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Online Continuous Trace Process Analytics Using Multiplexing Gas Chromatography.

Marco R Wunsch1, Rudolf Lehnig1, Oliver Trapp2

  • 1BASF SE , Carl-Bosch-Str. 38, 67056 Ludwigshafen, Germany.

Analytical Chemistry
|March 10, 2017
PubMed
Summary
This summary is machine-generated.

Multiplexing gas chromatography (mpGC) enhances trace impurity analysis in industrial settings. This novel technique improves signal-to-noise ratio by 10x, enabling detection of benzene, toluene, ethylbenzene, and xylene (BTEX) at 1 ppb levels in CO2 streams.

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Area of Science:

  • Analytical Chemistry
  • Process Analytics
  • Chemical Engineering

Background:

  • Trace analysis of impurities is critical for product safety in chemical, food, and pharmaceutical industries.
  • Analyzing low-concentration analytes in the presence of high-concentration matrix components presents significant challenges due to signal suppression and detector range limitations.
  • Existing methods struggle with accurate quantification of trace impurities when major components dominate the sample matrix.

Purpose of the Study:

  • To develop and validate a continuous, automated trace analysis technique for industrial process streams.
  • To enable precise quantification of benzene, toluene, ethylbenzene, and xylene (BTEX) at parts-per-billion (ppb) levels within a carbon dioxide (CO2) matrix.
  • To overcome limitations of conventional gas chromatography in handling complex samples with high-dynamic range components.

Main Methods:

  • Implementation of multiplexing gas chromatography (mpGC) with a flame ionization detector (FID) for automated, continuous analysis.
  • Utilizing pseudorandom binary sequence (PRBS) injection patterns for sample introduction into the gas chromatograph.
  • Applying Hadamard transformation for deconvolution of superimposed chromatograms and noise suppression.
  • Development of novel algorithms to maintain detector data acquisition rates and mitigate correlation noise.

Main Results:

  • Achieved a 10-fold increase in signal-to-noise ratio compared to conventional GC-FID.
  • Lowered detection limits for BTEX impurities in CO2 from 10 ppb to 1 ppb.
  • Successfully quantified BTEX at 0-10 ppb levels despite the presence of methane and methanol at concentrations up to 100 ppm (approx. 1000 times higher).
  • Demonstrated robustness and reliability through a two-month field test in a chemical production plant.

Conclusions:

  • mpGC with Hadamard transformation offers a robust solution for automated, continuous trace impurity analysis in challenging industrial process streams.
  • The developed technique significantly enhances detection limits and accuracy for BTEX compounds in CO2, surpassing conventional GC-FID capabilities.
  • This method provides a reliable tool for ensuring product quality and safety in chemical manufacturing by enabling sensitive detection of critical impurities.