Flame atomic absorption determination of zirconium in glass and refractory bricks after coprecipitation with aluminium hydroxide

Abstract

A simple preconcentration method for zirconium based on coprecipitation with aluminium hydroxide prior to flame atomic absorption (FAAS) determination was established. The recovery values of the analyte ions were higher than 95%. Such parameters as the type of hydroxide ion source for precipitation, type of acid for the dissolution step, amount of Al 3+ ion as the collector, pH, temperature, standing time and centrifuge time were optimized using 50 mL of a solution containing 150 g of zirconium. The effect of the solution volume and influences of matrix ions on the extraction of the analyte were also examined. Under the optimum conditions, the calibration curve was linear up to 10 mg L −1. The relative standard deviation for solutions containing 150 g of zirconium was found to be 3.9%. The limit of detection (LOD) and limit of quantitation (LOQ) were calculated as 0.17 and 0.57 mg L −1 , respectively. The method is capable of extracting the analyte in different samples with volumes of up to 250 mL. The preconcentration factor for 250 mL and enhancement factor for 50 mL of analyte solution were calculated to be 250 and 40, respectively. The proposed method was successfully applied for the determination of zirconium in glass and refractory brick samples.

Zirconium in modern analytical chemistry

“…It is not recommended to determine zirconium by the electrothermal atomization method because heat-resistant carbides and oxides of zirconium are formed in the graphite furnace (Burylin et al 2011). The most sensitive analytical line for zirconium is at 360.12 nm, and this line is used in a few methods presented in Table 4 (Fifth Commission Directive 93/73/EEC, 1999; Yadav, Bhowmik & Sikder, 2012;Afzali et al, 2014;Shokrollahi & Gohari, 2017). To reduce the detection limit of zirconium to 44 μg•l −1 , Afzali et al (2014) used the preliminary microextraction of analyte as a ternary complex with fluoride ions and the 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP).…”

Development of a simple and rapid EDXRF method for quantification of ZrO2 and HfO2 in aqueous and organic process stream solutions generated from a zirconium extraction facility

“…Various techniques are available in the literature for the determination of zirconium covering a wide range of concentrations. They include gravimetry, 3 wavelength dispersive X-ray fluorescence (WDXRF) spectrometry, 4,5 total reflection X-ray fluorescence (TXRF), 6 spectrophotometry, 7,8 ICP-AES, 9 AAS 10 etc. Among the available techniques, gravimetry and spectrophotometry methods are cumbersome and time-consuming methods and, therefore, are not preferred choices for reporting the results of process stream solutions where they are to be reported rapidly for taking decisions on downstream processing and also monitoring the zirconium extraction process on a real-time basis.…”