电感耦合等离子体原子发射光谱(ICP-AES)法测定尼日利亚铌钽锂矿石中的铌、钽、锂

经过三种样品前处理实验对比,选择采取氢氟酸-高氯酸-王水溶样,酒石酸-王水浸取,电感耦合等离子体原子发射光谱(ICP-AES)法测定尼日利亚地区铌钽矿石中铌、钽、锂元素。对元素的分析谱线、酒石酸浓度等工作条件进行了优化,选择各元素的最佳分析谱线,并进行加标回收实验,探讨了各元素的加标回收率。选取Nb 269.7 nm、Ta 240.0 nm、Li 670.78 nm作为仪器分析谱线,计算得到的方法检出限分别为:Nb 0.5μg/g、Ta 1.5μg/g、Li 15.0μg/g。对比各种溶样方法,选取一种最简洁方便的样品前处理途径,经国家一级标准物质GBW07153、GBW07155和GBW07185验证,测定值的相对误差为-2.82%~1.77%,方法精密度(RSD,n=6)为0.11%~1.2%,测定尼日利亚地区铌钽锂矿石中的铌、钽、锂元素,结果无显著性差异,方法能够满足尼日利亚铌钽矿石中相关组分的准确测定。     

电感耦合等离子体原子发射光谱法测定高纯铌中微量钽

应用电感耦合等离子体原子发射光谱法,采用标准加入法对高纯铌中微量钽进行测定。当铌的质量浓度为10g·L^-1时,钽的测定范围为50-500μg·g^-1,回收率为101％～103％,相对标准偏差（n=6）为4.0％～7.3％。     

电感耦合等离子体原子发射光谱法测定铌精矿中铌、锰、钛

采用电感耦合等离子体原子发射光谱法测定铌精矿中铌、锰、钛的含量。选择铌、锰、钛的分析谱线分别为309.418,257.610,334.940nm。铌、锰、钛的线性范围在1.00~10.00mg·L-1之间,方法的检出限(3s)在0.010~0.015mg·L-1之间。方法用于标准样品B-K1的分析,测定值与认定值一致。加标回收率在94.5%~103%之间,测定值的相对标准偏差(n=11)在1.4%~2.7%之间。     

电感耦合等离子体原子发射光谱法测定稀土钢中微量镧、铈

采用稀王水溶解样品,选择La408.672 nm、Ce456.236nm为分析线,建立了电感耦合等离子体原子发射光谱法(ICP-OES)测定稀土钢中微量镧、铈的方法。结果表明,各元素校准曲线线性良好,相关系数可达0.99999;方法测定范围为：0.0001%～0.10%。检出限为：镧0.00002%,铈0.00006%。按照实验方法测定标样中镧、铈,结果的相对标准偏差RSD(n=8)为2.18%、1.68%。     

电感耦合等离子体原子发射光谱法测定钛合金中锆

建立电感耦合等离子体原子发射光谱法(ICP-AES)测定钛合金中锆元素的含量。采用盐酸-氢氟酸-硝酸溶解钛合金样品,选择357.247 nm为锆的分析谱线,通过基体匹配法消除基体钛的干扰,以电感耦合等离子体原子发射光谱法测定钛合金中锆的含量。锆的质量分数在0%~0.4%范围内与光谱强度呈良好的线性关系,相关系数大于0.999,定量下限为0.21%。测定结果的相对标准偏差小于2%(n=11),样品加标回收率为99.0%~102.7%。该方法快速、准确,能够满足实际生产中钛合金样品的测定要求。     

电感耦合等离子体原子发射光谱法(ICP-AES)测定稀土镁合金中锆

以硝酸和硫酸溶解样品,通过选择元素间无干扰的光谱线343.823nm作为Zr的分析线,采用镁基体匹配,用电感耦合等离子体原子发射光谱法(ICP-AES)测定了稀土镁合金中锆,检出限为0.002μg/mL,方法用于稀土镁合金中锆的测定,加标回收率为103.5%,11次平行测定的相对标准偏差为0.8%。     

