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作 者:郭弘艺[1] 张旭光[1] 邵露[1] 殷曦敏[1]
机构地区:[1]上海海洋大学农业部淡水水产种质资源重点实验室,上海201306
出 处:《实验室研究与探索》2015年第5期24-26,共3页Research and Exploration In Laboratory
基 金:上海高校实验技术队伍建设计划(B1-5407-13-0000-1)
摘 要:研究能谱仪在鱼类耳石微化学分析中的应用,探索一套适用于鱼类耳石标准样品定量分析实验条件.结果表明,样品表面粗糙会对特征X射线产生几何效应,使得分析强度降低,造成实验结果误差.耳石样本最适用烘干干燥法,其操作过程为:耳石放入干净培养皿后,在恒温烤箱60℃烘干6~8h.样品干燥后,表面喷金待用.为获得精确的分析结果,实验参数应根据样品大小,实验目的所需要关注的组成元素和仪器性能来选择.加速电压Uo一般为临界激发电压Uk的2~10倍.最适工作距离为20 mm,单点扫描活时间为200 s以上,死时间10%~15%.聚焦参数应该根据耳石样品不同的大小选择,尽可能兼顾缩短测量时间和保证足够的空间分辨率.This paper studies the application of spectrometer in fish otolith microchemistry analysis, and explores a set of experiment conditions for quantitative analysis of fish otolith standard samples. For electron microprobe analysis the otoliths were ground into uniform thickness chips, then dried at 60℃ constant-temperature oven for 6-8 hours, and finally gold coated in a high-vacuum evaporator. In order to ensure the aecuracy of experimental results, experiment parameters should be determined in accordance with otolith size, experimental objective for key composition of fish otolith and instrument perfnrmance. Accelerating voltage must be higher than X-ray critical excitation woltage of all element properties measured, which is more than 2 times and Jess than 10 times of eritical excitation voltage Uk in general cases. The optimal working distance is 20 mm, with live time of over 200 s and deadtime between 10% -15% in single scan. Focusing parameters should be determined on line with otolith sample size, with full considerations to a short measurement time and sufficient spatial resolution.
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