Determination of Uranium, Thorium and Potassium for Optically Stimulated Luminescence Dating by ICP-MS and XRF
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摘要:
光释光(OSL)测年包括等效剂量和环境剂量率的测量，准确测定铀钍钾含量是保证环境剂量率计算准确的重要环节，常用测量方法为电感耦合等离子体质谱与发射光谱法(ICP-MS/OES)联用，但铀钍钾不能同时测定，测量时间长。本文采用ICP-MS和X射线荧光光谱法(XRF)测定光释光沉积物样品中铀钍钾含量并用于环境剂量率的计算。在ICP-MS分析中，对高含量的钾采用电子稀释，减少进入检测器的钾离子，使铀钍钾离子在同一个数量级上，实现了高含量钾和低含量铀钍同时分析，方法检出限铀为6.38ng/L，钍为8.52ng/L，钾为926ng/L。研究了封闭酸溶法和敞口酸溶法对铀钍钾测定的影响，两种溶样方法处理10个沉积物和土壤标准物质，铀钍钾测定结果准确可靠，相对误差无显著差异，均在0～9.33%；但敞口酸溶法操作更简便，样品处理时间(约9h)短于封闭酸溶法(约60h)，故ICP-MS分析时选取敞口酸溶法溶解样品。采用压片XRF法测定标准物质中铀钍钾的相对误差分别为4.78%～16.2%、1.20%～13.3%和0.00%～5.67%。ICP-MS和XRF测定20个渤海湾沉积物样品，计算获得环境剂量率的相对偏差在6%以内。XRF更适合测量钾含量高的释光样品；而ICP-MS测定铀钍的检出限更低，精密度和准确度更高，对于超痕量样品，该法测量结果更为准确。
Abstract:Optically stimulated luminescence (OSL) dating includes the measurement of the equivalent dose and the environmental dose rate. The accurate determination of uranium, thorium and potassium is an important step in ensuring the accurate calculation of the environmental dose rate. The commonly used measurement method is the combination of inductively coupled plasma-mass spectrometry/optical emission spectroscopy (ICP-MS/OES), but the determination of uranium, thorium and potassium can not be done at the same time, and the measurement time is long. In the research, two methods of ICP-MS and X-ray fluorescence spectrometry (XRF) measuring the three elements were compared. Using ICP-MS analysis, electronic dilution was used to reduce the potassium ions entering the detector, so that potassium ions were in the same order of magnitude as uranium and thorium ions. Thus, the simultaneous analysis of high content potassium and low content uranium and thorium was achieved. The detection limits for uranium, thorium, and potassium were 6.38ng/L, 8.52ng/L, and 926ng/L, respectively. The effects of closed acid dissolution method and open acid dissolution method on the determination of uranium, thorium, and potassium by ICP-MS method were studied. The two dissolution methods dissolved 10 sediment and soil standard substances, and the results of uranium, thorium, and potassium determination were accurate and reliable, with no significant difference in relative error, ranging from 0 to 9.33%. However, the operation of open acid dissolution method was simpler, and the sample processing time (about 9h) was much shorter than the closed acid dissolution method (about 60h). Therefore, open acid dissolution was selected to dissolve the sample in ICP-MS method. By XRF analysis, the relative errors for the determination of uranium, thorium and potassium in standard materials by pressed-powder pellets method were 4.78%−16.2%, 1.20%−13.3% and 0.00%−5.67%, respectively. ICP-MS and XRF were used to determine 20 sediment samples from Bohai Bay, and the relative deviation of the environmental dose rate was less than 6%. XRF has advantages in the measurement of potassium and is more suitable for luminescent samples with high potassium content. The ICP-MS method has a lower detection limit, and higher precision and accuracy for the determination of uranium and thorium. For ultra trace samples, this method provides more accurate measurement results.
