Accurate Measurement of Rare Earth Elements by ICP‐MS after Ion‐Exchange Separation: Application to Ultra‐Depleted Samples     

Marc Ulrich  Sarah Bureau  Catherine Chauvel  Christian Picard 《Geostandards and Geoanalytical Research》2012,36(1):7-20

This study reports precise and accurate data for rare earth elements (REE) measured on eight geological reference materials, five enriched in REE (BE‐N, BHVO‐2, BR, BR‐24 and RGM‐1) and three very depleted in REE (BIR‐1, UB‐N and DTS‐2). Data were acquired by quadrupole ICP‐MS after isolation of the REE using an ion‐exchange chromatography procedure. All the measured REE abundances were similar within ≈ 5% (10% for the most REE‐depleted sample DTS‐2) to the high‐quality measurements previously published in the literature. We also show that by using an internal Tm spike, the reproducibility of the data was improved to ～ 1%. Applying this technique to the analysis of ultra‐depleted rock samples (sub ng g^?1), we show that significant improvements were obtained relative to the routine trace element measurement method. The chondrite‐normalised patterns were smooth instead of displaying irregularities. Although the classical method gives excellent results on REE‐rich samples, we believe that our technique improves the precision and accuracy of measurements for highly REE‐depleted rocks.  相似文献   

过氧化钠碱熔-电感耦合等离子体发射光谱法测定钛铁矿中铬磷钒   总被引：3，自引：2，他引：1  

王卿  赵伟  张会堂  周长祥  回寒星 《岩矿测试》2012,31(6):971-974

样品经过氧化钠碱熔,溶解后的上层清液直接酸化,用电感耦合等离子体发射光谱测定钛铁矿中铬、磷、钒的含量。确定了钛铁矿石中Cr、P、V的分析谱线、光谱级次;为了消除钠盐基体的影响,确定稀释因子为1000,标准曲线基体与样品基体保持一致;为避免过氧化钠熔矿后溶液碱性较大对进样系统造成腐蚀,加入2.00 mL盐酸对溶液进行酸化。方法检出限为4.46～23.55μg/g,采用国家一级标准物质进行验证,方法准确度小于10%,精密度为0.68%～9.90%。本法与分光光度法单一元素测定相比较,具有测量范围宽、结果准确、操作简便、省时省力、适合大批量样品测定等突出的优点。  相似文献   

过硫酸钠氧化-流动注射化学发光法在地下水腐植酸含量测定中的应用     

杨胜科  崔文夏  赵钺  陈静  刘凯  李斌 《岩矿测试》2012,31(4):677-681

在碱性条件下过硫酸钠能氧化腐植酸发生化学发光反应。本研究以过硫酸钠-腐植酸化学发光体系为基础,建立了腐植酸的过硫酸钠氧化-流动注射化学发光测定方法,同时对测定方法的负高压及增益、泵速、过硫酸钠浓度、氢氧化钠浓度等影响因素进行了优化实验。方法的线性范围为0.1～500 mg/L(相关系数为0.9985),检出限为0.076 mg/L,对浓度为0.5 mg/L的腐植酸进行11次平行测定,相对标准偏差(RSD)为3.47%。利用该方法对5种不同地区地下水中的腐植酸进行测定,样品的加标回收率在98.33%～107.50%之间。该方法无需分离,简单易行,对实际样品测定结果满意。  相似文献   

