Collaborative Study on Ashing: 1969

1970 ◽  
Vol 53 (5) ◽  
pp. 926-927
Author(s):  
Joseph Kowalczuk

Abstract A collaborative study evaluated the effect of wet vs. dry ashing on the atomic absorption determination of calcium, iron, magnesium, manganese, and zinc in feeds. Ten laboratories analyzed 6 samples. The high relative standard deviations indicate that ashing methods should be further studied.

2019 ◽  
Vol 85 (2) ◽  
pp. 12-16
Author(s):  
I. V. Saunina ◽  
E. N. Gribanov ◽  
E. R. Oskotskaya

The sorption of Hg (II), Cd (II), and As (III) by natural aluminosilicate is studied. It is shown that the mineral absorbs those toxicants in a rather wide pH range, quantitative extraction of analytes being achieved in a neutral or close to neutral medium (pH values range within 7.0 - 8.0; 6.3 - 7.5; 7.4 - 8.5 for Hg (II), As (III), and Cd (II), respectively). The effect of the time of phase contact on the degree of extraction of elements is shown. The sorption capacity of the mineral in optimal conditions of the medium acidity (0.06 mmol/g for mercury, 0.31 mmol/g for cadmium, and 0.52 mmol/g for arsenic) is determined. The distribution coefficients attain values of aboutnX 103-nX 104. A new combined method for determination of Hg (II), Cd (II), and As (III) in natural and waste water is developed and tested. The method consists in a preliminary group sorption concentration of the analytes by aluminosilicate, desorption of the analytes from the surface of the mineral and their subsequent atomic absorption determination. The correctness of the method is verified in analysis of spiked samples. The method is easy to use and exhibits high sensitivity, reproducibility and accuracy of analyte determination. The relative standard deviation does not exceed 0.13. Economic availability and possibility of using domestic sorption materials are the important advantages of the proposed procedure which can be used in the practice of laboratories monitoring the quality and safety of environmental objects.


1989 ◽  
Vol 72 (3) ◽  
pp. 484-486
Author(s):  
William G Brumbaugh ◽  
Michael J Walther

Abstract A combined wet chemical and dry ash digestion and use of a continuous- flow hydride generator coupled with a flame-heated quartz cell enabled the simple, precise, and highly automated atomic absorption determination of arsenic and selenium in tissues of whole fish. Percent relative standard deviation averaged 4% for each element; method detection limits (μg/g dry wt) were about 0.06 for arsenic and 0.04 for selenium. Digestion of samples proceeded with little operator attention and without perchloric acid. Analysis for arsenic as As(V) simplified sample preparation but care had to be exercised to avoid interferences from high concentrations of selenium.


2000 ◽  
Vol 83 (5) ◽  
pp. 1204-1211 ◽  
Author(s):  
Lars Jorhem ◽  
G Afthan ◽  
G Cumont ◽  
H P Dypdahl ◽  
K Gadd ◽  
...  

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.


1990 ◽  
Vol 73 (5) ◽  
pp. 721-723
Author(s):  
Robert D Parker

Abstract An atomic absorption spectrophotometric method for determination of polydimethylsiloxane (PDMS) residues In pineapple juice was collaboratively studied by 9 laboratories. PDMS residues are extracted from pineapple Juice with 4- methyl-2-pentanone and the extracted silicone Is measured by atomic absorption spectrophotometry using a nitrous oxide/ acetylene flame. Collaborators analyzed 5 samples Including 1 blind duplicate. Reproducibility relative standard deviations (RSDR) were 13.1% at 31 ppm, 6.9% at 18 ppm, 14.8% at 7.9 ppm, and 16.1 % at 4.9 ppm PDMS. The method has been approved Interim official first action by AOAC.


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.


1964 ◽  
Vol 47 (4) ◽  
pp. 701-707
Author(s):  
Mary H Thompson

Abstract Wet-ash and dry-ash extraction methods for the flame photometric determination of sodium and potassium in fish and other marine products were studied collaboratively. The wet-ash method was more accurate primarily because potassium was lost during the dry-ashing procedure at 550°C. Statistical analyses of precision indicate that wetashing is equal to or superior to dryashing. The Associate Referee, using the wet-ash procedure, obtained 98% recoveries for sodium and 102% for potassium, and relative standard deviations of 1.3—2.2 for sodium, and 1.5—3.6 for potassium. Over-all average recoveries obtained by the collaborators were 112% for sodium and 96% for potassium. Collaborative study will be continued.


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.


1979 ◽  
Vol 62 (5) ◽  
pp. 1050-1053
Author(s):  
Edgar R Elkins ◽  
Arlene Sulek

Abstract Samples of green beans, applesauce, and a fruit juice were fortified with tin at 3 levels. Collaborators were asked to digest the samples, using HNO3-H2SO4, add methanol to enhance the absorption signal, and aspirate directly, using a nitrous oxide-acetylene flame. Results were received from 8 laboratories including 4 from Europe. However, only 6 laboratories used the prescribed methodology. All results were considered acceptable. The method has been adopted as interim official first action.


2010 ◽  
Vol 75 (5) ◽  
pp. 669-679 ◽  
Author(s):  
Tayyebeh Madrakian ◽  
Ali Zolfigol ◽  
Fathemeh Aboulghazi

A preconcentration method was developed for the determination of trace amounts of Co, Ni, Cd and Zn by atomic absorption spectrometry. The method is based on the retention of the metal cations by naphthalene- 2,4,6-trimorpholino-1,3,5-triazin adsorbent in a column. The adsorbed metals were then eluted from the column with hydrochloric acid and the Co, Ni, Cd and Zn were determined by flame atomic absorption spectrometry. The optimal extraction and elution conditions were studied. The effects of diverse ions on the preconcentration were also investigated. A preconcentration factor of 250 for Co(II), Ni(II) and Zn(II), and 400 for Cd(II) can easily be achieved. Calibration graphs were obtained and the detection limits of the method for Co(II), Ni(II), Cd(II) and Zn(II) were 0.51, 0.49, 0.17 and 0.10 ng mL-1, respectively. The relative standard deviations (RSD) of 0.37-2.31 % for Co, 0.37-3.73 % for Ni, 2.20-2.40% for Cd and 1.50-2.56% for Zn were obtained. The method was also used for the simultaneous preconcentration of these elements and the method was successfully applied to their preconcentration and determination. The method was applied to the determination of Co, Ni, Cd and Zn in several real samples.


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