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In the present work, a simple procedure is presented for the extraction and determination of pre-concentrated trace amounts of palladium ions through solid phase extraction (SPE) and flame atomic absorption spectrophotometry. This process was performed using Nylon-66/5-(4-dimethylaminobenzylidene) rhodanine composite nanofibres. These nanofibres were produced under optimised conditions via two-axial electrospinning technique and characterised by scanning electron microscopy and Fourier-transform infrared spectroscopy. The effect of experimental parameters including solution pH, the type and volume of eluent and contact time was investigated in extraction and desorption process. Under the optimised conditions, good linearity in the range of 0.07–8 μg L−1 and low detection limit of 0.015 μg L−1 were obtained. High enrichment factor of 187.5 and good relative standard deviation of ±2.2% at 5 μg L−1 of palladium had been achieved. The sorbent capacity for palladium adsorption was obtained 27 mg palladium per gram of nanofibres. So, the SPE was successfully applied to pre-concentrate and determine Pd(II) ions with flame atomic absorption spectrophotometer in real samples. [ABSTRACT FROM AUTHOR]

In the present study, multiwalled carbon nanotubes (MWCNTs) as solid phase extraction sorbent were developed for preconcentration of arsenic(V) species prior to graphite furnace atomic absorption spectrometry (GFAAS) determination. Arsenic(V) was selectively sorbed on the packed column with MWCNTs within a pH 9.5 in the presence of 2-(5-bromo-2-pyridylazo)-5-diethyl amino phenol (5-Br-PADAP). The adsorbed species was then desorbed with 1 mL of 2.0 M HNO3. Experimental parameters including pH, sample volume and flow rate, type, volume and concentration of eluent that influence the recovery of the arsenic(V) species were optimised. Under the optimised conditions, the calibration curve was linear in the range of 0.2–10.0 µg L−1with detection limit of 0.016 µg L−1. The relative standard deviations (RSD) for seven replicate determinations at 1.0 µg L−1level of arsenic was 6.69%. The proposed method was successfully applied to the determination of arsenic in water samples and certified reference material (NIST RSM 1643e). [ABSTRACT FROM AUTHOR]