极谱法测定化探样品中钨钼的技术改进
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摘要
针对传统极谱法测定化探样品中钨钼时操作手段繁琐问题加以改进。试样以硫酸-二苯乙醇酸-二苯胍-氯酸钠体系为混合底液,将经过碱熔融后的样品以甲基橙为指示剂,用硫酸(1+1)调酸度后,加入固定比例的混合底液,摇匀,无需定容,放置25~30min后直接测定。采用二次倒数波测定,钨峰电位在-660mV左右,钼峰电位在-30mV左右,钨钼的质量浓度在0.02~1.0μg/mL内呈线性关系,钨检出限为0.5μg/g,钼检出限为0.3μg/g。方法灵敏度高,快捷、简单,适用于大批量化探样品的测定。
In this paper,the complexity of the traditional polarographic method for the determination of tungsten and molybdenum in geochemical samples was improved.The sample was made of sodium sulphate-two benzilic acid-sodium chlorate system as a mixed substrate.Afterwards,the sample was melted with methyl orange as an indicator,then with sulfuric acid(1+1)to adjust the acidity.A fixed proportion of mixed liquor was added,shacked well,and without a constant volume,directly measured after 25—30 minutes.Using two reciprocal waves,the tungsten peak potential was about-660 mV,the molybdenum peak potential was about -30 mV,the mass concentration of tungsten and molybdenum was linear in the 0.02—1.0μg/mL range,and the detection limit of tungsten was 0.5μg/g,and for molybdenum was 0.3μg/g.This method is highly sensitive,fast,simple,and is suitable for the determination of large quantities of geochemical samples.
In this paper,the complexity of the traditional polarographic method for the determination of tungsten and molybdenum in geochemical samples was improved.The sample was made of sodium sulphate-two benzilic acid-sodium chlorate system as a mixed substrate.Afterwards,the sample was melted with methyl orange as an indicator,then with sulfuric acid(1+1)to adjust the acidity.A fixed proportion of mixed liquor was added,shacked well,and without a constant volume,directly measured after 25—30 minutes.Using two reciprocal waves,the tungsten peak potential was about-660 mV,the molybdenum peak potential was about -30 mV,the mass concentration of tungsten and molybdenum was linear in the 0.02—1.0μg/mL range,and the detection limit of tungsten was 0.5μg/g,and for molybdenum was 0.3μg/g.This method is highly sensitive,fast,simple,and is suitable for the determination of large quantities of geochemical samples.
引文
[1]梁云生,毛禹平.极谱法测定矿石中高含量钨[J].中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2013,3(2):32-34.
[2]中华人民共和国国土资源部.DZ/T0130—2006地质矿产实验室测试质量管理规范区域地球化学调查(1∶50000和1∶200000)样品化学成分分析[S].北京:中国标准出版社,2007.
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[6]赵宝,杨华.极谱法测定化探样品中的钨、钼[J].化学分析计量(Chemical Analysis and Meterage),2009,18(2):37-39.
[7]范春燕.土壤中微量钨钼示波极谱的连续测定[J].华北国土资源(Huabei Land and Resources),2008(4):64-66.
[2]中华人民共和国国土资源部.DZ/T0130—2006地质矿产实验室测试质量管理规范区域地球化学调查(1∶50000和1∶200000)样品化学成分分析[S].北京:中国标准出版社,2007.
[3]叶家瑜,汇宝林.区域地球化学勘察样品分析方法[M].北京:地质出版社,2004.
[4]中华人民共和国地质矿产部.DZG93—1993岩石和矿物分析规程[S].北京:地质出版社,1994.
[5]贾玉萍,王湘玲,肖建平.改进的极谱法测定化探样品中的钨钼[J].岩矿测试(Rock and Mineral Analysis),2009,28(5):494-496.
[6]赵宝,杨华.极谱法测定化探样品中的钨、钼[J].化学分析计量(Chemical Analysis and Meterage),2009,18(2):37-39.
[7]范春燕.土壤中微量钨钼示波极谱的连续测定[J].华北国土资源(Huabei Land and Resources),2008(4):64-66.