采用电感耦合等离子体原子发射光谱法（ICP-AES）测定钇铁合金中铝、硅、钙、镁、锰5种非稀土杂质元素.钇铁合金试样0.200 0 g溶于盐酸（1＋1）溶液10 m L中,所得溶液于100 m L容量瓶中定容后供ICP-AES测定.为选择合适的分析线,先根据...采用电感耦合等离子体原子发射光谱法（ICP-AES）测定钇铁合金中铝、硅、钙、镁、锰5种非稀土杂质元素.钇铁合金试样0.200 0 g溶于盐酸（1＋1）溶液10 m L中,所得溶液于100 m L容量瓶中定容后供ICP-AES测定.为选择合适的分析线,先根据光谱波长表预选几条强度大,激发电位低的谱线,然后对此谱线进行轮廓扫描,从而选出一条背景平坦,信背比大,基体及共存元素干扰少或无干扰的谱线作为分析线.用基体匹配法配制标准溶液,以铁（35%）与钇（65%）配制成混合基体,配制3个标准溶液系列,所提方法适用于钇铁合金铝、硅、钙、镁、锰含量分别在0.003%-0.1%范围内的分析测定.方法的相对标准偏差（n=11）在0.74%-4.58%之间,用标准加入法对方法的回收率做试验,测得回收率在92.30%与105.00%之间.展开更多
The boron content of uranium fuel samples with boron concentrations in the range of 0.05–10 μg/g was determined using inductively coupled plasma optical emission spectrometry(ICP-OES) after the uranium was separated...The boron content of uranium fuel samples with boron concentrations in the range of 0.05–10 μg/g was determined using inductively coupled plasma optical emission spectrometry(ICP-OES) after the uranium was separated by cation exchange. The samples were dissolved in 3 M HNO_3 on a hot plate at 150℃ and evaporated to near dryness. The residues were redissolved in 0.2 M HNO-_3 and passed through a column loaded with Dowex 50WX8-400 resin. Uranium was adsorbed on the resin,while boron was easily eluted with 0.2 M HNO_3. The boron content of the effluent was determined using ICPOES. Several strategies were employed to improve the reliability of the experimentally determined boron content.The addition of mannitol and proper control of the evaporation process were shown to be effective in preventing boron loss during sample dissolution and evaporation. The memory effect was eliminated by flushing the system with 1.5% ammonia for 30 s between successive sample runs,and the matrix match method was used to eliminate the matrix effect arising from mannitol during the ICP-OES analysis. The accuracy of the results of the analysis was determined by addition recovery tests and by comparison with the results of three Chinese certified reference materials(GBW04242, GBW04243, and GBW04232). Using the method we developed, the limit of detection for boron was as low as 0.05 μg/g in uranium fuel samples, and the relative standard deviations for 0.1–0.5 g uranium samples with 0.05–2 μg/g of boron were within 9%.展开更多
文摘采用电感耦合等离子体原子发射光谱法（ICP-AES）测定钇铁合金中铝、硅、钙、镁、锰5种非稀土杂质元素.钇铁合金试样0.200 0 g溶于盐酸（1＋1）溶液10 m L中,所得溶液于100 m L容量瓶中定容后供ICP-AES测定.为选择合适的分析线,先根据光谱波长表预选几条强度大,激发电位低的谱线,然后对此谱线进行轮廓扫描,从而选出一条背景平坦,信背比大,基体及共存元素干扰少或无干扰的谱线作为分析线.用基体匹配法配制标准溶液,以铁（35%）与钇（65%）配制成混合基体,配制3个标准溶液系列,所提方法适用于钇铁合金铝、硅、钙、镁、锰含量分别在0.003%-0.1%范围内的分析测定.方法的相对标准偏差（n=11）在0.74%-4.58%之间,用标准加入法对方法的回收率做试验,测得回收率在92.30%与105.00%之间.
文摘The boron content of uranium fuel samples with boron concentrations in the range of 0.05–10 μg/g was determined using inductively coupled plasma optical emission spectrometry(ICP-OES) after the uranium was separated by cation exchange. The samples were dissolved in 3 M HNO_3 on a hot plate at 150℃ and evaporated to near dryness. The residues were redissolved in 0.2 M HNO-_3 and passed through a column loaded with Dowex 50WX8-400 resin. Uranium was adsorbed on the resin,while boron was easily eluted with 0.2 M HNO_3. The boron content of the effluent was determined using ICPOES. Several strategies were employed to improve the reliability of the experimentally determined boron content.The addition of mannitol and proper control of the evaporation process were shown to be effective in preventing boron loss during sample dissolution and evaporation. The memory effect was eliminated by flushing the system with 1.5% ammonia for 30 s between successive sample runs,and the matrix match method was used to eliminate the matrix effect arising from mannitol during the ICP-OES analysis. The accuracy of the results of the analysis was determined by addition recovery tests and by comparison with the results of three Chinese certified reference materials(GBW04242, GBW04243, and GBW04232). Using the method we developed, the limit of detection for boron was as low as 0.05 μg/g in uranium fuel samples, and the relative standard deviations for 0.1–0.5 g uranium samples with 0.05–2 μg/g of boron were within 9%.
