Determination of cadmium in Zircaloys by electrolyte cathode discharge atomic emission spectrometry (ELCAD-AES)

Abstract

An electrolyte cathode discharge atomic emission spectrometric (ELCAD-AES) method has been reported for the determination of cadmium in Zircaloys. Formic and acetic acids are examined to improve the sensitivity of ELCAD-AES for cadmium determination. The sensitivity of ELCAD-AES is improved 2-fold with 20% (v/v) formic acid. With 20% (v/v) formic acid, the improved detection limit of ELCAD-AES for cadmium is found to be 2 ng mL À1 . A previously reported matrix separation procedure using ammonium pyrrolidine dithiocarbamate (APDC) and methylisobutylketone (MIBK) for the extraction of Cd from Zirconium matrices has been optimised for ELCAD-AES analysis of cadmium. This procedure is found to be useful for the quantitative determination of cadmium in Zircaloys by ELCAD-AES. The precision expressed as a percentage relative standard deviation of the signals of multiple analyses (N ¼ 5) of ELCAD-AES method using the above matrix separation procedure has been found to be 10-15% for trace Cd. This ELCAD-AES method is validated with the certified values of Zircaloy CRM and the glow discharge quadrupole mass spectrometry (GD-QMS) values of Zircaloy samples.

Flowing Liquid Anode Atmospheric Pressure Glow Discharge as an Excitation Source for Optical Emission Spectrometry with the Improved Detectability of Ag, Cd, Hg, Pb, Tl, and Zn

“…In this case, the analyzed solution is bombarded with the positive ions, and as a consequence of the sample sputtering, the dissolved metals can be transferred to the discharge phase where the excitation processes occur. At present, the number of interesting applications of different FLC-APGD systems is large and includes the analysis of various water samples, including tap, mineral, river, and waste waters (Ca, K, Mg, Na, Zn), 3 river and waste waters (Cr), 4 snow, tap, and well waters (In, Rh, Te), 5 ground waters (Tl), 6 as well as brines (Ca, K, Mg, Na), 7 human hair and stream sediments (Cd, Cr, Hg, Pb), 8,9 honeys (Ca, Cu, Fe, K, Li, Mg, Mn, Na, Rb, Zn), 10 titanium dioxide (Ag, Ca, Cu, Fe, K, Li, Mg, Na, Pb), 11 zirconium-based alloys (Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Ni, Pb), 12,13 colloidal silica (K, Li, Mg, Na). 14 For the APGD operated with a flowing liquid anode (FLA), the solution surface is struck by the electrons, which are not able to sputter the sample.…”

High-Sensitivity Determination of K, Ca, Na, and Mg in Salt Mines Samples by Atomic Emission Spectrometry with a Miniaturized Liquid Cathode Glow Discharge

“…In recent years, closed-type ELCAD has been applied for the analysis of several real samples including water samples [ 18 , 23 ], human hair and stream sediment [ 24 ], honeys [ 25 ], tuna fish and aquatic plant [ 26 ], titanium dioxide [ 27 ], zircaloys [ 28 , 29 ], colloidal silica [ 5 ], and soils and spruce needles [ 11 ]. Despite these progresses, to the best of our knowledge, ELCAD type is rarely applied for the determination of metal elements in salt mines samples, perhaps because of its complicated matrix.…”

Measurement of sample and plasma properties in solution-cathode glow discharge and effects of organic additives on these properties

“…26,27 This shi towards applications is vital for a technique to become truly relevant, 18 but there is a continued need for more basic research. Other studies 9,24,25 have used this enhancement. Concentration 1 and identity 28 of the sample solution's electrolyte have long been known to affect the strength of atomic emission.…”

“…Recent studies have shied to applications involving more complex samples. Since 2009, these discharges have been applied to tea infusions, 3 tea leaves, 3 mineral water, 3 tuna sh, [19][20][21] aquatic plant matter, 19 oyster tissue, 21 coal y ash, 21,22 groundwater, 22 hepatitis-B vaccine, 20 lake water, 5 soil leachates, 5 spruce needle leachates, 5 colloidal silica, 23 zirconium alloys, 24,25 simulated natural water, 8 honey, 15 human hair, 26,27 and stream sediment. 26,27 This shi towards applications is vital for a technique to become truly relevant, 18 but there is a continued need for more basic research.…”