Login for students

Login for employees

Publication detail

Direct determination of lead in bones using slurry sampling and high-resolution continuum source electrothermal atomic absorption spectrometry
Authors: Husáková Lenka | Šídová Tereza | Ibrahimová Lucie | Svízelová Monika | Mikysek Tomáš
Year: 2019
Type of publication: článek v odborném periodiku
Name of source: Analytical Methods
Publisher name: Royal Society of Chemistry
Place: Cambridge
Page from-to: 1254-1263
Titles:
Language Name Abstract Keywords
cze Stanovení olova v kostech metodou vysokorozlišovací atomové absorpční spektrometrie s elektrotermickou atomizací a kontinuálním zdrojem záření za využití přímého dávkování suspenzí Vyvinuta byla jednoduchá, rychlá a ekologicky šetrná metoda pro stanovení Pb v kostech metodou atomové absorpční spektrometrie s elektrotermickou atomizací s kontinuálním zdrojem záření a vysokým rozlišením (HR-CS-ETAAS). Optimalizace metody umožňující analýzu reálných vzorků formou přímého dávkování suspenzí byla provedena za využití nástrojů frakcionálního faktorového plánování. Pro korekci spektrální interference způsobené strukturovaným pozadím v důsledku přítomnosti PO molekulových absorpčních pásů bylo použito matematické korekce. Určeny byly analytické charakteristiky stanovení Pb pomocí navržené metody. Validace metody byla provedena s využitím komerčně dostupného certifikovaného materiálu NIST SRM 1486 Bone Meal a pomocí referenční metody TOF-ICP-MS. Stanovení olova; Analýza kostí; HR-CS-ETAAS; ICP-MS; Analýza suspenzí; Interference matrice; Plánování experimentu; Frakcionální faktorové plánování
eng Direct determination of lead in bones using slurry sampling and high-resolution continuum source electrothermal atomic absorption spectrometry A straightforward, quick, sensitive and reliable method is introduced for the determination of lead in bones using slurry sampling and high-resolution continuum source electrothermal atomic absorption spectrometry (HR-CS-ETAAS). The spectral interference caused by the molecular absorption of PO molecules with rotational fine structure coinciding with the analyte absorption at the most sensitive resonance line 217.001 nm in time was identified and successfully corrected by applying a mathematical correction algorithm using the spectrum obtained by vaporization of hydroxyapatite. The slurry preparation and measuring conditions were determined by means of a response surface methodology. Experiments were designed according to a 2(7-4) replicate (n = 3) fractional factorial design for seven factors (particle size, glycerol and HNO3 concentration, sonication time, concentration of the chemical modifier, pyrolysis and atomization temperature) each at three different levels, including central points. The optimized conditions were 100 mg of a ground sample with particle size < 315 mm, dilution in a liquid-phase composed of 10% w/w glycerol and 5.0% w/w nitric acid solutions, a sonication time of 2 min and the final slurry volume of 10.0 mL. A detection limit of 9.1 ug kg(-1) and characteristic mass of 7.6 pg were achieved using the suggested method under the optimized experimental conditions. Sufficient analyte stabilization was achieved by using 1 ug Pd and 50 ug citric acid. Accurate data were obtained with the use of matrix-free calibration. The accuracy of the method was established by analysing NIST SRM 1486 Bone Meal. Further, the results acquired for ten river otter samples by slurry sampling were compared with those determined after microwave-assisted digestion by inductively coupled plasma time of flight mass spectrometry (TOF-ICP-MS) to assess the accuracy of the method. The results obtained by the two methods were compared using a paired t-test (at the 95% confide Lead determination; Bone analysis; High-resolution continuum source AAS; Electrothermal atomic absorption spectrometry; Matrix effects; Design of experiments; Microwave-assisted digestion; Inductively coupled plasma mass spectrometry

Departments

Other Parts

Map

en.mapy.cz

Services

Popular Links

© 2023 University of Pardubice, Studentská 95, 532 10 Pardubice 2
Phone: +420 466 036 111, 466 036 112, 466 036 113
Webmaster, RSS
Data box ID: f5vj9hu
Accessibility Statement
CC BY-NC-ND 4.0Creative CommonsAttributionNonCommercialNoDerivatives