Development and validation of an analytical method for hydrocarbon residues using gas chromatography-mass spectrometry

Aree Choodum, Niamh Nic Daeid

Research output: Contribution to journalArticle

7 Citations (Scopus)

Abstract

This work outlines the development of a gas chromatographic mass spectrometric (GCMS) method for the analysis of hydrocarbon residues such as those encountered in the examination of fire debris. The work compares favourably against an existing ASTM E-1618-06 method for ignitable liquid analysis currently used for the development of the National Centre for Forensic Science (NCFS) ignitable liquid database. A test mixture comprising fourteen hydrocarbons as recommended by the ASTM-1618-06 method was used to evaluate and validate the separation conditions together with a matrix matched ignitable liquid mixture diluted to 2 mu L mL(-1) in dichloromethane. Optimised conditions were as follows: injection volume of 1 mu L with split ratio 50 to 1 at inlet temperature 280 degrees C, carrier gas flow rate was set as 1.0 mL min(-1), the column temperature was maintained at 40 degrees C for 3 minutes, then increased at a rate of 12.5 degrees C min(-1) to 290 degrees C, and held for 4 minutes. Undiluted ignitable liquid samples (50% gasoline : diesel) were also analysed with a high split ratio (300 : 1) and low injection volume (0.2 mu L) to avoid column overloading and to eliminate any difficulties associated with solvent masking. This method provided improved separation and sensitivity compared to the ASTM method. Excellent precision both intra-day and inter-day (<3% RSD for peak area) was also obtained. The stability of ignitable liquid storage was also investigated over a two week period for various types of vials and septa.

LanguageEnglish
Pages1136-1142
Number of pages7
JournalAnalytical Methods
Volume3
Issue number5
DOIs
Publication statusPublished - May 2011

Fingerprint

Hydrocarbons
Gas chromatography
Mass spectrometry
Liquids
Intake systems
Methylene Chloride
Dichloromethane
Debris
Gasoline
Flow of gases
Fires
Gases
Flow rate
Temperature

Keywords

  • automorive gasoline samples
  • carbon disulfide
  • gas chromatographic mass spectrometric

Cite this

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abstract = "This work outlines the development of a gas chromatographic mass spectrometric (GCMS) method for the analysis of hydrocarbon residues such as those encountered in the examination of fire debris. The work compares favourably against an existing ASTM E-1618-06 method for ignitable liquid analysis currently used for the development of the National Centre for Forensic Science (NCFS) ignitable liquid database. A test mixture comprising fourteen hydrocarbons as recommended by the ASTM-1618-06 method was used to evaluate and validate the separation conditions together with a matrix matched ignitable liquid mixture diluted to 2 mu L mL(-1) in dichloromethane. Optimised conditions were as follows: injection volume of 1 mu L with split ratio 50 to 1 at inlet temperature 280 degrees C, carrier gas flow rate was set as 1.0 mL min(-1), the column temperature was maintained at 40 degrees C for 3 minutes, then increased at a rate of 12.5 degrees C min(-1) to 290 degrees C, and held for 4 minutes. Undiluted ignitable liquid samples (50{\%} gasoline : diesel) were also analysed with a high split ratio (300 : 1) and low injection volume (0.2 mu L) to avoid column overloading and to eliminate any difficulties associated with solvent masking. This method provided improved separation and sensitivity compared to the ASTM method. Excellent precision both intra-day and inter-day (<3{\%} RSD for peak area) was also obtained. The stability of ignitable liquid storage was also investigated over a two week period for various types of vials and septa.",
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Development and validation of an analytical method for hydrocarbon residues using gas chromatography-mass spectrometry. / Choodum, Aree; Daeid, Niamh Nic.

In: Analytical Methods, Vol. 3, No. 5, 05.2011, p. 1136-1142.

Research output: Contribution to journalArticle

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