Chemical reactions in the atomization of molybdenum in graphite furnace atomic absorption spectrometry

Chakrabarti, Chuni L.; Wu, Shengji; Marcantonio, Franco; Headrick, Kurt L.

doi:10.1007/bf00467067

Cited by 15 publications

(4 citation statements)

References 23 publications

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“…This character of the dependence can be explained in that way: the molybdenum passes into the gaseous phase in the form of molybdenum oxide MoO2. 35 Thus, if it is necessary to use the pyrolysis step, it must be carried out at temperature equals 960 °C.…”

Section: Optimization Of the Etv-icp-ms Instrumental Parametersmentioning

confidence: 99%

Multi-elemental analysis of high-purity molybdenum by electrothermal vaporization inductively coupled plasma mass spectrometry

Medvedev¹,

Volzhenin²,

Saprykin³

2020

At.Spectrosc.

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High purity molybdenum and its compounds are used for the synthesis of ionizing radiation detectors for search for dark matter and double beta decay. Properties of these detectors largely depend on their trace composition. The new mass-spectrometry with inductively coupled plasma (ICP-MS) and electrothermal vaporization (ETV) method was developed for the analysis of high-purity molybdenum. The samples were introduced into the ICP using the ETV device. The vaporization curves of matrix element (molybdenum) and trace elements were studied in detail. The dependence of analytical signal and limits of detection (LODs) of analytes versus ETV-ICP-MS instrumental parameters (ICP power, transport flow, ion optics settings) was established. The proposed method of ETV-ICP-MS analysis allowed us to control the content of 28 trace elements in high-purity molybdenum with a purity of 6N (99.9999% wt.) and provided LODs from 0.3 to 200 ng g-1. Using of ETV for ICP-MS analysis of molybdenum led to decreasing of the LODs of trace elements from 3 to 200 times comparing with ICP-MS analysis with standard sample introduction system. The validation of proposed ETV-ICP-MS method was performed by spike experiment and by comparing the results of ETV-ICP-MS, ICP-MS, and atomic absorption spectrometry with electrothermal vaporization (GFAAS) analysis.

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Section: Optimization Of the Etv-icp-ms Instrumental Parametersmentioning

confidence: 99%

Multi-elemental analysis of high-purity molybdenum by electrothermal vaporization inductively coupled plasma mass spectrometry

Medvedev¹,

Volzhenin²,

Saprykin³

2020

At.Spectrosc.

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“…Both methods are disadvantageous in terms of cost and the instruments used in routine analysis. [3][4][5][6] Sensitive techniques for the determination of trace amounts of molybdenum include inductively coupled plasma-atomic emission spectrometry (ICP/AES) [7][8][9] and neutron activation analysis (NAA). 10,11 The high instrumental costs and need for preconcentration and/or separation are common disadvantages.…”

Section: Introductionmentioning

confidence: 99%

Kinetic Spectrophotometric Determination of Traces of Molybdenum(VI) by Its Inhibitory Effect on the Oxidation of 4-Hydroxycoumarine by Potassium Permanganate

Micić¹,

Simonović²,

Petković³

2006

ANAL. SCI.

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The present paper describes a simple, selective and sensitive kinetic method for the determination of trace amounts of molybdenum(VI) based on its inhibitory effect on the reaction oxidation of 4-hydroxycoumarine by KMnO4 in the presence of hydrochloric acid, at pH 1.75 at 25˚C. The rate of the indicator reaction was followed spectrophotometrically by measuring the decrease in the absorbance of KMnO4 at 525 nm. The development method includes optimization of the reagent concentration and temperature. The calibration graph was linear in the range of concentrations from 20 to 200 ng/cm 3 of molybdenum(VI). The probable relative error was in the interval 3.10 -10.52% for the concentration range of 200 -20 ng/cm 3 molybdenum(VI), respectively. The interference effects of the foreign ions were determined to assess the selectivity of the method. The developed method was found to have relatively good selectivity, sensitivity, simplicity and rapidity. The proposed method was applied to the determination of molybdenum(VI) in a particular type of steel and alloy (hastelloy).

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“…Variable information has been obtained recently by some instrumental techniques and particularly by use of surface examination techniques like SEM, STM, etc., in combination with analytically capable techniques in microscale areas, like XRD, XPS, SIMS, EDXRF, etc. [17,18]. For example, EDXRF analysis in combination with scanning electron microscopy gives very useful information for the analysis of the graphite Mikrochim.…”

mentioning

confidence: 99%

“…For example, EDXRF analysis in combination with scanning electron microscopy gives very useful information for the analysis of the graphite Mikrochim. Acta 136, 115±122 (2001) Ã To whom correspondence should be addressed surfaces [19,20] and the structural properties of the modi®ers [17,21].…”

mentioning

confidence: 99%

SEM-EDXRF Study of Two Chemical Modifiers Based on Platinum and Tungsten and Their Effect on ET-AAS Atomization of Lead

et al. 2001

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The behavior of two chemical modi®ers based on platinum and tungsten, is studied in the two parts of this work. At ®rst, the chemical and morphological alterations of these during pyrolysis and atomization stages in electrothermal atomic absorption spectrometry are studied. The compounds were H 2 PtCl 6 and Na 2 WO 4 . A cylindrical graphite tube was used, and ®xed shaped rectangular graphite plates were put inside as platforms to prepare the specimens. The crystalline formations on the platforms were studied by scanning electron microscopy and the energy dispersive X-ray spectra allowed the estimation of the chemical composition changes of the modi®ers and the graphite surface. According to the spectra and the images obtained, both modi®ers where found to change their crystalline form at temperatures between 500±1250 C. Severe corrosion of the graphite surface was observed in case of H 2 PtCl 6 at temperature higher than 750 C, while minor damages were observed in case of Na 2 WO 4 . In the second part of this work, the ef®ciency of these modi®ers was tested for maximum loss-free pyrolysis temperature and atomization of lead by electrothermal atomic absorption spectrometry. The optimum results, concerning these parameters, obtained for medium concentration of the modi®ers. The effect of each modi®er on the atomization signal is discussed, and the optimum concentration of each one is estimated.

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Chemical reactions in the atomization of molybdenum in graphite furnace atomic absorption spectrometry

Cited by 15 publications

References 23 publications

Multi-elemental analysis of high-purity molybdenum by electrothermal vaporization inductively coupled plasma mass spectrometry

Multi-elemental analysis of high-purity molybdenum by electrothermal vaporization inductively coupled plasma mass spectrometry

Kinetic Spectrophotometric Determination of Traces of Molybdenum(VI) by Its Inhibitory Effect on the Oxidation of 4-Hydroxycoumarine by Potassium Permanganate

SEM-EDXRF Study of Two Chemical Modifiers Based on Platinum and Tungsten and Their Effect on ET-AAS Atomization of Lead

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