Gould J H, Butler S W, Boyer K W, Steele E A
J Assoc Off Anal Chem. 1983 May;66(3):610-9.
A hot leach method published by the World Health Organization for determining Pb and Cd in ceramic and enameled ware was collaboratively studied in 14 laboratories. The method consisted of heating a solution of 4% acetic acid at the boil for 2 h in 6 samples of specially glazed ceramic ware and 6 samples of special enameled ware. The acid was allowed to cool and stand in contact with the ware for an additional 22 h. At the end of the 2 h heating period and again at the end of the 24 h period, the leach solution was assayed by atomic absorption spectrophotometry for Pb and Cd. Ruggedness testing before the collaborative study revealed that: (1) the quantity of metal released increased as the average leach temperature approached the boiling point, (2) the quantity of Pb and Cd released from enameled ware increased linearly with time during 7 h of boiling, (3) the concentration of acid could be varied from 2 to 6% with no apparent effect on the amount of metal released, and (4) the room temperature (RT) contact period lasting from 22 to 120 h (after the 2 h heating period) did not increase the amount of metal released. The quantities of Pb and Cd measured by the collaborators at the end of 2 h of heating and after 24 h of total contact were essentially identical. The amounts of Pb and Cd were not related to the quantity of acid solution required to restore the leach solution volume to its initial value after boiling. The collaborative results showed that the period of standing at RT is not necessary and probably can be eliminated from the method. The modified method, which requires analysis of the leach solution immediately after the 2 h heating period, has been adopted interim official first action by AOAC.
世界卫生组织公布的一种用于测定陶瓷和搪瓷器皿中铅和镉的热浸出法,在14个实验室进行了协同研究。该方法包括在6个特制釉面陶瓷器皿样品和6个特制搪瓷器皿样品中,将4%的醋酸溶液煮沸2小时。让酸冷却并与器皿再接触22小时。在加热2小时结束时以及24小时结束时,用原子吸收分光光度法测定浸出液中的铅和镉。协同研究前的耐用性测试表明:(1)随着平均浸出温度接近沸点,释放的金属量增加;(2)在煮沸7小时期间,从搪瓷器皿中释放的铅和镉的量随时间呈线性增加;(3)酸的浓度可在2%至6%之间变化,对释放的金属量没有明显影响;(4)在2小时加热期后,室温(RT)接触期持续22至120小时,并未增加释放的金属量。协同研究者在加热2小时结束时和总接触24小时后测得的铅和镉的量基本相同。铅和镉的量与煮沸后将浸出液体积恢复到初始值所需的酸溶液量无关。协同研究结果表明,室温静置期并非必要,可能可以从该方法中去除。经修改的方法,即在加热2小时后立即分析浸出液,已被AOAC临时采用为官方首次行动方法。