scholarly journals Determination of Magnesium and Calcium in Foods by Atomic Absorption Spectrometry after Microwave Digestion: NMKL Collaborative Study

1998 ◽  
Vol 81 (6) ◽  
pp. 1202-1208 ◽  
Author(s):  
Kaare Julshamn ◽  
Amund Maage ◽  
Harriet C Wallin ◽  
◽  
S Lierhagen ◽  
...  
Keyword(s):  
Atomic Absorption Spectrometry ◽  
Atomic Absorption ◽  
Microwave Digestion ◽  
Collaborative Study ◽  
Milk Powder ◽  
General Meeting ◽  
Absorption Spectrometry ◽  
Relative Standard ◽  
Standard Deviations ◽  
High Concentrations

Abstract On the basis of results of the performed collaborative study, the 49th Annual General Meeting of the Nordic Committee on Food Analysis (NMKL) in The Faroe Islands, August 1995, approved this method to be printed and included in NMKL's collection of methods of analysis of foods. Eleven laboratories participated in an interlaboratory methods-performance (collaborative) study of a method for determining magnesium and calcium in foodstuffs by atomic absorption spectrometry (AAS) after wet microwave digestion. The study was preceded by a practice round of familiarization samples. The method was tested on 7 materials: 5 foods (apple, milk powder, minced fish, wheat bran, and chocolate cake) and 2 composite diets ranging in Mg content from 240 to 3900 mg/kg and in Ca content from 290 to 9300 mg/kg. The materials were presented to study participants as blind duplicates, and participants were asked to perform single determinations on each sample. Repeatability relative standard deviations (RSDr) ranged from 1.9 to 4.9% for Mg and from 2.2 to 8.1 % for Ca. Reproducibility relative standard deviations (RSDR) ranged from 4.0 to 13% for Mg and from 5.9 to 23% for Ca. For Ca, lowest RSDR values were found for samples with high concentrations of Ca (>3800 mg/kg sample) and with nitrate ion residues of <1.3% (w/v).

scholarly journals Determination of Lead, Cadmium, Zinc, Copper, and Iron in Foods by Atomic Absorption Spectrometry after Microwave Digestion: NMKL1 Collaborative Study

2000 ◽  
Vol 83 (5) ◽  
pp. 1189-1203 ◽  
Author(s):  
Lars Jorhem ◽  
Joakim Engman ◽  
B-M Arvidsson ◽  
B Åsman ◽  
C Åstrand ◽  
...  
Keyword(s):  
Atomic Absorption Spectrometry ◽  
Atomic Absorption ◽  
Tissue Sample ◽  
Certified Reference Materials ◽  
Microwave Digestion ◽  
Collaborative Study ◽  
Absorption Spectrometry ◽  
Relative Standard ◽  
Cadmium Zinc

Abstract A method for determination of lead, cadmium, zinc, copper, and iron by atomic absorption spectrometry (AAS) after microwave digestion was subjected to a collaborative study in which 16 laboratories participated [including users of inductively coupled plasma (ICP) and ICP–mass spectrometry (MS)]. The types of samples included in the study were minced fish, wheat bran, milk powder, bovine and pig liver, mushroom, 2 simulated diets, and bovine muscle; the last 4 were certified reference materials. These were analyzed as single (4 samples), double blind (1 sample), or split level (2 samples) samples. Before the collaborative study, a pretrial was conducted in which 4 ready-made solutions and one fish tissue sample were analyzed for Pb and Cu. The reproducibility relative standard deviation (RSDR) values, for results above the detection limit, ranged from 59% at 0.155 mg/kg to 16% at 1.62 mg/kg for Pb, from 28% at 0.0124 mg/kg to 11% at 0.482 mg/kg for Cd, from 9.3% at 35.3 mg/kg to 1.7% at 147 mg/kg for Zn, from 39% at 0.241 mg/kg to 3.0% at 63.4 mg/kg for Cu, and from 17% at 7.4 mg/kg to 5.9% at 303 mg/kg for Fe. The RSDR values agreed well with the norms described by the International Union of Pure and Applied Chemistry. As a complement to the AAS determinations, a number of laboratories analyzed the samples either by ICP or by ICP–MS. The results of these analyses agreed well with the AAS results. On the basis of the results of the collaborative study, the method was adopted Official First Action by AOAC INTERNATIONAL.

scholarly journals Determination of Metals in Foods by Atomic Absorption Spectrometry after Dry Ashing: NMKL1 Collaborative Study

2000 ◽  
Vol 83 (5) ◽  
pp. 1204-1211 ◽  
Author(s):  
Lars Jorhem ◽  
G Afthan ◽  
G Cumont ◽  
H P Dypdahl ◽  
K Gadd ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Atomic Absorption Spectrometry ◽  
Atomic Absorption ◽  
Collaborative Study ◽  
Milk Powder ◽  
Absorption Spectrometry ◽  
Relative Standard ◽  
Dry Ashing ◽  
Zinc Concentrations

