Determination of Nb and Ta in Nb-Ta Ore by Inductively Coupled Plasma-Optical Emission Spectrometry with a Combined Microwave Digestion Hydrofluoric Acid-resistant System
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摘要: 铌、钽在氢氟酸介质中能够形成稳定的溶液,使用耐氢氟酸进样系统的电感耦合等离子体发射光谱(ICP-OES)有利于提高分析的准确性。本文采用模块化的小罐型、多罐体组合(70罐/组)酸溶罐体的微波消解溶样模式,结合ICP-OES仪器的耐氢氟酸进样系统,建立了测定铌钽矿中铌、钽的分析方法。本方法加快了酸溶的溶样速度,溶样时间从原来的48 h减少至1 h,且在氢氟酸介质中测定,避免了高含量铌、钽在低酸度介质中容易水解的影响。方法检出限为铌5.58 μg/g,钽5.87 μg/g。本方法应用于测定铌钽精矿(19%Nb2O5,27%Ta2O5)的分析结果与碱熔方法一致,能够测定Nb2O5含量在42 μg/g~19%和Ta2O5含量在86 μg/g~27%高低品位的铌钽矿,尤其对于铌、钽在百分含量以上的铌钽矿具有优势。Abstract: Niobium and tantalum in hydrofluoric acid can form a stable solution, and thus the Nb and Ta content of Nb-Ta ore can be determined accurately by Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) with a hydrofluoric acid resistant system. The determination method described in this paper for Nb and Ta in Nb-Ta ore, uses the microwave digestion mode of modular small tank and multiple digestion tank assembly (70 tank/group), and hydrofluoric acid resistant system of ICP-OES. This method shortens the dissolution time from 48 h to 1 h. By using a hydrofluoric acid medium the hydrolysis of high-level Nb and Ta in low acid concentration media is avoided. The detection limits of this method are 5.58 μg/g for Nb and 5.87 μg/g for Ta. The result of Nb-Ta concentrate with 19% Nb2O5 and 27% Ta2O5 is consistent with that acquired by the alkali fusion method and can be used to determine both high-grade and low-grade Nb-Ta ore with 42 μg/g-19% of Nb2O5 and 86 μg/g-27% of Ta2O5. The main advantage of this method is to accurately determine Nb and Ta in high-grade Nb-Ta ore.
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表 1 铌钽矿微波分解条件
Table 1. The microwave decomposition conditions of niobium-tantalum ore
微波消解步骤 控制温度(℃) 消解时间(min) 功率(W) 1 130 15 1200 2 160 15 1200 3 190 25 1200 
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表 2 不同酸度条件下铌、钽测定结果
Table 2. Analytical results of Nb and Ta under the different acidity
GBW07185样品 5.0 mL氢氟酸+1.0 mL硝酸 2.5 mL氢氟酸+1.0 mL硝酸 1.5 mL氢氟酸+1.0 mL硝酸 Nb Ta Nb Ta Nb Ta 3次分次测定值(μg/g) 3792 3539 3701 8596 8803 8734 3733 3767 3665 8313 8518 8535 3733 3767 3665 8513 8518 8563 测定平均值(μg/g) 3677 8711 3722 8455 3722 8531 标准值(μg/g) 3635±70 8353±164 3635±70 8353±164 3635±70 8353±164 RSD(%) 3.5 1.2 1.4 1.6 1.4 0.3 相对误差(%) 1.2 4.3 2.4 1.3 2.4 2.1
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表 3 称样量的影响
Table 3. Effect of sample weight
称样量(mg) Nb2O5 Ta2O5 测定值 (μg/g) 标准值 (μg/g) 测定值 (μg/g) 标准值 (μg/g) 50.0 5310 10314 100.0 5281 5200±100 10457 10200±20 200.0 5258 10351
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表 4 精密度和准确度实验
Table 4. Precision and accuracy tests of the method
标准物质编号 Nb2O5 Ta2O5 测定值(μg/g) 标准值(μg/g) RSD(%) 相对误差(%) 测定值(μg/g) 标准值(μg/g) RSD(%) 相对误差(%) GBW07154 43.3 42.3±2.5 6.0 2.3 85.9 88.6±6.0 5.2 -3.0 GBW07155 466 430±30 6.1 8.4 684 700±60 5.2 -2.3 GBW07185 5288 5200±100 3.7 1.7 10444 10200±20 1.9 2.4
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表 5 本法和碱熔ICP-OES方法的测定结果比较
Table 5. A comparison of analytical results of Nb and Ta determined by this method and alkali fusion method
样品编号 Nb2O5含量 Ta2O5含量 本方法测定值(%) 碱熔方法测定值(%) 相对误差(%) 本方法测定值(%) 碱熔方法测定值(%) 相对误差(%) 样品1 7.6 7.82 -2.7 15.32 14.7 4.2 样品2 19.28 18.99 1.5 27.4 26.9 1.9
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