聚乙烯亚胺螯合-超滤分离富集电感耦合等离子体质谱法测定海水中6种痕量金属元素

建立了高分子聚合物螯合-超滤(PCP-UF)分离富集、电感耦合等离子体质谱(ICP-MS)测定海水中痕量金属元素的方法.海水中的Cu(2+),Pb(2+),Cd(2+),Co(2+),Ni(2+)等金属离子与聚乙烯亚胺(PEI)形成高分子螯合物,经超滤截留、酸解离后,实现金属离子从海水中定量分离、富集.ICP-MS采用...     

PAN-S浸渍树脂富集方波溶出法测定痕量的铅、镉、铜和锌

用1-(2-吡啶偶氮)-2-萘酚-6-磺酸(PAN-S)水溶液处理201×7强碱性阴离子交换树脂,制备了具有PAN-S功能团的浸渍树脂。经过最佳条件选择,在同一水样中,可以同时富集Pb2 、Cu2 、Zn2 、Cd2 。实验结果表明,PAN-S树脂用于痕量元素的分离富集具有交换速度快、易于洗脱、富集倍数大、选择性好等优点。建立了PAN-S树脂富集-分离铅、镉、铜和锌离子的方波溶出法的测定方法,并可用于海水中的测定,结果令人满意。     

液膜富集技术与分光光度法测定痕量稀土

在分析化学中用液膜富集痕量物质是一个新课题,而关于痕量稀土的液膜富集方法,迄今报道甚少。为此,我们研究了液膜萃取富集分离ppb级稀土的方法,并提出了稀土的分组富集方法,从而提高了分光光度法测定稀土的灵敏度。 (一)主要试剂 兰113A(单丁二酰亚胺)作为液膜的表面活性剂,P507(2-乙基己基膦酸单2-乙基     

黄原脂棉分离-石墨炉原子吸收光谱法测定咸味食品中的镉

正黄原脂棉是由纤维素与氢氧化钠反应生成碱纤维后与二硫化碳发生磺化反应的产物,即二硫代甲酸钠纤维素酯,又称黄原酯棉,属纤维素改性产物~([1])。改性纤维素(一般指螯合纤维素)在分离富集金属元素方面有着广泛的应用。其中,巯基棉最为广泛,用巯基棉分离富集痕量金属元素已有许多报道~([2-10])。用巯基棉富集空气中的汞~([11]),已被列为行业标准,但其缺点是巯基棉制备过程较复杂,尤其是     

固相萃取-电感耦合等离子体质谱（ICP-MS）法测定海水中6种金属元素

为了实现海水中金属元素的绿色分离和快速检测,建立了新型螯合树脂为填料,固相萃取-电感耦合等离子体质谱（ICP-MS）测定海水中6种金属元素含量的方法。海水中Cu,Pb,Co,Ni,Cr,Mo金属离子与亚氨基二乙酸型螯合树脂形成螯合物,经固相萃取、洗脱,实现金属离子从海水中定量分离富集。在最佳实验条件下,测得方法的相对标准偏差（RSD）为1.7 %～3.6 % ,加标回收率为82.6 %～102 %,检出限为0.03 μg /L～0.15 μg /L。本研究采用亚氨基二乙酸型螯合树脂为填料的固相萃取,实现了海水分析的绿色样品前处理方法,与ICP-MS相结合用于海水标准样品和实际样品的分析,获得了满意的结果。     

多金属结核/结壳中稀土元素的富集特征及其资源效应

多金属结核/结壳是海洋中最重要的固体沉积矿产之一,蕴藏丰富的铁、锰、铜、钴、镍等金属元素,也是稀土元素的富集体.利用等离子质谱仪/光谱仪对太平洋、大西洋、印度洋及南海北部海多金属结核/结壳11个样品25份试样的稀土含量进行了分析,多金属结核/结壳中稀土平均含量为1265 57×10-6,其中结核平均含量为1096.96×10-6,结壳平均含量1623.88×10-6,人人超过地壳和玑积岩的平均含量.稀土元素的富集主要受控于结核/结壳中铁、锰氧化物及粘土矿物对海水和沉积物中稀土元素的吸附作用,Ce元素高度富集,使其成为多金属结核/结壳矿产开发中可能最先利用的稀土元素之一.     

