摘要
利用石墨消解仪斜坡升温7min至120℃,并在120℃保持20min,以10%（V/V）王水为介质,实现了电感耦合等离子体质谱法（ICP-MS）对影响海绵钯品级的18种杂质元素的测定。研究表明：通过选择20μg/L的^45Sc、^89 Y、^159 Tb作为内标及控制测定液Pd基体质量浓度为2.0mg/mL,可有效校正基体效应;铝、镍、铜、锌、钌、铑、铂、银、锡、铱、金、铅、铋以标准模式进行测定,镁、硅、铬、锰、铁以氨气反应模式进行测定可消除质谱干扰。在选定的实验条件下,各元素校准曲线线性相关系数不小于0.999 6,方法检出限为1.0～42ng/L。采用实验方法对海绵钯中杂质元素进行测定,所得结果的相对标准偏差（RSD,n=11）为0.8%～2.8%,加标回收率为90%～107%。将实验方法对海绵钯实际样品的测定结果与电感耦合等离子体原子发射光谱法（ICP-AES）进行对比,二者基本一致。
The temperature of graphite digester was increased to 120 ℃in 7min and then kept for 20 min.Thus,eighteen impurity elements in sponge palladium,which had an affect on the quality of sponge palladium,were determined by inductively coupled plasma mass spectrometry（ICP-MS）with 10%（V/V）aqua regia as medium.The results showed that the matrix effect could be effectively corrected with 20μg/L^45 Sc,^89 Y and ^159 Tb as internal standard respectively and the mass concentration of matrix Pd in determination solution as 2.0mg/mL.The elements including aluminum,nickel,copper,zinc,ruthenium,rhodium,platinum,silver,tin,iridium,gold,lead and bismuth were determined under standard mode,while magnesium,silicon,chromium,manganese and iron were determined under ammonia reaction mode to eliminate the mass spectrometry interference.Under the selected experimental conditions,the linear correlation coefficients of calibration curves of test elements were all not less than 0.999 6.The detection limit of method was 1.0-42ng/L.The proposed method was applied to the determination of impurity elements in sponge palladium.The relative standard deviations（RSD,n=11）of the results were between 0.8%and 2.8%,and the recoveries were between 90%and 107%.The results for sponge palladium actual samples obtained by the proposed method were compared with those obtained by inductively coupled plasma atomic emission spectrometry（ICP-AES）,and the consistency was good.
出处
《冶金分析》
CAS
CSCD
北大核心
2016年第7期46-50,共5页
Metallurgical Analysis
