Determination of Tin in Soil by Hydride Generation-Atomic Fluorescence Spectrometry with Microwave Assisted Digestion in Alkaline Solution
摘 要
土壤样品先在烘箱内于(102±3)℃下干燥2 h。称取此样品0.10 g置于聚四氟乙烯(PTFE)消解罐中,加入500 g·L-1氢氧化钠溶液2 mL,按程序升温模式在微波消解仪中进行消解。消解完成后,加二次去离子水将溶液稀释至25.0 mL,样品溶液经载流(1 mol·L-1氢氧化钠溶液)通过三通阀进入仪器,并在线被5%(体积分数)硫酸溶液中和后与由蠕动泵传送的还原剂硼氢化钾反应生成氢化锡,传送进入原子化器迅速原子化,在高性能空心阴极灯的作用下产生荧光,由检测器检测其峰面积。测得锡的标准曲线的线性范围在100 μg·L-1以内。以3倍空白值求得的标准偏差计算其检出限(3s)为0.062 μg·g-1。用此方法测定了7个GBW标准物质,所得结果与认定值之间的相对误差为-1.61%~3.07%,测定值的相对标准偏差(n=7)为1.8%~3.2%。
Abstract
The soil sample should be dried preliminarily at (102±3)℃ in an oven. 0.10 g of the dried sample was taken and digested with 2 mL of 500 g·L-1 sodium hydroxide solution in the PTFE vessel in the microwave digestor under programmed temperature elevation mode. At the end of digestion, the solution obtained was diluted to 25.0 mL with re-deionized water, and used as sample solution for atom fluorescence spectrometry analysis. The sample solution was introduced into the atom fluorescence spectrometry instrument by the carrier of 1 mol·L-1 sodium hydroxide solution and through the 3-way valve. 5% (volum fraction) sulfuric acid solution, as introduced also through the 3-way valve, was used for online neutralization of the alkaline sample solution, and then the acidic sample solution was reacted with potessium borohydride, delivered by the wriggling pump, to have the Sn(Ⅱ) reacted to form tin hydride which was atomized in the atomizer. By the action ofthe high performance hollow cathode lamp, fluorescence of tin atom was emitted and its intensity as shown by its peak area was measured by the detector. Linearity range of the standard curve of tin was found within 100 μg·L-1. Value of detection limit (3s) found was 0.062 μg·g-1. Seven GBW standard materials of soil were analyzed by the present method, giving relative errors between the results found by this method and the certified values of the CRMs in the range of -1.61%-3.07%. Values of RSDs (n=7) obtained were ranged from 1.8%-3.2%.
中图分类号 O657.31 DOI 10.11973/lhjy-hx202003017
所属栏目 工作简报
基金项目
收稿日期 2019/8/4
修改稿日期
网络出版日期
作者单位点击查看
备注王雪枫,工程师,主要从事矿产的理化检验工作,wxf111027@163.com
引用该论文: WANG Xuefeng,LI Xiang,KANG Wengui. Determination of Tin in Soil by Hydride Generation-Atomic Fluorescence Spectrometry with Microwave Assisted Digestion in Alkaline Solution[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(3): 344~348
王雪枫,李湘,康文贵. 碱性溶液微波消解-氢化物发生-原子荧光光谱法测定土壤中锡[J]. 理化检验-化学分册, 2020, 56(3): 344~348
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】《岩石矿物分析》编委会.岩石矿物分析[M].北京:地质出版社, 2011:185-208.
【2】国家环境保护总局《水和废水监测分析方法》编委会.水和废水监测分析方法[M].4版.北京:中国环境出版社, 2002.
【3】朱明娟,田新.原子荧光光度法测定土壤样品中锡的研究[J].现代盐化工, 2016(3):26-28.
【4】WANG J Y, LIU M, YAN H L. Study on the polarographic absorptive wave of tin with sulphuric acid-ammonium metavanadate-hydrobromic acid-ascorbic acid system and its application in ore[J]. Metallurgical Analysis, 2015,35(12):41-45.
【5】刘源源.微波消解石墨炉原子吸收法测定土壤中痕量锡[J].现代化工, 2015,35(6):183-185.
【6】王晓慧,齐文启,刘廷良,等.石墨炉原子吸收法测定土壤中的锡[J].环境科学研究, 1999,12(1):54-55.
【7】孛丽娟.发射光谱法测定化探样品中锡和钼的含量[J].新疆有色金属, 2015,38(5):47-48.
【8】姚建贞,郝志红,唐瑞玲,等.固体发射光谱法测定地球化学样品中的高含量锡[J].光谱学与光谱分析, 2013,33(11):3124-3127.
【9】张晔霞,沈清.碱熔法消解-原子荧光法测定土壤中的锡[J].污染防治技术, 2011,24(4):63-65.
【10】刘香英,崔建勇,夏晨光,等.原子荧光光谱法测定土壤样品中的微量锡[J].铀矿地质, 2015,31(5):531-535.
【11】王升章,郭小伟.氢化物-无色散原子荧光法测定地质样品中微量锡[J].理化检验-化学分册, 1984,20(5):15-16.
【12】周勇义,谷学新,范国强,等.微波消解技术及其在分析化学中的应用[J].冶金分析, 2004,24(2):30-36.
【2】国家环境保护总局《水和废水监测分析方法》编委会.水和废水监测分析方法[M].4版.北京:中国环境出版社, 2002.
【3】朱明娟,田新.原子荧光光度法测定土壤样品中锡的研究[J].现代盐化工, 2016(3):26-28.
【4】WANG J Y, LIU M, YAN H L. Study on the polarographic absorptive wave of tin with sulphuric acid-ammonium metavanadate-hydrobromic acid-ascorbic acid system and its application in ore[J]. Metallurgical Analysis, 2015,35(12):41-45.
【5】刘源源.微波消解石墨炉原子吸收法测定土壤中痕量锡[J].现代化工, 2015,35(6):183-185.
【6】王晓慧,齐文启,刘廷良,等.石墨炉原子吸收法测定土壤中的锡[J].环境科学研究, 1999,12(1):54-55.
【7】孛丽娟.发射光谱法测定化探样品中锡和钼的含量[J].新疆有色金属, 2015,38(5):47-48.
【8】姚建贞,郝志红,唐瑞玲,等.固体发射光谱法测定地球化学样品中的高含量锡[J].光谱学与光谱分析, 2013,33(11):3124-3127.
【9】张晔霞,沈清.碱熔法消解-原子荧光法测定土壤中的锡[J].污染防治技术, 2011,24(4):63-65.
【10】刘香英,崔建勇,夏晨光,等.原子荧光光谱法测定土壤样品中的微量锡[J].铀矿地质, 2015,31(5):531-535.
【11】王升章,郭小伟.氢化物-无色散原子荧光法测定地质样品中微量锡[J].理化检验-化学分册, 1984,20(5):15-16.
【12】周勇义,谷学新,范国强,等.微波消解技术及其在分析化学中的应用[J].冶金分析, 2004,24(2):30-36.
相关信息