Optical emission spectrometric determination of arsenic and antimony by continuous flow chemical hydride generation and a miniaturized microwave microstrip argon plasma operated inside a capillary channel in a sapphire wafer

摘要: Abstract Continuous flow chemical hydride generation coupled directly to a 40 W, atmospheric pressure, 2.45 GHz microwave microstrip Ar plasma operated inside capillary channel in sapphire wafer has been optimized for the emission spectrometric determination of As and Sb. The effect NaBH4 concentration, concentration HCl, HNO3 H2SO4 used sample acidification, rate, reagent rates, liquid volume separator as well presence interfering metals such Fe, Cu, Ni, Co, Zn, Cd, Mn, Pb Cr, was investigated detail. A considerable influence Fe(III) (enhancement up 50 %) As(V) Fe(III), Cu(II) Cr(III) (suppression 75%) Cd(II) Mn(II) by 25%) Sb(III) found occur, which did not change more than factor 2 range 2–20 μg ml− 1. tolerated introduction 4.2 ml min− 1 H2 working gas, corresponded an H2/Ar ratio 28%. Under these conditions, excitation temperature measured with atom lines electron number density determined from Stark broadening Hβ line order 5500 K 1.50 · 1014 cm− 3, respectively. Detection limits (3σ) 18 ng ml− 1 31 ng Sb were calibration curves linear over orders magnitude. With procedure developed could be at 45 6.4 μg level galvanic bath solution containing 2.5% NiSO4. Additionally, coal fly ash reference material (NIST SRM 1633a) certified 145 ± 15 μg g− 1 value 144 ± 4 μg found.