Copyright (c) 2026 Abdullah S. AlOwaysi, Abdulrahman R. AlAskar, Adel B. Shehata

This work is licensed under a Creative Commons Attribution 4.0 International License.
Preparation and Certification of Propane in Nitrogen as Reference Material for Ensuring Traceability of Hydrocarbon Emission Measurements
Corresponding Author(s) : Adel B. Shehata
Asian Journal of Chemistry,
Vol. 38 No. 10 (2026): Vol 38, Issue 10, 2026
Abstract
Propane in nitrogen (C3H8/N2) gas mixtures are widely used as calibration standards for hydrocarbon measurements in environmental monitoring, energy production and industrial process control. Five C3H8/N2 gas mixtures, covering the range of 804.8148-12053.8148 µmol/mol, were gravimetrically prepared according to ISO 6142 using a two-step dilution approach with high-purity propane and nitrogen. The prepared mixtures were validated by gas chromatography with flame ionization detection (GC-FID) in accordance with ISO 6143. The GC-FID results showed good agreement with the gravimetric values, confirming the validity of the preparation method. The certified values determined by gravimetry were established for 4 mixtures (B, C, D, E) as 12053.81 ± 97.49, 9013.23 ± 78.11, 5998.011 ± 57.72 and 2987.29 ± 66.91 µmol/mol, respectively. The mole fraction of the mixture F, 804.81 ± 35.97 µmol/mol was considered an information value since it was associated with large uncertainty of 7.016%. The performance of the produced certified reference materials (CRMs) was checked by using them to calibrate the GC-FID, then measure a CRM sample of 8010 µmol/mol as an unknown. The precision (%RSD) and accuracy of the measured results were found to be 0.12% and 99.75%, respectively. These results confirm that the prepared C3H8/N2 mixtures meet the criteria for certified reference materials and are suitable as calibrants for hydrocarbon emission measurement instruments in industrial gas analysis and environmental monitoring.
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- B.D. Skrbic and M.J. Zlatkovic, Chromatographia, 17, 44 (1983); https://doi.org/10.1007/BF02265109
- A.B. Shehata, A.R. AlAskar, N.H. AlYami and A.S. AlOwaysi, Green Sustain. Chem., 13, 269 (2023); https://doi.org/10.4236/gsc.2023.134015
- E.C. de Oliveira, Metrol. Meas. Syst., 19, 405 (2012); https://doi.org/10.2478/v10178-012-0035-6
- ISO, ISO 6974-3:2001, Natural Gas Determination of Composition with Defined Uncertainty by Gas Chromatography, Part 3: Deter-mination of Hydrogen, Helium, Oxygen, Nitrogen, Carbon Dioxide and Hydrocarbons up to C-8 using Two Packed Columns (2001); https://www.iso.org/standard/25854.html
- T.J. Lechner-Fish, Enhanced Performance of an Integrated Gas Chromatograph for On-Line Natural Gas Analysis, 4th International Symposium on Fluid Flow Measurement, Denver, 27-30 June (1999); https://es.studenta.com/content/111273256/14-02-gas-cromatographs-cesar-delgado
- H. Budiman, Nuryatini and O. Zuas, Procedia Chem., 16, 465 (2015); https://doi.org/10.1016/j.proche.2015.12.080
- M.F. Barbosa, J.R.B. Santos, A.N. Silva, S.F.C. Soares and M.C.U. Araujo, Microchem. J., 170, 106752 (2021); https://doi.org/10.1016/j.microc.2021.106752
- O. Zuas and H. Budiman, Hem. Ind., 70, 451 (2016); https://doi.org/10.2298/HEMIND150315051Z
- G.C. Rhoderick, J. Chromatogr. A, 1017, 131 (2003); https://doi.org/10.1016/j.chroma.2003.08.002
