Inline process monitoring of moisture content in tetrahydrofuran
Applications | 2022 | MetrohmInstrumentation
Solvent recovery is key for cost savings and environmental compliance in chemical and pharmaceutical production. Tetrahydrofuran (THF) is widely used but hygroscopic, making moisture control critical to ensure product quality and process efficiency.
This study demonstrates an inline near-infrared spectroscopy (NIRS) method for real-time monitoring of low-level moisture in recovered THF streams using the Metrohm 2060 The NIR-REx Analyzer.
NIRS measurements were performed in transmission mode over 1000–2250 nm with a 10 mm flow cell connected to the 2060 The NIR-REx Analyzer. A calibration model was built using 28 THF samples (20–500 mg/L water) referenced by Karl Fischer titration, and validated with 10 external samples. Partial least squares regression (PLS) with two factors and first derivative pretreatment (gap-segment: 11.5 nm gap, 1.5 nm segment) was used for quantification.
The NIRS model achieved high accuracy (R2 = 0.999) with a standard error of calibration (SEC) of 3.79 mg/L, cross-validation error (SECV) of 4.01 mg/L, and external prediction error (SEP) of 5.19 mg/L. Spectral changes correlate closely with KF reference values, confirming reliable inline moisture measurement.
The 2060 The NIR-REx Analyzer features an explosion-proof design with ATEX and IECEx certification, supporting up to five fiber-optic probes or flow cells. Its purge/pressurization system ensures safe operation in classified areas.
Inline NIRS will expand to monitor additional solvent impurities and process parameters simultaneously. Integration with digital twins and advanced chemometric algorithms will further enhance predictive process control and continuous manufacturing.
The inline NIRS approach with the 2060 The NIR-REx Analyzer provides fast, accurate, and robust moisture determination in THF recovery streams, replacing time-consuming laboratory methods and improving overall process performance.
NIR Spectroscopy
IndustriesEnergy & Chemicals
ManufacturerMetrohm
Summary
Importance of the Topic
Solvent recovery is key for cost savings and environmental compliance in chemical and pharmaceutical production. Tetrahydrofuran (THF) is widely used but hygroscopic, making moisture control critical to ensure product quality and process efficiency.
Aim and Study Overview
This study demonstrates an inline near-infrared spectroscopy (NIRS) method for real-time monitoring of low-level moisture in recovered THF streams using the Metrohm 2060 The NIR-REx Analyzer.
Methodology and Instrumentation
NIRS measurements were performed in transmission mode over 1000–2250 nm with a 10 mm flow cell connected to the 2060 The NIR-REx Analyzer. A calibration model was built using 28 THF samples (20–500 mg/L water) referenced by Karl Fischer titration, and validated with 10 external samples. Partial least squares regression (PLS) with two factors and first derivative pretreatment (gap-segment: 11.5 nm gap, 1.5 nm segment) was used for quantification.
Main Results and Discussion
The NIRS model achieved high accuracy (R2 = 0.999) with a standard error of calibration (SEC) of 3.79 mg/L, cross-validation error (SECV) of 4.01 mg/L, and external prediction error (SEP) of 5.19 mg/L. Spectral changes correlate closely with KF reference values, confirming reliable inline moisture measurement.
Benefits and Practical Applications
- Real-time, nondestructive moisture monitoring without sample preparation
- Reduced manual sampling and exposure to hazardous chemicals
- Improved process control, product quality, and return on investment
- Automated analysis supports multiple plant locations via remote fiber-optic probes
Instrumentation Used
The 2060 The NIR-REx Analyzer features an explosion-proof design with ATEX and IECEx certification, supporting up to five fiber-optic probes or flow cells. Its purge/pressurization system ensures safe operation in classified areas.
Future Trends and Applications
Inline NIRS will expand to monitor additional solvent impurities and process parameters simultaneously. Integration with digital twins and advanced chemometric algorithms will further enhance predictive process control and continuous manufacturing.
Conclusion
The inline NIRS approach with the 2060 The NIR-REx Analyzer provides fast, accurate, and robust moisture determination in THF recovery streams, replacing time-consuming laboratory methods and improving overall process performance.
References
- Markets and Markets. Tetrahydrofuran (THF) Market; CH 6125; 2018.
Content was automatically generated from an orignal PDF document using AI and may contain inaccuracies.
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