Study of parameters associated with the determination of cadmium in lake sediments by slurry sampling electrothermal atomic absorption spectrometry

被引:20
作者
Baralkiewicz, D [1 ]
Gramowska, H [1 ]
机构
[1] Adam Mickiewicz Univ, Fac Chem, PL-60780 Poznan, Poland
关键词
cadmium; lake sediments; slurry; sampling electrothermal atomic absorption spectrometry;
D O I
10.1016/j.aca.2004.01.001
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
Cadmium concentration in lake sediments is determined by suspending the solid samples in a solution containing 5% (v/v) concentrated nitric acid and 0.1% (v/v) Triton X-100. Three modifiers were tested for the direct determination. The furnace temperature programmes and appropriate amount for each modifier were optimised to get the highest signal and the best separation between the atomic and background signals. The drying stage is performed by programming a 400degreesC temperature, a ramp time of 25 s and hold time of 10 s on the power supply of the atomiser. No ashing step is used and platform atomisation is carried out at 2200degreesC. W-Rh permanent modifier combined with conventional modifier by delivering 10 mul of 0.50% (w/v) NH4H2PO4 solution was the best chemical modifier for cadmium determination. This modifier also acts as a liquid medium for the slurry, thus simplifying the procedure. Calibration is performed using aqueous standards in the 1-5 mug l(-1) range. The optimised method gave a limit of detection of 0.56 ng ml(-1), characteristic mass of 10.1 +/- 0.8 pg for aqueous standard, 9.6 +/- 0.7 pg for slurry samples containing different Cd concentrations and good precision (7.6-5.2%). The method was validated by analysing four certified reference lake sediment materials: LKSD-1, LKSD-2, LKSD-3 and LKSD-4; satisfactory recoveries were obtained (90.0-96.3%) and no statistical differences were observed between the experimental and the certified cadmium concentration. The developed methodology was used to determine cadmium in three 'real' sediment samples from lakes in the area of Wielkopolski National Park, Poland. (C) 2004 Elsevier B.V. All rights reserved.
引用
收藏
页码:249 / 256
页数:8
相关论文
共 37 条
[1]   Ultrasound-assisted extraction of lead from solid samples: a new perspective on the slurry-based sample preparation methods for electrothermal atomic absorption spectrometry [J].
Amoedo, L ;
Capelo, JL ;
Lavilla, I ;
Bendicho, C .
JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, 1999, 14 (08) :1221-1226
[2]  
Baralkiewicz D, 2002, CHEM ANAL-WARSAW, V47, P457
[3]   Fast determination of lead in lake sediment samples using electrothermal atomic absorption spectrometry with slurry samples introduction [J].
Baralkiewicz, D .
TALANTA, 2002, 56 (01) :105-114
[4]   Slurry sampling for electrothermal atomic absorption spectrometric determination of chromium, nickel, lead and cadmium in sewage sludge [J].
Baralkiewicz, D ;
Siepak, J .
ANALYTICA CHIMICA ACTA, 2001, 437 (01) :11-16
[5]   The use of chemical modifiers in the determination of cadmium in sewage sludge and tin in PVC by solid sampling-graphite furnace atomic absorption spectrometry [J].
Belarra, MA ;
Resano, M ;
Rodríguez, S ;
Urchaga, J ;
Castillo, JR .
SPECTROCHIMICA ACTA PART B-ATOMIC SPECTROSCOPY, 1999, 54 (05) :787-795
[6]   SOLID SAMPLING IN ELECTROTHERMAL ATOMIC-ABSORPTION SPECTROMETRY USING COMMERCIAL ATOMIZERS - A REVIEW [J].
BENDICHO, C ;
DELOOSVOLLEBREGT, MTC .
JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, 1991, 6 (05) :353-374
[7]   Factorial designs for Cd, Cr, Hg, Pb and Se ultrasound-assisted acid leaching from human hair followed by atomic absorption spectrometric determination [J].
Bermejo-Barrera, P ;
Moreda-Piñeiro, A ;
Bermejo-Barrera, A .
JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, 2000, 15 (02) :121-130
[8]   Slurry sampling electrothermal atomic absorption spectrometric determination of lead, cadmium and manganese in human hair samples using rapid atomizer programs [J].
BermejoBarrera, P ;
MoredaPineiro, A ;
MoredaPineiro, J ;
BermejoBarrera, A .
JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, 1997, 12 (03) :301-306
[9]  
BERNE JB, 1976, DYNAMIC LIGHT SCATTE
[10]  
Brown W., 1993, DYNAMIC LIGHT SCATTE