- C.J. Cowper, J. Chromatogr. A, 56, 1 (1995); https://doi.org/10.1016/S0301-4770(08)61280-4
- G.C. Rhoderick, J. Chromatogr. A, 1187, 226 (2008); https://doi.org/10.1016/j.chroma.2008.01.087
- A.S. Brown, M.J.T. Milton, C.J. Cowper, G.D. Squire, W. Bremser and R.W. Branch, J. Chromatogr. A, 1040, 215 (2004); https://doi.org/10.1016/j.chroma.2004.04.007
- J.S. Barrabin, B.C. Garrido, G.A. Machado, W. Wollinger, R.F.M. Freitas, A.C.S. Feliciano and M.N.S. De la Cruz, Accredit. Qual. Assur., 20, 483 (2015); https://doi.org/10.1007/s00769-015-1168-6
- JCGM, International Vocabulary of Metrology, Basic and General Concepts and Associated Terms (VIM), JCGM 200:2012, BIPM, IEC, IFCC, ILAC, ISO, IUPAC, IUPAP and OIML, edn 3 (2012): https://www.bipm.org/documents/20126/2071204/JCGM_200_2012.pdf
- ISO, ISO 6142-1:2015, Gas Analysis: Preparation of Calibration Gas Mixtures-Part 1: Gravimetric Method for Class I Mixtures (2015); https://www.iso.org/standard/59631.html
- ISO, ISO 6143:2025, Gas Analysis: Comparison Methods for Determining and Checking the Composition of Calibration Gas Mixtures (2025); https://www.iso.org/standard/85579.html
- ISO, ISO 19229:2019, Gas Analysis-Purity Analysis and the Treat-ment of Purity Data, edn 1 (2019); https://www.iso.org/standard/72010.html
- A. Alink, Metrologia, 37, 35 (2000); https://doi.org/10.1088/0026-1394/37/1/5
- A.M.H. van der Veen and M.G. Cox, Metrologia, 40, 18 (2003); https://doi.org/10.1088/0026-1394/40/2/303
- ISO, ISO 17034:2016, General Requirements for the Competence of Reference Material Producers (2016); https://www.iso.org/standard/29357.html
- A.B. Shehata, A.R. AlAskar, N.H. AlYami and A.S. AlOwaysi, Acta IMEKO, 14, 1 (2025); https://doi.org/10.21014/actaimeko.v14i1.1945
- A.B. Shehata, N.H. AlYami, A.S. AlOwaysi and A.R. Alaskar, J. Chem. Metrol., 15, 11 (2021); https://doi.org/10.25135/jcm.58.21.04.2055
- A.B. Shehata, A.R. AlAskar, N.H. AlYami and A.S. AlOwaysi, Sci. J. Chem., 10, 133 (2022).
- ISO, ISO 33405:2024, Reference Materials, Approaches for Charact-erization and Assessment of Homogeneity and Stability (2024); https://www.iso.org/standard/84226.html
- NIST, Certificate of Analysis: Standard Reference Material 2644a, Propane in Nitrogen (2022); https://tsapps.nist.gov/srmext/certificates/2644a.pdf
- NIST, Certificate of Analysis: Standard Reference Material 1665b, Propane in Air (2024); https://tsapps.nist.gov/srmext/certificates/1665b.pdf
- Eurachem, The Fitness for Purpose of Analytical Methods: A Laboratory Guide to Method Validation and Related Topics, edn 3 (2025); https://www.eurachem.org/index.php/publications/guides/mv
- ISO 13528 Statistical Methods for Use in Proficiency Testing by interlaboratory comparison (2022); https://www.iso.org/standard/78879.html
References
B.D. Skrbic and M.J. Zlatkovic, Chromatographia, 17, 44 (1983); https://doi.org/10.1007/BF02265109
A.B. Shehata, A.R. AlAskar, N.H. AlYami and A.S. AlOwaysi, Green Sustain. Chem., 13, 269 (2023); https://doi.org/10.4236/gsc.2023.134015
E.C. de Oliveira, Metrol. Meas. Syst., 19, 405 (2012); https://doi.org/10.2478/v10178-012-0035-6
ISO, ISO 6974-3:2001, Natural Gas Determination of Composition with Defined Uncertainty by Gas Chromatography, Part 3: Deter-mination of Hydrogen, Helium, Oxygen, Nitrogen, Carbon Dioxide and Hydrocarbons up to C-8 using Two Packed Columns (2001); https://www.iso.org/standard/25854.html
