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Quantitative Analysis of MEA-Triazine Hydrogen Sulfide Scavengers Through Innovative Transmission FTIR Spectroscopy

Applications | 2024 | Agilent TechnologiesInstrumentation
FTIR Spectroscopy
Industries
Energy & Chemicals
Manufacturer
Agilent Technologies

Summary

Importance of the Topic


Hydrogen sulfide (H₂S) contamination in oil and gas streams poses serious safety, environmental, and operational risks. Monoethanolamine-triazine (MEA-triazine) is widely used to scavenge H₂S, but accurate determination of its concentration in viscous aqueous solutions remains challenging. Conventional techniques—such as Kjeldahl digestion, ion-exchange chromatography, and gas chromatography—are often time-consuming, labor intensive, and prone to error. A rapid, robust analytical approach is essential for quality control in both laboratory and field environments.

Objectives and Study Overview


This study aimed to develop and validate a mid-infrared (mid-IR) transmission FTIR method using the Agilent Cary 630 spectrometer equipped with a DialPath accessory. Key objectives included:
  • Establishing a calibration model for MEA-triazine in water over a broad concentration range.
  • Evaluating method linearity, precision, and accuracy.
  • Assessing the impact of common viscosity-reducing additives (methanol, isopropyl alcohol) on quantification.

Methodology


Calibration and interference samples were prepared as follows:
  • Calibration standards: MEA-triazine in water at 15, 20, 25, 30, 40, 50, 60, and 75 % w/w.
  • Interference sets: 25 % and 50 % MEA-triazine with added MeOH or IPA at 10, 15, and 25 % v/v.
  • Spectra acquisition: 32 scans, 4 cm⁻¹ resolution, 4000–650 cm⁻¹, 50 µm path length, 7 µL sample volume.
  • Quantification metric: peak area between 1284.07 and 1203.93 cm⁻¹, reflecting characteristic triazine absorbance.

Instrumentation


The analysis employed:
  • Agilent Cary 630 FTIR spectrometer with ZnSe optics.
  • DialPath transmission module offering three selectable path lengths.
  • Agilent MicroLab Quant software for automated calibration curve generation, cross-validation, and independent-set prediction.

Main Results and Discussion


The method exhibited excellent linearity (R² = 0.9993) across the calibration range. Cross-validation yielded a standard error of 0.116 %.

Interference study findings:
  • Methanol addition caused a slight negative bias in measured MEA-triazine, with maximum deviation of 0.98 % at 25 % MeOH for a 25 % MEA sample and 4.36 % at 25 % MeOH for a 50 % sample.
  • Isopropyl alcohol induced a positive bias, up to 5.78 % deviation at 25 % IPA for the 25 % sample and 6.55 % for the 50 % sample.
  • Spectral overlays revealed an IPA-induced new band at 1325–1275 cm⁻¹, whereas MeOH only attenuated water-related absorptions.

The DialPath design minimized common errors—eliminating leaks, bubbles, and complex cell assembly—and high repeatability was achieved even with viscous solutions.

Benefits and Practical Applications


This FTIR-based approach offers:
  • Rapid analysis (<5 minutes per sample) with minimal sample volume.
  • Reduced susceptibility to pipetting and solvent-handling errors.
  • Flexible path length adjustment to limit water absorption interferences.
  • High throughput enabled by quick window cleaning and automated software routines.

These advantages suit both routine laboratory QC and potential on-site process monitoring.

Future Trends and Opportunities


Potential developments include:
  • Expanded calibration models that account for mixed-solvent matrices.
  • Inline or at-line FTIR probes for real-time scavenger monitoring.
  • Application of multivariate chemometric techniques to enhance selectivity in complex matrices.
  • Adaptation of the method for other amine-based scavengers or contaminants in process streams.

Conclusion


The Agilent Cary 630 FTIR with DialPath module, combined with MicroLab Quant software, provides a fast, accurate, and user-friendly method for quantifying MEA-triazine in aqueous solutions. It overcomes limitations of traditional analytical techniques, delivers high precision, and streamlines workflow, making it well suited for industrial quality control and process monitoring.

References


  1. Agbroko O.; Piler K.; Benson T. A Comprehensive Review of H₂S Scavenger Technologies from Oil and Gas Streams. ChemBioEng Rev. 2017;4(6):339–359.
  2. Wylde J.J.; Taylor G.N.; Sorbie K.S.; Samaniego W.N. Formation, Chemical Characterization, and Oxidative Dissolution of Amorphous Polymeric Dithiazine during the Use of the H₂S Scavenger Monoethanolamine-Triazine. Energy Fuels. 2020;34(8):9923–9931.
  3. Benhabib M.; Kleinman S.L.; Peterman M.C. Quantitative Analysis of Triazine-Based H₂S Scavengers via Raman Spectroscopy. Ind Eng Chem Res. 2021;60(44):15936–15941.
  4. Nunes Ferreira F.; Carlos Afonso J.; Veronesi Marinho Pontes F.; Castro Carneiro M.; Alcover Neto A.; Luiza Bragança Tristão M.; Inês Couto Monteiro M. Determination of Low-Molecular-Weight Amines and Ammonium in Saline Waters by Ion Chromatography After Their Extraction by Steam Distillation. J Sep Sci. 2016;39(8):1454–1460.
  5. Wystrach V.P.; Kaiser D.W.; Schaefer F.C. Preparation of Ethylenimine and Triethylenemelamine. J Am Chem Soc. 1955;77(22):5915–5918.
  6. Wylde J.J.; Taylor G.N.; Sorbie K.S.; Samaniego W.N. Scavenging Alkyl Mercaptans: Elucidation of Reaction Mechanisms and Byproduct Characterization. Energy Fuels. 2020;34(11):13883–13892.

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