铝灰中氟及其浸出毒性的高通量测定方法研究
收稿日期: 2023-12-06
网络出版日期: 2024-09-26
基金资助
广东省环保专项资金项目(粤财资环［2023］12号)
Research on high throughput determination method of fluorine and leaching toxicity in aluminum ash
Received date: 2023-12-06
Online published: 2024-09-26
为解决铝灰中氟的现有检测标准操作繁琐、耗时长等问题，建立了粉末压片X射线荧光光谱法（XRF）测定铝灰中氟的含量，同时利用响应面法优化浸提液固比、浸出时间和浸提温度，提出快速浸提铝灰中氟的方法。结果表明，粉末压片XRF法测定铝灰中氟的检出限值为0.84 g/kg，样品平行测定相对偏差小于5%，测定结果与参考值的相对误差在±5%之内。采用SPSS 25.0中t检验法分析可知，粉末压片XRF法与标准方法的测定结果在统计学上无显著差异。通过加强固液界面传质过程，在液固比为20∶1（体积质量比，L/kg）、温度为（25±5） ℃条件下，搅拌浸提40 min后测定铝灰中可溶性氟的相对偏差小于5%，测定结果与标准浸提法有显著相关性，两种浸提方法的相对误差绝对值范围为2.25%~6.29%，接近响应面模型预测值。粉末压片XRF法和快速浸提方法测定结果稳定可靠，简化了前处理过程，有望实现铝灰中氟及其浸出毒性的高通量检测。
陈灿 , 曹俊 , 张永波 . 铝灰中氟及其浸出毒性的高通量测定方法研究[J]. 无机盐工业, 2024 , 56(8) : 104 -109 . DOI: 10.19964/j.issn.1006-4990.2023-0586
In order to address the issues of complicated operation and time⁃consuming of current determination standards，X-ray fluorescence spectrometry（XRF） with powder pressing was established to determine the fluorine content in aluminum ash.Meanwhile，the response surface method was used to optimize the liquid⁃solid ratio，leaching time and leaching temperature，and rapid extraction method for fluorine in aluminum ash was proposed.The results revealed that the detection limit of fluorine in aluminum ash by XRF with powder pressing was 0.84 g/kg，relative deviation of sample parallel determination was less than 5%，and the relative error between the measurement results and the reference value was within 5%.There was no statistically significant difference between power pressing XRF method and standard method by t test analysis in SPSS 25.0.Under the conditions of liquid⁃solid ratio of 20∶1 and temperature of （25±5） ℃，the relative deviation of soluble fluorine in aluminium ash was less than 5% after stirring extraction for 40 min by strengthening the solid⁃liquid interface mass transfer.The test results were significantly correlated with the standard extraction method.The absolute value of relative error between rapid extraction method and standard extraction method ranged from 2.25% to 6.29%，which was closed to the predicted value of the response surface model.The results of XRF with powder pressing and rapid extraction method were stable and reliable，which simplified the pretreatment process and expected to achieve high throughput determination of fluorine and leaching toxicity in aluminum ash.
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