scholarly journals Determination of Sodium in Foods by Flame Atomic Absorption Spectrometry after Microwave Digestion: NMKL Interlaboratory Study

2005 ◽  
Vol 88 (4) ◽  
pp. 1212-1216 ◽  
Author(s):  
Kaare Julshamn ◽  
Per Lea ◽  
Hilde Skaar Norli ◽  
S Floren ◽  
T Furnes ◽  
...  

Abstract Nine laboratories participated in an interlaboratory method performance (collaborative) study of a method for the determination of sodium in foods by flame atomic absorption spectrometry after wet digestion, using a microwave oven technique. Before the study, the laboratories were able to practice on samples with defined sodium levels (pretrial test). The method was tested on a total of 6 foods (broccoli, carrot, bread, saithe fillet, pork, and cheese) with sodium concentrations of 1480–8260 mg/kg. The materials were presented to the participants in the study as blind duplicates, and the participants were asked to perform single determinations for each sample. The repeatability relative standard deviations (RSDr) for sodium ranged from 1.9 to 6.5%. The reproducibility relative standard deviations (RSDR) ranged from 4.2 to 6.9%. The HorRat values ranged from 0.9 to 1.6.

2000 ◽  
Vol 83 (6) ◽  
pp. 1423-1428 ◽  
Author(s):  
Kaare Julshamn ◽  
Arngriimur Thorlacius ◽  
Per Lea ◽  
Kjetil Barland ◽  
Kari Eidem ◽  
...  

Abstract Eight laboratories participated in an interlaboratory method performance (collaborative) study of a method for the determination of arsenic in foodstuffs of marine origin by electrothermal atomic absorption spectrometry after wet digestion using a microwave oven technique. The study was preceded by a practice round of familiarization samples. The method was tested on 8 materials (cod roe, krill, blue mussel, saithe, scampi, cod fillet, shrimp, and cod extract) ranging in As content from 2 to 75 mg/kg. The materials were sent to participants in the study as blind duplicates, and the participants were asked to perform single determinations on each sample. Repeatability relative standard deviations (RSDr) for As ranged from 6.8 to 17.4%. Reproducibility relative standard deviations (RSDR) ranged from 7.6 to 24%. The highest RSDR value was found for the sample with the highest concentration of As.


2008 ◽  
Vol 91 (6) ◽  
pp. 1446-1452 ◽  
Author(s):  
Saeed Hajialigol ◽  
Mohammad Ali Taher ◽  
Akbar Malekpour

Abstract Natural clinoptilolite was used as a sorbent material for solid-phase extraction and preconcentration of zinc. Clinoptilolite was first saturated with cadmium (II) and then modified with benzyldimethyltetradecylammonium chloride for increasing adsorption of 3-(2-arsenophenylazo)-4,5-dihydroxy-2,7-naphthalene disulfonic acid (neothorin). Zinc was quantitatively retained on the adsorbent by the column method in the pH range of 3.84.2 at a flow rate of 1 mL/min. It was eluted from the column with 5.0 mL 2 M nitric acid solution at a flow rate of 1 mL/min and determined by flame atomic absorption spectrometry at 213.9 nm. Zinc could be concentrated from a 0.03 g/L solution with a preconcentration factor of 170. Relative standard deviation for 8 replicate determinations of 2.5 g zinc in the final solution was 0.92. The interference of a large number of anions and cations was studied in detail to optimize the conditions, and the method was successfully applied for determination of zinc in standard and real water samples.


2002 ◽  
Vol 85 (3) ◽  
pp. 626-631 ◽  
Author(s):  
Kaare Julshamn ◽  
Jan Brenna ◽  
B Åsman ◽  
A Ekman ◽  
A El-Ghauoui ◽  
...  

Abstract Ten laboratories participated in an interlaboratory method-performance (collaborative) study of a method for the determination of mercury in foods of marine origin by flow injection–cold vapor atomic absorption spectrometry after wet digestion using a microwave oven technique. The study was preceded by a training round of samples of known identity. The method was tested on a total of 7 seafood products: blue mussel (Mytilus edulis), cod muscle (Gadus morhua), crab (Cancer pagurus), scampi (Nephrops norwegicus), black scabbard fish (Aphnopus carbo), longnose velvet dogfish (Centroscymus crepidater), and Portuguese dogfish (Cenbroscymus coelolepis) with mercury concentrations of 0.14, 0.24, 0.35, 0.59, 1.42, 4.2, and 13.2 μg/g, respectively. The materials were presented to the participants in the study as blind duplicates, and the participants were asked to perform single determinations on each sample. Repeatability relative standard deviations (RSDr) for mercury ranged from 2.4 to 14.0%. Reproducibility relative standard deviations (RSDR) ranged from 7.7 to 16.6%. HORRAT values for all samples were <1.0.


