Flameless atomic-absorption determination of impurities in high-purity silver after extractive separation of the matrix

1980 ◽  
Vol 300 (1) ◽  
pp. 28-32 ◽  
Author(s):  
E. A. Startseva ◽  
N. M. Popova ◽  
I. G. Yudelevich ◽  
N. G. Vanifatova ◽  
Yu. A. Zolotov
1980 ◽  
Vol 63 (3) ◽  
pp. 496-499 ◽  
Author(s):  
Nancy Thiex

Abstract This method for the determination of arsenic specifies wet digestion of biological materials, followed by reduction of arsenic(V) to arsenic(III) and extraction of arsenic(III) with diethylammonium diethyldithiocarbamate (DDDC) in chloroform. The extract is analyzed by flameless atomic absorption spectrometry (AAS). Recoveries of arsenic from plant and animal tissues ranged from 88 to 108%, averaging 99%. Analyses of rat tissues, using a radioisotope technique, averaged 103% of theoretical. Repeatability studies on rat tissues showed the method to be consistent with coefficients of variation ranging from 3.0 to 8.5%, and a test for ruggedness showed that the method is not affected by slight variations in procedure, but is affected by the presence of Fe and Cu. The method is sensitive to about 0.04 μg arsenic in the total digest (injections of 20 μl of a 4 ng/mL solution).


2021 ◽  
Vol 87 (2) ◽  
pp. 5-12
Author(s):  
L. V. Gudzenko ◽  
T. V. Sheina

The expanding use of sulfur in medicine, science and technology has tightened the requirements for the impurity composition, including the content of selenium in sulfur. Combined extraction-atomic absorption methods have been developed to determine selenium in purified sulfur. The possibility of using thiourea derivatives such as sodium diethyldithiocarbamate and diphenylthiocarbazone for the extraction of microgram amounts of selenium from sulfuric acid solutions was studied. Optimal conditions for the extraction of selenium from sulfate solutions are determined. Two procedures for selenium separation are proposed: extraction of selenium diethyldithiocarbamate with ethyl acetate from a solution of sulfuric acid with pH 3 or extraction of selenium dithizonate with chloroform from a 5.25 – 6.0 M sulfuric acid solution. The results of the extraction-atomic absorption determination of selenium in sulfur are compared for both procedures of selenium separation. The accuracy of the selenium determination in purified sulfur is confirmed by the method of varying sample weight. The optimal temperature-time parameters for the electrothermal atomic absorption determination of selenium are determined. The limit of selenium determination is 1 × 10–5 % wt. The values of sr in the range of selenium content 2 × 10–5 — 1 × 10–4 % wt. change from 0.10 to 0.12.


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