Headspace gas chromatography with flame ionization detection (HS-GC-FID) for the determination of dissolved methane in wastewater

2014 ◽  
Vol 70 (5) ◽  
pp. 901-908 ◽  
Author(s):  
D. J. Beale ◽  
G. Tjandraatmadja ◽  
M. Toifl ◽  
N. Goodman
Keyword(s):  
Gas Chromatography ◽  
Limit Of Detection ◽  
Wastewater Sludge ◽  
Flame Ionization Detection ◽  
Sampling Device ◽  
Dissolved Methane ◽  
Ionization Detection ◽  
Flame Ionization ◽  
Relative Standard ◽  
Wastewater Samples

There is currently a need for a simple, accurate and reproducible method that quantifies the amount of dissolved methane in wastewater in order to realize the potential methane that can be recovered and account for any emissions. This paper presents such a method, using gas chromatography with flame ionization detection fitted with a GS-Gas PRO column coupled with a headspace auto sampler. A practical limit of detection for methane of 0.9 mg L−1, with a retention time of 1.24 min, was obtained. It was found that the reproducibility and accuracy of the method increased significantly when samples were collected using an in-house constructed bailer sampling device and with the addition of 100 μL hydrochloric acid (HCl) and 25% sodium chloride (NaCl) and sonication for 30 min prior to analysis. Analysis of wastewater samples and wastewater sludge collected from a treatment facility were observed to range from 12.51 to 15.79 mg L−1 (relative standard deviation (RSD) 8.1%) and 17.56 to 18.67 mg L−1 (RSD 3.4%) respectively. The performance of this method was validated by repeatedly measuring a mid-level standard (n = 8; 10 mg L−1), with an observed RSD of 4.6%.

Study of Endocrine Disruptors in the Sediment of a South Brazilian River

2015 ◽  
Vol 1120-1121 ◽  
pp. 862-866
Author(s):  
Irajá Do Nascimento ◽  
Nathália Christine Vieceli ◽  
Michele Schmitz ◽  
Fernanda Glaeser
Keyword(s):  
Gas Chromatography ◽  
Bisphenol A ◽  
Endocrine Disruptors ◽  
River Sediment ◽  
Flame Ionization Detection ◽  
River Contamination ◽  
Ionization Detection ◽  
Flame Ionization ◽  
Organic Extracts ◽  
Ethylhexyl Phthalate

This study investigated the occurrence of di (2-ethylhexyl) phthalate (DEHP) di-n-butylphthalate (DBP) and bisphenol A (BPA) in river sediment. The samples were collected from three selected points and extracted by sonication, using n-hexane and ethanol. The organic extracts were analyzed by gas chromatography with flame ionization detection (GC/FID). DBP and BPA were not detected. The average concentrations of DEHP range from 0.72 (±0.04) to 27.90 (± 3.05) ng g-1 of sediment. The best solvent for the extractions was n-hexane. However ethanol also shows good extraction yields of DEHP. These results showed an important anthropic contribution for the river contamination by endocrine disruptors.

Determination of Chlorobenzenes in Wastewater by Single-Drop Microextraction Coupled to Capillary Gas Chromatography

2013 ◽  
Vol 838-841 ◽  
pp. 2566-2569
Author(s):  
Jian Qi Sun ◽  
Bo Qiao ◽  
Jun Dai
Keyword(s):  
Gas Chromatography ◽  
Capillary Gas Chromatography ◽  
Preparation Technique ◽  
Single Drop ◽  
Flame Ionization ◽  
Single Drop Microextraction ◽  
Relative Standard ◽  
Efficient Recovery ◽  
Wastewater Samples

This study describes an analytical method employing capillary gas chromatography (GC) using flame ionization detection (FID) that has been developed for the simultaneous determination of chlorobenzenes (m-dichlorobenzene (m-DCB),p-dichlorobenzene (p-DCB),o-dichlorobenzene (o-DCB) and 1,2,4-trichlorobenzene (1,2,4-TCB)) in wastewater. For this purpose, single-drop microextraction (SDME) was applied as a sample preparation technique. The SDME parameters such as types of extractants, volume of the microdroplet size, extraction time, stir rate and immersion depth of needle point were studyed and optimized. The method was linear in the ranges from 4.0×10-3to 40.0 μg·mL-1form-DCB,p-DCB ando-DCB, and 4.0×10-3to 30.0 μg·mL-1for 1,2,4-TCB withR2≥0.9955. The SDME procedure allowed efficient recovery of the investigated chlorobenzenes ranging between 80 % and 105 % with a relative standard deviation (RSD) ≤6.5 for actual wastewater sampes spiked with 2, 5 and 10 μg·mL-1of chlorobenzes, respectively. These results showed the potential of this technique for chlorobenzenes monitoring in wastewater samples. Furthermore, the investigated methods are simple, reliable, reproducible, and not expensive.

The secretion of ibuprofen metabolites interferes with the capillary chromatography of urinary homovanillic acid and 4-hydroxy-3-methoxymandelic acid in neuroblastoma diagnosis

2005 ◽  
Vol 43 (2) ◽  
Author(s):  
Isabella Levreri ◽  
Ubaldo Caruso ◽  
Franca Deiana ◽  
Antonella Buoncompagni ◽  
Bruno De Bernardi ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Capillary Gas Chromatography ◽  
Homovanillic Acid ◽  
Urine Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Catecholamine Metabolism ◽  
Flame Ionization Detection ◽  
Trimethylsilyl Ester ◽  
Ionization Detection ◽  
Flame Ionization

AbstractNeuroblastoma is the most common extracranial solid tumor in children. Abnormal secretion of catechol-amines in tissues and body fluids allows for the differential diagnosis of neuroblastoma from other neoplasms and its distinction from non-neoplastic inflammatory diseases. This is achieved by assaying homovanillic acid and 4-hydroxy-3-methoxymandelic acid, the catabolites of catecholamine metabolism. In the course of an evaluation of children with suspected neuroblastoma, homovanillic acid and 4-hydroxy-3-methoxymandelic acid were analyzed in urine samples by capillary gas chromatography with flame ionization detection after extraction and derivatization of these compounds as trimethylsilyl derivatives. In three urine samples a significant increase in biogenic amines was observed, but these results were not confirmed by thin-layer chromatography. Patient history revealed that these children had been treated with ibuprofen, an analgesic and anti-inflammatory drug. To verify how ibuprofen or its metabolites may have interfered with capillary gas chromatography with flame ionization detection, we analyzed the same samples by capillary gas chromatography-mass spectrometry. In urine samples from patients on the drug, the presence of a peak identified as the trimethylsilyl ester of hydroxyibuprofen, which had the same retention time as 4-hydroxy-3-methoxymandelic acid, was found to interfere with the capillary gas chromatography with flame ionization detection analysis of the metabolite. This interference must be taken into account during the laboratory diagnosis of neuroblastoma.

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