鐵礦石 金、銀、鉑、鈀含量的測定 電感耦合等離子體質(zhì)譜法 編制說明

《鐵礦石金、銀、鉑、鈀含量的測定電感耦合等離子體質(zhì)譜法》國家標(biāo)二、標(biāo)準(zhǔn)修訂的目的、意義及國內(nèi)外現(xiàn)行標(biāo)準(zhǔn)情況本標(biāo)準(zhǔn)的制定有利于提高我國伴生礦產(chǎn)資源的利用率，減少工業(yè)三廢的排三、標(biāo)準(zhǔn)的適用范圍及主要內(nèi)容金0.010~2.00銀0.010~2.00鉑0.0050~2.00鈀0.0050~2.00分別用硝酸和王水溶解貴金屬合粒得到測定銀和金、鉑、鈀的溶液,導(dǎo)入電感耦分析中除非特別說明，使用通常實(shí)驗(yàn)室儀器。單標(biāo)線容量瓶應(yīng)符合GB/TICP-MS分析鐵礦石樣品中多元素時(shí)的干擾主要來自氧化物、多原子離子和降低的效應(yīng)，采用在線內(nèi)標(biāo)和碰撞/反應(yīng)模式，可有效監(jiān)控和校正分析信號(hào)的短流量、發(fā)射功率等儀器參數(shù)使無碰撞模式下質(zhì)2.5.1三個(gè)實(shí)驗(yàn)方案的比較表5-1微波消解程序方案一步驟溫度(℃)1323步驟溫度(℃)13234步驟溫度(℃)13234相關(guān)計(jì)算公式為:金銀鉑鈀123456789差限表3.3-1混合標(biāo)準(zhǔn)溶液濃度和待測元素及內(nèi)標(biāo)元素測定質(zhì)量數(shù)123456金05鉑05鈀05金0.010~2.00銀0.010~2.00鉑0.0050~2.00鈀0.0050~2.00分析12個(gè)平行樣，計(jì)算添加樣品的分析物濃度的總平均值和相對(duì)標(biāo)準(zhǔn)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相對(duì)標(biāo)準(zhǔn)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相對(duì)標(biāo)準(zhǔn)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相對(duì)標(biāo)準(zhǔn)偏差%4.24.82.34.8采用有證標(biāo)準(zhǔn)物質(zhì)，考察所得結(jié)果與標(biāo)準(zhǔn)物質(zhì)定值間的符合程度。見表//金(mg/kg)銀(mg/kg)鉑(mg/kg)鈀(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具體結(jié)果見協(xié)同實(shí)驗(yàn)