摘要
针对甲基磺酸盐电镀锡泥样品中的有机物在常温消解条件下溶解不完全,且其成分复杂,易对待测元素造成干扰的问题,采用先高温灼烧再加入盐酸、硝酸、氢氟酸和高氯酸组合溶解的前处理方法,以火焰原子吸收光谱法分别在波长766.5、589.0和213.9 nm处测定钾、钠和锌的含量。讨论了样品前处理的灼烧温度、酸介质浓度以及锡基体和共存元素对测定的影响。结果表明:在仪器工作条件下,各元素校准曲线的线性相关系数均大于0.999 5,钾、钠、锌的检出限分别为0.004 2、0.005 1和0.006 6 mg/L。按照本法测定甲基磺酸盐电镀锡泥中钾、钠、锌元素的含量,各元素检测结果的相对标准偏差(n=7)均小于3%,加标回收率在98.00%~103.50%之间。
Aiming at the incomplete dissolution of organic substances at normal temperature during the determination of the slurry formed from methanesulfonate tin electroplating process and the interference caused easily due to the complicated composition of organic substances,the sample is pretreated by ignition at high temperature and dissolved with hydrochloric acid,nitric acid,hydrofluoric acid,and perchloric acid.K,Na,and Zn are determined by flame atomic absorption spectrometry at 766.5 nm,589.0 nm,and 213.9 nm,respectively.The effects of ignition temperature,acid medium concentration,and the existence of Sn matrix and some other elements on the determination were studied.The results showed that under the working conditions of instrument,the linear correlation coefficient of calibration curve for individual element is higher than 0.9995,and the detection limit is 0.0042 mg/L for K,0.0051 mg/L for Na,and 0.0066 mg/L for Zn.According to the method,the relative standard deviations(n=7)for determination of potassium,sodium,and zinc in methanesulfonate tin electroplating slurry were all less than 3%,and the recoveries ranged from 98.00%to 103.50%.
作者
董礼男
周莉莉
赵希文
张继明
DONG Li’nan;ZHOU Lili;ZHAO Xiwen;ZHANG Jiming(Institute of Research of Iron and Steel,Jiangsu Province and Sha Steel,Zhangjiagang 215625,China)
出处
《电镀与涂饰》
CAS
北大核心
2021年第16期1309-1313,共5页
Electroplating & Finishing
关键词
电镀锡泥
甲基磺酸盐镀液
钾
钠
锌
火焰原子吸收光谱法
tin electroplating slurry
methanesulfonate electrolyte
potassium
sodium
zinc
flame atomic absorption spectrometry
