Application of SEM and EDS to Analyze the Occurrence of Platinum Group Elements and Characteristics of Platinum Group Minerals in the Pt-Pd Deposit from Huili, Sichuan Province, China
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摘要: 四川会理铂钯矿床是独立的铂族元素矿床，局部地段的铂钯含量已达工业品位，当前迫切需要详细掌握铂族矿物和铂族元素赋存状态。由于原矿铂族元素品位总体较低，采用化学分析方法分析测试只能间接研究铂族元素的赋存状态，所得结论并不全面。本文结合化学分析方法的测试结果，利用扫描电镜及能谱获得了会理铂钯矿床铂族矿物的精细特征。结果表明：该矿床中铂族元素主要是铂和钯；铑、铱、钌、锇含量很低，且未发现这四种元素的独立矿物。铂和钯有单质和与砷、碲、锑、铋形成的化合物；独立铂族矿物有17种，主要是自然铂、砷铂矿、砷钯铂矿或砷铂钯矿、钯铂铜矿或铂钯铜矿，其次可见少量承铂矿及其他铂族矿物。铂族矿物嵌布状态有两种——被包裹和粒间，被包裹占52.39%，粒间占47.62%。绝大多数铂族矿物呈他形粒状，只有少量砷铂矿晶形较好。铂族矿物粒径范围为1.36~32.7 μm，大小差异大。有的铂族矿物表面具微孔结构，有的呈葡萄状，有的可见环边现象。接触方式以曲线接触为主，直线接触次之。这些信息为该矿床矿石选冶和铂族资源评价提供了科学依据。Abstract: The Huili Pt-Pd deposit in Sichuan Province is an independent platinum element ore deposit. In some ore sections, the contents of Pt and Pd have reached industrial grade. It is necessary to understand the occurrence of platinum group elements and characteristics of platinum group minerals. However, due to the low-grade platinum group elements (PGEs) in raw ore, chemical analysis is an indirect research method for the occurrence of platinum group elements, and the conclusion is thus not complete. Scanning Electron Microscope (SEM) and Energy Dispersive Spectrometer (EDS) were used to observe the inbuilt state, particle size, morphology characteristics, and the occurrence of the platinum group minerals. Results show that the PGEs in the deposit are mainly composed of pure Pt and Pd. The contents of Rh, Ir, Ru, and Os are very low, and the independent minerals composed of these four elements are undetected. Pt and Pd can exist in the form of simple substance elements and compounds with As, Te, Sb, Bi. There were 17 kinds of platinum group minerals, including Pt, As-Pt, As-Pd-Pt/As-Pt-Pd, and Pd-Pt-Cu/Pt-Pd-Cu. The pure Pt and the remaining Pt group minerals are found locally. The platinum group minerals have two kinds of inbuilt states, wrapped (52.39%) and intergranular (47.62%). Crystals of platinum group minerals are mainly xenomorphic granular, 1.36-32.7 μm, with a large range of particle sizes. The micropore structure, grapy structure and girdle zone can be found in some mineral crystals. The contact mode is mainly curve contact, followed by linear contact. These results provide a scientific basis for the platinum group minerals in beneficiation-metallurgy and resource evaluation.
