Quantification of Hydroperoxides by Gas Chromatography with Flame Ionisation Detection

Hydroperoxides are of great importance in the fields of atmospheric and biological chemistry. However, there are several analytical challenges in their analysis: unknown and usually low UV absorption coefficients, high reactivity, thermal instability, and a lack of available reference standards. To overcome these limitations, we propose a GC-FID approach involving pre-column silylation and quantification via the effective carbon number approach. Four hydroperoxides of α-pinene were synthesized in the liquid phase with singlet oxygen and identified using literature data on isomer yield distribution, MS spectra, estimated boiling temperatures of each isomer (retention time), their thermal stability and derivatisation rate. The developed procedure was used for the determination of hydroperoxides in bottled and autooxidised turpentine. We anticipate that this method could also be applied in atmospheric chemistry, where the reactivity of singlet oxygen could help explain the high formation rates of secondary organic aerosols.

Terpene Compounds of New Tunisian Extra-Virgin Olive Oil: Effect of Ripening Stage

The volatile profiles of Tunisian virgin olive oils were established by solid phase micro-extraction (SPME) and gas chromatography (GC), using flame ionisation and mass spectrometer detectors. Terpenes compounds were identified and characterized. Limonene, the main terpene compound extracted by SPME, characterized the studied olive oil. Significant differences in the proportions of terpenes constituents from oils of different maturity index were detected. The results demonstrated that the accumulation of the terpenes compounds in the studied oils obtained from different ripeness stage was strictly connected with the ripeness stage.

Monitoring Quality of Alcohol-Based Hand Sanitizers Used in Johannesburg Area During the Covid‐19 Pandemic.

Since the outbreak of the Coronavirus Disease 2019 (CoViD-19), the World Health Organization has recommended that, in the absence of soap and water, alcohol-based hand sanitizer can be used to prevent the transmission of coronaviruses. Unfortunately, many media reports indicate that majority of current alcohol-based hand sanitizers are substandard and some contain potentially toxic ingredients. The study aimed to identify sanitizers used in the Johannesburg area that do not contain the WHO-recommended alcohol concentration of at least 70% propanol or 60% ethanol, and contain traces of toxic ingredients. Hand sanitizers were randomly collected from various traders around Johannesburg. The samples were analyzed using Agilent Auto sampler coupled to a gas chromatograph utilizing flame ionisation detection. Of the 94 different hand sanitizers collected, three preparations were found to contain no alcohol, whereas the rest contained either ethanol or 2-propanol or a combination of the two. Of the alcohol-containing sanitizers, 37 (41%) contained less than 60% v/v alcohol. Ethyl acetate, isobutanol and other non-recommended alcohols (methanol, 1-propanol and 3-methyl-butanol) were also identified. Consumers are therefore warned that among the many brands of hand sanitizer found around Johannesburg, there are some substandard preparations and some that contain traces of toxic ingredients.

Extractives in Betula celtiberica stemwood and isolation and identification of diarylheptanoids in the hydrophilic extract

In Betula celtiberica (Iberian white birch) stemwood, the content and composition of lipophilic and hydrophilic extractives were determined; these have not been reported previously in this species. The total gravimetric amount of extractives was 2.2% of dry wood, of which lipophilic extractives accounted for 0.39% and hydrophilic extractives 1.84% (determined by gas chromatography–flame ionisation detection [GC–FID]). The lipophilic extract contained mainly triterpenoids and steroids. The hydrophilic extract (acetone–water 95:5 v v−1) contained mainly sugars, compounds not eluting on GC, and a large number of unidentified compounds, which accounted for 0.87% of dry wood and dominated the extract. The compounds were isolated from the extract by silica column chromatography and further purified. GC–electron impact (EI)-MS of the silylated compounds showed characteristic mass fragments that suggested them to be diarylheptanoids (DAHs). This is an interesting compound group, as many of them have shown a large variety of beneficial biological effects. Of over 80 detected DAHs, the exact mass of 17 compounds was determined by electrospray ionisation-quadrupole-time-of-flight (ESI-QTOF)-MS, and of these, the structure of 11 compounds was elucidated by nuclear magnetic resonance (NMR). One was a meta,para-bridged diphenylether and 10 were meta,meta-bridged biphenyls, of which one, 3,8,9,17-tetrahydroxy-[7,0]-metacyclophane, has not been described previously. Because of low concentrations, 21 DAHs were only tentatively identified, and of these, as many as 17 seem to be previously undescribed compounds.

