ICP-AES法测定煤矸石中的Ni、Fe、Mn、Cr

取1.000g矸石样品于聚四氟乙烯坩埚中,加入5mLH2O2放置过夜,加6mL浓HCl,4mL浓HNO3,在微波炉中消解至近干,再加2mLHF,继续消解至粘稠状,用温热稀HCl溶解残渣,转入50mL容量瓶中,加1%HNO3定容,用ICP-AES法测定煤矸中Ni、Fe、Mn、Cr。在选定的测定条件下,检出限分别为0.013mg/L、0.0044mg/L、0.0014mg/L和0.0069mg/L;精密度的相对标准偏差分别为2.9%、3.4%、3.1%、2.1%;准确度实验铬的回收率在97.5%～106.0%之间。

ICP-AES Determining Ni, Fe, Mn and Cr in Coal Gangue

Taking 1.000g coal gangue sample and put in Teflon pot, add in 5mL H2O2 and laid for the whole night. Then add in 6mL strong HCI and 4mL strong HNO3 for digestion in microwave stove. Then put in another 2mL HF and continue to digest until they become a kind of stick substance. Use distemper light HCl to dissolve leavings and transfer them into 50mL content bottle, add in 1% HNO3 for volume fixing. ICP-AES was used to determine Ni, Fe, Mn and Cr in coal gangue,under the selected conditions, the detection limit was 0.013mg/L, 0.0044mg/L, 0.0014mg/L and 0.0069mg/L, with relative standard errors of precision of 2.9%, 3.4%, 3.1% and 2.1% respectively. Recovery of Cu could be between 97.5% and 106.0%.