Influence of binders on infrared laser ablation of powdered tungsten carbide pressed pellets in comparison with sintered tungsten carbide hardmetals studied by inductively coupled plasma atomic emission spectrometry

Laser ablation (LA) was studied as a sample introduction technique for the analysis of powdered and sintered tungsten carbides (WC/Co) by inductively coupled plasma optical emission spectrometry (ICP–OES). The possibility to work with powdered and compact materials with close chemical composition provided the opportunity to compare LA sampling of similar substances in different forms that require different preparation procedures. Powdered WC/Co precursors of sintered hardmetals were prepared for the ablation as pressed pellets with and without powdered silver as a binder, while sintered hardmetal blocks were embedded into a resin to obtain discs, which were then smoothed and polished. A Q-switched Nd:YAG laser operated at its fundamental wavelength of 1064 nm with a pulse frequency of 10 Hz and maximum pulse energy of 220 mJ was used. A single lens was used for the laser beam focusing. An ablation cell (14 cm3) mounted on a PC-controlled XY-translator was connected to an ICP spectrometer Jobin Yvon 170 Ultrace (laterally viewed ICP, mono- and polychromator) using a 1.5-m tubing (4 mm i.d.). Ablation was performed in a circular motion (2 mm diameter). Close attention was paid to the study of the crater parametres depending on hardness, cohesion and Ag binder presence in WC/Co samples. The influence of the Co content on the depth and structure of the ablation craters of the binderless pellets was also studied. Linear calibration plots of Nb, Ta and Ti were obtained for cemented WC/Co samples, binderless and binder-containing pellets. Relative widths of uncertainty intervals about the centroids vary between ± 3% and ± 7%, and exceptionally reach a value above 10%. The lowest determinable quantities (LDQ) of Nb, Ta and Ti calculated from the calibration lines were less than 0.5% (m/m). To evaluate the possibility of quantitative elemental analysis by LA–ICP–OES, two real sintered WC/Co samples and two real samples of powdered WC/Co materials were analysed. The results of LA–ICP–OES real sample analysis correlated well with the results obtained by X-ray fluorescence (sintered samples) and pneumatic nebulization inductively coupled plasma optimal emmission spectrometry (powdered samples) with a bias not exceeding 6.5%.