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首页> 外文期刊>Journal of near infrared spectroscopy >Quantitative in-line analysis in supercritical CO{sub}2 using fibre-optic NIR spectroscopy and multivariate calibration: a potential method for monitoring continuous flow processes
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Quantitative in-line analysis in supercritical CO{sub}2 using fibre-optic NIR spectroscopy and multivariate calibration: a potential method for monitoring continuous flow processes

机译：使用光纤近红外光谱和多元校准对超临界CO {sub} 2进行在线定量分析：监测连续流过程的潜在方法

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摘要

A set-up for fibre-optical in-line near infrared spectroscopic monitoring of hydrocarbons in supercritical CO{sub}2 has been developed, which can be operated under flow-through conditions. It consists of a high-pressure optical cell, which is adapted to an FT-NIR spectrometer via a fibre-optic interface. NIR spectra of squalane in supercritical CO{sub}2 have been measured for varying concentration, temperature and pressure conditions. A partial least squares (PLS) regression model was developed with a calibration set of 36 samples spanning the 0.32 × 10{sup}(-3) g cm{sup}(-3) squalane concentration range and with CO{sub}2 densities between 0.62-0.86 g cm{sup}(-3). Based on the corresponding absorbance data in the 4900-4200 cm{sup}(-1) spectral range, squalane and CO{sub}2 were modelled with standard deviations of 0.24-10{sup}(-3) and 3.8 × 10{sup}(-3) g cm{sup}(-3), respectively. Comparable standard deviations were obtained by validating the model with independent test samples. The developed calibration models allow for the in-line quantification of both constituents under varying temperature and pressure conditions from a single spectral measurement. The results obtained encourage the use of NIR spectroscopy/PLS calibration for fast in-line analysis of continuous flow extraction processes for the deoiling of metal parts based on supercritical CO{sub}2.
机译：已经开发了用于对超临界CO {sub} 2中的碳氢化合物进行光纤在线近红外光谱监测的装置，该装置可以在流通条件下运行。它由高压光学元件组成，该元件通过光纤接口与FT-NIR光谱仪匹配。对于变化的浓度，温度和压力条件，已测量了超临界CO {sub} 2中角鲨烷的NIR光谱。开发了偏最小二乘（PLS）回归模型，其中包含36个样本的校准集，其范围为0.32×10 {sup}（-3）g cm {sup}（-3）角鲨烷浓度范围，并且具有CO {sub} 2密度在0.62-0.86 g cm {sup}（-3）之间。根据4900-4200 cm {sup}（-1）光谱范围内的相应吸光度数据，对角鲨烷和CO {sub} 2进行建模，其标准偏差为0.24-10 {sup}（-3）和3.8×10 { sup}（-3）g cm {sup}（-3）。通过使用独立的测试样本验证模型，获得了可比的标准偏差。开发的校准模型可通过单次光谱测量在变化的温度和压力条件下在线定量两种成分。获得的结果鼓励使用NIR光谱/ PLS校准对基于超临界CO {sub} 2的金属零件脱油的连续流萃取过程进行快速在线分析。

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