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    基于加速萃取的仿真饰品中镍释放量快速预报方法

    Rapid Forecast Method for Nickel Release in Simulated Jewelry Based on Accelerated Extraction

    • 摘要: 针对饰品中镍释放量标准方法测试周期长等问题,对标准方法中迁移温度、迁移时间、模拟汗液酸度、迁移液体积等关键迁移条件,以及不同迁移温度和时间下镍释放规律进行研究,提出了基于加速萃取的适用于不同基质仿真饰品中镍释放量测定的快速预报方法。采用面积为2.7 cm2的仿真饰品样品,悬挂于测试容器中,按样品测试面积(cm2)和模拟汗液体积(mL)比约1∶1加入2.7 mL模拟汗液,完全浸没样品,密封后于50 ℃静置31 h。加入1 mL 5%(体积分数)硝酸溶液,用模拟汗液定容至5 mL,采用电感耦合等离子体原子发射光谱法进行测定。结果显示:迁移温度相较其他迁移条件对镍释放量影响大,于30,40,50 ℃迁移24,48,72,168,240 h时50 ℃下镍释放量和相对镍释放率(上述方法和标准EN1811:2015镍释放量的比值)均较大;50 ℃下相对镍释放率与迁移时间的回归模型为幂函数,100%相对镍释放率下迁移时间为31 h,远低于标准EN1811:2015所用的168 h。方法应用于铜合金、镍合金、不锈钢和铜锌合金样品(仿真饰品)的分析,所得结果和EN1811:2015的一致,测定值的相对标准偏差(n=5)小于6.0%。

       

      Abstract: In response to the issue of long testing cycles for nickel release in jewelry of the standard method, key migration conditions such as migration temperature, migration time, simulated sweat acidity, and migration solution volume in standard method together with nickel release rules under different migration temperatures and time were studied, and a fast forecast method based on accelerated extraction was proposed for determining nickel release in simulated jewelry with different substrates. The simulated jewelry sample with area of 2.7 cm2 was intercepted, and suspended in a testing container. Then 2.7 mL approximately 1∶1 of the ratio of sample area (cm2) to volume (mL) of simulated sweat of simulated sweat was added, completely immersing the sample. After sealing, the testing system was settled at 50 ℃ for 31 h. 1 mL of 5% (volume fraction) nitric acid solution was added, and the mixed solution was diluted to 5 mL by simulated sweat. The resulting solution was determined by inductively coupled plasma atomic emission spectrometry. It was shown that the migration temperature had a greater impact on the nickel release compared to other migration conditions. At 30, 40, 50 ℃, the nickel release and relative nickel release rate (the ratio of nickel release between this method and standard EN 1811: 2015) were larger at 50 ℃ for 24, 48, 72, 168, 240 h of migration. The regression model between relative nickel release rate and migration time at 50 ℃ was a power function, and the migration time at 100% relative nickel release rate was 31 h, which was much lower than the 168 h used in standard EN1811: 2015. The proposed method was used for the analysis of copper alloy, nickel alloy, stainless steel, and copper zinc alloy samples (simulated jewelry), and the results obtained were consistent with those given by EN 1811: 2015, with RSDs (n=5) of the determined values less than 6.0%.

       

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