微波消解-光度法测定石膏中硅和铁含量
Photometric Determination of SiO2 and Fe2O3 in Gypsum with Microwave Assisted Sample Digestion
摘 要
利用改进的微波消解技术对石膏样品进行快速消解,并采用钼蓝法和邻二氮菲光度法分别测定石膏样品中二氧化硅和三氧化二铁的含量.微波消解溶剂为300 g·L-1氢氧化钠溶液5.0 mL,微波功率为700 W,微波消解时间为180 s.3个石膏标准物质的测定结果与标准值相符,3种实际样品的测定结果也与常规的碱熔法一致.
二氧化硅
三氧化二铁
石膏
Microwave assisted sample digestion
SiO2
Fe2O3
Gypsum
Abstract
In the photometric determination of SiO2 (by molybdenum blue method) and Fe2O3 (by o-phenanthroline method) in gypsum,modified microwave assisted sample digestion was adopted in the dissolution of gypsum sample in NaOH solution. Under the optimized conditions,including working parameters of the microwave oven and concentration of the NaOH solution,the dissolution of gypsum sample was completed in 180 s. Results of determination of SiO2 and Fe2O3 in 3 gypsum CRM′s by the present method were found in conformity with the certified values. No significant difference was observed between the values of SiO2 and Fe2O3 found by the microwave assisted sample digestion method and by the conventional alkali fusion method.
中图分类号 O657.3
所属栏目 工作简报
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收稿日期 2008/12/12
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备注蔡宏伟(1965-),男,陕西铜川人,副教授,主要研究方向为分析测试技术和计算化学.
引用该论文: CAI Hong-wei,WANG Zhi-Hua,HU Ji-Ming. Photometric Determination of SiO2 and Fe2O3 in Gypsum with Microwave Assisted Sample Digestion[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(7): 830～831
蔡宏伟,王志花,胡继明. 微波消解-光度法测定石膏中硅和铁含量[J]. 理化检验－化学分册, 2009, 45(7): 830～831
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【5】SANDRONI V,SMITH C M M,DONOVAN A. Microwave digestion of sediment,soils and urban particulate matter for trace metal analysis[J]. Talanta,2003,60:715-723．
【6】WILSON M A,BURT R,LEE C W. Improved elemental recoveries in soils with heating boric acid following microwave total digestion [J]. Communications in Soil Science and Plant Analysis,2006,37:513-524．
【7】CAI Hong-wei,JIANG Ping,JIN Ling,et al. Microwave enhanced alkaline digestion of silicate samples for determination of Fe2O3[J]. Talanta,2008,77:800-803．
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