电感耦合等离子体质谱法测定载银硅橡胶制品中银含量及迁移量

Determination of content and migration of silver in silver-loaded silicone rubber products by inductively coupled plasma mass spectrometry

中文关键词:  电感耦合等离子体质谱法  硅橡胶  银  含量  迁移量

英文关键词:inductively coupled plasma mass spectrometry  silicone rubber  silver  content  migration

中文摘要:

      目的 建立电感耦合等离子体质谱法测定载银硅橡胶制品中银含量及迁移量的分析方法。方法 银含量前处理采用3 mL硝酸-2 mL氢氟酸作为消解酸, 用微波消解法消解; 迁移量采用0.07 mol/L盐酸溶液、4%乙酸和人工唾液3种模拟液, 经40 ℃浸泡振荡24 h后, 浸泡液经过滤, 用电感耦合等离子体质谱法进行定量分析。结果 银含量测定在0~100 μg/L质量浓度范围内有好的线性, 相关系数(r)为1.0000, 检出限为0.0009 mg/kg, 定量限为0.0029 mg/kg, 加标回收率为95.5%~102.2%, 相对标准偏差(relative standard deviations, RSDs)为0.92%~2.25%。在0.07 mol/L盐酸溶液、4%乙酸溶液和人工唾液模拟物中, 银在0~100 μg/L质量浓度范围内有好的线性, 相关系数(r)均大于0.9995, 检出限分别为0.0002、0.0012和0.0024 mg/kg, 定量限为0.0006、0.0036和0.0077 mg/kg, 加标回收率为92.3%~101.8%, RSD为1.03%~2.67%。22个样品银总含量测定结果在未检出~9.76 mg/kg, 检出率为81.8%, 4%乙酸溶液迁移、0.07 mol/L盐酸溶液和人工唾液3种迁移结果分别为未检出~0.0767 mg/kg、未检出~0.1061 mg/kg和未检出~0.0270 mg/kg, 检出率分别为22.7%、45.5%和9.1%。结论 该方法操作简便、灵敏度高、准确性好, 能满足硅橡胶中银总量和迁移量的检测。

英文摘要:

      Objective To establish an analytical method for the determination of content and migration of silver in silver-loaded silicone rubber products by inductively coupled plasma mass spectrometry. Methods The 3 mL nitric acid and 2 mL hydrofluoric acid were used as digestion acid for pretreatment of silver content, which were digested by microwave digestion method. The migration was simulated with 0.07 mol/L hydrochloric acid solution, 4% acetic acid and artificial saliva. After shaking at 40 ℃ for 24 h, the immersion solution was filtered, and the quantitative analysis was performed by inductively coupled plasma mass spectrometry. Results The silver content had good linearity in the mass concentration range of 0–100 μg/L, the correlation coefficient (r) was 1.0000, the limit of detection was 0.0009 mg/kg, the limit of quantitation was 0.0029 mg/kg, and the recovery rates were 95.5%–102.2%. The relative standard deviations (RSDs) were 0.92%–2.25%. In 0.07 mol/L hydrochloric acid solution, 4% acetic acid solution and artificial saliva mimics, silver had good linearity in the mass concentration range of 0–100 μg/L, and the correlation coefficients (r) were greater than 0.9995. The limits of detection were 0.0002, 0.0012 and 0.0024 mg/kg, respectively. The limits of quantitation were 0.0006, 0.0036 and 0.0077 mg/kg, the recoveries were 92.3%–101.8%, and the RSD was 1.03%–2.67%. The total silver content of 22 samples was not detected to 9.76 mg/kg, and the detection rate was 81.8%. The migration results of 4% acetic acid solution, 0.07 mol/L hydrochloric acid solution and artificial saliva were not detected to 0.0767 mg/kg, not detected to 0.1061 mg/kg and not detected to 0.0270 mg/kg, respectively, and the detection rates were 22.7%, 45.5% and 9.1%, respectively. Conclusion This method is convenient, sensitive, accreted and is suitable for quantitative analysis of total content and migration of silver in silicone rubber.