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表 1 电感耦合等离子体质谱仪工作参数
Table 1. Woking parameters of ICP-MS instrument
工作参数 设定值 工作参数 设定值 雾化器气体流速 0.8L/min 射频功率 1600V AMS气流速 0.3L/min 脉冲电压 900V 辅助气流速 1.2L/min 模拟电压 −1875V 等离子体气流速 15L/min 偏转电压 −10V 甄别阈值 12mV 轴向场电压 475V 
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表 2 X射线荧光光谱仪工作参数
Table 2. Woking parameters of XRF instrument
元素 分析线 晶体 准直器
(μm)探测器 工作电压
(kV)工作电流
(mA)测量时间
(s)2θ(°) 峰值 背景 U Kα LiF200 150 Scint 50 50 30 26.14 28.85 Th Kα LiF200 150 Scint 50 50 30 27.43 27.65 K Kα LiF200 150 Flow 30 120 30 136.72 2.85
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表 3 ICP-MS测定的线性参数和方法检出限
Table 3. Linearity parameters and detection limits of the method in ICP-MS instrument
测定元素 线性回归方程 相关系数 空白测定结果
(ng/mL)方法检出限
(ng/L)K y=8.448×103x+6.39×102 0.9998 0.75 0.97 0.31 0.24 0.86 0.36 926 0.69 0.18 0.44 0.94 0.28 0.14 Th y=1.936×104x+0.91×102 0.9994 0.014 0.014 0.013 0.016 0.015 0.021 8.52 0.018 0.017 0.021 0.017 0.021 0.018 U y=2.563×104x+0.85×102 0.9991 0.012 0.014 0.010 0.015 0.015 0.016 6.38 0.011 0.012 0.011 0.013 0.010 0.015
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表 4 不同溶样条件下铀、钍、钾含量的ICP-MS测定结果
Table 4. Determination results of U, Th and K by ICP-MS under different sample dissolution conditions
标准物质
编号标准值 敞口酸溶法ICP-MS测定 封闭酸溶法ICP-MS测定 U含量
(μg/g)Th含量
(μg/g)K含量
(%)U含量 Th含量 K含量 U含量 Th含量 K含量 测定值
(μg/g)相对误差
(%)测定值
(μg/g)相对误差
(%)测定值
(%)相对误差
(%)测定值
(μg/g)相对误差
(%)测定值
(μg/g)相对误差
(%)测定值
(%)相对误差
(%)GBW07310 2.10±0.20 5.00±0.30 0.10±0.01 2.00 4.76 5.15 3.00 0.10 0.00 1.97 6.19 4.70 6.00 0.10 0.00 GBW07311 9.10±0.90 23.3±1.20 2.72±0.06 8.75 3.85 22.80 2.15 2.79 2.57 9.56 5.05 24.5 5.15 2.65 2.57 GBW07312 7.80±1.0 21.4±1.7 2.41±0.05 7.65 1.92 20.70 3.27 2.35 2.49 8.03 2.95 22.0 2.80 2.45 1.66 GBW07317 0.75±0.08 5.40±0.60 3.24±0.08 0.68 9.33 5.32 1.48 3.52 3.70 0.70 6.67 5.02 7.04 3.15 2.78 GBW07358 2.20±0.20 8.30±0.90 1.91±0.02 2.12 3.64 7.96 4.10 2.01 5.23 2.38 8.18 8.78 5.78 1.89 1.05 GBW07402 1.40±0.40 16.6±1.2 2.11±0.06 1.35 3.57 16.7 0.60 2.03 3.79 1.43 2.14 18.0 8.43 2.20 4.26 GBW07403 1.30±0.40 6.00±0.70 2.52±0.06 1.20 7.69 6.50 8.33 2.52 0.00 1.20 7.69 6.55 9.17 2.65 5.15 GBW07404 6.70±1.2 27.0±2.0 0.85±0.07 6.49 3.13 26.30 2.59 0.83 2.35 7.05 5.22 25.6 5.19 0.87 2.35 GBW07405 6.50±1.1 23.0±2.0 1.24±0.05 6.21 4.46 22.06 4.09 1.21 2.42 6.48 0.31 24.5 6.52 1.29 4.03 GBW07406 6.70±1.1 23.0±2.0 1.41±0.07 7.27 8.51 24.57 6.83 1.38 2.13 6.39 4.63 21.1 8.26 1.45 2.84
