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依据标准QB/T4340-2012《鞋类化学试验方法重金属总含量的测定电感耦合等离子体发射光谱法》,建立了橡胶鞋底微波消解的最优方法。试验表明,(0.2±0.01)g的橡胶鞋底材料,在0.7mL过氧化氢+5mL硝酸+0.5mL氢氟酸的酸性体系中,温度控制在230℃内,微波消解保持9min,可消解完全,消解液定容后呈无色透明状。本微波消解参数条件具备一定的抵抗样品质量波动干扰的能力,适用于丁苯类橡胶鞋底材料重金属检测的前处理过程,消解过程具备安全稳定、高效节能和对环境友好等特点。
According to the standard QB / T4340-2012 “Footwear chemical test method for determination of total heavy metals by inductively coupled plasma-atomic emission spectrometry,” the optimal method for rubber sole digestion was established. The results show that the rubber sole material of (0.2 ± 0.01) g can be completely digested in the acid system of 0.7mL hydrogen peroxide + 5mL nitric acid + 0.5mL hydrofluoric acid under the temperature control of 230 ℃ and microwave digestion for 9min, After digestion solution was colorless and transparent volume. The microwave digestion parameters have the ability to resist the interference of sample quality fluctuation and are suitable for the pretreatment process of the heavy metal detection of the butadiene rubber sole material. The digestion process has the characteristics of safety and stability, high efficiency, energy saving and environment friendliness.