铁矿石 金、银、铂、钯含量的测定 电感耦合等离子体质谱法 编制说明

《铁矿石金、银、铂、钯含量的测定电感耦合等离子体质谱法》国家标二、标准修订的目的、意义及国内外现行标准情况本标准的制定有利于提高我国伴生矿产资源的利用率，减少工业三废的排三、标准的适用范围及主要内容金0.010~2.00银0.010~2.00铂0.0050~2.00钯0.0050~2.00分别用硝酸和王水溶解贵金属合粒得到测定银和金、铂、钯的溶液,导入电感耦分析中除非特别说明，使用通常实验室仪器。单标线容量瓶应符合GB/TICP-MS分析铁矿石样品中多元素时的干扰主要来自氧化物、多原子离子和降低的效应，采用在线内标和碰撞/反应模式，可有效监控和校正分析信号的短流量、发射功率等仪器参数使无碰撞模式下质2.5.1三个实验方案的比较表5-1微波消解程序方案一步骤温度(℃)1323步骤温度(℃)13234步骤温度(℃)13234相关计算公式为:金银铂钯123456789差限表3.3-1混合标准溶液浓度和待测元素及内标元素测定质量数123456金05铂05钯05金0.010~2.00银0.010~2.00铂0.0050~2.00钯0.0050~2.00分析12个平行样，计算添加样品的分析物浓度的总平均值和相对标准偏差11.5610.2451.2450.53321.5020.2551.3310.56131.4810.2411.3280.52641.4610.2531.2260.57851.4910.2621.3270.55261.4780.2581.2740.54771.4390.2511.2980.53981.4870.2551.2550.56391.4310.2491.2190.5591.5170.2510.5621.4740.2471.2810.5361.4940.2611.2890.529平均值1.4850.2521.2790.549相对标准偏差%2.22.42.92.811.5230.3421.7410.81221.6210.3511.7150.75931.5240.3571.6280.74941.7110.3681.7610.77251.5860.3421.7890.74361.6240.3511.7220.81871.5870.3591.7820.78281.5820.3611.7460.77391.4890.2881.7630.7841.5680.3671.7950.7961.6670.3641.6380.7131.5290.2961.6940.734平均值1.5840.3461.7310.770相对标准偏差%3.97.33.03.9172.5961.0251.9021.953266.6540.9851.9341.948372.5950.9681.9281.816474.1561.0761.8461.948572.1250.9941.8281.826673.8720.9611.8461.848776.1561.0681.8571.912869.2541.0941.8591.937966.9851.0161.9371.65973.5980.9581.9581.98176.1581.0591.8541.99371.3210.9541.8621.922平均值72.1221.0131.8841.895相对标准偏差%4.24.82.34.8采用有证标准物质，考察所得结果与标准物质定值间的符合程度。见表//金(mg/kg)银(mg/kg)铂(mg/kg)钯(mg/kg)2.3324.912.412.31±0.124.83±12.43±0.11.68±0.117.5810.690.611.43±0.117.77±110.61±10.60±0.03具体结果见协同实验