合金钢中痕量锡的顺序注射分光光度测定研究-分析化学专业论文.docxVIP

东北大学硕士学位论文 东北大学硕士学位论文 摘要 合金钢中痕量锡的顺序注射分光光度测定研究 摘要 本研究将顺序注射(sI)分光光度系统用于痕量锡的测定。sI系统由计算 机控制，操作简单方便，样品和试剂的混合程度和反应时间完全通过软件控制， 很大程度地减少了操作中的人为干预。 实验采用均匀设计法对试剂浓度、载流流量进行优选及用单因素法对进样 ___--_●■___。。一 顺序、试剂用量和采样量进行优化。锡与水杨基荧光酮(SAF)、十二烷基硫 酸钠(SDS)形成的三元配合物在500 nln处检测，在进样体积为250 IJL，载 流流量为O．8mL／min下，线性范围为0-4．0mg／L，检出限为0．13mg／L，对2．0mg／L sn的分析精度RSD(n-11)为1．8％，进样频率为2l样／，J、时。该法样品和试 剂的消耗量很小，对比较昂贵的SAF试剂，用量仅为400乩。SDS在本体系 中由于形成三元配合物而提高了对锡的选择性，样品中的干扰离子除Fe(III) 外，均不用掩蔽。该法用于两种类型合金钢中痕量锡的测定，获得令人满意的 -__■-●__-一 结果。 ＼／+’＼／’ 关键词顺序注射分光光度锡 it 东北大学硕士学位论文 东北大学硕士学位论文 ABSTRCT Studies on the Determination of Trace Tin in Alloyed-Steel by Sequential Injection Spectrophotometry Abstract The work was mainly concentrated on the determination of trace tin by sequential injection(SI)spectrophotometry system．SI system is controlled by computer,and it is operated simply and conveniently．Mixability of sample and reagents and reaction time is completely controlled by software，which reduces man． made mistake extensively． A homogeneous design method was found to be better select regent concentration and flow rate and a univariate approach was used for the optimization of sample loading sequence，reagent amount and sample amount．The temary complex of tin formed with SAF and SDS was monitored at 500 nnl．With 250“L sample loaded and 0．8 mL／min carrier flow rate，the liner response range was O-4．0 mg／L，and the detection limit Was 0．13 mg／L．Precision of 1．8％RSD(n=11)for determination of 2mg／L，and a throughput of 21 samples per hour were achieved． The consumption of samples and reagents Was reduced，only 400 UL for better expensive SAF reagent．SDS due to form ternary complex improved selectivity for Sn，all the interfering ions in the sample did not’need to be masked but Fe(III)．The method Was applied。to-the determination oftrace tin in two types of alloyed steel and the result Was satisfactory． Key word：sequential injection，spectrophotometry