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表 5 XRF测定方法的准确度
Table 5. Accuracy tests of the XRF method
标准物质
编号标准值 压片法XRF测定值 与标准值的相对误差 U含量
(μg/g)Th含量
(μg/g)K含量
(%)U含量
(μg/g)Th含量
(μg/g)K含量
(%)U
(%)Th
(%)K
(%)GBW07310 2.10±0.20 5.00±0.30 0.10±0.01 2.32 4.42 0.10 10.5 11.6 0.00 GBW07311 9.10±0.90 23.3±1.20 2.72±0.06 9.75 24.50 2.67 7.14 5.15 1.84 GBW07312 7.80±1.0 21.4±1.7 2.41±0.05 8.32 20.6 2.40 6.67 3.73 0.41 GBW07317 0.75±0.08 5.40±0.60 3.24±0.08 0.85 5.03 3.33 13.3 6.85 2.78 GBW07358 2.20±0.20 8.30±0.90 1.91±0.02 2.33 7.96 1.98 5.91 4.10 3.66 GBW07402 1.40±0.40 16.6±1.2 2.11±0.06 1.60 16.8 2.07 14.3 1.20 1.90 GBW07403 1.30±0.40 6.00±0.70 2.52±0.06 1.51 5.20 2.48 16.2 13.3 1.59 GBW07404 6.70±1.2 27.0±2.0 0.85±0.07 7.02 29.30 0.82 4.78 8.52 3.53 GBW07405 6.50±1.1 23.0±2.0 1.24±0.05 6.01 21.20 1.28 7.54 7.83 3.23 GBW07406 6.70±1.1 23.0±2.0 1.41±0.07 7.03 21.60 1.49 4.93 6.09 5.67
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表 6 ICP-MS法和XRF法分析沉积物样品结果
Table 6. The analytical results of sediment samples by ICP-MS and XRF
样品编号 ICP-MS法测定值 XRF法测定值 剂量率D值
相对偏差
(%)U含量
(μg/g)Th含量
(μg/g)K含量
(%)剂量率D1
(Gy/ka)U含量
(μg/g)Th含量
(μg/g)K含量
(%)剂量率D2
(Gy/ka)OSL01 2.30 13.15 2.30 3.78 2.01 12.11 2.25 3.56 5.97 OSL02 1.90 10.12 2.20 3.32 1.70 10.55 2.20 3.29 0.77 OSL03 1.94 9.67 2.28 3.36 2.04 10.15 2.26 3.42 1.59 OSL04 2.50 13.66 2.44 4.01 2.79 14.91 2.36 4.13 3.09 OSL05 1.72 8.95 2.03 3.02 2.00 7.35 2.07 3.01 0.46 OSL06 1.72 9.12 2.33 3.29 1.85 8.56 2.37 3.32 0.83 OSL07 1.68 9.62 2.35 3.34 1.80 9.60 2.37 3.39 1.56 OSL08 2.57 12.61 2.02 3.58 2.86 12.32 2.14 3.75 4.58 OSL09 1.77 9.44 2.22 3.24 1.96 9.10 2.19 3.24 0.13 OSL10 1.77 9.42 2.28 3.29 2.13 9.56 2.29 3.42 3.91 OSL11 1.82 10.02 1.95 3.07 1.79 9.88 2.01 3.10 0.99 OSL12 2.90 12.32 2.27 3.87 3.13 11.35 2.31 3.90 0.61 OSL13 2.72 12.46 2.14 3.72 2.35 12.38 2.21 3.66 1.64 OSL14 3.16 16.48 2.15 4.20 3.32 16.49 2.03 4.15 1.26 OSL15 3.11 14.90 2.50 4.35 2.55 13.60 2.59 4.15 4.81 OSL16 1.75 9.17 2.45 3.41 1.75 9.67 2.41 3.42 0.23 OSL17 3.30 14.73 2.24 4.17 2.55 14.53 2.33 4.00 4.17 OSL18 2.28 12.35 2.19 3.62 1.96 11.50 2.31 3.55 1.87 OSL19 2.58 15.09 2.04 3.81 2.40 16.06 2.09 3.88 1.79 OSL20 2.13 11.55 2.07 3.40 2.01 10.02 2.10 3.26 4.19
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