Sensitive determination of arsenic and selenium in steels by high power nitrogen microwave induced plasma atomic emission spectrometry coupled with hydride generation technique
T. Nakahara et al., Sensitive determination of arsenic and selenium in steels by high power nitrogen microwave induced plasma atomic emission spectrometry coupled with hydride generation technique, TETSU HAGAN, 85(2), 1999, pp. 97-101
Citations number
9
Categorie Soggetti
Metallurgy
Journal title
TETSU TO HAGANE-JOURNAL OF THE IRON AND STEEL INSTITUTE OF JAPAN
:An annular-shaped high power nitrogen microwave induced plasma (Nz-MIP)pro
duced at atmospheric pressure by an Okamoto cavity in a surface wave mode h
as been used as a new and efficient excitation source for atomic emission s
pectrometry (AES). The results show that this kind of MIP source is more st
able than conventional low power MIPs and remarkably tolerant to direct and
continuous introduction of wet aerosols and molecular gases such as hydrog
en, oxygen? air and gaseous hydrides because of its high input microwave po
wer. Under the optimized experimental conditions. the best attainable detec
tion limits at As(I) 228.812 and Se(I) 196.026 nm by use of N-2-MIP-AES cou
pled with hydride generation technique were 2.99 ng As/ml and 0.86 ng Se:ml
with a linear dynamic ranges of 5 to 10,000 ng As/ml and I to 5,000 ng Se/
ml. The presence of several diverse elements has been found to cause more o
r less a depressing interference with :he determination of arsenic and sele
nium by the present technique. Of the several pre-reductants potassium iodi
de has been found to be the most preferable to reduce As(V) to As(III) prio
r to hydride generation for the determination of total arsenic, i.e., As(II
I)+As(V). To the contrary, the heating of sample solutions, previously acid
ified in 5 M with hydrochloric acid at 80 degrees C for 20 min was the best
way to pre-reduce Se(VI) to Se(IV) before hydride generation for the deter
mination of total selenium, i.e., Se(IV)+Se(VI). The proposed method was ap
plied to the determination of low concentrations of arsenic and selenium in
carbon steels and stainless steels, respectively. The results obtained by
this method were in good agreement with the certified values.