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表 1 样品中主次量元素分析
Table 1. Analytical results of major and minor elements in sample
元素 样品1测定值(×10-2) 样品2测定值(×10-2) SiO2 70.33 47.84 Al2O3 0.90 8.33 Fe2O3 9.25 10.02 MgO 2.68 9.16 CaO 6.51 6.32 Na2O 0.0031 0.093 K2O 0.032 0.52 MnO 0.023 0.085 TiO2 0.037 1.40 P2O5 0.080 0.10 S 6.82 4.52 Cr 0.0037 3.69 Ni 0.065 0.098 Co 0.0026 0.0067 Cu 1.17 0.86 Pb 0.10 0.026 Zn 0.12 0.046 注：样品1为蚀变破碎白云岩，样品2为蚀变破碎辉石岩。 
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表 2 贵金属化学分析结果
Table 2. Analytical results of precious metals in sample
样品编号 测定值(×10-9) Pt Pd Rh Ir Au 样品1 4847 1281 6.24 4.57 758 样品2 1558 439 11.5 32.6 261 注：样品1为蚀变破碎白云岩，样品2为蚀变破碎辉石岩，分析方法是锍镍试金-ICP-MS。
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表 3 样品相态分析结果
Table 3. Analytical results of phase states in sample
样品编号 元素 测定值(×10-9) 硫化物相 类质同象相 独立矿物相 总和 Pt 1049(22.10%) 734(15.47%) 2963(62.43%) 4746 Pd 219(18.00%) 114(9.37%) 884(72.64%) 1217 样品1 Rh 2.86(33.69%) 3.98(46.88%) 1.65(19.43%) 8.49 Ir 1.97(39.01%) 1.24(24.55%) 1.84(36.44%) 5.05 Au 83.2(11.65%) 383(53.63%) 248(34.72%) 714.2 Pt 147(10.20%) 70.9(4.92%) 1223(84.87%) 1441 Pd 40.5(8.72%) 196(42.20%) 228(49.09%) 464.5 样品2 Rh 3.84(32.05%) 4.52(37.73%) 3.62(30.22%) 11.98 Ir 11.1(31.28%) 7.68(21.65%) 16.7(47.07%) 35.48 Au 57.4(23.64%) 142(58.48%) 43.4(17.87%) 242.8 注：样品1为蚀变破碎白云岩，样品2为蚀变破碎辉石岩，括号内数据是各相态占总和百分含量。
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表 4 铂族矿物能谱点分析结果和矿物定名
Table 4. Analytical results of platinum group elements measured by EDS point analysis and mineral naming
序号 S Fe Ni Cu Cd Pb Bi Sb Te As Pt Pd 矿物名称 1 - 3.70 0.54 2.83 - - - 3.66 2.37 3.99 80.52 2.40 自然铂 2 - 0.77 - 2.48 - - - - - 2.01 94.74 - 自然铂 3 - - - 14.82 - - - - - 4.23 71.47 9.48 自然铂 4 - - - - - - - - - - 100.00 - 自然铂 5 - - - 2.20 - - - - - - 97.80 - 自然铂 6 - - - - - - - - - - 100.00 - 自然铂 7 - 4.69 - 9.18 - - - 1.75 - 12.29 72.09 - 自然铂 8 - - - - - - - - - - 100.00 - 自然铂 9 4.01 0.77 - 13.94 - - - - - - 69.09 7.74 自然铂 10 - - - 5.88 - - - - - - 94.12 - 自然铂 11 - 1.32 - 4.37 - - - - - - 94.30 - 自然铂 12 - 1.10 - - - - - - - - 98.90 - 自然铂 13 - 3.03 - 2.51 - - - - - 2.04 92.42 - 自然铂 14 - 3.89 - 16.47 - - - - - - 70.74 8.89 自然铂 15 1.74 3.13 2.25 11.43 - - - - - 22.35 50.29 8.80 砷铂矿 16 2.07 1.63 4.17 4.47 - - - 2.97 3.73 37.74 33.72 9.50 砷铂矿 17 4.57 4.26 7.56 3.86 - - - 3.73 3.43 38.92 31.88 1.78 砷铂矿 18 