2018 ◽  
Vol 35 (4) ◽  
pp. 87
Author(s):  
Renata Toledo Lima ◽  
Jorge Luiz Raposo Júnior ◽  
Alex Virgílio ◽  
José Anchieta Gomes Neto

This work describes a method to determine Cu at wide range concentrations in a single run without need of further dilutions employing high-resolution continuum source flame atomic absorption spectrometry. Different atomic lines for Cu at 324.754 nm, 327.396 nm, 222.570 nm, 249.215 nm and 224.426 nm were evaluated and main figures of merit established. Absorbance measurements at 324.754 nm, 249.215 nm and 224.426 nm allows the determination of Cu in the 0.07 – 5.0 mg L-1, 5.0 – 100 mg L-1 and 100 – 800 mg L-1 concentration intervals respectively with linear correlation coefficients better than 0.998. Limits of detection were 21 μg L-1, 310 μg L-1 and 1400 μg L-1 for 324.754 nm, 249.215 nm and 224.426 nm, respectively and relative standard deviations (n = 12) were £ 2.7%. The proposed method was applied to water samples spiked with Cu and the results were in agreement at a 95% of confidence level (paired t-test) with those obtained by line-source flame atomic absorption spectrometry.


2010 ◽  
Vol 35 (4) ◽  
pp. 87-92 ◽  
Author(s):  
Renata Toledo Lima ◽  
Jorge Luiz Raposo Jr. ◽  
Alex Virgílio ◽  
José Anchieta Gomes Neto

This work describes a method to determine Cu at wide range concentrations in a single run without need of further dilutions employing high-resolution continuum source flame atomic absorption spectrometry. Different atomic lines for Cu at 324.754 nm, 327.396 nm, 222.570 nm, 249.215 nm and 224.426 nm were evaluated and main figures of merit established. Absorbance measurements at 324.754 nm, 249.215 nm and 224.426 nm allows the determination of Cu in the 0.07 - 5.0 mg L-1, 5.0 - 100 mg L-1 and 100 - 800 mg L-1 concentration intervals respectively with linear correlation coefficients better than 0.998. Limits of detection were 21 µg L-1, 310 µg L-1 and 1400 µg L-1 for 324.754 nm, 249.215 nm and 224.426 nm, respectively and relative standard deviations (n = 12) were £ 2.7%. The proposed method was applied to water samples spiked with Cu and the results were in agreement at a 95% of confidence level (paired t-test) with those obtained by line-source flame atomic absorption spectrometry.


2002 ◽  
Vol 85 (6) ◽  
pp. 1410-1414 ◽  
Author(s):  
Ricardo Fernández Orsi ◽  
Rodolfo G Wuilloud ◽  
Jorgelina C A de Wuilloud ◽  
Roberto A Olsina ◽  
Luis D Martinez

Abstract An on-line cadmium preconcentration and determination system implemented with flame atomic absorption spectrometry (FAAS) associated with flow injection was studied. Cadmium was retained as Cd-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol Cd-(5-Br-PADAP) complex, pH 9.3. The Cd complex was removed from the knotted reactor (KR) with ethanol. A total enhancement factor of 140 was obtained with respect to FAAS (40 for KR and 3.5 due to the use of ethanol) with preconcentration time of 120 s. The detection limit value for preconcentration of 1 g sample was 0.5 ng/g. The repeatability for 10 replicate determinations at 5.0 ng/g Cd level was 3.5% relative standard deviation, calculated from peak heights obtained. The calibration graph using the preconcentration system for Cd was linear with a correlation coefficient of 0.9990 at levels near the detection limits to at least 2000 ng/g. The method was successfully applied to determination of total Cd in honey samples.


