Automatic On-line Solid-phase Extraction-Electrothermal Atomic Absorption Spectrometry Exploiting Sequential Injection Analysis for Trace Vanadium, Cadmium and Lead Determination in Human Urine Samples

Abstract

A fully automated sequential injection column preconcentration method for the on-line determination of trace vanadium, cadmium and lead in urine samples was successfully developed, utilizing electrothermal atomic absorption spectrometry (ETAAS). Polyamino-polycarboxylic acid chelating resin (Nobias chelate PA-1) packed into a handmade minicolumn was used as a sorbent material. Effective on-line retention of chelate complexes of analytes was achieved at pH 6.0, while the highest elution effectiveness was observed with 1.0 mol L(-1) HNO3 in the reverse phase. Several analytical parameters, like the sample acidity, concentration and volume of the eluent as well as the loading/elution flow rates, have been studied, regarding the efficiency of the method, providing appropriate conditions for the analysis of real samples. For a 4.5 mL sample volume, the sampling frequency was 27 h(-1). The detection limits were found to be 3.0, 0.06 and 2.0 ng L(-1) for V(V), Cd(II) and Pb(II), respectively, with the relative standard deviations ranging between 1.9 - 3.7%. The accuracy of the proposed method was evaluated by analyzing a certified reference material (Seronorm(TM) trace elements urine) and spiked urine samples.

Separation of 44Sc from Natural Calcium Carbonate Targets for Synthesis of 44Sc-DOTATATE

“…This can be explained both by the use of high-purity reagents that are available for the proposed procedure and by the specific properties of the resin used. Nobias shows extremely low affinity towards alkaline metals [ 17 ] combined with almost quantitative sorption of transition metals in pH 5–6 [ 18 ] while the affinity is decreased significantly in pH < 4 [ 19 , 20 ]. REE metals show quantitative sorption in a similar pH range to the transition metals [ 21 ] but extend this property to more acidic conditions: pH 4.2 was successfully reported [ 13 ] and even pH 2.5 is suitable for efficient sorption [ 22 ], which is consistent for scandium in the present results ( Figure 1 ).…”

Atomic spectrometry update: review of advances in the analysis of clinical and biological materials, foods and beverages

“…A number of papers were published describing online enhancement options for ETAAS such as pre-concentration and speciation. A rapid, online SPE system coupled to ETAAS was proposed by Giakisikli and co-workers 59 for the determination of Cd, Pb and V in human urine. A mini-column packed with polyamino-polycarboxylic acid chelating resin was used to preconcentrate the analytes online.…”