Method of Detecting Rhenium and Tungsten in Gold Jewelry
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摘要:
黄金饰品中掺杂的钨和铼, 检测时可以利用X射线荧光光谱法分辨这两种元素的特征峰。本研究通过金相显微镜对这类黄金饰品表面局部放大观察，发现多处银白色金相组织；样品经过研磨抛光后，其X射线荧光光谱中铼和钨的特征峰明显，可证实样品中含有元素铼和钨等其他杂质元素。利用ICP-OES法建立铼和钨元素的标准曲线，结果表明，铼的测试波长221.426 nm和钨的测试波长239.709 nm作为分析谱线时，回收率为95%~105%, 相对标准偏差小于2%。研究过程发现，对样品均匀取样，消解测试铼和钨及其他杂质元素的含量，最终差减后可以得到金含量。
Abstract:Tungsten and rhenium doped in gold jewelry can be distinguished by their characteristic peaks using X-ray fluorescence spectroscopy. By magnifying the surface of this kind of gold jewelry samples under a metallographic microscope, multiple silver white metallographic structures were found. Following grinding and polishing, X-ray flowrescence spectra showed obvious characteristic peaks of rhenium and tungsten, which confirmed the presence of the two elements, along with other impurity elements.Standard calibration curves for rhenium and tungsten were established using inductively coupled plasma optical emission spectrometer(ICP-OES). The results showed that the recovery rates of rhenium at the test wavelength of 221.426 nm and tungsten at the test wavelengh of 239.709 nm as the analytical spectral lines were between 95% and 105%, with the relative standard deviations below 2%. During study, it was found that after uniform sampling and digestion testing, the concentrations of rhenium, tungsten, and other impurities were determined, and the difference is subtracted to obtain the gold content.
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Keywords:
- gold jewelry /
- X-ray fluorescence spectrum /
- ICP-OES /
- rhenium /
- tungsten
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图 1 黄金样品1号和样品2号的正面(a，c)与底部(b，d)
Figure 1. Front (a, c) and bottom (b, d) view of the gold sample No.1 and sample No.2
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图 2 黄金样品研磨前(a)、后(b)在金相显微镜下的放大观察10×
Figure 2. Magnified observation under the metallographic microscope before (a) and after (b) grinding of the gold sample, 10×
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图 3 黄金样品经打磨和酸腐蚀后的X射线荧光光谱
Figure 3. X-ray fluorescence spectra of the gold samples after grinding and acid etching
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图 4 1.0、5.0、10.0 μg/mL和20 μg/mL铼的标准溶液谱图
Figure 4. Spectrograms of 1.0, 5.0, 10.0 μg/mL and 20 μg/mL rhenium standard solutions
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图 5 1.0、5.0、10.0 μg/mL和20 μg/mL钨的标准溶液谱图
Figure 5. Spectrograms of 1.0, 5.0, 10.0 μg/mL and 20 μg/mL tungsten standard solutions
表 1 样品研磨前后的X射线荧光光谱测试数据对比
Table 1 Comparison of testing data before and after sample grinding by XRF
wB/‰ 样品编号 测试点位 测试结果 研磨前 研磨后 Au Re W Ag Au Re W Ag 样品1 位置1 999.61 0 0 0.38 999.48 0 0 0.51 位置2 999.53 0 0 0.46 999.12 0.16 0.29 0.42 位置3 998.76 0.43 0.56 0.24 950.79 15.99 29.67 3.54 样品2 位置1 999.52 0 0 0.47 999.65 0 0 0.34 位置2 999.39 0 0 0.60 999.17 0.26 0.33 0.23 位置3 997.98 0.48 1.04 0.49 978.12 7.35 14.21 0.31 
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表 2 铼和钨推荐波长的相关系数、检出限及加标回收实验结果
Table 2 Correlation coefficients, detection limits, and spiked recovery experimental results of rhenium and tungsten at recommended wavelengths
推荐波长/nm 相关系数 检出限 加标浓度4.0 μg/mL 加标浓度12.0 μg/mL 加标浓度16.0 μg/mL 回收率/% RSD/% 回收率/% RSD/% 回收率/% RSD/% Re 213.904 0.999 549 0.741 300 114.5 1.99 116.9 0.66 110.1 2.61 Re 221.426 0.999 921 0.006 993 104.3 0.81 101.3 0.58 102.0 1.21 Re 227.525 0.999 923 0.011 520 106.2 0.79 100.1 0.65 97.4 2.20 W 207.911 0.999 536 0.004 152 95.2 1.04 93.8 0.31 92.3 1.19 W 220.448 0.998 667 0.029 910 115.6 1.05 119.5 0.27 110.1 1.35 W 224.875 0.997 796 0.028 770 97.8 1.13 104.8 0.42 93.5 1.31 W 239.709 0.999 227 0.005 802 99.0 1.02 96.4 0.33 95.3 1.31
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表 3 ICP-OES法测试结果
Table 3 Testing results by ICP-OES
样品编号 称样量/mg 质量分数/‰ 铼(Re) 钨(W) 银(Ag) 铑(Rh) 铜(Cu) 样品1号 100.27 110.78 210.07 0.05 2.29 0.05 100.83 120.58 191.52 0.05 1.67 0.05 样品2号 100.22 89.87 282.67 3.45 3.08 0.63 100.76 94.77 250.27 3.51 2.54 0.63
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