ICP-OES法测定废家电外壳HIPS中4种重金属
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摘要
针对现有消解方法对废家电塑料中存在消解不完全的现象,导致无法准确分析出Ro HS指令关注的塑料中的重金属Pb、Cd、Cr和Sb的具体含量,对后续研究废家电塑料中重金属的迁移转化造成困难。文章采用微波加热消解、电感耦合等离子体原子发射光谱(ICP-OES)法测定废家电外壳HIPS中重金属Pb、Cd、Cr、Sb的含量,并通过试验条件进行优化,达到了最佳消解效果。结果表明,与传统使用的电热板加热消解方法相比,该方法用时少,试验误差小;使用的酸危害性较小,安全性高。此外,优化后,试验方法回收率为93. 4%～107. 7%,精密度为0. 5%～5. 9%,可实现HIPS样品的全消解。该方法检测限度低,操作简单,可满足准确测定废家电塑料中重金属含量的需求。
The existed digestion methods had disadvantages of incomplete digestion to the waste appliances plastic,leading to inaccuracy analysis of metals ' concentration( Pb,Cd,Cr,Sb) in plastic regulated by Ro HS directive,thus providing a difficulty for investigating the migration of metals in waste appliances plastic. The combination of microwave digestion and inductively coupled plasma-optical emission spectrometry( ICP-OES) method was used to determine heavy metals( Pb、Cd、Cr、Sb) in HIPS came from the shell of waste appliances. The optimum dissolving effect was achieved by optimizing the test conditions. Results indicated that less time and smaller experimental error was achieved when compared with the conventional method consisted of electric heating plate,and the selected acid was less harmful. Besides,the recovery rate of selected method was ranged from 93. 4% to 107. 7%,while the RSD was from 0. 5% to 5. 9%,and the sample could be completely dissolved. It was showed that the method had advantages of convenient operation and low detection limit,thus the demand for exactly detecting the concentrations of heavy metals from waste appliances plastic was satisfied.
The existed digestion methods had disadvantages of incomplete digestion to the waste appliances plastic,leading to inaccuracy analysis of metals ' concentration( Pb,Cd,Cr,Sb) in plastic regulated by Ro HS directive,thus providing a difficulty for investigating the migration of metals in waste appliances plastic. The combination of microwave digestion and inductively coupled plasma-optical emission spectrometry( ICP-OES) method was used to determine heavy metals( Pb、Cd、Cr、Sb) in HIPS came from the shell of waste appliances. The optimum dissolving effect was achieved by optimizing the test conditions. Results indicated that less time and smaller experimental error was achieved when compared with the conventional method consisted of electric heating plate,and the selected acid was less harmful. Besides,the recovery rate of selected method was ranged from 93. 4% to 107. 7%,while the RSD was from 0. 5% to 5. 9%,and the sample could be completely dissolved. It was showed that the method had advantages of convenient operation and low detection limit,thus the demand for exactly detecting the concentrations of heavy metals from waste appliances plastic was satisfied.
引文
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[14]吴瑞林,丁曼蓉.微波能加热及其在化学分析中的应用[J].分析试验室,1991(2):51-54.
[15]王雪梅,杜彤彤,王娟,等.微波消解/ICP-MS同时测定粮食、蔬菜中的11种重金属元素[J].分析测试学报,2017,36(12):1522-1525.
[16] DURAND A,CHASE Z,TOWNSEND A T,et al. Improved methodology for the microwave digestion of carbonate-rich environmental samples[J]. International Journal of Environmental Analytical Chemistry,2016,96(2):119-136.
[17]李双琦,周良春,张晓飞,等. ICP-AES法同时测定塑胶跑道中的三种重金属[J].塑料,2017,46(5):127-129.
[18]贾会来,尹蓝,王茜,等.微波消解-ICP-MS测定皮革中7种重金属元素[J].分析试验室,2016,35(6):709-712.
[19]李险峰,张锦军,刘国聪.微波消解-ICP-AES法测定ABS塑料中的铅[J].湖北大学学报:自然科学版,2015,37(1):17-20.
[20]陶绪泉,王怀生,崔艳云,等. ICP-AES法测定PVC塑钢门窗中的重金属元素[J].塑料,2008,37(6):91-93.
