Abstract：The alternating current arc (AC-Are) has many advantages, for example, depended on solid sampling technology, no need of sample decomposition by acid dissolution or alkali fusion, simple operation, green and environmental protection, good stability and direct reading of data by spectrometer. The analysis method of silver, boron and tin in geochemical sample by AC Arc-optoelectronic direct reading emission spectrometry was established. The sample was uniformly mixed using automatic mixer for spectral samples. Thirty specimens could be mixed once, thus improving the analysis efficiency. The experimental conditions were optimized: the primary excitation current of 3A was used; it increased to secondary excitation current of 15A after arcing for 3s and kept for 22s; the total time of exposure was 25s; germanium (Ge) was selected as the internal standard element; silver and long wavelength germanium formed analysis line pair, while boron and tin formed analysis line pair with shortwave germanium. The sensitivity was high. Fourteen types of national first-class geochemical standard substance including rock, soil and stream sediment with similar composition to the matrix were used as standard series to establish the quadratic equation for the fitting of calibration curve, which avoided the influence of matrix interference. The background was corrected by difference method. It was found that the curve was smooth with good correlation coefficient. During the determination of sample with high content, the measurement results with and without background correction were basically same. However, for the determination of sample with low content, the measurement results of background correction by difference method were better. The results indicated that the relative standard deviations (RSD) were all less than 10% under the optimized experimental conditions. The determination range was wide. The detection limit of silver, boron and tin was 0.016, 0.63 and 0.32μg/g, respectively. The accuracy was verified using national first-class geochemical standard substance, and the found results were consistent with the certified values. The absolute value of logarithmic difference (ΔlgC) between the average of measurement results and certified value was less than 0.05 for three elements. The proposed method could meet the accuracy requirements in multi-objective geochemical mapping.
肖细炼, 王亚夫, 陈燕波, 杨小丽, 王迪民. 交流电弧光电直读发射光谱法测定地球化学样品中银硼锡[J]. 冶金分析, 2018, 38(7): 27-32.
XIAO Xi-lian, WANG Ya-fu, CHEN Yan-bo, YANG Xiao-li, WANG Di-min. Determination of silver, boron and tin in geochemical samples by alternating current arc optoelectronic direct reading emission spectrometry. , 2018, 38(7): 27-32.
陈郑辉,王登红,盛继福,等.中国锡矿成矿规律概要[J].地质学报,2015,89(6):1026-1037.CHEN Zheng-hui,WANG Deng-hong,SHENG Ji-fu,et al.The metallogenic regularity of tin deposits in China[J].Acta Geologica Sinica,2015,89(6):1026-1037.
丁春霞,王琳,孙慧莹,等.发射光谱法测定生态地球化学调查样品中的银锡硼[J].黄金,2012,33(10):55-58.DING Chun-xia,WANG Lin,SUN Hui-ying,et al.Determination of sliver,tin and boron in ecological geochemistry samples by emission spectrometry[J].Gold,2012,33(10):55-58.
[5]
张勤,樊守忠,潘宴山,等.X射线荧光光谱法测定化探样品中主、次和痕量组分[J].理化检验:化学分册,2005,41(8):547-552.ZHANG Qin,FAN Shou-zhong,PAN Yan-shan,et al.X-ray fluorescence spectrometric determination of major,minor and trace elements in geochemical samples[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2005,41(8):547-552.
[6]
孙中华,章志仁,毛英,等.电弧蒸馏光谱法测定化探样品中痕量银锡铅硼镓[J].岩矿测试,2004,23(2):153-156.SUN Zhong-hua,ZHANG Zhi-ren,MAO Ying,et al.Determination of trace amount of silver, tin,lead,boron and gallium in geochemical exploration samples by electric arc distillation-emission spectrometry[J].Rock and Mineral Analysis,2004,23(2):153-156.
[7]
李滦宁,赵淑杰,王烨.发射光谱载体蒸馏法测定地质样品中微量硼铍锡银[J].岩矿测试,2004,23(1):30-36.LI Luan-ning,ZHAO Shu-jie,WANG Ye.Determination of trace B,Be,Sn,Ag in geological samples by AES with carrier distillation[J].Rock and Mineral Analysis,2004,23(1):30-36.
[8]
张雪梅,张勤.发射光谱法测定勘查地球化学样品中银硼锡钼铅[J].岩矿测试,2006,25(4):323-326.ZHANG Xue-mei,ZHANG Qin.Determination of silver,boron,tin,molybdenum and lead in geochemical exploration samples by emission spectrometry[J].Rock and Mineral Analysis,2006,25(4):323-326.
[9]
叶晨亮.发射光谱快速测定银锡铜铅锌钼铍[J].岩矿测试,2004,23(3):238-240.YE Chen-liang.Rapid determination of silver,tin,copper,lead,zinc,molybdenum and beryllum by emission spectrometry[J].Rock and Mineral Analysis,2004,23(3):238-240.
[10]
杨婷,王佳丽,郭爽,等.双电极发射光谱法测定水系沉积物中硼锡银[J].吉林地质,2011,30(2):111-112.YANG Ting,WANG Jia-li,GUO Shuang,et al.Determination of boron,tin,silver in stream sediments by double electrode emission spectrometry[J].Jilin Geology,2011,30(2):111-112.
[11]
刘江斌,武永芝.原子发射光谱法快速测定矿石中锡[J].冶金分析,2013,33(3):65-68.LIU Jiang-bin,WU Yong-zhi.Rapid determination of tin in ore by atomic emission spectrometry[J].Metallurgical Analysis,2013,33(3):65-68.
[12]
王辉,马晓敏,郑伟,等.直流电弧原子发射光谱法测定钛和钛合金中微量杂质元素[J].岩矿测试,2014,33(4):506-511.WANG Hui,MA Xiao-min,ZHENG Wei,et al.Determination of 10 trace impurity elements in titanium and titanium alloys with dc arc atomic emission spectrometry[J].Rock and Mineral Analysis,2014,33(4):506-511.
[13]
孙红英.直读光谱法测定高锰钢中的锰及不确定度评估[J].光谱实验室,2012,29(2):992-995.SUN Hong-ying.Determination of Mn in high manganese steel by direct reading spectrometry and its evaluation of uncertainty[J].Chinese Journal of Spectroscopy Laboratory,2012,29(2):992-995.
[14]
张勤.多目标地球化学填图中的54种指标配套分析方案和分析质量监控系统[J].第四纪研究,2005,5(3):292-297.ZHANG Qin.A complete set of analytical schemes and analytical data monitoring systems for determinations of 54 components in multi-purpose geochemical mapping[J].Quaternary Sciences,2005,5(3):292-297.
