Slurry Sampling-Microwave Assisted Leaching Prior to Hydride Generation-Pervaporation-Atomic Fluorescence Detection for the Determination of Extractable Arsenic in Soil

2003 ◽  
Vol 75 (9) ◽  
pp. 2011-2017 ◽  
Author(s):  
A. Caballo-López ◽  
M. D. Luque de Castro
2012 ◽  
Vol 610-613 ◽  
pp. 1991-1995
Author(s):  
Mei Sun ◽  
Gui Jiang Liu ◽  
Qiang Hua Wu ◽  
Wenqi Liu

A new method was developed for the speciation of inorganic arsenic in coal samples by liquid chromatography coupled to hydride generation atomic fluorescence spectrometry after microwave-assisted extraction. Effective extract of As(III), As(V) in coal sample was achieved by 1.0molL-1 H3PO4 and 0.1 molL-1ascorbic acid. Under the optimized conditions, the limits of detection were 0.01 ugL-1and 0.02 ugL-1for As(III), As(V). The relative standard deviation were 2.4 %, 3.3 % (c= 20.0 gL-1, n=7). The proposed method was successfully applied for the determination of speciation of inorganic arsenic in coal samples and GBW11117.


2003 ◽  
Vol 86 (4) ◽  
pp. 815-822 ◽  
Author(s):  
Patricia Cava-Montesinos ◽  
M Luisa Cervera ◽  
Agustín Pastor ◽  
Miguel de la Guardia

Abstract A sensitive procedure was developed for determination of bismuth (Bi) in milk samples by hydride generation atomic fluorescence spectrometry (HG–AFS) after microwave-assisted sample digestion with HNO3 and H2O2. The method provides a sensitivity of 1832 fluorescence units (ng/mL) with a detection limit of 0.01 ng/mL, which corresponds to 20 pg absolute limit of detection, equivalent to 0.50 ng/g in the original sample. Application of the methodology to cow milk samples from the Spanish market showed the presence of Bi at a concentration of 11.8–28.8 ng/g, which compared well with data obtained after dry ashing of samples and with data obtained by inductively coupled plasma–mass spectrometry after microwave-assisted digestion.


2004 ◽  
Vol 57 (10) ◽  
pp. 937 ◽  
Author(s):  
Bronwyn D. Wake ◽  
Edward C. V. Butler ◽  
Alison M. Featherstone ◽  
Patti Virtue ◽  
Bernard Averty ◽  
...  

A method based on hydride generation with cryogenic trapping and atomic fluorescence detection was developed that is capable of determining both inorganic Se species (SeIV and SeVI) while at sea. Evaluation of the system for optimal performance was made for each stage of the analysis and detection sequence, as well as for the SeVI reduction step. A detection limit of 0.4 ng L−1 Se in a 10 mL sample was achieved using this method. Precision was better than 3.5% for 25, 100, and 1000 ng L−1 SeIV standard solutions. Accuracy was determined by recovery studies using natural samples and a certified reference seawater (NASS-5).


1995 ◽  
Vol 10 (11) ◽  
pp. 969 ◽  
Author(s):  
Alessandro D'ulivo ◽  
Leonardo Lampugnani ◽  
Giovanna Pellegrini ◽  
Roberto Zamboni

Author(s):  
Chandrasekaran Krishnan ◽  
Venkata Balarama Krishna Mullapudi ◽  
Nidhi Garg

A single-step microwave assisted digestion (MWAD) procedure employing very dilute solutions of HNO3 was developed for the quantitative determination of bismuth in bismuth-containing pharmaceuticals by hydride generation-atomic fluorescence spectrometry (HG-AFS). Experimental parameters affecting MWAD process such as acid concentration (HNO3), digestion time and temperature were optimized to get quantitative recovery of bismuth. The studies indicated that the method is rapid (within 15 min) including cooling time and recovery > 98% was obtained using 10mL of 5% (v/v) HNO3 as digestion medium with ~0.1g of sample. The optimum microwave digestion parameters obtained were: temperature – 180oC, pressure – 25 bar and hold time - 10 min. A clear solution with negligible residue was obtained after microwave digestion. The digested sample solution was appropriately diluted with 2% (v/v) HCl for subsequent analysis by HG-AFS. The reproducibility, expressed as % RSD was lower than 2% for the allopathic medicine. Under optimal conditions, the limit of detection (LOD) for Bi was calculated to be 0.024mg/kg. The methodology was optimized using a bismuth-containing pharmaceutical – Pylobis, purchased from a local pharmacy. The optimized MWAD approach was further applied to few other bismuth-containing pharmaceutical products. The developed method has significant advantages when compared to the conventional hot-plate digestion methods reported for Bi-containing pharmaceuticals, employing large volumes of concentrated acids. These investigations revealed that the proposed MWAD method in combination with HG-AFS can be utilized for the rapid determination of Bi in pharmaceutical products on regular basis.


Talanta ◽  
2004 ◽  
Vol 62 (1) ◽  
pp. 173-182 ◽  
Author(s):  
Patricia Cava-Montesinos ◽  
M.Luisa Cervera ◽  
Agustı́n Pastor ◽  
Miguel de la Guardia

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