SAMPLE TRASFORMATION AT TWO-STAGE PROBE ATOMIZATION IN GRAPHITE FURNACE FOR ATOMIC ABSORPTION SPECTROMETRY

Y. А. Zakharov, D. S. Irisov, R. R. Haibullin, I. B. Chistyakov

Аннотация


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. Irisov1, R.R. Haibullin, I.B. Chistyakov2

Kazan (Volga region) Federal University, Kazan`, Russian Federation

1LLC «Atzond», Kazan`, Russian Federation

2LLC «Interlab», Moscow, Russian Federation


Полный текст:

PDF (Russian)

Литература


Pupyshev A.A. Atomno-absorbtsionnyi spectral`nyi analiz [Atomic absorption spectral analysis]. Moscow, Tekhnosphera Publ., 2009. 782 с. (in Russian).

Gil'mutdinov A.K., Zakharov Y.A. [Fundamental investigations of electrothermal atomization for analytical spectroscopy]. Izv. AN USSR. Ser. Fizicheskaia [Bulletin of the Russian Academy of Sciences. Physics], 1989, vol. 53, no. 9, pp. 1820-1827 (in Russian).

Zakharov Y.A., Haibullin R.R., Irisov D. S., Sadykov M. F., Gainutdinov A. R. [Hardware-software complex for atomic absorption spectrometry with multistage probe atomization]. Nauchnoe priborostroenie [Scientific instrumentation], 2013, vol. 23, no. 4, pp. 104-111 (in Russian).

Zakharov Y.А., Kokorina O.B., Hasanova S.I., Irisov D.S., Haibullin R.R. [Direct atomic absorption determination of lead and cadmium in the liquid milk foods using double-stage probe atomization in the graphite furnace] Analitika i kontrol' [Analytics and control], 2013, vol. 17, no. 3, pp. 275-280 (in Russian).

Zakharov Y.А., Kokorina O.B. Electrothermal atomic absorption spectrometry with two-step probe atomization and primary absorption signal feedback. J. of Analytical Chemistry, 2012, vol. 67, no. 8, pp. 706-713. doi: 10.1134/S1061934812080084.

Zakharov Y.А., Okunev R.V., Hasanova S.I., Irisov D.S., Haibullin R.R. [Atomic absorption determination of gold and silver in rocks and ores using double-stage probe atomization in the graphite furnace]. Analitika i kontrol' [Analytics and control], 2013, vol. 17, no. 4, pp. 414-422 (in Russian).

Zakharov Y.А., Irisov D.S., Okunev R.V., Musin R.Kh., Haibullin R.R. [Direct determination of gold in suspensions of rock and ore reference materials using electrothermal high resolution atomic absorption spectrometry]. Analitika i kontrol' [Analytics and control], 2014, vol. 18, no. 4, pp. 392-403 (in Russian).

Zakharov Y.А., Kokorina О.B., Grigoryan B.R., Okunev R.V., Irisov D.S., Haibullin R.R., Sadykov M.F., Gainutdinov A.R. [Direct atomic absorption analysis of soils with accessory atzond-1 for double-stage probe atomization in the graphite furnace]. Analitika i kontrol' [Analytics and control], 2013, vol. 17, no. 2, pp. 159-169 (in Russian).

Zakharov Y.A., Okunev R.V., Haibullin R.R., Irisov D.S., Sadykov M.F. [Modernization of MGA-915 Atomic Absorption Spectrometers for Analysis of Rocks and Sediments as Suspensions]. Zavodskaia laboratoriia. Diagnostika materialov [Industrial laboratory], 2014, vol. 80, no. 2, pp. 12-17 (in Russian).

Morokhov I.D., Trusov L.I., Lapovok V.N. Fizicheskie iavleniia v ul`tradispersnykh sredakh [Physical phenomena in ultra-dispersed substances]. Moscow, Energoatomizdat, 1984. 224 pp. (in Russian).

Hirth J.P., Pound G.M. Condensation and evaporation—nucleation and growth kinetics. England, Pergamon Press, 1963. 190 p.

Powell K. et al. eds. Osazhdenie iz gazovoi fazy [Sedimentation from a gas phase]. Мoscow, Atomizdat, 1970. 472 p. (in Russian).

Ievlev B.M., Trusov L.I., Holmyanskyi V.A. Strukturnye prevrashcheniia v tonkikh plenkakh [Structural transformations in thin films]. Мoscow, Metallurgiia, 1988. 326 p. (in Russian).

Zakharov Yu.A., Kokorina O.B., Lysogorskii Yu.V., Staroverov A.E. Computer simulation of two-step atomization in graphite furnaces for analytical atomic spectrometry. J. of Analytical Chemistry, 2012, vol. 67, no. 8, pp. 790-798. doi: 10.1134/S1061934812060214.

Zakharov Yu.A., Kokorina O.B., Lysogorskǐ Yu.V., Sevastianov A.A. Dynamics of fractional condensation of a substance on a probe for spectral analysis. Optics and Spectroscopy. 2008, vol. 105, no. 5, pp. 680-685. doi: 10.1134/S0030400X08110064.

D.L. Styris, L.J. Prell, D.A. Redfield, J.A. Holcombe, D.A. Bass, V. Majidi. Mechanisms of selenium vaporization with palladium modifiers using electrothermal atomization and mass spectrometric detection. Anal. Chem. 1991, vol. 63, no. 5, pp. 508-517. doi: 10.1021/ac00005a024.

Federal state budgetary institution of science A.P. Vinogradov Institute of Geochemistry SB RAS. Available at: http:// http://www.igc.irk.ru/Innovation/Standarts-obr/Catalog-2013.pdf (accessed 01 July 2014).

Kantor T. Interpreting some analytical characteristics of thermal dispersion methods used for sample introduction in atomic spectrometry. Spectrochim. Acta.1988, vol. 43B, pp. 1299-1320. doi: 10.1016/0584-8547(88)80171-X.

Sparks C.M., Pinkston T.L., Holcombe J.A. Particle size distribution of sample transported from an electrothermal vaporizer to an inductively coupled plasma mass spectrometer. Spectrochim. Acta. 1993, vol. 48B, pp. 1607-1615. doi: 10.1016/0584-8547(93)80146-L.

Langer D., Holcombe J. Thermophoretic collection and analysis of submicrometer Ag particles emitted from a graphite tube-type electrothermal vaporizer. Anal. Chem. 1999, vol. 71, pp. 582-588. doi: 10.1021/ac9805089


Ссылки

  • На текущий момент ссылки отсутствуют.