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A case study for in-house method validation of gas chromatography technique using class-1 calibration gas mixtures for greenhouse gases monitoring

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Abstract

In this study, analytical method validation has been done for the measurement of carbon dioxide/nitrogen (CO2/N2) and methane/nitrogen (CH4/N2) calibration gas mixtures using gas chromatography with flame ionization detector (GC-FID). Class-I calibration gas mixtures (CGMs) of CO2 (500 µmol mol−1 to 1100 µmol mol−1) and CH4 (2 µmol mol−1 to 130 µmol mol−1) used in method validation process has been prepared gravimetrically following ISO 6142-1. All prepared gas mixtures have expanded uncertainty 1 % at coverage factor (k) of 2 with 95 % confidence. The following parameters are chosen for this case study which include selectivity, accuracy, precision, linearity, limit of detection (LOD), limit of quantification (LOQ), robustness, stability, and uncertainty. Different statistical approaches are taken into consideration for each parameter assessment. The results indicate that GC-FID is selective for CO2 and CH4. CGMs represent good repeatability and reproducibility having percentage relative deviation < 1 % among measurements. A good linear behaviour was observed for CGMs of CH4 and CO2 on basis of least square regression with R2 value 0.9995 and 1, respectively. LOD and LOQ for CH4 are calculated 0.47 and 1.59 µmol mol−1 based on signal-to-noise ratio by taking its lowest concentration of 2.9 µmol mol−1. The in-house validated method for GC-FID using CGMs for the measurement of greenhouse gases (CO2 and CH4) is found to be precise, accurate and fit for purpose.

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Data availability

The data supporting the findings of this study are available from the corresponding author on request.

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Acknowledgements

The author, Komal is thankful to Council of Scientific and Industrial Research (CSIR) for providing the fellowship under CSIR-SRF scheme (P- 81-101). Authors are thankful to the Director, CSIR-NPL for providing all support to carry out gas metrology work and further extend their thanks to Head of ESBM Division and Gas Metrology group members for their help and support.

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Authors and Affiliations

  1. CSIR-National Physical Laboratory, Dr. KS Krishnan Marg, New Delhi, 110012, India

    Komal, Daya Soni & Shankar G. Aggarwal

  2. Academy of Scientific and Innovative Research (AcSIR), Ghaziabad, 201002, India

    Komal, Daya Soni & Shankar G. Aggarwal

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  1. Komal
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Contributions

Ms. Komal did all the experimental analysis, data curation and writing manuscript. Dr Daya Soni supervised in all experimental part , constructing the manuscript and data processing. Dr. Shankar G. Aggarwal reviewed the manuscript.

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Correspondence to Daya Soni.

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Komal, Soni, D. & Aggarwal, S.G. A case study for in-house method validation of gas chromatography technique using class-1 calibration gas mixtures for greenhouse gases monitoring. Accred Qual Assur 28, 209–220 (2023). https://doi.org/10.1007/s00769-023-01552-z

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