铋锑试金测定硫化铜镍矿中钌铑钯铱铂
李可及 刘淑君++邵坤??
摘 要 建立了用于预富集硫化铜镍矿中钌铑钯铱铂5种铂族元素的铋锑试金方法。1 引 言
铂族元素作为我国短缺的战略高技术矿产之一,广泛应用于汽车、珠宝、电子等领域,其95%以上的储量分布于铜镍型矿床中,多以铜镍硫化物的伴生矿床形式产出[1],因此准确测定硫化铜镍矿中铂族元素的含量对于评价矿石价值及综合利用意义重大。目前,硫化铜镍矿中铂族元素分析的前处理方法多采用锍镍试金
2 实验部分
2.1 仪器与试剂
References
1 Rao C R M, Reddi G S. Trends in analytical chemistry, 2000, 19(9): 565-586
2 Barefoot R R, van Loon J C. Talanta, 1999, 49: 1-14
3 ZHAO Zheng, QI Liang, HUANG ZhiLong, XU Cheng. Earth Science Frontiers, 2009, 16(1): 181-193
赵 正, 漆 亮, 黄智龙, 许 成. 地学前缘, 2009, 16(1): 181-193
4 ZHANG ShiLin, TU HuiMin. Journal of Geological Science Institute, Ministry of Metallurgical Industry, 1981, 2: 90-102
张石林, 屠惠民. 冶金工业部地质研究所所报, 1981, 2: 90-102
5 Kelly Z, Ojebuoboh F. JOM, 2002, 54(4): 42-45
6 LIN YuNan, HU JinXing, SHEN ZhenXing. Chinese J. Anal. Chem., 1988, 16(1): 1-4
林玉南, 胡金星, 沈振兴. 分析化学, 1988, 16(1): 1-4
7 Precious Metal Analysis Unit of Institute of Multipurpose Utilization of Mineral Resources. Chinese J. Anal. Chem., 1974, 2(2): 31-37
四川省地质局矿产综合利用研究所贵金属分析组. 分析化学, 1974, 2(2): 31-37
8 LI KeJi, ZHAO ChaoHui, FAN JianXiong. Metallurgical Analysis, 2013, 33(8): 19-23
李可及, 赵朝辉, 范建雄. 冶金分析, 2013, 33(8): 19-23
9 YUAN ZhuoBin, LV YuanQi, ZHANG YuPing, YIN Ming. Metallurgical Analysis, 2003, 23(2): 24-30
袁倬斌, 吕元琦, 张裕平, 尹 明. 冶金分析, 2003, 23(2): 24-30
10 CAI ShuXing, HUANG Chao. Analysis of Precise Metals (1). Beijing: Melellurgical Industry Press. 1984: 86
蔡树型, 黄 超. 贵金属分析(第一版), 北京: 冶金工业出版社, 1984: 86
Determination of Ruthenium, Rhodium, Palladium, Iridium
and Platinum in CopperNickel Sulfide Ores by
BismuthAntimony Fire Assay
LI KeJi*, LIU ShuJun, SHAO Kun
(Institute of Multipurpose Utilization of Mineral Resources Chinese Academy of Geological Sciences, Chengdu 610041, China)
Abstract A bismuthantimony fire assay method for the preconcentration of ruthenium, rhodium, palladium, iridium and platinum in coppernickel sulfide ores was developed. 40.0 g bismuth trioxide, 25.0 g boric acid, 10.0 g sodium carbonate and 1.00 g starch were mixed with 10.0 g sample in a 120 mL porcelain bowl, which was put in a furnace at 850 ℃. After 20 min the temperature was raised to 1000 ℃ and held for another 40 min, and then the bowl was taken out, with the slag poured, which left the bismuth button to air cooling. A twostep cupellation procedure was developed. During the first step, the bismuth button was cupellated in a magnesia cupel until its diameter reached 5 mm or so, then it was transferred to a crucible cover containing 20 g melting antimony and kept cupellating, at last a bead with a diameter of 1 mm was obtained. The bead was microwavedigested, after cooling down to room temperature, the solvent of which was transferred to a volumetric flask and diluted to 10 ml with water. Pt and Pd were analyzed by inductively coupled plasmaatomic emission spectrometry (ICPAES), while 99Ru, 103Rh, 191Ir were analyzed by inductively coupled plasmamass spectrometry (ICPMS), with 115In, 185Re as internal standard. RSD (n=12) of the analysis results of five platinum group elements (PGEs) in standard reference material GBW07196 ranged from 7.04% to 9.48%. Under the condition of 10 g sample, the detection limits (ng/g) for PGEs are 0.027 for Ru, 0.016 for Rh, 0.11 for Pd, 0.10 for Ir and 0.11 for Pt. The method was applied to the determination of PGEs in GBW07194, GBW07195, GBW07196 with satisfactory results.
