挥发分离-铬天青S增敏分光光度法测定巴氏合金中铝  

Determination of aluminum in babbit alloy by chromazurol S sensitized spectrophotometry for volatile separation

作　　者：赵如琳 黄薇 

机构地区：[1]云南锡业集团公司研究设计院,个旧661000

出　　处：《分析试验室》2015年第6期698-701,共4页Chinese Journal of Analysis Laboratory

基　　金：国家发展和改革委员会有色行业标准制订项目(2003-17A)资助

摘　　要：建立了挥发分离-铬天青S增敏分光光度法测定巴氏合金中Al的方法。锡或铅基合金试样以HCl-HNO3或HBr-H2O2溶解,在少量H2SO4存在下,用HCl-HBr挥发Sn,Sb,在1.2 mol/L HCl中形成PbCl2沉淀,残余Sn,Pb小于0.01%或5%,于微酸性溶液中用适量Na2SO2掩蔽Cu2+,Fe3+以抗坏血酸还原。在p H 6.8乙酸-乙酸铵溶液中,Al与铬天青S及聚乙二醇辛基苯基醚生成绿色络合物。对试样分解、试剂用量、络合物稳定性、分离与回收、共存元素影响、标准曲线和HBr空白等条件进行了实验优化。Al含量在0.01~0.16μg/m L范围内符合朗伯-比尔定律,相关系数为0.99968,方法检出限(3s/k)为0.49μg/L。方法用于代表样中3.6×10-4%~9.9×10-2%Al的测定,RSD(n=11)为1.7%~7.2%,回收率为96.0%~101%。The method for determination of aluminum content in babbit alloy was proposed by sensitized chromazurol S spectrophotometry for volatile separation. The test specimens of tin or lead-base alloy were first decomposed with hydrochloric acid-nitric acid or hydrobromic acid-hydrogen peroxide. In the presence of sulphurie-acid, tin and antimony were volatilized with hydrochloric acid-hydrobromic acid. Lead chloride precipitates were formalized in the 1.2 mol/L hydrochloric acid medium, remaining residual tin-lead less than 0. 01% or 5%. Sodium hyposulfite was introduced to mask copper in slightly acidic solution, an ascorbic acid was utilized as the reductant for iron （ Ⅲ ）. In the acetic acid-ammonium acetate solution （ pH 6. 8）, aluminum and chrome azurol S （CAS） formed green complex with polyethylene glycol octyl phenyl ether. The analysis conditions were optimized for sample decomposition, reagent dosage , complex stability, separation and recovery, coexisting elements influence, the standard curve, the blank for hydrobromic acid, etc. The Lambert-Beer＇s law was obeyed in the range of 0. 01 -0. 16 μg/mL for aluminum, with the correlation coefficient more than 0. 9996 and the detection limit （3s/k） as low as 0. 49 i^g/L. The proposed method was applied to the determination of representative samples containing 0. 00036% - 0. 099% aluminum, The relative standard deviation （ n = 11 ） was calculated to be 1.7% -7.2% and recoveries were in the range of 96.0% - 101%.

关 键 词：分光光度法 铬天青S 挥发 巴氏合金 铝 

分 类 号：TF03[冶金工程—冶金物理化学]