电感耦合等离子体原子发射光谱(ICP-AES)法测定锂云母中的锂、钽、铌等7种元素

采用HNO_3-HF-HClO_4的酸体系将实验样品置于聚四氟乙烯坩埚中进行消解,用稀硝酸定容。用电感耦合等离子体原子发射光谱(ICP-AES)法测定锂云母中的锂、钽、铌等7种常见元素。通过对国家标准物质GBW07154、GBW07152的验证,测定值均在标准值的误差范围内,检出限为0.001 8～0.11μg/g,样品测定的相对标准偏差(RSD,n=6)在0.95%～3.5%,加标回收率在95.0%～108%。方法快速、准确,试剂用量少,适合大批量锂云母矿样品中Li、Ta、Nb等元素的分析测定。     

电感耦合等离子原子发射光谱法测定硅铁中五元素

报道了硅铁中锰、钙、铝、铬及铜五元素的电感耦合等离子原子发射光谱法(ICP-AES)同时测定方法.对仪器的工作条件和各元素分析谱线的选择进行了试验和优化.通过对多个硅铁标准样品的分析,证实了方法的可行性,所得测定结果与标准值一致.回收率试验所得结果在99.0%～105.0%之间.     

电感耦合等离子体原子发射光谱法测定钛合金中钯、钇、硼、铌、钽的含量北大核心CSCD

样品0.1000 g用硫酸(1+1)溶液10 mL低温加热溶解,加热至冒硫酸烟,在高温下滴加硝酸至紫色消失,并用水定容至100 mL。此溶液供电感耦合等离子体原子发射光谱法测定钛合金中钯、钇、硼、铌、钽的含量,选择的分析谱线分别为Pd 360.955 nm、Y 360.073 nm、B249.773 nm、Nb 269.706 nm、Ta 240.063 nm。以基体匹配法补偿基体效应制作工作曲线。5种元素的检出限(3s)依次为8.1,2.7,1.8,4.8,2.1μg·L^(-1)之间。测定值的相对标准偏差(n=8)在1.1%~2.9%之间。按上述方法分析英国标准物质(BS C101XTi60),测定值与认定值一致。     

电感耦合等离子体光谱法测定锂辉石选矿产品中铌和钽

用碘化铵灼烧,氢氟酸-硫酸分解矿样,不经分离,电感耦合等离子体光谱法测定锂辉石选矿产品中铌和钽(以其五氧化物表示)。Nb2O5的检出限为8.4×10-9g,Ta2O5的检出限为1.1×10-8g。相对标准偏差:铌为0.8%,钽为1.2%,测定范围为5×10-4%~20.00%。     

Preconcentration of Zr, Hf, Nb, Ta and W in seawater using solid-phase extraction on TSK-8-hydroxyquinoline resin and determination by inductively coupled plasma-mass spectrometry

Here, we present the first simultaneous preconcentration and determination of ultratrace (pmol kg⁻¹ level) Zr, Hf, Nb, Ta and W in seawater, both in the form of dissolved and acid-dissolvable species. 8-Hydroxyquinoline (8HQ) bonded covalently to a vinyl polymer resin, TSK-8HQ, was used in a chelating adsorbent column to concentrate the metals. The greatest advantage of this resin is its endurance to 5 M HF, since this is an effective eluent for all five metals. The analytes were successfully concentrated from 250 mL seawater with a 50-fold concentration factor through the column extraction and evaporation. The detection limit was 0.009-0.15 pmol kg⁻¹. The procedure blank determined using ultra pure water as a sample was 0.005-0.37 pmol kg⁻¹. The five metals were quantitatively recovered from seawater with good precision (2-4%). The effect of sample pH, sample flow rate, eluent composition and sample pretreatment were carefully studied. This method was applied to seawater.     

