and francolite are removed in descending order. Separation of clay minerals using cation exchange resins is less aggressive than that by other classic treatments. The efficiency of amberlite IRC-50H in the removal of associated minerals is greater than that of amberlite IR-120.     

D190型大孔巯基树脂分离富集原子吸收光谱法测定地质样品中微量金和钯

采用D190 型大孔巯基树脂分离富集微量金和钯 ,研究了各种条件对分离富集和测定的影响 ,证明了金和钯在 3 %王水介质中形成氯络阴离子与树脂上的巯基 (-SH)发生螯合作用形成螯合物而迅速地被吸附在树脂上。同时 ,溶液中一些贱金属离子不易与巯基生成螯合物而分离。采用酸性硫脲定量洗脱 ,树脂结构不被破坏 ,可重新使用     

锆石环氧树脂靶表面形貌特征及对LA-ICP-MS分析影响研究

激光剥蚀电感耦合等离子体质谱（LA-ICP-MS）是目前锆石研究常用方法之一,该法普遍采用环氧树脂靶为载体,对锆石环氧树脂靶表面形貌及平整度影响进行研究,有助于评估其制作工艺以及LA-ICP-MS锆石分析的准确性。本次研究采用原子力显微镜（AFM）对锆石环氧树脂靶表面进行形貌分析,并通过分析和对比193nm激光不同剥蚀模式和不同剥蚀条件下的锆石表面形貌,研究锆石表面形貌及平整度对LA-ICP-MS锆石分析的影响;同时实验采用氩离子抛光技术对锆石环氧树脂靶进行二次抛光,并探讨该技术对锆石环氧树脂靶影响。实验结果表明本次靶中表面总体平整性较好但存在细微的不平,锆石表面存在程度较小（几至几十纳米的不等）的擦痕,锆石颗粒边缘与靶面存在高差和间隙;而通过研究后认为锆石表面细微的不平对于分析的影响小于能量密度、频率、移动速率等其他激光参数的影响,对分析准确性的影响较小。实验分析并对比了锆石和玻璃标准等不同基体的线扫描形貌,发现其剥蚀深度以及剥蚀形貌存在差异,相同剥蚀条件下线扫描剥蚀深度：NIST610 > CGSG系列 > 锆石91500。经氩离子二次抛光后锆石样品表面擦痕不明显,但可能会对锆石造成损伤等影响。本次研究认为锆石环氧树脂靶表面总体平整性较好,锆石表面细微的不平对分析准确性的影响较小,不同基体的线扫描形貌研究则为LA-ICP-MS锆石及其他分析提供了参考,而氩离子抛光技术对LA-ICP-MS分析的影响及应用还有待进一步的研究。