Baldwin S, Deaker M, Maher W
Faculty of Applied Science, University of Canberra, Beclonnen, ACT, Australia.
Analyst. 1994 Aug;119(8):1701-4. doi: 10.1039/an9941901701.
The use of low-volume (7 ml) Teflon vessels and microwave heating is described for the digestion of three marine biological tissues representing a mollusc, a fish and a crustacean. Freeze-dried samples (< 0.1 g dry mass) and 1 ml of nitric acid were placed in 7 ml screw-topped Teflon vessels and treated using a programmed three-stage digestion. The first two stages were kept consistent (600 W, 2 min; 0 W, 2 min) and the third stage was varied from 150 to 450 W over 15-60 min to find the optimum microwave digestion conditions. Trace elements were determined using flame atomic absorption spectrometry, or electrothermal atomic absorption spectrometry when analysing samples containing very low concentrations of cadmium. Quantitative recoveries of copper, zinc and cadmium were obtained from the five marine reference materials under the following conditions: 600 W, 2 mins; 0 W, 2 min; 450 W, 45 mins.
本文描述了使用小容量(7毫升)的特氟龙容器和微波加热来消解三种海洋生物组织,分别代表软体动物、鱼类和甲壳类动物。将冷冻干燥的样品(干质量<0.1克)和1毫升硝酸放入7毫升带螺旋盖的特氟龙容器中,并采用程序化的三阶段消解处理。前两个阶段保持一致(600瓦,2分钟;0瓦,2分钟),第三阶段在15至60分钟内功率从150瓦变化到450瓦,以找到最佳的微波消解条件。使用火焰原子吸收光谱法测定微量元素,当分析含镉浓度极低的样品时则使用电热原子吸收光谱法。在以下条件下从五种海洋标准物质中获得了铜、锌和镉的定量回收率:600瓦,2分钟;0瓦,2分钟;450瓦,45分钟。