Keywords Bismuthantimony fire assay; Coppernickel sulfide ore; Platinum group elements; Inductively coupled plasmaatomic emission spectrometry; Inductively coupled plasmamass spectrometry
(Received 25 December 2013; accepted 17 February 2014)
摘 要 建立了用于预富集硫化铜镍矿中钌铑钯铱铂5种铂族元素的铋锑试金方法。1 引 言
铂族元素作为我国短缺的战略高技术矿产之一,广泛应用于汽车、珠宝、电子等领域,其95%以上的储量分布于铜镍型矿床中,多以铜镍硫化物的伴生矿床形式产出[1],因此准确测定硫化铜镍矿中铂族元素的含量对于评价矿石价值及综合利用意义重大。目前,硫化铜镍矿中铂族元素分析的前处理方法多采用锍镍试金
2 实验部分
2.1 仪器与试剂
References
1 Rao C R M, Reddi G S. Trends in analytical chemistry, 2000, 19(9): 565-586
2 Barefoot R R, van Loon J C. Talanta, 1999, 49: 1-14
3 ZHAO Zheng, QI Liang, HUANG ZhiLong, XU Cheng. Earth Science Frontiers, 2009, 16(1): 181-193
赵 正, 漆 亮, 黄智龙, 许 成. 地学前缘, 2009, 16(1): 181-193
4 ZHANG ShiLin, TU HuiMin. Journal of Geological Science Institute, Ministry of Metallurgical Industry, 1981, 2: 90-102
张石林, 屠惠民. 冶金工业部地质研究所所报, 1981, 2: 90-102
5 Kelly Z, Ojebuoboh F. JOM, 2002, 54(4): 42-45
6 LIN YuNan, HU JinXing, SHEN ZhenXing. Chinese J. Anal. Chem., 1988, 16(1): 1-4
林玉南, 胡金星, 沈振兴. 分析化学, 1988, 16(1): 1-4
7 Precious Metal Analysis Unit of Institute of Multipurpose Utilization of Mineral Resources. Chinese J. Anal. Chem., 1974, 2(2): 31-37
四川省地质局矿产综合利用研究所贵金属分析组. 分析化学, 1974, 2(2): 31-37
8 LI KeJi, ZHAO ChaoHui, FAN JianXiong. Metallurgical Analysis, 2013, 33(8): 19-23
李可及, 赵朝辉, 范建雄. 冶金分析, 2013, 33(8): 19-23
9 YUAN ZhuoBin, LV YuanQi, ZHANG YuPing, YIN Ming. Metallurgical Analysis, 2003, 23(2): 24-30
袁倬斌, 吕元琦, 张裕平, 尹 明. 冶金分析, 2003, 23(2): 24-30
10 CAI ShuXing, HUANG Chao. Analysis of Precise Metals (1). Beijing: Melellurgical Industry Press. 1984: 86
蔡树型, 黄 超. 贵金属分析(第一版), 北京: 冶金工业出版社, 1984: 86
Determination of Ruthenium, Rhodium, Palladium, Iridium
and Platinum in CopperNickel Sulfide Ores by
BismuthAntimony Fire Assay
LI KeJi*, LIU ShuJun, SHAO Kun
(Institute of Multipurpose Utilization of Mineral Resources Chinese Academy of Geological Sciences, Chengdu 610041, China)
Abstract A bismuthantimony fire assay method for the preconcentration of ruthenium, rhodium, palladium, iridium and platinum in coppernickel sulfide ores was developed. 40.0 g bismuth trioxide, 25.0 g boric acid, 10.0 g sodium carbonate and 1.00 g starch were mixed with 10.0 g sample in a 120 mL porcelain bowl, which was put in a furnace at 850 ℃. After 20 min the temperature was raised to 1000 ℃ and held for another 40 min, and then the bowl was taken out, with the slag poured, which left the bismuth button to air cooling. A twostep cupellation procedure was developed. During the first step, the bismuth button was cupellated in a magnesia cupel until its diameter reached 5 mm or so, then it was transferred to a crucible cover containing 