氢化物发生-原子荧光光谱法同时测定钼铁中的锑和锡含量
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摘要
采用硝酸溶解样品,在盐酸介质中,用硫脲-抗坏血酸作掩蔽剂,以硼氢化钾作为还原剂,采用双道原子荧光光度计同时测定锑和锡。并对还原剂浓度、酸度、预还原时间、基体及干扰元素的影响进行了试验研究。试验表明,锑和锡在0~10μg/L范围内,其校准曲线线性相关系数均大于0.999;锑和锡的检出限分别为0.052μg/L和0.23μg/L。按照试验方法测定钼铁标准样品中锑和锡,结果与认定值基本吻合,相对标准偏差(RSD,n=6)均不超过5%。与分光光度法的对照试验结果满意。
Dissolve samples with nitric acid,using thiourea and ascorbic acid in the medium of hydrochloric acid as a masking agent,potassium borohydride as a reductant,simultaneous determination of antimony and tin with a double channel atomic fluorescence photometer. The effects of reducing agent concentration,acidity,pre reduction time,matrix and interfering elements were investigated and studied. The results showed that the linear correlation coefficients of the calibration curves were greater than 0. 999 in the range of antimony and tin of 0~10 μg/L,while the detection limits of antimony and tin were 0.052 μg/L and 0.23 μg/L,respectively. Determination of antimony and tin in ferromolybdenum standard samples in accordance with the experimental method,the results are basically in agreement with the certified values. The relative standard deviation( RSD,n = 6) were less than 5%. The result of contrast experiment with spectrophotometric method is satisfactory.
Dissolve samples with nitric acid,using thiourea and ascorbic acid in the medium of hydrochloric acid as a masking agent,potassium borohydride as a reductant,simultaneous determination of antimony and tin with a double channel atomic fluorescence photometer. The effects of reducing agent concentration,acidity,pre reduction time,matrix and interfering elements were investigated and studied. The results showed that the linear correlation coefficients of the calibration curves were greater than 0. 999 in the range of antimony and tin of 0~10 μg/L,while the detection limits of antimony and tin were 0.052 μg/L and 0.23 μg/L,respectively. Determination of antimony and tin in ferromolybdenum standard samples in accordance with the experimental method,the results are basically in agreement with the certified values. The relative standard deviation( RSD,n = 6) were less than 5%. The result of contrast experiment with spectrophotometric method is satisfactory.
引文
[1]GB/T 5059.2-2014,钼铁锑含量的测定孔雀绿分光光度法[S].
[2]GB/T 3649-2008,钼铁(附录D钼铁锡含量的测定苯基荧光酮光度法)[S].
[3]成勇,肖军,宁燕平,等.ICP-AES法测定钼铁中Mo,Si,Ca,Sb,Sn[J].冶金分析,2003,23(3):28-30.
[4]黄冬根,廖世军,党志,等.ICP-MS法测定钼铁中Sb,Cu,Sn,Si,P元素的研究[J].广东有色金属学报,2005,15(4):20-23.
[5]陆军,夏扬.氢化物发生-原子荧光光谱法测定钼铁中锡量的试验[J].安徽冶金,2015(2):5-7,12.
[6]邱少花,张东雯,任娟玲.原子荧光法测定焙烧钼精矿及钼铁中的锑[J].中国钼业,2015,39(2):37-40.
[2]GB/T 3649-2008,钼铁(附录D钼铁锡含量的测定苯基荧光酮光度法)[S].
[3]成勇,肖军,宁燕平,等.ICP-AES法测定钼铁中Mo,Si,Ca,Sb,Sn[J].冶金分析,2003,23(3):28-30.
[4]黄冬根,廖世军,党志,等.ICP-MS法测定钼铁中Sb,Cu,Sn,Si,P元素的研究[J].广东有色金属学报,2005,15(4):20-23.
[5]陆军,夏扬.氢化物发生-原子荧光光谱法测定钼铁中锡量的试验[J].安徽冶金,2015(2):5-7,12.
[6]邱少花,张东雯,任娟玲.原子荧光法测定焙烧钼精矿及钼铁中的锑[J].中国钼业,2015,39(2):37-40.