在 HEH(EHP)萃取色谱柱上负载量对稀土色谱分离的影响

化学光谱法目前仍然是高纯稀土分析的主要方法。因此,稀土杂质的富集分离仍然是稀土分析研究的一项重要内容。高纯稀土中稀土杂质的化学分离,大多采用以α-羟基异丁酸或其它羟基羧酸为洗提剂的离子交换色谱。由于萃取色谱法兼有溶剂萃取法的高选择性和色谱法的高效性双重优点,因而发展很快。早在六十年代末,国外就有人将二-(2-乙基己基)磷酸(以下简称D_2EHPA)为固定相的萃取色谱技术应用于高纯稀土分析。近年来,国内有人在高纯稀土分析中采用以2-乙基己基膦酸2-乙基己酯(以下简称HEH(EHP)为固定相的萃取色谱。彭春霖等对HEH(EHP)-盐酸体系中各稀土元素的分配比已作了详细报导,为稀土的     

微柱分离富集电感耦合等离子体质谱法测定海水中痕量稀土元素

1　引　　言海水中的稀土元素 (ＲＥＥｓ)在海洋地球化学的研究中起着特殊的作用。常用的方法有共沉淀法、溶剂萃取等 ,溶剂萃取等 ,但操作都比较烦琐。本文采用螯合官能团纤维微柱可同时分离基体并富集痕量ＲＥＥｓ组分 ,分离与富集一步完成 ,是理想的预处理技术。本文根据前期工作制备了 8 羟基喹啉 5 磺酸纤维滤纸片 ,以此作为微柱填充物 ,分离和富集了海水中的多种痕量稀土元素 ,实验结果令人满意。2　实验部分2 1　仪器与试剂　电感偶合等离子体原子发射光谱仪 (美国Ｌｅｅｍａｎ公司 ) ,电感偶合等离子体质谱 (英国ＶＧ公司 )。定量…     

海水痕量金属元素分析中前处理技术的研究进展北大核心CSCD

痕量金属元素在海洋生态系统中发挥着不可或缺的作用,准确测定海洋中的痕量金属元素对海洋生态系统的结构和功能有重要意义。为降低海水基体效应,提高测定准确度,综述了海水痕量金属元素分析中的前处理技术,包括螯合-溶剂萃取法、共沉淀法、稀释-直接进样法、氩气在线稀释法和基于螯合树脂的固相萃取法,比较了各方法的优劣和适用性,并对该领域的发展趋势进行了展望(引用文献75篇)。     

异烷基膦酸1-甲庚基酯负载树脂分离原子吸收光谱法测定氧化钇中痕量铕铽铒和镱

异烷基膦酸1-甲庚基酯(代号5712)是在较低酸度下具有优良稀土分离性能的萃取剂。本文测定了15种稀土(Ⅲ)在5712-负载树脂与不同浓度的HNO_3之间的分配比。研究了5712-负载树脂柱分离Y、Tb、Dy、Ho、Er的最优条件。0.58mol/L HNO_3可使这5种元素分离良好。利用5712-负载树脂分离和富集高纯氧化钇中痕量Eu、Tb、Er和Yb,然后再以原子吸收光谱法测定。经过本法分离和富集,除去了大量基体,从而提高了测定的灵敏度。     

AG50W-x8树脂分离去除钡的多原子离子对电感耦合等离子体质谱法测定稀土元素的质谱干扰

采用AG50W－x8阳离子交换树脂,以HNO3作为梯度淋洗剂,可有效地分离Ba和稀土元素,实验表明：以2mol/L HNO3淋洗时,99．5％的Ba被分离去除;以5mol/L HNO3淋洗时,稀土的回收率在96－110％之间。标准参考物质的分析结果显示测定值与标准值十分接近,表明AG50W－x8阳离子交换树脂分离可有效地去除Ba元素的多原子离子（BaO^ ,BaOH^ )对ICP－MS法测定稀土元素测定的质谱干扰,该方法准确,可靠。同时,为准确测定Eu提供了一条新的途径。     