20 g melting antimony and kept cupellating, at last a bead with a diameter of 1 mm was obtained. The bead was microwavedigested, after cooling down to room temperature, the solvent of which was transferred to a volumetric flask and diluted to 10 ml with water. Pt and Pd were analyzed by inductively coupled plasmaatomic emission spectrometry (ICPAES), while 99Ru, 103Rh, 191Ir were analyzed by inductively coupled plasmamass spectrometry (ICPMS), with 115In, 185Re as internal standard. RSD (n=12) of the analysis results of five platinum group elements (PGEs) in standard reference material GBW07196 ranged from 7.04% to 9.48%. Under the condition of 10 g sample, the detection limits (ng/g) for PGEs are 0.027 for Ru, 0.016 for Rh, 0.11 for Pd, 0.10 for Ir and 0.11 for Pt. The method was applied to the determination of PGEs in GBW07194, GBW07195, GBW07196 with satisfactory results.
Keywords Bismuthantimony fire assay; Coppernickel sulfide ore; Platinum group elements; Inductively coupled plasmaatomic emission spectrometry; Inductively coupled plasmamass spectrometry
(Received 25 December 2013; accepted 17 February 2014)
摘 要 建立了用于预富集硫化铜镍矿中钌铑钯铱铂5种铂族元素的铋锑试金方法。1 引 言
铂族元素作为我国短缺的战略高技术矿产之一,广泛应用于汽车、珠宝、电子等领域,其95%以上的储量分布于铜镍型矿床中,多以铜镍硫化物的伴生矿床形式产出[1],因此准确测定硫化铜镍矿中铂族元素的含量对于评价矿石价值及综合利用意义重大。目前,硫化铜镍矿中铂族元素分析的前处理方法多采用锍镍试金
2 实验部分
2.1 仪器与试剂
References
1 Rao C R M, Reddi G S. Trends in analytical chemistry, 2000, 19(9): 565-586
2 Barefoot R R, van Loon J C. Talanta, 1999, 49: 1-14
3 ZHAO Zheng, QI Liang, HUANG ZhiLong, XU Cheng. Earth Science Frontiers, 2009, 16(1): 181-193
赵 正, 漆 亮, 黄智龙, 许 成. 地学前缘, 2009, 16(1): 181-193
4 ZHANG ShiLin, TU HuiMin. Journal of Geological Science Institute, Ministry of Metallurgical Industry, 1981, 2: 90-102
张石林, 屠惠民. 冶金工业部地质研究所所报, 1981, 2: 90-102
5 Kelly Z, Ojebuoboh F. JOM, 2002, 54(4): 42-45
6 LIN YuNan, HU JinXing, SHEN ZhenXing. Chinese J. Anal. Chem., 1988, 16(1): 1-4
林玉南, 胡金星, 沈振兴. 分析化学, 1988, 16(1): 1-4
7 Precious Metal Analysis Unit of Institute of Multipurpose Utilization of Mineral Resources. Chinese J. Anal. Chem., 1974, 2(2): 31-37
四川省地质局矿产综合利用研究所贵金属分析组. 分析化学, 1974, 2(2): 31-37
8 LI KeJi, ZHAO ChaoHui, FAN JianXiong. Metallurgical Analysis, 2013, 33(8): 19-23
李可及, 赵朝辉, 范建雄. 冶金分析, 2013, 33(8): 19-23
9 YUAN ZhuoBin, LV YuanQi, ZHANG YuPing, YIN Ming. Metallurgical Analysis, 2003, 23(2): 24-30
袁倬斌, 吕元琦, 张裕平, 尹 明. 冶金分析, 2003, 23(2): 24-30
10 CAI ShuXing, HUANG Chao. Analysis of Precise Metals (1). Beijing: Melellurgical Industry Press. 1984: 86
蔡树型, 黄 超. 贵金属分析(第一版), 北京: 冶金工业出版社, 1984: 86
Determination of Ruthenium, Rhodium, Palladium, Iridium
and Platinum in CopperNickel Sulfide Ores by
BismuthAntimony Fire Assay