温度和铜离子浓度对近江牡蛎超氧化物岐化酶活力的联合效应     

王辉  杨洪帅  刘加慧  李艳红  刘志刚 《海洋学报(英文版)》2016,35(4):51-57

Superoxide dismutase(SOD) is a crucial antioxidant enzyme playing the first defense line in antioxidant pathways against reactive oxygen species in various organisms including marine invertebrates. There exist mainly two specific forms, Cu/Zn-SOD(SOD1) and Mn-SOD(SOD2), in eukaryotes. SODs are known to be concurrently modulated by a variety of environmental stressors. By using central composite experimental design and response surface method, the joint effects of water temperature(18–34°C) and copper ion concentration(0.1–1.5 mg/L) on the total SOD activity in the digestive gland of Crassostrea ariakensis were studied. The results showed that the linear effect of temperature was highly significant(P0.01), the quadratic effect of temperature was significant(P0.05); the linear effect of copper ion concentration was not significant(P0.05), while the quadratic effect of copper ion concentration was highly significant(P0.01); the interactive effect of temperature and copper ion concentration was not significant(P0.05); the effect of temperature was greater than that of copper ion concentration. The model equation of digestive gland SOD enzyme activity towards the two factors of interest was established, with R2 and predictive R2 as high as 0.961 6 and 0.820 7, respectively, suggesting that the goodness-offit to experimental data be very satisfactory, and could be applied to prediction of digestive gland SOD activity in C. ariakensis under the conditions of the experiment. Our results would be conducive to addressing the health of aquatic animals and/or to detecting environmental problems by taking SOD as a potential bioindicator.  相似文献   

硫酸钠亚型盐湖卤水不同温度下Li~+富集、结晶行为研究——以西藏拉果错盐湖为例   总被引：1，自引：0，他引：1  

马艳芳  张志宏  李侃社  董生发  付振海  胡天琦 《地球学报》2016,37(3):307-312

西藏拉果错盐湖属于硫酸钠亚型盐湖,卤水含有钾、锂、硼等有价值组分,针对此类盐湖资源,研究锂的富集过程非常必要。通过硫酸钠亚型盐湖卤水的变温蒸发过程,对比了锂在不同温度下富集规律和饱和点,卤水中的锂在蒸发过程中主要以硫酸锂和锂芒硝等形式结晶,在此基础上建立了锂和硫酸根浓度与温度变化关系的相关性,根据组成和温度,计算了浓度熵,模拟了锂饱和点和浓度熵的关系方程;利用浓度熵方程,控制锂盐析出,从而实现获得高锂浓度的卤水,为硫酸钠亚型盐湖卤水天然蒸发富集锂和盐湖资源高效利用提供依据。  相似文献   

电感耦合等离子体发射光谱法测定稀土矿石中15种稀土元素——四种前处理方法的比较   总被引：4，自引：4，他引：0  

吴石头  王亚平  孙德忠  温宏利  许春雪  王伟 《岩矿测试》2014,33(1):12-19

稀土元素在矿石中有多种不同的赋存形式,主要有离子吸附型和矿物晶格型,稀土不同赋存形态对其本身准确分析测定有很大的影响。本文从稀土元素在矿石中不同赋存形态的角度出发,探讨了不同前处理方法对稀土准确测试结果的影响,采用盐酸-硝酸-氢氟酸-高氯酸(四酸)敞开酸溶、盐酸-硝酸-氢氟酸-高氯酸-硫酸(五酸)敞开酸溶、氢氟酸-硝酸封闭压力酸溶、氢氧化钠-过氧化钠碱熔四种方法对离子吸附型和矿物晶格型两类赋存类型的稀土矿石样品进行前处理,电感耦合等离子体发射光谱法测定其中的15种稀土元素。结果表明:对于离子吸附型的稀土矿石标准物质(GBW 07161、GBW 07188),四酸敞开酸溶法测定的结果明显偏低,15种稀土元素大都偏低10%~20%,五酸敞开酸溶法、封闭压力酸溶法和碱熔法的测定值与标准值吻合;而对于稀土以离子化合物及类质同象置换的形式赋存于矿物晶格中的白云鄂博轻稀土矿石样品,三种酸溶法结果较碱熔法均偏低,其中四酸敞开酸溶法偏低最多,约偏低20%左右,五酸敞开酸溶法和封闭压力酸溶法偏低5%~15%。本文提出,对于离子吸附型稀土矿,五酸敞开酸溶法和封闭压力酸溶法可以代替传统操作复杂的碱熔法,但对于稀土以离子形式赋存于矿物晶格型的稀土矿,目前最合适的前处理法是传统的碱熔法。  相似文献   

