ICP-AES法测定湿法磷酸中铝镁铁
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摘要
建立了电感耦合等离子体—原子发射光谱法(ICP-AES)快速、准确并同时测定湿法磷酸中的铝、镁和铁,选定灵敏度较高的特征谱线作为分析线,优化仪器工作参数,无需使用磷酸配制标准工作溶液即可消除基体效应对测定结果的影响。在光谱仪处于最佳分析条件下,选定波长分别为396.156 nm、279.077 nm、238.204 nm的特征谱线作为本方法中元素铝、镁和铁的分析线。利用方法同时测定湿法磷酸中铝、镁和铁金属元素含量,检出限分别为0.0013μg/mL、0.0022μg/mL、0.0054μg/mL,铝、镁和铁测定结果的相对标准偏差(RSD)分别为1.5~6.5%、1.8~5.3%、2.5~8.0%,各项加标回收率为96.9%~106.2%、92.5%~104.0%、97.0%~105.5%。同时与标准加入法进行对比实验,分析结果基本吻合,铝、镁和铁的相对偏差(SD)分别≤3.85%、2.84%、2.63%,验证方法的准确性,能够满足科研及企业日常生产对湿法磷酸中铝、镁和铁一次性测定的需要。
In this study,we developed a rapid and accurate method to simultaneously detect aluminum,magnesium and iron in wet-process phosphoric acid by inductively coupled plasma-atomic emission spectrometry( ICPAES). We selected spectral lines with higher sensitivity as the analytical lines,optimized the instrument parameters,and developed a method to eliminate the influence of the matrix effect on the determination results without using phosphoric acid to prepare the standard solution. Spectral lines with wavelengths of 396. 156 nm,279. 077 nm,238. 204 nm were selected as the analytical lines for aluminum,magnesium and iron,respectively. The detection limits of aluminum,magnesium and iron were 0. 0013 μg/mL,0. 0022 μg/mL,and 0. 0054 μg/mL,respectively. The RSD of aluminum,magnesium and iron were 1. 5% to 6. 5%,1. 8% to 5. 3%,and 2. 5% to 8. 0%,respectively. The recovery rates of aluminum,magnesium and iron were 96. 9% to 106. 2%,92. 5% to 104. 0%,and97. 0% to 105. 5%,respectively. The results of this new method were basically consistent with the results of the standard addition method,with the SD less than 3. 85%,2. 84% and 2. 63%,respectively. The accuracy of this new method was verified,and it was proved that this method could meet the demands of scientific research and daily production.
In this study,we developed a rapid and accurate method to simultaneously detect aluminum,magnesium and iron in wet-process phosphoric acid by inductively coupled plasma-atomic emission spectrometry( ICPAES). We selected spectral lines with higher sensitivity as the analytical lines,optimized the instrument parameters,and developed a method to eliminate the influence of the matrix effect on the determination results without using phosphoric acid to prepare the standard solution. Spectral lines with wavelengths of 396. 156 nm,279. 077 nm,238. 204 nm were selected as the analytical lines for aluminum,magnesium and iron,respectively. The detection limits of aluminum,magnesium and iron were 0. 0013 μg/mL,0. 0022 μg/mL,and 0. 0054 μg/mL,respectively. The RSD of aluminum,magnesium and iron were 1. 5% to 6. 5%,1. 8% to 5. 3%,and 2. 5% to 8. 0%,respectively. The recovery rates of aluminum,magnesium and iron were 96. 9% to 106. 2%,92. 5% to 104. 0%,and97. 0% to 105. 5%,respectively. The results of this new method were basically consistent with the results of the standard addition method,with the SD less than 3. 85%,2. 84% and 2. 63%,respectively. The accuracy of this new method was verified,and it was proved that this method could meet the demands of scientific research and daily production.
引文
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[16]卢艳蓉,战丽君,王永刚,等.电感耦合等离子体原子发射光谱法测定铝基复合造渣剂中金属铝[J].冶金分析,2015,35(11):69-73.
[17]刘宏伟,张萍,胡汉祥.有机溶剂溶样-电感耦合等离子体质谱法直接测定六氟磷酸锂中26种杂质元素[J].分析化学,2014,42(6):913-917.
[18]全国半导体材料和设备标准化技术委员会.电子级磷酸:GB/T 28159—2011[S].北京:中国标准出版社,2012.
