【摘要】 本文将样品制备成悬浮液，通过考察分散剂、悬浮液中样品质量浓度等因素对全反射X射线荧光光谱法(TXRF)分析结果的影响，建立了TXRF分析镍矿样品中Ca、Ti、Cr、Mn、Fe、Co、Ni、Cu、Zn等元素的方法，并将建立的方法在河北承德开展现场应用示范。由于Ga和Ge与所测元素Zn谱峰较近，Ga或Ge为内标元素时会影响Zn元素定量分析的准确度，实验中选择Se为内标元素。实验结果表明：超纯水作分散剂时各元素的回收率更接近100%;悬浮液中样品质量浓度增大时，元素的回收率先呈上升趋势并逐步稳定在100%随后呈明显下降趋势且严重偏离100%,为获得准确的测量结果，应控制在10～20 mg/mL;方法中各元素的检出限为0.009 0～0.068μg/g,相对标准偏差(RSD)优于15%。利用该方法测定了3个红土镍矿标准样品，TXRF分析结果与标准值或电感耦合等离子体质谱法(ICP-MS)测量结果一致性均良好，满足野外现场分析需求。在河北承德开展了镍矿样品的TXRF现场分析测试，镍矿样品的TXRF分析结果与电感耦合等离子体原子发射光谱法(ICP-AES)或ICP-MS测量结果一致性良好，大部分数据的相对误差(RE)绝对值小于20%,证明了悬浮液制样、TXRF现场分析镍矿样品的可靠性，为镍矿现场勘查工作提供技术支撑。更多还原

【Abstract】 The sample was prepared into suspension, and the effects of factors such as the dispersant and sample mass concentration in suspension on the analytical results by total reflection X-ray fluorescence spectrometry(TXRF) were investigated.The method for the determination of Ca, Ti, Cr, Mn, Fe, Co, Ni, Cu, and Zn in nickel ore samples by TXRF was established.The proposed method was applied for on-site application demonstration in Chengde, Hebei Province.The experimental results showed that the quantitative analysis accuracy of Zn would be affected when Ga or Ge was used as the internal standard element because the spectral peaks of Ga and Ge were close to those of the measured element Zn.Therefore, Se was selected as the internal standard element in experiments.The recoveries of elements were closer to 100% when ultrapure water was used as the dispersant.As the sample mass concentration in suspension increased, the recoveries of elements first showed an upward trend, then gradually stabilized at 100%,and then significantly decreased and seriously deviated from 100%.In order to obtain accurate measurement results, the sample mass concentration should be controlled in range of 10-20 mg/mL.The limits of detection were between 0.009 0 μg/g and 0.068 μg/g, and the relative standard deviations(RSD) were better than 15%.3 certified reference materials laterite nickel ore were determined according to the experimental method.The found results of TXRF analysis were consistent with the certified values and those obtained by inductively coupled plasma mass spectrometry(ICP-MS),which could meet the requirements of on-site analysis.The on-site analysis of nickel ore samples by TXRF was conducted in Chengde, Hebei Province, and the analysis results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry(ICP-AES) or ICP-MS.The absolute values of relative error for most data were less than 20%,which proved the reliability of suspension sample preparation and on-site analysis of nickel ore samples. The proposed method provided technical support for the on-site exploration of nickel ore.更多还原