Sample transformation at two-stage probe atomization in graphite furnace for atomic absorption spectrometry
Year: 2015
Type: article
Abstract: The surface of the U-shaped tungsten probe for a graphite furnace atomic absorption analysis with two-stage probe atomization was studied using scanning electron microscopy. The aim of the work was investigation of morphology of the sample after vapor phase transfer from the tube furnace to the tungsten probe and additional thermal treatment on the probe. It is shown for the sample having complex matrix (the slurry of milled up to 80 µm gold ore) that a polycrystalline layer of agglomerated particles of size less than 1 µm is formed on the surface of the probe after primary vaporization. After additional pyrolysis on the probe at the furnace temperature1500°Cthe deposit is modified into an amorphous film and drops of reduced metals with diameter up to 1 µm. In the case of simple matrix (water solution of palladium nitrate) a solid film with clots and flakes of 50 – 100 nm micro drops of palladium is deposited on the probe. The two stage treatment leads to the simplification of chemical and phase composition of the deposit and its localization on the probe tip within2 mm. This caused substantial improvement of analytical signal associated with atomization of the deposit from the probe inserted into the graphite furnace. Keywords : atomic absorption analysis, two-stage probe atomization, graphite furnace, ore, suspension, electron microscopy. (Russian) DOI: http://dx.doi.org/10.15826/analitika.2015.19.1.008 Y. А . Zakharov, D.S. Irisov 1 , R.R. Haibullin, I.B. Chistyakov 2 Kazan (Volga region) Federal University, Kazan`, Russian Federation 1 LLC «Atzond», Kazan`, Russian Federation 2 LLC «Interlab», Moscow, Russian Federation
Source: Analitika i kontrolʹ
Institution: Kazan Federal University
Language: Russian
Subfield: Analytical Chemistry
Field: Chemistry
Domain: Physical Sciences
Open Access status: bronze
OpenAlex ID: W4232050307