高效液相色谱法测定盐酸阿考替胺三水合物工业品含量     

周圩群  乔俊琴  练鸿振 《岩矿测试》2014,33(6):871-875

盐酸阿考替胺三水合物为第一个胃肠蠕动改善药物,用来治疗功能性消化不良,作为一种新药,其分析测定方面的报道甚少,已有的报道采用高效液相色谱(HPLC)以甲醇-磷酸二氢钾-辛烷磺酸钠为流动相进行测定,由于使用了离子对试剂辛烷磺酸钠,因而分析过程比较耗时且保留不够稳定。本文基于盐酸阿考替胺三水合物为两性化合物,建立了测定其含量的高效液相色谱分析方法。测定方法采用C18(4.6 mm×150 mm,5 μm)色谱柱,以甲醇-20 mmol/L乙酸铵水溶液=45:55(V/V)为流动相(pH 6.8)进行等度洗脱,紫外检测波长选择280 nm,盐酸阿考替胺三水合物的保留时间合适且峰形较好,出峰时间为8 min,总分析时间为23 min。在优化色谱条件下,盐酸阿考替胺三水合物的浓度在0.0006~1.0 mg/mL范围内线性关系良好,检出限为0.0002 mg/mL,日内、日间测定的相对标准偏差(RSD)均小于1.0%。该方法不添加离子对试剂,有利于色谱系统的快速平衡,提高了实验的重复性和可操作性,可对盐酸阿考替胺三水合物工业品进行快速分析,实现对原料药的质量控制。  相似文献   

广东禾尚田矿区新类型风化壳离子吸附型稀土矿的发现及意义   总被引：1，自引：0，他引：1  

黄华谷 《地质与勘探》2014,50(5):893-901

在广东禾尚田矿区,通过地表和钻孔岩芯样品的野外硫酸铵浸泡-草酸点滴试验、化学分析、稀土（REE）配分分析、稀土浸取率测定等工作,首次发现了灰岩风化壳中存在离子吸附型富铕稀土工业矿床。稀土矿与坡残积钨锡矿、铷矿共伴生,并伴生锂、镓和铯等元素,具有中稀土富集和高浸取率的特点,是离子吸附型稀土矿的新类型。它的发现将对离子吸附型稀土矿床勘查产生深远的影响,大大拓展找矿思路和对象;并说明了在一个矿田或一个矿区内寻找新的矿种、新的矿床类型、新的含矿层位的重要性。通过成矿地质条件分析,作者认为矿区西部找矿前景甚佳,禾尚田矿区将成为一个集有色、稀有、稀土、贵金属矿产的多矿种、多矿床类型、多含矿层位的矿区。  相似文献   

An Eco-Friendly High-Effective Scale Inhibitor for High Salt Brine     

ZHANG Xin  SHAO Qianqian  CUI Zhaojie  TAN Xianfeng 《《地质学报》英文版》2014,88(Z1):408-409

正Now the mining of high salt underground brine has been an important aspect of salt lake mining,which is the necessary support to the development of national economy.With the change of underground geological  相似文献   

广西岑溪糯垌稀土矿床地质特征及成矿规律     

黄长帅  廖航  卢见昆  吴继炜 《矿产与地质》2014,(5):551-554

文章阐述了岑溪糯垌稀土矿床地质特征及其矿石特征、矿石有用组分含量及变化规律、矿石化学成分、矿石浸取率及稀土元素配分类型等,认为岑溪糯垌稀土矿床属黑云钾长(二长)花岗岩风化壳离子吸附型稀土矿床,稀土元素配分类型为低铕富镧钕轻稀土型,矿层主要赋存于花岗岩全风化层中。  相似文献