电感耦合等离子体原子发射光谱法测定铝及铝合金中17种微量元素的含量

Determination of 17 Micro Elements in Aluminum and Aluminum Alloy by ICP-AES

在0.050 0 g样品中滴加10滴200 g·L^(-1)氢氧化钠溶液,于150℃加热15 s,待剧烈反应停止后,再加入200 g·L^(-1)氢氧化钠溶液6 mL,于200℃加热40 min。取下烧杯,加入30%(质量分数)过氧化氢溶液2 mL。继续于200℃加热20 min,以分解溶液中过量的过氧化氢。冷却,加入50%(体积分数)硝酸溶液20 mL,盐酸2 mL,于200℃加热至溶液变清亮,冷却,用水稀释至100 mL,供电感耦合等离子体原子发射光谱仪测定其中铁、铜、镁、锌、镍、铬、锆、锡、钛、锶、镓、铍、铅、镉、硅、锰、钒等17种元素含量,设置射频功率为1 300 W,观测高度为12 mm,雾化气流量为0.65 L·min^(-1)。通过优选谱线消除基体干扰中的光谱干扰,基体匹配法和同步背景校正法消除基体干扰中的物理干扰。按照上述方法处理10种标准样品,其中17种元素的质量分数均在一定范围内与其对应的谱线强度呈线性关系,检出限(3s)为0.000 3%~0.027 2%。方法分别用于实际样品以及标准样品的分析,实际样品测定值的相对标准偏差(n=11,RSD)为0.23%~3.1%,标准样品测定值的相对误差为-0.22%~5.0%,RSD(n=11)为0.17%~4.5%。

The 10 drops of 200 g·L^(-1) sodium hydroxide solution was dropped into 0.0500 g of sample,and the mixture was heated at 150℃for 15 s.After the violent reaction stoped,another 6 mL of 200 g·L^(-1) sodium hydroxide solution was added,and the mixture obtained was heated for 40 min at 200℃.After removing the breaker,2 mL of 30%(mass fraction)hydrogen peroxide solution was added for further reaction at 200℃for 20 min until the excess hydrogen peroxide was completely decomposed.After cooling,20 mL of 50%(volume fraction)nitric acid solution and 2 mL of hydrochloric acid were added into the solution,the mixture was heated at 200℃untill the solution became clear.After cooling,the solution obtained was diluted to 100 mL with water.Elements of Fe,Cu,Mg,Zn,Ni,Cr,Zr,Sn,Ti,Sr,Ga,Be,Pb,Cd,Si,Mn,V in the sample were determined by ICP-AES with radio frequency power of 1300 W,observation height of 12 mm and atomizing gas flow rate of 0.65 L·min^(-1).The spectral interference from matrix interference was eliminated by optimizing spectral lines,and the physical interference from matrix interference was eliminated by matrix matching method and synchronous background correction method.The proposed method was applied to the analysis of 10 standard samples,the mass concentrations of 17 elements in the standard sample were linearly related to their corresponding spectral line intensities in definite ranges,with detection limits(3s)in the range of 0.0003%-0.0272%.RSDs(n=11)of the determined values of the actual samples were found in the range of 0.23%-3.1%.Relative errors of the standard sample ranged from-0.22%to 5.0%,with RSDs(n=11)of the determined values in the range of 0.17%-4.5%.