LI KeJi*, LIU ShuJun, SHAO Kun
(Institute of Multipurpose Utilization of Mineral Resources Chinese Academy of Geological Sciences, Chengdu 610041, China)
Abstract A bismuthantimony fire assay method for the preconcentration of ruthenium, rhodium, palladium, iridium and platinum in coppernickel sulfide ores was developed. 40.0 g bismuth trioxide, 25.0 g boric acid, 10.0 g sodium carbonate and 1.00 g starch were mixed with 10.0 g sample in a 120 mL porcelain bowl, which was put in a furnace at 850 ℃. After 20 min the temperature was raised to 1000 ℃ and held for another 40 min, and then the bowl was taken out, with the slag poured, which left the bismuth button to air cooling. A twostep cupellation procedure was developed. During the first step, the bismuth button was cupellated in a magnesia cupel until its diameter reached 5 mm or so, then it was transferred to a crucible cover containing 20 g melting antimony and kept cupellating, at last a bead with a diameter of 1 mm was obtained. The bead was microwavedigested, after cooling down to room temperature, the solvent of which was transferred to a volumetric flask and diluted to 10 ml with water. Pt and Pd were analyzed by inductively coupled plasmaatomic emission spectrometry (ICPAES), while 99Ru, 103Rh, 191Ir were analyzed by inductively coupled plasmamass spectrometry (ICPMS), with 115In, 185Re as internal standard. RSD (n=12) of the analysis results of five platinum group elements (PGEs) in standard reference material GBW07196 ranged from 7.04% to 9.48%. Under the condition of 10 g sample, the detection limits (ng/g) for PGEs are 0.027 for Ru, 0.016 for Rh, 0.11 for Pd, 0.10 for Ir and 0.11 for Pt. The method was applied to the determination of PGEs in GBW07194, GBW07195, GBW07196 with satisfactory results.
Keywords Bismuthantimony fire assay; Coppernickel sulfide ore; Platinum group elements; Inductively coupled plasmaatomic emission spectrometry; Inductively coupled plasmamass spectrometry
(Received 25 December 2013; accepted 17 February 2014)
摘 要 建立了用于预富集硫化铜镍矿中钌铑钯铱铂5种铂族元素的铋锑试金方法。1 引 言
铂族元素作为我国短缺的战略高技术矿产之一,广泛应用于汽车、珠宝、电子等领域,其95%以上的储量分布于铜镍型矿床中,多以铜镍硫化物的伴生矿床形式产出[1],因此准确测定硫化铜镍矿中铂族元素的含量对于评价矿石价值及综合利用意义重大。目前,硫化铜镍矿中铂族元素分析的前处理方法多采用锍镍试金
2 实验部分
2.1 仪器与试剂
References
1 Rao C R M, Reddi G S. Trends in analytical chemistry, 2000, 19(9): 565-586
2 Barefoot R R, van Loon J C. Talanta, 1999, 49: 1-14
3 ZHAO Zheng, QI Liang, HUANG ZhiLong, XU Cheng. Earth Science Frontiers, 2009, 16(1): 181-193
赵 正, 漆 亮, 黄智龙, 许 成. 地学前缘, 2009, 16(1): 181-193
4 ZHANG ShiLin, TU HuiMin. Journal of Geological Science Institute, Ministry of Metallurgical Industry, 1981, 2: 90-102
张石林, 屠惠民. 冶金工业部地质研究所所报, 1981, 2: 90-102
