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Simultaneous determination of aliphatic and aromatic amines in indoor and outdoor air samples by gas chromatography-mass spectrometry

Akyüz M.

Article | 2007 | Talanta71 ( 1 ) , pp.486 - 492

A gas chromatography-mass spectrometry (GC-MS) method has been proposed for the simultaneous determination of aliphatic and aromatic amines in indoor and outdoor air samples. The method includes pre-concentration of the compounds by percolating the air samples through the acidic solution, ion-pair extraction with bis-2-ethylhexylphosphate (BEHPA), derivatisation of compounds with isobutyl chloroformate (IBCF) and their GC-MS analysis. Aliphatic and aromatic amines were isolated from aqueous samples using BEHPA as ion-pair reagent and derivatised with IBCF for their chromatographic analysis. Aliphatic and aromatic amines were then an . . .alysed with GC-MS in both electron impact (EI) and positive and negative ion chemical ionisation (PNICI) mode as their isobutyloxycarbonyl (isoBOC) derivatives. The obtained recoveries ranged from 75.6 to 96.8% and the precision of this method, as indicated by the relative standard deviations (R.S.D.) was within the range of 1.0-4.4%. The detection limits obtained from calculations by using GC-MS results based on S/N: 3 were within the range of 0.08-0.01 ng/m3. © 2006 Elsevier B.V. All rights reserved Daha fazlası Daha az

Determination of low level nitrite and nitrate in biological, food and environmental samples by gas chromatography-mass spectrometry and liquid chromatography with fluorescence detection

Akyüz M. | Ata S.

Article | 2009 | Talanta79 ( 3 ) , pp.900 - 904

Gas chromatography-mass spectrometry (GC-MS) and liquid chromatography with fluorescence detection (LC-FL) methods have been proposed for the determination of low level nitrite and nitrate in biological, food and environmental samples. The methods include derivatization of aqueous nitrite with 2,3-diaminonaphthalene (DAN), enzymatic reduction of nitrate to nitrite, extraction with toluene and chromatographic analyses of highly fluorescent 2,3-naphthotriazole (NAT) derivative of nitrite by using GC-MS in selected-ion-monitoring (SIM) mode and LC-FL. Nitrite and nitrate ions in solid samples were extracted with 0.5 M aqueous NaOH by s . . .onication. The recoveries of nitrite and nitrate ions based on GC-MS and LC-FL results were 98.40% and 98.10% and the precision of these methods, as indicated by the relative standard deviations (RSDs) were 1.00% for nitrite and 1.20% for nitrate, respectively. The limits of detection of the GC-MS in SIM mode and LC-FL methods based on S/N = 3 were 0.02 and 0.29 pg/ml for nitrite and 0.03 and 0.30 pg/ml for nitrate, respectively. © 2009 Elsevier B.V. All rights reserved Daha fazlası Daha az

Ion-pair extraction and GC-MS determination of linear alkylbenzene sulphonates in aqueous environmental samples

Akyüz M.

Article | 2007 | Talanta71 ( 1 ) , pp.471 - 478

A GC-MS method was developed for the determination of linear alkylbenzene sulphonates (LAS) and sulphophenylcarboxylic acids (SPC) in aqueous environmental samples. LAS and SPC were isolated from aqueous samples using methylene green (MG) as ion-pair reagent and derivatised with diazomethane for their chromatographic analysis. LAS and SPC were then analysed with GC-MS in EI mode as their methyl esters. The method eliminates positive and negative interferences found by the methylene blue method and considered to be selective and sensitive for the determination of LAS and SPC in aqueous samples. The recovery of LAS was 98% with a rela . . .tive standard deviation (R.S.D.) of 2.0% and the detection limit obtained from calculations by using GC-MS results based on S/N:3 was lower than 10 ppb. Obtained results revealed that the method can also be employed in the analysis of organic compounds bearing sulphate and sulphonate groups. © 2006 Elsevier B.V. All rights reserved Daha fazlası Daha az

The use of simulation in the EPR spin probe technique for detection of irradiated seeds

Sünnetçioglu M.M. | Dadayli D.

