摘要
建立了微波消解-电感耦合等离子体质谱法(ICP-MS)同时测定铝土矿中锂、铬、铜、铁、钛、钾、钠、钙、镁、铅、锌等11种金属元素含量的方法。将铝土矿粉碎、研磨和干燥后,取0.1 g样品,加入3 mL硫酸、1 mL硝酸、2 mL氢氟酸和3 mL盐酸,按升温程序微波消解样品,加40 g·L^(-1)硼酸溶液10 mL,继续在120℃下消解10 min,使消解液变澄清。冷却后取出,180℃加热至近干,用1%(体积分数)硝酸溶液稀释,按照ICP-MS条件测定。通过用10 g·L^(-1)铝基体溶液配制混合标准溶液系列并加入内标元素Sc、Ge、Bi的方法来消除基体干扰,选择合适的待测元素同位素的方法来消除谱线重叠干扰。结果显示:11种元素的质量浓度均在一定范围内与其对应的响应值与内标元素响应值的比值呈线性关系,检出限(3s)为0.011-1.400 mg·kg^(-1)。对实际样品进行加标回收试验,测定值为0.13-72.21 mg·L^(-1),测定值的相对标准偏差(n=6)为0.69%-2.6%,回收率为94.0%-106%;此方法用于分析3种铝土矿成分分析标准物质GBW 07177、GBW 07179、GBW 07180,所得测定值均在认定值要求的范围内。
A method for simultaneous determination of 11 metal elements(Li,Cr,Cu,Fe,Ti,K,Na,Ca,Mg,Pb and Zn)in bauxite was established by microwave digestion-ICP-MS.After crushing,grinding and drying of bauxite sample,0.1 g of sample was taken and mixed with 3 mL of sulfuric acid,1 mL of nitric acid,2 mL of hydrofluoric acid and 3 mL of hydrochloric acid,and the mixture was digested by microwave according to the temperature program;then 10 mL of 40 g·L^(-1) boric acid solution was added and kept on digesting at 120℃for 10 min,to make the digestion solution clear.The sample solution was taken out after cooling,heated to nearly dryness at 180℃,diluted with 1%(volume fraction)nitric acid solution,and determined by ICP-MS.The matrix interference was eliminated by using the series of matrix matching mixed standard solution prepared with 10 g·L^(-1) aluminum matrix solution and adding Sc,Ge and Bi as internal standard elements,and the overlapping interference of spectral lines was eliminated by selecting the appropriate isotope.The results showed that linearity relationships between mass concentrations and the response value ratios of 11 elements to internal standard elements were kept in the definite ranges,with detection limits(3s)in the range of 0.011-1.400 mg·kg^(-1).The spiked recovery test was made on the actual samples,the determined values were found in the range of 0.13-72.21 mg·L^(-1),RSDs(n=6)of the determined values was in the range of 0.69%-2.6%,and values of recovery was in the range of 94.0%-106%.The proposed method was used to analyze 3 bauxite composition analysis reference materials,including GBW 07177,GBW 07179 and GBW 07180,giving the determined values within the range of certified values.
作者
吕善胜
陈晴林
赖宣汉
徐金龙
吴永盛
LUY Shansheng;CHEN Qinglin;LAI Xuanhan;XU Jinlong;WU Yongsheng(Zhanjiang Yanke Testing TechnologyCo.,Ltd.,Zhanjiang 524000,China;Guangdong Jingheng Engineering Testing Co.,Ltd.,Zhanjiang 524000,China;Guangdong University of Petrochemical Technology,Maoming 525000,China;Guangdong University of Technology,Guangzhou 510000,China;Zhanjiang Customs,Zhanjiang 524000,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2021年第7期654-659,共6页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