5 Kelly Z, Ojebuoboh F. JOM, 2002, 54(4): 42-45
6 LIN YuNan, HU JinXing, SHEN ZhenXing. Chinese J. Anal. Chem., 1988, 16(1): 1-4
林玉南, 胡金星, 沈振兴. 分析化学, 1988, 16(1): 1-4
7 Precious Metal Analysis Unit of Institute of Multipurpose Utilization of Mineral Resources. Chinese J. Anal. Chem., 1974, 2(2): 31-37
四川省地质局矿产综合利用研究所贵金属分析组. 分析化学, 1974, 2(2): 31-37
8 LI KeJi, ZHAO ChaoHui, FAN JianXiong. Metallurgical Analysis, 2013, 33(8): 19-23
李可及, 赵朝辉, 范建雄. 冶金分析, 2013, 33(8): 19-23
9 YUAN ZhuoBin, LV YuanQi, ZHANG YuPing, YIN Ming. Metallurgical Analysis, 2003, 23(2): 24-30
袁倬斌, 吕元琦, 张裕平, 尹 明. 冶金分析, 2003, 23(2): 24-30
10 CAI ShuXing, HUANG Chao. Analysis of Precise Metals (1). Beijing: Melellurgical Industry Press. 1984: 86
蔡树型, 黄 超. 贵金属分析(第一版), 北京: 冶金工业出版社, 1984: 86
Determination of Ruthenium, Rhodium, Palladium, Iridium
and Platinum in CopperNickel Sulfide Ores by
BismuthAntimony Fire Assay
LI KeJi*, LIU ShuJun, SHAO Kun
(Institute of Multipurpose Utilization of Mineral Resources Chinese Academy of Geological Sciences, Chengdu 610041, China)
Abstract A bismuthantimony fire assay method for the preconcentration of ruthenium, rhodium, palladium, iridium and platinum in coppernickel sulfide ores was developed. 40.0 g bismuth trioxide, 25.0 g boric acid, 10.0 g sodium carbonate and 1.00 g starch were mixed with 10.0 g sample in a 120 mL porcelain bowl, which was put in a furnace at 850 ℃. After 20 min the temperature was raised to 1000 ℃ and held for another 40 min, and then the bowl was taken out, with the slag poured, which left the bismuth button to air cooling. A twostep cupellation procedure was developed. During the first step, the bismuth button was cupellated in a magnesia cupel until its diameter reached 5 mm or so, then it was transferred to a crucible cover containing 20 g melting antimony and kept cupellating, at last a bead with a diameter of 1 mm was obtained. The bead was microwavedigested, after cooling down to room temperature, the solvent of which was transferred to a volumetric flask and diluted to 10 ml with water. Pt and Pd were analyzed by inductively coupled plasmaatomic emission spectrometry (ICPAES), while 99Ru, 103Rh, 191Ir were analyzed by inductively coupled plasmamass spectrometry (ICPMS), with 115In, 185Re as internal standard. RSD (n=12) of the analysis results of five platinum group elements (PGEs) in standard reference material GBW07196 ranged from 7.04% to 9.48%. Under the condition of 10 g sample, the detection limits (ng/g) for PGEs are 0.027 for Ru, 0.016 for Rh, 0.11 for Pd, 0.10 for Ir and 0.11 for Pt. The method was applied to the determination of PGEs in GBW07194, GBW07195, GBW07196 with satisfactory results.