Article | 2000 | Talanta53 ( 1 ) , pp.69 - 74

An electron paramagnetic resonance (EPR) spin probe study of irradiated wheat seeds was performed depending on irradiation dose. The structural changes in the membrane integrity were followed using aqueous solutions of 4-hydroxy-TEMPO (TANOL) spin probe and a line broadening material. In the studies dry seed embryos were kept in these solutions for 150 min. The spectra were recorded at various times of air drying process. The simulation of these spectra indicated a decrease in the water content of the embryos depending on the increasing irradiation dose. This indicates the increase in the permeability of the membranes as a result of . . . the radiation damage. From the decay curves it is possible to determine about irradiation dose, however, this approach is not very successful at close irradiation doses. (C) 2000 Elsevier Science B.V.An electron paramagnetic resonance (EPR) spin probe study of irradiated wheat seeds was performed depending on irradiation dose. The structural changes in the membrane integrity were followed using aqueous solutions of 4-hydroxy-TEMPO (TANOL) spin probe and a line broadening material. In the studies dry seed embryos were kept in these solutions for 150 min. The spectra were recorded at various times of air drying process. The simulation of these spectra indicated a decrease in the water content of the embryos depending on the increasing irradiation dose. This indicates the increase in the permeability of the membranes as a result of the radiation damage. From the decay curves it is possible to determine about irradiation dose, however, this approach is not very successful at close irradiation doses Daha fazlası Daha az

Inorganic arsenic speciation in water samples by miniaturized solid phase microextraction using a new polystyrene polydimethyl siloxane polymer in micropipette tip of syringe system

Ali, Jamshed | Tüzen, Mustafa | Kazi,Tasneem G. | Hazer, Baki

Article | 2016 | Talanta161 , pp.450 - 458

The polymer, polystyrene polydimethyl siloxane was loaded into the micropipette tip of the syringe system as an adsorbent to developed miniaturized solid phase microextraction. Standard solutions of arsenate and arsenite were passed through the adsorbent loaded in micropipette tip to check the adsorption behaviors. It was observed that arsenate adsorbed on the polystyrene polydimethyl siloxane in the pH rang of 6–8, while arsenite was directly passed through the micropipette tip of syringe system. The adsorbed arsenate in micropipette tip of syringe system were eluted by 1.0 M hydrochloric acid. The total inorganic arsenic contents . . .were obtained by the addition of oxidizing agent potassium permanganate into the studied samples before passing to the micropipette tip of syringe system. Arsenite concentration in water samples were measured by subtracting arsenate from total inorganic arsenic concentration. Different characteristics which effect the determination of arsenate specie like amount of adsorbent, adsorption capacity, pH, pulled and pushed cycles for adsorption and desorption, volume of sample, eluent type and it volume were also studied in detail. Enrichment factor and detection limit of arsenate by desired method were 218 and 6.9 ng L-1 respectively. The relative standard deviation was 4.1% (n=10, C=0.12 µg L-1). Accuracy of the desired technique was confirmed by analysis of the CRMs (Lake Ontario Water TM-28.3 and Riverine Water NRCC-SLRS-4). Desired technique was significantly useful for determination of the total arsenic, arsenate, and arsenite contents in different natural water samples. © 2016 Elsevier B.V Daha fazlası Daha az

Solid phase microextraction method using a novel polystyrene oleic acid imidazole polymer in micropipette tip of syringe system for speciation and determination of antimony in environmental and food samples

Panhwar, Abdul Haleem | Tüzen, Mustafa | Hazer, Baki | Kazi, Tasneem Gul

Article | 2018 | Talanta184 , pp.115 - 121

A simple, rapid and sensitive solid phase microextraction method was used for the speciation of inorganic antimony (Sb) by using a novel synthesized polymeric material in micropipette tip of syringe system. In present methodology, the specie of Sb (III) made hydrophobic complex with diethyl dithiocarbamate (DDTC) at pH 5.5 and subsequently adsorbed on polystyrene oleic acid imidazole polymer (POIP), whereas Sb(V) did not made complex and adsorbed on the polymer, remained in aqueous solutions. The strategy of multivariate was carried out to screen out the different variables and assessed the optimum values of their experimental value . . .s for the extraction efficiency of analyte. Then the analyte was sorbed on the polymer in micropipette tip of syringe system was quantitatively eluted by different types of acids at different levels for 2–6 aspirating/dispensing cycles. The extracted Sb(III) ions with modifiers were directed into the graphite furnace atomic absorption spectrometry for analysis. The limit of detection (LOD), limit of quantification (LOQ) and preconcentration factor (PF) for Sb(III) was found to be 6 ng L-1, 20 ng L-1 and 100. The RSD value was found to be 4.2%. The standard addition method and certified reference materials were checked for accuracy and validity of method. The developed method was effectively applied for the determination of total and inorganic species of Sb(III) and Sb(V) in different types of water samples, whereas only total Sb was determined in acid digested soil, Tuna fish, rice, spinach, black tea, mixed fruit juice and ice tea samples. © 2018 Elsevier B.V Daha fazlası Daha az

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