[21] STEHRER T,HEITZ J,PEDARNIG J D,et a1. LA-ICP-MS analysis of waste polymer materials[J]. Analytical and Bioanalytical Chemistry. 2010,398(1):415-424.
[2]孙凯,徐东东,娄小安,等.阻燃聚丙烯在家电行业中的应用和发展[J].塑料工业,2013,41(6):5-9.
[3]代秀娟,徐海萍,翟月,等.废家电塑料再生资源化技术应用及发展趋势[J].再生资源与循环经济,2016,9(11):23-27.
[4] BALDC P,FORTI V,GRAY V,et al. The global e-waste monitor2017:quantities, flows, and resourses[M/OL]. Tokyo:United Nations University,2017. https://www. itu. int/en/ITU-D/ClimateChange/Documents/GEM%202017/Global-E-waste%20Monitor%202017%20. pdf.
[5] HERMABESSIERE L,DEHAUT A,PAUL-PONT I,et al. Occurrence and effects of plastic additives on marine environments and organisms:a review[J]. Chemosphere,2017,182:781-793.
[6] POWELL-TURNER J,ANTILL P D,FISHER RE. The United Kingdom Ministry of Defence and the European Union's electrical and electronic equipment directives[J]. Resources Policy,2016,49:422-432.
[7]刘芳,郑莉霞,谭全银,等.废旧电器电子产品越境转移国际管理制度比较[J].中国环境科学,2018,38(6):2193-2201.
[8] BRNO F,RICHTER S,DEITING D,et al. Direct multi-element analysis of plastic materials via solid sampling electrothermal vaporization inductively coupled plasma optical emission spectroscopy[J]. Journal of Analytical Atomic Spectrometry,2015,30(5):1064-1071.
[9]杨帆,白建峰,顾卫华,等.不同消解方法对废电视机外壳聚丙烯塑料中重金属含量测定的影响[J].上海第二工业大学学报,2017,34(2):106-111.
[10]贾会来,尹蓝,王茜,等.微波消解-ICP-MS测定皮革中7种重金属元素[J].分析试验室,2016,35(6):709-712.
[11] ENDERS A,LEHMANN J. Comparison of wet-digestion and dryashing methods for total elemental analysis of biochar[J].Communications in Soil Science and Plant Analysis,2012,43(7):1042-1052.
[12] RAMANATHAN T,TING Y. Selection of wet digestion methods for metal quantification in hazardous solid wastes[J]. Journal of Environmental Chemical Engineering,2015,3(3):1459-1467.
[13]丁伟.标准IEC62321—2013对电子电气产品中微量重金属(汞、铅、镉、铬)的规范检测[J].电子测试,2017(14):105-106.
[14]吴瑞林,丁曼蓉.微波能加热及其在化学分析中的应用[J].分析试验室,1991(2):51-54.
[15]王雪梅,杜彤彤,王娟,等.微波消解/ICP-MS同时测定粮食、蔬菜中的11种重金属元素[J].分析测试学报,2017,36(12):1522-1525.
[16] DURAND A,CHASE Z,TOWNSEND A T,et al. Improved methodology for the microwave digestion of carbonate-rich environmental samples[J]. International Journal of Environmental Analytical Chemistry,2016,96(2):119-136.
[17]李双琦,周良春,张晓飞,等. ICP-AES法同时测定塑胶跑道中的三种重金属[J].塑料,2017,46(5):127-129.
[18]贾会来,尹蓝,王茜,等.微波消解-ICP-MS测定皮革中7种重金属元素[J].分析试验室,2016,35(6):709-712.
[19]李险峰,张锦军,刘国聪.微波消解-ICP-AES法测定ABS塑料中的铅[J].湖北大学学报:自然科学版,2015,37(1):17-20.
[20]陶绪泉,王怀生,崔艳云,等. ICP-AES法测定PVC塑钢门窗中的重金属元素[J].塑料,2008,37(6):91-93.
[21] STEHRER T,HEITZ J,PEDARNIG J D,et a1. LA-ICP-MS analysis of waste polymer materials[J]. Analytical and Bioanalytical Chemistry. 2010,398(1):415-424.