混合酸溶解-电感耦合等离子体原子发射光谱法测定土壤中17种元素
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摘要
称取0.250 0g样品置于聚四氟乙烯坩埚中,加几滴水润湿样品,加入1.5mL硝酸、1.5mL盐酸、3mL氢氟酸和1mL高氯酸,盖上坩埚盖,置于排风橱中,放置过夜。将聚四氟乙烯坩埚放置于控温电热板上,于190～210℃加热,蒸发至白烟冒尽,关闭电源,然后加入5mL盐酸(1+1)溶液,加入2滴过氧化氢,在电热板上利用余温加热至固体盐类完全溶解,继续加热5～10min至溶液清亮,冷却后将溶液用水定容至25.0mL,静置3h后用电感耦合等离子体原子发射光谱法同时测定样品溶液中硫、铍、铈、钴、铜、锂、锰、镍、钪、镧、钒、锌、镁、钙、钾、钠和铁等17种元素。17种元素的质量浓度在一定范围内与其发射强度呈线性关系,检出限在0.02～50μg·g~(-1)之间。方法用于土壤国家标准物质中上述17种元素的测定,结果与认定值相符,测定值的相对标准偏差(n=12)小于4.0%。
The sample(0.250 0 g) was added into a Teflon crucible,and a few drops of water was added to wet the sample.Then 1.5 mL of nitric acid,1.5 mL of hydrochloric acid,3 mL of hydrofluoric acid and 1 mL of perchloric acid were added,and the crucible was covered with a lid and placed in the fume hood overnight.The Teflon crucible was placed on a temperature-controlled electric heating plate,and heated at 190-210 ℃.The solution was evaporated until the white smoke was exhausted,and the power was turned off. 5 mL of hydrochloric acid(1+1) solution and 2 drops of hydrogen peroxide were added.The residual temperature of the hot plate was used to continue to dissolve the solid salt,and the crucible was heated further for 5-10 min until the solution was clear.After cooling,the solution was made up to 25.0 mL with water and let stand still for 3 h.Inductively coupled plasma atomic emission spectrometry was used to simultaneously determine 17 elements,such as sulfur,bismuth,antimony,cobalt,copper,lithium, manganese,nickel,strontium,barium,vanadium,zinc, magnesium,potassium,calcium,sodium and iron in the sample solution.Linear relationships were found between emission intensity and mass concentration of the 17 elements in definite ranges,and the detection limits were in the range of0.02-50μg·g~(-1) .The method was applied to the determination of the above 17 elements in the national standard materials of soil,giving the results consistent with the certified values,and the relative standard deviations(n=12) of the measured values less than 4.0%.
The sample(0.250 0 g) was added into a Teflon crucible,and a few drops of water was added to wet the sample.Then 1.5 mL of nitric acid,1.5 mL of hydrochloric acid,3 mL of hydrofluoric acid and 1 mL of perchloric acid were added,and the crucible was covered with a lid and placed in the fume hood overnight.The Teflon crucible was placed on a temperature-controlled electric heating plate,and heated at 190-210 ℃.The solution was evaporated until the white smoke was exhausted,and the power was turned off. 5 mL of hydrochloric acid(1+1) solution and 2 drops of hydrogen peroxide were added.The residual temperature of the hot plate was used to continue to dissolve the solid salt,and the crucible was heated further for 5-10 min until the solution was clear.After cooling,the solution was made up to 25.0 mL with water and let stand still for 3 h.Inductively coupled plasma atomic emission spectrometry was used to simultaneously determine 17 elements,such as sulfur,bismuth,antimony,cobalt,copper,lithium, manganese,nickel,strontium,barium,vanadium,zinc, magnesium,potassium,calcium,sodium and iron in the sample solution.Linear relationships were found between emission intensity and mass concentration of the 17 elements in definite ranges,and the detection limits were in the range of0.02-50μg·g~(-1) .The method was applied to the determination of the above 17 elements in the national standard materials of soil,giving the results consistent with the certified values,and the relative standard deviations(n=12) of the measured values less than 4.0%.
引文
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[13] 沈亚婷,李迎春,孙梦荷,等.波长与能量色散复合式X射线荧光光谱仪特性研究及矿区土壤分析[J].光谱学与光谱分析,2017,37(7):2216-2224.
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[16] 陈静,高志军,陈冲科,等.X射线荧光光谱法分析地质样品的应用技巧[J].岩矿测试,2015,34(1):91-98.
