Abstract:The determination method of fifteen components (As, Co, Cr, Cu, Fe2O3, K2O, Li, Mn, Mo, Na2O, Ni, Pb, Ti, V and Zn) in soil and stream sediment by inductively coupled plasma atomic emission spectrometry after microwave digestion was established. Several analysis lines of each element were compared and analyzed. The spectral lines with high intensity, good shape and little interference were selected as the analysis lines. The effect of acid for the dissolution of salts after microwave treatment and evaporation as well as the instrumental operation parameters of ICP-AES (such as carries gas flow and observation method) was studied. The researches indicated that the satisfactory results could be obtained under the following conditions: the sample was dissolved with mixed aqua regia and hydrofluoric acid; after solution evaporation, the salts were dissolved in 5 % (V/V) HCl; the RF power was 1 150 W; the flow rate of carrier gas was 0.6 L/min; the axial observation mode was adopted. The detection limits were between 0.06 μg/g and 49 μg/g. The proposed method was applied to the determination of certified reference materials of soil and stream sediment. The relative standard deviations (RSD) were less than 10%. The mean log errors between found results and certified values were less than 0.05, which could meet the requirements of <The specification of testing quality management for geological laboratories>.
孙晓慧,李章,刘希良. 微波消解-电感耦合等离子体原子发射光谱法测定土壤和水系沉积物中15种组分[J]. 冶金分析, 2014, 34(11): 56-60.
SUN Xiao-hui, LI Zhang, LIU Xi-liang. Determination of fifteen components in soil and stream sediment byinductively coupled plasma atomic emission spectrometry after microwave digestion. , 2014, 34(11): 56-60.
Walsh J N. The simultaneous determination of the major, minor and trace constituents of silicate rocks using inductively coupled plasma spectrometry [J]. Spectra Chimica, 1980(35B):107-111.
[5]
张保科,温宏利,王蕾,等. 封闭压力酸溶-盐酸提取-电感耦合等离子体质谱法测定地质样品中的多元素[J]. 岩矿测试(Rock and Mineral Analysis), 2011,30(6):737-744.
[6]
陈永欣,黎香荣,韦新红,等. 微波消解-电感耦合等离子体质谱法测定土壤和沉积物中痕量稀土元素[J]. 岩矿测试(Rock and Mineral Analysis), 2011,30(5):560-565.
[7]
胡德新,王昊云,王兆瑞,等.微波消解样品-电感耦合等离子体原子发射光谱法测定铅精矿中铅、砷、镉、汞[J].理化检验:化学分册(Physical Testing and Chemical Analysis: Part B Chemical Analysis), 2012,48(7):828-830.
袁秀茹,谈建安,王建波,等. ICP-AES法测定铜镍矿、铅锌矿中铜、镍、铅、锌、钴[J].分析测试技术与仪器(Analysis and Testing Technology and Instruments), 2009, 15(1): 47-50.
[13]
Christoph Moor, Theopisti Lymberopoulou, Volker J. Dietrich. Determination of heavy metals in soils, sediments and geological materials by ICP-AES and ICP-MS[J]. Mikrochimica Acta, 2001, 136 (3-4):123-128.
[14]
陈江,姚玉鑫,费勇,等.微波消解等离子体发射光谱和石墨炉原子吸收光谱法联合测定土壤中多元素[J]. 岩矿测试(Rock and Mineral Analysis), 2009, 28(1): 25-28.
[15]
吴庆梅,余海,张瑜龙,等. 微波消解-电感耦合等离子体发射光谱法测定土壤中钴的研究[J]. 安徽农业科学(Journal of Anhui Agricultural Sciences), 2012, 40(29): 159-160.