Determination of lead in sediments and sewage sludge by on-line hydride-generation axial-view inductively-coupled plasma optical-emission spectrometry using slurry sampling

Abstract

Among the "traditional" hydride-forming elements, lead is probably the most difficult, and its determination in this form has rarely been reported in the literature. In this paper a simple and rapid method, axial-view inductively-coupled plasma optical-emission spectrometry using on-line hydride generation (HG-ICP-OES) from samples prepared as slurry, is proposed for determination of lead in environmental samples. The samples (20-50 mg, particle size <or=120 microm) were treated with 1 mL aqua regia in a 40-kHz ultrasonic bath for 60 min. The slurry was diluted to a final volume of 50 mL with a 10% m/v solution of (NH(4))(2)S(2)O(8). The concentrations of NaBH(4), tartaric acid, and (NH(4))(2)S(2)O(8), used for on-line plumbane generation were optimized by means of a complete factorial analysis applied to an aqueous standard solution and to the slurry of a sediment certified reference material (CRM). External calibration against aqueous standards in the concentration range 10-100 microg L(-1) was used for analysis of six CRM--three marine sediments, one river sediment, and two sewage sludges. Analysis of the filtered slurry showed that Pb was only partially extracted into the liquid phase. Several major concomitants tested did not affect the Pb signal. The detection limit (3s, n = 10) for 20 mg sample in a final volume of 50 mL was 5.0 microg g(-1). Tin was the only other hydride-forming analyte that could be determined satisfactorily with Pb; for tin the detection limit was 1.0 microg g(-1). The values obtained for Pb and Sn were not significantly different from the certified concentrations, according to the t-test at the 95% confidence level. Nine river sediments collected locally were also analyzed and the concentrations were in agreement with results obtained after total digestion.

Continuous flow hydride generation laser induced fluorescence spectrometry for trace determination of lead in water and sediment samples

“…The final concentration of Pb in the undiluted sample digest solution was determined by the HG-LIF calibration curve method to be 3.166 AE 0.020 mg mL À1 , which corresponded to a mass concentration of 316.60 AE 20.37 mg Pb/g in the dry sediment. This is consistent with the range of Pb concentrations in the sediment that have been reported previously [30,32].…”

Determination of lead by hydride generation inductively coupled plasma mass spectrometry (HG-ICP-MS): On-line generation of plumbane using potassium hexacyanomanganate(III)

“…Therefore, various oxidizing agents have been utilized in most studies to oxidize Pb(II) to Pb(IV) in acidic solutions. These include hydrogen peroxide [18–22], ammonium or sodium persulfate [19,23,24], potassium dichromate [19,21], ammonium cerium (IV) nitrate [25,26] The use of chelating agents is rather scarce. Chen at al.…”

Slurry Sampling—An Analytical Strategy for the Determination of Metals and Metalloids by Spectroanalytical Techniques

“…In Table 5, the analytical features of recent methods exploiting slurry sampling for determination of volatile species of metal and metalloid species are shown (46,(68)(69)(70)(71).…”