Glow Discharge Sputter Atomization for Atomic Absorption Analysis of Nonconducting Powder Samples

1988 ◽  
Vol 42 (6) ◽  
pp. 941-944 ◽  
Author(s):  
Michael R. Winchester ◽  
R. Kenneth Marcus

A methodology has been developed for the analysis of nonconducting (oxide) powder samples by glow discharge atomization-atomic absorption spectrometry (GDA-AAS). The mixing of an oxide powder with a copper host matrix (1:9) allows pressing of a disk sample for glow discharge sputtering. Sample-to-sample precisions are on the order of 3–4% for iron in a geological specimen. The ability to generate analytical working curves is demonstrated for the analysis of iron by mixing Fe (III) and Al (III) oxides in the copper matrix material. The possible utility of the methodology is illustrated by the analysis of iron in an NBS geological reference material. The ability to perform analyses of these sample types suggests its applicability to such matrices as ceramics, glasses, and refractory-based catalysts.

1994 ◽  
Vol 48 (6) ◽  
pp. 713-719 ◽  
Author(s):  
Pingxin Wang ◽  
James A. Holcombe

The spatial distribution of Pb in a NIST Standard Reference Material (SRM) C1253a copper alloy is determined by using an electrothermal atomizer atomic absorption spectrometry (ETA-AAS) system operated at reduced pressure. Three Pb absorbance peaks have been consistently observed at 0.1 Torr. It is proposed that the first peak belongs to the release process of Pb from the surface, the second peak may originate from grains until the Cu-Pb binary phase transformation to a homogeneous solution occurs, and the third peak arises from Pb in the bulk of the sample. The areas of the first two peaks may be used to determine the “near surface” and grain concentrations of analyte. However, the expulsion of analyte because of the coincident bulk vaporization of copper matrix produces a severely depressed analytical signal for the third peak. The data presented for the pressure-regulated ETA-AAS system suggest the feasibility of isolating and quantitatively measuring metals within the bulk and on or near the surface of solid samples when the metal of interest is of lower volatility than the host matrix.


1979 ◽  
Vol 33 (4) ◽  
pp. 393-399 ◽  
Author(s):  
R. C. Fry ◽  
M. B. Denton

Studies are presented to characterize a new nebulizer developed for direct atomic absorption analysis of extremely complex clinical and environmental materials. Important parameters are described concerning the design and performance of “high solids” spectrochemical nebulizers based on the Babington principle. A new simplified design is presented and mechanisms of undesirable sample wastage are considered. Data are presented concerning the effect of impaction on conventional and “high solids” aerosol generation.


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