Wet oxidation decomposition of graphite for determination of impurity elements.

Hashitani, Hiroshi; Yoshida, Hideyo; Adachi, T.; Izawa, Kimie

doi:10.2116/bunsekikagaku.35.11_911

Cited by 7 publications

(2 citation statements)

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“…16 Considering the inertness of graphite, concentrated acids, high temperature and timeconsuming digestion programs are necessary to effectively solubilize this material. 2,17 Besides this, polyatomic spectral interference [18][19][20] can take place particularly in the determination of REE by ICP-MS. The large amounts of acids, used for graphite digestion, can enhance the formation of REE oxides, 21,22 which can cause spectral overlapping in its determination.…”

Section: Introductionmentioning

confidence: 99%

Determination of rare earth elements in graphite by solid sampling electrothermal vaporization-inductively coupled plasma mass spectrometry

Mello

Pedrotti

Cruz

et al. 2015

J. Anal. At. Spectrom.

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A method is proposed for the determination of trace rare earth elements (REEs) in graphite by solid sampling electrothermal vaporization-inductively coupled mass spectrometry (ETV-ICP-MS). The operating parameters of the ETV system such as gas flow-rate, heating program, the use of a modifier gas (Freon R-12) as well as sample mass were evaluated. The determination of REE in graphite samples was performed by directly weighing a solid sample (0.5 to 2.5 mg) on the graphite platform of the ETV system. Calibration was carried out using aqueous standards. According to the results, the presence of the modifier gas (Freon R-12) promoted an enhancement of vaporization for all analytes, besides the reduction of the vaporization temperature (about 500 C lower). The accuracy was evaluated by an analyte recovery experiment and also by comparison of results with those obtained by microwaveassisted extraction (MAE) with further determination of REE by ICP-MS equipped with an ultrasonic nebulizer (USN-ICP-MS). Agreement was observed between the results obtained by ETV-ICP-MS and MAE with USN-ICP-MS analysis for most of the elements. Analyte recovery ranged from 100.3 to 118.7% and the obtained RSDs were always lower than 24%. The limits of detection were at the ng g À1 level and were similar to those obtained by USN-ICP-MS with previous sample preparation by MAE. The proposed method was suitable for direct determination of REE in graphite. In addition, direct analysis of graphite by ETV-ICP-MS avoided the laborious sample preparation step of graphite and the use of concentrated acids for digestion, minimizing interferences in the determination step by ICP-MS.

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Section: Introductionmentioning

confidence: 99%

Determination of rare earth elements in graphite by solid sampling electrothermal vaporization-inductively coupled plasma mass spectrometry

Mello

Pedrotti

Cruz

et al. 2015

J. Anal. At. Spectrom.

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show abstract

“…For analysis of graphite by solution electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma atomic emission and mass spectrometries (ICP-AES and ICPMS), several procedures have been reported for wet digestion with acids using open, closed pressure, or microwave oven techniques. ,− However, with most of these common decomposition techniques, no complete digestion of graphite could be achieved. Therefore, direct instrumental methods, such as glow discharge emission and absorption spectrometry (GD-AES and GD-AAS), , direct current arc emmision spectrometry (dc-AES), ,− and instrumental neutron activation analysis (INAA), ,, have frequently been employed.…”

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confidence: 99%