T.J. Lechner-Fish, Enhanced Performance of an Integrated Gas Chromatograph for On-Line Natural Gas Analysis, 4th International Symposium on Fluid Flow Measurement, Denver, 27-30 June (1999); https://es.studenta.com/content/111273256/14-02-gas-cromatographs-cesar-delgado
H. Budiman, Nuryatini and O. Zuas, Procedia Chem., 16, 465 (2015); https://doi.org/10.1016/j.proche.2015.12.080
M.F. Barbosa, J.R.B. Santos, A.N. Silva, S.F.C. Soares and M.C.U. Araujo, Microchem. J., 170, 106752 (2021); https://doi.org/10.1016/j.microc.2021.106752
O. Zuas and H. Budiman, Hem. Ind., 70, 451 (2016); https://doi.org/10.2298/HEMIND150315051Z
G.C. Rhoderick, J. Chromatogr. A, 1017, 131 (2003); https://doi.org/10.1016/j.chroma.2003.08.002
C.J. Cowper, J. Chromatogr. A, 56, 1 (1995); https://doi.org/10.1016/S0301-4770(08)61280-4
G.C. Rhoderick, J. Chromatogr. A, 1187, 226 (2008); https://doi.org/10.1016/j.chroma.2008.01.087
A.S. Brown, M.J.T. Milton, C.J. Cowper, G.D. Squire, W. Bremser and R.W. Branch, J. Chromatogr. A, 1040, 215 (2004); https://doi.org/10.1016/j.chroma.2004.04.007
J.S. Barrabin, B.C. Garrido, G.A. Machado, W. Wollinger, R.F.M. Freitas, A.C.S. Feliciano and M.N.S. De la Cruz, Accredit. Qual. Assur., 20, 483 (2015); https://doi.org/10.1007/s00769-015-1168-6
JCGM, International Vocabulary of Metrology, Basic and General Concepts and Associated Terms (VIM), JCGM 200:2012, BIPM, IEC, IFCC, ILAC, ISO, IUPAC, IUPAP and OIML, edn 3 (2012): https://www.bipm.org/documents/20126/2071204/JCGM_200_2012.pdf
ISO, ISO 6142-1:2015, Gas Analysis: Preparation of Calibration Gas Mixtures-Part 1: Gravimetric Method for Class I Mixtures (2015); https://www.iso.org/standard/59631.html
ISO, ISO 6143:2025, Gas Analysis: Comparison Methods for Determining and Checking the Composition of Calibration Gas Mixtures (2025); https://www.iso.org/standard/85579.html
ISO, ISO 19229:2019, Gas Analysis-Purity Analysis and the Treat-ment of Purity Data, edn 1 (2019); https://www.iso.org/standard/72010.html
A. Alink, Metrologia, 37, 35 (2000); https://doi.org/10.1088/0026-1394/37/1/5
A.M.H. van der Veen and M.G. Cox, Metrologia, 40, 18 (2003); https://doi.org/10.1088/0026-1394/40/2/303
ISO, ISO 17034:2016, General Requirements for the Competence of Reference Material Producers (2016); https://www.iso.org/standard/29357.html
A.B. Shehata, A.R. AlAskar, N.H. AlYami and A.S. AlOwaysi, Acta IMEKO, 14, 1 (2025); https://doi.org/10.21014/actaimeko.v14i1.1945
A.B. Shehata, N.H. AlYami, A.S. AlOwaysi and A.R. Alaskar, J. Chem. Metrol., 15, 11 (2021); https://doi.org/10.25135/jcm.58.21.04.2055
A.B. Shehata, A.R. AlAskar, N.H. AlYami and A.S. AlOwaysi, Sci. J. Chem., 10, 133 (2022).
ISO, ISO 33405:2024, Reference Materials, Approaches for Charact-erization and Assessment of Homogeneity and Stability (2024); https://www.iso.org/standard/84226.html
NIST, Certificate of Analysis: Standard Reference Material 2644a, Propane in Nitrogen (2022); https://tsapps.nist.gov/srmext/certificates/2644a.pdf
NIST, Certificate of Analysis: Standard Reference Material 1665b, Propane in Air (2024); https://tsapps.nist.gov/srmext/certificates/1665b.pdf
Eurachem, The Fitness for Purpose of Analytical Methods: A Laboratory Guide to Method Validation and Related Topics, edn 3 (2025); https://www.eurachem.org/index.php/publications/guides/mv
ISO 13528 Statistical Methods for Use in Proficiency Testing by interlaboratory comparison (2022); https://www.iso.org/standard/78879.html