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首页> 外文期刊>Crystal growth & design >A comparative study of ATR-FTIR and FT-NIR spectroscopy for in-situ concentration monitoring during batch cooling crystallization processes
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A comparative study of ATR-FTIR and FT-NIR spectroscopy for in-situ concentration monitoring during batch cooling crystallization processes

机译：ATR-FTIR和FT-NIR光谱用于间歇冷却结晶过程中原位浓度监测的比较研究

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摘要

Crystallization is a widely used separation and purification process in the chemical industry. The final product properties such as the crystal size distribution and the morphology are largely defined during this process. In order to achieve proper control over the crystallization process, accurate in situ measurements are necessary. This paper presents the assessment of in situ infrared spectroscopic techniques for solute concentration measurements. It presents a comparative study of attenuated total reflectance (ATR), Fourier transform infrared (FTIR), and Fourier transform (FT) near infrared (NIR) spectroscopy for batch cooling crystallization of four different crystallization systems. These two techniques were compared based on the partial least square models developed by extensive calibration in the laboratory, the independent data sets generated while determining saturation concentrations in the presence of crystals and monitoring the batch cooling crystallization processes. The ATR-FTIR spectroscopy was found to perform better statistically and also in the presence of crystals. The FT-NIR spectroscopy was less reliable as the probe head was more susceptible to scaling. The average relative error in predicting the solubilities in the presence of crystals was sensitive to the crystallizing system and was on the order to 2% for ATR-FTIR while it was much higher for FT-NIR.
机译：结晶是化学工业中广泛使用的分离和纯化方法。在此过程中，主要定义了最终产品的性能，例如晶体尺寸分布和形态。为了实现对结晶过程的适当控制，必须进行准确的原位测量。本文介绍了用于溶质浓度测量的原位红外光谱技术的评估。它提供了衰减全反射率（ATR），傅立叶变换红外（FTIR）和傅立叶变换（FT）近红外（NIR）光谱的比较研究，用于四个不同结晶系统的批量冷却结晶。基于在实验室中通过广泛校准开发的偏最小二乘模型，对这两种技术进行了比较，生成了独立的数据集，同时确定了晶体存在下的饱和浓度并监控了分批冷却的结晶过程。发现ATR-FTIR光谱在统计学上以及在晶体存在下表现更好。 FT-NIR光谱的可靠性较差，因为探头更容易结垢。预测存在晶体时的溶解度的平均相对误差对结晶系统敏感，对于ATR-FTIR约为2％，而对于FT-NIR则要高得多。

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