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The application of graphite furnace atomic absorption spectrometry to determination of ultra-trace platinum and ultra-trace palladium in rock ore |
Dong-Chao GUAN |
Guangxi Geological and Mineral Testing Research Center, Nanning 530023, China |
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Abstract This paper presents a method for the determination of ultra-trace platinum and ultra-trace palladium in rock ore by graphite furnace atomic absorption spectrometry after extraction from phenylthiourea-octanol. The conditions for extraction of platinum and palladium, the interference of co-existing ions and the optimum instrumentation conditions were studied. The liquid phase extraction was conducted after the sample was dissolved by aqua regia, and then the sample test was measured in the organic phase. The detection limit of platinum and that of palladium were 0.5×10 -9 and 0.1×10 -9. The relative standard deviations of the method were 6.0% and 4.7%, respectively, for eight samples with platinum 14.7×10 -9 and palladium15.2×10 -9 from the repeated sampling and dissolution. The relative standard deviations are 6.0% and 4.7% respectively, showing relatively good analytical quality.
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Received: 08 August 2017
Published: 24 October 2018
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元素 | 波长/nm | 狭逢/nm | 灯电流/mA | 步骤 | 起始温度/℃ | 终止温度/℃ | 时间/s | Pt | 265.9 | 0.2 | 7.5 | 1 | 80 | 120 | 10 | | | | | 2 | 120 | 120 | 10 | | | | | 3 | 120 | 1400 | 10 | | | | | 4 | 1400 | 1400 | 10 | | | | | 5 | 2900 | 2900 | 5 | | | | | 6 | 3000 | 3000 | 3 | Pd | 244.8 | 0.4 | 7.5 | 1 | 80 | 120 | 10 | | | | | 2 | 120 | 120 | 10 | | | | | 3 | 120 | 1100 | 10 | | | | | 4 | 1100 | 1100 | 10 | | | | | 5 | 2600 | 2600 | 5 | | | | | 6 | 2700 | 2700 | 3 |
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元素 | 盐酸浓度/% | 回收率/% | | 5 | 92.1 | | 10 | 93.4 | | 15 | 97.8 | | 25 | 98.7 | Pt | 35 | 97.2 | | 45 | 95.9 | | 50 | 92.1 | | 55 | 91.8 | | 60 | 91.3 | | 5 | 91.4 | | 10 | 92.6 | | 15 | 97.7 | | 25 | 99.0 | Pd | 35 | 98.1 | | 45 | 96.9 | | 50 | 93.3 | | 55 | 92.2 | | 60 | 92.5 |
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元素 | 王水浓度/% | 回收率/% | | 5 | 93.3 | | 10 | 93.7 | | 12 | 94.5 | | 15 | 98.7 | Pt | 18 | 97.6 | | 20 | 98.1 | | 22 | 93.6 | | 25 | 93.5 | | 30 | 92.8 | | 5 | 92.4 | | 10 | 93.1 | | 12 | 93.4 | | 15 | 99.2 | Pd | 18 | 96.8 | | 20 | 97.2 | | 22 | 94.4 | | 25 | 94.6 | | 30 | 93.6 |
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元素 | 萃取时间/s | 回收率/% | 元素 | 萃取时间/s | 回收率/% | Pt | 10 | 93.2 | Pd | 10 | 92.7 | | 15 | 93.6 | | 15 | 94.0 | | 20 | 94.4 | | 20 | 94.1 | | 30 | 98.6 | | 30 | 98.8 | | 60 | 99.1 | | 60 | 99.1 | | 90 | 98.4 | | 90 | 98.8 | | 180 | 99.3 | | 180 | 98.2 | | 300 | 98.5 | | 300 | 99.1 |