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[18] 黄元.XRF-ICP-AES法测定土壤中的主次元素[J].化学分析计量,2015,24(6):73-76.
[19] 刘峰,秦樊鑫,胡继伟,等.不同混合酸消解样品对电感耦合等离子体原子发射光谱法测定土壤中重金属含量的影响[J].理化检验-化学分册,2011,47(8):951-954.
[20] 王龙山,郝辉,王光照,等.偏硼酸锂熔矿-超声提取-电感耦合等离子体发射光谱法测定岩石水系沉积物土壤样品中硅铝铁等10种元素[J].岩矿测试,2008,27(4):287-290.
[21] 赵庆令,李清彩,蒲军,等.电感耦合等离子体发射光谱法同时测定土壤样品中砷硼铈碘铌硫钪锶钍锆等31种元素[J].岩矿测试,2010,29(4):455-457.
[22] 武汉地质学院,长春地质学院,成都地质学院.岩石矿物分析教程[M].北京:地质出版社,1980.
[2] 冯新长,罗伟.微波消解-石墨炉原子吸收光谱法测定土壤中铍[J].环保科技,2013,19(4):36-38.
[3] 马剑丽,倪群英.微波消解-火焰原子吸收法测定土壤中铜锌铅镍锰[J].广州化工,2006,34(4):61-62.
[4] 鲁绍坤,贺冬仙,胡娟秀,等.基于多元素复合空心阴极灯的土壤有效养分测试[J].光谱学与光谱分析,2011,31(7):1930-1934.
[5] 况辉,卢邦俊.微波消解-原子吸收分光光度法测定土壤中的Cu、Zn、Pb、Cd、Cr和Ni[J].分析仪器,2007,1(4):29-31.
[6] 王世芳,韩平,王纪华,等.X射线荧光光谱分析法在土壤重金属检测中的应用研究进展[J].食品安全质量检测学报,2016,7(11):4394-4400.
[7] 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.
[8] 何恬叶,张颖红,胡子文.微波消解ICP-OES法测定土壤样品中22种元素[J].分析试验室,2018,37(1):84-87.
[9] 黎卫亮,王鹏.直接燃烧-红外吸收光谱法测定土壤、水系沉积物中的碳和硫[J].理化检验-化学分册,2013,49(10):1268-1269.
[10] 莫达松,罗平,蒋天成,等.红外吸收法测定土壤中硫含量结果的不确定度评定[J].广西科学,2012,19(3):247-248.
[11] 黄利英.西藏土壤全硫测定的初探[J].西藏农业科技,2013,35(2):28-30.
[12] 梁运献.硫酸钡比浊法测定土壤全硫的改进[J].广西农业科学,2002,1(4):186-187.
[13] 沈亚婷,李迎春,孙梦荷,等.波长与能量色散复合式X射线荧光光谱仪特性研究及矿区土壤分析[J].光谱学与光谱分析,2017,37(7):2216-2224.
[14] 李小平,黄春长.XRF光谱法研究城市工业区的土壤环境污染[J].土壤,2007,39(4):567-572.
[15] 张莉娟,刘义博,李小莉,等.超细粉末压片法-X射线荧光光谱仪测定水系沉积物和土壤中的主量元素[J].岩矿测试,2014,33(4):517-522.
[16] 陈静,高志军,陈冲科,等.X射线荧光光谱法分析地质样品的应用技巧[J].岩矿测试,2015,34(1):91-98.
[17] 叶家瑜,江宝林.区域地球化学勘查样品分析方法[M].北京:地质出版社,2004:73-76.
[18] 黄元.XRF-ICP-AES法测定土壤中的主次元素[J].化学分析计量,2015,24(6):73-76.
[19] 刘峰,秦樊鑫,胡继伟,等.不同混合酸消解样品对电感耦合等离子体原子发射光谱法测定土壤中重金属含量的影响[J].理化检验-化学分册,2011,47(8):951-954.
[20] 王龙山,郝辉,王光照,等.偏硼酸锂熔矿-超声提取-电感耦合等离子体发射光谱法测定岩石水系沉积物土壤样品中硅铝铁等10种元素[J].岩矿测试,2008,27(4):287-290.
[21] 赵庆令,李清彩,蒲军,等.电感耦合等离子体发射光谱法同时测定土壤样品中砷硼铈碘铌硫钪锶钍锆等31种元素[J].岩矿测试,2010,29(4):455-457.
[22] 武汉地质学院,长春地质学院,成都地质学院.岩石矿物分析教程[M].北京:地质出版社,1980.