0.69 0.58 - 3.89 - - - - - 41.89 52.95 - 砷铂矿 19 1.00 - - 0.86 - - - - - 41.67 56.47 - 砷铂矿 20 1.44 0.74 - 1.14 - - - - - 41.26 55.42 - 砷铂矿 21 - 0.66 - 2.81 - - - - - 41.87 54.67 - 砷铂矿 22 1.03 - - - - - - - - 42.10 56.87 - 砷铂矿 23 - - - 3.84 - - - - - 41.81 54.36 - 砷铂矿 24 2.18 2.90 4.19 6.78 - - - 2.27 2.69 36.13 33.11 9.76 砷铂矿 25 0.75 - - 1.77 - - - - - 42.21 55.27 - 砷铂矿 26 - - - 1.26 - - - - - 41.36 57.39 - 砷铂矿 27 - 2.20 - 1.19 - - - - - 41.39 55.21 - 砷铂矿 28 - - 4.12 - - - - 3.33 3.64 41.48 41.43 6.00 砷铂矿 29 0.91 - - - - - - - - 42.41 56.68 - 砷铂矿 30 0.51 - 2.67 3.58 - - - - 1.60 36.63 19.32 35.68 砷铂钯矿 31 2.06 2.62 1.72 8.89 - - - 2.42 - 26.06 39.26 16.89 砷钯铂矿 32 2.74 - 4.86 2.61 - - - - 2.43 44.24 30.07 13.05 砷钯铂矿 33 1.51 - 2.76 9.44 - - - 1.91 - 32.68 28.24 23.45 砷钯铂矿 34 - - 1.64 6.94 - - - 3.59 3.80 26.76 41.08 16.19 砷钯铂矿 35 - 1.66 2.66 7.20 - - - - 3.00 30.39 40.04 15.04 砷钯铂矿 36 - 4.42 4.70 2.37 - - - - - 43.64 21.85 23.02 砷铂钯矿 37 1.72 1.05 0.70 2.64 - - - 11.94 - 21.55 28.45 30.97 砷铂钯矿 38 1.42 2.98 3.19 4.23 - - - 5.74 - 28.36 30.79 23.30 砷钯铂矿 39 2.11 - 1.70 23.59 - - - 1.61 - 6.81 44.31 19.86 钯铂铜矿 40 1.84 1.50 - 25.74 - - - - - 5.21 49.88 15.82 钯铂铜矿 41 - - - 28.39 - - - - - 7.34 33.36 30.91 钯铂铜矿 42 - - 1.49 28.63 - - - - 9.60 3.81 40.07 16.41 钯铂铜矿 43 0.79 12.96 - 23.38 - - - - - 3.83 31.33 25.67 钯铂铜矿 44 - 1.23 - 37.31 - - - - - - 36.99 24.48 钯铂铜矿 45 - 1.99 - 20.93 - - - - - 1.85 43.58 27.00 钯铂铜矿 46 - - - 29.69 - - - 4.84 - 9.87 12.53 43.07 铂钯铜矿 47 - 1.20 - 32.25 - 1.80 - - - - 25.70 17.61 钯铂铜矿 48 - - - 15.07 - - - - 3.88 2.38 56.75 21.92 铜钯铂矿 49 - - 1.28 0.79 - - - - 57.08 1.54 35.65 3.67 承铂矿 50 - - - - - - - - 57.81 - 37.38 4.81 承铂矿 51 - 0.90 - 1.80 - - 16.50 - 30.21 6.76 8.01 35.81 黄铋碲钯矿 52 - - 0.63 6.78 - - 7.04 - 37.82 2.52 43.06 2.15 铋碲铂矿 53 - - 1.23 1.32 - - 6.51 - 53.61 - 32.16 5.17 铋碲铂矿 54 3.69 - 2.35 12.72 - - - 5.72 14.28 10.58 45.18 5.49 砷碲铜铂矿 55 - - 2.28 2.14 - - 9.34 - 56.73 - 17.08 12.43 铋碲钯铂矿 56 - - - 1.06 - - 6.16 - 56.38 - 25.69 10.72 铋碲钯铂矿 57 - 0.82 - 4.14 - - - 27.88 - - - 67.16 锑钯矿 58 - - - 24.57 - - - 18.95 - - - 56.48 铜锑钯矿 59 - - - 1.24 - - - - 62.56 - 18.44 17.76 碲铂钯矿 60 - 30.24 - 6.62 - 4.41 - - - 2.57 51.13 5.03 铂铁矿 61 - 22.49 - 22.40 - - - - - - 39.08 16.03 铜铁钯铂矿 62 2.01 - - 22.24 - - - - - - 71.61 4.14 红石矿 63 - 1.31 - 11.08 3.96 17.19 - - - 9.31 49.66 7.50 铜铅铂矿 注：表格中数据为质量分数；“-”表示矿物不含该元素或低于能谱检出限而未被检出。
