3 years ago

Sulfur and Total Carboxylic Acid Number Determination in Vacuum Gas Oil by Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy

Sulfur and Total Carboxylic Acid Number Determination
in Vacuum Gas Oil by Attenuated Total Reflectance Fourier Transform
Infrared Spectroscopy
Anilkumar Savalia, Kalagouda B. Gudasi, Ramachandra Chakravarthy, Chandra Saravanan, Anurag Verma, Manjula Paramati, Asit Kumar Das
Sulfur removal is one of the key functions of vacuum gas oil (VGO) hydrotreating reactors. Knowing feed and product properties real-time or near-real-time improves reactor operations. The VGO section of crude distillation unit is also prone to severe high-temperature sulfidic and naphthenic acid corrosion. In this article, we evaluate a single-reflectance attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy as a possible quick and cost-effective methodology to determine total carboxylic acid number (TCAN) and total sulfur content of VGO. The study shows that single-reflectance diamond ATR crystal methodology has the right signal-to-noise ratio to accurately predict TCAN and total sulfur within the primary method’s repeatability. Statistical models have been developed using 64 sample sets of vacuum gas oil and out of which 10 samples were used for the cross-validation of the model. The range of TCAN in VGO samples used in this study was between 0.37 and 13.8 mg KOH/g, and sulfur content was between 0.8 to 5.4% by mass. Models have been evaluated by determining the correlation coefficient (R2), linearity curves obtained by plotting measured versus predicted values, and the errors associated with the prediction and cross-validation. The models showed a correlation coefficient of 0.9991 for TCAN and 0.9974 for total sulfur between reference and the measured values for calibration set of samples. A root-mean-square error of calibration (RMSEC) and prediction (RMSEP) for TCAN were found to be 0.0903 and 0.0885 mg KOH/g. Similarly, RMSEC and RMSEP values for sulfur content were 0.0829 and 0.107% by mass, respectively. The proposed methodology for the prediction of total sulfur and TCAN is fast, efficient, and cost-effective and has several advantages over the standard methods.

Publisher URL: http://dx.doi.org/10.1021/acs.energyfuels.7b03712

DOI: 10.1021/acs.energyfuels.7b03712

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