Direct multielement determination of trace elements in boron carbide powders by total reflection X-ray fluorescence spectrometry and analysis of the powders by ICP atomic emission spectrometry subsequent to sample digestion

Amberger, Martin A.; Broekaert, J. A. C.

doi:10.1039/b906417f

Cited by 13 publications

(13 citation statements)

References 28 publications

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“…The ICP results indicated that adequate modification of the fundamental ICP-MS parameters such as dilution factors, RF power and nebulizer gas flow could be an initial way to improve the analytical results of ICP-MS. Results from experiments for the direct determination of trace elements in boron carbide powders with different particle size distributions were reported by Amberger et al 113 Samples were prepared as slurry and stability was monitored by measuring the zeta potential for different pH values and different concentrations of polyethylenimine (PEI). The elements Ca, Co, Cr, Cu, Fe, Mn, Ni and Ti were determined by TXRF and ICP-OES after wet chemical digestion of the samples.…”

Section: Chemical Analysis and Speciation Using Txrfmentioning

confidence: 93%

Atomic spectrometry update–X-ray fluorescence spectrometry

West

Ellis

Potts

et al. 2010

J. Anal. At. Spectrom.

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Section: Chemical Analysis and Speciation Using Txrfmentioning

confidence: 93%

Atomic spectrometry update–X-ray fluorescence spectrometry

West

Ellis

Potts

et al. 2010

J. Anal. At. Spectrom.

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“…When defining d 90 as the particle size corresponding to the cumulative mass percentage of 90% BC-1 with d 90 ¼ 3.5 mm was found to be the finer powder and BC-2 with d 90 ¼ 9.2 mm the coarser one. In a former study 15 we analyzed the two powders by SlS-TXRF and by Sol-ICP-OES and the concentrations of the trace elements were found to range from 0.7 mg g À1 to 370 mg g À1 for Al, Ca, Co, Cr, Cu, Fe, Mg, Mn, Na, Ni and Ti.…”

Section: Methodsmentioning

confidence: 99%

“…13 However, until now only three studies focused on the direct analysis of boron carbide powders. [14][15][16] K antor et al 14 reported on the determination of trace metals in industrial boron carbide powders by direct current arc optical emission spectrometry (DC-arc-OES). Here, it was found that the developed analytical procedure could meet most of the demands for fast routine analyses of boron carbide powders.…”

Section: Introductionmentioning

confidence: 99%

“…Recently, we used slurry sampling total reflection X-ray fluorescence spectrometry (SlS-TXRF) 15 for the determination of Ca, Co, Cr, Cu, Fe, Mn, Ni and Ti at the trace element level in three boron carbide powders with different particle size distributions. Except for Ca and Mn, the detection limits of SlS-TXRF for the analysis of boron carbide powders are in the same range as those obtained by ICP-OES subsequent to wet chemical dissolution (Sol-ICP-OES) and for Cr, Cu, Fe, Mn and Ti they are lower than those obtained in DC-arc-OES.…”

Section: Introductionmentioning

confidence: 99%

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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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“…For trace and ultra trace analysis chemicals used for fusion are often not clean enough and high salt contents are often not desirable for the analytical methods performed. Solid sampling methods such as instrumental photon activation analysis (IPAA), total reflection X‐ray fluorescence spectrometry (TXRF), ICP optical emission spectrometry (ICP OES) combined with slurry technique, DC arc optical emission spectrometry (DC‐arc‐OES), electrothermal vaporation ICP OES (ETV‐ICP OES), solid sampling electrothermal evaporation atomic absorption spectrometry (SS ET AAS) or carrier gas hot extraction (CGHE, for the elements hydrogen, nitrogen, oxygen) can be used for analysis of boron carbide and other advanced ceramics. These methods avoid any time‐consuming sample dissolution steps before the analysis, thus bearing fewer risks of contamination .…”

Section: Introductionmentioning

confidence: 99%

Certification of a Boron Carbide Powder Reference Material for Chemical Analysis

et al. 2011

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The certification of a boron carbide reference material for chemical composition is described. The mass fractions of 16 elements and two boron species are certified in an international interlaboratory comparison with 35 participating laboratories from six different countries. Beside chemical characterization the certification process includes homogeneity and stability testing of the candidate material boron carbide (type F360, 305M422). Details of the analytical methods used for chemical characterization and of the calculation of the uncertainties of the certified mass fractions are given. The new reference material ERM®‐ED102 with certified mass fractions of 18 parameters (elements and species) and of the amount fraction of the isotope 10B is a valuable tool for laboratories working in the field of advanced ceramic materials analysis to improve their analytical results.

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Direct multielement determination of trace elements in boron carbide powders by total reflection X-ray fluorescence spectrometry and analysis of the powders by ICP atomic emission spectrometry subsequent to sample digestion

Cited by 13 publications

References 28 publications

Atomic spectrometry update–X-ray fluorescence spectrometry

Atomic spectrometry update–X-ray fluorescence spectrometry

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

Certification of a Boron Carbide Powder Reference Material for Chemical Analysis

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