Abstract A method for determination of lead, cadmium, zinc, copper, and iron in foods by atomic absorption spectrometry (AAS) after dry ashing at 450°C was collaboratively studied in 16 laboratories. The study was preceded by a practice round of familiarization samples and another round in which solutions were distributed and the metals were determined directly by AAS. The study included 5 different foods (liver paste, apple sauce, minced fish, wheat bran, and milk powder) and 2 simulated diets. A single analysis was carried out with each sample. Suitable sample combinations were used as split-level combinations for determination of the repeatability standard deviation. The reproducibility relative standard deviation for each of the elements ranged from 20 to 50% for lead concentrations of 0.040–0.25 mg/kg, from 12 to 352% for cadmium concentrations of 0.001–0.51 mg/kg, from 4 to 8% for zinc concentrations of 0.7–38 mg/kg, from 7 to 45% for copper concentrations of 0.51–45 mg /kg, and from 11 to 14% for iron concentrations of 4–216 mg/kg.

scholarly journals Determination of Arsenic in Seafood by Electrothermal Atomic Absorption Spectrometry after Microwave Digestion: NMKL Collaborative Study

2000 ◽  
Vol 83 (6) ◽  
pp. 1423-1428 ◽  
Author(s):  
Kaare Julshamn ◽  
Arngriimur Thorlacius ◽  
Per Lea ◽  
Kjetil Barland ◽  
Kari Eidem ◽  
...  
Keyword(s):  
Atomic Absorption Spectrometry ◽  
Atomic Absorption ◽  
Blue Mussel ◽  
Collaborative Study ◽  
Electrothermal Atomic Absorption Spectrometry ◽  
Absorption Spectrometry ◽  
Method Performance ◽  
Relative Standard ◽  
Standard Deviations

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.

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 ◽  
...  
Keyword(s):  
Atomic Absorption Spectrometry ◽  
Atomic Absorption ◽  
Flame Atomic Absorption Spectrometry ◽  
Collaborative Study ◽  
Absorption Spectrometry ◽  
Method Performance ◽  
Flame Atomic Absorption ◽  
Relative Standard ◽  
Standard Deviations

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.

scholarly journals Application of atomic absorption spectrometry with continuous light source to analyze selected metals important for human health in different parts of oranges

2014 ◽  
Vol 27 (3) ◽  
pp. 145-147
Author(s):  
Wojciech Szwerc ◽  
Ireneusz Sowa
Keyword(s):  
Atomic Absorption Spectrometry ◽  
Atomic Absorption ◽  
Microwave Digestion ◽  
Continuous Light ◽  
Absorption Spectrometry ◽  
Citrus Fruits ◽  
Continuum Source ◽  
Relative Standard ◽  
Validation Parameters ◽  
Different Origins

ABSTRACT The publication describes the application of high-resolution continuum source atomic absorption spectrometry (H-R CS AAS) to determine some physiologically essential and toxic elements occurring in citrus fruits of different origins. Before analysis, the samples were mineralized using a mixture of deionized water and 69% nitric acid 3:1 (v/v) in high pressure microwave digestion at 188°C during one hour. The obtained validation parameters for AAS such as high linearity (the correlation coefficient R > 0.997) and high precision expressed as relative standard deviation (%RSD) were satisfactory for quantification. Cadmium at concentration range from 0.29 to 0.43 mg/kg was determined in all tested samples, however the obtained values did not exceed Polish standards. The higher concentration of potassium comparing to sodium and calcium was noted in each investigated samples. The highest variation was observed for calcium, its concentration strongly depended on the country of origin.

scholarly journals Optimization of Selenium Determination in Human Milk and Whole Blood by Flow Injection Hydride Atomic Absorption Spectrometry

1998 ◽  
Vol 81 (2) ◽  
pp. 457-461 ◽  
Author(s):  
Amparo Alegría ◽  
Reyes Barberá ◽  
Rosaura Farré ◽  
Emilia Ferrer ◽  
M Jesús Lagarda ◽  
...  
Keyword(s):  
Human Milk ◽  
Atomic Absorption Spectrometry ◽  
Atomic Absorption ◽  
Flow Injection ◽  
Whole Blood ◽  
Microwave Digestion ◽  
Milk Powder ◽  
Absorption Spectrometry ◽  
Sample Volume ◽  
Selenium Determination

abstract A flow injection hydride atomic absorption spectrometry (FI-HAAS) method was developed for determining selenium in human milk and whole blood after microwave digestion of the sample. The sample (2 mL human milk or 0.25 mL blood) was introduced into the microwave vessel with 1.5 mL HN03 and 0.25 mL H202 and 300 W (4 min) and 600 W (4 min) were applied. The digestion was completed by heating to 140 C (2-3 h). Se (VI) was reduced to Se (IV) with hydrochloric acid. The instrumental conditions for FI-HAAS (concentrations of reducing agent and carrier acid, flow rate of argon carrier gas, and sample volume injected) were optimized. The detection limit of the proposed method was 0.23 ng/mL (assay) or 115 pg Se (absolute) in biological samples (1.15 ng/mL milk, 10.4 ng/mL blood). The precision values were 5.0% for milk and 4.0% for blood. The accuracy was evaluated with 2 reference materials, National Institute of Standards and Technology Non-Fat Milk Powder (found: 104.3 ± 7.2 ng/g, certified: 110 ± 10 ng/g) and Whole Blood Seronorm (found: 81 ± 7.3 ng/mL, reference: 83 ± 4 ng/mL). The results show the suitability of the method for selenium determination in human milk and whole blood. The method was applied to whole blood samples obtained from pregnant women and to human milk.

