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高纯氧化钆中稀土杂质的化学光谱分析 总被引:4,自引:1,他引:4
化学光谱法是高纯稀土分析的主要方法,近年来,以P507萃淋树脂为固定相的萃取色谱法,对稀土元素的分离进行了系统的研究。本工作是在高纯氧化钕中14个稀土杂质化学光谱分析的基础上,研究高纯氧化钆中稀土杂质的分离条件。在φ14×1000的恒温色层柱上,以盐酸为淋洗剂,偶氮胂Ⅲ柱上显色,梯度淋洗,分离富集高纯氧化钆中稀土杂质,富集倍数2000倍以上,富集物经化学处理,光谱测定。测定下限∑RE7ppm,变异系数为10—25%,适用于99.999%氧化钆中14个稀土杂质元素的测定。 相似文献
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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 相似文献
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感耦等离子体质谱法(ICP—MS)测定高纯氧化镝中痕量稀土杂质 总被引:1,自引:0,他引:1
本文报道用2-乙基己基膦酸单酯萃淋树脂为固定相,HCl为淋洗液的萃取色谱法研究了高纯Dy2O3中的痕量稀土杂质和Dy2O3基体的分离条件,并用ICP-MS法测定了高纯Dy2O3中的14个稀土杂质,稀土元素的测定限为0.001-0.005ICP-MS法测定了高纯Dy2O3 相似文献
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ICP-MS 法测定高纯氧化铕中稀土杂质的研究 总被引:5,自引:1,他引:4
深入考察了ICP-MS法测定高纯氧化铕时基体对稀土杂质测定的影响,研究了P507萃淋树脂分离大量基体Eu2O3的实验条件,建立了采用内标补偿直接测定大部分稀土杂质和经P507萃淋树脂分离基体后测定被干扰离子Tm相结合的高纯Eu2O3中稀土杂质的ICP-MS分析方法。方法检出限为0.005~0.021μg/L,加标回收率为84%~112%。RSD为1.4%~8.1%。本法适用于质量分数为99.99%~99.9999%的高纯Eu2O3中稀土杂质的分析。 相似文献
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高纯氧化铕中微量稀土杂质的化学光谱测定 总被引:2,自引:0,他引:2
将高纯Eu2O2通过P507萃淋树脂分离富集,分离掉大量基体Eu2O3剩下微量稀土杂质用碳粉吸附,加KBH4作载体进行光谱测定,本方法可测定99.9999%,纯度的Eu2O3中微量稀土杂质。 相似文献
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Cyanex272负载树脂分离-ICP-MS法测定高纯氧化钕中痕量稀土杂质 总被引:4,自引:0,他引:4
采用萃取色谱法,以Cyanex272负载树脂为固定相制成微型分离柱,以HCl为淋洗液,研究了Nd2O3基体的分离条件,分离周期为35min。建立了分离Nd后测定Tb、Dy、Ho以及内标补偿法直接测定其它稀土杂质的高纯Nd2O3中14个稀土杂质的ICP MS分析方法。方法检出限为0.03~0.30μg g,加标回收率为91.0%~110.0%,相对标准偏差为2.0%~4.9%。方法可满足快速测定99 999%Nd2O3中14个稀土杂质的要求。 相似文献
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T. R. Bangia B. A. Dhawale V. C. Adya M. D. Sastry 《Fresenius' Journal of Analytical Chemistry》1988,332(7):802-804
Summary Inductively Coupled Plasma-Atomic Emission Spectrometric and Direct Current Arc-Emission Spectrometric methods have been developed for the determination of rare earths in nuclear grade graphite. The graphite matrix was selectively removed from the analytes by controlled heating in air at 900°C in a muffle furnace. The residual ash containing analytes was dissolved and analysed by ICP-AES for rare earths specially required for assessing the nuclear purity, viz. Dy, Eu, Gd and Sm and for all rare earths, Sc and Y by D.C.arc-AES by photographing their spectra in III order on an 3.4 M Ebert Spectrograph. The recovery of rare earths after ashing was confirmed using -activities of141Ce,152–154Eu,153Gd,170Tm and169Yb which was found to be quantitative within experimental error.
