Mass spectrometry insight of the process mechanism during the vacuum distillation of zinc

Anil, G.; Kipphardt, Heinrich; Matschat, Ralf; Panne, Ulrich

doi:10.1039/b904133h

Cited by 8 publications

(3 citation statements)

References 6 publications

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“…The process of zinc vacuum distillation was monitored by an online gas quadrupole mass spectrometer as described by Gopala et al 31 Results from high resolution GD-MS of the zinc before and after purification were also used to elucidate the mechanism of vacuum distillation. A systematic study of the effect of isotopes on depth profile metal coatings on metal substrates by LA-ICP-MS was conducted by Farinas and colleagues.…”

Section: Non-ferrous Metals and Alloysmentioning

confidence: 99%

Atomic spectrometry update. Industrial analysis: metals, chemicals and advanced materials

Carter

Fisher

Goodall

et al. 2010

J. Anal. At. Spectrom.

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Section: Non-ferrous Metals and Alloysmentioning

confidence: 99%

Atomic spectrometry update. Industrial analysis: metals, chemicals and advanced materials

Carter

Fisher

Goodall

et al. 2010

J. Anal. At. Spectrom.

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“…The vacuum reduction distillation system consists of a cylindrically shaped recipient (V ϳ 55 L) on a base plate connected to the mass spectrometer [7]. The schematic of the set-up, originally developed by EMPA, Switzerland, is given in Supplemental Figure S1, which can be found in the electronic version of this article.…”

Section: Methodsmentioning

confidence: 99%

Mass spectrometric study of the impurity profile in Zn during reduction-distillation of ZnO with activated and inactivated Al

Anil

Zellmann

Kipphardt

et al. 2010

J. Am. Soc. Mass Spectrom.

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In this work, we report on the application of hyphenated gas source mass spectrometry to study and understand the mechanism of the reduction-distillation of ZnO using Al powder as reductant in its activated and inactivated form. The experiments revealed that the purity of the Zn metal produced were superior using activated Al with respect to inactivated Al, i.e., m5N8 (99.9998% metallic based) versus m5N3. The achieved purity levels of Zn and the absence of high volatile Cd, Mg, and Sb impurities in the gas phase and the material collected were explained with respect to the impurity elements free-energy values, vapor pressure data, and an observed scavenging effect of the Ta crucible, which was supported by the on-line observed mass spectrometric profiles of the residual gas. [1,2]. Several researchers have carried out work on the aluminothermic reduction of ZnO using activated and inactivated Al for the preparation of Al 2 O 3 . However, the reduction was seldom utilized for the purification of zinc [3][4][5]. The present study focuses on the behavior of impurities during the purification of Zn by reduction-distillation of zinc oxide with activated and inactivated Al powder in vacuum. The experiments were conducted at different temperatures and the evolving metal atoms were monitored in real-time to investigate the impurity element's oxide reduction ability and the impurity element's ability for co-distillation. All experiments were performed in a resistance heated vacuum reduction distillation system connected to a gas source mass spectrometer.The activation process of Al is discussed in detail in [6]. The mechanical treatment of Al with added carbon powder as surfactant in vibration milling results in an extremely high chemical activated Al with the removal of inhibiting alumina layer. The addition of graphite also allows one to conserve the powder state of the material without getting oxidized after mechanical milling. The Al powder without pretreatment inherently contains an alumina film at its surface, and is usually denoted as inactivated Al [1]. A smaller particle size presents, in general, a faster reaction rate in the reduction process because of the greater contact area between the reactants; however, in the case of Al, more than particle size, the surface coating matters. ExperimentalThe vacuum reduction distillation system consists of a cylindrically shaped recipient (V ϳ 55 L) on a base plate connected to the mass spectrometer [7]. The schematic of the set-up, originally developed by EMPA, Switzerland, is given in Supplemental Figure S1, which can be found in the electronic version of this article. A turbo pump (PFEIFFER TCP-121) backed by a membrane pump is connected via a vacuum valve. The vacuum achieved was ϳ2.0 ϫ 10 7 mbar measured using a Pirani and a cold cathode gauge. The two copper electrodes mounted side by side to carry the crucible assembly are connected to a high current/low voltage supply. The crucible used for the reduction is made out of tantalum (9.0 mm o.d. ϫ 7.0 mm i.d. ϫ 8 mm ...

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“…Recently our research has been focused on the online monitoring using gas source mass spectrometry for understanding the melting and volatilisation process of Zn metal in the vacuum distillation system which can be regarded as fundamental steps in a purification procesess. 5…”

Section: Introductionmentioning

confidence: 99%

Use of mass spectrometric detection as a versatile process monitoring tool: reduction patterns in a milled ZnO/Al mixture

et al. 2010

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Mass spectrometric detection can play a prominent role in the assessment of different reactions occurring at varied temperatures in a milled ZnO/Al mixture. This is the first time that online mass spectrometric information was used as a tool for monitoring and understanding the chemical reduction process mechanism. We have observed four different types of reaction taking place: (1) distillation of Zn metal, (2) reduction of ZnO by activated Al, (3) melting of Al and finally (4) reduction of ZnO by inactivated Al. The experimental conditions and results observed by QMS were supported with literature data and physical measurement data from X-Ray Diffraction (XRD) which gave us an idea about the complex reaction cascade which occurred during the formation of the zinc metal.

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Mass spectrometry insight of the process mechanism during the vacuum distillation of zinc

Cited by 8 publications

References 6 publications

Atomic spectrometry update. Industrial analysis: metals, chemicals and advanced materials

Atomic spectrometry update. Industrial analysis: metals, chemicals and advanced materials

Mass spectrometric study of the impurity profile in Zn during reduction-distillation of ZnO with activated and inactivated Al

Use of mass spectrometric detection as a versatile process monitoring tool: reduction patterns in a milled ZnO/Al mixture

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