2003
Direct solid analysis of powdered tungsten carbide hardmetal precursors by laser-induced argon spark ablation with inductively coupled plasma atomic emission spectrometry
KANICKÝ, Viktor, Markéta HOLÁ, Jean-Michel MERMET a Vítězslav OTRUBAZákladní údaje
Originální název
Direct solid analysis of powdered tungsten carbide hardmetal precursors by laser-induced argon spark ablation with inductively coupled plasma atomic emission spectrometry
Název česky
Přímá analýza práškových karbidů wolframu laserovou ablací s optickou emisní spektrometrií v indukčně vázaném plazmatu
Autoři
KANICKÝ, Viktor (203 Česká republika), Markéta HOLÁ (203 Česká republika), Jean-Michel MERMET (250 Francie) a Vítězslav OTRUBA (203 Česká republika, garant)
Vydání
ANALYTICAL AND BIOANALYTICAL CHEMISTRY, HEIDELBERG, GERMANY, SPRINGER-VERLAG HEIDELBERG, 2003, 1618-2642
Další údaje
Jazyk
angličtina
Typ výsledku
Článek v odborném periodiku
Obor
10402 Inorganic and nuclear chemistry
Stát vydavatele
Německo
Utajení
není předmětem státního či obchodního tajemství
Impakt faktor
Impact factor: 1.715
Kód RIV
RIV/00216224:14310/03:00008410
Organizační jednotka
Přírodovědecká fakulta
UT WoS
000186778700014
Klíčová slova anglicky
LA-ICP-MS; MASS-SPECTROMETRY; INTERNAL STANDARDS; BULK ANALYSIS; CALIBRATION GRAPHS; TRACE-ELEMENTS; SILICATE ROCKS; PRESSED PELLET; SAMPLES; LIMESTONES
Štítky
Změněno: 2. 7. 2009 09:35, Mgr. Markéta Holá, Ph.D.
V originále
The potential of the laser-induced argon spark atomizer (LINA-Spark atomizer) coupled with ICP-AES as a convenient device for direct analysis of WC/Co powdered precursors of sintered hardmetals was studied. The samples were presented for the ablation as pressed pellets prepared by mixing with powdered silver binder containing GeO2 as internal standard. The pellets were ablated with the aid of a Q-switched Nd:YAG laser (1064 nm) focused 16 mm behind the target surface with a resulting estimated power density of 5 GW cm(-2). Laser ablation ICP-AES signals were studied as a function of ablation time, and the duration of time prior to measurement (pre-ablation time) which was necessary to obtain reliable results was about 40 s. Linear calibration plots were obtained up to 10% (m/m) Ti, 9% Ta and 3.5% Nb both without internal standardization and by using germanium as an added internal standard or tungsten as a contained internal standard. The relative uncertainty at the centroid of the calibration line was in the range from +/-6% to +/-11% for Nb, Ta and Ti both with and without internal standardisation by Ge. A higher spread of points about the regression was observed for cobalt for which the relative uncertainty at the centroid was in the range from +/-9% to +/-14%. Repeatability of results was improved by the use of both Ge and W internal standards. The lowest determinable quantities calculated for calibration plots were 0.060% Co, 0.010% Nb, 0.16% Ta and 0.030% Ti with internal standardization by Ge. The LA-ICP-AES analyses of real samples led to good agreement with the results obtained by solution-based ICP determination with a relative bias not exceeding 10%. The elimination of the dissolution procedure of powdered tungsten (Nb, Ta, Ti) carbide is the principal advantage of the developed LA-ICP-AES method.
Česky
The potential of the laser-induced argon spark atomizer (LINA-Spark atomizer) coupled with ICP-AES as a convenient device for direct analysis of WC/Co powdered precursors of sintered hardmetals was studied. The samples were presented for the ablation as pressed pellets prepared by mixing with powdered silver binder containing GeO2 as internal standard. The pellets were ablated with the aid of a Q-switched Nd:YAG laser (1064 nm) focused 16 mm behind the target surface with a resulting estimated power density of 5 GW cm(-2). Laser ablation ICP-AES signals were studied as a function of ablation time, and the duration of time prior to measurement (pre-ablation time) which was necessary to obtain reliable results was about 40 s. Linear calibration plots were obtained up to 10% (m/m) Ti, 9% Ta and 3.5% Nb both without internal standardization and by using germanium as an added internal standard or tungsten as a contained internal standard. The relative uncertainty at the centroid of the calibration line was in the range from +/-6% to +/-11% for Nb, Ta and Ti both with and without internal standardisation by Ge. A higher spread of points about the regression was observed for cobalt for which the relative uncertainty at the centroid was in the range from +/-9% to +/-14%. Repeatability of results was improved by the use of both Ge and W internal standards. The lowest determinable quantities calculated for calibration plots were 0.060% Co, 0.010% Nb, 0.16% Ta and 0.030% Ti with internal standardization by Ge. The LA-ICP-AES analyses of real samples led to good agreement with the results obtained by solution-based ICP determination with a relative bias not exceeding 10%. The elimination of the dissolution procedure of powdered tungsten (Nb, Ta, Ti) carbide is the principal advantage of the developed LA-ICP-AES method.
Návaznosti
| GA203/00/0415, projekt VaV |
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| MSM 143100003, záměr |
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