[19]CLOUGH R,SELA H,MILNE A,et al.Uncertainty contributions to the measurement of dissolved Co,Fe,Pb and V in seawater using flow injection with solid phase preconcentration and detection by collision/reaction cell-quadrupole ICP-MS[J].Talanta,2015,133:162-169.
[20]CHEVALLIER E,CHEKRI R,ZINCK J,et al.Simultaneous determination of 31 elements in foodstuffs by ICP-MS after closed-vessel microwave digestion:method validation based onthe accuracy profile[J].Journal of Food Composition and Analysis,2015,41:35-41.
[2]BELBOOM S,SZCS C,LONARD A.Environmental impacts of phosphoric acid production using di-hemihydrate process:a Belgian case study[J].Journal of Cleaner Production,2015,108:978-986.
[3]北京矿冶研究总院测试研究所.有色冶金分析手册[M].北京:冶金工业出版社,2004:155-499.
[4]中国石油和化学工业协会.食品添加剂磷酸:GB3149—2004[S].北京:中国标准出版社,2004.
[5]中国石油和化学工业协会.工业磷酸:GB/T 2091—2008[S].北京:中国标准出版社,2008.
[6]龙萍,梁骏.湿法磷酸中钾,钠,钙,镁的原子吸收光谱法测定[J].化学研究与应用,2006,18(7):837-839.
[7]PERONICO V C D,RAPOSO J L.Ultrasound-assisted extraction for the determination of Cu,Mn,Ca,and Mg in alternative oilseed crops using flame atomic absorption spectrometry[J].Food Chemistry,2016,196:1287-1292.
[8]TRINDADE A S N,DANTAS A F,LIMA D C,et al.Multivariate optimization of ultrasound-assisted extraction for determination of Cu,Fe,Ni and Zn in vegetable oils by high-resolution continuum source atomic absorption spectrometry[J].Food Chemistry,2015,185:145-150.
[9]LEAO D J,JUNIOR M M S,BRANDAO G C,et al.Simultaneous determination of cadmium,iron and tin in canned foods using high-resolution continuum source graphite furnace atomic absorption spectrometry[J].Talanta,2016,153:45-50.
[10]俞金生.火焰原子吸收光谱法测定载金炭中铜和铁[J].冶金分析,2015,35(12):28-31.
[11]罗少华,李华昌,许翠端.火焰原子吸收光谱法测定高纯铅中痕量钙,镁和钠[J].冶金分析,2007,27(7):1-4.
[12]孙丽丽.电感耦合等离子体发射光谱法测定湿法精制磷酸中镁,钙,铁,砷含量[J].中国无机分析化学,2013(1):71-73.SUN L L.Quantitative determination of Mg,Ca,Fe and As in the wet refining process for manufacturing phosphoric acid by ICPOES[J].Inorganic Analytical Abstracts of China,2013(1):71-73.
[13]OZBEK N,AKMAN S.Method development for the determination of calcium,copper,magnesium,manganese,iron,potassium,phosphorus and zinc in different types of breads by microwave induced plasma-atomic emission spectrometry[J].Food Chemistry,2016,200:245-248.
[14]XU Y,ZHANG W,YUE X,et al.Determination of aluminum in bamboo pulp black liquor by ICP-AES[J].BioResources,2016,11(2):3964-3971.
[15]王斌,李强.电感耦合等离子体原子发射光谱法测定铀矿石中全铁[J].冶金分析,2016,36(4):66-70.
[16]卢艳蓉,战丽君,王永刚,等.电感耦合等离子体原子发射光谱法测定铝基复合造渣剂中金属铝[J].冶金分析,2015,35(11):69-73.
[17]刘宏伟,张萍,胡汉祥.有机溶剂溶样-电感耦合等离子体质谱法直接测定六氟磷酸锂中26种杂质元素[J].分析化学,2014,42(6):913-917.
[18]全国半导体材料和设备标准化技术委员会.电子级磷酸:GB/T 28159—2011[S].北京:中国标准出版社,2012.
[19]CLOUGH R,SELA H,MILNE A,et al.Uncertainty contributions to the measurement of dissolved Co,Fe,Pb and V in seawater using flow injection with solid phase preconcentration and detection by collision/reaction cell-quadrupole ICP-MS[J].Talanta,2015,133:162-169.
[20]CHEVALLIER E,CHEKRI R,ZINCK J,et al.Simultaneous determination of 31 elements in foodstuffs by ICP-MS after closed-vessel microwave digestion:method validation based onthe accuracy profile[J].Journal of Food Composition and Analysis,2015,41:35-41.