2013 ◽  
Vol 69 (3) ◽  
pp. 580-586 ◽  
Author(s):  
Lifen Meng ◽  
Jiaxi Cheng ◽  
Yaling Yang

A simple and practical extraction method of supramolecular solvents (SUPRAS) was developed for separation and enrichment of trace amounts of palladium (Pd) and silver (Ag) in water samples prior to flame atomic absorption spectrometry (FAAS) analysis. The SUPRAS selected was made up of an aqueous solution containing tetrahydrofuran and nonanoic acid. Pd and Ag reacted with diethyldithiocarbamate to form hydrophobic chelates, which were extracted into the vesicles of SUPRAS. Different parameters such as the concentration of chelating agent, sample pH, supramolecular solvent and the effect of foreign ions were studied. Under the optimal conditions, the linear ranges of Pd and Ag were from 10 to 1,000 μg/L. The relative recoveries of Pd and Ag in tap and river water samples at the spiking level of 10 ug/mL ranged from 90.8 to 116%. The relative standard deviations were 3.6–4.0% (n = 9), the limits of detection were 2.8 and 1.9 μg/L and the enrichment factors were 36 and 18 for Pd and Ag, respectively. The quantification limits were 3.2 and 2.4 μg/L. The method was successfully applied to the determination of Pd and Ag in water samples.


2014 ◽  
Vol 70 (12) ◽  
pp. 1913-1918 ◽  
Author(s):  
Lifen Meng ◽  
Jinyan Ning ◽  
Yaling Yang

A sensitive and simple method for flame atomic absorption spectrometry determination of traces of cadmium and chromium(III) species in water samples after preconcentration by cloud point extraction has been developed. A novel complex agent of alizarin complexone with cadmium (Cd) and chromium (Cr(III)) was quantitatively extracted in surface primary alcohol ethoxylate-rich phase at 33 °C. The effects of experimental conditions including pH of sample solution, concentration of chelating agent and salt, equilibration temperature and time, and foreign ions were evaluated in order to enhance sensitivity of the method. Under optimal conditions, the low limit detections were 6.7 and 3.2 μg/L, and the enrichment factors were 24 and 20 for Cd and Cr(III), respectively. The relative standard deviations were 3.8 and 2.5% for Cd and Cr(II), respectively (n = 11). The high recoveries of the spiked Cd and Cr(III) ions were obtained in the range of 90–116%. The proposed method has been successfully applied for the determination of Cd and Cr(III) in water samples.


2012 ◽  
Vol 535-537 ◽  
pp. 2591-2595
Author(s):  
Zhi Xi Gao ◽  
Yan Hong Wu ◽  
Yan Wen Luo ◽  
Qin Song Mu ◽  
Ke Hou Ao ◽  
...  

Temperature-controlled HNO3-H2O2 wet digestion and flame atomic absorption spectrometry (FAAS) were employed in the determination of mineral elements in the fermented liquid residue of livestock dung. The 8 most common mineral elements-K, Na, Fe, Mn, Cu, Zn, Ca and Mg-in fermented liquid were selected for analysis, and the experimental results showed that the correlation coefficient (r) of each mineral element’s quantitative standard curve was >0.9993, the quantitation limit was 0.90-67.0 ng/L, the relative standard deviation (RSD) was 0.79%-2.51%, and the standard addition recovery rate was 95%-103%. It was found that the average content of the 8 mineral elements in fermented liquid was in a descending order of K, Na, Ca, Mg, Fe, Mn, Zn and Cu.


2016 ◽  
Vol 2016 ◽  
pp. 1-8 ◽  
Author(s):  
Teslima Daşbaşı ◽  
Şenol Kartal ◽  
Şerife Saçmacı ◽  
Ahmet Ülgen

A dispersive liquid-liquid microextraction method for the determination of bismuth in various samples by flame atomic absorption spectrometry is described. In this method, crystal violet was used as counter positive ion forBiCl4-complex ion, chloroform as extraction solvent, and ethanol as disperser solvent. The analytical parameters that may affect the extraction efficiency like acidity of sample, type and amount of extraction and disperser solvents, amount of ligand, and extraction time were studied in detail. The effect of interfering ions on the analyte recovery was also investigated. The calibration graph was linear in the range of 0.040–1.00 mg L−1with detection limit of 4.0 μg L−1(n=13). The precision as relative standard deviation was 3% (n=11, 0.20 mg L−1) and the enrichment factor was 74. The developed method was applied successfully for the determination of bismuth in various water, pharmaceutical, and cosmetic samples and the certified reference material (TMDA-64 lake water).


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