石油炼制与化工

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溴化容量法测定水质中挥发酚两种标准方法的比较

刘玲1,彭敬雪2,齐敏2   

  1. 1. 抚顺石油化工研究院环保所
    2. 抚顺石油化工研究院
  • 收稿日期:2011-05-03 修回日期:2011-06-10 出版日期:2011-12-12 发布日期:2011-12-12
  • 通讯作者: 刘玲

COMPARISON STUDY ON TWO STANDARD METHODS FOR DETERMINATION OF VOLATILE PHENOLIC COMPOUNDS IN WATER BY BROMINE METHOD

  • Received:2011-05-03 Revised:2011-06-10 Online:2011-12-12 Published:2011-12-12

摘要: 从测定范围、分析步骤、溴酸钾-溴化钾及滴定剂消耗量、精密度和准确度等方面对溴化容量法测定水质中挥发酚GB7491-1987和HJ 502-2009两种标准进行了比较。结果表明: HJ 502-2009标准明确了挥发酚的测定范围为0.1~45.0 mg/L,增加了精密度和准确度条款,预蒸馏方式由二次蒸馏改为一次蒸馏;操作中固定溴酸钾-溴化钾溶液的体积为3 mL,仅一个空白试验可测试多个样品,更适合试样的批量分析。当100 mL 馏出液中挥发酚质量为2.35 mg时,两种标准消耗的溴酸钾-溴化钾溶液的量相同;当100 mL 馏出液中挥发酚质量小于2.35 mg时,标准HJ 502-2009标准消耗溴酸钾-溴化钾溶液和硫代硫酸钠标准溶液的量均大于GB 7491-1987标准中溴酸钾-溴化钾溶液和硫代硫酸钠标准溶液用量,当100 mL馏出液中挥发酚的质量大于2.35 mg时,结果正好相反。建议溴酸钾-溴化钾溶液的加入量由3 mL变为2.5 mL,100 mL馏出液中挥发酚的质量小于2.35 mg,以便于操作并提高试验准确度。

关键词: 挥发酚, 溴化容量法, GB 7491-1987, HJ 502-2009

Abstract: Two standards for determination of volatile phenolic compounds with bromine method, GB 7491-1987 and HJ 502-2009, were compared including determination range, analysis procedure, consumption of potassium bromated-potassium bromide solution and titrant, precision and accuracy. Comparison results show that in HJ 502-2009 standard method, the determination range of volatile phenolic compounds (0.1-45.0 mg/L) is definite, which is not clear in GB 7491-1987; the content of precision and accuracy is added, and sample pre-distillation is only once, which is twice in GB 7491-1987. According to HJ 502-2009 standard method, for 100 mL distillate, the adding volume of potassium bromated-potassium bromide solution is fixed to 3 mL, thus one blank test is enough for multiple samples analysis, which is more suitable to batch analysis. When the content of volatile phenolic compounds in 100 mL distillate is 2.35 mg, the consumptions of potassium bromated-potassium bromide solution of these two standard method are the same; when the content of volatile phenolic compounds in 100 mL distillate is less than 2.35 mg, the consumption of potassium bromated-potassium bromide solution and sodium thiosulfate standard solution in HJ 502-2009 standard method is more than those in GB 7491-1987; however, it is contrary when the content of volatile phenolic compounds in 100 mL distillate is more than 2.35 mg. It is suggested to change the fixed volume of potassium bromated-potassium bromide solution from 3 mL to 2.5 mL, and the content of volatile phenolic compounds in 100 mL distillate should be less than 2.35 mg for easy operation and better accuracy.

Key words: volatile phenolic compounds, bromine method, GB 7491-1987, HJ 502-2009