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测定黄磷中砷方法的样品前处理的改进
引用本文:李佳,朱晓帆,梁进,张志斌.测定黄磷中砷方法的样品前处理的改进[J].理化检验(化学分册),2011(1).
作者姓名:李佳  朱晓帆  梁进  张志斌
作者单位:四川大学建筑与环境学院;四川大学分析测试中心;
基金项目:“十一五”国家科技支撑计划(2007BAE58B07)
摘    要:标准方法(GB 7816-1998)测定黄磷中砷时,采用敞开式消解法预处理样品。实践表明该方法耗时,易引入污染,造成测定误差,而且稍有不慎易使黄磷自燃。作为改进,提出了回流冷凝消解法,即2~3 g试样于硝酸(3+2)溶液60 mL中,在160℃电热板上加热回流消解。消解完成后的试液按Ag-DDTC方法进行砷的测定。结果表明:回流冷凝消解法不仅避免了试样的自燃,而且大大缩短了试样消解时间,所测得砷结果的准确度达到原标准方法的水平。

关 键 词:黄磷    试样预处理  回流冷凝消解法  

Modification for Pretreatment of Sample in the Determination of Arsenic in Yellow Phosphorus
LI Jia,ZHU Xiao-fan,LIANG Jin,ZHANG Zhi-bin.Modification for Pretreatment of Sample in the Determination of Arsenic in Yellow Phosphorus[J].Physical Testing and Chemical Analysis Part B:Chemical Analgsis,2011(1).
Authors:LI Jia  ZHU Xiao-fan  LIANG Jin  ZHANG Zhi-bin
Institution:LI Jia1,ZHU Xiao-fan2*,LIANG Jin1,ZHANG Zhi-bin1(1.College of Architecture and Environments,Sichuan University,Chengdu 610065,China,2.Analytical and Testing Center,China)
Abstract:In the determination of arsenic in yellow phosphorus by the GB standard method(GB 7816-1998),the sample pretreatment was carried out by digestion with HNO3 in an open vessel.As happened actually,this method of sample pretreatment had the defects of time-consuming,accidental error due to contamination and unsafety of self-burning of sample.As a modification,sample pretreatment by reflux digestion was proposed,i.e.,the sample(2-3 g) was digested with 60 mL of HNO3(3+2) under refluxing at a heating temperature...
Keywords:Yellow phosphorus  Arsenic  Sample pretreatment  Refluxing condensation digestion  
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