摘要
称取0.100 0g试样于聚四氟乙烯消解罐中,加入3mL盐酸,1mL硝酸,1mL氢氟酸,进行微波消解,消解完成后冷却,加入50g·L-1硼酸溶液10mL,继续消解3min后,将试液用水定容至100mL,采用电感耦合等离子体原子发射光谱法测定其中的钛、硅、铝、钙、镁、钒、锰、磷、镍和铬。运用基体匹配法消除了基体效应。各元素的质量浓度在一定范围内与分析谱线的强度呈线性关系,检出限(3s)在1.2~44μg·L^(-1)之间。采用本方法测定标准样品,结果与认定值相符,测定值的相对标准偏差(n=8)均小于5.0%。本方法对实际样品的测定值与湿法化学法及原子吸收光谱法测得结果一致。
0.100 0 g of sample was placed in a PTFE digestion tank,and 3 mL of hydrochloric acid,1 mL of nitric acid,1 mL of hydrofluoric acid were added for microwave digestion.After digestion,the solution was cooled,and 10 mL of 50 g·L-1 boric acid solution was added for further digestion for 3 min.Then the solution was diluted to 100 mL with water.Inductively coupled plasma atomic emission spectrometry was used to determine titanium,silicon,aluminum,calcium,magnesium,vanadium,manganese,phosphorus,nickel,and chromium.Matrix effect was elimited by using matrix matching.Linear relationships were found between the intensity of the analytical lines and the mass concentration of each element within definite ranges,with detection limits（3 s）in the range of 1.2-44μg·L^（-1）.The proposed method was applied to analysis of standard samples,giving results in consistency with the certified values and RSDs（n=8）less than 5.0%.The determination results of actual samples by the wet proposed method were in consistency with those obtained by wet chemical method and atomic absorption spectrometry.
作者
闫月娥
YAN Yue＇e(State Key Laboratory of Vanadium and Titanium Testing,Panzhihua University,Panzhihua 617000,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2018年第9期1044-1048,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词
微波消解
电感耦合等离子体原子发射光谱法
钒钛铁精矿
主次元素
microwave digestion
inductively coupled plasma atomic emission spectrometry
vanadiumtitanium-iron concentrate
major and minor element