Flow injection on-line solid phase extraction coupled with inductively coupled plasma mass spectrometry for determination of (Ultra)trace rare earth elements in environmental materials using maleic acid grafted polytetrafluoroethylene fibers as sorbent

A new sorbent, maleic acid grafted polytetrafluoroethylene fiber (MA-PTFE), was prepared and evaluated for on-line solid-phase extraction coupled with inductively coupled plasma mass spectrometry (ICP-MS) for fast, selective, and sensitive determination of (ultra)trace rare earth elements (REEs) in environmental samples. The REEs in aqueous samples at pH = 3.0 were selectively extracted onto a microcolumn packed with the MA-PTFE fiber, and the adsorbed REEs were subsequently eluted on-line with 0.9 mol l(-1) HNO3 for ICP-MS determination. The new sorbent extraction system allows effective preconcentration and separation of the REEs from the major matrix constituents of alkali and alkali earth elements, particularly their separation from barium that produces considerable isobaric interferences of 134Ba16O1H+, 135Ba16O+, 136Ba16O1H+, and 137Ba16O+ on 151Eu+ and 153Eu+. With the use of a sample loading flow rate of 7.4 ml min(-1) for 120 s preconcentration, enhancement factors of 69-97 and detection limits (3s) of 1-20 pg l(-1) were achieved at a sample throughput of 22 samples h(-1). The precision (RSD) for 16 replicate determinations of 50 ng l(-1) of REEs was 0.5-1.1%. The developed method was successfully applied to the determination of (ultra)trace REEs in sediment, soil, and seawater samples.     

Sequential determination of ultra-trace highly siderophile elements and rare earth elements by radiochemical neutron activation analysis: Application to pallasite meteorites

An analytical scheme of radiochemical neutron activation for the sequential determination of ultra-trace rare earth elements (REEs) and highly siderophile elements (HSEs) in geological and cosmochemical samples is presented. Using this procedure, several selected elements of REEs and HSEs were successively determined for geological reference samples and olivine crystals separated from pallasite meteorites. Based on the data for geological reference samples, it was concluded that the procedure presented in this study could yield data usable for cosmochemical discussion of the genesis of pallasite meteorites.     

Determination of rare earth and other elements in algae by ICP-MS and neutron activation analysis

Several rare earth elements (REEs) and other elements in algae were investigated by ICP-MS and INAA. Algae materials were supplied from an IAEA Intercomparison Study:Chlorella vulg. grown under reduced levels of toxic elements (IAEA-391) and IAEA-393 algae was grown in a medium to which certain toxic elements were added. 34–691 mg of algae samples were dissolved in conc, nitric acid using a microwave sampleppreparation system. REEs could be detected in the order of magnitude of 10⁻³ ng/g by ICP-MS. Activation analysis failed to detect any REEs because of a strong interference due mainly to²⁴Na and³²P. The distriubtion patterns of these REEs in algae slightly differed from those ofCarya sp. and tobacco leaves, and differed significantly from that of fern leaves. The distribution pattern was rather similar to that found in the North American shale composite (NASC).     

Comparative Coprecipitation of Phosphate and Arsenate with Yttrium and the Rare Earths: The Influence of Solution Complexation

Coprecipitation of yttrium (Y) and rare earth elements (REEs) with phosphate and arsenate removes these elements from solution in variable proportions. During both phosphate and arsenate Coprecipitation, middle REEs (Sm and Eu) are progressively depleted in solution relative to heavier and lighter elements. Solution complexation by oxalate (Ox ^2-) influences Y and REE removal patterns by strongly enhancing the retention of Y and the heaviest REEs in solution. The extent of this enhancement is well described by a quantitative account of the comparative solution complexation of Y and REEs as M(Ox)⁺ and M(Ox) . The comparative behavior of phosphate and arsenate coprecipitation exhibits both similarities and differences. During arsenate coprecipitation the light REEs are retained in solution, relative to the heavy REEs, to a greater extent than is the case for phosphate coprecipitation. Notable irregularities are observed in the comparative coprecipitation behavior of nearest-neighbor elements (e.g., Eu–Gd–Tb and Tm–Yb–Lu). Such irregularities are very similar for phosphate and arsenate coprecipitation in the absence and in the presence of solution complexation.     