Keywords Bismuthantimony fire assay; Coppernickel sulfide ore; Platinum group elements; Inductively coupled plasmaatomic emission spectrometry; Inductively coupled plasmamass spectrometry
(Received 25 December 2013; accepted 17 February 2014)
摘 要 建立了用于预富集硫化铜镍矿中钌铑钯铱铂5种铂族元素的铋锑试金方法。1 引 言
铂族元素作为我国短缺的战略高技术矿产之一,广泛应用于汽车、珠宝、电子等领域,其95%以上的储量分布于铜镍型矿床中,多以铜镍硫化物的伴生矿床形式产出[1],因此准确测定硫化铜镍矿中铂族元素的含量对于评价矿石价值及综合利用意义重大。目前,硫化铜镍矿中铂族元素分析的前处理方法多采用锍镍试金
2 实验部分
2.1 仪器与试剂
References
1 Rao C R M, Reddi G S. Trends in analytical chemistry, 2000, 19(9): 565-586
2 Barefoot R R, van Loon J C. Talanta, 1999, 49: 1-14
3 ZHAO Zheng, QI Liang, HUANG ZhiLong, XU Cheng. Earth Science Frontiers, 2009, 16(1): 181-193
赵 正, 漆 亮, 黄智龙, 许 成. 地学前缘, 2009, 16(1): 181-193
4 ZHANG ShiLin, TU HuiMin. Journal of Geological Science Institute, Ministry of Metallurgical Industry, 1981, 2: 90-102
张石林, 屠惠民. 冶金工业部地质研究所所报, 1981, 2: 90-102
5 Kelly Z, Ojebuoboh F. JOM, 2002, 54(4): 42-45
6 LIN YuNan, HU JinXing, SHEN ZhenXing. Chinese J. Anal. Chem., 1988, 16(1): 1-4
林玉南, 胡金星, 沈振兴. 分析化学, 1988, 16(1): 1-4
7 Precious Metal Analysis Unit of Institute of Multipurpose Utilization of Mineral Resources. Chinese J. Anal. Chem., 1974, 2(2): 31-37
四川省地质局矿产综合利用研究所贵金属分析组. 分析化学, 1974, 2(2): 31-37
8 LI KeJi, ZHAO ChaoHui, FAN JianXiong. Metallurgical Analysis, 2013, 33(8): 19-23
李可及, 赵朝辉, 范建雄. 冶金分析, 2013, 33(8): 19-23
9 YUAN ZhuoBin, LV YuanQi, ZHANG YuPing, YIN Ming. Metallurgical Analysis, 2003, 23(2): 24-30
袁倬斌, 吕元琦, 张裕平, 尹 明. 冶金分析, 2003, 23(2): 24-30
10 CAI ShuXing, HUANG Chao. Analysis of Precise Metals (1). Beijing: Melellurgical Industry Press. 1984: 86
蔡树型, 黄 超. 贵金属分析(第一版), 北京: 冶金工业出版社, 1984: 86
Determination of Ruthenium, Rhodium, Palladium, Iridium
and Platinum in CopperNickel Sulfide Ores by
BismuthAntimony Fire Assay
LI KeJi*, LIU ShuJun, SHAO Kun
(Institute of Multipurpose Utilization of Mineral Resources Chinese Academy of Geological Sciences, Chengdu 610041, China)
Abstract A bismuthantimony fire assay method for the preconcentration of ruthenium, rhodium, palladium, iridium and platinum in coppernickel sulfide ores was developed. 40.0 g bismuth trioxide, 25.0 g boric acid, 10.0 g sodium carbonate and 1.00 g starch were mixed with 10.0 g sample in a 120 mL porcelain bowl, which was put in a furnace at 850 ℃. After 20 min the temperature was raised to 1000 ℃ and held for another 40 min, and then the bowl was taken out, with the slag poured, which left the bismuth button to air cooling. A twostep cupellation procedure was developed. During the first step, the bismuth button was cupellated in a magnesia cupel until its diameter reached 5 mm or so, then it was transferred to a crucible cover containing 20 g melting antimony and kept cupellating, at last a bead with a diameter of 1 mm was obtained. The bead was microwavedigested, after cooling down to room temperature, the solvent of which was transferred to a volumetric flask and diluted to 10 ml with water. Pt and Pd were analyzed by inductively coupled plasmaatomic emission spectrometry (ICPAES), while 99Ru, 103Rh, 191Ir were analyzed by inductively coupled plasmamass spectrometry (ICPMS), with 115In, 185Re as internal standard. RSD (n=12) of the analysis results of five platinum group elements (PGEs) in standard reference material GBW07196 ranged from 7.04% to 9.48%. Under the condition of 10 g sample, the detection limits (ng/g) for PGEs are 0.027 for Ru, 0.016 for Rh, 0.11 for Pd, 0.10 for Ir and 0.11 for Pt. The method was applied to the determination of PGEs in GBW07194, GBW07195, GBW07196 with satisfactory results.
