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 and Vítězslav OTRUBA. Direct solid analysis of powdered tungsten carbide hardmetal precursors by laser-induced argon spark ablation with inductively coupled plasma atomic emission spectrometry. ANALYTICAL AND BIOANALYTICAL CHEMISTRY. HEIDELBERG, GERMANY: SPRINGER-VERLAG HEIDELBERG, 2003, vol. 377, 7-8, p. 1165-1174. ISSN 1618-2642.

Basic information

• Original name: Direct solid analysis of powdered tungsten carbide hardmetal precursors by laser-induced argon spark ablation with inductively coupled plasma atomic emission spectrometry
• Name in Czech: Přímá analýza práškových karbidů wolframu laserovou ablací s optickou emisní spektrometrií v indukčně vázaném plazmatu
• Authors: KANICKÝ, Viktor (203 Czech Republic), Markéta HOLÁ (203 Czech Republic), Jean-Michel MERMET (250 France) and Vítězslav OTRUBA (203 Czech Republic, guarantor).
• Edition: ANALYTICAL AND BIOANALYTICAL CHEMISTRY, HEIDELBERG, GERMANY, SPRINGER-VERLAG HEIDELBERG, 2003, 1618-2642.

Other information

• Original language: English
• Type of outcome: Article in a journal
• Field of Study: 10402 Inorganic and nuclear chemistry
• Country of publisher: Germany
• Confidentiality degree: is not subject to a state or trade secret
• Impact factor: Impact factor: 1.715
• RIV identification code: RIV/00216224:14310/03:00008410
• Organization unit: Faculty of Science
• UT WoS: 000186778700014
• Keywords in English: LA-ICP-MS; MASS-SPECTROMETRY; INTERNAL STANDARDS; BULK ANALYSIS; CALIBRATION GRAPHS; TRACE-ELEMENTS; SILICATE ROCKS; PRESSED PELLET; SAMPLES; LIMESTONES
• Tags: BULK ANALYSIS, CALIBRATION GRAPHS, INTERNAL STANDARDS, LA-ICP-MS, limestones, MASS-SPECTROMETRY, PRESSED PELLET, SAMPLES, SILICATE ROCKS, TRACE-ELEMENTS

Abstract

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.

Abstract (in Czech)

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.

Links

• GA203/00/0415, research and development project: Name: Studium interakce laserového záření s práškovými materiály v optické emisní spektrometrii s indukčně vázaným plazmatem

Investor: Czech Science Foundation, The study of interaction of laser radiation with pressed powdered materials for laser ablation inductively coupled plasma atomic emission spectrometry

• MSM 143100003, plan (intention): Name: Studium plazmochemických reakcí v neizotermickém nízkoteplotním plazmatu a jeho interakcí s povrchem pevných látek

Investor: Ministry of Education, Youth and Sports of the CR, Study of plasmachemical reactions in non-isothermic low pressure plasma and its interaction with the surface of solid substrates