微波消解-电感耦合等离子体原子发射光谱法测定采矿废石中的铅、铬、镉、铜、镍含量  

Determination of Lead,chromium,cadmium,copper,nickel in mining waste rock by Inductively Coupled Plasma Optical Emission Spectrometry with Microwave Digestio

作　　者：谢丽芳 XIE Li-fang(Chenzhou Commodity Quality Supervision and Inspection Institute,Chenzhou 423000,China)

机构地区：[1]郴州市产商品质量监督检验所,湖南郴州423000

出　　处：《世界有色金属》2024年第3期35-37,共3页World Nonferrous Metals

摘　　要：建立了用微波消解法对采矿废石进行前处理,电感耦合等离子体原子发射光谱法测定试样中铅、铬、镉、铜、镍5种元素含量的分析方法。探讨了酸的种类及用量、功率、温度、时间等微波消解条件对试样消解的影响,确定最佳消解条件为:6mL硝酸、2mL盐酸、2 mL氢氟酸、1mL双氧水,微波功率1400W,消解温度200℃,保温50min。消解后赶酸、用硝酸复溶,比较了酸度的影响,确定酸度为5%。将方法应用于采矿废石中铅、铬、镉、铜、镍含量的测定,结果表明校准曲线线性良好,各元素相关系数均大于0.9999,方法检出限为0.0006mg/kg~0.0060mg/kg,相对标准偏差为0.49%~2.21%,加标回收率为96.5%~102.8%。本方法耗酸量少、消解时间短、准确度高,适用于采矿废石中铅、铬、镉、铜、镍金属元素的定量测定。An analytical method was established to pretreat mining waste rock by microwave digestion method,and then to determine the contents of five elements in the samples:lead,chromium,cadmium,copper and nickel by inductively coupled plasma atomic emission spectrometry.The effects of acid types,dosage,power,temperature,time and other microwave digestion conditions on the digestion of the samples were discussed,and the optimal digestion conditions were determined as follows:6mL nitric acid,2mL hydrochloric acid,2mL hydrofluoric acid,1mL hydrogen peroxide,microwave power 1400W,digestion temperature 200℃,and heat preservation for 50min.After digestion,the acid was driven and reconstituted with nitric acid,and the effect of acidity was compared,and the acidity was determined to be 5%.This method was applied to the determination of lead,chromium,cadmium,copper and nickel in mining waste,the results showed that the calibration curve was linear,the correlation coefficient of each element was greater than 0.9999,the detection limit of the method was 0.0006mg/kg~0.0060mg/kg,the relative standard deviation was 0.49%~2.21%,and the recovery rate was 96.5%~102.8%.This method has low acid consumption,short digestion time and high accuracy,and is suitable for the quantitative determination of lead,chromium,cadmium,copper and nickel metal elements in mining waste rock.

关 键 词：采矿废石 微波消解 电感耦合等离子体原子发射光谱法 金属元素 

分 类 号：O657.31[理学—分析化学]