Decomposition applying elemental fluorine for the analysis of element traces in fine ceramics

Richts, U.; Garten, R. P. H.; Jacob, Eberhard; Tlg, G.

doi:10.1007/bf00323303

Cited by 7 publications

(5 citation statements)

References 5 publications

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“…Fluorination. A detailed description of the fluorination apparatus with a unit for fluorine dosing, a vacuum, and an absorber system and a combustion cell is given in refs −9. For a decomposition with elemental fluorine, a cylindrical reactor made of pure nickel (DIN 17740, Deutsche Nickel AG Schwerte, Germany) with a volume of 10 mL is used.…”

Section: Methodsmentioning

confidence: 99%

Determination of Main and Minor Components of Silicon Based Materials by a Combustion with Elemental Fluorine. Separation of Gaseous Fluorination Products by Carrier Gas Distillation and Gas Mass Spectrometry

Ruße¹,

Kipphardt²,

Broekaert³

2000

Anal. Chem.

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For the determination of main and minor components in silicon-based ceramic powders, a decomposition by a combustion with elemental fluorine and separation of the volatile fluorination products by a carrier-gas distillation with a subsequent detection by quadrupole mass spectrometry is described. The necessity and success of the separation step is demonstrated for the determination of boron as a minor constituent in SiC, where the spectral interferences of silicon on the boron signals are decreased considerably. The method developed is shown to be directly applicable to determination of silicon in Si3N4, SiC, and SiO2. The determination of nitrogen in Si3N4 requires additional effort, to separate nitrogen from the excess of fluorine. For the determination of boron, a complete mobilization of BF3 is assured by the presence of an adequate amount of GeF4. Analysis results obtained with different types of calibration show a precision of 30 microg for boron at the milligram-per-gram level and a precision between 0.5 and 2% (m/m) for the main components, silicon and nitrogen. Within these standard deviations, the results agree well with the values expected from the stoichiometry, with the results for silicon and boron obtained by wet chemical decomposition and slurry techniques in combination with ICP-OES and with the results for nitrogen obtained by carrier gas heat extraction.

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Section: Methodsmentioning

confidence: 99%

Determination of Main and Minor Components of Silicon Based Materials by a Combustion with Elemental Fluorine. Separation of Gaseous Fluorination Products by Carrier Gas Distillation and Gas Mass Spectrometry

Ruße¹,

Kipphardt²,

Broekaert³

2000

Anal. Chem.

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“…1) and its handling are similar to those described by Richts et al [5]. The apparatus is made of commercially available stainless steel and monel fittings.…”

Section: Fluorination Apparatusmentioning

confidence: 99%

“…These problems have been overcome [8,9]. Accordingly, its use became possible and it has been described that a decomposition of SiC, Si3N 4, B4C and BN is complete after 10 minutes at 250~ and results in mixtures of volatile and nonvolatile products [5,9]. The solid residue can be determined by atomic spectrometry [5,6].…”

mentioning

confidence: 99%

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Mass spectrometric analysis of ceramics after decomposition with elemental fluorine

Kipphardt

Garten

Jacob³

et al. 1997

Mikrochim Acta

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Abstract. The features of a combustion with elementary fluorine for the case of compact SiC ceramics and model substances for boron containing ceramics (H3BO 3 and Na2B407) were investigated with the aim of their decomposition and analysis. On-line detection of the gaseous decomposition products by quadrupole mass spectrometry using electron impact ionisation was studied. Limitations by blanks and transport interferences were investigated. Standard addition as well as the isotope dilution technique were used for calibration in the case of B, C and W at the trace and major component level.

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“…Richts et al 29 showed that boron carbide powders can be completely decomposed when treating them with elemental fluorine at a temperature of 350 C. As a result of these literature data it therefore can be assumed that through the introduction of the Freon R12 BCl 3 and BF 3 are formed.…”

Section: Optimization Of the Temperature Programmentioning

confidence: 99%

Direct multielement determination of trace elements in boron carbide powders by slurry sampling ETV-ICP-OES

Amberger

Broekaert

2010

J. Anal. At. Spectrom.

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The use of slurry sampling electrothermal evaporation inductively coupled plasma optical emission spectrometry (SlS-ETV-ICP-OES) for the direct determination of trace elements in boron carbide powders with different particle size distributions was investigated. It was found that the addition of 6 mL min À1 of Freon R12 (Cl 2 F 2 C) to the 500 mL min À1 Ar carrier gas flow as a thermochemical reagent resulted in an increase of the net line intensity for Ti by a factor of 25 in SlS-ETV-ICP-OES, when analyzing 20 mL of a slurry containing 1% of the boron carbide powder BC-1. After heating the dry residue of 20 mL of a slurry of 1% of boron carbide for 12 s to 2600 C on a L'vov platform the residues on the platforms were analyzed by total reflection X-ray fluorescence spectrometry (TXRF). The evaporation efficiency for Ti was found to have increased from 12 to 97% by the addition of 6 mL min À1 of R12 as compared to evaporation in Ar only. When heating dry residues of boron carbide slurries on L'vov platforms to temperatures ranging from 2000 to 2600 C without adding R12 to the Ar, it could be observed visually that only a small fraction of the boron carbide matrix is evaporated. However, when heating at 2600 C under the addition of R12 almost no residues were found on the platform after the evaporation step. For the analysis of boron carbide powders with SlS-ETV-ICP-OES the limits of detection were found to be between 0.002 and 2 mg g À1 for the elements Al, Ca, Co, Cr, Cu, Fe, Mg, Mn, Na, Ni and Ti. For Fe a wide variety of samples could be analyzed by SlS-ETV-ICP-OES with one calibration under the use of R12. This was shown for different samples, namely three boron carbide powders, three boron nitride powders, an aluminium oxide powder (NIST 699), silicon carbide powder (BAM S-003), powdered apple leaves (NIST 1515), a reference sample for trace elements in natural water (NIST 1643d) and an aqueous standard solution. When plotting the net line intensities versus the accepted concentrations a coefficient of determination of 0.990 is obtained. By SlS-ETV-ICP-OES under the addition of R12 the values obtained were found to be between 78 to 128% of the mean of the results of slurry sampling-TXRF and of ICP-OES subsequent to wet chemical digestion. 11 trace elements with concentrations ranging from 0.7 to 370 mg g À1 for Co and Fe, respectively, could be determined in two boron carbide powders with particle size distributions of d 90 ¼ 3.5 mm and d 90 ¼ 9.2 mm, respectively.

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Decomposition applying elemental fluorine for the analysis of element traces in fine ceramics

Cited by 7 publications

References 5 publications

Determination of Main and Minor Components of Silicon Based Materials by a Combustion with Elemental Fluorine. Separation of Gaseous Fluorination Products by Carrier Gas Distillation and Gas Mass Spectrometry

Determination of Main and Minor Components of Silicon Based Materials by a Combustion with Elemental Fluorine. Separation of Gaseous Fluorination Products by Carrier Gas Distillation and Gas Mass Spectrometry

Mass spectrometric analysis of ceramics after decomposition with elemental fluorine

Direct multielement determination of trace elements in boron carbide powders by slurry sampling ETV-ICP-OES

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