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表 5 铂族矿物特征
Table 5. Characteristics of platinum group minerals
矿物名称 化学组成 晶系 颗粒数 晶形 粒径(μm) 嵌布状态 接触方式 自然铂 Pt。成分中常含有Ir、Pd、Fe、Cu、Rh、Ni等。自然铂中这些元素含量较高时，可分别称为自然铂的成分变种 等轴晶系 14 呈他形粒状，有的晶体表面有微孔结构 2.5~24.5 被包裹(6粒)：被褐铁矿包裹(3粒)、赤铜矿包裹(1粒)、石英包裹(2粒)；粒间(8粒)：石英粒间(7粒)，与砷铂矿连生(1粒)，一起分布在石英粒间 多数曲线接触，少数直线接触 砷铂矿 PtAs2。Pt 56.58，As 43.42。混入物有Sb、Rh、Cu、Fe，有时有Sn 等轴晶系 15 多数晶形较好，少部分呈他形粒状，有的晶体表面有微孔结构 2.5~24.5 被包裹(9粒)：被褐铁矿包裹(3粒)、赤铜矿包裹(2粒)、石英包裹(2粒)、其他铜矿物包裹(2粒)；粒间(6粒)：石英粒间(2粒)、石英与自然铂粒间(1粒)、石英与黄铜矿粒间(1粒)、石英与砷铂钯矿粒间(2粒，这两粒均围绕砷铂钯矿分布) 多数直线接触，少数曲线接触 砷钯铂矿或砷铂钯矿 主要成分是As、Pd、Pt，当Pd多于Pt，称为砷铂钯矿；当Pd小于Pt，称为砷钯铂矿 - 9 呈他形粒状，有圆形、长条形，有的晶体表面有微孔结构 2.7~25.5 被包裹(4粒)：被褐铁矿包裹(1粒)、铜矿物包裹(2粒)、石英包裹(1粒)；粒间(5粒)：石英粒间(2粒)、石英与砷铂矿粒间(2粒)、石英与铜矿物粒间(1粒) 多数曲线接触，少数直线接触 钯铂铜矿或铂钯铜矿 主要成分Cu、Pd、Pt，当Pd多于Pt，称为铂钯铜矿；当Pd小于Pt，称为钯铂铜矿，属于Cu-Pd-Pt合金 - 9 呈他形粒状，可见葡萄状，有的晶体表面有微孔结构 2.7~32.7 被包裹(3粒)：被褐铁矿包裹(1粒)、石英包裹(1粒)、砷钯铂矿包裹(1粒)；粒间(6粒)：石英粒间(5粒)、石英与铜矿物粒间(1粒)。有的晶体中包裹有铜矿物 多数曲线接触，少数直线接触 铜钯铂矿 本矿物类似自然铂变种铜钯自然铂，但铜含量偏高 - 1 呈他形粒状 5.45 被石英包裹 - 承铂矿 PtTe2。组分中含钯 六方晶系 2 呈他形粒状 9.27~19.0 石英粒间 - 黄铋碲钯矿 Pd(Te，Bi)。组成中有铜、铁、铋代替碲。可含银和汞 六方晶系 1 呈他形粒状 22.0 黄铜矿与石英粒间 - 铋碲铂矿 (Pt)(Te，Bi)2。成分中Pt:Pd>4:1(原子数) 三方晶系 2 呈他形粒状 8.18~13.6 被包裹在赤铜矿中(1粒)，被石英包裹(1粒) - 砷碲铜铂矿 主要成分是As、Te、Cu、Pt - 1 呈他形粒状 3.8 石英粒间 - 铋碲钯铂矿 (Pt、Pd)(Te，Bi)2。成分中Pt:Pd为4:1~1:1(原子数) 三方晶系 2 呈他形粒状 2.7~5.45 被石英包裹 - 锑钯矿 Pd3Sb(Pd 72.44，Sb 27.56)。含少量铁和痕量Rh、Ir、Pt、Ag、Au - 1 呈他形粒状 6.06 被石英包裹 - 铜锑钯矿 主要成分是Cu、Sb、Pd - 1 呈他形粒状 8.18 被石英包裹 - 碲铂钯矿 可能是承铂矿变种 - 1 呈柱状 8.18 被石英包裹 - 铂铁矿 Fe Pt。铂可被钯替代(可达9.9%) 四方晶系 1 呈他形粒状，晶体表面有微孔结构 15.0 被石英包裹 - 铜铁钯铂矿 可能是一种Fe-Cu-Pd-Pt互化物 - 1 呈他形粒状 16.36 分布在石英和赤铜矿粒间 - 红石矿 PtCu 三方晶系 1 呈他形粒状 10.9 被石英包裹 - 铜铅铂矿 主要成分是Cu、Pb、Pt - 1 呈他形粒状 1.36 分布在石英粒间 -
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表 6 铂族矿物粒度统计结果
Table 6. The statistical results of platinum group elements size
粒径范围(μm) 颗粒数(n) 含量(%) 平均粒径(d) 颗粒数×平均粒径n·d(μm) 近似面积含量(%) -40.0+20.0 10 15.87 24.13 241.30 33.90 -20.0+10.0 21 33.33 14.31 300.51 42.22 -10.0+5.0 18 28.57 7.11 127.98 17.98 -5.0+2.5 14 22.22 3.00 42.00 5.90 合计 63 100 - 711.79 100
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表 7 铂族矿物嵌布状态统计结果
Table 7. The statistical results of platinum group elements state
类型 嵌布状态 颗粒数 含量(%) 各类含量(%) 被包裹铂族矿物 被包裹在褐铁矿中 8 12.70 52.39 被包裹在石英中 15 23.81 被包裹在铜矿物中 9 14.29 被包裹在其他铂族矿物 1 1.59 粒间铂族矿物 石英粒间 19 30.16 47.62 石英与铜矿物粒间 4 6.35 铜矿物粒间 1 1.59 石英与铂族矿物之间 6 9.52 合计 63 100 100 -
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