ICP-AES法测定镍铜合金中的Fe,Mn,Cr,Nb

建立了ICP–AES法测定镍铜合金中Fe,Mn,Cr,Nb元素的分析方法。进行了基体元素Ni,Cu及共存元素对分析元素的光谱干扰研究,分别选择259.940,257.610,283.563,316.340 nm作为分析谱线,确定内标用量为2.00 mL。测定结果的相对标准偏差为0.48%～4.71%(n=8),加标回收率为95.0%～103.4%。该法满足分析要求。     

Determination of Nb and Ta in Nb/Ta minerals by inductively coupled plasmas optical emission spectrometry using slurry sample introduction

The determination of Nb and Ta in Nb–Ta minerals was accomplished by slurry nebulization inductively coupled plasma optical emission spectrometry (ICP-OES), using a clog-free V-groove ceramic nebulizer. Samples were first wet-ground to appropriate particle sizes with narrow size distribution and 90% of the particles in the slurry were smaller than 2.32 μm in diameter. Subsamples were then dispersed in pH 9 aqueous solutions, and agitated in an ultrasonic bath for 15 min prior to analysis. Due to the lack of slurry standards matching well with the samples, calibration was simply carried out using aqueous solution standards. Results were compared with those obtained from a conventional fusion decomposition procedure and acid digestion procedures and a good agreement between the measured and referred values was obtained. The technique provided a good alternative for the rapid determination of Nb and/or Ta in their corresponding minerals.     

ICP-AES法测定钛合金中的铝、钒、钼、铁、锆

用ICP-AES法测定钛合金中的铝、钒、钼、铁、锆,研究了高频功率、雾化压力、辅助气流量、泵速对待测元素发射谱线强度的影响,优化的测定条件为：高频功率1150W,雾化压力165．7kPa,辅助气流量0．5L／min,泵速100r／rain。该法测定结果的相对标准偏差不大于1．2％,待测元素的回收率为98．0％～101．1％。     

电感耦合等离子体发射光谱(ICP-OES)法快速测定华阳川铀多金属矿中铌和铅

采用氢氟酸-硝酸-高氯酸体系对华阳川铀多金属矿进行高温消解,并对消解条件进行优化,建立了电感耦合等离子体发射光谱(ICP-OES)法对华阳川铀多金属矿中铌和铅元素进行测定的方法。结果表明,方法线性相关系数分别为0.9998和0.9999,两种元素在标准样品中的加标回收率为96.0%~104%,平行样的相对标准偏差为0.50%~3.3%。实际样品加标回收率为96.1%~102%。方法快速、准确。     

电感耦合等离子体原子发射光谱法测定铬矿石中硅、铝、镁、铁

采用过氧化钠和氢氧化钠高温熔融铬矿石样品,以盐酸溶解熔块,合并溶液后用电感耦合等离子体原子发射光谱法测定样品中硅、铝、镁和铁的含量。选择212.412,308.215,285.213,238.204 nm分别作为硅、铝、镁、铁的分析谱线。用铬矿石标准样品配制标准溶液,对标准溶液的贮存方法进行了研究,对影响标准曲线稳定性的因素进行了讨论。SiO2、Fe2O3、Al2O3和MgO的线性范围依次为0.61%～14.64%,13.62%～27.74%,9.29%～15.17%和9.87%～21.49%。采用该法对铬矿石样品进行30d的连续测定,SiO2、Fe2O3、Al2O3和MgO测定值的相对标准偏差分别在0.51%～1.3%,0.45%～2.0%,0.50%～2.5%和1.4%～2.3%之间。     

Electronic Structure Research on Lattice Stability of V,Nb, and Ta by Density Functional Theory

The difference of energy and electronic structure of V, Nb, and Ta in different crystalline structures were investigated by different methods in density functional theory (DFT). Latticeconstants, total energies, and densities of states of these metals were calculated using the plane-wave pseudopotential method in DFT. Results were compared with those of projector augmented wave method, CALPHAD method, and experiments. Total energy and electronic structure analyses showed that valence electrons mostly transferred from s to p or d state, changing obviously with both the crystal structure and the elemental period number from V to Ta and leading to stronger cohesion, higher cohesive energy and more stable lattice of heavier metals.     

电感耦合等离子体原子发射光谱法测定硫化物矿石中的硫

采用高氯酸-硝酸-氢氟酸-王水处理样品,电感耦合等离子体原子发射光谱法测定硫化物矿石中的硫,筛选了样品溶液静置时间和分析谱线,测定的相对标准偏差小于1.50%,经国家一级标准物质分析验证,结果与推荐值吻合.