scholarly journals Determination of Mercury in Seafood by Flow Injection–Cold Vapor Atomic Absorption Spectrometry after Microwave Digestion: NMKL Interlaboratory Study

2002 ◽  
Vol 85 (3) ◽  
pp. 626-631 ◽  
Author(s):  
Kaare Julshamn ◽  
Jan Brenna ◽  
B Åsman ◽  
A Ekman ◽  
A El-Ghauoui ◽  
...  
Keyword(s):  
Atomic Absorption Spectrometry ◽  
Atomic Absorption ◽  
Flow Injection ◽  
Absorption Spectrometry ◽  
Method Performance ◽  
Cold Vapor ◽  
Cold Vapor Atomic Absorption ◽  
Relative Standard ◽  
Standard Deviations

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.

scholarly journals Trace Arsenic Determination in a TiO2 Pigment Matrix Using Electrothermal Atomic Absorption Spectrometry

2019 ◽  
Vol 25 (2) ◽  
pp. 123-131
Author(s):  
Matjaž Finšgar ◽  
Tamara Govejšek ◽  
Ksenija Gradišek
Keyword(s):  
Atomic Absorption Spectrometry ◽  
Atomic Absorption ◽  
Microwave Digestion ◽  
Pyrolytic Graphite ◽  
Electrothermal Atomic Absorption Spectrometry ◽  
Absorption Spectrometry ◽  
Calibration Procedure ◽  
Chemical Modifier ◽  
Relative Standard ◽  
Arsenic Determination

This work describes the use of electrothermal atomic absorption spectrometry in combination with a pyrolytic graphite-coated tube with a platform for trace arsenic (As) determination in titanium dioxide (TiO2) pigment. This type of matrix is challenging, as complete digestion in hydrofluoric acid-containing solution is needed. First, closed-vessel microwave digestion was performed for the full-sample decomposition. Next, a temperature program was optimized for drying, pyrolysis, and atomization temperatures. Furthermore, the use of a chemical modifier mixture was proposed that reduced the background contribution and prevented significant analyte loss and therefore improved the analytical procedure. The optimized method was validated for the detection (LOD) and quantification (LOQ) limits, the linear concentration range, accuracy, and precision. Special attention was devoted to the matrix-matching solutions in the calibration procedure. Linearity was confirmed in the 5.0 to 100.0 µg/L concentration range ( R2 = 0.999). The average recovery for 16 different real TiO2 pigment samples was 92.0%, and the relative standard deviation value for six replicate measurements was ≤10.4%. Moreover, the LOD and LOQ in terms of the TiO2 pigment mass was determined to be 0.2 µg/(g TiO2) and 0.7 µg/(g TiO2), respectively. The latter complies with Commission Directive 2008/128/EC, which does not allow more than 3 µg As/(g product) as the specific criteria of purity. Finally, based on scanning electron microscopy analysis of unused and several times used pyrolytic graphite-coated tubes, usage of the tube 250 times before replacement is recommended.

scholarly journals Determination of cobalt in water samples by atomic absorption spectrometry after pre-concentration with a simple ionic liquid-based dispersive liquid-liquid micro-extraction methodology

2010 ◽  
Vol 8 (3) ◽  
pp. 617-625 ◽  
Author(s):  
Hossein Abdolmohammad-Zadeh ◽  
Elnaz Ebrahimzadeh
Keyword(s):  
Ionic Liquid ◽  
Atomic Absorption Spectrometry ◽  
Atomic Absorption ◽  
Water Samples ◽  
Limit Of Detection ◽  
Absorption Spectrometry ◽  
Experimental Conditions ◽  
Flame Atomic Absorption ◽  
Relative Standard

AbstractA rapid dispersive liquid-liquid micro-extraction (DLLME) methodology based on the application of 1-hexylpyridinium hexafluorophosphate [C6py][PF6] ionic liquid (IL) as an extractant solvent was applied for the pre-concentration of trace levels of cobalt prior to determination by flame atomic absorption spectrometry (FAAS). 1-Phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) was employed as a chelator forming a Co-PMBP complex to extract cobalt ions from aqueous solution into the fine droplets of [C6py][PF6]. Some effective factors that influence the micro-extraction efficiency include the pH, the PMBP concentration, the amount of ionic liquid, the ionic strength, the temperature and the centrifugation time which were investigated and optimized. In the optimum experimental conditions, the limit of detection (3s) and the enrichment factor were 0.70 µg L−1 and 60, respectively. The relative standard deviation (RSD) for six replicate determinations of 50 µg L−1 Co was 2.36%. The calibration graph using the pre-concentration system was linear at levels 2–166 µg L−1 with a correlation coefficient of 0.9982. The applicability of the proposed method was evaluated by the determination of trace amounts of cobalt in several water samples.

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