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元素 | | 回收率/% | 元素 | | 回收率/% | Pt | 0.1 | 93.3 | Pd | 0.1 | 92.2 | | 0.2 | 94.2 | | 0.2 | 94.4 | | 0.3 | 95.7 | | 0.3 | 94.7 | | 0.5 | 99.6 | | 0.5 | 98.7 | | 1.0 | 99.1 | | 1.0 | 99.1 | | 2.0 | 99.4 | | 2.0 | 98.8 | | 3.0 | 98.7 | | 3.0 | 99.2 | | 4.0 | 98.9 | | 4.0 | 99.1 |
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元素 | | 回收率/% | 元素 | | 回收率/% | Pt | 2 | 93.2 | Pd | 2 | 94.4 | | 5 | 94.6 | | 5 | 95.7 | | 10 | 99.1 | | 10 | 98.6 | | 15 | 99.2 | | 15 | 99.5 | | 20 | 98.5 | | 20 | 98.6 | | 25 | 99.3 | | 25 | 99.1 |
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加入的铂 含量/ng | | | 加入的钯 含量/ng | | | 50 | 50.1 | 100 | 50 | 49.9 | 99.8 | 100 | 100.0 | 100 | 100 | 99.2 | 99.2 | 500 | 495.4 | 99.1 | 500 | 490.5 | 98.1 | 1000 | 984.9 | 98.5 | 1000 | 979.2 | 97.9 | 2000 | 1954.0 | 97.7 | 2000 | 1953 | 97.6 |
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样 品 | 样品含量/ng | 加标量/ng | 测定值/ng | 回收率/% | Pt | Pd | Pt | Pd | Pt | Pd | Pt | Pd | GPt-1 | 2.6 | 2.6 | 100 | 100 | 104.7 | 105.0 | 102 | 102 | GPt-2 | 16 | 23 | 100 | 100 | 120.3 | 124.0 | 104 | 101 | GPt-4 | 580 | 600 | 100 | 100 | 679.7 | 699.2 | 100 | 99 | GPt-7 | 147 | 152 | 100 | 100 | 244.0 | 249.0 | 97 | 97 |
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样 品 | Pt含量/ng | Pd含量/ng | 本方法 | 原结果 | 本方法 | 原结果 | GPt-1 | 0.25 | 0.26 | 0.27 | 0.26 | GPt-2 | 1.5 | 1.6 | 2.1 | 2.3 | GPt-4 | 57.7 | 58 | 60.3 | 60 | GPt-7 | 15.9 | 14.7 | 16.5 | 15.2 |
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[1] |
孙丽亚, 管希云, 杜安道 . 等离子体质谱法测定地质样品中痕量铂族元素[J]. 岩矿测试, 1997,16(1):12-17.
|
[2] |
何红蓼, 吕彩芬, 周肈茹 , 等. 锍镍试金—等离子体质谱法测定地球化学勘探样品中的铂族元素和金Ⅰ[J]. 岩矿测试, 2001,20(3):19-194.
|
[3] |
何红蓼, 吕彩芬, 周肈茹 , 等. 锍镍试金—等离子体质谱法测定地球化学勘探样品中的铂族元素和金Ⅱ[J]. 岩矿测试, 2002,21(1):7-11.
|
[4] |
张洪, 陈方伦 . 铂族元素分析方法矿床地球化学及地球化学勘查[M]. 北京: 地质出版社, 1996.
|
[5] |
陈春军, 种宁 . 铅火试金富集—发射光谱法测定化探样品痕量金、铂和钯[J]. 当代化工, 2014,43(8):1657-1662.
|
[6] |
GT/B17418. 1-17417.6 地球化学样品中贵金属分析方法[S].北京: 中国标准出版社, 1998.
|
[7] |
高洪涛, 屈文俊, 杜安道 , 等. 低空白镍锍试金预富集中子活化分析测定地球化学标准物质中铂族元素[J]. 分析化学, 1999,27(5):1024-1026.
|
[8] |
杨志平 . 小试金光谱法测定地质样品中铂钯金[J]. 地质实验室, 1993,9(4):205.
|
[9] |
林玉南, 沈振兴, 胡金星 . 小试金光谱法同时测定地质样品中超痕量铂钯金[J]. 岩矿测试, 1991,10(1):247-253.
|
[10] |
孙中华 . 铅试金—光谱法同时测定地质样品中痕量铂族元素的探索[J]. 贵金属, 2004,25(3):45-48.
|
[11] |
孙红林 . 电感耦合等离子体发射光谱法测定地质样品中铂钯金. 冶金分析, 2015,35(11):8-15.
|
[12] |
李丹 . 717阴离子交换树脂富集—电感耦合等离子体质谱法测定地质样品中痕量铂钯金[J]. 冶金分析, 2011,31(14):14-19.
|
[13] |
孙爱琴 . 石墨炉原吸收光谱法测定岩矿中超痕量铂[J]. 贵金属, 2006,27(3):40-44.
|
[14] |
孙爱琴 . 树脂分离富集—石墨炉原吸收光谱法测定岩矿中超痕量钯[J]. 贵金属, 2003,24(3):36-60.
|
[15] |
李蓉 . 复硫脲的活性炭富集—发射光谱测定化探样品中金铂钯[J]. 云南冶金, 2006,35(4):58-61.
|
[16] |
刘先国 . 活性炭吸附电感耦合等离子体测定化探样品中痕量金铂钯[J]. 贵金属, 2002,23(1):33-35.
|
[17] |
赵平 . 泡沫富集发射光谱法连测化探样品中超痕量金、铂、钯[J]. Spectroscopy and Spectral Analysis, 2001,21(4):235-236.
|
[18] |
张彦斌, 程忠洲, 李华 . 硫脲树脂富集—电感耦合等离子体质谱法测定地质样品中超痕量金、银、铂、钯[J]. 分析实验室, 2006,25(7):105-108.
|
[19] |
余建民 . 贵金属萃取化学(第二版)[M]. 北京: 化学工业出版社, 2010: 42-299.
|
[20] |
蔡树型, 黄超 . 贵金属分析[M]. 北京: 冶金工业出版社, 1984: 108.
|
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