Determination of Gold in Gold Ores by Inductively Coupled Plasma-Optical Emission Spectrometry with Carbon-loaded Foam Plastic Adsorption
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摘要:
载炭泡塑吸附法对金有良好的吸附性能, 但只能用于抽滤吸附不能振荡吸附, 分析手续繁杂。本文以载炭泡塑振荡吸附-电感耦合等离子体发射光谱法测定金矿石的金量。样品在650℃高温灼烧2 h, 用50%王水和10%氯化铁加热溶解, 溶液冷却后加入5%高锰酸钾氧化, 用中密度规格的载炭泡塑两次振荡吸附溶液中的金, 然后于580℃高温灼烧后以50%王水溶解灰分, 直接用ICP-OES测定金量。方法检出限(3σ)为0.002 μg/g, 精密度(RSD, n=11) 小于3.7%。本方法对金的吸附率大于99.9%, 测定范围为0.01~90 μg/g, 对不同类型金矿石的适应性强, 解决了以往泡塑吸附法吸附率较低、标准系列与样品需同时预处理的问题, 对低含量和高含量样品均有较高的准确度。
Abstract:The method of carbon-loaded foam plastic adsorption has good adsorption properties of gold, but is only suitable for filtration adsorption with complicated analytical procedures. Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) with carbon-loaded foam plastic adsorption was used to determine the content of gold in gold ore and is described in this paper. The gold ore sample was firstly burned at 650℃ for 2 h, followed by dissolution with 50% aqua regia and 10% ferric chloride, then oxidated with 5% potassium permanganate. Gold in the solution was adsorbed twice by carbon-loaded foam plastic. The carbon-loaded foam plastic with gold was burned at 580℃ and dissolved in 50% aqua regia, after which the content of gold could be measured by ICP-OES. The detection limit is 0.002 μg/g and precision (RSD, n=11) is less than 3.7%. The method of gold adsorption rate is greater than 99.9% and the measured range is 0.01-90 μg/g. The method has a strong adaptability to different types of gold ore with higher accuracy for low content and high content of the samples than the previous method.
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表 1 不同泡塑处理方法对金的吸附率
Table 1. Adsorption rate of Au with different processing methods of foam plastic
泡塑处理方法 Au标准加入量
(μg)Au回收量
(μg)Au吸附率
(%)不处理 80 76.86 96.08 水煮1 h 80 76.67 95.84 2%氢氧化钠煮1 h 80 76.09 95.12 5%王水处理 80 78.15 97.69 酒精浸4 h 80 75.91 94.89 MIBK浸4 h 80 78.34 97.93 0.05%双硫腙酒精浸12 h 80 79.53 99.41 0.05%双硫腙MIBK浸12 h 80 79.45 99.31 MIBK-TBP浸12 h 80 75.24 94.05 TBP浸12 h 80 52.43 65.54 载炭泡塑 80 79.60 99.50 
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表 2 不同矿石类型样品的分析结果
Table 2. Analytical results of Au in different ore samples
样品编号 矿石类型 Au的含量(μg/g) 参考值 本法测定值 样品1 矽卡岩型 20.45 20.28 样品2 矽卡岩型 30.57 28.44 样品3 矽卡岩型 64.88 61.62 样品4 蚀变岩型 41.92 41.65 样品5 蚀变岩型 89.92 90.13 样品6 石英脉型 61.02 61.62 样品7 石英脉型 92.36 92.17 样品8 石英脉型 100.36 95.43 样品9 石英脉型 130.01 95.03 GBW07299 石英脉型 53 52.35
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表 3 共存元素含量及应用本法测定金的含量
Table 3. Content of coexistence elements and the analytical results of Au with this method
样品编号 元素含量(%) 元素含量(μg/g) Cu Pb Zn Mo W Ag 活性炭吸附法
测定的Au量本法测定的
Au量样品10 2.77 11.99 0.85 - - 105.87 6.47 4.81 样品11 0.31 3.2 0.18 - - 68.79 92.36 92.27 样品12 - 3.84 - 4.99 - 139.28 9.92 10.1 样品13 - 1.8 - 6.27 - 25.16 6.86 6.85 样品14 2.64 - - - - 95.28 61.02 61.62 样品15 - 5.1 3.13 - - 78.52 4.2 4.23 样品16 - 5.49 8.76 - - 77.87 13.95 13.83 样品17 - - - - 22.5 3.96 1.39 1.13 样品18 - - - - 3.6 - 20.45 20.28 样品19 0.62 - - - - - 1.21 1.28 注：“-”表示该元素对Au的检测结果未达到干扰含量，未检测。
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表 4 方法准确度和精密度
Table 4. Accuracy and precision tests of the method
标准物质
名称金量的标准值
(μg/g)金量的测定值
(μg/g)相对误差
(%)YG
(%)RSD
(%)GBW07247 0.05 0.051 2.00 11.3 3.7 GBW07248 0.1 0.103 3.00 9.81 2.6 GBW(E)070012 0.3 0.31 3.33 7.7 1.5 GBW07807 1.1 1.08 1.82 5.55 1.0 GBW07808 3.2 3.14 1.88 4.03 0.7 GBW07809 10.6 10.8 1.89 2.55 1.4 GBW07801 57.2 56.9 0.52 0.82 1.4 GBW07802 37.3 37 0.80 1.22 2.0
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