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TPH Methods

The document details the GC-MS characterization and qualitative analysis of Total Petroleum Hydrocarbons (TPHs) using a 1000ppm standard from AccuStandard and a five-point calibration method. It describes the calibration process, the equipment used, and the operational parameters for the analysis, including the Agilent 7820A gas chromatograph and 5975C mass spectrometer. The analysis was conducted in selective ion monitoring mode to accurately determine the levels of TPHs in the samples.

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Precious Oluwatomisin
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12 views2 pages

TPH Methods

The document details the GC-MS characterization and qualitative analysis of Total Petroleum Hydrocarbons (TPHs) using a 1000ppm standard from AccuStandard and a five-point calibration method. It describes the calibration process, the equipment used, and the operational parameters for the analysis, including the Agilent 7820A gas chromatograph and 5975C mass spectrometer. The analysis was conducted in selective ion monitoring mode to accurately determine the levels of TPHs in the samples.

Uploaded by

Precious Oluwatomisin
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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GC-MS Characterization: Qualitative Analysis

TPHs standard, 1000ppm (Catalog Number: H-QME-01) containing 24 environmental TPHs


components was purchased from AccuStandard. Five (5) point serial dilution calibration
standards (1.00, 5.00, 10.00, 50.00, 100.00ppm) was prepared from the stock and used to
calibrate the GC-MS.

Prior to calibration, the MS was auto-tuned to perfluorotributylamine (PFTBA) using already


established criteria to check the abundance of m/z 69, 219, 502 and other instrument optimal &
sensitivity conditions.

Determination of the levels of TPHs in the sample was carried out using GC-MS by operating
MSD in selective ion monitoring (SIM) and Scan mode to ensure low level detection of the
target constituents.
Agilent 7820A gas chromatograph coupled to 5975C inert mass spectrometer (with triple axis
detector) with electron-impact source (Agilent Technologies) was used. The stationary phase of
separation of the compounds was HP-5 capillary column coated with 5% Phenyl Methyl
Siloxane (30m length x 0.32mm diameter x 0.25µm film thickness) (Agilent Technologies). The
carrier gas was Helium used at constant flow of 1.48 mL/min at an initial nominal pressure of
1.49 psi and average velocity of 44.22 cm/sec. 1µL of the samples were injected in splitless
mode at an injection temperature of 300 °C. Purge flow to spilt vent was 10.0 mL/min at 2 min
with a total flow of 16.67 mL/min; gas saver mode was switched off. Oven was initially
programmed at 80 °C (3 min) then ramped at 15 °C/min to 320 °C (8 min). Run time was 32 min
with a 3 min solvent delay. The mass spectrometer was operated in electron-impact ionization
mode at 70eV with ion source temperature of 230 °C, quadrupole temperature of 150 °C and
transfer line temperature of 300 °C.

After calibration, the samples were analyzed and corresponding PAHs concentration obtained

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