Determination of rare earth elements in human blood serum by inductively coupled plasma mass spectrometry after chelating resin preconcentration

The determination of all rare earth elements (REEs) in human blood serum by inductively coupled plasma mass spectrometry (ICP-MS) was performed with the aid of chelating resin (Chelex 100) preconcentration after acid digestion with HNO3 and HClO4. When chelating resin preconcentration was carried out at room temperature, the recoveries of heavy REEs were lower than those of light REEs because of their stable complex formation with residual organic compounds remaining in the digested serum solution. These problems were overcome by heating the solution at 80 degrees C during the chelating resin preconcentration process. As a result, the recoveries for all REEs were improved to 92-102% in the case of a concentration factor of 4, where the analytical detection limits for REEs were below 0.2 x 10(-12) g ml-1. Consequently, all REEs in individual human blood sera collected from five healthy volunteers could be determined by ICP-MS with good precision. The concentrations of REEs in human blood serum were extremely low, in the range from ca. 1 x 10(-12) g ml-1 of Eu to ca. 230 x 10(-12) g ml-1 of Ce.     

REE bound DNA in natural plant

The binding of rare earth elements (REEs) with nucleic acids in the leaves of fern Dicranopteris dichotoma (DD) has been studied by molecular activation analysis (MAA). The REEs bound DNA (REE-DNA) was obtained from the leaves of DD. The CTAB-based procedure was modified for extraction of total DNA. The purity of DNA was examined by UV spectroscopy. The DNA obtained was separated and determined by agarose gel electrophoresis further. Meanwhile, the contents of eight rare earth elements (La, Ce, Nd, Sm, Eu,Tb, Yb and Lu) in REE-DNA were detected by instrumental neutron activation analysis (INAA). The results showed that REE-DNA with higher purity could be extracted from plant using this method. It was also found that REEs were bound firmly with DNA in the leaves of DD. The molecular weight (MW) of REE-DNA band was about 22 kb in agarose gel electrophoresis.     

Determination of REEs distribution in monazite and xenotime minerals by ion chromatography and ICP-AES

Ion chromatographic techniques were investigated for the separation and the quantitative determination of some rare earth elements (REEs) in monazite and xenotime minerals. The influences of selected eluents containing complexing acids including oxalic and alpha-hydroxy isobutyric acid (alpha-HIBA) on the retention and hence the separation efficiency of REEs was studied. Different variables affecting the separation of different REEs such as pH, type, and concentration of the mobile phase were investigated. Gradient elution, using an advanced gradient pump, was controlled automatically by the Dionex AI-450 computer software. Separation of REEs was carried out using an Ion Pac CS5A column followed by a post column derivatization reaction with 4-(2-pyridylazo)resorcinol (PAR) and UV-VIS spectrophotometric detection. Mineral dissolution was carried out using sulfuric acid. A comparative evaluation of REE distribution in monazite and xenotime minerals using both ion chromatography (IC) and inductively coupled plasma atomic emission spectrometric (ICP-AES) techniques was carried out.     

Determination of rare earth elements in chloroplasts of Brassia napus by INAA and biochemical separation techniques

Intact chloroplasts were isolated from mesophyll protoplasts of Brassia napus. Concentrations of 8 rare earth elements (REEs) in the chloroplasts were determined by instrumental neutron activation analysis (INAA). The results showed that there were trace amounts of REEs in the chloroplasts, which corresponded to 1 atom of REEs per 2000 chlorophyll molecules. About 30% of the total REEs in the leaves are localized in the chloroplasts and the light REEs were enriched with respect to the heavy elements of the series.     

Development of a Mixed Organic Acid Extractant for the Evaluation of Plant Availability of Rare Earth Elements in Soils

In recent years, fertilizers containing rare earth elements (REEs) have been used widely in agriculture (1, 2) and it may result in a potential increase in the contents of REEs in soil and cause environmental pollution. Therefore it is very important to obtain more knowledge of environmental effects of REEs in order to predict any possible deleterious effect occasioned by their use.