Geochemical Fingerprinting pf Oil-Impacted Soil and Water Samples In Some Selected Areas in the Niger Delta

With over 50 years of oil exploration and exploitation in the Niger Delta, there has been an increasing rate of environmental degradation due to hydrocarbon pollution. This study is aimed at tracing the sources of the oil spills and the distribution of pollutants in selected communities in the Niger Delta using geo-chemical techniques. A total of sixteen samples made up of ten crude oil-impacted soil samples taken at a depth of 30 cm and six water samples (two from boreholes, two from burrow pits and two from surface water – one from a river and the other from rain harvest as control) were collected. The identification and quantification of aliphatic hydrocarbons (AHs) and polycyclic aromatic hydrocarbons (PAHs) in the samples were performed with an Agilent 7890B gas chromatography flame ionisation detector (GCFID). The AHs including pristane and phytane, together with seventeen priority PAHs, were identified. The values of AHs and PAHs in the water samples ranged from 0.13 mg/l to 5.78 mg/l and 0.09 mg/l to 1.109 mg/l, respectively, while that for the soil samples ranged from 22.52 mg/kg to 929.44 mg/kg and 10.544 mg/kg to 16.879 mg/kg, respectively. Z več kot petdesetimi leti raziskovanja in pridobivanja nafte na območju delte reke Niger narašča stopnja degradacije okolja zaradi onesnaževanja z ogljikovodiki. Namen raziskave je slediti virom razlitij nafte in porazdelitev onesnaževal v izbranih skupnostih v delti reke Niger z uporabo geokemičnih pristopov. Skupno je bilo odvzetih 16 vzorcev, od tega 10 vzorcev z nafto nasičenih zemljin iz globine 30 cm ter 6 vzorcev vode, od tega dva iz vrtin, dva iz jame ter dva iz površinske vode (en vzorec iz reke in en iz deževnice). Z detektorjem plamenskega ioniziranja s plinskim kromatografom Agilent 7890B (GC-FID) je bila izvedena identifikacija in kvantifikacija alifatskih ogljikovodikov (AH) in policikličnih aromatskih ogljikovodikov (PAH). Identificirani so bili AH z vključujočim pristanom (pristane) in fitanom (phytane) skupaj s 17 PAH. Vrednosti AH in PAH v vzorcih vode se gibajo med 0.13 mg/l do 5.78 mg/l in 0.09 mg/l do 1.109 mg/l. Vrednosti AH in PAH v vzorcih zemljine se gibajo med 22.52 mg/kg do 929.44 mg/kg in 10.544 mg/kg do 16.879 mg/kg.

Influence of Reaction Parameters on the Gelation of Silanised Linseed Oil

The subject of this work was to characterize the catalytic course of the linseed oil silylation reaction with vinyltrimethoxysilane (VTMOS), carried out under elevated pressure and temperature conditions, and an explanation of the reasons for rapid gelation of the reaction product. To explain and describe the process, analytical methods were used, i.e., 1H and 13C NMR (nuclear magnetic resonance), GC-FID (gas chromatography coupled with flame ionisation detection), and GPC (gel permeation chromatography). Reaction products were monitored after 3, 6 and 12 h. The molar mass of the VTMOS-modified oil in only 3 h was comparable with the molar mass of the product obtained by conventional polymerisation. An increase in the reaction time resulted in further transformations resulting from the hydrolysis and condensation reactions taking place. In contrast to reactivity of soybean oil, the silanisation of linseed oil occurred much faster and without the need for cross-linking catalysts. The reason for the high reactivity of linseed oil to VTMOS and rapid gelation of the resulting product was primarily the amount of double bonds present in linseed oil and their high availability, in particular the double bond in the acid linolenic acid located at the C16 carbon.