摘要
建立石墨炉原子吸收光谱法直接测定铁镍基高温合金中的锡元素。通过研究基体效应、溶样酸、基体改进剂、灰化温度、原子化温度以及不同激发光源类型,确定最佳测定方案:用2 m L盐酸和0.4 m L硝酸溶解合金样品,灰化温度为1 200℃,原子化温度为2 200℃,选用0.003 mg Pd(NO_3)_2和0.03 mg NH_4H_2PO_4作为基体改进剂。在空心阴极灯(HCL)和无极放电灯(EDL)两光源条件下,标准工作曲线的线性相关系数均大于0.999,分别对GBW 01632和GBW 01634的测定结果与认可值进行t检验(α=0.05),均无显著性差异,短期稳定性好(RSD<5.0%,n=8),锡的检出限分别为0.82μg/L(HCL)和0.75μg/L(EDL)。该方法无需萃取或其它复杂的前处理过程,测定结果准确、可靠,可实现铁镍基合金样品中锡的直接测定。
A method for the direct determination of stannum in iron-nickel-base superalloy by graphite furnace atomic absorption spectrometry was established.The optimum determination method was ensured by studing the matrix effect,dissolved sample acid,matrix modifier,ashing temperature,atomization temperature conditions and the types of different excitation light sources.Alloy samples was dissolved by using 2 mL hydrochloric acid and 0.4 mL nitric acid.Ashing temperature was 1 200℃,atomization temperature was 2 200℃,0.003 mg Pd(NO3)2 and 0.03 mg NH4H2PO4 was used as matrix modifier.The linear relative coefficient of the standard working curves were more than 0.999 under the conditions of hollow cathode lamp(HCL)and electrodeless discharge light(EDL)source.There was no significant difference between the detection results of GBW 01632,GBW 01634 and recognized value by t test(α=0.05).The short-term stability was good(RSD<5.0%,n=8),and the detection limit of tin was 0.82μg/L(HCL)and 0.75μg/L(HCL),respectively.The method is accurate and reliable without extraction or other complex pretreatment processes,and the direct determination of stannum in iron-nickel-base superalloy samples can be achieved.
作者
张亮亮
雷亚宁
ZHANG Liangliang;LEI Yaning(AVIC Metal Test Technology Company Limited,Xi’an 713801,China)
出处
《化学分析计量》
CAS
2018年第2期52-55,共4页
Chemical Analysis And Meterage
关键词
石墨炉原子吸收光谱法
铁镍基高温合金
锡
graphite furnace atomic absorption spectrometry
iron-nickel-base superalloy
stannum
