光谱学与光谱分析, 2017, 37 (2): 646, 网络出版: 2017-06-20
微波消解ICP-MS测定铝塑包装材料中的Pb, Cr, Cd和As含量
Determination of Pb, Cr, Cd, and As in Aluminum-Plastic Packaging Materials via Inductively Coupled Plasma-Mass Spectrometry with Microwave Digestion
微波消解 电感耦合等离子体质谱 铝塑包装 铅 铬 镉 砷 Microwave digestion ICP-MS Aluminum-plastic packaging Lead Chromium Cadmium Arsenic
摘要
通过微波消解法对铝塑包装材料的前处理方法进行了深入的研究, 考虑了5种不同的消解试剂组合以及不同的浓度配比关系对铝塑包装材料消解效果的影响, 并对消解现象产生的可能性原因进行了简单的分析, 结果发现硫酸-硝酸试剂组合消解效果最佳, 正交试验结果表明试剂组合的最佳配比为1∶7。 随后采用电感耦合等离子体质谱法(ICP-MS)测定了铝塑包装材料中的Pb, Cr, Cd和As, 各元素仪器检出限依次为0215, 0067, 0006和0020 ng·mL-1, 线性相关系数在0999 5以上; 2#试样进行加标回收试验, 回收率在838%~1116%之间, 相对标准偏差(RSD)在05%~74%之间; 5种试样两次独立平行测定结果均比较接近, t检验法(取置信水平α=005)结果表明两次测定结果均无显著性差异。 综上表明该方法线性关系好, 检出限低, 回收率高, 精密度好, 可准确测定铝塑包装材料及类似材料中的Pb, Cr, Cd, As含量。
Abstract
Microwave digestion was performed to study the pretreatment methods of aluminum-plastic packaging materials (APPMs). Five different digestion reagent combinations and proportions were thoroughly considered. Digestion results indicated that the most suitable reagent combination was sulfuric and nitric acids with the optimal proportion of 1∶7 after the orthogonal experiment. Moreover, the possible reasons of the experimental phenomenon were analyzed. The contents of Pb, Cr, Cd, and As in APPMs were subsequently determined via inductively coupled plasma-mass spectrometry (ICP-MS). The satisfactory linearity of calibration curves was obtained with the linear correlation coefficients above 0999 5, and the instrument detection limits of Pb, Cr, Cd, and As for the current method were 0215, 0067, 0006 and 0020 ng·mL-1, respectively. Furthermore, the recoveries of standard addition ranged from 838% to 1116%, and the relative standard deviations ranged from 05% to 74%. Two independent parallel determination results of Pb, Cr, Cd, and As in APPMs were approaching, and the student’s t-test (confidence level, α=005) showed that the determination results had no significant differences. In conclusion, the present method exhibited fine linearity, low detection limit, high recovery, and good precision, which can accurately be utilized to analyze Pb, Cr, Cd, and As elements in APPMs or other similar materials.
弥海鹏, 朱宏明, 李根容, 于翔, 马兵兵, 周西林, 王亚森, 苏中华, 邓雄. 微波消解ICP-MS测定铝塑包装材料中的Pb, Cr, Cd和As含量[J]. 光谱学与光谱分析, 2017, 37(2): 646. MI Hai-peng, ZHU Hong-ming, LI Gen-rong, YU Xiang, MA Bing-bing, ZHOU Xi-lin, WANG Ya-sen, SU Zhong-hua, DENG Xiong. Determination of Pb, Cr, Cd, and As in Aluminum-Plastic Packaging Materials via Inductively Coupled Plasma-Mass Spectrometry with Microwave Digestion[J]. Spectroscopy and Spectral Analysis, 2017, 37(2): 646.