Keywords Bismuthantimony fire assay; Coppernickel sulfide ore; Platinum group elements; Inductively coupled plasmaatomic emission spectrometry; Inductively coupled plasmamass spectrometry
(Received 25 December 2013; accepted 17 February 2014)
摘 要 建立了用于预富集硫化铜镍矿中钌铑钯铱铂5种铂族元素的铋锑试金方法。1 引 言
铂族元素作为我国短缺的战略高技术矿产之一,广泛应用于汽车、珠宝、电子等领域,其95%以上的储量分布于铜镍型矿床中,多以铜镍硫化物的伴生矿床形式产出[1],因此准确测定硫化铜镍矿中铂族元素的含量对于评价矿石价值及综合利用意义重大。目前,硫化铜镍矿中铂族元素分析的前处理方法多采用锍镍试金
2 实验部分
2.1 仪器与试剂
References
1 Rao C R M, Reddi G S. Trends in analytical chemistry, 2000, 19(9): 565-586
2 Barefoot R R, van Loon J C. Talanta, 1999, 49: 1-14
3 ZHAO Zheng, QI Liang, HUANG ZhiLong, XU Cheng. Earth Science Frontiers, 2009, 16(1): 181-193
赵 正, 漆 亮, 黄智龙, 许 成. 地学前缘, 2009, 16(1): 181-193
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Determination of Ruthenium, Rhodium, Palladium, Iridium
and Platinum in CopperNickel Sulfide Ores by
BismuthAntimony Fire Assay
LI KeJi*, LIU ShuJun, SHAO Kun
(Institute of Multipurpose Utilization of Mineral Resources Chinese Academy of Geological Sciences, Chengdu 610041, China)
Abstract A bismuthantimony fire assay method for the preconcentration of ruthenium, rhodium, palladium, iridium and platinum in coppernickel sulfide ores was developed. 40.0 g bismuth trioxide, 25.0 g boric acid, 10.0 g sodium carbonate and 1.00 g starch were mixed with 10.0 g sample in a 120 mL porcelain bowl, which was put in a furnace at 850 ℃. After 20 min the temperature was raised to 1000 ℃ and held for another 40 min, and then the bowl was taken out, with the slag poured, which left the bismuth button to air cooling. A twostep cupellation procedure was developed. During the first step, the bismuth button was cupellated in a magnesia cupel until its diameter reached 5 mm or so, then it was transferred to a crucible cover containing 20 g melting antimony and kept cupellating, at last a bead with a diameter of 1 mm was obtained. The bead was microwavedigested, after cooling down to room temperature, the solvent of which was transferred to a volumetric flask and diluted to 10 ml with water. Pt and Pd were analyzed by inductively coupled plasmaatomic emission spectrometry (ICPAES), while 99Ru, 103Rh, 191Ir were analyzed by inductively coupled plasmamass spectrometry (ICPMS), with 115In, 185Re as internal standard. RSD (n=12) of the analysis results of five platinum group elements (PGEs) in standard reference material GBW07196 ranged from 7.04% to 9.48%. Under the condition of 10 g sample, the detection limits (ng/g) for PGEs are 0.027 for Ru, 0.016 for Rh, 0.11 for Pd, 0.10 for Ir and 0.11 for Pt. The method was applied to the determination of PGEs in GBW07194, GBW07195, GBW07196 with satisfactory results.
Keywords Bismuthantimony fire assay; Coppernickel sulfide ore; Platinum group elements; Inductively coupled plasmaatomic emission spectrometry; Inductively coupled plasmamass spectrometry
(Received 25 December 2013; accepted 17 February 2014)