H. Elfering et al., DETERMINATION OF ORGANIC LEAD IN SOILS AND WATERS BY HYDRIDE GENERATION INDUCTIVELY-COUPLED PLASMA-ATOMIC EMISSION-SPECTROMETRY, Analyst, 123(4), 1998, pp. 669-674
This paper describes a simple and rapid method for the determination o
f the sum of tetraalkyllead (TAL) compounds (Me4Pb, Et4Pb) and their i
ntermediate decomposition products, the trialkyllead (Me3Pb+, Et3Pb+)
and dialkyllead (Me2Pb2+, Et2Pb2+) species. The lead species in soluti
on are transformed into the corresponding hydrides by sodium tetrahydr
oborate and directly introduced into the ICP torch, Hydride generation
takes place in a continuous Bow hydride generator and the products ar
e fed into an inductively coupled plasma atomic emission spectrometer,
This arrangement avoids the necessity for solvent extraction and samp
le transfer. The reaction conditions (argon flow rate, concentration o
f acid and concentration of sodium borohydride) have been optimized, T
he acid is decisive for obtaining strongly different sensitivities for
organic lead and inorganic lead; 2.0% (m/v) citric acid suppresses th
e signal of inorganic lead and this offers the possibility to determin
e the organolead compounds in the presence of excess amounts of inorga
nic lead, thus characterizing the method as a screening method. Linear
calibration for six organolead compounds of varying polarity (neutral
and ionic species) was established over the concentration range of 0.
1 to 100 mu g l(-1). Spiked natural water and soil samples were analyz
ed by this method with recoveries of 71-107%, Best extraction efficien
ces were found for a mixture of 5 ml of 1% ammonical methanol and 5 ml
of 0.2 M sodium acetate, The optimized method was tested for soil sam
ples with varying matrices and a wide range of concentrations of alkyl
lead obtained from an old industrial production site.