Bestimmung von Sc, Y und Lanthaniden in nuklear-reinem Graphit mit Hilfe der ICP-AES und der Gleichstrombogen-Spektrometrie相似文献
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本文采用国产WPG-100型一米光栅摄谱仪、GP3.5-D1型高频等离子体发生器、气动雾化器,以不去溶方式进样直接测定纯度为99.995%的氧化钇中十四个稀土杂质元素。其中除镨(17μg/g)和钸(7μg/g)外,测定下限均为0.3-3μg/g(以氧化物计)。当被测元素的含量为3-17μg/g时,相对标准偏差为2.3-7.3%(钸和镨除外)。样品用盐酸溶解,酸度和共存元素的影响很小,方法简便、快速。 相似文献
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R. Vijayalakshmi D. K. Singh M. K. Kotekar H. Singh 《Journal of Radioanalytical and Nuclear Chemistry》2014,300(1):129-135
A solvent extraction process for the production of nuclear grade Gd2O3 for its applications in pressurized heavy water reactor (PHWR) from a crude concentrate of rare earths containing ~70 % Gd2O3 has been developed and tested on bench-scale and continuous counter-current operations. The separation of gadolinium from other rare earths with similar chemical properties has been successfully accomplished by adopting a dual cycle solvent extraction employing 2-ethylhexylphosphonic acid, mono-2 ethylhexyl ester (EHEHPA) as an extractant. Taking advantage of the extraction order of rare earths with EHEHPA, in the first cycle, heavy rare earths including Tb, Dy and Y were separated in the product strip solution, while gadolinium was separated in the raffinate solution along with samarium and neodymium. In the second cycle, gadolinium was purified to the extent of >99.5 % with respect to other rare earths. Effects of process variables such as aqueous acidity, phase ratio, metal concentration in the aqueous feed, scrubbing and stripping acidity etc. on separation of terbium and other heavy rare earths in the first cycle and upgrading the purity of Gd2O3 in the second cycle have been investigated. The experimental conditions were optimized using computer simulation and validated by bench scale counter-current operations. Under optimized conditions of process parameters, continuous operations of mixer settler yielded kilogram quantity of nuclear pure Gd2O3 which was subsequently converted to gadolinium nitrate for PHWR application. The overall recovery was found to be >98 %. 相似文献
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稀土在烤烟植株中的分布及其对烟叶化学成份影响的研究 总被引:1,自引:0,他引:1
作为一种生理活性物质,稀土施用在烟草上平均增产11%,上中等烟比例提高7.53%左右,稀土应用于烤烟大部分限于田间试验,缺深入的机理研究^[2-4]。本试验用低浓度混合硝酸稀土喷施烤烟叶面,研究了稀土在烤烟植株中的含量,分布及土壤中可溶态稀土的变化情况及稀土对烟叶化学成份的影响,旨在为烤烟施用稀土提供科学依据。 相似文献
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N. I. Molla S. M. Hossain S. Basunia R. U. Miah M. Rahman D. H. Sikder M. I. Chowdhury 《Journal of Radioanalytical and Nuclear Chemistry》1997,216(2):213-215
The concentration of rare earths and other elements have been determined in the bed sediment samples of Karnafuli estuarine zone in the Bay of Bengal by instrumental neutron activation analysis (INAA). The samples and the standards soil-5, soil-7, coal fly ash and pond sediment were prepared and simultaneously irradiated for short and long time at the TRIGA Mark-II research reactor facility of Atomic Energy Research Establishment, Savar, Dhaka. The maximum themal neutron flux was of the order of 1013 n·cm–2·s–1. After irradiation the radioactivity of the product nuclides was measured by using a high resolution high purity germanium detector system. Analysis of -ray spectra and quantitative analysis of the elemental concentration were done via the software GANAAS, it has been possible to determine the concentration level of 27 elements including the rare earths La, Ce, Sm, Eu, Tb, Dy and Yb and uranium and thorium. 相似文献
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Nguyen Van Suc H. B. Desai R. Parthasarathy S. Gangadhaŕan 《Journal of Radioanalytical and Nuclear Chemistry》1992,164(5):321-325
Individual rare earth impurities in high purity La2O3 (99.9%) have been determined by NAA after pre-separation of the matrix (La). The separation is carried out on an anion exchanger (Dowex 1×8) using different mixtures of methanol/nitric acid as eluants. The rare earth elements from Dy to Lu are eluted quantitatively using a 10% 1M HNO3-90% methanol mixture, while the light rare earths from Ce to Gd are eluted quantitatively using a 10% 0.05M HNO3-90% methanol mixture. La, which is retained on the column, is eluted using 0.1M HNO3. The recoveries of the various rare earth elements have been checked using radiotracers and also by spiking the sample with known amount of elements, and the recoveries are found to be quantitative. Results obtained on a typical high purity lanthanum oxide are reported here. 相似文献
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偶氮氯膦Ⅲ吸光光度法测定轻、重稀土元素和钇 总被引:1,自引:0,他引:1
本文研究了稀土元素与偶氮氯膦Ⅲ的α型及β型显色反应。在一定条件下,重稀土元素(Gd-Lu)同偶氮氯膦Ⅲ螯合物可由α型转变成β型,其中钇的螯合物转成β型倾向最大,而轻稀土元素在相同条件下仅形成α型,利用Zn-EDTA和Zn-CyDTA的掩蔽效应,可扩大显色反应的差异性。提出了在HCl-NaAc介质中分别测定轻、重稀土元素及钇的方法:在pH2.9-3.4范围内,用Zn-CyDTA作掩蔽剂,可在重稀土存在下测定轻稀土元素。在pH1.8-2.4和pH2.8-3.6,用Zn-EDTA、NaF或NaF作掩蔽剂可分别测定钇及重稀土元素。 相似文献
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The determination of rare earths in minerals by activation analysis is described. The rare earths are separated as a group from the bulk of the material before irradiation. After irradiation the rare earths are separated from each other by gradient elution with ammonium α-hydroxyisobutyrate on a cation-exchange column. The elements are determined by the single comparator technique. This method permits a practical application of activation analysis to the routine determination of rare earths in complex matrices, 相似文献