摘要
研究了电解法除去大量基体铅后，采用火焰原子吸收光谱法测定高纯铅中痕量钙、镁和钠。对电解酸度，电解时间及铂电极的清洗进行探究，结果表明，选用HNO3（1＋3）作为溶解电解样品的介质且电解时间为3h，铅残余量最小；与盐酸清洗铂电极相比，采用20g／L抗坏血酸一乙酸（Ф=4％）混合溶液清洗铂电极可减小铂电极的损耗。铅中其他共存元素不干扰钙、镁、钠的测定，方法检出限分别为0．061μg／mL，0．0066μg／mL，0．011μg／mL。对铅样中Ca，Mg，Na的测定，相对标准偏差为14％～19％，加标回收率为89．0％～107。5％。
The determination of trace calcium, magnesium and sodium in high-purity lead by flame atomic absorption spectrometry was proposed after the lead matrix was removed by electrolysis. The acidity and time of electrolysis and the rinse of platinum electrode were investigated. It was found that the remainder amount of lead in the solution after eletrolysis was the least when HNO3 （1 ＋3） was used as the medium of dissolution and electrolysis and eletrolysis time was set up as 3 h. Compared with hydrochloric acid, use of the mixed solution of 20 g/L ascorbic acid and 4% （V/V） acetic acid for rinsing platinum electrode which adsorbed PbO2 could decrease the loss of platinum electrode. The impurities in lead did not interfere in the determination. It was applicable for the determination of calcium, magnesium and sodium with the linear ranges of 0--4.00 μg/mL, 0--0.80 μg/mL and 0--0.80 μg/mL respectively. The detection limits were 0. 061 μg/mL for Ca,0. 006 6 μg/mL for Mg and 0. 011 μg/mL for Na. The relative standard deviation were 14 %-- 19% for nine determination of Ca, Mg and Na in a high-purity lead sample, and the recoveries were in the range of 89.0%--107.5%.
出处
《冶金分析》
EI
CAS
CSCD
北大核心
2007年第7期50-53,共4页
Metallurgical Analysis
关键词
火焰原子吸收光谱法
高纯铅
钙
镁
钠
电解法
flame atomic absorption spectrometry
high-purity lead
calcium
magnesium
sodium
electrolysis
