摘要
电感耦合等离子体发射光谱仪（ICP-OES）可以完成多种元素的同时测定,在测试金属元素方面具有快速、高效、准确的特点,已被越来越多的高校、科研院所和企业使用。但在实际应用中,由于固废样品的复杂性,样品中多种元素的同时消解往往成为ICP-OES测试固废的主要难点。该文利用电热板、石墨炉和微波消解仪3种设备,研究了具有较高回收价值的阳极泥危险固废的消解方法,并通过ICP-OES测试了阳极泥中锡、铜、砷、铅、锑和镍6种金属元素的含量,对测试结果进行了分析比较。结果表明：选用合适的酸和设计合适的消解条件,3种消解设备都能完全消解阳极泥,其中微波消解耗时最短,效率最高;电热板消解、石墨消解和微波消解对同一样品中各金属含量的相对标准偏差分别为0.2%-1.3%、0.1%-1.2%和0.1%-0.9%,加标回收率分别为93%-113%、101%-116%和91%-108%,均符合质量保证要求。3种消解方法之间的各金属测试结果相对标准偏差在0.6%-4.5%之间,表明3种方法的测试结果具有可比性。实际应用中,可根据实验条件,在3种消解方法中进行选用,得到可靠的测试数据。该文的分析方法和相关数据可为相关危险固废的监测和有价金属的提取提供有益的参考,具有很好的应用意义。
The inductively coupled plasma emission spectroscopy（ICP-OES）has been widely used in universities,research institutes and enterprises since it can determine multiple elements at the same time with a fast,efficient and accurate characteristics. However,in practice,due to the complexity of solid waste samples,the multi-element digestion simultaneously becomes the major difficulty to use ICP-OES. The anode mud has a high recovery value and is a sort of hazardous solid waste. In this paper,the digestion methods of anode mud were researched using hot plate,graphite digestion apparatus and microwave digestion instrument. The six metal content of tin,copper,arsenic,lead,antimony and nickel in the anode mud were measured using ICP-OES and the results were compared. The results showed that three digestions can completely digest the anode mud by choosing appropriate acids and designing suitable digestion conditions. The microwave digestion method took the shortest time and had the best digestion efficiency among the three digestion methods. The relative standard deviations of hot plate digestion,graphite digestion and microwave digestion for the metal content of the same sample were0.2% to 1.3%,0.1% to 1.2% and 0.1% to 0.9%,respectively,with the recoveries as 93% to 113%,101% to 116% and 91% to108%,respectively,which meet the requirements of quality assurance. The relative standard deviations of the three digestion methods for the metal content of the same sample were between 0.6% and 4.5%,which implied that the test results of the three digestion methods are comparable. In practice,the three digestion methods can be chosen to attain the reliable dataaccording to the actual experimental conditions. The analytical methods and data in this paper have useful reference to monitor relevant hazardous wastes and extract valuable metals from solid wastes.
出处
《环境科学与技术》
CAS
CSCD
北大核心
2016年第3期100-104,共5页
Environmental Science & Technology
基金
2013年度院长基金(KY20130101
KY20130102)
